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Sample records for absorption spectrometry f-aas

  1. Determination of Iron (Fe) and Calcium (Ca) in NIST SRM 1566b (Oyster tissue) using Flame Atomic Absorption Spectrometry (F-AAS) by Standard Addition Method

    OpenAIRE

    Fitri Dara; Y Susanto Ridwan

    2017-01-01

    NIST Standard Reference Material (SRM 1566b) was employed for the determination of Iron (Fe) andCalcium (Ca) as nutrients in food matrix using Flame Atomic Absorption Spectrometry (F-AAS). Thecertified value of SRM 1566b for Fe and Ca are 205.8 ± 6.8 mg/kg and 0.0838 ± 0.0020 (%) or 838 ±20 mg/kg, respectively. This certified values are based on results obtained by single primary method(Isotope Dilution Inductively Couple Plasma Mass Spectrometry) at NIST with confirmation by othermethods at ...

  2. Determination of Iron (Fe and Calcium (Ca in NIST SRM 1566b (Oyster tissue using Flame Atomic Absorption Spectrometry (F-AAS by Standard Addition Method

    Directory of Open Access Journals (Sweden)

    Fitri Dara

    2017-03-01

    Full Text Available NIST Standard Reference Material (SRM 1566b was employed for the determination of Iron (Fe andCalcium (Ca as nutrients in food matrix using Flame Atomic Absorption Spectrometry (F-AAS. Thecertified value of SRM 1566b for Fe and Ca are 205.8 ± 6.8 mg/kg and 0.0838 ± 0.0020 (% or 838 ±20 mg/kg, respectively. This certified values are based on results obtained by single primary method(Isotope Dilution Inductively Couple Plasma Mass Spectrometry at NIST with confirmation by othermethods at National Metrology Institute of P.R. China. This paper proposed a method fordetermination of Fe and Ca in food matrix as recommended by AOAC official with a littlemodification. The method was commenced from the destruction of all organic matter by dry oxidationbefore analysis by standard addition. Under optimum condition, the results of the determination of Feand Ca in SRM 1566b were agreed well with the certificate value. This method would be useful forroutine analysis in food testing laboratories.

  3. Flow Injection and Atomic Absorption Spectrometry (FI-AAS) -

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    1996-01-01

    absorption spectrometry (AAS). Initially with flame-AAS (fAAS) procedures, later for hydride generation (HG) techniques, and most recently in combination with electrothermal AAS (ETAAS). The common denominator for all these procedures is the inherently precise and strictly reproducible timing in FI from...... the point of sample injection/introduction to the point of detection. Hence, in FI-fAAS this feature allows not only to obtain improved repeatability but also improved accuracy, and because the wash to sample ratio is high it permits the handling of samples with elevated salt contents - which...... of (especially HG- forming) elements. In the words of the one of the authorities of AAS and foremost pioneers of FI-AAS - Professor Z. L. Fang, who is the author on two recently published monographs on this hyphenated technique - the impact of FI on AAS is "so dramatic" that it has brought "new vitality...

  4. Zeeman atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hadeishi, T.; McLaughlin, R.

    1978-08-01

    The design and development of a Zeeman atomic absorption spectrometer for trace element analysis are described. An instruction manual is included which details the operation, adjustment, and maintenance. Specifications and circuit diagrams are given. (WHK)

  5. Reliability of graphite furnace atomic absorption spectrometry as ...

    African Journals Online (AJOL)

    Purpose: To evaluate the comparative efficiency of graphite furnace atomic absorption spectrometry (GFAAS) and hydride generation atomic absorption spectrometry (HGAAS) for trace analysis of arsenic (As) in natural herbal products (NHPs). Method: Arsenic analysis in natural herbal products and standard reference ...

  6. Feasibility of dispersive liquid–liquid microextraction for extraction and preconcentration of Cu and Fe in red and white wine and determination by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Seeger, Tassia S.; Rosa, Francisco C.; Bizzi, Cezar A.; Dressler, Valderi L.; Flores, Erico M.M.; Duarte, Fabio A., E-mail: fabioand@gmail.com

    2015-03-01

    A method for extraction and preconcentration of Cu and Fe in red and white wines using dispersive liquid–liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Extraction was performed using sodium diethyldithiocarbamate as chelating agent and a mixture of 40 μL of 1,2-dichlorobenzene (extraction solvent) and 900 μL of methanol (dispersive solvent). Some parameters that influencing the extraction efficiency such as pH (2 to 5), concentration of chelating agent (0 to 2%), effect of salt addition (0 to 10%), number of washing steps (1 to 4) and centrifugation time (0 to 15 min) were studied. Accuracy was evaluated after microwave-assisted digestion in closed vessels and analytes were determined by inductively coupled plasma optical emission spectrometry. Agreement with the proposed method ranged from 91 to 110 and from 89 to 113% for Cu and Fe, respectively. Calibration of F AAS instrument was performed using analyte addition method and limits of detection were 6.3 and 2.4 μg L{sup −1} for Cu and Fe, respectively. The proposed method was applied for the determination of Cu and Fe in five samples of red wine and three samples of white wine, with concentration ranging from 21 to 178 μg L{sup −1} and from 1.38 to 3.74 mg L{sup −1}, respectively. - Highlights: • Determination of Cu and Fe in wine using DLLME and F AAS • High preconcentration factors and low LODs were achieved. • Alternative method for the determination of Cu and Fe in wine for routine analysis.

  7. Feasibility of dispersive liquid-liquid microextraction for extraction and preconcentration of Cu and Fe in red and white wine and determination by flame atomic absorption spectrometry

    Science.gov (United States)

    Seeger, Tassia S.; Rosa, Francisco C.; Bizzi, Cezar A.; Dressler, Valderi L.; Flores, Erico M. M.; Duarte, Fabio A.

    2015-03-01

    A method for extraction and preconcentration of Cu and Fe in red and white wines using dispersive liquid-liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Extraction was performed using sodium diethyldithiocarbamate as chelating agent and a mixture of 40 μL of 1,2-dichlorobenzene (extraction solvent) and 900 μL of methanol (dispersive solvent). Some parameters that influencing the extraction efficiency such as pH (2 to 5), concentration of chelating agent (0 to 2%), effect of salt addition (0 to 10%), number of washing steps (1 to 4) and centrifugation time (0 to 15 min) were studied. Accuracy was evaluated after microwave-assisted digestion in closed vessels and analytes were determined by inductively coupled plasma optical emission spectrometry. Agreement with the proposed method ranged from 91 to 110 and from 89 to 113% for Cu and Fe, respectively. Calibration of F AAS instrument was performed using analyte addition method and limits of detection were 6.3 and 2.4 μg L- 1 for Cu and Fe, respectively. The proposed method was applied for the determination of Cu and Fe in five samples of red wine and three samples of white wine, with concentration ranging from 21 to 178 μg L- 1 and from 1.38 to 3.74 mg L- 1, respectively.

  8. Atomic Absorption, Atomic Fluorescence, and Flame Emission Spectrometry.

    Science.gov (United States)

    Horlick, Gary

    1984-01-01

    This review is presented in six sections. Sections focus on literature related to: (1) developments in instrumentation, measurement techniques, and procedures; (2) performance studies of flames and electrothermal atomizers; (3) applications of atomic absorption spectrometry; (4) analytical comparisons; (5) atomic fluorescence spectrometry; and (6)…

  9. Absorption Mode FTICR Mass Spectrometry Imaging

    NARCIS (Netherlands)

    Smith, D.F.; Kilgour, D.P.A.; Konijnenburg, M.; O'Connor, P.B.; Heeren, R.M.A.|info:eu-repo/dai/nl/105188476

    2013-01-01

    Fourier transform ion cyclotron resonance mass spectrometry offers the highest mass resolving power for molecular imaging experiments. This high mass resolving power ensures that closely spaced peaks at the same nominal mass are resolved for proper image generation. Typically higher magnetic fields

  10. Reliability of graphite furnace atomic absorption spectrometry as ...

    African Journals Online (AJOL)

    Original Research Article. Reliability of graphite furnace atomic absorption spectrometry as alternative method for trace analysis of arsenic in natural medicinal products. Reem Saadi Khalid1*, ABM Helaluddin1, Reem Saadi Khalid1, Mohamed. Alaama1, Abdualrahman M Abdualkader1, Abdulrazak Kasmuri2 and Syed Atif.

  11. combination of flame atomic absorption spectrometry with ligandless

    African Journals Online (AJOL)

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    separation and flame atomic absorption spectrometry determination of trace amount of lead(II) ion. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction .... in ethanol was added to it. The final solution was aspirated directly into the flame of AAS. The extraction scheme of Pb(II) ion is shown in.

  12. Absorption Mode FT-ICR Mass Spectrometry Imaging

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Donald F.; Kilgour, David P.; Konijnenburg, Marco; O' Connor, Peter B.; Heeren, Ronald M.

    2013-12-03

    Fourier transform ion cyclotron resonance mass spectrometry offers the highest mass resolving power for molecular imaging experiments. This high mass resolving power ensures that closely spaced peaks at the same nominal mass are resolved for proper image generation. Typically higher magnetic fields are used to increase mass resolving power. However, a gain in mass resolving power can also be realized by phase correction of the data for absorption mode display. In addition to mass resolving power, absorption mode offers higher mass accuracy and signal-to-noise ratio over the conventional magnitude mode. Here we present the first use of absorption mode for Fourier transform ion cyclotron resonance mass spectrometry imaging. The Autophaser algorithm is used to phase correct each spectrum (pixel) in the image and then these parameters are used by the Chameleon work-flow based data processing software to generate absorption mode ?Datacubes? for image and spectral viewing. Absorption mode reveals new mass and spatial features that are not resolved in magnitude mode and results in improved selected ion image contrast.

  13. Simultaneous Atomic Absorption Spectrometry for Cadmium and Lead Determination in Wastewater: A Laboratory Exercise

    Science.gov (United States)

    Correia, Paulo R. M.; Oliveira, Pedro V.

    2004-01-01

    The simultaneous determination of cadmium and lead by multi-element atomic absorption spectrometry with electrochemical atomization is proposed by employing a problem-based approach. The reports indicate that the students assimilated the principles of the simultaneous atomic absorption spectrometry (SIMAAS), the role of the chemical modifier, the…

  14. The role of atomic absorption spectrometry in geochemical exploration

    Science.gov (United States)

    Viets, J.G.; O'Leary, R. M.

    1992-01-01

    In this paper we briefly describe the principles of atomic absorption spectrometry (AAS) and the basic hardware components necessary to make measurements of analyte concentrations. Then we discuss a variety of methods that have been developed for the introduction of analyte atoms into the light path of the spectrophotometer. This section deals with sample digestion, elimination of interferences, and optimum production of ground-state atoms, all critical considerations when choosing an AAS method. Other critical considerations are cost, speed, simplicity, precision, and applicability of the method to the wide range of materials sampled in geochemical exploration. We cannot attempt to review all of the AAS methods developed for geological materials but instead will restrict our discussion to some of those appropriate for geochemical exploration. Our background and familiarity are reflected in the methods we discuss, and we have no doubt overlooked many good methods. Our discussion should therefore be considered a starting point in finding the right method for the problem, rather than the end of the search. Finally, we discuss the future of AAS relative to other instrumental techniques and the promising new directions for AAS in geochemical exploration. ?? 1992.

  15. Pigment identification in artwork using graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Goltz, D M; Coombs, J; Marion, C; Cloutis, E; Gibson, J; Attas, M; Choo-Smith, L-P; Collins, C

    2004-06-17

    The use of a sampling technique is described for the identification of metals from inorganic pigments in paint. The sampling technique involves gently contacting a cotton swab with the painted surface to physically remove a minute quantity ( approximately 1-2mug) of pigment. The amount of material removed from the painted surface is invisible to the unaided eye and does not cause any visible effect to the painted surface. The cotton swab was then placed in a 1.5ml polystyrene beaker containing HNO(3) to extract pigment metals prior to analysis using graphite furnace atomic absorption spectrometry (GFAAS). GFAAS is well suited for identifying pigment metals since it requires small samples and many pigments consist of main group elements (e.g. Al) as well as transition metals (e.g. Zn, Fe and Cd). Using Cd (cadmium red) as the test element, the reproducibility of sampling a paint surface with the cotton swab was approximately 13% in either a water or oil medium. To test the feasibility of cotton sampling for pigment identification, samples were obtained from paintings (watercolour and oil) of a local collection. Raman spectra provided complementary information to the GFAAS, which together are essential for positive identification of some pigments. For example, GFAAS indicated the presence of Cu, but the Raman spectra positively identified the modern copper pigment phthalocyanine green (Cu(C(32)Cl(16)N(8)). Both Raman spectroscopy and GFAAS were useful for identifying ZnO as a white pigment.

  16. Determination of mercury in hair: Comparison between gold amalgamation-atomic absorption spectrometry and mass spectrometry.

    Science.gov (United States)

    Domanico, Francesco; Forte, Giovanni; Majorani, Costanza; Senofonte, Oreste; Petrucci, Francesco; Pezzi, Vincenzo; Alimonti, Alessandro

    2017-09-01

    Mercury is a heavy metal that causes serious health problems in exposed subjects. The most toxic form, i.e., methylmercury (MeHg), is mostly excreted through human hair. Numerous analytical methods are available for total Hg analysis in human hair, including cold vapour atomic fluorescence spectrometry (CV-AFS), inductively coupled plasma mass spectrometry (ICP-MS) and thermal decomposition amalgamation atomic absorption spectrometry (TDA-AAS). The aim of the study was to compare the TDA-AAS with the ICP-MS in the Hg quantification in human hair. After the washing procedure to minimize the external contamination, from each hair sample two aliquots were taken; the first was used for direct analysis of Hg by TDA-AAS and the second was digested for Hg determination by the ICP-MS. Results indicated that the two data sets were fully comparable (median; TDA-AAS, 475ngg -1 ; ICP-MS, 437ngg -1 ) and were not statistically different (Mann-Whitney test; p=0.44). The two techniques presented results with a good coefficient of correlation (r=0.94) despite different operative ranges and method limits. Both techniques satisfied internal performance requirements and the parameters for method validation resulting sensitive, precise and reliable. Finally, the use of the TDA-AAS can be considered instead of the ICP-MS in hair analysis in order to reduce sample manipulation with minor risk of contamination, less time consuming due to the absence of the digestion step and cheaper analyses. Copyright © 2016 Elsevier GmbH. All rights reserved.

  17. DETERMINATION OF TOTAL MERCURY IN FISH TISSUES USING PYROLYSIS ATOMIC ABSORPTION SPECTROMETRY WITH GOLD AMALGAMATION

    Science.gov (United States)

    A simple and rapid procedure for measuring total mercury in fish tissues is evaluated and compared with conventional techniques. Using an automated instrument incorporating combustion, preconcentration by amalgamation with gold, and atomic absorption spectrometry (AAS), mill...

  18. EPA Method 245.1: Determination of Mercury in Water by Cold Vapor Atomic Absorption Spectrometry

    Science.gov (United States)

    SAM lists this method for preparation and analysis of aqueous liquid and drinking water samples. This method will determine mercuric chloride and methoxyethylmercuric acetate as total mercury using cold vapor atomic absorption spectrometry.

  19. Differentiation and classification of beers with flame atomic spectrometry and molecular absorption spectrometry and sample preparation assisted by microwaves

    Science.gov (United States)

    Bellido-Milla, Dolores; Moreno-Perez, Juana M.; Hernández-Artiga, María. P.

    2000-07-01

    The characterization of beer samples has a lot of interest because their composition can affect the taste and stability of beer and consumer health. Flame atomic absorption spectrometry was used to determine Fe, Mn, Zn, Cu, Mg, Ca and Al. Sodium and K were determined by flame atomic emission spectrometry. A sample preparation method was developed, based on treatment with HNO 3 and H 2O 2 in a microwave oven. This has many advantages over the methods found in the literature. The combination of the results of atomic spectrometry and the spectrum obtained by molecular absorption spectrometry provides information on the inorganic and organic components of the samples. The application of chemometric techniques to chemical composition data could be extremely useful for food quality control. The metal concentrations, the molecular absorption spectrum, the pH and conductivity of each sample were subject to analysis of variance and linear discriminant analysis. Twenty-five different beer samples were used to differentiate and classify different types of beers.

  20. Determination of silicon in biomass and products of pyrolysis process via high-resolution continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Nakadi, Flávio V; Prodanov, Caroline; Boschetti, Wiliam; Vale, Maria Goreti R; Welz, Bernhard; de Andrade, Jailson B

    2018-03-01

    Thermochemical processes can convert the biomass into fuels, such as bio-oil. The biomass submitted to pyrolysis process, such as fibers, are generally rich in silicon, an element that can lead to damages in an engine when there is high concentration in a fuel. High-resolution continuum source atomic absorption spectrometry (HR-CS AAS) is an interesting alternative for Si determination in the products and byproducts of the pyrolysis process because, besides the flame (F) and graphite furnace (GF) atomizers, it has enhanced the application of direct analysis of solid samples (SS) within GF. This study aimed the development of methods to determine Si in biomass samples, their products and byproducts using HR-CS AAS. A high-resolution continuum source atomic absorption spectrometer contrAA 700 equipped with F and GF atomizers was used throughout the study. HR-CS F AAS (λ = 251.611nm, 1 detection pixel, N2O/C2H2 flame) was used to evaluate Si content in biomass and ash, after a microwave-assisted acid digestion with HNO3 and HF. HR-CS GF AAS (Tpyr = 1400°C, Tatom = 2650°C) has evaluated Si in pyrolysis water and bio-oil at 251.611nm, and in peach pit biomass and ash at 221.174nm using SS, both wavelengths with 1 detection pixel. Rhodium (300μg) was applied as permanent modifier and 10μgPd + 6μg Mg were pipetted onto the standards/samples at each analysis. Three different biomass samples were studied: palm tree fiber, coconut fiber and peach pit, and three certified reference materials (CRM) were used to verify the accuracy of the methods. The figures of merit were LOD 0.09-20mgkg-1, and LOQ 0.3-20mgkg-1, considering all the methods. There were no significant differences between the CRM certified values and the determined ones, using a Student t-test with a confidence interval of 95% (n = 5). Si concentration ranged from 0.11-0.92% mm-1, 1.1-1.7mgkg-1, 3.3-13mgkg-1, and 0.41-1.4%mm-1, in biomass, bio-oil, pyrolysis water and ash, respectively. Si remained mostly

  1. determination of vanadium in foods by atomic absorption spectrometry

    African Journals Online (AJOL)

    This paper presents an assessment of the level of vanadium in foods (Plantain, Musa spp; Yam, Discorea rotundata; and Maize, Zea mays) from ten popular market places in Lagos metropolis, Nigeria. Total acid leaching digestion method was employed and determination was by Flame Atomic Absorption ...

  2. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    Science.gov (United States)

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC.

  3. Continuum Source Atomic Absorption Spectrometry with a Photodiode Array Detector

    Science.gov (United States)

    Fernando, Reshan Armedious

    The designed continuum source atomic absorption spectrometer consists of a 300W xenon arc lamp (ILC Technology), a flame (Perkin-Elmer) or graphite furnace (Perkin-Elmer, Model HGA 2200) atomizer, a 1.33M focal length high resolution monochromator with 3600 gr/mm grating (McPherson, Model 209), and a 2048-element self scanning linear photodiode array detector (Princeton Instruments, Model PDA-2048). Detector operation, data acquisition and processing was done by using a 66MHz 486 DX/2 personal computer (Gateway 2000). In stage one, the system was optimized for flame atomization. The optimum lamp current, entrance slit width and height were found to be 10A, 20 mum, and 4 mm respectively. The resulted spectral band-pass of the monochromator/PDA combination is on the order of the average atomic absorption profile half-width (0.003 -0.004 nm). The flame parameters such as observation height, air/fuel ratio, and solution uptake rate were optimized along with the detector parameters such as exposure and accumulation for the lowest possible detection limit. The system has clearly demonstrated its multi-element detection capabilities. The calculated detection limits for the present system with an air-acetylene flame is approximately one order of magnitude lower than previously reported CSAAS detection limits, and are on the same order of magnitude as those commonly observed with single element hollow cathode lamp systems. In stage two, flame atomizer was replaced by a graphite furnace atomizer. When compared to the static signal given out by flame atomizer, the graphite furnace produces transient signals. Fast response time of the PDA is well within the time scale of the transient signals produce in graphite furnace and the multi-wavelength detection allows the background correction to be performed by visual inspection. The detection limits calculated for the present system are significantly lower than those previously reported for multi-element CSAAS systems, and are on

  4. Rapid accurate analysis of metal (oxide)-on-silica catalysts by atomic absorption spectrometry

    NARCIS (Netherlands)

    Jütte, B.A.H.G.; Heikamp, A.; Agterdenbos, J.

    1979-01-01

    The catalysts, which contain 10–60% copper, chromium, nickel and silicon, are decomposed in sealed Teflon-lined vessels and analyzed by atomic absorption spectrometry. Matrix matching and bracketing standards are applied. The RSD of a single determination is about 1% for all components.

  5. COMPREHENSIVE ANALYSIS OF BIOLOGICALLY RELEVANT ARSENICALS BY PH-SELECTIVE HYDRIDE GENERATION-ATOMIC ABSORPTION SPECTROMETRY

    Science.gov (United States)

    A method based on pH-selective generation and separation of arsines is commonly used for analysis of inorganic, methylated, and dimethylated trivalent and pentavalent arsenicals by hydride generation-atomic absorption spectrometry (HG-AAS). We have optimized this method to pe...

  6. Dielectric barrier discharge plasma atomizer for hydride generation atomic absorption spectrometry-Performance evaluation for selenium

    Czech Academy of Sciences Publication Activity Database

    Duben, Ondřej; Boušek, J.; Dědina, Jiří; Kratzer, Jan

    2015-01-01

    Roč. 111, SEP (2015), s. 57-63 ISSN 0584-8547 Grant - others:GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation-atomic absorption spectrometry * selenium Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.289, year: 2015

  7. Determination of Cd in urine by cloud point extraction-tungsten coil atomic absorption spectrometry.

    Science.gov (United States)

    Donati, George L; Pharr, Kathryn E; Calloway, Clifton P; Nóbrega, Joaquim A; Jones, Bradley T

    2008-09-15

    Cadmium concentrations in human urine are typically at or below the 1 microgL(-1) level, so only a handful of techniques may be appropriate for this application. These include sophisticated methods such as graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry. While tungsten coil atomic absorption spectrometry is a simpler and less expensive technique, its practical detection limits often prohibit the detection of Cd in normal urine samples. In addition, the nature of the urine matrix often necessitates accurate background correction techniques, which would add expense and complexity to the tungsten coil instrument. This manuscript describes a cloud point extraction method that reduces matrix interference while preconcentrating Cd by a factor of 15. Ammonium pyrrolidinedithiocarbamate and Triton X-114 are used as complexing agent and surfactant, respectively, in the extraction procedure. Triton X-114 forms an extractant coacervate surfactant-rich phase that is denser than water, so the aqueous supernatant is easily removed leaving the metal-containing surfactant layer intact. A 25 microL aliquot of this preconcentrated sample is placed directly onto the tungsten coil for analysis. The cloud point extraction procedure allows for simple background correction based either on the measurement of absorption at a nearby wavelength, or measurement of absorption at a time in the atomization step immediately prior to the onset of the Cd signal. Seven human urine samples are analyzed by this technique and the results are compared to those found by the inductively coupled plasma mass spectrometry analysis of the same samples performed at a different institution. The limit of detection for Cd in urine is 5 ngL(-1) for cloud point extraction tungsten coil atomic absorption spectrometry. The accuracy of the method is determined with a standard reference material (toxic metals in freeze-dried urine) and the determined values agree with

  8. A double cell for X-ray absorption spectrometry of atomic Zn

    CERN Document Server

    Mihelic, A; Arcon, I; Padeznik-Gomilsek, J; Borowski, M

    2002-01-01

    A high-temperature cell with a double wall design has been constructed for X-ray absorption spectrometry of metal vapors. The inner cell, assembled from a corundum tube and thin plates without welding or reshaping, serves as a container of the vapor sample. It is not vacuum tight: instead, the outer tube provides inert atmosphere. Several spectra of K-edge atomic absorption of Zn were obtained in the stationary working regime below the Zn boiling point. The K-edge profile shows an extremely strong resonance and, above the continuum threshold, coexcitations of the outer electrons.

  9. Direct determination of selenoproteins in polyvinylidene difluoride membranes by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Sidenius, U; Gammelgaard, Bente

    2000-01-01

    A method for the direct determination of selenoproteins in plastic membranes after protein separation by gel electrophoresis was developed. Quantification was based on the determination of the selenium content of the proteins by electrothermal atomic absorption spectrometry (ET-AAS) after manual...... were excised and chemical modifier was added on top of the excised membrane prior to atomic absorption measurement. Acceptable linearity was achieved in the range 2-10 ng Se, corresponding to selenium concentrations close to 1 mg/L, when aqueous solutions of selenomethionine standard as well...

  10. [Determination of stannum in urine by graphite furnace atomic absorption spectrometry].

    Science.gov (United States)

    Chen, Jiu; Wu, Shihua; Guo, Guanhao; Liu, Yimin

    2015-12-01

    To establish the method of graphite furnace atomic absorption spectrometry for the measurement of stannum in urine with calcium nitrate as the matrix modifier. Graphite tube was pretreated with calcium nitrate as the matrix modifier, the urine sample was diluted with 1% nitric acid and then direct injection was performed for these samples, and graphite furnace atomic absorption spectrometry was applied for measurement. The concentration of stannum in urine showed a good linear relationship within the range of 8.0~40.0 μg/L, with a correlation coefficient of 0.9981. The minimum detectable concentration was 0.72 μg/L, the degree of precision was 1.54%~6.69%, and the recovery rate was 99.23%~107.63%. This method can determine the content of stannum in urine accurately and rapidly, with a high sensitivity and a low cost.

  11. Cadmium determination in urine by atomic absorption spectrometry as a screening test in industrial medicine

    Science.gov (United States)

    Lehnert, G.; Klavis, G.; Schaller, K. H.; Haas, T.

    1969-01-01

    Lehnert, G., Klavis, G., Schaller, K. H., and Haas, T. (1969).Brit. J. industr. Med.,26, 156-158. Cadmium determination in urine by atomic absorption spectrometry as a screening test in industrial medicine. Cadmium was determined by atomic absorption spectrometry in the urine and serum of 18 workers exposed to cadmium dust and fume in a zinc smelting plant. In all cases the concentrations of cadmium in the serum were within the normal range, but those in the urine were elevated. The elevated urine concentrations showed that the exposed group had taken up more cadmium than normal, although they showed no clinical symptoms of cadmium poisoning. Analysis of urine for cadmium is therefore of value in preventive medicine, and should be used for periodic check-ups on those occupationally exposed. PMID:5780108

  12. Determination of elements by atomic absorption spectrometry in medicinal plants employed to alleviate common cold symptoms.

    Science.gov (United States)

    Küçükbay, F Zehra; Kuyumcu, Ebru

    2014-09-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of common cold have been studied for their mineral contents. Eleven minor and major elements (essential, non-essential and toxic) were identified in the Asplenium adiantum-nigrum L. , Althaea officinalis L. , Verbascum phlomoides L., Euphorbia chamaesyce L., Zizyphus jujube Miller, Peganum harmala L., Arum dioscoridis Sm., Sambucus nigra L., Piperlongum L., Tussilago farfara L. and Elettaria cardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrometry. Microwave digestion procedure for total concentration was applied under optimized conditions for dissolution of medicinal plants. Plant based biological certified reference materials (CRMs) served as standards for quantification. These elements are found to be present in varying concentrations in the studied plants. The baseline data presented in this work can be used in understanding the role of essential, non-essential and toxic elements in nutritive, preventive and therapeutic properties of medicinal plants.

  13. Gold volatile species atomization and preconcentration in quartz devices for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Arslan, Y.; Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan; Dědina, Jiří

    103-104, JAN-FEB (2015), s. 155-163 ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant - others:GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : gold * volatile species generation * quartz atomizers * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.289, year: 2015

  14. Bismuth as a general internal standard for lead in atomic absorption spectrometry.

    Science.gov (United States)

    Bechlin, Marcos A; Fortunato, Felipe M; Ferreira, Edilene C; Gomes Neto, José A; Nóbrega, Joaquim A; Donati, George L; Jones, Bradley T

    2014-06-11

    Bismuth was evaluated as internal standard for Pb determination by line source flame atomic absorption spectrometry (LS FAAS), high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and line source graphite furnace atomic absorption spectrometry (LS GFAAS). Analysis of samples containing different matrices indicated close relationship between Pb and Bi absorbances. Correlation coefficients of calibration curves built up by plotting A(Pb)/A(Bi)versus Pb concentration were higher than 0.9953 (FAAS) and higher than 0.9993 (GFAAS). Recoveries of Pb improved from 52-118% (without IS) to 97-109% (IS, LS FAAS); 74-231% (without IS) to 96-109% (IS, HR-CS FAAS); and 36-125% (without IS) to 96-110% (IS, LS GFAAS). The relative standard deviations (n=12) were reduced from 0.6-9.2% (without IS) to 0.3-4.3% (IS, LS FAAS); 0.7-7.7% (without IS) to 0.1-4.0% (IS, HR-CS FAAS); and 2.1-13% (without IS) to 0.4-5.9% (IS, LS GFAAS). Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Analysis of Dithiocarbamate Fungicides in Vegetable Matrices Using HPLC-UV Followed by Atomic Absorption Spectrometry.

    Science.gov (United States)

    Al-Alam, Josephine; Bom, Laura; Chbani, Asma; Fajloun, Ziad; Millet, Maurice

    2017-04-01

    A simple method combining ion-pair methylation, high-performance liquid chromatography (HPLC) analysis with detection at 272 nm and atomic absorption spectrometry was developed in order to determine 10 dithiocarbamate fungicides (Dazomet, Metam-sodium, Ferbam, Ziram, Zineb, Maneb, Mancozeb, Metiram, Nabam and Propineb) and distinguish ethylenbisdithiocarbamates (EBDTCs) Zineb, Maneb and Mancozeb in diverse matrices. This method associates reverse phase analysis by HPLC analysis with detection at 272 nm, with atomic absorption spectrometry in order to distinguish, with the same extraction protocol, Maneb, Mancozeb and Zineb. The limits of detection (0.4, 0.8, 0.5, 1.25 and 1.97) and quantification (1.18, 2.5, 1.52, 4.2 and 6.52) calculated in injected nanogram, respectively, for Dazomet, Metam-Na, dimethyldithiocarbamates (DMDTCs), EBDTCs and propylenebisdithiocarbamates (PBDTCs) justify the sensitivity of the method used. The coefficients of determination R2 were 0.9985, 0.9978, 0.9949, 0.988 and 0.9794, respectively, for Dazomet, Metam-Na, DMDTCs, EBDTCs and PBDTCs, and the recovery from fortified apple and leek samples was above 90%. Results obtained with the atomic absorption method in comparison with spectrophotometric analysis focus on the importance of the atomic absorption as a complementary specific method for the distinction between different EBDTCs fungicides. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  16. Determination of serum lithium: comparison between atomic emission and absorption spectrometry methods

    Directory of Open Access Journals (Sweden)

    Carlos Elielton do Espírito Santo

    2014-02-01

    Full Text Available Introduction: The therapeutic monitoring of lithium, through concentration measurements, is important for individual dose adjustment, as a marker of treatment adherence and to prevent poisoning and side effects. Objectives: Validate and compare two methods - atomic emission and atomic absorption - for the determination of lithium in serum samples. Methodology: Parameters such as specificity, precision, accuracy, limit of detection (LOD and linearity were considered. The atomic absorption spectrometer was used, operating in either emission or absorption mode. For the quantitative comparison of 30 serum samples from patients with mood disorder treated with lithium, the results were submitted to Student's t-test, F-test and Pearson's correlation. Results: The limit of quantification (LOQ was established as 0.05 mEq/l of lithium, and calibration curves were constructed in the range of 0.05-2 mEq/l of lithium, using aqueous standards. Sample preparation time was reduced, what is important in medical laboratory. Conclusion: Both methods were considered satisfactory, precise and accurate and can be adopted for lithium quantification. In the comparison of quantitative results in lithium-treated patients through statistical tests, no significant differences were observed. Therefore the methods for lithium quantification by flame atomic absorption spectrometry (FAAS and flame atomic emission spectrometry (FAES may be considered similar.

  17. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  18. Flow Injection and Atomic Absorption Spectrometry - An Effective and Attractive Analytical Chemical Combination

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Nielsen, Steffen

    1998-01-01

    One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atomic...... absorption spectrometry (AAS). Initially with flame-AAS (FAAS) procedures, later for hydride generation (HG) techniques, and most recently in combination with electrothermal AAS (ETAAS). The common denominator for all these procedures is the inherently precise and strictly reproducible timing that the sample...

  19. Determination of nanogram amounts of bismuth in rocks by atomic absorption spectrometry with electrothermal atomization

    Science.gov (United States)

    Kane, J.S.

    1979-01-01

    Bismuth concentrations as low as 10 ng g-1 in 100-mg samples of geological materials can be determined by atomic absorption spectrometry with electrothermal atomization. After HF-HClO4 decomposition of the sample, bismuth is extracted as the iodide into methyl isobutyl ketone and is then stripped with ethylenediaminetetraacetic acid into the aqueous phase. Aliquots of this solution are pipetted into the graphite furnace and dried, charred, and atomized in an automated sequence. Atomic absorbance at the Bi 223.1-nm line provides a measure of the amount of bismuth present. Results are presented for 14 U.S. Geological Survey standard rocks. ?? 1979.

  20. Direct solid sampling by flame atomic absorption spectrometry: determination of manganese in coal samples

    Directory of Open Access Journals (Sweden)

    Flores Érico M. M.

    2004-01-01

    Full Text Available A new device for the direct solid analysis by flame atomic absorption spectrometry was investigated as an alternative technique for the determination of trace elements in coal. The potential application of the proposed procedure for the determination of manganese was investigated. Ground coal test samples were weighed directly into polyethylene vials and carried as a dry aerosol to a slotted quartz vaporization cell placed between the flame burner and optical path. The transient signals obtained were totally integrated in 1 second. The effect of operating conditions on the analytical signal was investigated. Background signals were always low and a Mn characteristic mass of 1.9 ng was found. Results were considered satisfactory regarding to both accuracy (between 97.5 and 103.2% and precision (RSD better than 6%. The proposed system is simple and can be easily adapted to any conventional atomic absorption spectrometers allowing the analysis of more than 80 test samples in an hour.

  1. Determination of tetraalkyllead compounds in gasoline by liquid chromatography-atomic absorption spectrometry

    Science.gov (United States)

    Messman, J.D.; Rains, T.C.

    1981-01-01

    A liquid chromatography-atomic absorption spectrometry (LC-AAS) hybrid analytical technique is presented for metal speciation measurements on complex liquid samples. The versatility and inherent metal selectivity of the technique are Illustrated by the rapid determination of five tetraalkyllead compounds in commercial gasoline. Separation of the individual tetraalkyllead species is achieved by reversed-phase liquid chromatography using an acetonitrile/water mobile phase. The effluent from the liquid Chromatograph Is introduced directly into the aspiration uptake capillary of the nebulizer of an air/acetylene flame atomic absorption spectrometer. Spectral interferences due to coeluting hydrocarbon matrix constituents were not observed at the 283.3-nm resonance line of lead used for analysis. Detection limits of this LC-AAS hydrid analytical technique, based on a 20-??L injection, are approximately 10 ng Pb for each tetraalkyllead compound.

  2. [Determination of indium in whole blood by graphite furnace atomic absorption spectrometry].

    Science.gov (United States)

    He, Juntao; Liu, Fen; Xiang, Yingping; Li, Zhimin

    2015-08-01

    To investigate the sensitization effect of different chemical modifiers in the determination of indium in whole blood by graphite furnace atomic absorption spectrometry, and to develop a new method for the determination of indium in whole blood. A mixture of 0.3% HNO3 (V/V) + 0.1% Triton X-100 (V/V) was used as a diluent, and a solution of 1 000 µg/ml Pd (NO3)2 + 3 000 µg/ml Mg (NO3)2 was used as modifier. After being diluted five times, the concentration of indium of the blood was directly determined by graphite furnace atomic absorption spectrometry. The detection limit of the method was 0.33 µg/L, the linear range was 0.33~100.00 µg/L, the relative standard deviation was 1.43%~2.65%, and the recovery rate was 98.3%~105.3%. The method is simple and fast and has high recovery and precision, and it is suitable for the determination of indium in whole blood.

  3. Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

    2016-12-01

    The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

  4. Determination of total mercury by vapor generation in situ trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, H.; Krawczyk, M. [Poznan Technical University, Poznan (Poland)

    2008-07-01

    The analytical performance of non-chromatographic coupled hydride generation, integrated atom trap (HG-IAT) atomizer flame absorption spectrometry (FAAS) systems were evaluated for the determination of total mercury in environmental samples. Mercury, using formation of mercury vapors were atomized in air-acetylene flame-heated IAT. A new design of vapor generation integrated atom trap flame atomic absorption spectrometry (VG-IAT-FAAS) hyphenated technique that would exceed the operational capabilities of existing arrangements was investigated. This novel approach enables to decrease the detection limit down to low pg mL{sup -1} levels. The concentration detection limit, defined as 3 times the blank standard deviation was 0.4 ng mL{sup -1}. For a 120 s in situ pre-concentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 750 folds for Hg, using vapor generation-atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed by RSD, was 9.3% (n = 6) for Hg. Reference and real sample materials were analyzed. The accuracy of the method was verified by the use of certified reference materials and by aqueous standard calibration technique. The measured Hg content, in reference materials, were in satisfactory agreement with the certified values, The hyphenated technique was applied for mercury determinations in coal fly ash, sewage and water.

  5. [The application of atomic absorption spectrometry in automatic transmission fault detection].

    Science.gov (United States)

    Chen, Li-dan; Chen, Kai-kao

    2012-01-01

    The authors studied the innovative applications of atomic absorption spectrometry in the automatic transmission fault detection. After the authors have determined Fe, Cu and Cr contents in the five groups of Audi A6 main metal in automatic transmission fluid whose travel course is respectively 10-15 thousand kilometers, 20-26 thousand kilometers, 32-38 thousand kilometers, 43-49 thousand kilometers, and 52-58 thousand kilometers by atomic absorption spectrometry, the authors founded the database of primary metal content in the Audi A6 different mileage automatic transmission fluid (ATF). The research discovered that the main metal content in the automatic transmission fluid increased with the vehicles mileage and its normal metal content level in the automatic transmission fluid is between the two trend lines. The authors determined the main metal content of automatic transmission fluid which had faulty symptoms and compared it with its database value. Those can not only judge the wear condition of the automatic transmission which had faulty symptoms but also help the automobile detection and maintenance personnel to diagnose automatic transmission failure reasons without disintegration. This reduced automobile maintenance costs, and improved the quality of automobile maintenance.

  6. Feasibility of high-resolution continuum source molecular absorption spectrometry in flame and furnace for sulphur determination in petroleum products

    Energy Technology Data Exchange (ETDEWEB)

    Kowalewska, Zofia, E-mail: zofia.kowalewska@obr.pl

    2011-07-15

    For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the {Delta}{nu} = 0 vibrational sequence within the electronic transition X{sup 1}{Sigma}{sup +} {yields} A{sup 1}{Pi}, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of Pd{sub x}S{sub y} molecules. At the 258.056 nm line, with the wavelength range covering central pixel {+-} 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg{sup -1} in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg{sup -1} in flame molecular absorption spectrometry. The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with

  7. Implementation of suitable flow injection/sequential-sample separation/preconcentration schemes for determination of trace metal concentrations using detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    2002-01-01

    Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS...

  8. Determination of some heavy metals by flame atomic absorption spectrometry before coprecipitation with neodymium hydroxide.

    Science.gov (United States)

    Soylak, Mustafa; Kizil, Nebiye

    2011-01-01

    A procedure is described for the determination of trace amounts of Cd(II), Ni(II), Cu(II), Pb(II), Fe(III), Co(II), and Mn(II) that combines flame atomic absorption spectrometry with neodymium hydroxide coprecipitation. The influences of analytical parameters (amount of neodymium, pH of the model solutions, etc.) that affect quantitative recoveries of the analyte ions were investigated. The effects of concomitant ions were also examined. The detection limits for analytes were found in the range of 0.2-3.3 microg/L. The validation of the presented procedure was controlled by analysis of certified reference materials (National Institute of Standards and Technology 1570a spinach leaves and TMDA 54.4 fortified lake water). The applications of the procedure were performed by the analysis of water, food, and herbal plants from Turkey.

  9. Determination of Aluminum in Dialysis Concentrates by Atomic Absorption Spectrometry after Coprecipitation with Lanthanum Phosphate.

    Science.gov (United States)

    Selvi, Emine Kılıçkaya; Şahin, Uğur; Şahan, Serkan

    2017-01-01

    This method was developed for the determination of trace amounts of aluminum(III) in dialysis concentrates using atomic absorption spectrometry after coprecipitation with lanthanum phosphate. The analytical parameters that influenced the quantitative coprecipitation of analyte including amount of lanthanum, amount of phosfate, pH and duration time were optimized. The % recoveries of the analyte ion were in the range of 95-105 % with limit of detection (3s) of 0.5 µg l-1. Preconcentration factor was found as 1000 and Relative Standard Deviation (RSD) % value obtained from model solutions was 2.5% for 0.02 mg L-1. The accuracy of the method was evaluated with standard reference material (CWW-TMD Waste Water). The method was also applied to most concentrated acidic and basic dialysis concentrates with satisfactory results.

  10. Determination of cobalt in human biological liquids from electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Dragan, Felicia; Hîncu, Lucian; Bratu, Ioan

    2009-08-01

    Problems and possibilities of the determination of Co in serum and urine samples by electrothermal atomic absorption spectrometry (ETAAS) are described. Optimal instrumental parameters as well as a suitable atomizer, calibration procedure and hydrogen peroxide as modifier are proposed for direct ETAAS measurement of Co in serum and urine. The detection limit achieved was 0.1 μg L-1 for both matrices and relative standard deviations varied in the range 5-20% depending on the Co concentration in the sample. The validity of the method was verified by the analyses of standard reference materials. For serum samples with Co content lower than the detection limit, a separation and preconcentration procedure based on liquid/liquid extraction is suggested prior to determination of Co in the organic phase by ETAAS. This procedure permits determination of 0.02 μg L-1 Co in serum samples with a relative standard deviation of 10-18%.

  11. Multicomutation flow system for manganese speciation by solid phase extraction and flame atomic absorption spectrometry

    Science.gov (United States)

    Tobiasz, Anna; Sołtys, Monika; Kurys, Ewa; Domagała, Karolina; Dudek-Adamska, Danuta; Walas, Stanisław

    2017-08-01

    In the paper an application of solid phase extraction technique for speciation analysis of manganese in water samples with the use of flame atomic absorption spectrometry is presented. Two types of sorbents, activated silica gel and Dowex 1 × 4, were used respectively for simultaneously Mn2 + and MnO42 - retention and preconcentration. The whole procedure was realized in multicomutation flow system. Different conditions like: type and concentration of eluent, sample pH and loading time were tested during the study. Under appropriate conditions, it was possible to obtained enrichment factors of 20 and 16 for Mn(II) and Mn(VII), respectively. Precision of the procedure was close to 4% (measured as relative standard deviation), whereas the detection limit (3σ) was 1.4 μg·L- 1 for Mn(II) and 4.8 μg·L- 1 for Mn(VII).

  12. Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

    Science.gov (United States)

    de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2016-09-14

    An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. [Graphite furnace atomic absorption spectrometry for determination of thallium in blood].

    Science.gov (United States)

    Zhang, Q L; Gao, G

    2016-04-20

    Colloidal palladium was used as chemical modifier in the determination of blood thallium by graphite furnace atomic absorption spectrometry. Blood samples were precipitated with 5% (V/V)nitric acid, and then determined by GFAAS with colloidal palladium used as a chemical modifier. 0.2% (W/V)sodium chloride was added in the standard series to improve the matrix matching between standard solution and sample. The detection limit was 0.2 μg/L. The correlation coefficient was 0.9991. The recoveries were between 93.9% to 101.5%.The relative standard deviations were between 1.8% to 2.7%.The certified reference material of whole blood thallium was determined and the result was within the reference range Conclusion: The method is accurate, simple and sensitive, and it can meet the needs of detection thallium in blood entirely.

  14. Chromium determination in fly ash by slurry-sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Baralkiewicz, D; Lamont, S.; Stemerowicz, M. [Adam Mickiewicz University of Poznan, Poznan (Poland). Dept. of Water & Soil Analysis

    2002-07-01

    The paper reports analytical conditions for determination of chromium in fly ash by slurry sampling electrothermal atomic absorption spectrometry (SS ETAAS). Stability test for slurries have been carried out. Triton X-100 was used as a stabilizing agent. The procedure was validated by analysis of certified reference coal fly ash material SRM 1633B. The results of determination of chromium by SS ETAAS in three real fly ash samples from Poland (Szczecin area) and Canada (Sydney, Nova Scotia area) were compared with the results of these samples analysed by the wet digestion method. The detection limit calculated to 0.077 mg/kg and relative standard deviation (RSD) of measurements for the slurry sampling method was 3.5-5.2% for SRM 1633B.

  15. Determination of selenium in Teucrium species by hydride generation atomic absorption spectrometry.

    Science.gov (United States)

    Jurisić, Renata; Vladimir-Knezević, Sanda; Kalodera, Zdenka; Grgić, Jerica

    2003-01-01

    Hydride generation atomic absorption spectrometry (HGAAS) was applied for determination of selenium content in dried aerial parts of wild and cultivated Teucrium species (Lamiaceae) growing in Croatia: T. arduini L., T. chamaedrys L., T. flavum L., T. montanum L., T. polium L., and T. scordium L. subsp. scordioides Schreb. Special attention was paid to the wet oxidation procedure for the sample dissolution. The proposed procedure involved microwave-assisted sample digestion using a mixture of HNO3/H2O2. Wild specimens generally had a higher content of selenium, with concentrations of 0.030-0.095 mg/kg of the dry drug. Cultivated plants contained 0.020-0.055 mg Se/kg.

  16. Determination of vanadium in mussels by electrothermal atomic absorption spectrometry without chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Saavedra, Y.; Fernandez, P. [Centro de Control do Medio Marino, Peirao de Vilaxoan s/n, Vilagarcia de Arousa, 36611 Pontevedra (Spain); Gonzalez, A. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, 15706, Santiago de Compostela (Spain)

    2004-05-01

    A method was developed for the quantitative determination of total vanadium concentration in mussels via electrothermal atomic absorption spectrometry (ETAAS). After the microwave digestion of the samples, a program using temperatures of 1600 C and 2600 C for ashing and atomization respectively, without any matrix modifiers, allowed us to obtain results that were satisfactory since they agreed closely with certified reference material values. The detection limit was 0.03 mg kg{sup -1} (dry weight), indicating that the method is suitable for the analysis of mussel samples. This determination was compared with matrix modifiers that have been reported previously. The method was applied to various cultivated and wild mussels from the Galician coast, yielding levels below 1 mg kg{sup -1} (wet weight). (orig.)

  17. High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

    2017-03-01

    In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

  18. Application of thermospray flame furnace atomic absorption spectrometry for investigation of silver nanoparticles.

    Science.gov (United States)

    Sirirat, Natnicha; Tetbuntad, Kornrawee; Siripinyanond, Atitaya

    2017-03-01

    Thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was applied to investigate the time-dependent absorption peak profile of various forms of silver. The thermospray flame furnace was set up with a 10-cm-long nickel tube with six holes, each 2.0 mm in diameter, to allow the flame to enter, and this nickel tube acted as a furnace. A sample of 300 μL was introduced into this furnace by use of water as a carrier at a flow rate of 0.5 mL min-1 through the ceramic capillary (0.5-mm inner diameter and 2.0-mm outer diameter), which was inserted into the front hole of the nickel tube. The system was applied to examine atomization behaviors of silver nanoparticles (AgNPs) with particle sizes ranging from 10 to 100 nm. The atomization rate of AgNPs was faster than that of the dissolved silver ion. With increased amount of silver, the decay time observed from the time-dependent absorption peak profile was shortened in the case of dissolved silver ion, but it was increased in the case of AgNPs. With the particle size ranging from 10 to 100 nm, the detection sensitivity was indirectly proportional to the particle size, suggesting that TS-FF-AAS may offer insights into the particle size of AgNPs provided that the concentration of the silver is known. To obtain quantitative information on AgNPs, acid dissolution of the particles was performed before TS-FF-AAS analysis, and recoveries of 80-110% were obtained.

  19. Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection

    Czech Academy of Sciences Publication Activity Database

    Huber, C. S.; Vale, M. G. R.; Dessuy, M. B.; Svoboda, Milan; Musil, Stanislav; Dědina, Jiří

    2017-01-01

    Roč. 175, DEC (2017), s. 406-412 ISSN 0039-9140 R&D Projects: GA MŠk(CZ) LH15174 Institutional support: RVO:68081715 Keywords : slurry sampling * methyl-substituted arsenic species * hydride generation-cryotrapping-atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 4.162, year: 2016

  20. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2014-11-01

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L{sup −1} HNO{sub 3} solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L{sup −1} and 36.4 mg L{sup −1}, respectively. The repeatability of the results expressed as relative standard deviation was typically < 5%. The accuracy of the method was tested by analysis of digested biological certified reference materials (soya bean flour, corn flour and herbs) and recovery experiment for beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93–105% with the repeatability in the range of 4.1–5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg{sup −1}), egg white (2188 ± 29 mg kg{sup −1}), mineral water (31.0 ± 0.9 mg L{sup −1}), white wine (260 ± 4 mg L{sup −1}) and red wine (82 ± 2 mg L{sup −1}), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L{sup −1}). - Highlights: • HR-CS FMAS technique was used for sulfur measurement via molecular absorption of carbon monosulfide, CS. • Organic DL

  1. Low-resolution continuum source simultaneous multi-element electrothermal atomic absorption spectrometry: steps into practice

    Science.gov (United States)

    Katskov, Dmitri

    2015-03-01

    The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D2 and Xe lamps within 200-400 nm wavelengths range with a low resolution spectral instrument and linear charge-coupled device. The setup permits the acquisition of 200 spectra during 1 s atomization pulse. Respective data matrix absorbance vs wavelength/time is employed for the quantification of elements in the sample. The calculation algorithm developed includes broad band and continuum background correction, linearization of function absorbance vs. concentration of atomic vapor and integration of thus modified absorbance at the resonance lines of the elements to be determined. Practical application shows that the method can be employed for the direct simultaneous determination of about 20 elements above microgram per liter level within 3-5 orders of the magnitude concentration range. The investigated sources of measurement errors are mainly associated with the atomization and vapor transportation problems, which are aggravated for the simultaneous release of major and minor sample constituents. Respective corrections concerning the selection of analytical lines, optimal sampling volume, matrix modification and cleaning of the atomizer have been introduced in the SMET AAS analytical technology. Under the optimized experimental conditions the calibration curves in Log-Log coordinates for all the investigated analytes in the single or multi-element reference solutions are approximated by the first order equations. The use of these equations as permanent characteristics of the setup enables instant quantification of Al, Ca, Co, Cr, Cu, Fe, Mg, Mn and Ni in the underground water

  2. Pointing errors in solar absorption spectrometry - correction scheme and its validation

    Science.gov (United States)

    Reichert, A.; Hausmann, P.; Sussmann, R.

    2015-09-01

    A method for quantification of sun-pointing inaccuracies in solar absorption spectrometry is presented along with a correction scheme for the resulting errors in trace gas vertical column or profile retrievals. A posteriori correction of pointing errors requires knowledge of both coordinates of the mispointing vector on the solar disk. In principle, quantitative information on the mispointing can be retrieved from Doppler shifts of solar lines derived from measured spectra. However, this yields only one component of the mispointing vector, namely the one which is perpendicular to the solar rotation axis. Missing information on the second vector component has hindered a posteriori correction of mispointing errors so far. Our idea of how to overcome this problem is to obtain estimates of both coordinates of the mispointing by combining subsequent measurements with differing orientations of the solar rotation axis relative to the zenith direction. The proposed concept is suitable in the case of systematic mispointing, i.e., if the mispointing is approximately constant within a given set of measurements. An implementation of this original concept is demonstrated using measurements from the solar absorption Fourier transform infrared (FTIR) spectrometer at the Zugspitze (47.42° N, 10.98° E, 2964 m a.s.l.). Soundings in the September 2012-September 2014 time interval were impacted by mispointing problems due to a non-optimum solar tracking optics configuration. They show a mean mispointing in the zenith direction of -0.063°. This causes biases in vertical soundings of trace gases, e.g., -2.82 ppb in monthly means of dry-air column-averaged mole fractions of methane (XCH4). Measurements made with the more stable pre-September 2012 and post-September 2014 optics configurations show considerably smaller mispointing effects. Applying the mispointing correction, the April 2006-March 2014 XCH4 trend determined from Zugspitze measurements is reduced from 6.45 [5.84, 7.04] to

  3. Arsenic speciation in natural water samples by coprecipitation-hydride generation atomic absorption spectrometry combination.

    Science.gov (United States)

    Tuzen, Mustafa; Citak, Demirhan; Mendil, Durali; Soylak, Mustafa

    2009-04-15

    A speciation procedure for As(III) and As(V) ions in environmental samples has been presented. As(V) was quantitatively recovered on aluminum hydroxide precipitate. After oxidation of As(III) by using dilute KMnO(4), the developed coprecipitation was applied to determination of total arsenic. Arsenic(III) was calculated as the difference between the total arsenic content and As(V) content. The determination of arsenic levels was performed by hydride generation atomic absorption spectrometry (HG-AAS). The analytical conditions for the quantitative recoveries of As(V) including pH, amount of aluminum as carrier element and sample volume, etc. on the presented coprecipitation system were investigated. The effects of some alkaline, earth alkaline, metal ions and also some anions were also examined. Preconcentration factor was calculated as 25. The detection limits (LOD) based on three times sigma of the blank (N: 21) for As(V) was 0.012 microg L(-1). The satisfactory results for the analysis of arsenic in NIST SRM 2711 Montana soil and LGC 6010 Hard drinking water certified reference materials for the validation of the method was obtained. The presented procedure was successfully applied to real samples including natural waters for arsenic speciation.

  4. Determination of mercury distribution inside spent compact fluorescent lamps by atomic absorption spectrometry.

    Science.gov (United States)

    Rey-Raap, Natalia; Gallardo, Antonio

    2012-05-01

    In this study, spent compact fluorescent lamps were characterized to determine the distribution of mercury. The procedure used in this research allowed mercury to be extracted in the vapor phase, from the phosphor powder, and the glass matrix. Mercury concentration in the three phases was determined by the method known as cold vapor atomic absorption spectrometry. Median values obtained in the study showed that a compact fluorescent lamp contained 24.52±0.4ppb of mercury in the vapor phase, 204.16±8.9ppb of mercury in the phosphor powder, and 18.74±0.5ppb of mercury in the glass matrix. There are differences in mercury concentration between the lamps since the year of manufacture or the hours of operation affect both mercury content and its distribution. The 85.76% of the mercury introduced into a compact fluorescent lamp becomes a component of the phosphor powder, while more than 13.66% is diffused through the glass matrix. By washing and eliminating all phosphor powder attached to the glass surface it is possible to classified the glass as a non-hazardous waste. Copyright © 2011 Elsevier Ltd. All rights reserved.

  5. Determination of mercury by multisyringe flow injection system with cold-vapor atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Leal, L.O. [Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa km.7.5, E-07122 Palma de Mallorca (Spain); Elsholz, O. [Hamburg University of Applied Sciences, Lohbruegger Kirchstrasse 65, 21033 Hamburg (Germany); Forteza, R. [Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa km.7.5, E-07122 Palma de Mallorca (Spain); Cerda, V. [Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa km.7.5, E-07122 Palma de Mallorca (Spain)]. E-mail: victor.cerda@uib.es

    2006-07-28

    A new software-controlled time-based multisyringe flow injection system for mercury determination by cold-vapor atomic absorption spectrometry is proposed. Precise known volumes of sample, reducing agent (1.1% SnCl{sub 2} in 3% HCl) and carrier (3% HCl) are dispensed into a gas-liquid separation cell with a multisyringe burette coupled with one three-way solenoid valve. An argon flow delivers the reduced mercury to the spectrometer. The optimization of the system was carried out testing reaction coils and gas-liquid separators of different design as well as changing parameters, such as sample and reagents volumes, reagent concentrations and carrier gas flow rate, among others. The analytical curves were obtained within the range 50-5000 ng L{sup -1}. The detection limit (3{sigma} {sub b}/S) achieved is 5 ng L{sup -1}. The relative standard deviation (R.S.D.) was 1.4%, evaluated from 16 successive injections of 250 ng L{sup -1} Hg standard solution. The injection and sample throughput per hour were 44 and 11, respectively. This technique was validated by means of solid and water reference materials with good agreement with the certified values and was successfully applied to fish samples.

  6. Use of atomic absorption spectrometry in assessment of biomonitor plants for lead, cadmium and copper pollution.

    Science.gov (United States)

    Gokce, Kaya; Mehmet, Yaman

    2012-01-01

    Eleven plant species were collected from the vicinity of lead-battery plant in the city of Gaziantep, Turkey. Lead, cadmium and copper concentrations in the soil and leaves of plants were determined by atomic absorption spectrometry. Lead, Cd and Cu concentrations in the soil samples taken from battery area were found to be in the ranges of 304-602, 0.4-0.44 and 31-37 mg x kg(-1), respectively. Significantly increased lead concentration up to 2 750 mg x kg(-1) was found in the leaves of Eleagnus angustifolia L. plant. The lead concentrations in the other plant leaves taken from 50 m around battery factory followed the order Ailanthus altissima > Morus sp. > Juglans regia L. > Ficus carica L. > Cydonia oblonga Miller > Prunus x domestica L. The plants, Populus nigra L. , Eleagnus angustifolia L. and Salix sp. were found useful for Cd, and the plant, Eleagnus angusti folia L. for Pb, to be considered as potential biomonitor. Especially, leaves of trees and plants taken from the distance of 50 m from battery plant have relatively higher Pb concentrations. Therefore, people who and animals which live in this area and benefit from these soil and plants have vital risks.

  7. Bismuth determination in environmental samples by hydride generation-electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Moscoso-Perez, Carmen; Moreda-Pineiro, Jorge; Lopez-Mahia, Purificacion; Muniategui-Lorenzo, Soledad; Fernandez-Fernandez, Esther; Prada-Rodriguez, Dario [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071, A Coruna (Spain)

    2003-12-04

    A hydride generation procedure, via flow injection, coupled to electrothermal atomic absorption spectrometry was optimised for Bi determination in sea water and hot-spring water and acid extracts from coal, coal fly ash and slag samples. The effects of several variables such as hydrochloric acid and sodium tetrahydroborate concentrations, hydrochloric acid and sodium tetrahydroborate flow rates, reaction coil length, trapping and atomisation temperatures, trapping time and the Ar flow rate have been investigated by using a 2{sup 9}*3/128 Plackett-Burman design. From these studies, certain variables (sodium tetrahydroborate concentration and trapping time) showed up as significant, and they were optimised by a 2{sup 2}+star central composite design. In addition, a study of the bismuthine trapping and atomisation efficiency from graphite tubes (GTs) permanently treated with uranium, tantalum, lanthanum oxide, niobium, beryllium oxide, chromium oxide and tantalum carbide were investigated. The results obtained were compared with those achieved by iridium and zirconium-treated GTs. The best analytical performances, with characteristic mass of 35 pg and detection limit of 70 ng l{sup -1}, were achieved by using U-treated GTs. Accuracy were checked using several reference materials: 1643d (Trace Elements in Water), TM-24 (Reference Water), GBW-07401 (Soil) and 1632c (Trace Elements in Coal)

  8. EVALUATION OF HEAVY METALS CONTENT IN EDIBLE MUSHROOMS BY MICROWAVE DIGESTION AND FLAME ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Cristiana Radulescu

    2011-05-01

    Full Text Available The aim of this work was to determine the heavy metal (Cd, Cr, Ni, Pb, Mn, Zn, Fe and Cu content of the fruiting bodies (cap and stipe of four species (Amanita caesarea, Pleurotus ostreatus, Fistulina hepatica and Armillariella mellea and their substrate, collected from forest sites in Dâmboviţa County, Romania. The elements were determined by Flame Atomic Absorption Spectrometry (FAAS after microwave assisted digestion. From the same collecting point were taken n = 5 samples of young and mature fruiting bodies of mushrooms and their substrate. The high concentrations of lead, chrome and cadmium (Pb: 0.25 – 1.89 mg.kg-1, Cr: 0.36 – 1.94 mg.kg-1, Cd: 0.23 – 1.13 mg.kg-1 for all collected wild edible mushrooms, were determined. These data were compared with maximum level for certain contaminants in foodstuffs established by the commission of the European Committees (EC No 466/2001. A quantitative evaluation of the relationship of element uptake by mushrooms from substrate was made by calculating the accumulation coefficient (Ka. The moderately acid pH value of soil influenced the accumulation of Zn and Cd inside of the studied species. The variation of heavy metals content between edible mushrooms species is dependent upon the ability of the species to extract elements from the substrate and on the selective uptake and deposition of metals in tissue.

  9. Determination of iron in natural and mineral waters by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    ROLANDAS KAZLAUSKAS

    2004-05-01

    Full Text Available Simple methods for the determination of Fe in natural and mineral waters by flame atomic absorption spectrometry (AAS are suggested. The results of the investigation of selectivity of the proposed AAS method proved that this procedure is not affected by high concentrations of other metals. The calibration graph for iron was linear at levels near the detection limit up to at least 0.10 mg ml-1. For the determination of microamounts of iron in mineral waters, an extraction AAS technique was developed. Iron was retained as Fe-8-oxyquinoline complex and extracted into chloroform. The optimal conditions for the extraction of the iron complex were determined. The AAS method was applied to the determination of Fe in mineral waters and natural waters from different areas of Lithuania. The accuracy of the developed method was sufficient and evaluated in comparison with a photometric method. The obtained results demonstrated that the procedure could be successfully applied for the analysis of water samples with satisfactory accuracy.

  10. Stabilizing Agents for Calibration in the Determination of Mercury Using Solid Sampling Electrothermal Atomic Absorption Spectrometry

    Science.gov (United States)

    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef

    2012-01-01

    Tetramethylene dithiocarbamate (TMDTC), diethyldithiocarbamate (DEDTC), and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS). These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK) extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L−1 TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants. PMID:22654606

  11. [Determination of trace gallium by graphite furnace atomic absorption spectrometry in urine].

    Science.gov (United States)

    Zhou, L Z; Fu, S; Gao, S Q; He, G W

    2016-06-20

    To establish a method for determination trace gallium in urine by graphite furnace atomic absorption spectrometry (GFAAS). The ammonium dihydrogen phosphate was matrix modifier. The temperature effect about pyrolysis (Tpyr) and atomization temperature were optimized for determination of trace gallium. The method of technical standard about within-run, between-run and recoveries of standard were optimized. The method showed a linear relationship within the range of 0.20~80.00 μg/L (r=0.998). The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 5.0, 10.0, 20.0 μg/L concentration levels were 2.1%~5.5% and 2.3%~3.0%. The detection limit was 0.06 μg/L. The recoveries of gallium were 98.2%~101.1%. This method is simple, low detection limit, accurate, reliable and reproducible. It has been applied for determination of trace gallium in urine samples those who need occupation health examination or poisoning diagnosis.

  12. Optimization of electrothermal atomization parameters for simultaneous multielement atomic absorption spectrometry

    Science.gov (United States)

    Harnly, J.M.; Kane, J.S.

    1984-01-01

    The effect of the acid matrix, the measurement mode (height or area), the atomizer surface (unpyrolyzed and pyrolyzed graphite), the atomization mode (from the wall or from a platform), and the atomization temperature on the simultaneous electrothermal atomization of Co, Cr, Cu, Fe, Mn, Mo, Ni, V, and Zn was examined. The 5% HNO3 matrix gave rise to severe irreproducibility using a pyrolyzed tube unless the tube was properly "prepared". The 5% HCl matrix did not exhibit this problem, and no problems were observed with either matrix using an unpyrolized tube or a pyrolyzed platform. The 5% HCl matrix gave better sensitivities with a pyrolyzed tube but the two matrices were comparable for atomization from a platform. If Mo and V are to be analyzed with the other seven elements, a high atomization temperature (2700??C or greater) is necessary regardless of the matrix, the measurement mode, the atomization mode, or the atomizer surface. Simultaneous detection limits (peak height with pyrolyzed tube atomization) were comparable to those of conventional atomic absorption spectrometry using electrothermal atomization above 280 nm. Accuracies and precisions of ??10-15% were found in the 10 to 120 ng mL-1 range for the analysis of NBS acidified water standards.

  13. Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, H.; Krawczyk, M. [Politechn Poznanska, Poznan (Poland)

    2007-03-15

    The analytical performance of coupled hydride generation - integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H{sub 2}Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangernents (a water-cooled single silica tube, double-slotted quartz tube or an 'integrated trap') was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3{sigma}), was 0.9 ng mL{sup -1} for Te. For a 2 min in situ preconcentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% (n = 6) for Te. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

  14. Determination of silicon in serum and urine by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Huang, Zhuo-er

    1995-09-01

    A sensitive, simple and accurate method for the routine determination of trace silicon in serum and urine by Zeeman electrothermal atomic absorption spectrometry is described. The samples are directly determined after 20-fold dilution of serum and 100-fold dilution of urine. No L'vov platform is used. The signal enhancement of silicon atomization in pyrolytic graphite coated graphite tubes is achieved by using a mixture of calcium chloride and lanthanum nitrate as chemical modifier. The interferences arising from the biological matrices have been eliminated by the addition of ammonium dihydrogenphosphate in the sample solutions. The aqueous calibration curve is linear to at least 300 μg l -1, the characteristic mass is 37 pg (integrated absorbance signal), whereas the detection limit (3SD) is 1.5 μg l -1 for silicon in both diluted serum and urine samples. The recoveries of silicon added to the diluted samples are 101 ± 1.8% for sera and 98.2 ± 3.5% for the urine specimens, independent of the dilution ratio. The silicon measurement results for the serum and urine from healthy adults and for the serum from the patients with chronic renal failure on hemodialysis are presented.

  15. Ultraviolet differential optical absorption spectrometry: quantitative analysis of the CS2 produced by SF6 decomposition

    Science.gov (United States)

    Zhang, Xiaoxing; Zhou, Hong; Chen, Chuan; Li, Xin; Cui, Zhaolun; Xiao, Song; Tang, Ju

    2017-11-01

    The occurrence of partial discharge or partial overthermal fault in sulfur hexafluoride (SF6)-insulated electrical equipment frequently causes SF6 and solid insulation materials to decompose into various products. One of the most characteristic products of this process is carbon disulfide (CS2). The internal fault type and severity of the fault in the insulation equipment can be detected through the accurate quantitative detection of CS2. A device for simultaneously determining and quantifying gaseous CS2 via ultraviolet differential optical absorption spectrometry is developed in this study. A Sym14 wavelet transform and fast Fourier transform (FFT) are applied to process the spectral data of the feature regions, namely 190 nm to 210 nm. The concentration of CS2 is determined, and the detection limit of the developed device is identified. A good linear relationship is observed between the characteristic peaks of FFT and the concentration of CS2 after the operational parameters are optimized. Along the light path at 600 mm, the average detection limit for CS2 is 8.65 ppb based on three times the standard deviation of the system noises. The proposed device, which exhibits high sensitivity and effective cost, addresses the urgent demand for the monitoring and diagnosis of SF6-insulated electrical equipment via online detection of trace CS2.

  16. Separation and preconcentration of trace amounts of gold from water samples prior to determination by flame atomic absorption spectrometry

    OpenAIRE

    Sabermahani,Fatemeh; Taher,Mohammad Ali; Bahrami, Habibe

    2016-01-01

    A preconcentration/separation procedure is presented for the solid phase extraction of trace gold(III) as its rubeanic acid (dithiooxamide) chelate on silica gel, prior to determination by flame atomic absorption spectrometry. The influences of analytical parameters including pH of the aqueous solution, the amount of the sorbent, time of the complex formation, ligand amount, flow rates of sample and elution solutions and the type, concentration and volume of elution solution on the quantitati...

  17. Determination of Mercury in Mainstream Cigarette Smoke by Conventional and Amalgamation Cold Vapor Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    McDaniel RL

    2014-12-01

    Full Text Available A method for differentiation of gas- and particulate-phase mercury in mainstream cigarette smoke was developed using electrostatic precipitation (EP as the trap for the particulate phase and impingers containing acidic potassium permanganate solution as the trap for the gas-phase portion. The mercury collected from the gas phase was analyzed by conventional cold vapor atomic absorption spectrometry (CVAAS and the particulate phase was analyzed by gold amalgamation CVAAS. Cigarettes were smoked under two smoking regimes, FTC (35-mL puff volume, 2 s puff duration and one puff every 60 s and an alternative (45-mL puff volume, 2 s puff duration, one puff every 30 s and 50% of any ventilation holes blocked currently recommended by the Massachusetts Department of Health. For the 1R4F reference cigarette smoked under the FTC smoking regime, the mercury found in the particulate phase was less than 0.2 ng/cig, compared with 4.9 ng/cig in the gas phase. By changing smoking parameters, the mercury concentration in mainstream smoke was found to change proportional to the delivery of cigarette smoke condensate (CSC for the same type of cigarette. However, the mercury level for different types of cigarettes smoked under the same smoking parameters had no linear relationship with CSC delivery. Spiked recovery was 98% AA± 8% for gas-phase mercury and 97% AA± 2% for the particulate phase. These results indicate that the analytical method developed is suitable for the determination of mercury in mainstream smoke. For routine analytical work in a smoking laboratory, only the gas phase needs to be analyzed for determination of mercury in mainstream smoke because the amount of mercury in the particulate phase is negligible.

  18. Exploiting flow injection and sequential injection for trace metal determinations in conjunction with detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Despite their excellent analytical chemical capacities, Electrothermal Atomic Absorption Spectrometry (ETAAS) and Inductively Coupled Plasma Mass Spectrometry (ICPMS), nevertheless, often require suitable pretreatment of the sample material in order to obtain the necessary sensitivity...... and selectivity. Either in order to separate/preconcentrate the analyte material, or because of the presence of potentially interfering matrix constituents. Such pretreatments are advantageously performed in flow injection (FI) or sequential injection (SI) manifolds, where all appropriate unit operations can......, such as liquid-liquid extraction, (co)precipitation with collection in knotted reactors, adsorption, hydride generation, or the use of ion-exchange columns. Apart from hydride generation, where the analyte is converted into a gaseous species, the common denominator for these approaches is that the analyte...

  19. Cadmium, copper, lead, and zinc determination in precipitation: A comparison of inductively coupled plasma atomic emission spectrometry and graphite furnace atomization atomic absorption spectrometry

    Science.gov (United States)

    Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

    1987-01-01

    Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

  20. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sardans, Jordi, E-mail: j.sardans@creaf.uab.ca [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain); Montes, Fernando [Departamento de Ciencias Analiticas, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia (UNED), C/ Senda del Rey 9. 28040 Madrid (Spain); Penuelas, Josep [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain)

    2010-02-15

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at mug L{sup -1} levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages

  1. A Sensitive Method for Cadmium Determination Using an On-line Polyurethane Foam Preconcentration System and Thermospray Flame Furnace Atomic Absorption Spectrometry

    National Research Council Canada - National Science Library

    TARLEY, César Ricardo Teixeira; ARRUDA, Marco Aurélio Zezzi

    2004-01-01

    A new sensitive and low cost method for cadmium determination at µg l-1 levels that combines an on-line preconcentration system with the thermospray flame furnace atomic absorption spectrometry technique (TS-FF-AAS...

  2. Speciation analysis of arsenic in biological matrices by automated hydride generation-cryotrapping-atomic absorption spectrometry with multiple microflame quartz tube atomizer (multiatomizer).

    Science.gov (United States)

    This paper describes an automated system for the oxidation state specific speciation of inorganic and methylated arsenicals by selective hydride generation - cryotrapping- gas chromatography - atomic absorption spectrometry with the multiatomizer. The corresponding arsines are ge...

  3. Mercury in Environmental and Biological Samples Using Online Combustion with Sequential Atomic Absorption and Fluorescence Measurements: A Direct Comparison of Two Fundamental Techniques in Spectrometry

    Science.gov (United States)

    Cizdziel, James V.

    2011-01-01

    In this laboratory experiment, students quantitatively determine the concentration of an element (mercury) in an environmental or biological sample while comparing and contrasting the fundamental techniques of atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). A mercury analyzer based on sample combustion,…

  4. Determination of Sodium, Potassium, Magnesium, and Calcium Minerals Level in Fresh and Boiled Broccoli and Cauliflower by Atomic Absorption Spectrometry

    Science.gov (United States)

    Nerdy

    2018-01-01

    Vegetables from the cabbage family vegetables consumed by many people, which is known healthful, by eaten raw, boiled, or cooked (stir fry or soup). Vegetables like broccoli and cauliflower contain vitamins, minerals, and fiber. This study aims to determine the decrease percentage of sodium, potassium, magnesium, and calcium minerals level caused by boiled broccoli and cauliflower by atomic absorption spectrometry. Boiled broccoli and cauliflower prepared by given boiled treatment in boiling water for 3 minutes. Fresh and boiled broccoli and cauliflower carried out dry destruction, followed by quantitative analysis of sodium, potassium, magnesium, and calcium minerals respectively at a wavelength of 589.0 nm; 766.5 nm; 285.2 nm; and 422.7 nm, using atomic absorption spectrometry methods. After the determination of the sodium, potassium, magnesium, and calcium minerals level followed by validation of analytical methods with accuracy, precision, linearity, range, limit of detection (LOD), and limit of quantitation (LOQ) parameters. Research results show a decrease in the sodium, potassium, magnesium, and calcium minerals level in boiled broccoli and cauliflower compared with fresh broccoli and cauliflower. Validation of analytical methods gives results that spectrometry methods used for determining sodium, potassium, magnesium, and calcium minerals level are valid. It concluded that the boiled gives the effect of decreasing the minerals level significantly in broccoli and cauliflower.

  5. [Evaluation of uncertainty for determination of tin and its compounds in air of workplace by flame atomic absorption spectrometry].

    Science.gov (United States)

    Wei, Qiuning; Wei, Yuan; Liu, Fangfang; Ding, Yalei

    2015-10-01

    To investigate the method for uncertainty evaluation of determination of tin and its compounds in the air of workplace by flame atomic absorption spectrometry. The national occupational health standards, GBZ/T160.28-2004 and JJF1059-1999, were used to build a mathematical model of determination of tin and its compounds in the air of workplace and to calculate the components of uncertainty. In determination of tin and its compounds in the air of workplace using flame atomic absorption spectrometry, the uncertainty for the concentration of the standard solution, atomic absorption spectrophotometer, sample digestion, parallel determination, least square fitting of the calibration curve, and sample collection was 0.436%, 0.13%, 1.07%, 1.65%, 3.05%, and 2.89%, respectively. The combined uncertainty was 9.3%.The concentration of tin in the test sample was 0.132 mg/m³, and the expanded uncertainty for the measurement was 0.012 mg/m³ (K=2). The dominant uncertainty for determination of tin and its compounds in the air of workplace comes from least squares fitting of the calibration curve and sample collection. Quality control should be improved in the process of calibration curve fitting and sample collection.

  6. Determination of lithium isotopes at natural abundance levels by atomic absorption spectrometry

    Science.gov (United States)

    Meier, A.L.

    1982-01-01

    The relationships of the absorption of 6Li and 7Li hollow cathode lamp emissions are used to determine lithium isotopic composition in the natural abundance range of geologic materials. Absorption was found to have a nonlinear dependence upon total lithium concentration and isotopic composition. A method using nonlinear equations to describe the relationship of the absorption of 6Li and 7Li lamp radiation is proposed as a means of calculating isotopic composition that is independent of total lithium concentration.

  7. Determination of total selenium in nutritional supplements and selenised yeast by Zeeman-effect graphite furnace atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Ekelund, J.

    1989-01-01

    A method for the determination of total selenium in nutritional supplements and selenised yeast is described. The samples were ashed in nitric acid. Hydrochloric acid was used to prevent precipitation of, in particular, iron salts. After appropriate dilutions, the selenium was determined by Zeeman......-effect background corrected graphite furnace atomic absorption spectrometry. A furnace ashing step at 1100 °C was necessary in order to obtain a total recovery of selenium when present in the organic form. Palladium nitrate-magnesium nitrate was used as a matrix modifier. Independent methods were used to determine...

  8. Arsenic speciation by hydride generation-quartz furnace atomic absorption spectrometry. Optimization of analytical parameters and application to environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Molenat, N.; Astruc, A.; Holeman, M.; Pinel, R. [Laboratoire de Chimie Analytique Bioinorganique et Environnement, Dept. de Chimie, Faculte des Sciences et Techniques, 64 - Pau (France); Maury, G. [Montpellier-2 Univ., 34 (France). Dept. de Chimie Organique Fine

    1999-11-01

    Analytical parameters of hydride generation, trapping, gas chromatography and atomic absorption spectrometry detection in a quartz cell furnace (HG/GC/QFAAS) device have been optimized in order to develop an efficient and sensitive method for arsenic compounds speciation. Good performances were obtained with absolute detection limits in the range of 0.1 - 0.5 ng for arsenite, arsenate, mono-methyl-arsonic acid (MMAA), dimethyl-arsinic acid (DMAA) and trimethyl-arsine oxide (TMAO). A pH selective reduction for inorganic arsenic speciation was successfully reported. Application to the accurate determination of arsenic compounds in different environmental samples was performed. (authors)

  9. Determination of Copper-Based Fungicides by Flame Atomic Absorption Spectrometry Using Digestion Procedure with Sulfuric and Nitric Acid

    Directory of Open Access Journals (Sweden)

    Jelena Milinović

    2007-01-01

    Full Text Available Copper-based fungicides can be effectively digested by treatment with a mixture of concentrated sulfuric and nitric acid in exactly 15 minutes for the rapid determination via copper using flame atomic absorption spectrometry (AAS. Under optimum conditions, the results of copper fungicide analysis were consistent to those obtained by the AOAC’s recommended method. Recovery values ranged from 98.63 to 103.40%. Relative standard deviation values are lower than 2%. The proposed digestion procedure applied for determination of copper ranged from 100 to 594 g Cu kg-1 in different commercial fungicideproducts.

  10. Determination of gold in geologic materials by solvent extraction and atomic-absorption spectrometry

    Science.gov (United States)

    Huffman, Claude; Mensik, J.D.; Riley, L.B.

    1967-01-01

    The two methods presented for the determination of traces of gold in geologic materials are the cyanide atomic-absorption method and the fire-assay atomic-absorption method. In the cyanide method gold is leached with a sodium-cyanide solution. The monovalent gold is then oxidized to the trivalent state and concentrated by extracting into methyl isobutyl ketone prior to estimation by atomic absorption. In the fire-assay atomic-absorption method, the gold-silver bead obtained from fire assay is dissolved in nitric and hydrochloric acids. Gold is then concentrated by extracting into methyl isobutyl ketone prior to determination by atomic absorption. By either method concentrations as low as 50 parts per billion of gold can be determined in a 15-gram sample.

  11. Arsenic in marine tissues — The challenging problems to electrothermal and hydride generation atomic absorption spectrometry

    Science.gov (United States)

    Karadjova, Irina B.; Petrov, Panayot K.; Serafimovski, Ivan; Stafilov, Trajče; Tsalev, Dimiter L.

    2007-03-01

    Analytical problems in determination of arsenic in marine tissues are addressed. Procedures for the determination of total As in solubilized or extracted tissues with tetramethylammonium hydroxide and methanol have been elaborated. Several typical lyophilized tissues were used: NIST SRM 1566a 'Oyster Tissue', BCR-60 CRM 'Trace Elements in an Aquatic Plant ( Lagarosiphon major)', BCR-627 'Forms of As in Tuna Fish Tissue', IAEA-140/TM 'Sea Plant Homogenate', NRCC DOLT-1 'Dogfish Liver' and two representatives of the Black Sea biota, Mediterranean mussel ( Mytilus galloprovincialis) and Brown algae ( Cystoseira barbata). Tissues (nominal 0.3 g) were extracted in tetramethylammonium hydroxide (TMAH) 1 ml of 25% m/v TMAH and 2 ml of water) or 5 ml of aqueous 80% v/v methanol (MeOH) in closed vessels in a microwave oven at 50 °C for 30 min. Arsenic in solubilized or extracted tissues was determined by electrothermal atomic absorption spectrometry (ETAAS) after appropriate dilution (nominally to 25 ml, with further dilution as required) under optimal instrumental parameters (pyrolysis temperature 900 °C and atomization temperature 2100 °C) with 1.5 μg Pd as modifier on Zr-Ir treated platform. Platforms have been pre-treated with 2.7 μmol of zirconium and then with 0.10 μmol of iridium which served as a permanent chemical modifier in direct ETAAS measurements and as an efficient hydride sequestration medium in flow injection hydride generation (FI-HG)-ETAAS. TMAH and methanol extract 96-108% and 51-100% of As from CRMs. Various calibration approaches have been considered and critically evaluated. The effect of species-dependent slope of calibration graph or standard additions plot for total As determination in a sample comprising of several individual As species with different ETAAS behavior has been considered as a kind of 'intrinsic element speciation interference' that cannot be completely overcome by standard additions technique. Calibration by means of CRMs has

  12. Determination of Chlorine in Milk via Molecular Absorption of SrCl Using High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-07-20

    Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1).

  13. Determination of some trace elements in food and soil samples by atomic absorption spectrometry after coprecipitation with holmium hydroxide.

    Science.gov (United States)

    Saracoglu, Sibel; Soylak, Mustafa; Cabuk, Dilek; Topalak, Zeynep; Karagozlu, Yasemin

    2012-01-01

    The determination of trace elements in food and soil samples by atomic absorption spectrometry was investigated. A coprecipitation procedure with holmium hydroxide was used for separation-preconcentration of trace elements. Trace amounts of copper(II), manganese(II), cobalt(II), nickel(ll), chromium(lll), iron(Ill), cadmium(ll), and lead(ll) ions were coprecipitated with holmium hydroxide in 2.0 M NaOH medium. The optimum conditions for the coprecipitation process were investigated for several commonly tested experimental parameters, such as amount of coprecipitant, effect of standing time, centrifugation rate and time, and sample volume. The precision, based on replicate analysis, was lower than 10% for the analytes. In order to verify the accuracy of the method, the certified reference materials BCR 141 R calcareous loam soil and CRM 025-050 soil were analyzed. The procedure was successfully applied for separation and preconcentration of the investigated ions in various food and soil samples. An amount of the solid samples was decomposed with 15 mL concentrated hydrochloric acid-concentrated nitric acid (3 + 1). The preconcentration procedure was then applied to the final solutions. The concentration of trace elements in samples was determined by atomic absorption spectrometry.

  14. Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers

    Science.gov (United States)

    Abad, Carlos; Florek, Stefan; Becker-Ross, Helmut; Huang, Mao-Dong; Heinrich, Hans-Joachim; Recknagel, Sebastian; Vogl, Jochen; Jakubowski, Norbert; Panne, Ulrich

    2017-10-01

    Boron isotope amount ratios n(10B)/n(11B) have been determined by monitoring the absorption spectrum of boron monohydride (BH) in a graphite furnace using high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Bands (0 → 0) and (1 → 1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Clean and free of memory effect molecular spectra of BH were recorded. In order to eliminate the memory effect of boron, a combination of 2% (v/v) hydrogen gas in argon and 1% trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers was used. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, for the evaluated region of 437 nm, an accuracy of 0.15‰ is obtained as the average deviation from the isotope reference materials. Expanded uncertainties with a coverage factor of k = 2 range between 0.15 and 0.44‰. This accuracy and precision are compatible with those obtained by mass spectrometry for boron isotope ratio measurements.

  15. Direct determination of Cd, Cu and Pb in wines and grape juices by thermospray flame furnace atomic absorption spectrometry.

    Science.gov (United States)

    Schiavo, Daniela; Neira, José Y; Nóbrega, Joaquim A

    2008-09-15

    The applicability of thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was evaluated for direct determination of Cu, Cd and Pb in wines and grape juices. The developed procedure does not require preliminary acid digestion of the samples. The optimum conditions for determination of Cu, Cd and Pb in wines were studied and the performance was compared to those typically obtained by flame atomic absorption spectrometry (FAAS). A sample volume of 150 microL was introduced into a heated nickel tube at a flow rate of 0.54 mLmin(-1) and 0.14 molL(-1) HNO(3) was used as sample carrier flowing at 2.5 mLmin(-1) for determining all analytes. The effect of ethanol concentrations on Cu, Cd and Pb absorbance signals were studied. All determinations were carried out by adopting optimized conditions and quantification was based on the standard additions method. Limits of detection (LOD) of 12.9, 1.8 and 5.3 microgL(-1) (n=14) for Cu, Cd and Pb, respectively, were obtained for wine samples (3sigma(blank)/slope, n=14). Relative standard deviations (R.S.D., %) of 2.7, 2.1 and 2.6 for Cu, Cd and Pb, were obtained (n=6) for wine samples. The values determined for grape juice samples were similar to these ones. The analytical throughput was 45 determinations h(-1) and accuracy was checked by addition-recovery experiments.

  16. Contents of cadmium, mercury and lead in fish from the Atlantic sea (Morocco) determined by atomic absorption spectrometry.

    Science.gov (United States)

    Chahid, Adil; Hilali, Mustapha; Benlhachimi, Abdeljalil; Bouzid, Taoufiq

    2014-03-15

    As a part of a specific monitoring program, lead (Pb) cadmium (Cd) and mercury (Hg) concentrations in important species of fish from various fishing ports of the southern Kingdom of Morocco (Sardina pilchardus, Scomber scombrus, Plectorhinchus mediterraneus, Trachurus trachurus, Octopus vulgaris, Boops boops, Sarda sarda, Trisopterus capelanus, and Conger conger) were investigated by the Moroccan Reference Laboratory (NRL) for trace elements in foodstuffs of animal origin. The samples were analysed for lead and cadmium by a graphite furnace atomic absorption spectrometry (GFAAS); and for mercury by cold vapour atomic absorption spectrometry (CVAAS). The results were expressed as μg/g of wet weight (w/w). The levels of Cd, Pb and Hg in muscles of fish were 0.009-0.036, 0.013-0.114 and 0.049-0.194 μg/g, respectively. The present study showed that different metals were present in the sample at different levels but within the maximum residual levels prescribed by the EU for the fish and shellfish from these areas, in general, should cause no health problems for consumers. Copyright © 2013 Elsevier Ltd. All rights reserved.

  17. Determination of total selenium in pharmaceutical and herbal supplements by hydride generation and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Kazi, Tasneem G; Kolachi, Nida F; Afridi, Hassan I; Brahman, Kapil Dev; Shah, Faheem

    2014-01-01

    The total selenium (Se) was determined in herbal and pharmaceutical supplements used for liver diseases. The total Se contents were determined in different pharmaceutical and herbal supplements by hydride generation atomic absorption spectrometry (HGAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after microwave-assisted acid digestion. The accuracy of the techniques was evaluated by using certified reference material and the standard addition method. The recoveries of total Se were 99.4 and 99.0% for HGAAS and GFAAS, respectively. The precision of the techniques expressed as RSD were 2.34 and 4.54% for HGAAS and GFAAS measurements, respectively. The LOD values for HGAAS and GFAAS were 0.025 and 0.052 pglg, respectively. The concentrations of Se in pharmaceutical and herbal supplements were found in the range of 19.2-53.8 and 25.0-42.5 pg/g, respectively, corresponding to 35-76% and 45-76% of the total recommended dose of Se for adults.

  18. Electrothermal atomization atomic absorption spectrometry for the determination of lead in urine: results of an interlaboratory study

    Science.gov (United States)

    Parsons, Patrick J.; Slavin, Walter

    1999-05-01

    Results of an interlaboratory study are reported for the determination of lead in urine. Two levels of a lyophilized material containing biologically-bound lead were prepared using pooled urine obtained from lead-poisoned children undergoing the CaNa 2EDTA mobilization test. The materials were circulated to a group of reference laboratories that participate in the `New York State Proficiency Testing Program for Blood Lead'. Results of the initial round-robin gave all-method consensus target values of 145±22 μg/l (S.D.) for lot 17 and 449±43 μg/l (S.D.) for lot 20. The interlaboratory exercise was repeated some 5 years later and consensus target values were re-calculated using the grand mean (excluding outliers) of results reported by laboratories using electrothermal atomization atomic absorption spectrometry (ETAAS). The re-calculated target values were 139±10 μg/l (S.D.) and 433±12 μg/l (S.D.). The urine reference materials were also analyzed for lead by several laboratories using other instrumental techniques including isotope dilution (ID), inductively coupled plasma (ICP) mass spectrometry (MS), flame atomic absorption with extraction, ICP-atomic emission spectrometry, ID-gas chromatography MS and flow injection-hydride generation AAS, thus providing a rich source of analytical data with which to characterize them. The materials were also used in a long-term validation study of an ETAAS method developed originally for blood lead determinations that has since been used unmodified for the determination of lead in urine also. Recently, urine lead method performance has been tracked in a proficiency testing program specifically for this analysis. In addition, a number of commercial control materials have been analyzed and evaluated.

  19. Absorption coefficient of nearly transparent liquids measured using thermal lens spectrometry

    Directory of Open Access Journals (Sweden)

    H.Cabrera

    2006-01-01

    Full Text Available We use an optimized pump-probe mode-mismatched thermal lens scheme to determine the optical absorption coefficient and thermal diffusivity of ethanol, benzene, acetone, methanol, toluene and chloroform. In this scheme the excitation beam is focused in the presence of a collimated probe beam. The agreement between experimentally obtained results and values reported in the literature is good.

  20. Design and evaluation of a continuous flow, integrated nebulizer-hydride generator for flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Miguel Murillo

    2008-01-01

    Full Text Available An evaluation of the performance of a continuous flow hydride generator-nebulizer for flame atomic absorption spectrometry was carried out. Optimization of nebulizer gas flow rate, sample acid concentration, sample and tetrahydroborate uptake rates and reductant concentration, on the As and Se absorbance signals was carried out. A hydrogen-argon flame was used. An improvement of the analytical sensitivity relative to the conventional bead nebulizer used in flame AA was obtained (2 (As and 4.8 (Se µg L-1. Detection limits (3σb of 1 (As and 1.3 (Se µg L-1 were obtained. Accuracy of the method was checked by analyzing an oyster tissue reference material.

  1. Determination of silver, bismuth, cadmium, copper, lead, and zinc in geologic materials by atomic absorption spectrometry with tricaprylylmethylammonium chloride

    Science.gov (United States)

    Viets, J.G.

    1978-01-01

    Interferences commonly encountered in the determination of silver, bismuth, cadmium, copper, lead, and zinc at crustal abundance levels are effectively eliminated using a rapid, sensitive, organic extraction technique. A potassium chlorate-hydrochloric acid digestion solubilizes the metals not tightly bound in the silicate lattice of rocks, soils, and stream sediments. The six metals are selectively extracted into a 10% Aliquat 336-MIBK organic phase in the presence of ascorbic acid and potassium iodide. Metals in the organic extract are determined by flame atomic absorption spectrometry to the 0.02-ppm level for silver, cadmium, copper, and zinc and to the 0.2-ppm level for bismuth and lead with a maximum relative standard deviation of 18.8% for known reference samples. An additional hydrofluoric acid digestion may be used to determine metals substituted in the silicate lattice.

  2. Determination of arsenic, antimony, bismuth, cadmium, copper, lead, molybdenum, silver and zinc in geological materials by atomic-absorption spectrometry

    Science.gov (United States)

    Viets, J.G.; O'Leary, R. M.; Clark, Robert J.

    1984-01-01

    Arsenic, antimony, bismuth, cadmium, copper, lead, molybdenum, silver and zinc are very useful elements in geochemical exploration. In the proposed method, geological samples are fused with potassium pyrosulphate and the fusate is dissolved in a solution of hydrochloric acid, ascorbic acid and potassium iodide. When this solution is shaken with a 10% V/V Aliquat 336 - isobutyl methyl ketone organic phase, the nine elements of interest are selectively partitioned in the organic phase. All nine elements can then be determined in the organic phase using flame atomic-absorption spectrometry. The method is rapid and allows the determination of Ag and Cd at levels down to 0.1 p.p.m., Cu, Mo, and Zn down to 0.5 p.p.m., Pb, Bi and Sb down to 1 p.p.m. and As down to 5 p.p.m. in geological materials.

  3. A New Cross-Shaped Graphite Furnace with Ballast Body for Reduction of Interferences in Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    A. A. Asweisi

    2010-01-01

    Full Text Available A new crossed graphite furnace for atomic absorption spectrometry (GFAAS was designed and installed in heated graphite atomizer (HGA500 combined with Perkin-Elmer spectrometer (AAS1100. The Tungsten ballast body was inserted inside one part of the crossed furnace in a way perpendicular to light path. The analyzed sample was injected manually on the ballast body inside the cross and pushed into the measuring zone using the original inner and additional purge gas. The sample was adsorbed strongly on the ballast and evaporated and transferred with different rates at different temperatures during the temperature program allowing the separation of analyte and matrix signals. Analysis of middle volatile element such as copper and manganese in standard urine sample (seronorm 2525 showed complete separation of analyte and background signals with good sensitivity and repeatability.

  4. Performance of permanent iridium modifier in the presence of corrosive matrix in graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Piascik, M.; Bulska, E. [Univ. of Warsaw (Poland). Dept. of Chemistry

    2001-12-01

    The influence of up to 16% HNO{sub 3}, 28% HCl, and the mixture of both acids in aqua regia on the analytical performance of electrodeposited modifiers (Ir or Ir+Pd) was evaluated and discussed. Cadmium was used as an example of volatile elements often determined by graphite furnace atomic absorption spectrometry (GF AAS). In the presence of HCl, the maximum pyrolysis temperature that could be applied was found to be 600 C. In the presence of HNO{sub 3} and aqua regia, both modifiers stabilized cadmium up to 800 C. The long-term performance of electrodeposited Ir or Ir+Pd was not influenced by mineral acids; moreover the tube lifetime was significantly prolonged compared with a non-modified tube. (orig.)

  5. Application of radiochemical neutron activation and atomic absorption spectrometry methods for the study of nutrition-pollution interactions in children

    Energy Technology Data Exchange (ETDEWEB)

    Tran Bang Diep [Institute for Nuclear Science and Technique, VAEC, P.O. Box 5T-160, Hanoi (Viet Nam)]. E-mail: tranfbangdiepj@yahoo.com; Tran Dai Nghiep [Institute for Nuclear Science and Technique, VAEC, P.O. Box 5T-160, Hanoi (Viet Nam)]. E-mail: tdnghiep@vaec.gov.vn

    2005-07-01

    The application of radiochemical neutron activation analysis (RNAA) and atomic absorption spectrometry (AAS) is expected to aid in understanding and evaluating the effects of environmental pollution on the nutritional status of children already exposed to marginal malnutrition. Samples of placenta, of low-weight and control newborns groups, were collected for determination of nutritional elements and pollutants. The mean ratios of pollutants and nutrients such as Cd/Zn, Hg/Se and Pb/Ca were evaluated for both groups. All these ratios in the placenta of the low-weight newborns are higher than that of the healthy group. The degree of the nutrient-pollutant interaction is evaluated by quantity R, with mercury considered as the most active pollutant while calcium the most active nutrient among the involved elements in process of the interaction. (author)

  6. Application of a mixed solvent system in the determination of metals in lubricating oils using atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    E.O. Ojeka

    2006-06-01

    Full Text Available Analysis of lubricating oils and their additives for Ni, Zn, Mg and Ca was carried out by the proposed method using benzene-acetic acid/methyl isobutyl ketone (MIBK mixed solvent system. Flame atomic absorption spectrometry using air-acetylene flame was employed with the incorporation of concentrated hydrochloric acid into the solvent mixture. The large dilution of samples employed due to flexible working range of this procedure eliminates the need for matched standard hence the same standards are adequate for all types of lubricating oil samples and additives. No effect on the analysis arising from varying viscosities of the oil samples was observed. Results obtained for a wide range of lubricating oils and automatic transmission fluids revealed good agreement with those obtained by established ASTM chemical procedure.

  7. Application of Plackett-Burman and Doehlert designs for optimization of selenium analysis in plasma with electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    El Ati-Hellal, Myriam; Hellal, Fayçal; Hedhili, Abderrazek

    2014-10-01

    The aim of this study was the optimization of selenium determination in plasma samples with electrothermal atomic absorption spectrometry using experimental design methodology. 11 variables being able to influence selenium analysis in human blood plasma by electrothermal atomic absorption spectrometry (ETAAS) were evaluated with Plackett-Burman experimental design. These factors were selected from sample preparation, furnace program and chemical modification steps. Both absorbance and background signals were chosen as responses in the screening approach. Doehlert design was used for method optimization. Results showed that only ashing temperature has a statistically significant effect on the selected responses. Optimization with Doehlert design allowed the development of a reliable method for selenium analysis with ETAAS. Samples were diluted 1/10 with 0.05% (v/v) TritonX-100+2.5% (v/v) HNO3 solution. Optimized ashing and atomization temperatures for nickel modifier were 1070°C and 2270°C, respectively. A detection limit of 2.1μgL(-1) Se was obtained. Accuracy of the method was checked by the analysis of selenium in Seronorm™ Trace element quality control serum level 1. The developed procedure was applied for the analysis of total selenium in fifteen plasma samples with standard addition method. Concentrations ranged between 24.4 and 64.6μgL(-1), with a mean of 42.6±4.9μgL(-1). The use of experimental designs allowed the development of a cheap and accurate method for selenium analysis in plasma that could be applied routinely in clinical laboratories. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  8. Interference of nitrite and nitrogen dioxide on mercury and selenium determination by chemical vapor generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lopes Nunes, Dayana [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900, Santa Maria, RS (Brazil); Pereira dos Santos, Eliane Pereira [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900, Santa Maria, RS (Brazil); Barin, Juliano Smanioto [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900, Santa Maria, RS (Brazil); Mortari, Sergio Roberto [Curso de Ciencias Farmaceuticas, Centro Universitario Franciscano, UNIFRA, 97010-032, Santa Maria, RS (Brazil); Dressler, Valderi Luiz [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900, Santa Maria, RS (Brazil); Moraes Flores, Erico Marlon de [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900, Santa Maria, RS (Brazil)]. E-mail: flores@quimica.ufsm.br

    2005-06-30

    In this study, a systematic investigation was performed concerning the interference of nitrogen oxides on the determination of selenium and mercury by hydride generation atomic absorption spectrometry (HG AAS) and cold vapor atomic absorption spectrometry (CV AAS). The effect of nitrate, nitrite and NO{sub 2} dissolved in the condensed phase was evaluated. No effect of NO{sub 3} {sup -} on Se and Hg determination was observed up to 100 mg of sodium nitrate added to the reaction vessel. The Se signal was reduced by about 80% upon the addition of 6.8 mg NO{sub 2} {sup -}. For Hg, no interference of nitrite was observed up to 20 mg of NO{sub 2} {sup -}. A complete suppression of the Se signal was observed when gaseous NO{sub 2} was introduced into analytical solutions. For Hg, a signal decrease between 8 and 13% occurred. For Se, bubbling argon or heating the solution was not able to recover the original absorbance values, whereas Hg signals were recovered with these procedures. When gaseous NO{sub 2} was passed directly into the atomizer, Se signals decreased similarly to when NO{sub 2} was bubbled in analytical solutions. The addition of urea, hydroxylamine hydrochloride and sulfamic acid (SA) was investigated to reduce the NO{sub 2} effect in sample digests containing residual NO{sub 2}, but only SA was effective in reducing the interference. Based on the results, it is possible to propose the use of SA to prevent interferences in Se and Hg determinations by HG AAS and CV AAS, respectively.

  9. [Determination of lead in water samples by graphite furnace atomic absorption spectrometry after cloud point extraction with dithizone].

    Science.gov (United States)

    Xiao, Shan-Mei; Chen, Jian-Rong; Shen, Yu-Qin

    2006-05-01

    Cloud point extraction was used for the preconcentration of lead after the formation of a complex with dithizone in the presence of surfactant Triton X-114, and then the lead was determined by graphite furnace atomic absorption spectrometry. The conditions affecting the separation and detection process were optimized. Separation of the two phases was accomplished by centrifugation for 15 min at 4 000 rpm. Upon cooling in an ice-bath, the surfactant-rich phase became viscous. The aqueous phase could then be separated by inverting the tubes. Later, a solution of methanol containing 0.1 mol x L(-1) of HNO3 was added to the surfactant-rich phase up to 0.5 mL. The samples were determined by graphite furnace atomic absorption spectrometry with NH4H2PO4 and Mg(NO3)2 as a chemical modifier. At pH 8.0, the preconcentration of only 10 mL sample in the presence of 0.05% Triton X-114 and 20 micromol x L(-1) dithizone permitted the detection of 0.089 microg x L(-1) lead. The enhancement factors were 19.1 times for lead. The calibration graph using the preconcentration system for lead was linear with a correlation coefficient of 0.998 from levels near the detection limits up to at least 30 microg x L(-1). The regression equation was A = 0.026 1c (microg x L(-1)) + 0.010 6. The proposed method has been applied to the determination of lead in water samples.

  10. Fast sequential determination of antimony and lead in pewter alloys using high-resolution continuum source flame atomic absorption spectrometry.

    Science.gov (United States)

    Dessuy, Morgana B; de Jesus, Robson M; Brandao, Geovani C; Ferreira, Sergio L C; Vale, Maria Goreti R; Welz, Bernhard

    2013-01-01

    A simple method has been developed to determine antimony and lead in pewter alloy cups produced in Brazil, using fast sequential determination by high-resolution continuum source flame atomic absorption spectrometry. The samples were dissolved in HCl and H(2)O(2), employing a cold finger system in order to avoid analyte losses. The main resonance line of lead at 217.001 nm and a secondary line of antimony at 212.739 nm were used. The limits of detection for lead and antimony were 0.02 and 5.7 mg L(-1), respectively. The trueness of the method was established by recovery tests and comparing the results obtained by the proposed method with those obtained by inductively coupled plasma optical emission spectrometry. The results were compared using a student's t-test and there was no significant difference at a 95% confidence interval. With the developed methods, it was possible to determine accurately antimony and lead in pewter samples. The lead concentration found in the analysed samples was around 1 mg g(-1), which means that they are not lead free; however, the content was below the maximum allowed level of 5 mg g(-1). The antimony content, which was found to be between 40 and 46 mg g(-1), is actually of greater concern, as antimony is known to be potentially toxic already at very low concentrations, although there is no legislation yet for this element.

  11. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Citak, Demirhan [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Ferreira, Hadla S.; Korn, Maria G.A. [Universidade Federal da Bahia, Instituto de Quimica, 40170-290 Salvador (Brazil); Bezerra, Marcos A. [Universidade Estadual do Sudoeste da Bahia, 45200-190 Jequie (Brazil)

    2009-03-15

    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L{sup -1} nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 {mu}g L{sup -1}, respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 {mu}g L{sup -1}. The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

  12. High-resolution continuum source electrothermal atomic absorption spectrometry - An analytical and diagnostic tool for trace analysis

    Energy Technology Data Exchange (ETDEWEB)

    Welz, Bernhard [Instituto de Quimica, Departamento de Quimica Analitica, Universidade Federal da Bahia, Campus Universitario de Ondina, 40170-290 Salvador - BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis - SC (Brazil)], E-mail: w.bernardo@terra.com.br; Borges, Daniel L.G.; Lepri, Fabio G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis - SC (Brazil); Vale, Maria Goreti R. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre - RS (Brazil); Heitmann, Uwe [ISAS - Institute for Analytical Sciences, Department of Interface Spectroscopy, Albert-Einstein-Str. 9, 12489 Berlin (Germany)

    2007-09-15

    The literature about applications of high-resolution continuum source atomic absorption spectrometry (HR-CS AAS) with electrothermal atomization is reviewed. The historic development of HR-CS AAS is briefly summarized and the main advantages of this technique, mainly the 'visibility' of the spectral environment around the analytical line at high resolution and the unequaled simultaneous background correction are discussed. Simultaneous multielement CS AAS has been realized only in a very limited number of cases. The direct analysis of solid samples appears to have gained a lot from the special features of HR-CS AAS, and the examples from the literature suggest that calibration can be carried out against aqueous standards. Low-temperature losses of nickel and vanadyl porphyrins could be detected and avoided in the analysis of crude oil due to the superior background correction system. The visibility of the spectral environment around the analytical line revealed that the absorbance signal measured for phosphorus at the 213.6 nm non-resonance line without a modifier is mostly due to the PO molecule, and not to atomic phosphorus. The future possibility to apply high-resolution continuum source molecular absorption for the determination of non-metals is discussed.

  13. Nonchromatographic speciation of selenium in edible oils using dispersive liquid-liquid microextraction and electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    López-García, Ignacio; Vicente-Martínez, Yesica; Hernández-Córdoba, Manuel

    2013-10-02

    A methodology for the nonchromatographic separation of the main selenium species present in edible oils is presented. Dispersive liquid-liquid microextraction is used to extract inorganic selenium (iSe), seleno-L-cystine (SeCys₂), seleno-L-methionine (SeMet), and selenocystamine (SeCM) into a slightly acidic aqueous medium. The selenium total (tSe) content is measured in the extracts by electrothermal atomic absorption spectrometry. By repeating the microextraction stage using an ionic liquid instead of water, the sum of SeCys₂, SeMet, and SeCM is obtained and iSe is calculated by difference. The detection limit is 0.03 ng of Se per gram of oil. The fractionation of the edible oils by solid phase extraction followed by dispersive liquid-liquid extraction and atomic absorption measurement also permits speciation of iSe to be carried out. Data for tSe and iSe levels of 15 samples of different origin are given.

  14. Surfactant/oil/water system for the determination of selenium in eggs by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ieggli, C.V.S. [Departamento de Quimica, Avenida Roraima, 1000, Universidade Federal de Santa Maria, CEP 97110-970, Santa Maria, RS (Brazil); Bohrer, D. [Departamento de Quimica, Avenida Roraima, 1000, Universidade Federal de Santa Maria, CEP 97110-970, Santa Maria, RS (Brazil)], E-mail: ndenise@quimica.ufsm.br; Noremberg, S.; Nascimento, P.C. do; Carvalho, L.M. de [Departamento de Quimica, Avenida Roraima, 1000, Universidade Federal de Santa Maria, CEP 97110-970, Santa Maria, RS (Brazil); Vieira, S.L.; Reis, R.N. [Faculdade de Agronomia, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 7712, CEP 90540-000, Porto Alegre (Brazil)

    2009-06-15

    An oil-in-water formulation has been optimized to determine trace levels of selenium in whole hen eggs by graphite furnace atomic absorption spectrometry. This method is simpler and requires fewer reagents when compared with other sample pre-treatment procedures. Graphite furnace atomic absorption spectrometric (GF AAS) measurement was carried out using standard addition calibration and Pd as a modifier. The precision, expressed as relative standard deviation, was better than 5% and the limit of detection was 1 {mu}g L{sup - 1}. The validation of the method was performed against a standard reference material Whole Egg Powder (RM 8415), and the measured Se corresponded to 95.2% of the certified value. The method was used for the determination of the Se level in eggs from hens treated with Se dietary supplements. Inorganic and organic Se sources were added to hen feed. The Se content of eggs was higher when hens were fed with organic Se compared to the other treatments. The proposed method, including sample emulsification for subsequent Se determination by GF AAS has proved to be sensitive, reproducible, simple and economical.

  15. Matching the laser wavelength to the absorption properties of matrices increases the ion yield in UV-MALDI mass spectrometry.

    Science.gov (United States)

    Wiegelmann, Marcel; Soltwisch, Jens; Jaskolla, Thorsten W; Dreisewerd, Klaus

    2013-09-01

    A high analytical sensitivity in ultraviolet matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) is only achieved if the laser wavelength corresponds to a high optical absorption of the matrix. Laser fluence and the physicochemical properties of the compounds, e.g., the proton affinity, also influence analytical sensitivity significantly. In combination, these parameters determine the amount of material ejected per laser pulse and the ion yield, i.e., the fraction of ionized biomolecules. Here, we recorded peptide ion signal intensities as a function of these parameters. Three cinnamic acid matrices were investigated: α-cyano-4-hydroxycinnamic acid, α-cyano-4-chlorocinnamic acid, and α-cyano-2,4-difluorocinnamic acid. In addition, 2,5-dihydroxybenzoic acid was used in comparison experiments. Ion signal intensities "per laser shot" and integrated ion signal intensities were acquired over 900 consecutive laser pulses applied on distinct positions on the dried-droplet sample preparations. With respect to laser wavelength, the two standard MALDI wavelengths of 337/355 nm were investigated. Also, 305 or 320 nm was selected to account for the blue-shifted absorption profiles of the halogenated derivatives. Maximal peptide ion intensities were obtained if the laser wavelength fell within the peak of the absorption profile of the compound and for fluences two to three times the corresponding ion detection threshold. The results indicate ways for improving the analytical sensitivity in MALDI-MS, and in particular for MALDI-MS imaging applications where a limited amount of material is available per irradiated pixel.

  16. Multi-element analysis of manganese nodules by atomic absorption spectrometry without chemical separation

    Science.gov (United States)

    Kane, J.S.; Harnly, J.M.

    1982-01-01

    Five manganese nodules, including the USGS reference nodules A-1 and P-1, were analyzed for Co, Cu, Fe, K, Mg, Mn, Na, Ni and Zn without prior chemical separation by using a simultaneous multi-element atomic absorption spectrometer with an air-cetylene flame. The nodules were prepared in three digestion matrices. One of these solutions was measured using sixteen different combinations of burner height and air/acetylene ratios. Results for A-1 and P-1 are compared to recommended values and results for all nodules are compared to those obtained with an inductively coupled plasma. The elements Co, Cu, Fe, K, Mg, Mn, Na, Ni, and Zn are simultaneously determined with a composite recovery for all elements of 100 ?? 7%, independent of the digestion matrices, heights in the flame, or flame stoichiometries examined. Individual recoveries for Co, K, and Ni are considerably poorer in two digests than this composite figure, however. The optimum individual recoveries of 100 ?? 5% and imprecisions of 1-4%, except for zinc, are obtained when Co, K, Mn, Na and Ni are determined simultaneously in a concentrated digest, and in another analytical sequence, when Cu, Fe, Mg, Mn and Zn are measured simultaneously after dilution. Determination of manganese is equally accurate in the two sequences; its measurement in both assures internal consistency between the two measurement sequences. This approach improves analytical efficiency over that for conventional atomic absorption methods, while minimizing loss of accuracy or precision for individual elements. ?? 1982.

  17. Direct determination of particulate elements in edible oils and fats using an ultrasonic slurry sampler with graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    van Dalen, Gerard; de Galan, Leo

    1994-12-01

    Through the use of an ultrasonic slurry mixer, graphite furnace atomic absorption spectrometry (GFAAS) can be applied for the fully automated determination of particulate iron and nickel in edible oils and fats. The unsupervised ultrasonic slurry autosampler yields the same accuracy and somewhat better precision than the much more laborious manual GFAAS method.

  18. Speciation of arsenic(III)/arsenic(V) and selenium(IV)/ selenium(VI) using coupled ion chromatography - hydride generation atomic absorption spectrometry

    Science.gov (United States)

    Simple analytical methods have been developed to speciate inorganic arsenic and selenium in the ppb range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determinations of the redox states arsenite A...

  19. Selective Flow Injection Analysis of Ultra-trace Amounts of Cr(VI), Preconcentration of It by Solvent Extraction, and Determination by Electrothermal Atomic Absorption Spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Sturup, Stefan; Spliid, Henrik

    1999-01-01

    A rapid, robust, sensitive and selective time-based flow injection (FI) on-line solvent extraction system interfaced with electrothermal atomic absorption spectrometry (ETAAS) is described for analyzing ultra-trace amounts of Cr(VI). The sample is initially mixed on-line with isobutyl methyl ketone...

  20. Investigations into the Role of Modifiers for Entrapment of Hydrides in Flow Injection Hydride Generation Electrothermal Atomic Absorption Spectrometry as Exemplified for the Determination of Germanium

    DEFF Research Database (Denmark)

    Hilligsøe, Bo; Andersen, Jens Enevold Thaulov; Hansen, Elo Harald

    1997-01-01

    Pd-conditioned graphite tubes, placed in the furnace of an atomic absorption spectrometry instrument, are used for entrapment of germane as generated in an associated flow injection system. Two different approaches are tested with the ultimate aim to allow multiple determinations, that is, introd...

  1. Determination of bismuth by dielectric barrier discharge atomic absorption spectrometry coupled with hydride generation: Method optimization and evaluation of analytical performance

    Czech Academy of Sciences Publication Activity Database

    Kratzer, Jan; Boušek, J.; Sturgeon, R. E.; Mester, Z.; Dědina, Jiří

    2014-01-01

    Roč. 86, č. 19 (2014), s. 9620-9625 ISSN 0003-2700 Grant - others:GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

  2. Determination of methane emission rates on a biogas plant using data from laser absorption spectrometry.

    Science.gov (United States)

    Groth, Angela; Maurer, Claudia; Reiser, Martin; Kranert, Martin

    2015-02-01

    The aim of the work was to establish a method for emission control of biogas plants especially the observation of fugitive methane emissions. The used method is in a developmental stage but the topic is crucial to environmental and economic issues. A remote sensing measurement method was adopted to determine methane emission rates of a biogas plant in Rhineland-Palatinate, Germany. An inverse dispersion model was used to deduce emission rates. This technique required one concentration measurement with an open path tunable diode laser absorption spectrometer (TDLAS) downwind and upwind the source and basic wind information, like wind speed and direction. Different operating conditions of the biogas plant occurring on the measuring day (December 2013) could be represented roughly in the results. During undisturbed operational modes the methane emission rate averaged 2.8 g/s, which corresponds to 4% of the methane gas production rate of the biogas plant. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Arsenic Speciation of Waters from the Aegean Region, Turkey by Hydride Generation: Atomic Absorption Spectrometry.

    Science.gov (United States)

    Çiftçi, Tülin Deniz; Henden, Emur

    2016-08-01

    Arsenic in drinking water is a serious problem for human health. Since the toxicity of arsenic species As(III) and As(V) is different, it is important to determine the concentrations separately. Therefore, it is necessary to develop an accurate and sensitive method for the speciation of arsenic. It was intended with this work to determine the concentrations of arsenic species in water samples collected from Izmir, Manisa and nearby areas. A batch type hydride generation atomic absorption spectrometer was used. As(V) gave no signal under the optimal measurement conditions of As(III). A certified reference drinking water was analyzed by the method and the results showed excellent agreement with the reported values. The procedure was applied to 34 water samples. Eleven tap water, two spring water, 19 artesian well water and two thermal water samples were analyzed under the optimal conditions.

  4. Determination of trace amounts of tin in geological materials by atomic absorption spectrometry

    Science.gov (United States)

    Welsch, E.P.; Chao, T.T.

    1976-01-01

    An atomic absorption method is described for the determination of traces of tin in rocks, soils, and stream sediments. A dried mixture of the sample and ammonium iodide is heated to volatilize tin tetraiodide -which is then dissolved in 5 % hydrochloric acid, extracted into TOPO-MIBK, and aspirated into a nitrous oxide-acetylene flame. The limit of determination is 2 p.p.m. tin and the relative standard deviation ranges from 2 to 14 %. Up to 20 % iron and 1000 p.p.m. Cu, Pb, Zn, Mn, Hg, Mo, V, or W in the sample do not interfere. As many as 50 samples can be easily analyzed per man-day. ?? 1976.

  5. Matrix effects in the determination of molybdenum in plants by carbon furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Studnicki, M.

    1979-07-01

    Molybdenum is a microelement taken by plants in lower quantities than other microelements. The effects of different acids, cations, and anions important in plant materials are analyzed. A double-beam Instrumentation Laboratory atomic absorption spectrometer Model 251 with hydrogen background corrector, a graphite furnace IL 455, and Dohrmann Envirotech recorder Model SC 1200 were used. Acids strongly influence the Mo signal. Most of the phosphoric acid in the range 0.01 to 1% increased the signal. Ammonium salts of these acids also changed the Mo signal, but the sign of the change may be other than for the acids (for example, ammonium nitrates). Calcium chloride strongly decreased the signal. This influence was reduced in the presence of ammonium phosphate and the disodium salt of EDTA. 5 figures.

  6. [Efficiency of hemoperfusion on clearing thallium based on atomic absorption spectrometry].

    Science.gov (United States)

    Tian, Tian; Wang, Yongan; Nie, Zhiyong; Wang, Jiao; Peng, Xiaobo; Yuan, Ye; Li, Wanhua; Qiu, Zewu; Xue, Yanping; Xiong, Yiru

    2015-04-01

    To determine thallium in whole blood by atomic absorption detection method, and to investigate the eliminating effect of hemoperfusion (HP) for thallium in blood. The blood of Beagle dogs which had not exposed to thallium before were obtained for preparation of thallium nitrate ( TlNO3 )-containing solution in three concentrations according to the conversion formula based on animal weight and volume of blood. HP was performed in the simulated in vivo environment. The content of TlNO3 in blood of the next group was determined on the amount of TlNO3 for the last HP of the former dose group. Thallium quantity in different samples was measured with atomic absorption spectrometer blood samples before and after HP. Finally, the thallium concentration in blood was analyzed statistically. Thallium concentrations showed a good linear relationship in the range of 0-200 μg/L (r = 0.998 4). The intra-day precision (RSD) was lower than 4.913%, the intra-day recovery rate was 96.2%-111.9%; the inter-day precision (RSD) was lower than 7.502%, the inter-day recovery rate was 89.6%-105.2%. The concentration of thallium in blood was significantly reduced after HP per time in high, middle, and low dose groups [(453.43 ± 27.80) mg/L to (56.09 ± 14.44) mg/L in high dose group, F = 8.820, P = 0.003; (64.51 ± 13.60) mg/L to (3.19 ± 0.23) mg/L in middle dose group, F = 36.312, P = 0.000; (5.40 ± 0.98) mg/L to (0.38 ± 0.25) mg/L in low dose group, F = 46.240, P = 0.000 ]. The adsorption rate of four times of HP in high, middle and low dose group were (87.63 ± 2.48 )%, (95.06 ± 1.54 )% and (92.76 ± 4.87)%, respectively, without significant difference (F = 4.231, P = 0.070). The method for measuring thallium was established, and it shows a very stable, simple, sensitive for determination of thallium. HP can effectively remove thallium from blood. Thallium concentration can be reduced by 90% after four times of HP. HP is also effective even when thallium concentration is not high.

  7. Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Elsheimer, H.N.; Fries, T.L.

    1990-01-01

    A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of tricotylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 ??g l-1 of tin in the MIBK solution or 0.2-0.3 ??g g-61 in the rock. The concentration range is linear between 2.5 and 500 ??g l-1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 ??g l-1 level and < 7% at the 10-30 ??g l-1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 ??g g-1 or less.

  8. Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection.

    Science.gov (United States)

    Huber, Charles S; Vale, Maria Goreti R; Dessuy, Morgana B; Svoboda, Milan; Musil, Stanislav; Dědina, Jiři

    2017-12-01

    A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO3, HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL-1 HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg-1 for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg-1 which were below the limits of 300, 200 and 100µgkg-1 set by the Brazilian, Chinese and European legislation, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Chemical modifiers in arsenic determination in biological materials by tungsten coil electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bruhn, C.G.; Huerta, V.N.; Neira, J.Y. [Departamento de Analisis Instrumental, Facultad de Farmacia, Universidad de Concepcion, P.O. Box 237, Concepcion (Chile)

    2004-01-01

    Palladium, iridium, and rhodium are evaluated as possible chemical modifiers in the determination of As in digest solutions of biological materials (human hair and clam) by tungsten coil electrothermal atomic absorption spectrophotometry (TCA-AAS). The modifier in solution was applied onto the coil and thermally pre-reduced; the pre-reduction conditions, the amount of modifier, and the thermal program were optimized. Palladium was not satisfactory, whereas Ir and Rh were effective modifiers and rendered better relative sensitivity for As by a factor of 1.4 and 1.9, respectively compared to the case without modifier. Upon optimization of thermal conditions for As in pre-reduced Ir (2.0 {mu}g) and Rh (2.0 {mu}g) modifiers and in the digest solutions of the study matrices, Rh (2.0 {mu}g) was more effective modifier and was selected as such. The mean within-day repeatability was 2.8% in consecutive measurements (25-100 {mu}g L{sup -1}) (3 cycles, each of n=6) and confirmed good short-term stability of the absorbance measurements. The mean reproducibility was 4.4% (n=20 in a 3-day period) and the detection limit (3{sigma}{sub blank}/slope) was 29 pg (n=15). The useful coil lifetime in Rh modifier was extended to 300-400 firings. Validation was by determination of As in the certified reference material (CRM) of ''Oyster tissue'' solution with a percentage relative error (E{sub rel}%) of 2% and percentage relative standard deviation (RSD%) of 3% (n=4), and by analytical recovery of As spiked in CRM of human hair [94{+-}8% (n=4)]. The methodology is simple, fast (sample readout frequency 21 h{sup -1}), reliable, of low cost, and was applied to the determination of As in hair samples of exposed and unexposed workers. (orig.)

  10. Atomic Absorption Spectrometry in Wilson's Disease and Its Comparison with Other Laboratory Tests and Paraclinical Findings.

    Science.gov (United States)

    Mahjoub, Fatemeh; Fereiduni, Rana; Jahanzad, Isa; Farahmand, Fatemeh; Monajemzadeh, Maryam; Najafi, Mehri

    2012-03-01

    Wilson's disease (WD) is an autosomal recessive disease with genetic abnormality on chromosome 13 causing defect in copper metabolism and increased copper concentration in liver, central nervous system and other organs, which causes different clinical manifestations. The aim of this study was to determine the sensitivity of different clinical and paraclinical tests for diagnosis of Wilson's disease. Paraffin blocks of liver biopsy from 41 children suspicious of WD were collected. Hepatic copper concentrations were examined with atomic absorption spectrophotometry (Australian GBC, model: PAL 3000). Fifteen specimens had hepatic copper concentration (dry weight) more than 250μg/g. Clinical and laboratory data and histologic slides of liver biopsies of these 15 children were reviewed retrospectively. Liver tissue was examined for staging and grading of hepatic involvement and also stained with rubeonic acid method for copper. Patients were 5-15 years old (mean age=9.3 years, standard deviation=2.6) with slight male predominance (9/15=60%). Five (33%) patients were 10 years old. Three (20%) of them were referred for icterus, 8 (54%) because of positive family history, 2 (13%) due to abdominal pain and 2 (13%) because of hepatosplenomegaly and ascites. Serum AST and ALT levels were elevated at the time of presentation in all patients. In liver biopsy, histological grade and stage was 0-8 and 0-6 respectively, 2 (13%) had cirrhosis, 1 (7%) had normal biopsy and 12 (80%) showed chronic hepatitis. Hepatic copper concentrations were between 250 and 1595 μg/g dry weight. The sensitivity of various tests were 85% for serum copper, 83% for serum ceruloplasmin, 53% for urinary copper excretion, 44% for presence of KF ring and 40% for rubeonic acid staining on liver biopsies. None of the tests stated in the article were highly sensitive for diagnosis of WD, so we suggest that diagnosis should be based on combination of family history, physical examination and different tests.

  11. Matrix elimination method for the determination of precious metals in ores using electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Salih, Bekir [Hacettepe University, Department of Chemistry, Ankara (Turkey)]. E-mail: bekir@hacettepe.edu.tr; Celikbicak, Omuer [Hacettepe University, Department of Chemistry, Ankara (Turkey); Doeker, Serhat [Hacettepe University, Department of Chemistry, Ankara (Turkey); Dogan, Mehmet [Hacettepe University, Department of Chemistry, Ankara (Turkey)

    2007-03-28

    Poly(N-(hydroxymethyl)methacrylamide)-1-allyl-2-thiourea) hydrogels, poly(NHMMA-ATU), were synthesized by gamma radiation using {sup 60}Co {gamma} source in the ternary mixture of NHMMA-ATU-H{sub 2}O. These hydrogels were used for the specific gold, silver, platinum and palladium recovery, pre-concentration and matrix elimination from the solutions containing trace amounts of precious metal ions. Elimination of inorganic matrices such as different transition and heavy metal ions, and anions was performed by adjusting the solution pH to 0.5 that was the selective adsorption pH of the precious metal ions. Desorption of the precious metal ions was performed by using 0.8 M thiourea in 3 M HCl as the most efficient desorbing agent with recovery values more than 95%. In the desorption medium, thiourea effect on the atomic signal was eliminated by selecting proper pyrolysis and atomization temperatures for all precious metal ions. Precision and the accuracy of the results were improved in the graphite furnace-atomic absorption spectrometer (GFAAS) measurements by applying the developed matrix elimination method performing the adsorption at pH 0.5. Pre-concentration factors of the studied precious metal ions were found to be at least 1000-fold. Detection limits of the precious metal ions were found to be less than 10 ng L{sup -1} of the all studied precious metal ions by using the proposed pre-concentration method. Determination of trace levels of the precious metals in the sea-water, anode slime, geological samples and photographic fixer solutions were performed using GFAAS clearly after applying the adsorption-desorption cycle onto the poly(NHMMA-UTU) hydrogels.

  12. Simultaneous determination of rhodium and ruthenium by high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Zambrzycka-Szelewa, Elżbieta; Lulewicz, Marta; Godlewska-Żyłkiewicz, Beata

    2017-07-01

    In the present paper a fast, simple and sensitive analytical method for simultaneous determination of rhodium and ruthenium by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) was developed. Among six pairs of absorption atomic lines of Rh and Ru, which are close enough to enable their simultaneous detection, two pairs were selected for further studies. Best results were obtained for measurements of the resonance line of rhodium at 343.489 nm and the adjacent secondary line of ruthenium at 343.674 nm (23% intensity of this line). For evaluated lines, the absorbance values were obtained using three pixels. The pyrolysis and atomization temperatures were 1200 °C and 2600 °C, respectively. Under these conditions the limits of detection achieved for Rh and Ru were found to be 1.0 μg L- 1 and 1.9 μg L- 1, respectively. The characteristic mass was 12.9 pg for Rh and 71.7 pg for Ru. Repeatability of the results expressed as a relative standard deviation was typically below 6%. The trueness of the method was confirmed by analysis of the certified reference material - platinum ore (SARM 76). The recovery of Rh and Ru from the platinum ore was 93.0 ± 4.6% and 90.1 ± 2.5%, respectively. The method was successfully applied to the direct simultaneous determination of trace amounts of rhodium and ruthenium in spiked river water, road runoff, and municipal sewage. Separation of interfering matrix on cation exchange resin was required before analysis of road dust and tunnel dust (CW-7) by HR-CS GFAAS.

  13. The chemical generation of NO for the determination of nitrite by high-resolution continuum source molecular absorption spectrometry.

    Science.gov (United States)

    Brandao, Geovani C; Lima, Daniel C; Ferreira, Sergio L C

    2012-08-30

    In the present work, we propose a method for the determination of nitrite based on the chemical generation of nitric oxide (NO) and its detection by high-resolution continuum source molecular absorption spectrometry. NO is generated by the reduction of nitrite in acidic media with ascorbic acid as the reducing agent and then transferred into a quartz cell by a stream of argon carrier gas. The conditions under which the NO is generated are as follows: 0.4 mol L(-1) hydrochloric acid, 1.5%(w/v) ascorbic acid, an argon gas pressure of 0.03 MPa and an injection time of the reducing agent of 4s. All measurements of molecular absorption were performed using the NO line at 215.360 nm, and the signal was measured by peak height. Under these conditions, the method described has limits of detection and quantification of 0.045 and 0.150 μg mL(-1) of nitrite, respectively. The calibration curve is linear for nitrite concentrations in the range 0.15-15 μg mL(-1). The precision, estimated as the relative standard deviation (RSD), was 3.5% and 4.4% for solutions with nitrite concentrations of 0.5 and 5.0 μg mL(-1), respectively. This method was applied to the analysis of different water samples (well water, drinking water and river water) collected in Cachoeira City, Bahia State, Brazil. The results were in agreement with those obtained by a spectrophotometric method using the Griess reaction. Addition/recovery tests were also performed to check the validity of the proposed method. Recoveries of 93-106% were achieved. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Human vitamin B12 absorption measurement by accelerator mass spectrometry using specifically labeled (14)C-cobalamin.

    Science.gov (United States)

    Carkeet, Colleen; Dueker, Stephen R; Lango, Jozsef; Buchholz, Bruce A; Miller, Joshua W; Green, Ralph; Hammock, Bruce D; Roth, John R; Anderson, Peter J

    2006-04-11

    There is a need for an improved test of human ability to assimilate dietary vitamin B(12). Assaying and understanding absorption and uptake of B(12) is important because defects can lead to hematological and neurological complications. Accelerator mass spectrometry is uniquely suited for assessing absorption and kinetics of carbon-14 ((14)C)-labeled substances after oral ingestion because it is more sensitive than decay counting and can measure levels of (14)C in microliter volumes of biological samples with negligible exposure of subjects to radioactivity. The test we describe employs amounts of B(12) in the range of normal dietary intake. The B(12) used was quantitatively labeled with (14)C at one particular atom of the dimethylbenzimidazole (DMB) moiety by exploiting idiosyncrasies of Salmonella metabolism. To grow aerobically on ethanolamine, Salmonella enterica must be provided with either preformed B(12) or two of its precursors, cobinamide and DMB. When provided with (14)C-DMB specifically labeled in the C2 position, cells produced (14)C-B(12) of high specific activity (2.1 GBq/mmol, 58 mCi/mmol) (1 Ci = 37 GBq) and no detectable dilution of label from endogenous DMB synthesis. In a human kinetic study, a physiological dose (1.5 microg, 2.2 kBq/59 nCi) of purified (14)C-B(12) was administered and showed plasma appearance and clearance curves consistent with the predicted behavior of the pure vitamin. This method opens new avenues for study of B(12) assimilation.

  15. Human vitamin B12 absorption measurement by accelerator mass spectrometry using specifically labeled 14C-cobalamin

    Science.gov (United States)

    Carkeet, Colleen; Dueker, Stephen R.; Lango, Jozsef; Buchholz, Bruce A.; Miller, Joshua W.; Green, Ralph; Hammock, Bruce D.; Roth, John R.; Anderson, Peter J.

    2006-01-01

    There is a need for an improved test of human ability to assimilate dietary vitamin B12. Assaying and understanding absorption and uptake of B12 is important because defects can lead to hematological and neurological complications. Accelerator mass spectrometry is uniquely suited for assessing absorption and kinetics of carbon-14 (14C)-labeled substances after oral ingestion because it is more sensitive than decay counting and can measure levels of 14C in microliter volumes of biological samples with negligible exposure of subjects to radioactivity. The test we describe employs amounts of B12 in the range of normal dietary intake. The B12 used was quantitatively labeled with 14C at one particular atom of the dimethylbenzimidazole (DMB) moiety by exploiting idiosyncrasies of Salmonella metabolism. To grow aerobically on ethanolamine, Salmonella enterica must be provided with either preformed B12 or two of its precursors, cobinamide and DMB. When provided with 14C-DMB specifically labeled in the C2 position, cells produced 14C-B12 of high specific activity (2.1 GBq/mmol, 58 mCi/mmol) (1 Ci = 37 GBq) and no detectable dilution of label from endogenous DMB synthesis. In a human kinetic study, a physiological dose (1.5 μg, 2.2 kBq/59 nCi) of purified 14C-B12 was administered and showed plasma appearance and clearance curves consistent with the predicted behavior of the pure vitamin. This method opens new avenues for study of B12 assimilation. PMID:16585531

  16. Human Vitamin B12 Absorption and Metabolism are Measured by Accelerator Mass Spectrometry Using Specifically Labeled 14C-Cobalamin

    Energy Technology Data Exchange (ETDEWEB)

    Carkeet, C; Dueker, S R; Lango, J; Buchholz, B A; Miller, J W; Green, R; Hammock, B D; Roth, J R; Anderson, P J

    2006-01-26

    There is need for an improved test of human ability to assimilate dietary vitamin B{sub 12}. Assaying and understanding absorption and uptake of B{sub 12} is important because defects can lead to hematological and neurological complications. Accelerator mass spectrometry (AMS) is uniquely suited for assessing absorption and kinetics of {sup 14}C-labeled substances after oral ingestion because it is more sensitive than decay counting and can measure levels of carbon-14 ({sup 14}C) in microliter volumes of biological samples, with negligible exposure of subjects to radioactivity. The test we describe employs amounts of B{sub 12} in the range of normal dietary intake. The B{sub 12} used was quantitatively labeled with {sup 14}C at one particular atom of the DMB moiety by exploiting idiosyncrasies of Salmonellametabolism. In order to grow aerobically on ethanolamine, S. entericamust be provided with either pre-formed B{sub 12} or two of its precursors: cobinamide and dimethylbenzimidazole (DMB). When provided with {sup 14}C-DMB specifically labeled in the C2 position, cells produced {sup 14}C-B{sub 12} of high specific activity (2.1 GBq/mmol, 58 mCi/mmol) and no detectable dilution of label from endogenous DMB synthesis. In a human kinetic study, a physiological dose (1.5 mg, 2.2 KBq/59 nCi) of purified {sup 14}C-B{sub 12} was administered and showed plasma appearance and clearance curves consistent with the predicted behavior of the pure vitamin. This method opens new avenues for study of B{sub 12} assimilation.

  17. Investigations on Freon-assisted atomization of refractory analytes (Cr, Mo, Ti, V) in multielement electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Heinrich, Hans-Joachim [Federal Institute for Materials Research and Testing (BAM), Division I.1 Inorganic Chemical Analysis, Reference Materials, Richard-Willstaetter-Strasse 11, D-12489 Berlin (Germany)], E-mail: hans-joachim.heinrich@bam.de; Matschat, Ralf [Federal Institute for Materials Research and Testing (BAM), Division I.1 Inorganic Chemical Analysis, Reference Materials, Richard-Willstaetter-Strasse 11, D-12489 Berlin (Germany)

    2007-08-15

    Premixed 1% Freon in argon inner gas of various composition (CCl{sub 2}F{sub 2}, CHClF{sub 2}, CHF{sub 3}) was applied to graphite furnace atomizer to minimize unfavorable effects of carbide formation, such as signal tailing and memory effects in the simultaneous determination of Cr, Mo, Ti and V refractory analytes by electrothermal atomic absorption spectrometry using a multielement atomic absorption spectrometer. The effect of these gaseous additives was investigated when applied separately in atomization, pyrolysis and clean-out steps. The halogenation effects were analytically useful only under the precondition of using Ar-H{sub 2} outer gas to the furnace to all heating steps, and also using this gas in the pre-atomization (drying, pyrolysis) steps. Optimum analytical performance was obtained when mixtures of 1% Freon in argon were applied just before and during the atomization step at a flow rate of 50 mL min{sup -1} and 2% hydrogen was used as purge gas. Using optimum conditions, signal tailings and carry-over contamination were reduced effectively and good precision (relative standard deviation below 1%) could be attained. Applying 1% CHClF{sub 2} and an atomization temperature of 2550 deg. C, the characteristic masses obtained for simple aqueous solutions were 8.8 pg for Cr, 17 pg for Mo, 160 pg for Ti, and 74 pg for V. The limits of detection were 0.05, 0.2, 2.3 and 0.5 {mu}g L{sup -1} for Cr, Mo, Ti and V, respectively. The developed method was applied to the analysis of digests of advanced ceramics. The accuracy of the procedure was confirmed by analyzing the certified reference material ERM-ED 102 (Boron Carbide Powder) and a silicon nitride powder distributed in the inter-laboratory comparison CCQM-P74.

  18. Determination of selected elements in whole coal and in coal ash from the eight argonne premium coal samples by atomic absorption spectrometry, atomic emission spectrometry, and ion-selective electrode

    Science.gov (United States)

    Doughten, M.W.; Gillison, J.R.

    1990-01-01

    Methods for the determination of 24 elements in whole coal and coal ash by inductively coupled argon plasma-atomic emission spectrometry, flame, graphite furnace, and cold vapor atomic absorption spectrometry, and by ion-selective electrode are described. Coal ashes were analyzed in triplicate to determine the precision of the methods. Results of the analyses of NBS Standard Reference Materials 1633, 1633a, 1632a, and 1635 are reported. Accuracy of the methods is determined by comparison of the analysis of standard reference materials to their certified values as well as other values in the literature.

  19. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Sun, Mei; Wu, Qianghua

    2010-04-15

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL(-1). The relative standard deviation (n=7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin. 2009 Elsevier B.V. All rights reserved.

  20. Determination of vanadium in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry using permanent modifiers.

    Science.gov (United States)

    Dobrowolski, Ryszard; Adamczyk, Agnieszka; Otto, Magdalena

    2013-09-15

    A new analytical procedure for vanadium (V) determination in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry (slurry sampling GFAAS) using the mixed permanent modifiers is described. Moreover, the comparison of action of the modifiers based on the iridium (Ir) and carbide-forming elements: tungsten (W) and niobium (Nb) deposited on the graphite tubes is studied, especially in terms of their analytical utility and determination sensitivity. The mechanism of their action was investigated using an X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray detector (EDX). Finally, the mixture of 0.3 μg of Ir and 0.04 μg of Nb was used for the graphite tube permanent modification. The analytical procedure was optimized on the basis of the data from pyrolysis and atomization temperature curves studies. The results obtained for the four certified reference materials (marine sediments: PACS-1 and MESS-1, lake sediment: SL-1, soil: San Joaquin Soil SRM 2709), using the slurry sampling GFAAS and the standard calibration method, were in good agreement with the certified values. The detection and quantification limits and characteristic mass calculated for the proposed procedure were 0.04 µg/g, 0.16 µg/g and 11.9 pg, respectively. The precision (RSD% less than 8%) and the accuracy of vanadium determination in the soil and sediment samples were acceptable. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A., E-mail: djan@terra.com.br

    2013-08-01

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v{sup −1} of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L{sup −1} with a limit of detection of 4.9 μg L{sup −1} and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L{sup −1} Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials. - Highlights: ► Molybdenum was determined in plants by flame AAS. ► Flame AAS sensitivity was improved using microextraction and discrete nebulization. ► The developed procedure can be easily implemented in routine analysis. ► Green chemistry principles are followed.

  2. Sensitive determination of cadmium in water samples by room temperature ionic liquid-based preconcentration and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martinis, Estefania M. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Olsina, Roberto A. [Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis (Argentina); Altamirano, Jorgelina C. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina); Wuilloud, Rodolfo G. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)], E-mail: rwuilloud@mendoza-conicet.gov.ar

    2008-10-17

    A sensitive preconcentration methodology for Cd determination at trace levels in water samples was developed in this work. 1-Butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]) room temperature ionic liquid (RTIL) was successfully used for Cd preconcentration, as cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex [Cd-5-Br-PADAP]. Subsequently, Cd was back-extracted from the RTIL phase with 500 {mu}L of 0.5 mol L{sup -1} nitric acid and determined by electrothermal atomic absorption spectrometry (ETAAS). A preconcentration factor of 40 was achieved with 20 mL of sample. The limit of detection (LOD) obtained under optimum conditions was 3 ng L{sup -1} and the relative standard deviation (R.S.D.) for 10 replicates at 1 {mu}g L{sup -1} Cd{sup 2+} concentration level was 3.5%, calculated at peak heights. The calibration graph was linear from concentration levels near the detection limits up to at least 5 {mu}g L{sup -1}. A correlation coefficient of 0.9997 was achieved. Validation of the methodology was performed by standard addition method and analysis of certified reference material (CRM). The method was successfully applied to the determination of Cd in river and tap water samples.

  3. Determination of trace copper in food samples by flame atomic absorption spectrometry after solid phase extraction on modified soybean hull

    Energy Technology Data Exchange (ETDEWEB)

    Xiang Guoqiang, E-mail: xianggq@126.com [School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001 (China); Zhang Yingming; Jiang Xiuming; He Lijun; Fan Lu; Zhao Wenjie [School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001 (China)

    2010-07-15

    Soybean hull was chemically modified with citric acid and used as a solid phase extraction adsorbent for the determination of trace amounts of Cu{sup 2+} in food samples by flame absorption spectrometry (FAAS). The effect of pH, sample flow rate and volume, elution flow rate and volume and co-existing ions on the recovery of the analyte were investigated. The results showed that Cu{sup 2+} could be adsorbed on the modified soybean hull at pH 8.0 and eluted by 2.0 mL of 1.0 mol L{sup -1} HCl. Under the optimized conditions, the adsorption capacity of modified soybean hull was found to be 18.0 mg g{sup -1} for Cu{sup 2+}. The detection limit of the proposed method was 0.8 ng mL{sup -1} for Cu{sup 2+} with an enrichment factor of 18. The analytical result for the certified reference tea sample (GBW07605) was in a good agreement with the certified value. The proposed method has also been successfully applied to the determination of trace Cu{sup 2+} in dried sweet potato, lake water and milk powder, the recovery of Cu{sup 2+} for spiked samples was between 91% and 109.6%.

  4. Separation and preconcentration of trace amounts of gold from water samples prior to determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Fatemeh Sabermahani

    2016-11-01

    Full Text Available A preconcentration/separation procedure is presented for the solid phase extraction of trace gold(III as its rubeanic acid (dithiooxamide chelate on silica gel, prior to determination by flame atomic absorption spectrometry. The influences of analytical parameters including pH of the aqueous solution, the amount of the sorbent, time of the complex formation, ligand amount, flow rates of sample and elution solutions and the type, concentration and volume of elution solution on the quantitative recoveries of Au(III were investigated. At pH 3.5, the maximum sorption capacity of Au3+ was 7.5 mg g−1, by column method. The linearity was maintained in the concentration range of 1.0–3.4 × 104 ng mL−1 for gold in the original solution. The preconcentration factor of 100 and relative standard deviation of ±1.7% were obtained, under optimum conditions. The limit of detection (LOD was calculated as 0.80 ng mL−1, based on 3σbl/m (n = 8 in the original solutions. The proposed method was successfully applied to the determination trace amounts of gold in the water samples.

  5. Multiwalled carbon nanotubes microcolumn preconcentration and determination of gold in geological and water samples by flame atomic absorption spectrometry

    Science.gov (United States)

    Liang, Pei; Zhao, Ehong; Ding, Qiong; Du, Dan

    2008-06-01

    The potential of multiwalled carbon nanotubes (MWNTs) as solid-phase extraction adsorbent for the separation and preconcentration of gold has been investigated. Gold could be adsorbed quantitatively on MWNTs in the pH range of 1-6, and then eluted completely with 2 mL of 3% thiourea in 1 mol L - 1 HCl solution at a flow rate of 0.5 mL min - 1 . A new method using a microcolumn packed with MWNTs as sorbent has been developed for the preconcentration of trace amount of Au prior to its determination by flame atomic absorption spectrometry. Parameters influencing the preconcentration of Au, such as pH of the sample, sample flow rate and volume, elution solution and interfering ions, have been examined and optimized. Under the optimum experimental conditions, the detection limit of this method for Au was 0.15 µg L - 1 with an enrichment factor of 75, and the relative standard deviation (R.S.D) was 3.1% at the 100 µg L - 1 Au level. The method has been applied for the determination of trace amount of Au in geological and water samples with satisfactory results.

  6. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Teslima Daşbaşı

    2016-01-01

    Full Text Available A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4- complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1 with detection limit of 4.0 μg L−1 (n=13. The precision as relative standard deviation was 3% (n=11, 0.20 mg L−1 and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water.

  7. [Determination of metals in waste bag filter of steel works by microwave digestion-flame atomic absorption spectrometry].

    Science.gov (United States)

    Ning, Xun-An; Zhou, Yun; Liu, Jing-Yong; Wang, Jiang-Hui; Li, Lei; Ma, Xiao-Guo

    2011-09-01

    A method of microwave digestion technique-flame atomic absorption spectrometry was proposed to determine the total contents of Cu, Zn, Pb, Cd, Cr and Ni in five different kinds of waste bag filters from a steel plant. The digestion effects of the six acid systems on the heavy metals digestion were studied for the first time. The relative standard deviation (RSD) of the method was between 1.02% and 9.35%, and the recovery rates obtained by standard addition method ranged from 87.7% to 105.6%. The results indicated that the proposed method exhibited the advantages of simplicity, speediness, accuracy and repeatability, and it was suitable for determining the metal elements of the waste bag filter. The results also showed that different digestion systems should be used according to different waste bag filters. The waste bag filter samples from different production processes had different metal elements content. The Pb and Zn were the highest in the waste bag filters, while the Cu, Ni, Cd and Cr were relatively lower. These determination results provided the scientific data for further treatment and disposal of the waste bag filter.

  8. Determination of Gold in Various Environment Samples by Flame Atomic Absorption Spectrometry Using Dispersive Liquid–Liquid Microextraction Sampling

    Directory of Open Access Journals (Sweden)

    Şerife Saçmacı

    2015-07-01

    Full Text Available A new dispersive liquid–liquid microextraction separation/preconcentration procedure as a rapid sample-preparation technique is proposed for detection of ultra trace amounts of Au(III in various media by flame atomic absorption spectrometry using 1,5-diphenyl-1,3,5-pentanetrione as chelating agent. Carbon tetrachloride and methanol were used as extraction and dispersive solvents, respectively. Various parameters that affect the extraction efficiency such as pH, centrifugation rate and time, chelating agent concentration and sampling volume on the recovery of Au(III were investigated. Under optimum conditions, the enhancement factor of 750, relative standard deviation of 2.7 % and calibration graphs obtained in the concentration range of 0.04–5.6 μg L−1 for gold were obtained. The limit of detection was 1.1 ng L−1. The accuracy of the method was performed by analysis of the certified reference material (CDN-PGMS-10. The developed method was applied successfully to the determination of gold in the catalytic converter, anode slime, ore and seawater samples. The results show that dispersive liquid–liquid microextraction procedure is sensitive, rapid, simple and safe for the separation/preconcentration of gold from complex sample media.

  9. Total mercury determination in different tissues of broiler chicken by using cloud point extraction and cold vapor atomic absorption spectrometry.

    Science.gov (United States)

    Shah, A Q; Kazi, T G; Baig, J A; Afridi, H I; Kandhro, G A; Arain, M B; Kolachi, N F; Wadhwa, S K

    2010-01-01

    A cloud point extraction (CPE) method has been developed for the determination of total mercury (Hg) in different tissues of broiler chicken by cold vapor atomic absorption spectrometry (CVAAS). The broiler chicken tissues (leg, breast, liver and heart) were subjected to microwave assisted digestion in a mixture of nitric acid and hydrogen peroxide (2:1 ratio), prior to preconcentration by CPE. Various parameters such as the amount of ammonium O,O-diethyldithiophosphate (DDTP), concentrations of Triton X-114, equilibrium temperature, time and centrifugation have been studied in order to find the best conditions for the determination of mercury. For validation of proposed method a certified reference material, DORM-2 was used. No significant difference p>0.05 was observed between the experimental results and the certified values of CRM (paired t-test). The limit of detection and quantitation obtained under the optimal conditions were 0.117 and 0.382 microg/kg, respectively. The accumulation of Hg in different tissues were found in the order of, liver>muscles>heart. The concentration of Hg in chicken tissues were found in the range of 1.57-2.75, 1.40-2.27, 1.55-4.22, and 1.39-2.61 microg/kg in leg, breast, liver and heart, respectively. Copyright 2009 Elsevier Ltd. All rights reserved.

  10. In-situ suspended aggregate microextraction of gold nanoparticles from water samples and determination by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Choleva, Tatiana G; Kappi, Foteini A; Tsogas, George Z; Vlessidis, Athanasios G; Giokas, Dimosthenis L

    2016-05-01

    This work describes a new method for the extraction and determination of gold nanoparticles in environmental samples by means of in-situ suspended aggregate microextraction and electrothermal atomic absorption spectrometry. The method relies on the in-situ formation of a supramolecular aggregate phase through ion-association between a cationic surfactant and a benzene sulfonic acid derivative. Gold nanoparticles are physically entrapped into the aggregate phase which is separated from the bulk aqueous solution by vacuum filtration on the surface of a cellulose filter in the form of a thin film. The film is removed from the filter surface and is dissociated into an acidified methanolic solution which is used for analysis. Under the optimized experimental conditions, gold nanoparticles can be efficiently extracted from water samples with recovery rates between 81.0-93.3%, precision 5.4-12.0% and detection limits as low as 75femtomolL(-1) using only 20mL of sample volume. The satisfactory analytical features of the method along with the simplicity indicate the efficiency of this new approach to adequately collect and extract gold nanoparticle species from water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Xu, Hongbo; Wu, Yun; Wang, Jian; Shang, Xuewei; Jiang, Xiaojun

    2013-12-01

    A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results. Copyright © 2013 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

  12. Determining the arsenic, cadmium, lead, copper and chromium contents by atomic absorption spectrometry in Pangasius fillets from Vietnam.

    Science.gov (United States)

    Molognoni, Luciano; Vitali, Luciano; Ploêncio, Leandro As; Santos, Jacson N; Daguer, Heitor

    2016-07-01

    Pangasius is a fish produced on a large scale in Vietnam and exported to many countries. Since river contamination from human activities can affect the safety of this food, fish consumption can cause exposure to potentially toxic elements for humans. The aim of this study, therefore, was to assess arsenic, cadmium, lead, copper and chromium contents by atomic absorption spectrometry in Pangasius fillet produced in the provinces of Dong Thap and Can Tho (Vietnam) and exported to Brazil. The limits of detection were: arsenic 0.5443 µg kg(-1) , cadmium 0.0040 mg kg(-1) , chromium 0.0004 mg kg(-1) , copper 0.0037 mg kg(-1) and lead 0.0284 mg kg(-1) . Analysis of 20 samples showed results below the limit of detection for arsenic, chromium and lead, while copper average concentration was 0.0234 mg kg(-1) . Cadmium average concentration was 0.0547 mg kg(-1) , with no significant difference between the two regions studied. The samples of Pangasius had no detectable concentrations of arsenic, chromium, copper and lead, and do not represent a hazard to public health. However, cadmium analysis revealed non-compliant samples, demonstrating the importance of monitoring the quality of imported Pangasius fish. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

  13. Comparative study of pretreatment methods for the determination of metals in atmospheric aerosol by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Karanasiou, A A; Thomaidis, N S; Eleftheriadis, K; Siskos, P A

    2005-03-15

    A comparative study of pretreatment methods for the determination of 10 elements (As, Cd, Pb, V, Ni, Mn, Cr, Cu, Fe, Al) in atmospheric aerosols by electrothermal atomic absorption spectrometry (ETAAS) was conducted. For the digestion of the particulates collected in filters, six methods were compared using a mixture of HNO(3) and HF with or without the addition of various oxidative agents (HClO(4) or H(2)O(2)) or acids (HCl). The comparative study was performed using loaded cellulose filter samples, which were digested in Parr bombs and heated in a conventional oven at 170 degrees C for 5h. The extraction efficiency and blanks were compared and it was proved that the digestion method using only HNO(3)-HF extracted most of the metals and gave the lowest blanks. The HNO(3)-HF mixture was selected for the development of an improved microwave digestion method specific for aerosol-loaded filters. The operating parameters were optimized, so that quantitative recovery of the reference materials NIST 1649a urban dust and NIST 1648 urban particulate matter was achieved. The blank of cellulose and teflon filters were also determined and compared. Teflon filters present the lowest blanks for all the elements. The obtained limits of detection for each type of filters were adequate for environmental monitoring purposes. ETAAS instrumental operation was also optimized for the compensation and the elimination of interferences. The temperature optimization was performed for each metal in every type of filter and optimized parameters are proposed for 10 elements.

  14. Investigation of the levels of some element in edible oil samples produced in Turkey by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mendil, Durali, E-mail: dmendil@gop.edu.tr [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Uluoezlue, Ozguer Dogan; Tuezen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Department of Chemistry, 38039 Kayseri (Turkey)

    2009-06-15

    The element contents (Fe, Mn, Zn, Cu, Pb, Co, Cd, Na, K, Ca and Mg) in edible oils (olive oil, hazelnut oil, sunflower oil, margarine, butter and corn oil) from Turkey were determined using atomic absorption spectrometry after microwave digestion. The concentrations of trace element in the samples were found to be 291.0-52.0, 1.64-0.04, 3.08-1.03, 0.71-0.05, 0.03-0.01, 1.30-0.50, 84.0-0.90, 50.1-1.30, 174.2-20.8 and 20.8-0.60 {mu}g/g for iron, manganese, zinc, copper, lead, cobalt, sodium, potassium, calcium, and magnesium, respectively. Cadmium was found to be 4.57-0.09 {mu}g/kg. The high heavy metal and minerals accumulation levels in the samples were found in olive oil for Cu, Pb, Co, margarine for Fe, K, corn oil for Zn, Mn, butter for Na, Mg, sunflower oil for Ca and hazelnut oil for Cd, respectively.

  15. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Daşbaşı, Teslima; Kartal, Şenol; Saçmacı, Şerife; Ülgen, Ahmet

    2016-01-01

    A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4 − complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1 with detection limit of 4.0 μg L−1 (n = 13). The precision as relative standard deviation was 3% (n = 11, 0.20 mg L−1) and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water). PMID:26881186

  16. Determination of Trace Silver in Water Samples by Online Column Preconcentration Flame Atomic Absorption Spectrometry Using Termite Digestion Product

    Science.gov (United States)

    Bianchin, Joyce Nunes; Martendal, Edmar; Carasek, Eduardo

    2011-01-01

    A new method for Ag determination in water samples using solid phase extraction (SPE) coupled to a flow injection system and flame atomic absorption spectrometry was developed. The sorbent used for Ag preconcentration and extraction was the termite digestion product. Flow and chemical variables of the system were optimized through a multivariate procedure. The factors selected were adsorbent mass, buffer type and concentration, sample pH, and sample flow rate. The detection limit and precision were 3.4 μg L−1 and 3.8% (n = 6, 15 μg L−1), respectively. The enrichment factor and the linear working range were, respectively, 21 and 10–50 μg L−1. Results for recovery tests using different water samples were between 96 and 107%. The proposed methodology was applied with success for the determination of Ag in water used to wash clothes impregnated with silver nanoparticles, supplied by a factory located in Santa Catarina, Brazil. PMID:21804766

  17. A new approach to mineralization of flaxseed (Linum usitatissimum L.) for trace element analysis by flame atomic absorption spectrometry.

    Science.gov (United States)

    Oliveira, João P S; Silva, Francisco L F; Monte, Raimundo J G; Matos, Wladiana O; Lopes, Gisele S

    2017-06-01

    A new approach to the analysis of Cu, Fe, Mn and Zn in flaxseed was developed based on infrared-assisted acid digestion. Quantitation by flame atomic absorption spectrometry yields results in agreement with those arising from aggressive total decomposition using conventional microwave-assisted (MW) digestions. A full factorial design in two levels was applied to evaluate the impact of significant variables for all elements to determine optimal experimental conditions. A desirability function revealed these to be: 2.0g sample mass, 8mL of HNO3 and 8min of heating time in the IR system. Precision better than 10% (RSD) was obtained, superior to that of a combined IR-MW approach. Sample preparation based on IR-assisted digestion provides a rapid and inexpensive alternative to other conventional techniques for the analysis of complex samples and is able to accommodate relatively large masses of sample, alleviating potential homogeneity issues as well as enhancing detection power. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. Slurry sampling hydride generation atomic absorption spectrometry for the determination of extractable/soluble As in sediment samples

    Science.gov (United States)

    Mierzwa, Jerzy; Dobrowolski, Ryszard

    1998-01-01

    A method combining the sampling of slurry pretreated by ultrasonic agitation and microwave assisted extraction with hydride generation atomic absorption spectrometry (HGAAS) for the determination of arsenic in sediment samples is proposed and evaluated. The pretreatment of slurried samples by ultrasonication enabled the extraction of (approximately) up to 85% of arsenic from the studied sediment samples. The further (slight) improvement of the efficiency of extraction was accomplished by the introduction of a short microwave-accelerated treatment. L-cysteine was used as an efficient pre-reduction reagent. The accuracy and precision of the slurry sampling HGAAS method were studied using the certified reference materials: Sediment GBW 30043 (NRCCRM, People's Republic of China), Sediment NIST 2704 (NIST, USA) and Marine Sediment BCSS-1 (NRCC, Canada). The relative standard deviation of the full (overall) analytical procedure was 8.5% and an absolute limit of detection of 2.75 ng was achieved. Factors which influence the reliability of this method are, for example, the choice of slurry liquid phase (extraction medium), sample homogeneity and, in particular, very effective mixing of slurries.

  19. Determination of cadmium by flame-atomic absorption spectrometry after preconcentration on silica gel modified with cupferron

    Directory of Open Access Journals (Sweden)

    Bortoleto Gisele G.

    2004-01-01

    Full Text Available A method for the determination of cadmium by flame atomic absorption spectrometry (FAAS after its preconcentration onto a column containing silica gel modified with cupferron was developed. The pH, amount of adsorbent material, concentration of eluent, volume of sample and amount of Cd were optimized. The effect of several foreign ions was also investigated and showed that the retention of cadmium depended on the amounts of Zn(II and Cu(II present and that these interferences could be overcome by using a 0.05 mmol KI. An enrichment factor of up to 30 was obtained , the LOD was 0.5 µg L-1 (3sigma and the LOQ was 2.0 µg L-1 (10sigma with rsd of 1.1% (n = 10. The accuracy of the proposed method was ascertained by using certified reference material and the obtained result (3.93 ± 0.01 µg g-1 agrees with the certified value (4.15 ± 0.38 µg g-1. The determination of Cd in nail polish showed quantitative recoveries for the spiked samples. The proposed method is characterized by simplicity, efficiency and low cost.

  20. Direct analysis of Antarctic krill by slurry sampling: determination of copper, iron, manganese and zinc by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Alves Flávia L.

    2000-01-01

    Full Text Available Slurry sampling in combination with flame atomic absorption spectrometry was employed for the direct determination of four essential trace elements, namely Cu, Fe, Mn and Zn in Antarctic krill. The effect of instrumental operating conditions and slurry sampling preparation on the analytical signal was investigated. For the determination of Cu, Fe and Zn, samples were suspended in a solution containing 2 mol L-1 HNO3. In the case of Mn, 4 mol L-1 HNO3 was necessary for the preparation of the slurry. The precision between sample replicates was better than 5%. The method was applied to the direct determination of Cu, Fe, Mn and Zn in Antarctic krill samples using aqueous reference solutions to prepare the calibration curves. The results obtained were in good agreement with those achieved by FAAS and ICP-AES after microwave-assisted wet digestion of the krill samples. The detection limits were 4.5, 1.0, 4.9 and 8.4 mug L-1 for Cu, Zn, Mn and Fe, respectively.

  1. Analysis of trace element in intervertebral disc by Atomic Absorption Spectrometry techniques in degenerative disc disease in the Polish population

    Directory of Open Access Journals (Sweden)

    Andrzej Nowakowski

    2015-05-01

    Full Text Available Objective. Although trace elements are regarded crucial and their content has been determined in number of tissue there are only few papers addressing this problem in intervertebral disc in humans. Most of the trace elements are important substrates of enzymes influencing metabolism and senescence process. Others are markers of environmental pollution. Therefore the aim of the research was to analyzed of the trace element content in the intervertebral disc, which may be a vital argument recognizing the background of degenerative changes to be the effect of the environment or metabolic factors. Materials and methods. Material consist of 18 intervertebral disc from 15 patients, acquired in surgical procedure of due to the degenerative disease with Atomic Absorption Spectrometry content of Al, Cd, Co, Pb, Cu, Ni, Mo, Mg, Zn was evaluated. Results. Only 4 of the trace elements were detected in all samples. The correlation analysis showed significant positive age correlation with Al and negative in case of Co. Among elements significant positive correlation was observed between Al/Pb, Co/Mo, Al/Mg, Al/Zn Pb/Zn and Mg/Zn. Negative correlation was observed in Al/Co, Cd/Mg, Co/Mg, Mo/Mg, Co/Zn and Mo/Zn. Conclusions. This study is the first to our knowledge that profiles the elements in intervertebral disc in patients with degenerative changes. We have confirmed significant differences between the trace element contents in intervertebral disc and other tissue. It can be ground for further investigation.

  2. Discussion of parameters associated with the determination of arsenic by electrothermal atomic absorption spectrometry in slurried environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Vassileva, E.; Baeten, H.; Hoenig, M. [Centre for Veterinary and Agrochemical Research (CERVA), Tervuren (Belgium)

    2001-01-01

    A slurry sampling - fast program procedure has been developed for the determination of arsenic in plants, soils and sediments by electrothermal atomic absorption spectrometry. Efficiencies of various single and mixed modifiers for thermal stabilization of arsenic and for a better removal of the matrix during pyrolysis step were compared. The influence of the slurry concentration, amounts of modifier and parameters of the pyrolysis step on the As integrated absorbance signals have been studied and a comparison between fast and conventional furnace programs was also made. The ultrasonic agitation of the slurry followed by a fast electrothermal program using an Ir/Mg modifier provides the most consistent performance in terms of precision and accuracy. The reliability of the whole procedure has been compared with results obtained after application of a wet digestion method with an HF step and validated by analyzing eleven certified reference materials. Arsenic detection and quantitation limits expressed on dry sample matter were about 30 and 100 {mu}g kg{sup -1}, respectively. (orig.)

  3. Determination of inorganic arsenic and its organic metabolites in urine by flow-injection hydride generation atomic absorption spectrometry.

    Science.gov (United States)

    Hanna, C P; Tyson, J F; McIntosh, S

    1993-08-01

    A method has been developed for the determination of inorganic arsenic [As(III) and As(V)] and its organic metabolites (monomethylarsenic and dimethylarsenic) in urine by flow-injection hydride generation atomic absorption spectrometry. The nontoxic seafood-derived arsenobetaine and arsenocholine species were first separated by a solid-phase extraction procedure. The remaining sample was digested with a mixture of nitric and sulfuric acids and potassium dichromate, followed by attack with hydrogen peroxide. The resulting As(V) was reduced to As(III) with potassium iodide in hydrochloric acid before injection into the flow-injection manifold. The percentage analytical recoveries (mean +/- 95% confidence interval) of various arsenic species added to a urine specimen at 250 micrograms/L were 108 +/- 2, 112 +/- 11, 104 +/- 7, and 95 +/- 5 for As(III), As(V), monomethylarsenic, and dimethylarsenic, respectively. For the determination of arsenic in Standard Reference Material 2670 (toxic metals in human urine), results agreed with the certified value (480 +/- 100 micrograms/L). Analyses of samples for the Centre de Toxicologie du Quebec, containing seafood-derived species, demonstrated the viability of the separation procedure. Detection limits were between 0.1 and 0.2 microgram/L in the solution injected into the manifold, and precision at 10 micrograms/L was between 2% and 3% (CV). These preliminary results show that the method might be applicable to determinations of arsenic in a range of clinical urine specimens.

  4. Selective speciation of inorganic antimony on tetraethylenepentamine bonded silica gel column and its determination by graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Mendil, Durali; Bardak, Hilmi; Tuzen, Mustafa; Soylak, Mustafa

    2013-03-30

    A speciation system for antimony (III) and antimony (V) ions that based on solid phase extraction on tetraethylenepentamine bonded silica gel has been established. Antimony was determined by graphite furnace atomic absorption spectrometry (GF-AAS). Analytical conditions including pH, sample volume, etc., were studied for the quantitative recoveries of Sb (III) and Sb (V). Matrix effects on the recovery were also investigated. The recovery values and detection limit for antimony (III) at optimal conditions were found as >95% and 0.020 μg L(-1), respectively. Preconcentration factor was calculated as 50. The capacity of adsorption for the tetraethylenepentamine bonded silica gel was 7.9 mg g(-1). The validation was checked by analysis of NIST SRM 1573a Tomato laves and GBW 07605 Tea certified reference materials. The procedure was successfully applied to speciation of antimony in tap water, mineral water and spring water samples. Total antimony was determined in refined salt, unrefined salt, black tea, rice, tuna fish and soil samples after microwave digestion and presented enrichment method combination. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Determination of arsenic in petroleum refinery streams by electrothermal atomic absorption spectrometry after multivariate optimization based on Doehlert design

    Science.gov (United States)

    Cassella, Ricardo J.; de Sant'Ana, Otoniel D.; Santelli, Ricardo E.

    2002-12-01

    This paper reports the development of a methodology for the determination of arsenic in petroleum refinery aqueous streams containing large amounts of unknown volatile organic compounds, employing electrothermal atomic absorption spectrometry with polarized Zeeman-effect background correction. In order to make the procedure applicable, the influence of chemical modification and the drying step was examined. Also, pyrolysis and atomization temperatures and the amount of nitric acid added to the sample were optimized using a multivariate approach based on Doehlert matrix. Obtained results indicate that, in this kind of sample, arsenic must be determined by standard addition procedure with a careful control of the drying step temperature and ramp pattern. In order to evaluate the accuracy of the procedure, a test was performed in six spiked samples of petroleum refinery aqueous streams and the relative errors verified in the analysis of such samples (added As between 12.5 and 190 μg l -1) ranged from -7.2 to +16.7%. The detection limit and the relative standard deviation were also calculated and the values are 68 pg and 7.5% (at 12.5 μg l -1 level), respectively.

  6. Graphene for separation and preconcentration of trace amounts of cobalt in water samples prior to flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Yukun Wang

    2016-09-01

    Full Text Available A new sensitive and simple method was developed for the preconcentration of trace amounts of cobalt (Co using 1-(2-pyridylazo-2-naphthol (PAN as chelating reagent prior to its determination by flame atomic absorption spectrometry. The proposed method is based on the utilization of a column packed with graphene as sorbent. Several effective parameters on the extraction and complex formation were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 5.0–240.0 μg L−1 with a detection limit of 0.36 μg L−1. The relative standard deviation for ten replicate measurements of 20.0 and 100.0 μg L−1 of Co were 3.45 and 3.18%, respectively. Comparative studies showed that graphene is superior to other adsorbents including C18 silica, graphitic carbon, and single- and multi-walled carbon nanotubes for the extraction of Co. The proposed method was successfully applied in the analysis of four real environmental water samples. Good spiked recoveries over the range of 95.8–102.6% were obtained.

  7. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Vilar Farinas, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Barciela Garcia, J. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Garcia Martin, S. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena Crecente, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Herrero Latorre, C. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)]. E-mail: cherrero@lugo.usc.es

    2007-05-22

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO{sub 3}){sub 2} and (NH{sub 4})H{sub 2}PO{sub 4}-Mg(NO{sub 3}){sub 2}] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 {mu}g L{sup -1}), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged

  8. Speciation of arsenic in baby foods and the raw fish ingredients using liquid chromatography-hydride generation-atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Vinas, P.; Lopez-Garcia, I.; Merino-Merono, B.; Campillo, N.; Hernandez-Cordoba, M. [Murcia Univ. (Spain). Dept. of Analytical Chemistry

    2003-07-01

    The speciation of arsenic in different baby foods and the raw fish ingredients using the direct hybridisation of liquid chromatography (LC) and hydride generation atomic absorption spectrometry (HGAAS) is described. Good resolution of the species, arsenic(III), dimethylarsinic acid (DMAA), monomethylarsenic acid (MMAA) and arsenic(V) is achieved using an anion-exchange column with potassium phosphate as the mobile phase and gradient elution. Arsenobetaine (AsB) is determined by on-line oxidation using peroxydisulphate and hydride generation. The arsenicals were extracted by an enzymatic digestion procedure based on the action of trypsin or pancreatin. Arsenobetaine was the only arsenic species detected. The reliability of the procedure was checked by analyzing the total arsenic content of the samples by electrothermal atomic absorption spectrometry with microwave-oven digestion and by analyzing a certified reference material. The arsenic content in the baby foods comes from the raw fish ingredients and is highest when plaice is used. (orig.)

  9. Comparison of different sample preparation methods for platinum determination in cultured cells by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Man Xiao

    2017-01-01

    Full Text Available Background Platinum-based agents are widely used in chemotherapy against solid tumors and insufficient intracellular drug accumulation is one of the leading causes of platinum resistance which is associated with poor survival of tumor patients. Thus, the detection of intracellular platinum is pivotal for studies aiming to overcome platinum resistance. In the present study, we aimed to establish a reliable graphite furnace atomic absorption spectrometry (GFAAS-based assay to quantify the intracellular platinum content for cultured cells. Methods Several most commonly applied cell preparation methods, including 0.2% HNO3, 0.2% Triton X-100, concentrated nitric acid, RIPA combined with concentrated nitric acid and hydroxide, followed by GFAAS for platinum detection were compared in ovarian, cervical and liver cancer cell lines to obtain the optimal one, and parameters regarding linearity, accuracy, precision and sensitivity were evaluated. Influence of other metals on platinum detection and the storage conditions of samples were also determined. Results The treatment of cells with 0.2% HNO3 was superior to other approaches with fewer platinum loss and better repeatability. The recovery rate and precision of this method were 97.3%–103.0% and 1.4%–3.8%, respectively. The average recoveries in the presence of other metals were 95.1%–103.1%. The detection limit was 13.23 ug/L. The recovery rate of platinum remained acceptable even in cell samples stored in −20 °C or −80 °C for two months. Discussion After comparison, we found that 0.2% HNO3 was optimal for intracellular platinum quantification based on GFAAS, which presented values compatible with that of inductively-coupled plasma mass-spectrometry (ICP-MS, and this is partially attributed to the simplicity of this method. Moreover, the assay was proved to be accurate, sensitive, cost-effective and suitable for the research of platinum-based antitumor therapy.

  10. Use of factorial design and Doehlert matrix for multivariate optimisation of an on-line preconcentration system for lead determination by flame atomic absorption spectrometry

    OpenAIRE

    Ferreira, Sergio Luis Costa; Santos, W. N. L. dos; Bezerra, Marcos de Almeida; Lemos, Valfredo Azevedo; Bosque-Sendra, Juan M.

    2003-01-01

    Texto Completo: acesso restrito. p. 443–449. A system for on-line preconcentration and determination of lead by flame atomic absorption spectrometry (FAAS) was proposed. It was based on the sorption of lead(II) ions on a minicolumn of polyurethane foam loaded with 2-(2-thiazolylazo)-5 dimethylaminophenol (TAM). The optimisation step was carried out using twolevel full factorial and Doehlert designs for the determination of the optimum conditions for lead preconcentration. The proposed p...

  11. Determination of trace amounts of copper in river and sea water samples by flame atomic absorption spectrometry (FAAS) after cloud-point preconcentration

    OpenAIRE

    Goudarzi,Nasser

    2007-01-01

    A new preconcentration method was proposed using the cloud point approach for copper determination. The reagent 1,5-diphenyl-benzoin (Cupron) was used as a complexing agent and Triton X-114 was added as a surfactant. After phase separation, dilution of the surfactant-rich phase was carried out using acidified methanol and the copper content was subsequently measured by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions, the enrichment factor...

  12. Application of factorial design and Doehlert matrix in the optimisation of instrumental parameters for direct determination of silicon in naphtha using graphite furnace atomic absorption spectrometry

    OpenAIRE

    Amaro, Joana Angélica de Azerêdo; Ferreira, Sergio Luis Costa

    2004-01-01

    p. 246 – 249 A method for direct determination of silicon in naphtha samples using graphite furnace atomic absorption spectrometry (GFAAS) is proposed. The optimisation of the instrumental conditions was multivariate using a fractional factorial design and Doehlert matrix. Firstly, the fractional factorial design was performed for preliminary evaluation of the significance of the factors, the factors chosen being: sample volume, atomisation temperature, pyrolysis time and pyrolysis temp...

  13. Quality assessment of trace Cd and Pb contaminants in Thai herbal medicines using ultrasound-assisted digestion prior to flame atomic absorption spectrometry

    OpenAIRE

    Siriangkhawut, Watsaka; Sittichan, Patcharee; Ponhong, Kraingkrai; Chantiratikul, Piyanete

    2017-01-01

    A simple, efficient, and reliable ultrasound-assisted digestion (UAD) procedure was used for sample preparation prior to quantitative determination of trace Cd and Pb contaminants in herbal medicines using flame atomic absorption spectrometry. The parameters influencing UAD such as the solvent system, sample mass, presonication time, sonication time, and digestion temperature were evaluated. The efficiency of the proposed UAD procedure was evaluated by comparing with conventional acid digesti...

  14. Determination of toxic elements in plastics from waste electrical and electronic equipment by slurry sampling electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Santos, Mirian C; Nóbrega, Joaquim A; Baccan, Nivaldo; Cadore, Solange

    2010-06-15

    Cadmium, chromium, lead and antimony were determined in slurries prepared using pulverized samples of personal computers and mobile phones dispersed in dimethylformamide medium. Determinations were carried out by electrothermal atomic absorption spectrometry (ETAAS) using a graphite furnace atomic absorption spectrometer. The optimization of the experimental conditions (chemical modifier, pyrolysis time, pyrolysis temperature and atomization temperatures) was accomplished by evaluating pyrolysis and atomization curves. Optimization was also used to determine the temperatures corresponding to the best sensitivities and the lowest background signals. The pyrolysis temperatures were fixed at 600 degrees C (for Cd), 700 degrees C (for Pb), 1100 degrees C (for Sb), and 1200 degrees C (for Cr); atomization temperatures were established as 1400 degrees C (for Cd), 1300 degrees C (for Pb), 1900 degrees C (for Sb), and 2300 degrees C (for Cr), and the chemical modifier (50microg NH(4)H(2)PO(4)+3microg Mg(NO(3))(2) was used for Cd and Pb while 5microg Pd+3microg Mg(NO(3))(2) was used for Sb). The use of a chemical modifier for Cr determination was not necessary. The characteristic masses were 1.9pg for Cd, 32.3pg for Pb, 54.1pg for Sb, and 9.1pg for Cr. Calibration was performed using standard additions in a range of 5-20microgL(-1) for Cd, 5-30microgL(-1) for Cr, 12.5-50microgL(-1) for Pb, and 25-100microgL(-1) for Sb with linear correlation coefficients higher than 0.99. Limits of detection were 0.9, 1.4, 6.8, and 2.9microgL(-1) for Cd, Pb, Sb, and Cr, respectively. The results indicate that recoveries for all metals agreed at a 95% confidence level when a paired t-test was applied and presented good precision. The accuracy of the proposed method was evaluated by addition-recovery experiments, showing results in the 96-112% range, and also by comparison of the results using Student's t-test with another method developed using ETAAS for digested samples. Analyte

  15. Determination of platinum traces contamination by graphite furnace atomic absorption spectrometry after preconcentration by cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Chappuy, M. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Caudron, E., E-mail: eric.caudron@eps.aphp.fr [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Groupe de Chimie Analytique de Paris-Sud, EA 4041, IFR 141, School of Pharmacy, Univ Paris-Sud, 92296 Chatenay-Malabry (France); Bellanger, A. [Department of Pharmacy, Pitie-Salpetriere Hospital (Paris Public Hospital Authority), 47 boulevard de l' hopital, 75013 Paris (France); Pradeau, D. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France)

    2010-04-15

    A simple and sensitive method is described for the determination of platinum surface contamination originating from cisplatin, carboplatin and oxaliplatin. Following extraction from swabs and preconcentration with the cloud point extraction (CPE) method, detection was by graphite furnace atomic absorption spectrometry (GFAAS). After desorption of platinum compounds from the swab, CPE involved on preconcentration of platinum in aqueous solution with diethyldithiocarbamate (DDTC) as chelating agent and Triton X-114 as extraction medium. DDTC is not only a chelating agent, but may also be a good candidate for the inactivation of platinum compounds. DDTC is recommended by the Word Health Organization (WHO) for the destruction of platinum-based anticancer drugs. The main factors affecting CPE efficiency, pH of the sample solution, concentrations of DDTC and Triton X-114, equilibration temperature and incubation time, were evaluated in order to enhance sensitivity of the method. The desorption of platinum compounds from the swab was investigated in parallel. Since platinum is bound to DDTC, it must exchange with copper in order to enhance platinum atomizing by GFAAS. A preconcentration factor of 29 was obtained for 10 mL of a platinum solution at 10 {mu}g mL{sup -1}. In optimal conditions, the limit of detection was 0.2 ng mL{sup -1}, corresponding to 2.0 ng of platinum metal on the swab. Absorbance was linear between 0.7 and 15 ng mL{sup -1}. The proposed method was applied for the determination of surface contamination by platinum compounds with correct results.

  16. [Determination of trace gold by flame atomic absorption spectrometry after separation and preconcentration with load nanometer titanium dioxide].

    Science.gov (United States)

    Liu, Zheng-Hua; Zhou, Fang-Qin; Jiang, Fang-Ming; Huang, Rong-Hui; Yang, Liu; Zhou, Le-Zhou

    2008-02-01

    A new method for the determination of trace gold by flame atomic absorption spectrometry (FAAS) after preconcentration with p-dimethylaminobenzylidenerhodanine (DMABR) loaded with nanometer TiO2 was developed. The method is convenient, highly precise and linear in a wide range. Under dynamic condition, the optimum pH of solution, flow rate, elution conditions were obtained for preconcentration of trace gold. And the effect of interfering ions was also investigated. It was found that the studied gold could be quantitatively preconcentrated on loaded nanometer TiO2 at pH = 3.5, and the flow rate of sample solution was 0.6 mL x min(-1), and the flow rate of eluting solution with 0.1 mol x L(-1) HCl-0.5 mol x L(-1) thiourea was 0.5 mL x min(-1), sufficient for complete elution. The dynamic adsorption capacity of gold on load nanometer TiO2 was 23.19 mg x g(-1). The linear range for gold was 0-0.40 microg x mL(-1), correlation coefficient was 0. 999 3, detection limit (3sigma, n = 11) for gold was 2.34 ng x mL(-1), and the relative standard deviation was 2.9% (n = 6, c = 0.10 microg x mL(-1)), the recovery was in the range of 96.7%-101.7%. The method has been applied to the determination of trace gold in water samples with satisfactory results.

  17. Feasibility of using direct determination of cadmium and lead in fresh meat by electrothermal atomic absorption spectrometry for screening purposes

    Energy Technology Data Exchange (ETDEWEB)

    Damin, Isabel C.F. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre - RS (Brazil); Silva, Marcia M. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre - RS (Brazil)], E-mail: mmsilva@iq.ufrgs.br; Vale, Maria Goreti R. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre - RS (Brazil); Welz, Bernhard [Instituto de Quimica, Universidade Federal da Bahia, 40170-290 Salvador - BA (Brazil)

    2007-09-15

    A method for the direct determination of cadmium and lead in fresh meat for screening purposes is proposed using electrothermal atomic absorption spectrometry. The fresh meat samples were homogenized, weighed directly onto solid sampling platforms and introduced into a transversely heated solid sampling graphite tube. The main challenges associated with this procedure, such as weighing errors and optimization of the temperature program were investigated in detail. Calibration was performed against aqueous standards and two modifiers were investigated: 0.05% Pd + 0.03% Mg + 0.05% Triton X-100 and 0.01% Pd + 10% NH{sub 4}NO{sub 3} + 0.05% Triton X-100. The former one is recommended due to the higher pyrolysis temperature obtained for cadmium and the better limits of detection of 1.9 {mu}g kg{sup -} {sup 1} for lead and 0.13 {mu}g kg{sup -} {sup 1} for cadmium, based on 10 mg of sample mass. The results obtained for cadmium and lead in two certified reference materials were statistically not different from the certified values on a 95% confidence level, indicating that calibration against aqueous standards is suitable for this application. In order to evaluate weighing errors the fresh samples were dried (at 60 deg. C) to constant weight; the results obtained with fresh and dried samples were in agreement, taking the loss of weight into consideration for the latter ones. The average relative standard deviation of 14% is in concordance with the results of others using fresh meat. Comparison with the digestion method adopted by the Brazilian Ministry of Agriculture shows no significant differences between the results at the 95% confidence level. This study shows that direct analysis of fresh meet can be applied as a rapid routine screening procedure for residue control in products of animal origin, helping the implementation and maintenance of sanitary control.

  18. X-ray photoelectron spectroscopy study of pyrolytically coated graphite platforms submitted to simulated electrothermal atomic absorption spectrometry conditions

    Energy Technology Data Exchange (ETDEWEB)

    Ruiz, Frine [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Benzo, Zully [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Quintal, Manuelita [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Garaboto, Angel [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Albornoz, Alberto [Laboratorio de Fisicoquimica de Superficies, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Brito, Joaquin L. [Laboratorio de Fisicoquimica de Superficies, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela)]. E-mail: joabrito@ivic.ve

    2006-10-15

    The present work is part of an ongoing project aiming to a better understanding of the mechanisms of atomization on graphite furnace platforms used for electrothermal atomic absorption spectrometry (ETAAS). It reports the study of unused pyrolytic graphite coated platforms of commercial origin, as well as platforms thermally or thermo-chemically treated under simulated ETAAS analysis conditions. X-ray photoelectron spectroscopy (XPS) was employed to study the elements present at the surfaces of the platforms. New, unused platforms showed the presence of molybdenum, of unknown origin, in concentrations up to 1 at.%. Species in two different oxidations states (Mo{sup 6+} and Mo{sup 2+}) were detected by analyzing the Mo 3d spectral region with high resolution XPS. The analysis of the C 1s region demonstrated the presence of several signals, one of these at 283.3 eV related to the presence of Mo carbide. The O 1s region showed also various peaks, including a signal that can be attributed to the presence of MoO{sub 3}. Some carbon and oxygen signals were consistent with the presence of C=O and C-O- (probably C-OH) groups on the platforms surfaces. Upon thermal treatment up to 2900 deg. C, the intensity of the Mo signal decreased, but peaks due to Mo oxides (Mo{sup 6+} and Mo{sup 5+}) and carbide (Mo{sup 2+}) were still apparent. Thermo-chemical treatment with 3 vol.% HCl solutions and heating up to 2900 deg. C resulted in further diminution of the Mo signal, with complete disappearance of Mo carbide species. Depth profiling of unused platforms by Ar{sup +} ion etching at increasing time periods demonstrated that, upon removal of several layers of carbonaceous material, the Mo signal disappears suggesting that this contamination is present only at the surface of the pyrolytic graphite platform.

  19. Determination of silicon and aluminum in silicon carbide nanocrystals by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Dravecz, Gabriella; Bencs, László; Beke, Dávid; Gali, Adam

    2016-01-15

    The determination of Al contaminant and the main component Si in silicon carbide (SiC) nanocrystals with the size-distribution of 1-8nm dispersed in an aqueous solution was developed using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS). The vaporization/atomization processes were investigated in a transversally heated graphite atomizer by evaporating solution samples of Al and Si preserved in various media (HCl, HNO3). For Si, the best results were obtained by applying a mixture of 5µg Pd plus 5µg Mg, whereas for Al, 10µg Mg (each as nitrate solution) was dispensed with the samples, but the results obtained without modifier were found to be better. This way a maximum pyrolysis temperature of 1200°C for Si and 1300°C for Al could be used, and the optimum (compromise) atomization temperature was 2400°C for both analytes. The Si and Al contents of different sized SiC nanocrystals, dispersed in aqueous solutions, were determined against aqueous (external) calibration standards. The correlation coefficients (R values) of the calibrations were found to be 0.9963 for Si and 0.9991 for Al. The upper limit of the linear calibration range was 2mg/l Si and 0.25mg/l Al. The limit of detection was 3µg/l for Si and 0.5µg/l for Al. The characteristic mass (m0) was calculated to be 389pg Si and 6.4pg Al. The Si and Al content in the solution samples were found to be in the range of 1.0-1.7mg/l and 0.1-0.25mg/l, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Speciation of platinum in blood plasma and urine by micelle-mediated extraction and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Mortada, Wael I; Hassanien, Mohammed M; El-Asmy, Ahmed A

    2013-10-01

    A highly sensitive and selective technique for the speciation of platinum by cloud point extraction prior to determination by graphite furnace atomic absorption spectrometry (GFAAS) was described. The separation of Pt(II) from Pt(IV) was performed in the presence of 4-(p-chlorophenyl)-1-(pyridin-2-yl)thiosemicarbazide (HCPTS) as chelating agent and Triton X-114 as a non-ionic surfactant. The extraction of Pt(II)-HCPTS complex needs temperature higher than the cloud point temperature of Triton X-114 and pH = 7, while Pt(IV) remains in the aqueous phase. The Pt(II) in the surfactant phase was analyzed by GFAAS, and the concentration of Pt(IV) was calculated by subtraction of Pt(II) from total platinum which was directly determined by GFAAS. The effect of pH, concentration of chelating agent, surfactant, and equilibration temperature were investigated. An enrichment factor of 42 was obtained for the preconcentration of Pt(II) with 50 mL solution. Under the optimum experimental conditions, the calibration curve was linear up to 30 μgL(-1) with detection limit of 0.08 μgL(-1) and the relative standard deviation was 1.8%. No considerable interference was observed due to the presence of coexisting anions and cations. The accuracy of the results was verified by analyzing different spiked samples (tap water, blood plasma and urine). The proposed method was applied to the speciation analysis of Pt in blood plasma and urine with satisfactory results. Copyright © 2013 Elsevier GmbH. All rights reserved.

  1. Rhodium as permanent modifier for atomization of lead from biological fluids using tungsten filament electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Zhou, Ying; Parsons, Patrick J.; Aldous, Kenneth M.; Brockman, Paul; Slavin, Walter

    2002-04-01

    Rhodium (Rh) was investigated as a permanent modifier for the atomization of Pb from biological fluids in W-filament atomic absorption spectrometry (AAS). Heating the W-filament with a Rh solution provided a protective coating for subsequent determinations of Pb in blood and urine matrices. The W-filament AAS instrumentation used was based on a prototype design that utilized self-reversal background correction scheme and peak area measurements. We found that Rh not only stabilized Pb during the pyrolysis step, but also facilitated the removal of carbonaceous residues during the cleaning step, requiring much less power than with phosphate modifier. Thus, the filament lifetime was greatly extended to over 300 firings. Periodic reconditioning with Rh was necessary every 30 firings or so. Conditioning the filament with Rh also permitted direct calibration using simple aqueous Pb standards. The method detection limit for blood Pb was approximately 1.5 μg dl -1, similar to that reported previously. Potential interferences from concomitants such as Na, K, Ca and Mg were evaluated. Accuracy was verified using lead reference materials from the National Institute of Standards and Technology and the New York State Department of Health. Blood lead results below 40 μg dl -1 were within ±1 μg dl -1 of certified values, and within ±10% above 40 μg dl -1; within-run precision was ±10% or better. Additional validation was reported using proficiency test materials and human blood specimens. All blood lead results were within the acceptable limits established by regulatory authorities in the US. When measuring Pb in urine, sensitivity was reduced and matrix-matched calibration became necessary. The method of detection limit was 27 μg l -1 for urine Pb. Urine lead results were also validated using an acceptable range comparable to that established for blood lead by US regulatory agencies.

  2. Determination of inorganic and total mercury by vapor generation atomic absorption spectrometry using different temperatures of the measurement cell

    Energy Technology Data Exchange (ETDEWEB)

    Kaercher, Luiz Eduardo [Universidade Federal de Santa Maria, Departamento de Quimica, Campus de Camobi, 97105900 Santa Maria, RS (Brazil); Goldschmidt, Fabiane [Universidade Federal de Santa Maria, Departamento de Quimica, Campus de Camobi, 97105900 Santa Maria, RS (Brazil); Paniz, Jose Neri Gottfried [Universidade Federal de Santa Maria, Departamento de Quimica, Campus de Camobi, 97105900 Santa Maria, RS (Brazil); Moraes Flores, Erico Marlon de [Universidade Federal de Santa Maria, Departamento de Quimica, Campus de Camobi, 97105900 Santa Maria, RS (Brazil); Dressler, Valderi Luiz [Universidade Federal de Santa Maria, Departamento de Quimica, Campus de Camobi, 97105900 Santa Maria, RS (Brazil)]. E-mail: valdres@quimica.ufsm.br

    2005-06-30

    A simple and inexpensive laboratory-built flow injection vapor generation system coupled to atomic absorption spectrometry (FI-VG AAS) for inorganic and total mercury determination has been developed. It is based on the vapor generation of total mercury and a selective detection of Hg{sup 2+} or total mercury by varying the temperature of the measurement cell. Only the inorganic mercury is measured when the quartz cell is at room temperature, and when the cell is heated to 650 deg. C or higher the total Hg concentration is measured. The organic Hg concentration in the sample is calculated from the difference between the total Hg and Hg{sup 2+} concentrations. Parameters such as the type of acid (HCl or HNO{sub 3}) and its concentration, reductant (NaBH{sub 4}) concentration, carrier solution (HCl) flow rate, carrier gas flow rate, sample volume and quartz cell temperature, which influence FI-VG AAS system performance, were systematically investigated. The optimized conditions for Hg{sup 2+} and total Hg determinations were: 1.0 mol l{sup -1} HCl as carrier solution, carrier flow rate of 3.5 ml min{sup -1}, 0.1% (m/v) NaBH{sub 4}, reductant flow rate of 1.0 ml min{sup -1} and carrier gas flow rate of 200 ml min{sup -1}. The relative standard deviation (RSD) is lower than 5.0% for a 1.0 {mu}g l{sup -1} Hg solution and the limit of quantification (LOQ, 10 s) is 55 ng g{sup -1}. Certified samples of dogfish muscle (DORM-1 and DORM-2) and non-certified fish samples were analyzed, using a 6.0 mol l{sup -1} HCl solution for analyte extraction. The Hg{sup 2+} and CH{sub 3}Hg{sup +} concentrations found were in agreement with certified ones.

  3. Coacervative extraction of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hagarová, Ingrid, E-mail: hagarova@fns.uniba.sk; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb–dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l{sup −1} HNO{sub 3}. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l{sup −1}, quantification limit of 0.38 μg l{sup −1}, relative standard deviation of 4.2% (for 2 μg l{sup −1} of Pb; n = 26), linearity of the calibration graph in the range of 0.5–4.0 μg l{sup −1} (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91–96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters. - Highlights: • The potential of coacervates for the extraction of metal ions is examined. • No difficulties in coupling of ETAAS with the proposed CAE are observed. • Achieved preconcentration factor results in enhanced sensitivity. • Analytical performance is confirmed by the reliable determination of trace Pb. • The proposed CAE is ecofriendly and efficient.

  4. Comparison of two methods for blood lead analysis in cattle: graphite-furnace atomic absorption spectrometry and LeadCare(R) II system.

    Science.gov (United States)

    Bischoff, Karyn; Gaskill, Cynthia; Erb, Hollis N; Ebel, Joseph G; Hillebrandt, Joseph

    2010-09-01

    The current study compared the LeadCare(R) II test kit system with graphite-furnace atomic absorption spectrometry for blood lead (Pb) analysis in 56 cattle accidentally exposed to Pb in the field. Blood Pb concentrations were determined by LeadCare II within 4 hr of collection and after 72 hr of refrigeration. Blood Pb concentrations were determined by atomic absorption spectrometry, and samples that were coagulated (n = 12) were homogenized before analysis. There was strong rank correlation (R(2) = 0.96) between atomic absorption and LeadCare II (within 4 hr of collection), and a conversion formula was determined for values within the observed range (3-91 mcg/dl, although few had values >40 mcg/dl). Median and mean blood pb concentrations for atomic absorption were 7.7 and 15.9 mcg/dl, respectively; for LeadCare II, medians were 5.2 mcg/dl at 4 hr and 4.9 mcg/dl at 72 hr, and means were 12.4 and 11.7, respectively. LeadCare II results at 4 hr strongly correlated with 72 hr results (R(2) = 0.96), but results at 72 hr were lower (P atomic absorption. Although there have been several articles that compared LeadCare with other analytical techniques, all were for the original system, not LeadCare II. The present study indicated that LeadCare II results correlated well with atomic absorption over a wide range of blood Pb concentrations and that refrigerating samples for up to 72 hr before LeadCare II analysis was acceptable for clinical purposes.

  5. Determination of serum aluminum by electrothermal atomic absorption spectrometry: A comparison between Zeeman and continuum background correction systems

    Science.gov (United States)

    Kruger, Pamela C.; Parsons, Patrick J.

    2007-03-01

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass ( m0), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 ± 0.6 pg, compared to 16.1 ± 0.7 pg for the Z5100, and 23.3 ± 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection limits (3

  6. Mercury speciation in sea food by flow injection cold vapor atomic absorption spectrometry using selective solid phase extraction.

    Science.gov (United States)

    Vereda Alonso, E; Siles Cordero, M T; García de Torres, A; Cañada Rudner, P; Cano Pavón, J M

    2008-10-19

    An on-line inorganic and organomercury species separation, preconcentration and determination system consisting of cold vapor atomic absorption spectrometry (CV-AAS or CV-ETAAS) coupled to a flow injection (FI) method was studied. The inorganic mercury species was retained on a column (i.d., 3 mm; length 3 cm) packed to a height of 0.7 cm with a chelating resin aminopropyl-controlled pore glass (550 A) functionalized with [1,5-bis (2 pyridyl)-3-sulphophenyl methylene thiocarbonohydrazyde] placed in the injection valve of a simple flow manifold. Methylmercury is not directly determined. Previous oxidation of the organomercurial species permitted the determination of total mercury. The separation of mercury species was obtained by the selective retention of inorganic mercury on the chelating resin. The difference between total and inorganic mercury determined the organomercury content in the sample. The inorganic mercury was removed on-line from the microcolumn with 6% (m/v) thiourea. The mercury cold vapor generation was performed on-line with 0.2% (m/v) sodium tethrahydroborate and 0.05% (m/v) sodium hydroxide as reducing solution. The determination was performed using CV-AAS and CV-ETAAS, both approaches have been used and compared for the speciation of mercury in sea food. A detection limit of 10 and 6 ng l(-1) was achieved for CV-AAS and CV-ETAAS, respectively. The precision for 10 replicate determinations at the 1 microg l(-1) Hg level was 3.5% relative standard deviation (R.S.D.), calculated from the peak heights obtained. Both approaches were validated with the use of two certified reference materials and by spiking experiments. By analyzing the two biological certified materials, it was evident that the difference between the total mercury and inorganic mercury corresponds to methylmercury. The concentrations obtained by both techniques were in agreement with the certified values or with differences of the certified values for total Hg(2+) and CH(3)Hg

  7. Lead and cadmium in human teeth from Jordan by atomic absorption spectrometry: Some factors influencing their concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Alomary, A. [Department of Chemistry, Yarmouk University, Irbid (Jordan)]. E-mail: ahmedalomary1000@hotmail.com; Al-Momani, I.F. [Department of Chemistry, Yarmouk University, Irbid (Jordan); Massadeh, A.M. [Department of Medicinal Chemistry and Pharmacognosy, Faculty of Pharmacy, Jordan University of Science and Technology, Irbid (Jordan)

    2006-10-01

    The aim of this study was to measure the concentrations of lead (Pb) and cadmium (Cd) in human teeth and to investigate the affecting factors. Teeth samples (n = 268) were collected from people living in different cities in Jordan including Amman, Zarqa, Al-Mafraq and Irbid and analyzed for Pb and Cd using atomic absorption spectrometry (AAS). A questionnaire was used to gather information on each person, such as age, sex, place where the patient lives, smoking, presence of amalgam fillings inside the mouth, and whether the patient uses toothpaste or not. The mean concentrations of Pb and Cd were 28.91 {mu}g/g and 0.44 {mu}g/g, respectively. The results indicate that there is a clear relation between Pb and Cd concentrations and the presence of amalgam fillings, smoking, and place of living. Pb was sex-dependent, whereas Cd was not. Our results show that Pb and Cd concentrations in samples obtained from Al-Mafraq and Irbid are higher than those obtained from Amman and Zarqa. Pb was highest in Mafraq, whereas Cd was highest in Irbid. The Pb and Cd concentrations in teeth from smokers (means: Pb = 31.89 {mu}g/g, Cd = 0.49 {mu}g/g) were significantly higher than those from nonsmokers (means: Pb = 24.07 {mu}g/g, Cd = 0.37 {mu}g/g). Pb and Cd concentrations in teeth of patients with amalgam fillings (means: Pb = 31.02 {mu}g/g and Cd = 0.52 {mu}g/g) were significantly higher than those from patients without amalgam fillings (means: Pb = 26.87 {mu}g/g and Cd = 0.41 {mu}g/g). Our results show that brushing the teeth daily with toothpaste does not significantly decrease the concentration of both Pb and Cd. The mean concentrations of Pb and Cd do not vary significantly between the ages 20-30, 31-40, and 41-50, but both increased rapidly at age 51-60.

  8. Determination of palladium in various samples by atomic absorption spectrometry after preconcentration with dimethylglyoxime on silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Tokalioglu, Serife; Oymak, Tuelay; Kartal, Senol

    2004-05-31

    A preconcentration method based on the adsorption of palladium-dimethylglyoxime (DMG) complex on silica gel for the determination of palladium at trace levels by atomic absorption spectrometry (AAS) has been developed. The retained palladium as Pd(DMG){sub 2} complex was eluted with 1 mol l{sup -1} HCl in acetone. The effect of some analytical parameters such as pH, amount of reagent and the sample volume on the recovery of palladium was examined in synthetic solutions containing street dust matrix. The influence of some matrix ions on the recovery of palladium was investigated by using the developed method when the elements were present both individually and together. The results showed that 2500 {mu}g ml{sup -1} Na{sup +}, K{sup +}, Mg{sup 2+}, Al{sup 3+} and Fe{sup 3+}; 5000 {mu}g ml{sup -1} Ca{sup 2+} ; 500 {mu}g ml{sup -1} Pb{sup 2+}; 125 {mu}g ml{sup -1} Zn{sup 2+}; 50 {mu}g ml{sup -1} Cu{sup 2+} and 25 {mu}g ml{sup -1} Ni{sup 2+} did not interfere with the palladium signal. At the optimum conditions determined experimentally, the recovery for palladium was found to be 95.3{+-}1.2% at the 95% confidence level. The relative standard deviation and limit of detection (3s/b) of the method were found to be 1.7% and 1.2 {mu}g l{sup -1}, respectively. In order to determine the adsorption behaviour of silica gel, the adsorption isotherm of palladium was studied and the binding equilibrium constant and adsorption capacity were calculated to be 0.38 l mg{sup -1} and 4.06 mg g{sup -1}, respectively. The determination of palladium in various samples was performed by using both flame AAS and graphite furnace AAS. The proposed method was successfully applied for the determination of palladium in the street dust, anode slime, rock and catalytic converter samples.

  9. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Science.gov (United States)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6-4.3%), repeatability (4-9%), reproducibility (9-11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as straightforward

  10. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

  11. Restricted access carbon nanotubes for direct extraction of cadmium from human serum samples followed by atomic absorption spectrometry analysis.

    Science.gov (United States)

    Barbosa, Adriano F; Barbosa, Valéria M P; Bettini, Jefferson; Luccas, Pedro O; Figueiredo, Eduardo C

    2015-01-01

    In this paper, we propose a new sorbent that is able to extract metal ions directly from untreated biological fluids, simultaneously excluding all proteins from these samples. The sorbent was obtained through the modification of carbon nanotubes (CNTs) with an external bovine serum albumin (BSA) layer, resulting in restricted access carbon nanotubes (RACNTs). The BSA layer was fixed through the interconnection between the amine groups of the BSA using glutaraldehyde as cross-linker. When a protein sample is percolated through a cartridge containing RACNTs and the sample pH is higher than the isoelectric point of the proteins, both proteins from the sample and the BSA layer are negatively ionized. Thus, an electrostatic repulsion prevents the interaction between the proteins from the sample on the RACNTs surface. At the same time, metal ions are adsorbed in the CNTs (core) after their passage through the chains of proteins. The Cd(2+) ion was selected for a proof-of-principle case to test the suitability of the RACNTs due to its toxicological relevance. RACNTs were able to extract Cd(2+) and exclude almost 100% of the proteins from the human serum samples in an online solid-phase extraction system coupled with thermospray flame furnace atomic absorption spectrometry. The limits of detection and quantification were 0.24 and 0.80 μg L(-1), respectively. The sampling frequency was 8.6h(-1), and the intra- and inter-day precisions at the 0.80, 15.0, and 30.0 μg L(-1) Cd(2+) levels were all lower than 10.1% (RSD). The recoveries obtained for human blood serum samples fortified with Cd(2+) ranged from 85.0% to 112.0%. The method was successfully applied to analyze Cd(2+) directly from six human blood serum samples without any pretreatment, and the observed concentrations ranged from

  12. Determination of serum aluminum by electrothermal atomic absorption spectrometry: A comparison between Zeeman and continuum background correction systems

    Energy Technology Data Exchange (ETDEWEB)

    Kruger, Pamela C. [Department of Environmental Health Sciences, School of Public Health, University at Albany, State University of New York, P.O. Box 509, Albany, NY 12201-0509 (United States); Parsons, Patrick J. [Department of Environmental Health Sciences, School of Public Health, University at Albany, State University of New York, P.O. Box 509, Albany, NY 12201-0509 (United States); Lead Poisoning/Trace Elements Laboratory, Wadsworth Center, New York State Department of Health, P.O. Box 509, Albany, NY 12201-0509 (United States)], E-mail: patrick.parsons@wadsworth.org

    2007-03-15

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass (m{sub 0}), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 {+-} 0.6 pg, compared to 16.1 {+-} 0.7 pg for the Z5100, and 23.3 {+-} 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection

  13. Determination of traces of copper and zinc in honeys by the solid phase extraction pre-concentration followed by the flame atomic absorption spectrometry detection.

    Science.gov (United States)

    Stecka, Helena; Jedryczko, Dominika; Welna, Maja; Pohl, Pawel

    2014-10-01

    A simple and fast solid phase extraction procedure was developed to pre-concentrate traces of Cu and Zn prior to their determination in honey samples by flame atomic absorption spectrometry. The sample preparation included dissolution of honey samples and the passage (at 20 ml/min) of resulting 10% m/v solutions (100 ml) through Dowex 50W × 8-400 resin beds in order to quantitatively retain Cu and Zn and separate them from the glucose and fructose matrix. Enriched Cu and Zn traces were recovered with 5.0 ml of a 3.0 mol/l HCl solution and quantified by flame atomic absorption spectrometry. The procedure proposed was used to analyze sixty nine commercially available and freshly ripened honey samples coming from the Lower Silesia region (Poland). It enabled to measure Cu and Zn within the range of 0.01-1.42 and 0.03-15.38 μg/g, respectively, with precision better than 4%. Accuracy, assessed on the basis of the recovery test and the comparison of results with those obtained using wet digestion and inductively coupled plasma optical emission spectrometry, was ranged from -4% to +6%. Detection limits of Cu and Zn achieved with this method were 5 and 7 ng/g, respectively.

  14. Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of sulfite after on-line reduction of solid-phase manganese (IV) dioxide reactor.

    Science.gov (United States)

    Zare-Dorabei, Rouholah; Boroun, Shokoufeh; Noroozifar, Meissam

    2018-02-01

    A new and simple flow injection method followed by atomic absorption spectrometry was developed for indirect determination of sulfite. The proposed method is based on the oxidation of sulfite to sulphate ion using solid-phase manganese dioxide (30% W/W suspended on silica gel beads) reactor. MnO2 will be reduced to Mn(II) by sample injection in to the column under acidic carrier stream of HNO3 (pH 2) with flow rate of 3.5mLmin-1 at room temperature. Absorption measurement of Mn(II) which is proportional to the concentration of sulfite in the sample was carried out by atomic absorption spectrometry. The calibration curve was linear up to 25mgL-1 with a detection limit (DL) of 0.08mgL-1 for 400µL injection sample volume. The presented method is efficient toward sulfite determination in sugar and water samples with a relative standard deviation (RSD) less than 1.2% and a sampling rate of about 60h-1. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. [Determination of Al, Be, Cd, Co, Cr, Mn, Ni, Pb, Se and Tl in whole blood by atomic absorption spectrometry without preliminary sample digestion].

    Science.gov (United States)

    Ivanenko, N B; Ivanenko, A A; Solov'ev, N D; Navolotskiĭ, D V; Pavlova, O V; Ganeev, A A

    2014-01-01

    Methods of whole blood trace element determination by Graphite furnace atomic absorption spectrometry (in the variant of Zeeman's modulation polarization spectrometry) have been proposed. They do not require preliminary sample digestion. Furnace programs, modifiers and blood dilution factors were optimized. Seronorm™ human whole blood reference materials were used for validation. Dynamic ranges (for undiluted blood samples) were: Al 8 ¸ 210 мg/L; Be 0.3 ¸ 50 мg/L; Cd 0.2 ¸ 75 мg/L; Сo 5 ¸ 350 мg/L; Cr 10 ¸ 100 мg/L; Mn 6 ¸ 250 мg/L; Ni 10 ¸ 350 мg/L; Pb 3 ¸ 240 мg/L; Se 10 ¸ 500 мg/L; Tl 2 ¸ 600 мg/L. Precision (RSD) for the middle of dynamic range ranged from 5% for Mn to 11 for Se.

  16. Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination

    Energy Technology Data Exchange (ETDEWEB)

    Molaakbari, Elaheh [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Research Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mostafavi, Ali, E-mail: mostafavi.ali@gmail.com [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Environment and Nanochemistry Department, Research Institute of Environmental Science, International Center for Science, High Technology and Environmental Science, Kerman (Iran, Islamic Republic of); Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2011-01-30

    In this article, we consider ionic liquid based ultrasound-assisted dispersive liquid-liquid microextraction of trace amounts of rhodium from aqueous samples and show that this is a fast and reliable sample pre-treatment for the determination of rhodium ions by flame atomic absorption spectrometry. The Rh(III) was transferred into its complex with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol as a chelating agent, and an ultrasonic bath with the ionic liquid, 1-octyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide at room temperature was used to extract the analyte. The centrifuged rhodium complex was then enriched in the form of ionic liquid droplets and prior to its analysis by flame atomic absorption spectrometry, 300 {mu}L ethanol was added to the ionic liquid-rich phase. Finally, the influence of various parameters on the recovery of Rh(III) was optimized. Under optimum conditions, the calibration graph was linear in the range of 4.0-500.0 ng mL{sup -1}, the detection limit was 0.37 ng mL{sup -1} (3S{sub b}/m, n = 7) and the relative standard deviation was {+-}1.63% (n = 7, C = 200 ng mL{sup -1}). The results show that ionic liquid based ultrasound assisted dispersive liquid-liquid microextraction, combined with flame atomic absorption spectrometry, is a rapid, simple, sensitive and efficient analytical method for the separation and determination of trace amounts of Rh(III) ions with minimum organic solvent consumption.

  17. Advantages of the iridium permanent modifier in fast programs applied to trace-element analysis of plant samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Vassileva, E.; Baeten, H.; Hoenig, M. [Centre for Veterinary and Agrochemical Research (CERVA), Tervuren (Belgium)

    2001-03-01

    The application of a fast program combined with the advantages of the iridium permanent modifier is proposed for trace element analysis of plant samples by electrothermal atomic absorption spectrometry (ETAAS). For two volatile elements (Cd, Pb) and two mid-refractory elements (Cr, Ni) it was demonstrated that coating of the platform or of the tube atomization area with Ir is an efficient means of improving the accuracy and precision of results. A detailed study of interference from individual main matrix components and from composite plant matrices has confirmed the usefulness of the whole approach. The validity of the method has been confirmed by analysis of eight reference plant materials. (orig.)

  18. Determination of macro- and micronutrients in plant leaves by high-resolution continuum source flame atomic absorption spectrometry combining instrumental and sample preparation strategies

    Science.gov (United States)

    Oliveira, Silvana R.; Gomes Neto, José A.; Nóbrega, Joaquim A.; Jones, Bradley T.

    2010-04-01

    A method for determination of B, Ca, Cu, Fe, K, Mg, Mn, Mo, P, S and Zn in plant tissues by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) is proposed. This method is based on special features of HR-CS-AAS, such as side pixel registration, wavelength integrated absorbance, and molecular absorption bands, for determining macro- and micronutrients in foliar analysis without requiring several different strategies for sample preparation and adjustment of the analytes concentration ranges. Plant samples were analyzed and results for certified materials were in agreement at a 95% confidence level (paired t-test) with reference values. Recoveries of analytes added to plant digests varied within the 82-112% interval. Relative standard deviations ( n = 12) were lower than or equal to 5.7% for all analytes in all concentration ranges.

  19. Immobilized stearic acid as a new sorbent for on-line preconcentration and determination of lead by flow injection flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Dadfarnia Shayessteh

    2006-01-01

    Full Text Available The present study examines the possibility of immobilization of stearic acid on microcrystalline naphthalene for preparation of microcolumn and evaluation of its potential for adsorption and preconcentration of trace amounts of metal ions. It was found that this sorbent has high affinity for lead. Consequently, a rapid on-line preconcentration technique for the determination of lead by Flow Injection Flame Atomic Absorption Spectrometry had been devised. Preconcentration was based on accumulation of analyte on immobilized stearic acid microcolumn and subsequent elution by injection of a small volume of nitric acid (250 µL of 1 mol L-1. A sample volume of 20 mL resulted in a preconcentration factor of 84, and relative standard deviations for solutions containing 40 and 200 µg L-1 were 5.1 and 1.2%, respectively. The procedure was applied to tap water, river water, sea water, apple juice, beet leaf, urine, and certified stainless steel. The accuracy was proved by performing recovery experiments, Graphite Furnace Atomic Absorption Spectrometry measurements, and analysis of a stainless steel certified reference material.

  20. Method development for the determination of bromine in coal using high-resolution continuum source graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Science.gov (United States)

    Pereira, Éderson R.; Castilho, Ivan N. B.; Welz, Bernhard; Gois, Jefferson S.; Borges, Daniel L. G.; Carasek, Eduardo; de Andrade, Jailson B.

    2014-06-01

    This work reports a simple approach for Br determination in coal using direct solid sample analysis in a graphite tube furnace and high-resolution continuum source molecular absorption spectrometry. The molecular absorbance of the calcium mono-bromide (CaBr) molecule has been measured using the rotational line at 625.315 nm. Different chemical modifiers (zirconium, ruthenium, palladium and a mixture of palladium and magnesium nitrates) have been evaluated in order to increase the sensitivity of the CaBr absorption, and Zr showed the best overall performance. The pyrolysis and vaporization temperatures were 800 °C and 2200 °C, respectively. Accuracy and precision of the method have been evaluated using certified coal reference materials (BCR 181, BCR 182, NIST 1630a, and NIST 1632b) with good agreement (between 98 and 103%) with the informed values for Br. The detection limit was around 4 ng Br, which corresponds to about 1.5 μg g- 1 Br in coal, based on a sample mass of 3 mg. In addition, the results were in agreement with those obtained using electrothermal vaporization inductively coupled plasma mass spectrometry, based on a Student t-test at a 95% confidence level. A mechanism for the formation of the CaBr molecule is proposed, which might be considered for other diatomic molecules as well.

  1. Application of dual-cloud point extraction for the trace levels of copper in serum of different viral hepatitis patients by flame atomic absorption spectrometry: A multivariate study

    Science.gov (United States)

    Arain, Salma Aslam; Kazi, Tasneem G.; Afridi, Hassan Imran; Abbasi, Abdul Rasool; Panhwar, Abdul Haleem; Naeemullah; Shanker, Bhawani; Arain, Mohammad Balal

    2014-12-01

    An efficient, innovative preconcentration method, dual-cloud point extraction (d-CPE) has been developed for the extraction and preconcentration of copper (Cu2+) in serum samples of different viral hepatitis patients prior to couple with flame atomic absorption spectrometry (FAAS). The d-CPE procedure was based on forming complexes of elemental ions with complexing reagent 1-(2-pyridylazo)-2-naphthol (PAN), and subsequent entrapping the complexes in nonionic surfactant (Triton X-114). Then the surfactant rich phase containing the metal complexes was treated with aqueous nitric acid solution, and metal ions were back extracted into the aqueous phase, as second cloud point extraction stage, and finally determined by flame atomic absorption spectrometry using conventional nebulization. The multivariate strategy was applied to estimate the optimum values of experimental variables for the recovery of Cu2+ using d-CPE. In optimum experimental conditions, the limit of detection and the enrichment factor were 0.046 μg L-1 and 78, respectively. The validity and accuracy of proposed method were checked by analysis of Cu2+ in certified sample of serum (CRM) by d-CPE and conventional CPE procedure on same CRM. The proposed method was successfully applied to the determination of Cu2+ in serum samples of different viral hepatitis patients and healthy controls.

  2. Investigating effects of sample pretreatment on protein stability using size-exclusion chromatography and high-resolution continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Rakow, Tobias; El Deeb, Sami; Hahne, Thomas; El-Hady, Deia Abd; AlBishri, Hassan M; Wätzig, Hermann

    2014-09-01

    In this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 μm column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin. Ambient temperature storage was found to be harmful to all model proteins, whereas short-term storage up to 14 days could be done in an ordinary refrigerator. Freezing the protein solutions was always complicated and had to be evaluated for each protein in the corresponding solvent. To keep the proteins in their native state a gentle freezing temperature should be chosen, hence liquid nitrogen should be avoided. Furthermore, a high-resolution continuum source atomic absorption spectrometry method was developed to observe the adsorption of proteins on container material and chromatographic columns. Adsorption to any container led to a sample loss and lowered the recovery rates. During the pretreatment and high-performance size-exclusion chromatography, adsorption caused sample losses of up to 33%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Application of dual-cloud point extraction for the trace levels of copper in serum of different viral hepatitis patients by flame atomic absorption spectrometry: a multivariate study.

    Science.gov (United States)

    Arain, Salma Aslam; Kazi, Tasneem G; Afridi, Hassan Imran; Abbasi, Abdul Rasool; Panhwar, Abdul Haleem; Naeemullah; Shanker, Bhawani; Arain, Mohammad Balal

    2014-12-10

    An efficient, innovative preconcentration method, dual-cloud point extraction (d-CPE) has been developed for the extraction and preconcentration of copper (Cu(2+)) in serum samples of different viral hepatitis patients prior to couple with flame atomic absorption spectrometry (FAAS). The d-CPE procedure was based on forming complexes of elemental ions with complexing reagent 1-(2-pyridylazo)-2-naphthol (PAN), and subsequent entrapping the complexes in nonionic surfactant (Triton X-114). Then the surfactant rich phase containing the metal complexes was treated with aqueous nitric acid solution, and metal ions were back extracted into the aqueous phase, as second cloud point extraction stage, and finally determined by flame atomic absorption spectrometry using conventional nebulization. The multivariate strategy was applied to estimate the optimum values of experimental variables for the recovery of Cu(2+) using d-CPE. In optimum experimental conditions, the limit of detection and the enrichment factor were 0.046μgL(-1) and 78, respectively. The validity and accuracy of proposed method were checked by analysis of Cu(2+) in certified sample of serum (CRM) by d-CPE and conventional CPE procedure on same CRM. The proposed method was successfully applied to the determination of Cu(2+) in serum samples of different viral hepatitis patients and healthy controls. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Evaluation of solid sampling for determination of Mo, Ni, Co, and V in soil by high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Babos, Diego Victor; Barros, Ariane Isis; Ferreira, Edilene Cristina; Neto, José Anchieta Gomes

    2017-04-01

    New methods are proposed for the determination of Mo, Ni, Co, and V in soils using high-resolution continuum source graphite furnace atomic absorption spectrometry with direct solid sampling. Cobalt and V were simultaneously determined, and different analytical lines of Ni and V were monitored to adjust sensitivity for each sample. Accuracy was checked by means of soil certified reference materials, and also by flame atomic absorption spectrometry as comparative technique. The results for Mo, Ni, Co, and V found by proposed methods were in agreement with certified values and with those obtained by the comparative technique at 95% confidence level. The concentrations found in different soil samples were in the ranges 0.19-1.84 mg kg- 1 (Mo), 9.2-22.7 mg kg- 1 (Ni), 1.1-10.7 mg kg- 1 (Co), and 35.6-426.1 mg kg- 1 (V). The relative standard deviations were in the ranges 3.2-10% (Mo), 2.8-9.8% (Ni), 4.0-9.2% (Co), and 1.2-8.0% (V). The limits of quantification for Mo, Ni, Co, and V were 0.027, 0.071, 0.15, and 1.43 ng, respectively.

  5. Monitoring content of cadmium, calcium, copper, iron, lead, magnesium and manganese in tea leaves by electrothermal and flame atomizer atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Prkić Ante

    2017-08-01

    Full Text Available Due to the simplicity of tea preparation (pouring hot water onto different dried herbs and its high popularity as a beverage, monitoring and developing a screening methodology for detecting the metal content is very important. The concentrations of Cd, Ca, Cu, Fe, Pb, Mg and Mn in 11 different samples of sage (Salvia officinalis L., linden (Tilia L. and chamomile (Matricaria chamomilla L. purchased at local herbal pharmacy were determined using electrothermal atomizer atomic absorption spectrometry (ETAAS and flame atomizer atomic absorption spectrometry (FAAS. The concentrations determined were: Cd (0.012 – 0.470 mg kg−1, Ca (5209 – 16340 mg kg−1, Cu (22.01 – 33.05 mg kg−1, Fe (114.2 – 440.3 mg kg−1, Pb (0.545 – 2.538 mg kg−1, Mg (2649 – 4325 mg kg−1 and Mn (34.00 – 189.6 mg kg−1. Principal Component Analysis (PCA was applied to identify factors (soil and climate influencing the content of the measured elements in herbal samples. The proposed methodology developed in this work was successfully applied to the detection of metals in herbal samples. The analysis showed that the content of toxic metals in herbal teas was below the maximum dose recommended by the World Health Organization (WHO.

  6. Organic, inorganic and total mercury determination in fish by chemical vapor generation with collection on a gold gauze and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Duarte, Fabio Andrei; Bizzi, Cezar Augusto; Goldschmidt Antes, Fabiane; Dressler, Valderi Luiz [Departamento de Quimica, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Flores, Erico Marlon de Moraes [Departamento de Quimica, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil)], E-mail: flores@quimica.ufsm.br

    2009-06-15

    A method for organic, inorganic and total mercury determination in fish tissue has been developed using chemical vapor generation and collection of mercury vapor on a gold gauze inside a graphite tube and further atomization by electrothermal atomic absorption spectrometry. After drying and cryogenic grinding, potassium bromide and hydrochloric acid solution (1 mol L{sup - 1} KBr in 6 mol L{sup - 1} HCl) was added to the samples. After centrifugation, total mercury was determined in the supernatant. Organomercury compounds were selectively extracted from KBr solution using chloroform and the resultant solution was back extracted with 1% m/v L-cysteine. This solution was used for organic Hg determination. Inorganic Hg remaining in KBr solution was directly determined by chemical vapor generation electrothermal atomic absorption spectrometry. Mercury vapor generation from extracts was performed using 1 mol L{sup - 1} HCl and 2.5% m/v NaBH{sub 4} solutions and a batch chemical vapor generation system. Mercury vapor was collected on the gold gauze heated resistively at 80 deg. C and the atomization temperature was set at 650 deg. C. The selectivity of extraction was evaluated using liquid chromatography coupled to chemical vapor generation and determination by inductively coupled plasma mass spectrometry. The proposed method was applied for mercury analysis in shark, croaker and tuna fish tissues. Certified reference materials were used to check accuracy and the agreement was better than 95%. The characteristic mass was 60 pg and method limits of detection were 5, 1 and 1 ng g{sup - 1} for organic, inorganic and total mercury, respectively. With the proposed method it was possible to analyze up to 2, 2 and 6 samples per hour for organic, inorganic and total Hg determination, respectively.

  7. Organic, inorganic and total mercury determination in fish by chemical vapor generation with collection on a gold gauze and electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Duarte, Fábio Andrei; Bizzi, Cezar Augusto; Antes, Fabiane Goldschmidt; Dressler, Valderi Luiz; Flores, Érico Marlon de Moraes

    2009-06-01

    A method for organic, inorganic and total mercury determination in fish tissue has been developed using chemical vapor generation and collection of mercury vapor on a gold gauze inside a graphite tube and further atomization by electrothermal atomic absorption spectrometry. After drying and cryogenic grinding, potassium bromide and hydrochloric acid solution (1 mol L - 1 KBr in 6 mol L - 1 HCl) was added to the samples. After centrifugation, total mercury was determined in the supernatant. Organomercury compounds were selectively extracted from KBr solution using chloroform and the resultant solution was back extracted with 1% m/v L-cysteine. This solution was used for organic Hg determination. Inorganic Hg remaining in KBr solution was directly determined by chemical vapor generation electrothermal atomic absorption spectrometry. Mercury vapor generation from extracts was performed using 1 mol L - 1 HCl and 2.5% m/v NaBH 4 solutions and a batch chemical vapor generation system. Mercury vapor was collected on the gold gauze heated resistively at 80 °C and the atomization temperature was set at 650 °C. The selectivity of extraction was evaluated using liquid chromatography coupled to chemical vapor generation and determination by inductively coupled plasma mass spectrometry. The proposed method was applied for mercury analysis in shark, croaker and tuna fish tissues. Certified reference materials were used to check accuracy and the agreement was better than 95%. The characteristic mass was 60 pg and method limits of detection were 5, 1 and 1 ng g - 1 for organic, inorganic and total mercury, respectively. With the proposed method it was possible to analyze up to 2, 2 and 6 samples per hour for organic, inorganic and total Hg determination, respectively.

  8. Comparison of atomic absorption, mass and X-ray spectrometry techniques using dissolution-based and solid sampling methods for the determination of silver in polymeric samples

    Energy Technology Data Exchange (ETDEWEB)

    Schrijver, Isabel de [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium); University College West-Flanders, Department of Industrial Engineering and Technology, Research group EnBiChem, Graaf Karel de Goedelaan 5, B-8500 Kortrijk (Belgium); Aramendia, Maite; Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium); Resano, Martin [University of Zaragoza, Department of Analytical Chemistry, Pedro Cerbuna 12, E-50009 Zaragoza (Spain); Dumoulin, Ann [University College West-Flanders, Department of Industrial Engineering and Technology, Research group EnBiChem, Graaf Karel de Goedelaan 5, B-8500 Kortrijk (Belgium); Vanhaecke, Frank [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium)], E-mail: Frank.Vanhaecke@UGent.be

    2007-11-15

    In this work, the capabilities and limitations of solid sampling techniques - laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS), wavelength dispersive X-ray fluorescence spectrometry (WD-XRFS) and solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS) - for the determination of silver in polymers have been evaluated and compared to those of acid digestion and subsequent Ag determination using pneumatic nebulization ICPMS (PN-ICPMS) or flame AAS (FAAS). In a first stage, two dissolution procedures were examined: conventional acid digestion in a Kjeldahl flask and the combination of dry ashing and microwave-assisted digestion. Accurate results for Ag could be obtained, although occasionally, problems of analyte losses and/or incomplete dissolution were observed. LA-ICPMS shows potential for direct analysis of solid materials, but calibration was found to be difficult. A polypropylene sample was used as standard. This approach provided satisfactory results for other polypropylene samples and even for other types of plastics, provided that the {sup 13}C{sup +} signal was used as internal reference, correcting for variations in ablation efficiency. However, the results for polyoxymethylene were overestimated. Similar calibration problems appeared with WD-XRFS, due to differences in absorption efficiency of X-rays. In this case, the accuracy could be improved by using a matrix correction procedure, which however required the matrix composition to be known into sufficient detail. SS-ETAAS, proved to be a fast approach that allowed accurate determination of Ag in polymers using aqueous standard solutions for calibration. Due to the high Ag content and the excellent sensitivity, the use of a 3-field mode Zeeman-effect background correction system was essential for the extension of the working range.

  9. Application of Internal Standard Method for Several 3d-Transition Metallic Elements in Flame Atomic Absorption Spectrometry Using a Multi-wavelength High-resolution Spectrometer.

    Science.gov (United States)

    Toya, Yusuke; Itagaki, Toshiko; Wagatsuma, Kazuaki

    2017-01-01

    We investigated a simultaneous internal standard method in flame atomic absorption spectrometry (FAAS), in order to better the analytical precision of 3d-transition metals contained in steel materials. For this purpose, a new spectrometer system for FAAS, comprising a bright xenon lamp as the primary radiation source and a high-resolution Echelle monochromator, was employed to measure several absorption lines at a wavelength width of ca. 0.3 nm at the same time, which enables the absorbances of an analytical line and also an internal standard line to be estimated. In considering several criteria for selecting an internal standard element and the absorption line, it could be suggested that platinum-group elements: ruthenium, rhodium, or palladium, were suitable for an internal standard element to determine the 3d-transition metal elements, such as titanium, iron, and nickel, by measuring an appropriate pair of these absorption lines simultaneously. Several variances of the absorption signal, such as a variation in aspirated amounts of sample solution and a short-period drift of the primary light source, would be corrected and thus reduced, when the absorbance ratio of the analytical line to the internal standard line was measured. In Ti-Pd, Ni-Rh, and Fe-Ru systems chosen as typical test samples, the repeatability of the signal respnses was investigated with/without the internal standard method, resulting in better precision when the internal standard method was applied in the FAAS with a nitrous oxide-acetylene flame rather than an air-acetylene flame.

  10. Determination of lead, cadmium and mercury in blood for assessment of environmental exposure: A comparison between inductively coupled plasma-mass spectrometry and atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Palmer, Christopher D. [Wadsworth Center, New York State Department of Health, P.O. Box 509, Albany, NY 12201-0509 (United States); Lewis, Miles E. [Wadsworth Center, New York State Department of Health, P.O. Box 509, Albany, NY 12201-0509 (United States); Geraghty, Ciaran M. [Wadsworth Center, New York State Department of Health, P.O. Box 509, Albany, NY 12201-0509 (United States); Barbosa, Fernando [Faculdade de Cinecias Farmaceuticas de Ribeirao Preto, Universidade de Sao Paolo, Ribeirao Preto-Sao Paolo (Brazil); Parsons, Patrick J. [Wadsworth Center, New York State Department of Health, P.O. Box 509, Albany, NY 12201-0509 (United States) and Department of Environmental Health Sciences, School of Public Health, University of Albany, State University of New York, Albany, NY 12201-0509 (United States)]. E-mail: patrick.parsons@wadsworth.org

    2006-08-15

    A biomonitoring method for the determination of Pb, Cd, and Hg at background levels in whole blood by inductively coupled plasma-mass spectrometry is described. While this method was optimized for assessing Pb, Cd and Hg at environmental levels, it also proved suitable for assessing concentrations associated with occupational exposure. The method requires as little as 200 {mu}l of blood that is diluted 1 + 49 for direct analysis in the inductively coupled plasma-mass spectrometer. Method performance is compared to well-established AAS methods. Initial method validation was accomplished using National Institute of Standards and Technology (NIST) Standard Reference Material 966, Toxic Metals in Bovine Blood. Method detection limits (3s) are 0.05 {mu}g dl{sup -1} for Pb, 0.09 {mu}g l{sup -1} for Cd; and 0.17 {mu}g l{sup -1} for Hg. Repeatability ranged from 1.4% to 2.8% for Pb; 3% to 10% for Cd; and 2.6% to 8.8% for Hg. In contrast, AAS method detection limits were 1 {mu}g dl{sup -1}, 0.54 {mu}g l{sup -1}, and 0.6 {mu}g l{sup -1}, for Pb, Cd, and Hg, respectively. Further performance assessments were conducted over a 2-year period via participation in four international External Quality Assessment Schemes (EQAS) operated specifically for toxic metals in blood. This includes schemes operated by (a) the New York State Department of Health's Wadsworth Center, Albany, NY, USA (b) L'Institut National de Sante Publique du Quebec, Centre de Toxicologie du Quebec, Canada (c) Friedrich-Alexander University, Erlangen, Germany, and (d) the University of Surrey, Guildford, UK Trace Elements scheme. The EQAS data reflect analytical performance for blind samples analyzed independently by both inductively coupled plasma-mass spectrometry and AAS methods.

  11. Determination of lead, cadmium and mercury in blood for assessment of environmental exposure: A comparison between inductively coupled plasma mass spectrometry and atomic absorption spectrometry

    Science.gov (United States)

    Palmer, Christopher D.; Lewis, Miles E.; Geraghty, Ciaran M.; Barbosa, Fernando; Parsons, Patrick J.

    2006-08-01

    A biomonitoring method for the determination of Pb, Cd, and Hg at background levels in whole blood by inductively coupled plasma-mass spectrometry is described. While this method was optimized for assessing Pb, Cd and Hg at environmental levels, it also proved suitable for assessing concentrations associated with occupational exposure. The method requires as little as 200 μl of blood that is diluted 1 + 49 for direct analysis in the inductively coupled plasma-mass spectrometer. Method performance is compared to well-established AAS methods. Initial method validation was accomplished using National Institute of Standards and Technology (NIST) Standard Reference Material 966, Toxic Metals in Bovine Blood. Method detection limits (3s) are 0.05 μg dl - 1 for Pb, 0.09 μg l - 1 for Cd; and 0.17 μg l - 1 for Hg. Repeatability ranged from 1.4% to 2.8% for Pb; 3% to 10% for Cd; and 2.6% to 8.8% for Hg. In contrast, AAS method detection limits were 1 μg dl - 1 , 0.54 μg l - 1 , and 0.6 μg l - 1 , for Pb, Cd, and Hg, respectively. Further performance assessments were conducted over a 2-year period via participation in four international External Quality Assessment Schemes (EQAS) operated specifically for toxic metals in blood. This includes schemes operated by (a) the New York State Department of Health's Wadsworth Center, Albany, NY, USA (b) L'Institut National de Santé Publique du Québec, Centre de Toxicologie du Québec, Canada, (c) Friedrich-Alexander University, Erlangen, Germany, and (d) the University of Surrey, Guildford, UK Trace Elements scheme. The EQAS data reflect analytical performance for blind samples analyzed independently by both inductively coupled plasma-mass spectrometry and AAS methods.

  12. High-resolution continuum source graphite furnace molecular absorption spectrometry compared with ion chromatography for quantitative determination of dissolved fluoride in river water samples.

    Science.gov (United States)

    Ley, Philip; Sturm, Manfred; Ternes, Thomas A; Meermann, Björn

    2017-10-03

    In addition to beneficial health effects, fluoride can also have adverse effects on humans, animals, and plants if the daily intake is strongly elevated. One main source of fluoride uptake is water, and thus several ordinances exist in Germany that declare permissible concentrations of fluoride in, for example, drinking water, mineral water, and landfill seepage water. Controlling the fluoride concentrations in aqueous matrices necessitate valid and fast analytical methods. In this work an alternative method for the determination of fluoride in surface waters based on high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) was applied. Fluoride detection was made possible by the formation of a diatomic molecule, GaF, and detection of characteristic molecular absorption. On HR-CS-GFMAS parameter optimization, the method was adapted to surface water sample analysis. The influence of potential main matrix constituents such as Na+, Ca2+, Mg2+, and Cl- as well as surface water sampling/storage conditions on the molecular absorption signal of GaF was investigated. Method validation demonstrated a low limit of detection (8.1 μg L-1) and a low limit of quantification (26.9 μg L-1), both sufficient for direct river water sample analysis after 0.45-μm filtration. The optimized HR-CS-GFMAS method was applied for the analysis of real water samples from the rivers Rhine and Moselle. For method validation, samples were also analyzed by an ion chromatography (IC) method. IC and HR-CS-GFMAS results both agreed well. In comparison with IC, HR-CS-GFMAS has higher sample throughput, a lower limit of detection and a lower limit of quantification, and higher selectivity, and is a very suitable method for the analysis of dissolved fluoride in river water. Graphical abstract High-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) was applied for the quantitative analysis of dissolved fluoride in river

  13. Micro-sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry for calcium determination in blood and mitochondrial suspensions.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Satrústegui, Jorgina; Procopio, Jesús R

    2017-08-01

    A micro-sampling and straightforward method based on high resolution continuum source atomic absorption spectrometry (HR-CS AAS) was developed to determine extracellular and intracellular Ca in samples of interest in clinical and biomedical analysis. Solid sampling platforms were used to introduce the micro-samples into the graphite furnace atomizer. The secondary absorption line for Ca, located at 239.856nm, was selected to carry out the measurements. Experimental parameters such as pyrolysis and atomization temperatures and the amount of sample introduced for the measurements were optimized. Calibration was performed using aqueous standards and the approach to measure at the wings of the absorption lines was employed for the expansion of the linear response range. The limit of detection was of 0.02mgL-1 Ca (0.39ng Ca) and the upper limit of linear range was increased up to 8.0mgL-1 Ca (160ng Ca). The proposed method was used to determine Ca in mitochondrial suspensions and whole blood samples with successful results. Adequate recoveries (within 91-107%) were obtained in the tests performed for validation purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Direct determination of fluorine in niobium oxide using slurry sampling electrothermal high-resolution continuum source molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Mao Dong; Becker-Ross, Helmut [Leibniz-Institut für Analytische Wissenschaften—ISAS—e.V., Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany); Okruss, Michael, E-mail: michael.okruss@isas.de [Leibniz-Institut für Analytische Wissenschaften—ISAS—e.V., Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany); Geisler, Sebastian; Florek, Stefan [Leibniz-Institut für Analytische Wissenschaften—ISAS—e.V., Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany); Richter, Silke; Meckelburg, Angela [BAM Federal Institute for Materials Research and Testing, Department of Analytical Chemistry, Reference Materials, Richard-Willstätter-Str. 11, 12489 Berlin (Germany)

    2014-04-01

    Aiming for a round-robin test, a new method for the direct determination of fluorine in niobium oxide has been developed. It is based on the use of high-resolution molecular absorption spectra of calcium mono-fluoride (CaF) generated in the graphite tube, combined with the slurry sampling technique. The absorption measurement was performed at the 606.44 nm CaF rotational line. By using graphite tubes with zirconium carbide (ZrC) modified platform, the molecular absorption sensitivity of CaF has been improved by a factor of 20, and no additional chemical modifier was necessary. Generally, non-spectral interferences were observed in the presence of HCl, H{sub 2}SO{sub 4}, and H{sub 3}PO{sub 4}. For HCl, additional spectral interference occurred due to an overlap of the absorption spectra of CaF and CaCl. However, due to the absence of these mentioned substances in the current material, such interferences do not exist for this application. The characteristic mass found for the CaF 606.44 nm line was 0.1 ng; the limit of detection was 5 mg fluorine per kg solid sample (3σ criterion). The results obtained by the method were within the range of certified values. Comparing to the classical method such as the pyrohydrolysis-photometric method, the developed new method showed clear advantages regarding sensitivity and specificity. The time requirement for one sample analysis was strongly shortened from several hours to only some minutes. - Highlights: • First time determination of fluorine in niobium oxide using the slurry sampling technique • Application of calcium fluoride molecular absorption in graphite tube with ZrC modification • Higher specificity, better sensitivity, and huge time saving compared with the classical method based on pyrohydrolysis • New method verified by successful participation in round robin test.

  15. Quantification of absorption, retention and elimination of two different oral doses of vitamin A in Zambian boys using accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Aklamati, E K; Mulenga, M; Dueker, S R; Buchholz, B A; Peerson, J M; Kafwembe, E; Brown, K H; Haskell, M J

    2009-10-12

    A recent survey indicated that high-dose vitamin A supplements (HD-VAS) had no apparent effect on vitamin A (VA) status of Zambian children <5 y of age. To explore possible reasons for the lack of response to HD-VAS among Zambian children, we quantified the absorption, retention, and urinary elimination of either a single HDVAS (60 mg) or a smaller dose of stable isotope (SI)-labeled VA (5 mg), which was used to estimate VA pool size, in 3-4 y old Zambian boys (n = 4 for each VA dose). A 25 nCi tracer dose of [{sup 14}C{sub 2}]-labeled VA was co-administered with the HD-VAS or SI-labeled VA, and 24-hr stool and urine samples were collected for 3 and 7 consecutive days, respectively, and 24-hr urine samples at 4 later time points. Accelerator Mass Spectrometry (AMS) was used to measure the cumulative excretion of {sup 14}C in stool and urine 3d after dosing to estimate, respectively, absorption and retention of the VAS and SI-labeled VA. The urinary elimination rate (UER) was estimated by plotting {sup 14}C in urine vs. time, and fitting an exponential equation to the data. Estimates of mean absorption, retention and the UER were 83.8 {+-} 7.1%, 76.3 {+-} 6.7%, and 1.9 {+-} 0.6%/d, respectively, for the HD-VAS and 76.5 {+-} 9.5%, 71.1 {+-} 9.4%, and 1.8 {+-} 1.2%/d, respectively for the smaller dose of SI-labeled VA. Estimates of absorption, retention and the UER did not differ by size of the VA dose administered (P=0.26, 0.40, 0.88, respectively). Estimated absorption and retention were negatively associated with reported fever (P=0.011) and malaria (P =0.010). HD-VAS and SI-labeled VA were adequately absorbed, retained and utilized in apparently healthy Zambian preschool-age boys, although absorption and retention may be affected by recent infections.

  16. Ultra-Trace Determination of Copper and Silver in Environmental Samples by Using Ionic Liquid-Based Single Drop Microextraction-Electrothermal Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    J. Abolhasani

    2013-11-01

    Full Text Available A sensitive, selective and effective ionic liquid-based single drop microextraction technique wasdeveloped by using ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate, C6MIMPF6, coupledwith electrothermal atomic absorption spectrometry (ETAAS for the determination of copper and silver inenvironmental samples. Dithizone was used as chelating agent. Several factors that influence themicroextraction efficiency and ETAAS signal, such as pH, dithizone concentration, extraction time, amounts ofionic liquid, stirring rate, pyrolysis and atomization temperature were investigated and the microextractionconditions were established. In the optimum experimental conditions, the detection limits (3 s of the methodwere 4 and 8 ng L-1 and corresponding relative standard deviations (0.1 μg L-1, n = 6 were 4.2% and 4.8% forAg and Cu, respectively. The developed method was validated by analysis of a certified reference material andapplied to the determination of silver and copper.

  17. Temperature-controlled electrothermal atomization-atomic absorption spectrometry using a pyrometric feedback system in conjunction with a background monitoring device

    Science.gov (United States)

    Van Deijck, W.; Roelofsen, A. M.; Pieters, H. J.; Herber, R. F. M.

    The construction of a temperature-controlled feedback system for electrothermal atomization-atomic absorption spectrometry (ETA-AAS) using an optical pyrometer applied to the atomization stage is described. The system was used in conjunction with a fast-response background monitoring device. The heating rate of the furnace amounted to 1400° s -1 with a reproducibility better than 1%. The precision of the temperature control at a steady state temperature of 2000°C was 0.1%. The analytical improvements offered by the present system have been demonstrated by the determination of cadmium and lead in blood and finally by the determination of lead in serum. Both the sensitivity and the precision of the method have been improved. The accuracy of the method was checked by determining the lead content for a number of scrum samples both by ETA-AAS and differential pulse anodic stripping voltametry (DPASV) and proved to be satisfactory.

  18. ESTIMATION OF MEASUREMENT UNCERTAINTY IN THE DETERMINATION OF Fe CONTENT IN POWDERED TONIC FOOD DRINK USING GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Harry Budiman

    2010-06-01

    Full Text Available The evaluation of uncertainty measurement in the determination of Fe content in powdered tonic food drink using graphite furnace atomic absorption spectrometry was carried out. The specification of measurand, source of uncertainty, standard uncertainty, combined uncertainty and expanded uncertainty from this measurement were evaluated and accounted. The measurement result showed that the Fe content in powdered tonic food drink sample was 569.32 µg/5g, with the expanded uncertainty measurement ± 178.20 µg/5g (coverage factor, k = 2, at confidende level 95%. The calibration curve gave the major contribution to the uncertainty of the final results.   Keywords: uncertainty, powdered tonic food drink, iron (Fe, graphite furnace AAS

  19. Investigation of Pb species in soils, celery and duckweed by synchrotron radiation X-ray absorption near-edge structure spectrometry

    Science.gov (United States)

    Luo, Liqiang; Shen, Yating; Liu, Jian; Zeng, Yuan

    2016-08-01

    The Pb species play a key role in its translocation in biogeochemical cycles. Soils, sediments and plants were collected from farmlands around Pb mines, and the Pb species in them was identified by X-ray absorption near-edge structure spectrometry. In soils, Pb5(PO4)3Cl and Pb3(PO4)2 were detected, and in sediments, Pb-fulvic acids (FAs) complex was identified. A Pb complex with FA fragments was also detected in celery samples. We found that (1) different Pb species were present in soils and sediments; (2) the Pb species in celery, which was grown in sediments, was different from the species present in duckweed, which grew in water; and (3) a Pb-FA-like compound was present in celery roots. The newly identified Pb species, the Pb-FA-like compound, may play a key role in Pb tolerance and translocation within plants.

  20. Separation/preconcentration of trace Pb(II and Cd(II with 2-mercaptobenzothiazole impregnated Amberlite XAD-1180 resin and their determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Şerife Tokalıoğlu

    2017-01-01

    Full Text Available A new chelating resin, 2-mercaptobenzothiazole loaded Amberlite XAD-1180 was prepared and used for separation and preconcentration of Cd(II and Pb(II ions prior to their determinations by flame atomic absorption spectrometry. The optimum pH for simultaneous retention of the elements and the best elution means for their simultaneous elution were 9.5 and 2 mol L−1 HNO3, respectively. The detection limits for Cd(II and Pb(II were 0.35 and 5.0 μg L−1, respectively. The accuracy of the method was confırmed both by analyzing the certified reference material (RM 8704 Buffalo river sediment and performing recovery studies.

  1. Dithizone chloroform single drop microextraction system combined with electrothermal atomic absorption spectrometry using Ir as permanent modifier for the determination of Cd in water and biological samples

    Science.gov (United States)

    Fan, Zhefeng; Zhou, Wei

    2006-07-01

    A simple and sensitive method using dithizone-chloroform single drop microextraction has been developed for separation and preconcentration of trace Cd prior to its determination by electrothermal atomic absorption spectrometry with Ir as permanent modifier. Parameters, such as pyrolysis and atomization temperature, solvent type, pH, dithizone concentration, extraction time, organic drop volume, stirring rate and sample volume were investigated. Under the optimized conditions, a detection limit (3 σ) of 0.7 ng/l and enrichment factor of 65 were achieved. The relative standard deviation was 7.4% ( c = 0.2 μg/l, n = 5). The developed method has been applied to the determination of trace Cd in water samples and biological reference materials with satisfactory results.

  2. Speciation analysis of mercury in water samples by cold vapor atomic absorption spectrometry after preconcentration with dithizone immobilized on microcrystalline naphthalene.

    Science.gov (United States)

    Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Nasirizadeh, Navid

    2004-03-01

    Trace amounts of inorganic mercury (Hg(2+)) and methylmercury cations (MeHg(2+)) were adsorbed quantitatively from acidic aqueous solution onto a column packed with immobilized dithizone on microcrystalline naphthalene. The trapped mercury was eluted with 10 ml of 7 mol L(-1) hydrochloric acid solution. The Hg(2+) was then directly reduced with tin (II) chloride, and volatilized mercury was determined by cold vapor atomic absorption spectrometry (CVAAS). Total mercury (Hgt) was determined after decomposition of MeHg(+) into Hg(2+). Hg(2+) and MeHg(+) cations were completely recovered from the water with a preconcentration factor of 200. The relative standard deviation obtained for eight replicate determinations at a concentration of 0.3 microg L(-1 )was 1.8%. The procedure was applied to analysis of water samples, and the accuracy was assessed via recovery experiment.

  3. Dithizone-chloroform single drop microextraction system combined with electrothermal atomic absorption spectrometry using Ir as permanent modifier for the determination of Cd in water and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Fan Zhefeng [Department of Chemistry, Shanxi Normal University, Linfen 041004 (China)]. E-mail: zhefengfan@163.com; Zhou Wei [Department of Chemistry, Shanxi Normal University, Linfen 041004 (China)

    2006-07-15

    A simple and sensitive method using dithizone-chloroform single drop microextraction has been developed for separation and preconcentration of trace Cd prior to its determination by electrothermal atomic absorption spectrometry with Ir as permanent modifier. Parameters, such as pyrolysis and atomization temperature, solvent type, pH, dithizone concentration, extraction time, organic drop volume, stirring rate and sample volume were investigated. Under the optimized conditions, a detection limit (3{sigma}) of 0.7 ng/l and enrichment factor of 65 were achieved. The relative standard deviation was 7.4% (c = 0.2 {mu}g/l, n = 5). The developed method has been applied to the determination of trace Cd in water samples and biological reference materials with satisfactory results.

  4. Preconcentration, Separation and Determination of lead(II) with Methyl Thymol Blue Adsorbed on Activated Carbon Using Flame Atomic Absorption Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ensafi, Ali A.; Ghaderi, Ali R. [Isfahan University of Technology, Isfahan (Iran, Islamic Republic of)

    2008-02-15

    An on-line system for preconcentration and separation of lead(II) is presented. The method is based on the complex formation of Pb(II) with adsorbed Methyl thymol blue on activated carbon. The conditions of preparing the solid phase reagent and of quantitative recovery of Pb(II) from diluted solutions, such as acidity of aqueous phase, solid phase capacity, and flow variables were studied as well as effect of potential interfering ions. After preconcentration step, the metal ions are eluted automatically by 5 ml of 0.5 M HNO{sub 3} solution and the lead ions content was determined by flame atomic absorption spectrometry. Under the optimum conditions, the lead ions in aqueous samples were separated and preconcentrated about 1000-fold by the column. The detection limit was 0.001 μg mL{sup -1}. Lead has been determined in river and tap water samples, with recovery of 98 to 102%.

  5. Cold vapor-solid phase microextraction using amalgamation in different Pd-based substrates combined with direct thermal desorption in a modified absorption cell for the determination of Hg by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Romero, Vanesa; Costas-Mora, Isabel; Lavilla, Isela; Bendicho, Carlos, E-mail: bendicho@uvigo.es

    2011-02-15

    In this work, different Pd-based substrates (i.e. Pd wire, Pd-coated stainless steel wire and Pd-coated SiO{sub 2}) are tried for microextraction of Hg prior to its release into a modified quartz T-cell so as to develop a cost-effective, sensitive and easy-to-handle coupling between solid-phase microextraction (SPME) and atomic absorption spectrometry. The new design allows a direct sample injection from the SPME device into a quartz T-cell thus avoiding analyte dilution. Mercury amalgamation onto a Pd wire provided the best performance in respect to sensitivity and fiber lifetime, but Pd wires could not be implemented in the SPME device due to their poor mechanical characteristics. On the contrary, Pd-coated SiO{sub 2} fibers could be easily adapted to the typical sampling device used for SPME. Narrow time-dependent absorption signal profiles that could be integrated within 25 s were obtained. The detection limit was 90 pg mL{sup -1} of Hg, and the repeatability expressed as relative standard deviation was 4.3%.

  6. Intrinsic UV absorption spectrometry observed with a liquid core waveguide as a sensor technique for monitoring ozone in water.

    Science.gov (United States)

    Le, Trang; Tao, Shiquan

    2011-08-21

    The industrial use of ozone as a sanitizing agent in water treatment and food processing in recent years calls for sensor technologies for monitoring ozone in water for process control. Ozone molecules absorb UV light with a peak absorption wavelength at 254 nm. This property has been used in this work to develop a simple sensor technology for online, real-time continuous monitoring of trace ozone in water. A Teflon AF2400 tube filled with pure water forms a liquid core waveguide (LCW), which is used as a long-path-length optical absorption cell. This pure water filled tube was deployed into a water sample. Ozone molecules dissolved in the water sample permeate through the Teflon AF2400 tube wall and dissolve in water filled in the tube. This prevents interference species from entering the LCW, and eliminates interferences. The optical absorption signal of the long-path-length cell at 254 nm measured by guiding light through the LCW is used as a sensing signal. This simple structured sensor does not involve any chemical reagent, is reversible, and has a response time <4.5 minutes. It can be used to detect ozone in water samples down to 3.6 × 10(-9) mol L(-1).

  7. Determination of trace amount of cadmium using dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry

    Science.gov (United States)

    Fırat, Merve; Bakırdere, Sezgin; Fındıkoğlu, Maral Selin; Kafa, Emine Betül; Yazıcı, Elif; Yolcu, Melda; Büyükpınar, Çağdaş; Chormey, Dotse Selali; Sel, Sabriye; Turak, Fatma

    2017-03-01

    This study was performed to develop a sensitive analytical method for the determination of cadmium by slotted quartz tube-flame atomic absorption spectrometry (SQT-FAAS) after dispersive liquid-liquid microextraction (DLLME). The parameters affecting the cadmium complex formation and its extraction output were optimized to obtain high extraction efficiency. These included the pH and amount of the buffer solution, and the concentration of the ligand. The DLLME method was comprehensively optimized based on the type and amount of extraction solvent, dispersive solvent and salt. The type and period of mixing needed for a more effective extraction was also investigated. In order to further improve the sensitivity for the determination of cadmium, the flame atomic absorption spectrometry was fitted with a slotted quartz tube to increase the residence time of cadmium atoms in the pathway of incident light from a hollow cathode lamp. The limits of detection and quantitation (LOD and LOQ) for the FAAS were found to be 42 and 140 μg L- 1, respectively. Under the optimum conditions, LOD and LOQ of the FAAS after DLLME were calculated as 1.3 and 4.4 μg L- 1, respectively. Combining both optimized parameters of the DLLME and SQT-FAAS gave 0.5 and 1.5 μg L- 1 as LOD and LOQ, respectively. Accuracy of the method was also checked using a wastewater certified reference material (EU-L-2), and the result was in good agreement with the certified value.

  8. Chemometric evaluation of Cd, Co, Cr, Cu, Ni (inductively coupled plasma optical emission spectrometry) and Pb (graphite furnace atomic absorption spectrometry) concentrations in lipstick samples intended to be used by adults and children.

    Science.gov (United States)

    Batista, Érica Ferreira; Augusto, Amanda dos Santos; Pereira-Filho, Edenir Rodrigues

    2016-04-01

    A method was developed for determining the concentrations of Cd, Co, Cr, Cu, Ni and Pb in lipstick samples intended to be used by adults and children using inductively coupled plasma optical emission spectrometry (ICP OES) and graphite furnace atomic absorption spectrometry (GF AAS) after treatment with dilute HNO3 and hot block. The combination of fractional factorial design and Desirability function was used to evaluate the ICP OES operational parameters and the regression models using Central Composite and Doehlert designs were calculated to stablish the best working condition for all analytes. Seventeen lipstick samples manufactured in different countries with different colors and brands were analyzed. Some samples contained high concentrations of toxic elements, such as Cr and Pb, which are carcinogenic and cause allergic and eczematous dermatitis. The maximum concentration detected was higher than the permissible safe limits for human use, and the samples containing these high metal concentrations were intended for use by children. Principal component analysis (PCA) was used as a chemometrics tool for exploratory analysis to observe the similarities between samples relative to the metal concentrations (a correlation between Cd and Pb was observed). Copyright © 2015 Elsevier B.V. All rights reserved.

  9. A comparison of laser ablation-inductively coupled plasma-mass spectrometry and high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers

    Science.gov (United States)

    de Gois, Jefferson S.; Van Malderen, Stijn J. M.; Cadorim, Heloisa R.; Welz, Bernhard; Vanhaecke, Frank

    2017-06-01

    This work describes the development and comparison of two methods for the direct determination of Br in polymer samples via solid sampling, one using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and the other using high-resolution continuum source graphite furnace molecular absorption spectrometry with direct solid sample analysis (HR-CS SS-GF MAS). The methods were optimized and their accuracy was evaluated by comparing the results obtained for 6 polymeric certified reference materials (CRMs) with the corresponding certified values. For Br determination with LA-ICP-MS, the 79Br+ signal could be monitored interference-free. For Br determination via HR-CS SS-GF MAS, the CaBr molecule was monitored at 625.315 nm with integration of the central pixel ± 1. Bromine quantification by LA-ICP-MS was performed via external calibration against a single CRM while using the 12C+ signal as an internal standard. With HR-CS SS-GF MAS, Br quantification could be accomplished using external calibration against aqueous standard solutions. Except for one LA-ICP-MS result, the concentrations obtained with both techniques were in agreement with the certified values within the experimental uncertainty as evidenced using a t-test (95% confidence level). The limit of quantification was determined to be 100 μg g- 1 Br for LA-ICP-MS and 10 μg g- 1 Br for HR-CS SS-GF MAS.

  10. In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

    2018-03-01

    In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

  11. Evaluation of the memory effect on gold-coated silica adsorption tubes used for the analysis of gaseous mercury by cold vapor atomic absorption spectrometry.

    Science.gov (United States)

    Rahman, Mohammad Mahmudur; Brown, Richard J C; Kim, Ki-Hyun; Yoon, Hye-On; Phan, Nhu-Thuc

    2013-01-01

    In an effort to reduce the experimental bias involved in the analysis of gaseous elemental mercury (Hg(o)), the blank response from gold-coated adsorption tubes has been investigated using cold vapor atomic absorption spectrometry (CVAAS). Our study has been compared with our recent investigation on memory effect in a cold vapour atomic fluorescence spectrometry (CVAFS). The pattern of blank responses was quantified after loading different amounts of mercury and after different time intervals of 1, 14, and 45 days. In case of the one day interval, the result of five to six instant blank heating cycles confirmed successful liberation of mercury following the second and third blank heating cycles. The results of 14 or 45 days generally suggest that liberation of excess mercury is affected by both the initial loading amount and the length of storage time prior to analysis. We have demonstrated a possibly effective way to reduce memory effects. Some similarities of these results with those from CVAFS experiment suggests that the blank response is caused by a combination of mercury absorbed within the bulk gold and micro- and nanoparticles liberated during heating and not from coabsorbing interfering gaseous species.

  12. A simple and fast method for assessment of the nitrogen-phosphorus-potassium rating of fertilizers using high-resolution continuum source atomic and molecular absorption spectrometry

    Science.gov (United States)

    Bechlin, Marcos André; Fortunato, Felipe Manfroi; da Silva, Ricardo Moutinho; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta

    2014-11-01

    The determination of N, P, and K in fertilizers by high-resolution continuum source flame atomic and molecular absorption spectrometry is proposed. Under optimized conditions, measurements of the diatomic molecules NO and PO at 215.360 and 247.620 nm, respectively, and K using the wing of the alternative line at 404.722 nm allowed calibration curves to be constructed in the ranges 500-5000 mg L- 1 N (r = 0.9994), 100-2000 mg L- 1 P (r = 0.9946), and 100-2500 mg L- 1 K (r = 0.9995). Commercial fertilizers were analyzed by the proposed method and the concentrations of N, P, and K were found to be in agreement with those obtained by Kjeldahl, spectrophotometric, and flame atomic emission spectrometry methods, respectively, at a 95% confidence level (paired t-test). A phosphate rock certified reference material (CRM) was analyzed and the results for P and K were in agreement with the reference values. Recoveries from spiked CRM were in the ranges 97-105% (NO3--N), 95-103% (NH4+-N), 93-103% (urea-N), 99-108% (P), and 99-102% (K). The relative standard deviations (n = 12) for N, P, and K were 6, 4, and 2%, respectively.

  13. Solid sampling determination of total fluorine in baby food samples by high-resolution continuum source graphite furnace molecular absorption spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-11-15

    This study describes the applicability of solid sampling technique for the determination of fluorine in various baby foods via molecular absorption of calcium monofluoride generated in a graphite furnace of high-resolution continuum source atomic absorption spectrometry. Fluorine was determined at CaF wavelength, 606.440nm in a graphite tube applying a pyrolysis temperature of 1000°C and a molecule forming temperature of 2200°C. The limit of detection and characteristic mass of the method were 0.20ng and 0.17ng of fluorine, respectively. The fluorine concentrations determined in standard reference sample (bush branches and leaves) were in good agreement with the certified values. By applying the optimized parameters, the concentration of fluorine in various baby foods were determined. The fluorine concentrations were ranged from

  14. Determination and Uncertainty Analysis of Inorganic Arsenic in Husked Rice by Solid Phase Extraction and Atomic Absorption Spectrometry with Hydride Generation.

    Science.gov (United States)

    Saxena, Sushil Kumar; Karipalli, Agnes Raju; Krishnan, Anoop A; Rangasamy, Rajesh; Malekadi, Praveen; Singh, Dhirendra P; Vasu, Vimesh; Singh, Vijay K

    2017-05-01

    This study enables the selective determination of inorganic arsenic (iAs) with a low detection limit using an economical instrument [atomic absorption spectrometer with hydride generation (HG)] to meet the regulatory requirements as per European Commission (EC) and Codex guidelines. Dry rice samples (0.5 g) were diluted using 0.1 M HNO3-3% H2O2 and heated in a water bath (90 ± 2°C) for 60 min. Through this process, all the iAs is solubilized and oxidized to arsenate [As(V)]. The centrifuged extract was loaded onto a preconditioned and equilibrated strong anion-exchange SPE column (silica-based Strata SAX 500 mg/6 mL), followed by selective and sequential elution of As(V), enabling the selective quantification of iAs using atomic absorption spectrometry with HG. In-house validation showed a mean recovery of 94% and an LOQ of 0.025 mg/kg. The repeatability (HorRatr) and reproducibility (HorRatR) values were determination of iAs in husked rice samples and has potential applications in other food commodities.

  15. Determination of platinum and palladium in environmental samples by graphite furnace atomic absorption spectrometry after separation on dithizone sorbent.

    Science.gov (United States)

    Chwastowska, J; Skwara, W; Sterlińska, E; Pszonicki, L

    2004-09-08

    A graphite furnace atomic absorption method of platinum and palladium determination after their separation from environmental samples has been presented. The samples were digested by aqua regia and the analyte elements were separated on the dithizone sorbent. The procedure of sorbent preparation was described and their properties were established. Two various procedures of elution by thiourea and concentrated nitric acid were described and discussed. The low limit of detection was established as 1ngg(-1) for platinum and 0.2ngg(-1) for palladium. There was also investigated the behaviour of platinum and palladium introduced into the soil in various chemical forms.

  16. Determination of arsenic, antimony, and selenium in coal by atomic absorption spectrometry with a graphite tube atomizea

    Science.gov (United States)

    Aruscavage, Philip

    1977-01-01

    Submicrogram quantities of antimony, arsenic, and selenium in coal samples are determined by an atomic absorption procedure using an electrically heated graphite atomizer. The samples are decomposed in a mixture of nitric, sulfuric, and perchloric acids and are separated and concentrated by extraction from sulfuric acid-iodide solution into toluene. The results obtained on several intralaboratory reference samples and the National Bureau of Standards coal 1632 are compared with results from other methods. The determination can be made routinely for concentrations as small as 0.1 parts per million for arsenic, antimony, and selenium in the coal.

  17. Determination of total arsenic in fish by hydride-generation atomic absorption spectrometry: method validation, traceability and uncertainty evaluation

    Science.gov (United States)

    Nugraha, W. C.; Elishian, C.; Ketrin, R.

    2017-03-01

    Fish containing arsenic compound is one of the important indicators of arsenic contamination in water monitoring. The high level of arsenic in fish is due to absorption through food chain and accumulated in their habitat. Hydride generation (HG) coupled with atomic absorption spectrometric (AAS) detection is one of the most popular techniques employed for arsenic determination in a variety of matrices including fish. This study aimed to develop a method for the determination of total arsenic in fish by HG-AAS. The method for sample preparation from American of Analytical Chemistry (AOAC) Method 999.10-2005 was adopted for acid digestion using microwave digestion system and AOAC Method 986.15 - 2005 for dry ashing. The method was developed and validated using Certified Reference Material DORM 3 Fish Protein for trace metals for ensuring the accuracy and the traceability of the results. The sources of uncertainty of the method were also evaluated. By using the method, it was found that the total arsenic concentration in the fish was 45.6 ± 1.22 mg.Kg-1 with a coverage factor of equal to 2 at 95% of confidence level. Evaluation of uncertainty was highly influenced by the calibration curve. This result was also traceable to International Standard System through analysis of Certified Reference Material DORM 3 with 97.5% of recovery. In summary, it showed that method of preparation and HG-AAS technique for total arsenic determination in fish were valid and reliable.

  18. Determination of As(III) and As(V) by Flow Injection-Hydride Generation-Atomic Absorption Spectrometry via On-line Reduction of As(V) by KI

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Hansen, Elo Harald

    1997-01-01

    A volume-based flow injection (FI) procedure is described for the determination and speciation of trace inorganic arsenic, As(III) and As(V), via hydride generation-atomic absorption spectrometry (HG-AAS) of As(III). The determination of total arsenic is obtained by on-line reduction of As(V) to As...

  19. Improved limit of detection and quantitation development and validation procedure for quantification of zinc in Insulin by atomic absorption spectrometry.

    Science.gov (United States)

    Qadir, Muhammad Abdul; Ahmed, Mahmood; Haq, Iftikharul; Ahmed, Saghir

    2015-05-01

    A simple and expeditious analytical method for determination of zinc in human insulin isophane suspension by flame atomic absorption spectrophotometer (FAAS) was validated. The method was carried out on atomic absorption spectrometer with 0.4 nm bandwidth, 1.0 filter factor on deuterium (D2) background correction. The integration time was set at 3.0 second with 5.0 mA lamp current. The parameters of method validation showed adequate linearity, efficiency and relative standard deviation values were between 0.64%-1.69% (n=7), 1.31%-1.58% (n=10) for repeatability and intermediate precision respectively. The limit of detection 0.0032 μg/mL, 0.0173 μg/mL, 0.0231 μg/mL and limit of quantitation 0.0107μg/mL, 0.0578 μg/mL, 0.0694 μg/mL based on signal to noise (SN), calibration curve method (CCM) and fortification of blank (FB) were obtained respectively. The percentages of recovery for low, medium and high spiked concentration levels of zinc in human insulin were 99.38 ± 0.04 to 100.3 ± 0.03, 98.45 ± 0.38 to 100.3 ± 0.07 and 99.42 ± 0.03 to 99.42 ± 0.08 respectively. With the use of this method, five samples from each vial of human insulin isophane suspension were analyzed and the zinc content was determined. The zinc content were 22.1 ± 0.025 μg/mL and 24.3 ± 0.028 μg/mL which compliance the British Pharmacopoeia standard.

  20. Dithizone immobilized silica gel on-line preconcentration of trace copper with detection by flame atomic absorption spectrometry.

    Science.gov (United States)

    Yu, Hong-Mei; Song, Hua; Chen, Ming-Li

    2011-07-15

    A novel adsorbent-silica gel bound dithizone (H(2)Dz-SG) was prepared and used as solid-phase extraction of copper from complex matrix. The H(2)Dz-SG is investigated by means of FT-IR spectra and the SEM images, demonstrating the bonding of dithizone. The H(2)Dz-SG quantitatively adsorb copper ions, and the retained copper is afterwards collected by elution of 10% (v/v) nitric acid. An on-line flow injection solid-phase extraction procedure was developed for trace copper separation and preconcentration with detection by flame atomic spectrometry. By loading 5.4 mL of sample solution, a liner range of 0.5-120 μg L(-1), an enrichment factor of 42.6, a detection limit of 0.2 μg L(-1) and a precision of 1.7% RSD at the 40 μg L(-1) level (n=11) were obtained, along with a sampling frequency of 47 h(-1). The dynamic sorption capacity of H(2)Dz-SG to Cu(2+) was 0.76 mg g(-1). The accuracy of the proposed procedure was evaluated by determination of copper in reference water sample. The potential applications of the procedure for extraction of trace copper were successfully accomplished in water samples (tap, rain, snow, sea and river). The spiking recoveries within 91-107% are achieved. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Determination of some heavy metals in food and environmental samples by flame atomic absorption spectrometry after coprecipitation.

    Science.gov (United States)

    Soylak, Mustafa; Aydin, Ayse

    2011-06-01

    A novel preconcentration procedure based coprecipitation of Cu(II), Co(II), Cd(II), Ni(II), Mn(II), Fe(III) and Pb(II) on thulium hydroxide precipitate has been presented prior to flame atomic absorption spectrometric determination of them in environmental samples. The analytical parameters that influenced the quantitative coprecipitation of analytes including amount of thulium, pH, duration time, etc. were investigated. The effects of alkali, earth alkali, and some transition metals on the recoveries were also studied. Under the optimized conditions, the detection limits (3 sigma, N=10) for the analytes were in the range of 0.1-1.6 μg/L, respectively. The validation of the presented coprecipitation method was checked by the analysis of certified reference materials (TMDA 54.4 fortified lake water and HR-1 Humber river sediment). The proposed coprecipitation method has been successfully applied for the determination of traces of copper, cobalt, cadmium, nickel, manganese, iron and lead in food and environmental samples. Copyright © 2011 Elsevier Ltd. All rights reserved.

  2. Back-extraction of trace elements from organometallic-halide extracts for determination by flameless atomic absorption spectrometry

    Science.gov (United States)

    Clark, J.R.; Viets, J.G.

    1981-01-01

    The Methyl isobutyl ketone-Amine synerGistic Iodkte Complex (MAGIC) extraction system offers the advantage that a large number of trace elements can be rapidly determined with a single sample preparation procedure. However, many of the elements extracted by the MAGIC system form volatile organometallic halide salts when the organic extract is heated in the graphite furnace. High concentrations of some elements such as Cu and Zn extracted by the system from anomalous geological samples produce serious interferences when certain other elements are determined by flameless atomic absorption. Stripping systems have been developed using solutions of HNO3, H2SO4, and CH3COOH individually or combined with H2O2 in order to circumvent these problems. With these systems most of the elements in the organic extract can be sequentially stripped into an aqueous phase. Organometallic volatilization and the most serious interelement interferences, therefore, can be eliminated by stripping with various combinations of reagents in a series of steps.

  3. Radiocarbon dating of archaeological samples (sambaqui) using CO(2) absorption and liquid scintillation spectrometry of low background radiation.

    Science.gov (United States)

    Mendonça, Maria Lúcia T G; Godoy, José M; da Cruz, Rosana P; Perez, Rhoneds A R

    2006-01-01

    Sambaqui means, in the Tupi language, a hill of shells. The sambaquis are archaeological sites with remains of pre-historical Brazilian occupation. Since the sambaqui sites in the Rio de Janeiro state region are older than 10,000 years, the applicability of CO(2) absorption on Carbo-sorb and (14)C determination by counting on a low background liquid scintillation counter was tested. In the present work, sambaqui shells were treated with H(3)PO(4) in a closed vessel in order to generate CO(2). The produced CO(2) was absorbed on Carbo-sorb. On saturation about 0.6g of carbon, as CO(2), was mixed with commercial liquid scintillation cocktail (Permafluor), and the (14)C activity determined by counting on a low background counter, Packard Tricarb 3170 TR/SL, for a period of 1000 mins to enable detection of a radiocarbon age of 22,400 BP. But only samples with ages up to 3500 BP were submitted to the method because the samples had been collected in the municipality of Guapimirim, in archaeological sambaqui-type sites belonging to this age range. The same samples were sent to the (14)C Laboratory of the Centro de Energia Nuclear na Agricultura (CENA/USP) where similar results were obtained.

  4. A versatile microcomputer interface and peripheral devices: An application in deuterium lamp background correction graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Gökmen, A.; Yalcin, S.

    1992-01-01

    A versatile interface card for Apple IIe computer and various peripheral devices are designed to control instruments which generates transient signals like in graphite furnace atomic spectrometer. The interface card consists of a multiplexed analog-to-digital converter, a digital-to-analog converter, and a timer/counter chip. The timer/counter chip with 16 built-in registers can be programmed in many modes which provides a time base for real-time measurements. A stepper motor runs under the control of timer/counter chip independent of computer. A light chopper connected to the stepper motor is controlled easily by computer. A dual high-voltage switch can modulate dc light sources under computer control. This system is applied to D2-lamp background correction graphite furnace atomic absorption spectrometer. The D2 lamp is chopped by a mechanical chopper driven by a stepper motor and a hollow cathode lamp is modulated electronically. The data acquisition program is written in machine language and synchronization between light sources and computer is provided by chopper position signal through the interrupts. A sampling rate of 16 during a signal period at 50-Hz chopping frequency is found to be the optimum value. A large number of data collected during atomization period is compressed in machine code. This saved storage space and analysis time.

  5. Radiocarbon dating of archaeological samples (sambaqui) using CO{sub 2} absorption and liquid scintillation spectrometry of low background radiation

    Energy Technology Data Exchange (ETDEWEB)

    Mendonca, Maria Lucia T.G. [Department of Chemistry, Pontificia Universidade Catolica does Rio de Janeiro, Rua Marques de Sao Vicente 225, Gavea, Rio de Janeiro, RJ, CEP 22453-900 (Brazil)]. E-mail: luguerra@uol.com.br; Godoy, Jose M. [Department of Chemistry, Pontificia Universidade Catolica does Rio de Janeiro, Rua Marques de Sao Vicente 225, Gavea, Rio de Janeiro, RJ, CEP 22453-900 (Brazil); Instituto de Radioprotecao e Dosimetria, Comissao Nacional de Energia Nuclera, Caixa Postal 37750, Barra da Tijuca, Rio de Janeiro, RJ, CEP 22642-970 (Brazil); Cruz, Rosana P. da [Department of Chemistry, Pontificia Universidade Catolica does Rio de Janeiro, Rua Marques de Sao Vicente 225, Gavea, Rio de Janeiro, RJ, CEP 22453-900 (Brazil); Perez, Rhoneds A.R. [Museology Sector, National Museum, Federal University of Rio de Janeiro, Quinta da Boa Vista, s/no, Sao Cristovao, Rio de Janeiro, RJ, CEP 20940-040 (Brazil)

    2006-07-01

    Sambaqui means, in the Tupi language, a hill of shells. The sambaquis are archaeological sites with remains of pre-historical Brazilian occupation. Since the sambaqui sites in the Rio de Janeiro state region are older than 10,000 years, the applicability of CO{sub 2} absorption on Carbo-sorb[reg] and {sup 14}C determination by counting on a low background liquid scintillation counter was tested. In the present work, sambaqui shells were treated with H{sub 3}PO{sub 4} in a closed vessel in order to generate CO{sub 2}. The produced CO{sub 2} was absorbed on Carbo-sorb[reg]. On saturation about 0.6 g of carbon, as CO{sub 2}, was mixed with commercial liquid scintillation cocktail (Permafluor[reg]), and the {sup 14}C activity determined by counting on a low background counter, Packard Tricarb 3170 TR/SL, for a period of 1000 mins to enable detection of a radiocarbon age of 22,400 BP. But only samples with ages up to 3500 BP were submitted to the method because the samples had been collected in the municipality of Guapimirim, in archaeological sambaqui-type sites belonging to this age range. The same samples were sent to the {sup 14}C Laboratory of the Centro de Energia Nuclear na Agricultura (CENA/USP) where similar results were obtained.

  6. A simple and fast method for assessment of the nitrogen–phosphorus–potassium rating of fertilizers using high-resolution continuum source atomic and molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bechlin, Marcos André; Fortunato, Felipe Manfroi; Moutinho da Silva, Ricardo; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta, E-mail: anchieta@iq.unesp.br

    2014-11-01

    The determination of N, P, and K in fertilizers by high-resolution continuum source flame atomic and molecular absorption spectrometry is proposed. Under optimized conditions, measurements of the diatomic molecules NO and PO at 215.360 and 247.620 nm, respectively, and K using the wing of the alternative line at 404.722 nm allowed calibration curves to be constructed in the ranges 500–5000 mg L{sup −1} N (r = 0.9994), 100–2000 mg L{sup −1} P (r = 0.9946), and 100–2500 mg L{sup −1} K (r = 0.9995). Commercial fertilizers were analyzed by the proposed method and the concentrations of N, P, and K were found to be in agreement with those obtained by Kjeldahl, spectrophotometric, and flame atomic emission spectrometry methods, respectively, at a 95% confidence level (paired t-test). A phosphate rock certified reference material (CRM) was analyzed and the results for P and K were in agreement with the reference values. Recoveries from spiked CRM were in the ranges 97–105% (NO{sub 3}{sup −}-N), 95–103% (NH{sub 4}{sup +}-N), 93–103% (urea-N), 99–108% (P), and 99–102% (K). The relative standard deviations (n = 12) for N, P, and K were 6, 4, and 2%, respectively. - Highlights: • A single technique is proposed to analyze NPK fertilizer. • HR-CS FAAS is proposed for the first time for N, P and K determination in fertilizers. • The method employs the same sample preparation and dilution for the three analytes. • Addition of H{sub 2}O{sub 2} allows analysis of fertilizers with different nitrogen species. • Proposal provides advantages over traditional methods in terms of cost and time.

  7. Crosslinked poly (4-vinylpyridine-ethylene glycol dimethacrylate) used for preconcentration of Cd(II) and its determination by flow injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Tarley, César Ricardo Teixeira; Farias, Natália Cristina Botteon; Lima, Giovana de Fátima; de Oliveira, Fernanda Midori; Bonfílio, Rudy; Dragunski, Douglas Cardoso; Clausen, Débora Nobile; Segatelli, Mariana Gava

    2014-01-01

    The main purpose of this research was to synthesize crosslinked poly(4-vinylpyridine-ethylene glycol dimethacrylate) and evaluate its feasibility for highly sensitive and selective determination of Cd in water samples by using flow injection flame atomic absorption spectrometry. The crosslinked polymer, prepared by bulk polymerization, was characterized by FTIR spectrometry and scanning electron microscopy. The flow injection solid-phase method was based on preconcentration of 20.0 mL of sample through 100 mg of the polymer packed into a minicolumn at pH 8.25 using a flow rate of 6.0 mL/min, followed by elution with 1.0 M HNO3. The sample solution parameters influencing the preconcentration behavior of Cd ions, such as pH, buffer concentration, and flow rate, were simultaneously studied and optimized using a Doehlert matrix. Values of 0.10 microg/L, 2.0-210 microg/L, 32.3, 18/h, 9.7/min, and 0.62 mL were obtained for LOD, linear range, preconcentration factor, sample throughput, concentration efficiency, and consumption index, respectively. The effect of the presence of the inorganic cations Pb(II), U(IV), Co(II), Hg(II), Cu(II), As(II), Mg(II), Sb(III), Ni(II), Th(IV), Ba(II), and Ca(II) on the method was studied, and the preconcentration of Cd was observed to have no interference. The accuracy of the method was assessed by analysis of natural water samples using addition and recovery tests and inductively coupled plasma/MS as a reference technique, as well as by analysis of a standard reference material of trace elements in water.

  8. On-line electrochemically controlled in-tube solid phase microextraction of inorganic selenium followed by hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of); Shamsayei, Maryam; Safari, Meysam; Rezaei, Fatemeh [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

    2016-05-30

    In this work, for the first time, a rapid, simple and sensitive microextraction procedure is demonstrated for the matrix separation, preconcentration and determination of inorganic selenium species in water samples using an electrochemically controlled in-tube solid phase microextraction (EC-in-tube SPME) followed by hydride generation atomic absorption spectrometry (HG-AAS). In this approach, in which EC-in-tube SPME and HG-AAS system were combined, the total analysis time, was decreased and the accuracy, repeatability and sensitivity were increased. In addition, to increases extraction efficiency, a novel nanostructured composite coating consisting of polypyrrole (PPy) doped with ethyleneglycol dimethacrylate (EGDMA) was prepared on the inner surface of a stainless-steel tube by a facile electrodeposition method. To evaluate the offered setup and the new PPy-EGDMA coating, it was used to extract inorganic selenium species in water samples. Extraction of inorganic selenium species was carried out by applying a positive potential through the inner surface of coated in-tube under flow conditions. Under the optimized conditions, selenium was detected in amounts as small as 4.0 parts per trillion. The method showed good linearity in the range of 0.012–200 ng mL{sup −1}, with coefficients of determination better than 0.9996. The intra- and inter-assay precisions (RSD%, n = 5) were in the range of 2.0–2.5% and 2.7–3.2%, respectively. The validated method was successfully applied for the analysis of inorganic selenium species in some water samples and satisfactory results were obtained. - Graphical abstract: An electrochemically controlled in-tube solid phase microextraction followed by hydride generation atomic absorption spectrometry was developed for extraction and determination ultra-trace amounts of Se in aqueous solutions. - Highlights: • A nanostructured composite coating consisting of PPy doped with EGDMA was prepared. • The coating was

  9. In situ emulsification microextraction using a dicationic ionic liquid followed by magnetic assisted physisorption for determination of lead prior to micro-sampling flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shokri, Masood; Beiraghi, Asadollah [Faculty of Chemistry, Kharazmi University, Tehran (Iran, Islamic Republic of); Seidi, Shahram, E-mail: s.seidi@kntu.ac.ir [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of)

    2015-08-19

    For the first time, a simple and efficient in situ emulsification microextraction method using a dicationic ionic liquid followed by magnetic assisted physisorption was presented to determine trace amounts of lead. In this method, 400 μL of 1.0 mol L{sup −1} lithium bis (trifluoromethylsulfonyl) imide aqueous solution, Li[NTf{sub 2}], was added into the sample solution containing 100 μL of 1.0 mol L{sup −1} 1,3-(propyl-1,3-diyl) bis (3-methylimidazolium) chloride, [pbmim]Cl{sub 2}, to form a water immiscible ionic liquid, [pbmim][NTf{sub 2}]{sub 2}. This new in situ formed dicationic ionic liquid was applied as the acceptor phase to extract the lead-ammonium pyrrolidinedithiocarbamate (Pb-APDC) complexes from the sample solution. Subsequently, 30 mg of Fe{sub 3}O{sub 4} magnetic nanoparticles (MNPs) were added into the sample solution to collect the fine droplets of [pbmim][NTf{sub 2}]{sub 2}, physisorptively. Finally, MNPs were eluted by acetonitrile, separated by an external magnetic field and the obtained eluent was subjected to micro-sampling flame atomic absorption spectrometry (FAAS) for further analysis. Comparing with other microextraction methods, no special devices and centrifugation step are required. Parameters influencing the extraction efficiency such as extraction time, pH, concentration of chelating agent, amount of MNPs and coexisting interferences were studied. Under the optimized conditions, this method showed high extraction recovery of 93% with low LOD of 0.7 μg L{sup −1}. Good linearity was obtained in the range of 2.5–150 μg L{sup −1} with determination coefficient (r{sup 2}) of 0.9921. Relative standard deviation (RSD%) for seven repeated measurements at the concentration of 10 μg L{sup −1} was 4.1%. Finally, this method was successfully applied for determination of lead in some water and plant samples. - Highlights: • A dicationic ionic liquid was used as the extraction solvent, for the first time. • A

  10. Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Nomura, Cassiana S.; Silva, Cíntia S.; Nogueira, Ana R. A.; Oliveira, Pedro V.

    2005-06-01

    This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 °C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 °C and 2300 °C for Cu, and 700 °C and 1700 °C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 μg of W + 200 μg of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg - 1 and 128 mg kg - 1, respectively. The relative standard deviations were lower than 6% ( n = 5). The accuracy of the entire

  11. Investigation of spectral interferences in the determination of lead in fertilizers and limestone samples using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; François, Luciane L.; Jesus, Alexandre de [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2014-11-01

    In the present work, spectral interferences on the determination of lead in fertilizer and limestone samples were investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry at the main analytical lines: 217.001 and 283.306 nm. For these investigations, samples were introduced into the furnace as slurry together with a mixture of Pd and Mg as chemical modifier. Spectral interferences were observed for some samples at both analytical lines. In order to verify whether a wet digestion procedure would avoid these interferences, a reference method for wet digestion of fertilizers was employed as an alternative sample preparation procedure. However, the same interferences were also observed in the digested samples. In order to identify and eliminate the fine-structured background using a least-squares background correction, reference spectra were generated using the combination of different species. The use of the latter technique allowed the elimination of spectral interferences for most of the investigated samples, making possible the determination of lead in fertilizer and limestone samples free of interferences. The best results were found using a reference spectrum of NH{sub 4}H{sub 2}PO{sub 4} at 217.001 nm, and a mixture of H{sub 2}SO{sub 4} + Ca and HNO{sub 3} + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material “Trace Elements in Multi-Nutrient Fertilizer”. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part. - Highlights: • Spectral interferences on the determination of lead in fertilizers and limestone. • The analytical lines at 217.001 nm and 283.306 nm using HR-CS GF AAS. • Various combinations of compounds were used to create reference spectra. • LSBC

  12. Quantifying uncertainty in the measurement of arsenic in suspended particulate matter by Atomic Absorption Spectrometry with hydride generator

    Directory of Open Access Journals (Sweden)

    Ahuja Tarushee

    2011-04-01

    Full Text Available Abstract Arsenic is the toxic element, which creates several problems in human being specially when inhaled through air. So the accurate and precise measurement of arsenic in suspended particulate matter (SPM is of prime importance as it gives information about the level of toxicity in the environment, and preventive measures could be taken in the effective areas. Quality assurance is equally important in the measurement of arsenic in SPM samples before making any decision. The quality and reliability of the data of such volatile elements depends upon the measurement of uncertainty of each step involved from sampling to analysis. The analytical results quantifying uncertainty gives a measure of the confidence level of the concerned laboratory. So the main objective of this study was to determine arsenic content in SPM samples with uncertainty budget and to find out various potential sources of uncertainty, which affects the results. Keeping these facts, we have selected seven diverse sites of Delhi (National Capital of India for quantification of arsenic content in SPM samples with uncertainty budget following sampling by HVS to analysis by Atomic Absorption Spectrometer-Hydride Generator (AAS-HG. In the measurement of arsenic in SPM samples so many steps are involved from sampling to final result and we have considered various potential sources of uncertainties. The calculation of uncertainty is based on ISO/IEC17025: 2005 document and EURACHEM guideline. It has been found that the final results mostly depend on the uncertainty in measurement mainly due to repeatability, final volume prepared for analysis, weighing balance and sampling by HVS. After the analysis of data of seven diverse sites of Delhi, it has been concluded that during the period from 31st Jan. 2008 to 7th Feb. 2008 the arsenic concentration varies from 1.44 ± 0.25 to 5.58 ± 0.55 ng/m3 with 95% confidence level (k = 2.

  13. Fast sequential multi-element determination of major and minor elements in environmental samples and drinking waters by high-resolution continuum source flame atomic absorption spectrometry.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Ma Jesús; Sevilla, Ma Teresa; Procopio, Jesús R

    2015-01-07

    The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88-115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8-9 mL of sample. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Simultaneous determination of Cd and Fe in grain products using direct solid sampling and high-resolution continuum source electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    dos Santos, Lisia M G; Araujo, Rennan G O; Welz, Bernhard; Jacob, Silvana do C; Vale, Maria Goreti R; Becker-Ross, Helmut

    2009-04-30

    Cadmium and iron are antagonistic elements in the sense that they produce different effects in the human body. Both elements have to be determined routinely in grain products, cadmium because of its toxicity, and iron because all grain products, according to Brazilian law, have to contain a minimum of 42 mg kg(-1) Fe to combat anemia. A routine screening method has been developed for the quasi simultaneous determination of cadmium and iron using high-resolution continuum source electrothermal atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for Cd, and an adjacent secondary line at 228.726 nm for the determination of Fe. Various chemical modifiers have been investigated, and a mixture of tungsten and iridium, applied as a permanent modifier, showed the best performance; it stabilized Cd up to a pyrolysis temperature of 700 degrees C and did not over-stabilize Fe. Two atomization temperatures were used sequentially, 1700 degrees C for Cd and 2600 degrees C for Fe, because of their significantly different volatilities. The characteristic masses obtained were 0.9 pg for Cd and 1.2 ng for Fe. The limits of detection (3 sigma, n=10) were 0.6 microg kg(-1) for Cd and 0.5 mg kg(-1) for Fe. The relative standard deviation ranged from 3 to 7% for Cd and from 4 to 13% for Fe, which is satisfactory for the purpose. The accuracy of the method was confirmed by the analysis of three certified reference materials; the results were in agreement with the certified values at a 95% confidence interval. The Cd content in the investigated grain products was between 0.9 and 10.5 microg kg(-1), but most of them did not contain the required minimum amount of iron.

  15. Determination of mercury in airborne particulate matter collected on glass fiber filters using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling

    Energy Technology Data Exchange (ETDEWEB)

    Araujo, Rennan G.O., E-mail: rgoa01@terra.com.br [Laboratorio de Quimica Analitica Ambiental, Departamento de Quimica, Universidade Federal de Sergipe, Campus Sao Cristovao, 49.100-000, Sao Cristovao, SE (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Vignola, Fabiola; Castilho, Ivan N.B. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borges, Daniel L.G.; Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Vale, Maria Goreti R. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal do Rio Grande do Sul, 91501-970 Porto Alegre, RS (Brazil); Smichowski, Patricia [Comision Nacional de Energia Atomica (CNEA) and Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Buenos Aires (Argentina); Ferreira, Sergio L.C. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal da Bahia, 40170-290, Salvador, BA (Brazil); Becker-Ross, Helmut [Leibniz-Institut fuer Analytische Wissenschaften-ISAS-e.V., Department Berlin, 12489 Berlin (Germany)

    2011-05-15

    A study has been undertaken to assess the capability of high-resolution continuum source graphite furnace atomic absorption spectrometry for the determination of mercury in airborne particulate matter (APM) collected on glass fiber filters using direct solid sampling. The main Hg absorption line at 253.652 nm was used for all determinations. The certified reference material NIST SRM 1648 (Urban Particulate Matter) was used to check the accuracy of the method, and good agreement was obtained between published and determined values. The characteristic mass was 22 pg Hg. The limit of detection (3{sigma}), based on ten atomizations of an unexposed filter, was 40 ng g{sup -1}, corresponding to 0.12 ng m{sup -3} in the air for a typical air volume of 1440 m{sup 3} collected within 24 h. The limit of quantification was 150 ng g{sup -1}, equivalent to 0.41 ng m{sup -3} in the air. The repeatability of measurements was better than 17% RSD (n = 5). Mercury concentrations found in filter samples loaded with APM collected in Buenos Aires, Argentina, were between < 40 ng g{sup -1} and 381 {+-} 24 ng g{sup -1}. These values correspond to a mercury concentration in the air between < 0.12 ng m{sup -3} and 1.47 {+-} 0.09 ng m{sup -3}. The proposed procedure was found to be simple, fast and reliable, and suitable as a screening procedure for the determination of mercury in APM samples.

  16. Peat as a natural solid-phase for copper preconcentration and determination in a multicommuted flow system coupled to flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gonzales, A.P.S. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil); Firmino, M.A. [Departamento de Engenharia de Materiais, Escola de Engenharia, Universidade Presbiteriana Mackenzie, Rua da Consolacao, 930, 01302-970 Sao Paulo (Brazil); Nomura, C.S. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil); Rocha, F.R.P.; Oliveira, P.V. [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 748, 05508-000 Sao Paulo (Brazil); Gaubeur, I. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil)], E-mail: ivanise.gaubeur@ufabc.edu.br

    2009-03-23

    The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 mol L{sup -1} HNO{sub 3}. The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 {mu}g L{sup -1}, with a detection limit estimated as 3 {mu}g L{sup -1} at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n = 20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111% range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level.

  17. Validation of an analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals in soil.

    Science.gov (United States)

    Frentiu, Tiberiu; Ponta, Michaela; Hategan, Raluca

    2013-03-01

    The aim of this paper was the validation of a new analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals (Ag, Cd, Co, Cr, Cu, Ni, Pb and Zn) in soil after microwave assisted digestion in aqua regia. Determinations were performed on the ContrAA 300 (Analytik Jena) air-acetylene flame spectrometer equipped with xenon short-arc lamp as a continuum radiation source for all elements, double monochromator consisting of a prism pre-monocromator and an echelle grating monochromator, and charge coupled device as detector. For validation a method-performance study was conducted involving the establishment of the analytical performance of the new method (limits of detection and quantification, precision and accuracy). Moreover, the Bland and Altman statistical method was used in analyzing the agreement between the proposed assay and inductively coupled plasma optical emission spectrometry as standardized method for the multielemental determination in soil. The limits of detection in soil sample (3σ criterion) in the high-resolution continuum source flame atomic absorption spectrometry method were (mg/kg): 0.18 (Ag), 0.14 (Cd), 0.36 (Co), 0.25 (Cr), 0.09 (Cu), 1.0 (Ni), 1.4 (Pb) and 0.18 (Zn), close to those in inductively coupled plasma optical emission spectrometry: 0.12 (Ag), 0.05 (Cd), 0.15 (Co), 1.4 (Cr), 0.15 (Cu), 2.5 (Ni), 2.5 (Pb) and 0.04 (Zn). Accuracy was checked by analyzing 4 certified reference materials and a good agreement for 95% confidence interval was found in both methods, with recoveries in the range of 94-106% in atomic absorption and 97-103% in optical emission. Repeatability found by analyzing real soil samples was in the range 1.6-5.2% in atomic absorption, similar with that of 1.9-6.1% in optical emission spectrometry. The Bland and Altman method showed no statistical significant difference between the two spectrometric

  18. Magnetic stirrer induced dispersive ionic-liquid microextraction for the determination of vanadium in water and food samples prior to graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa

    2015-04-01

    A new dispersive liquid-liquid microextraction, magnetic stirrer induced dispersive ionic-liquid microextraction (MS-IL-DLLME) was developed to quantify the trace level of vanadium in real water and food samples by graphite furnace atomic absorption spectrometry (GFAAS). In this extraction method magnetic stirrer was applied to obtained a dispersive medium of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] in aqueous solution of (real water samples and digested food samples) to increase phase transfer ratio, which significantly enhance the recovery of vanadium - 4-(2-pyridylazo) resorcinol (PAR) chelate. Variables having vital role on desired microextraction methods were optimised to obtain the maximum recovery of study analyte. Under the optimised experimental variables, enhancement factor (EF) and limit of detection (LOD) were achieved to be 125 and 18 ng L(-1), respectively. Validity and accuracy of the desired method was checked by analysis of certified reference materials (SLRS-4 Riverine water and NIST SRM 1515 Apple leaves). The relative standard deviation (RSD) for 10 replicate determinations at 0.5 μg L(-1) of vanadium level was found to be <5.0%. This method was successfully applied to real water and acid digested food samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

  19. Automatic On-line Solid-phase Extraction-Electrothermal Atomic Absorption Spectrometry Exploiting Sequential Injection Analysis for Trace Vanadium, Cadmium and Lead Determination in Human Urine Samples.

    Science.gov (United States)

    Giakisikli, Georgia; Ayala Quezada, Alejandro; Tanaka, Junpei; Anthemidis, Aristidis N; Murakami, Hiroya; Teshima, Norio; Sakai, Tadao

    2015-01-01

    A fully automated sequential injection column preconcentration method for the on-line determination of trace vanadium, cadmium and lead in urine samples was successfully developed, utilizing electrothermal atomic absorption spectrometry (ETAAS). Polyamino-polycarboxylic acid chelating resin (Nobias chelate PA-1) packed into a handmade minicolumn was used as a sorbent material. Effective on-line retention of chelate complexes of analytes was achieved at pH 6.0, while the highest elution effectiveness was observed with 1.0 mol L(-1) HNO3 in the reverse phase. Several analytical parameters, like the sample acidity, concentration and volume of the eluent as well as the loading/elution flow rates, have been studied, regarding the efficiency of the method, providing appropriate conditions for the analysis of real samples. For a 4.5 mL sample volume, the sampling frequency was 27 h(-1). The detection limits were found to be 3.0, 0.06 and 2.0 ng L(-1) for V(V), Cd(II) and Pb(II), respectively, with the relative standard deviations ranging between 1.9 - 3.7%. The accuracy of the proposed method was evaluated by analyzing a certified reference material (Seronorm(TM) trace elements urine) and spiked urine samples.

  20. Separation/preconcentration and determination of vanadium with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) and electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Asadollahi, Tahereh; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

    2010-06-30

    A novel dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for separation/preconcentration of ultra trace amount of vanadium and its determination with the electrothermal atomic absorption spectrometry (ETAAS) was developed. The DLLME-SFO behavior of vanadium (V) using N-benzoyl-N-phenylhydroxylamine (BPHA) as complexing agent was systematically investigated. The factors influencing the complex formation and extraction by DLLME-SFO method were optimized. Under the optimized conditions: 100 microL, 200 microL and 25 mL of extraction solvent (1-undecanol), disperser solvent (acetone) and sample volume, respectively, an enrichment factor of 184, a detection limit (based on 3S(b)/m) of 7 ng L(-1) and a relative standard deviation of 4.6% (at 500 ng L(-1)) were obtained. The calibration graph using the preconcentration system for vanadium was linear from 20 to 1000 ng L(-1) with a correlation coefficient of 0.9996. The method was successfully applied for the determination of vanadium in water and parsley. Copyright 2010 Elsevier B.V. All rights reserved.

  1. Use of factorial design and Doehlert matrix for multivariate optimisation of an on-line preconcentration system for lead determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Ferreira, S L C; dos Santos, W N L; Bezerra, M A; Lemos, V A; Bosque-Sendra, J M

    2003-02-01

    A system for on-line preconcentration and determination of lead by flame atomic absorption spectrometry (FAAS) was proposed. It was based on the sorption of lead(II) ions on a minicolumn of polyurethane foam loaded with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM). The optimisation step was carried out using two-level full factorial and Doehlert designs for the determination of the optimum conditions for lead preconcentration. The proposed procedure allowed the determination of lead with a detection limit of 2.2 microg L(-1), and a precision, calculated as relative standard deviation (RSD), of 2.4 and 6.8 for a lead concentration of 50.0 and 10.0 microg L(-1), respectively. A preconcentration factor of 45 and a sampling frequency of 27 samples per hour were obtained. The recovery achieved for lead determination in the presence of several cations demonstrated that this procedure has enough selectivity for analysis of environmental samples. The validation was carried out by analysis of certified reference material. This procedure was applied to lead determination in natural food.

  2. Determination of total chromium at ultratrace levels in water and soil samples by coprecipitation microsample injection system flame atomic absorption spectrometry.

    Science.gov (United States)

    Baig, Jameel Ahmed; Elci, Latif; Khan, Muhammad Irfan; Kazi, Tasneem Gul

    2014-01-01

    A simple, robust, and novel analytical procedure was developed for determination of total chromium (Cr) by carrier element coprecipitation (CECP) coupled microsample injection system with flame atomic absorption spectrometry. For this method, Cr(III) was oxidized by Ce(SO4)2 in acidic media, and the resulting solution formed coprecipitates with ammonium pyrrolidine dithiocarbamate in the presence of Ce(III). The effective parameters of the developed method have been optimized and studied in detail. The LOD and enrichment factor of CECP were 2.13 μg/L and 100 ± 2.8, respectively, with 40 mL initial volumes. The RSD values (n = 6) were 96%). The accuracy of total Cr by CECP after microwave acid digestion was checked by using a certified reference material (GBW 07309 Stream Sediment). The difference between the found and certified values was not significant (P > 0.05). The proposed method was successfully applied to natural drinking water, industrial effluent wastewater, and the exchangeable fraction of garden soil from Denizli, Turkey.

  3. Speciation of Mn(II), Mn(VII) and total manganese in water and food samples by coprecipitation-atomic absorption spectrometry combination.

    Science.gov (United States)

    Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

    2010-01-15

    A speciation procedure based on the coprecipitation of manganese(II) with zirconium(IV) hydroxide has been developed for the investigation of levels of manganese species. The determination of manganese levels was performed by flame atomic absorption spectrometry (FAAS). Total manganese was determined after the reduction of Mn(VII) to Mn(II) by ascorbic acid. The analytical parameters including pH, amount of zirconium(IV), sample volume, etc., were investigated for the quantitative recoveries of manganese(II). The effects of matrix ions were also examined. The recoveries for manganese(II) were in the range of 95-98%. Preconcentration factor was calculated as 50. The detection limit for the analyte ions based on 3 sigma (n=21) was 0.75 microg L(-1) for Mn(II). The relative standard deviation was found to be lower than 7%. The validation of the presented procedure was performed by analysis of certified reference material having different matrices, NIST SRM 1515 (Apple Leaves) and NIST SRM 1568a (Rice Flour). The procedure was successfully applied to natural waters and food samples.

  4. Ultrasound-assisted emulsification-microextraction combined with graphite furnace atomic absorption spectrometry for the determination of trace lead in water

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Hongmei; Zhang, Yu; Qiu, Bocheng; Li, Wenhua [College of Science, Nanjing Agricultural University, Nan Jing (China)

    2012-04-15

    The ultrasound-assisted emulsification-microextraction (USAEME) method was combined with graphite furnace atomic absorption spectrometry (GFAAS) for the determination of trace Pb using dithizone (H{sup 2}DZ) as chelating reagent. Some effective parameters influenced the detection and microextraction, such as ashing temperature and atomization temperature, pH, extraction solvent, sample volume, extraction time, and extraction temperature were selected and optimized. After extraction, the calibration curves for Pb was in the concentration range of 0.1-10 ng mL{sup -1}, and the linear equation was y = 0.097 x + 0.023 (R = 0.99). Under the optimized conditions, the detection limit of the method was 20 pg mL{sup -1} with an enrichment factor of 70 and the relative standards deviation (RSD) for seven determinations of 1 ng mL{sup -1} Pb was 11%. The proposed method was successfully applied to determine trace Pb in Yueya Lake water, pond water, and spiked samples. Furthermore, a certified reference material of Environment Water (GBW08607) was analyzed and the determined value was in good agreement with the certified value, which showed the accuracy, recovery, and applicability of the reported method. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  5. Sensitive determination of bismuth by flame atomic absorption spectrometry using atom trapping in a slotted quartz tube and revolatilization with organic solvent pulse

    Science.gov (United States)

    Kılınç, Ersin; Bakırdere, Sezgin; Aydın, Fırat; Ataman, O. Yavuz

    2012-07-01

    Sensitivity of flame atomic absorption spectrometry (FAAS) for Bi determination was improved by slotted quartz tube (SQT) that was used also for atom trapping (AT). The trapped analyte was released by aspirating a small volume of organic solvent after a reasonable analyte collection time. Sensitivity was improved by 2.9 times by SQT-FAAS and 256 times by SQT-AT-FAAS with respect to FAAS. Optimum trapping period was found to be 6.0 min (36.0 mL of solution). Limit of detection (LOD) for SQT-AT-FAAS was found to be 1.6 ng mL- 1. %RSD was calculated as 4.0% for five replicate measurements of 7.5 ng mL- 1 Bi by SQT-AT-FAAS. Accuracy of the method developed was checked by analyzing a standard reference material of simulated fresh water (NIST 1643e) and result found was in good agreement with the certified one. The method can be applied in any laboratory equipped with a flame AA spectrometer. The consumption of time and sample volume is fairly low and application is simple and easy.

  6. Fast arsenic speciation in water by on-site solid phase extraction and high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Mihucz, Victor G.; Bencs, László; Koncz, Kornél; Tatár, Enikő; Weiszburg, Tamás; Záray, Gyula

    2017-02-01

    A method of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS), combined with on-site separation/solid phase extraction (SPE) has been developed for the speciation of inorganic As (iAs) in geothermal and drinking water samples. The HR-CS-GFAAS calibration curves were linear up to 200 μg/L As, but using second order polynomial fitting, accurate calibration could be performed up to 500 μg/L. It has been demonstrated that sample pH should not be higher than 8 for an accurate speciation of As(V) with a recovery of ≈ 95%. Geothermal water had fairly high salt content (≈ 2200 mg/L) due to the presence of chlorides and sulfates at mg/L levels. Therefore, a two-fold dilution of these types of samples before SPE is recommended, especially, for total As determinations, when the As concentration is as high as 400 μg/L. For drinking water, sampled from public wells with records of As concentrations higher than the 10 μg/L in the past, the reduction of As contamination below the WHO's health limit value could be observed. However, the electrical conductivity was close to 2500 μS/cm, i.e., the guideline limit for drinking water, which was due to their higher chloride content. The proposed fit-for-purpose SPE-HR-CS-GFAAS method could be a candidate for screening drinking water quality.

  7. Accuracy of a method based on atomic absorption spectrometry to determine inorganic arsenic in food: Outcome of the collaborative trial IMEP-41.

    Science.gov (United States)

    Fiamegkos, I; Cordeiro, F; Robouch, P; Vélez, D; Devesa, V; Raber, G; Sloth, J J; Rasmussen, R R; Llorente-Mirandes, T; Lopez-Sanchez, J F; Rubio, R; Cubadda, F; D'Amato, M; Feldmann, J; Raab, A; Emteborg, H; de la Calle, M B

    2016-12-15

    A collaborative trial was conducted to determine the performance characteristics of an analytical method for the quantification of inorganic arsenic (iAs) in food. The method is based on (i) solubilisation of the protein matrix with concentrated hydrochloric acid to denature proteins and allow the release of all arsenic species into solution, and (ii) subsequent extraction of the inorganic arsenic present in the acid medium using chloroform followed by back-extraction to acidic medium. The final detection and quantification is done by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS). The seven test items used in this exercise were reference materials covering a broad range of matrices: mussels, cabbage, seaweed (hijiki), fish protein, rice, wheat, mushrooms, with concentrations ranging from 0.074 to 7.55mgkg(-1). The relative standard deviation for repeatability (RSDr) ranged from 4.1 to 10.3%, while the relative standard deviation for reproducibility (RSDR) ranged from 6.1 to 22.8%. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

  8. Separation and Enrichment of Gold in Water, Geological and Environmental Samples by Solid Phase Extraction on Multiwalled Carbon Nanotubes Prior to its Determination by Flame Atomic Absorption Spectrometry.

    Science.gov (United States)

    Duran, Ali; Tuzen, Mustafa; Soylak, Mustafa

    2015-01-01

    This study proposes the application of multi-walled carbon nanotubes as a solid sorbent for the preconcentration of gold prior to its flame atomic absorption spectrometry determination. Extraction was achieved by using a glass column (15.0 cm in length and 1.0 cm in diameter). Quantitative recoveries were obtained in the pH range of 2.5-4.0; the elution step was carried out with 5.0 ml of 1.0 mol/L HNO3 in acetone. In the ligand-free study, variables such as pH, eluent type, sample volume, flow rates, and matrix effect were examined for the optimum recovery of gold ions. The gold ions were able to be pre-concentrated by a factor of 150 and their LOD was determined to be 1.71 μg/L. In order to evaluate the accuracy of the developed method, addition-recovery tests were applied for the tap water, mineral water, and sea water samples. Gold recovery studies were implemented using a wet digestion technique for mine and soil samples taken from various media, and this method was also applied for anodic slime samples taken from the factories located in the Kayseri Industrial Zone of Turkey.

  9. Trace mercury determination in drinking and natural water after preconcentration and separation by DLLME-SFO method coupled with cold vapor atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Abdollahi Atousa

    2014-07-01

    Full Text Available A novel dispersive liquid–liquid microextraction based on solidification of floating organic drop (DLLME-SFO for simultaneous separation/preconcentration of ultra trace amounts of mercury was used. A method based on amalgamation was used for collection of gaseous mercury on gold coated sand (Gold trap. The concentration of mercury was determined by cold vapor atomic absorption spectrometry (CV-AAS. The DLLME-SFO behavior of mercury by using dithizone as complexing agent was systematically investigated. The factors influencing, the complex formation and extraction of DLLME-SFO method such as type and volume of extraction and disperser solvents, pH, concentration of salt, centrifuging time and concentration of the chelating agent were optimized. The method was successfully applied to the determination of mercury in drinking and natural water and satisfactory relative recoveries (95–105% were achieved. The proposed procedure was based on very low consumption of organic solvents. The other benefits of the system were sensitive, simple, friendly to the environment, rejection of matrix constituent, low cost, the time consuming and high enrichment factor.

  10. A new room temperature ionic liquid 1-butyl-3-trimethylsilylimidazolium hexafluorophosphate as a solvent for extraction and preconcentration of mercury with determination by cold vapor atomic absorption spectrometry.

    Science.gov (United States)

    Li, Zaijun; Wei, Qin; Yuan, Rui; Zhou, Xia; Liu, Huizhen; Shan, Haixia; Song, Qijun

    2007-01-15

    A new room temperature ionic liquid 1-butyl-3-trimethylsilylimidazolium hexafluorophosphate abbreviated as [C(4)tmsim][PF(6)] was synthesized and developed as a novel medium for liquid/liquid extraction of inorganic mercury in this work. Under optimal condition, o-carboxyphenyldiazoamino-p-azobenzene abbreviated as CDAA reacted with inorganic mercury to form a neutral Hg-CDAA complex, the complex was rapidly extracted into ionic liquid phase. After back-extracting into aqueous phase with sulfide sodium solution, the mercury concentration was detected by cold vapor atomic absorption spectrometry. The extraction and back-extraction efficiencies were 99.9 and 100.1% for 5.0microg L(-1) standard mercury in 1000mL of water solution, respectively. The detection limit, calculated using three times the standard error of estimate of the calibration graph, is 0.01ng of mercury per milliliter water sample. The proposed method has been used to the determination of trace inorganic mercury in natural water with satisfactory results. Moreover, Zeta potential and surface tension of [C(4)tmsim][PF(6)] solution were measured and applied to explain the extraction mechanism of [C(4)tmsim][PF(6)] system.

  11. On-line solid-phase separation/preconcentration for the determination of copper in urine by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Saçmacı, Şerife, E-mail: sacmaci@erciyes.edu.tr; Şahan, Serkan; Şahin, Uğur; Kartal, Şenol; Ülgen, Ahmet

    2014-11-01

    A new on-line separation/preconcentration system was developed for the determination of Cu(II) ions by flame atomic absorption spectrometry in urine samples. A newly synthesized chelating resin, by anchoring eriochrome blue black R reagent to Amberlite XAD-16 resin, was used as a packing material for the selective separation/preconcentration of Cu(II) ions. The influence of the parameters on the determination of Cu(II) ions such as pH of sample solution, amount of the resin, eluent type, interfering ions and flow variables was studied. The detection limit of the method was 1.0 μg L{sup −1} while precision was 2.3% (n = 15) at 50 μg L{sup −1} Cu(II) level. The adsorption capacity of the resin was 217 μg g{sup −1} Cu(II). The accuracy of the method was proven using TMDA-64 standard lake water and synthetic urine sample. The developed method has been applied successfully to the determination of copper in urine with satisfactory results. - Highlights: • The method was applied to the urine samples taken from Wilson’s patients. • The on-line determination of copper and satisfactory results were obtained. • All processes are made automatically by the system itself in the proposed method.

  12. Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martinis, Estefania M.; Berton, Paula [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, CC. 131, M 5502 IRA Mendoza (Argentina); Olsina, Roberto A. [INQUISAL-CONICET, Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, San Luis (Argentina); Altamirano, Jorgelina C. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, CC. 131, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@lab.cricyt.edu.ar [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, CC. 131, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

    2009-08-15

    A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}mim][PF{sub 6}]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 {mu}l of 9.0 mol L{sup -1} hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3 ng L{sup -1} and the relative standard deviation (RSD) for 10 replicates at 1 {mu}g L{sup -1} Hg{sup 2+} was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

  13. Slurry analysis of cadmium and copper collected on 11-mercaptoundecanoic acid modified TiO{sub 2} core-Au shell nanoparticles by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gunduz, S. [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak-Istanbul (Turkey); Akman, S., E-mail: akmans@itu.edu.tr [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak-Istanbul (Turkey); Kahraman, M. [Yeditepe University, Faculty of Engineering and Architecture, Department of Genetics and Bioengineering, 34755 Kayisdagi-Istanbul (Turkey)

    2011-02-15

    Separation/preconcentration of copper and cadmium using TiO{sub 2} core-Au shell nanoparticles modified with 11-mercaptoundecanoic acid and their slurry analysis by flame atomic absorption spectrometry were described. For this purpose, at first, titanium dioxide nanoparticles were coated with gold shell by reducing the chloroauric acid with sodium borohydride and then modified with 11-mercaptoundecanoic acid. The characterization of modified nanoparticles was performed using ultra-violet spectroscopy and dynamic light scattering. Copper and cadmium were then collected on the prepared sorbent by batch method. The solid phase loaded with the analytes was separated by centrifugation and the supernatant was removed. Finally, the precipitate was slurried and directly aspirated into the flame for the determination of analytes. Thus, elution step and its all drawbacks were eliminated. The effects of pH, amount of sorbent, slurry volume, sample volume and diverse ions on the recovery were investigated. After optimization of experimental parameters, the analytes in different certified reference materials and spiked water samples were quantitatively recovered with 5% RSD. The analytes were enriched up to 20-fold. Limits of detection (N = 10, 3{sigma}) for copper and cadmium were 0.28 and 0.15 ng mL{sup -1}, respectively.

  14. Effects of Iron Concentration Level in Extracting Solutions from Contaminated Soils on the Determination of Zinc by Flame Atomic Absorption Spectrometry with Two Background Correctors

    Directory of Open Access Journals (Sweden)

    Christophe Waterlot

    2012-01-01

    Full Text Available Zinc and iron concentrations were determined after digestion, water, and three-step sequential extractions of contaminated soils. Analyses were carried out using flame absorption spectrometry with two background correctors: a deuterium lamp used as the continuum light source (D2 method and the high-speed self-reversal method (HSSR method. Regarding the preliminary results obtained with synthetic solutions, the D2 method often emerged as an unsuitable configuration for compensating iron spectral interferences. In contrast, the HSSR method appeared as a convenient and powerful configuration and was tested for the determination of zinc in contaminated soils containing high amounts of iron. Simple, fast, and interference-free method, the HSSR method allows zinc determination at the ppb level in the presence of large amounts of iron with high stability, sensitivity, and reproducibility of results. Therefore, the HSSR method is described here as a promising approach for monitoring zinc concentrations in various iron-containing samples without any pretreatment.

  15. On-line preconcentration employing a tannin resin for copper determination in plant material and food stuff by atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Miranda Carlos E. S.

    2000-01-01

    Full Text Available A flow system for copper on-line preconcentration, employing a tannin resin prepared from Eucalyptus Saligna Sm, with determination by flame atomic absorption spectrometry is proposed. The manifold was designed by assembling an automatic injector-commutator and a set of three-way solenoid valves which were controlled by a microcomputer with a PCL-711 interface card running a software written in QuickBASIC 4.5. The analyte was concentrated by pumping the sample solution through the resin column during 60 s, followed by elution with a 1.0 mol L-1 hydrochloric acid solution. Accuracy was assessed by analyzing acidic digests of certificate reference materials and no significant difference at 95% confidence level was observed. Other profitable features such as throughput of 48 determinations per hour, reagent consumption of 67 mL per determination, relative standard deviation of 3% (n=10 for a typical sample presenting concentration of 21.75 ng mL-1 Cu, detection limit of 1 ng mL-1 and enrichment factor of 10 times were also achieved.

  16. Preconcentration and determination of copper and cadmium ions with 1,6-bis(2-carboxy aldehyde phenoxy)butane functionalized Amberlite XAD-16 by flame atomic absorption spectrometry.

    Science.gov (United States)

    Oral, Elif V; Dolak, Ibrahim; Temel, Hamdi; Ziyadanogullari, Berrin

    2011-02-15

    A new chelating resin, covalently linked 1,6-bis(2-carboxy aldehyde phenoxy)butane with the Amberlite XAD-16 was synthesized and used for preconcentration of Cu(II) and Cd(II) prior to their determination by flame atomic absorption spectrometry (FAAS). It was characterized by elemental analyses and Fourier Transform Infrared Spectroscopy (FT-IR). Cu(II) and Cd(II) ions were quantitatively preconcentrated on minicolumn loaded with synthesised resin at pH 4.00 and 6.00, respectively. They were eluated with 5 mL of 0.5 mol L(-1) HCl. Recoveries of Cu(II) and Cd(II) were found to be 100±2.15, 100±1.40 (N=5), the limits of detection of Cu(II) and Cd(II) in the determination by FAAS (3s, N=20) were found to be 0.33 and 1.19 μg L(-1), respectively. The effect of foreign ions on the recovery has been investigated. The proposed method has been applied for the determination of Cu(II) and Cd(II) ions to the real samples collected from Tigris river water in Diyarbakir and Elaziğ cities in Turkey. Standard addition method and analysis of the certified reference material (NCS-DC 73350) was employed to check the accuracy of the method. Copyright © 2010 Elsevier B.V. All rights reserved.

  17. Real-time monitoring of respiratory absorption factors of volatile organic compounds in ambient air by proton transfer reaction time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Zhonghui [State Key Laboratory of Organic Geochemistry and Guangdong Key Laboratory of Environmental Protection and Resources Utilization, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Zhang, Yanli [State Key Laboratory of Organic Geochemistry and Guangdong Key Laboratory of Environmental Protection and Resources Utilization, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Center for Excellence in Urban Atmospheric Environment, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021 (China); Yan, Qiong [Department of Respiratory Diseases, Guangzhou No. 12 People' s Hospital, Guangzhou 510620 (China); Zhang, Zhou [State Key Laboratory of Organic Geochemistry and Guangdong Key Laboratory of Environmental Protection and Resources Utilization, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Wang, Xinming, E-mail: wangxm@gig.ac.cn [State Key Laboratory of Organic Geochemistry and Guangdong Key Laboratory of Environmental Protection and Resources Utilization, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Center for Excellence in Urban Atmospheric Environment, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021 (China)

    2016-12-15

    Respiratory absorption factors (AFs) are essential parameters in the evaluation of human health risks from toxic volatile organic compounds (VOCs) in ambient air. A method for the real time monitoring of VOCs in inhaled and exhaled air by proton transfer reaction time-of-flight mass spectrometry (PTR-TOF-MS) has been developed to permit the calculation of respiratory AFs of VOCs. Isoprene was found to be a better breath tracer than O{sub 2}, CO{sub 2}, humidity, or acetone for distinguishing between the expiratory and inspiratory phases, and a homemade online breath sampling device with a buffer tube was used to optimize signal peak shapes. Preliminary tests with seven subjects exposed to aromatic hydrocarbons in an indoor environment revealed mean respiratory AFs of 55.0%, 55.9%, and 66.9% for benzene, toluene, and C8-aromatics (ethylbenzene and xylenes), respectively. These AFs were lower than the values of 90% or 100% used in previous studies when assessing the health risks of inhalation exposure to hazardous VOCs. The mean respiratory AFs of benzene, toluene and C8-aromatics were 66.5%, 70.2% and 82.3% for the three female subjects; they were noticeably much higher than that of 46.4%, 45.2% and 55.3%, respectively, for the four male subjects.

  18. Multivariate optimization of ultrasound-assisted extraction for determination of Cu, Fe, Ni and Zn in vegetable oils by high-resolution continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Trindade, Alex S N; Dantas, Alailson F; Lima, Daniel C; Ferreira, Sérgio L C; Teixeira, Leonardo S G

    2015-10-15

    An assisted liquid-liquid extraction of copper, iron, nickel and zinc from vegetable oil samples with subsequent determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) was optimized by applying a full factorial design in two levels and the response surface methodology, Box-Behnken. The effects of the acid concentration and the amplitude, cycle and time of sonication on the extraction of the analytes, as well as their interactions, were assessed. In the selected condition (sonication amplitude = 66%, sonication time = 79 s, sonication cycle = 74%), using 0.5 mol L(-1) HCl as the extractant, the limits of quantification were 0.14, 0.20, 0.21 and 0.04 μg g(-1) for Cu, Fe, Ni and Zn, respectively, with R.S.D. ranging from 1.4% to 3.6%. The proposed method was applied for the determination of the analytes in soybean, canola and sunflower oils. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. In situ flow cell for combined X-ray absorption spectroscopy, X-ray diffraction, and mass spectrometry at high photon energies under solar thermochemical looping conditions

    Science.gov (United States)

    Rothensteiner, Matthäus; Jenni, Joel; Emerich, Hermann; Bonk, Alexander; Vogt, Ulrich F.; van Bokhoven, Jeroen A.

    2017-08-01

    An in situ/operando flow cell for transmission mode X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), and combined XAS/XRD measurements in a single experiment under the extreme conditions of two-step solar thermochemical looping for the dissociation of water and/or carbon dioxide was developed. The apparatus exposes materials to relevant conditions of both the auto-reduction and the oxidation sub-steps of the thermochemical cycle at ambient temperature up to 1773 K and enables determination of the composition of the effluent gases by online quadrupole mass spectrometry. The cell is based on a tube-in-tube design and is heated by means of a focusing infrared furnace. It was tested successfully for carbon dioxide splitting. In combined XAS/XRD experiments with an unfocused beam, XAS measurements were performed at the Ce K edge (40.4 keV) and XRD measurements at 64.8 keV and 55.9 keV. Furthermore, XRD measurements with a focused beam at 41.5 keV were carried out. Equimolar ceria-hafnia was auto-reduced in a flow of argon and chemically reduced in a flow of hydrogen/helium. Under reducing conditions, all cerium(iv) was converted to cerium(iii) and a cation-ordered pyrochlore-type structure was formed, which was not stable upon oxidation in a flow of carbon dioxide.

  20. Optimization of cloud point extraction procedure with response surface methodology for quantification of iron by means of flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Abdolmohammad-Zadeh Hossein

    2013-01-01

    Full Text Available A simple micelle-mediated phase separation method has been developed for the pre-concentration of trace levels of iron as a prior step to determination by flame atomic absorption spectrometry (FAAS. The method is based on the cloud point extraction (CPE of iron using non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5 without adding any chelating agent. Several variables affecting the extraction efficiency were studied and optimized utilizing central composite design (CCD and three levels full factorial design. Under the optimum conditions, the limit of detection (LOD, limit of quantification (LOQ and pre-concentration factor were 1.5 μg L-1, 5.0 μg L-1 and 100, respectively. The relative standard deviation (RSD for six replicate determinations at 50 μg L−1 Fe(III level was 1.97%. The calibration graph was linear in the rage of 5-100 μg L-1, with a correlation coefficient of 0.9921. The developed method was validated by the analysis of two certified reference materials and applied successfully to the determination of trace amounts of Fe(III in water and rice samples.

  1. Selenium analysis by an integrated microwave digestion-needle trap device with hydride sorption on carbon nanotubes and electrothermal atomic absorption spectrometry determination

    Science.gov (United States)

    Maratta Martínez, Ariel; Vázquez, Sandra; Lara, Rodolfo; Martínez, Luis Dante; Pacheco, Pablo

    2018-02-01

    An integrated microwave assisted digestion (MW-AD) - needle trap device (NTD) for selenium determination in grape pomace samples is presented. The NTD was filled with oxidized multiwall carbon nanotubes (oxMWCNTS) where Se hydrides were preconcentrated. Determination was carried out by flow injection-electrothermal atomic absorption spectrometry (FI-ETAAS). The variables affecting the system were established by a multivariate design (Plackett Burman), indicating that the following variables significantly affect the system: sample amount, HNO3 digestion solution concentration, NaBH4 volume and elution volume. A Box-Behnken design was implemented to determine the optimized values of these variables. The system improved Se atomization in the graphite furnace, since only trapped hydrides reached the graphite furnace, and the pyrolysis stage was eliminated according to the aqueous matrix of the eluate. Under optimized conditions the system reached a limit of quantification of 0.11 μg kg- 1, a detection limit of 0.032 μg kg- 1, a relative standard deviation of 4% and a preconcentration factor (PF) of 100, reaching a throughput sample of 5 samples per hour. Sample analysis show Se concentrations between 0.34 ± 0.03 μg kg- 1 to 0.48 ± 0.03 μg kg- 1 in grape pomace. This system provides minimal reagents and sample consumption, eliminates discontinuous stages between samples processing reaching a simpler and faster Se analysis.

  2. Excessive aluminum accumulation in the bones of patients on long-term parenteral nutrition: postmortem analysis by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Kruger, Pamela C; Parsons, Patrick J; Galusha, Aubrey L; Morrissette, Michelle; Recker, Robert R; Howard, Lyn J

    2014-08-01

    Aluminum (Al) contamination of parenteral nutrition (PN) solutions remains a concern for long-term PN patients. Al accumulates particularly in bone. Excessive exposure to Al may result in increased Al body burden and impaired bone formation and mineralization, leading to bone disease. Although the U.S. Food and Drug Administration (FDA) has limited Al contamination in large-volume parenteral solutions, small-volume parenterals may still contribute considerable amounts of Al to PN solutions. The goal of this study is to determine whether or not long-term adult PN patients remain at risk for increased bone Al accumulation. We measured Al accumulation in autopsy bones from 7 patients who had received PN for 2-21 years and compared bone Al levels with those in living control patients undergoing hip or knee replacement. Electrothermal atomic absorption spectrometry was used for bone Al measurements. When compared with bone Al content in controls, markedly elevated Al levels (P < .0001) were found in the bones of all but 1 patient, who received PN for only 2 years before death. Even greater Al accumulation was found for PN patients who developed late renal impairment (P = .0159). We conclude that long-term adult PN patients continue to be at risk for Al toxicity. © 2013 American Society for Parenteral and Enteral Nutrition.

  3. A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

    2013-01-01

    A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

  4. Direct extraction of lead (II) from untreated human blood serum using restricted access carbon nanotubes and its determination by atomic absorption spectrometry.

    Science.gov (United States)

    Barbosa, Valéria Maria Pereira; Barbosa, Adriano Francisco; Bettini, Jefferson; Luccas, Pedro Orival; Figueiredo, Eduardo Costa

    2016-01-15

    Oxidized carbon nanotubes were covered with layers of bovine serum albumin to result in so-called restricted-access carbon nanotubes (RACNTs). This material can extract Pb(2+) ions directly from untreated human blood serum while excluding all the serum proteins. The RACNTs have a protein exclusion capacity of almost 100% and a maximum Pb(2+) adsorption capacity of 34.5mg g(-1). High resolution transmission electron microscopy, scanning transmission electron microscopy and energy dispersive spectroscopy were used to confirm the BSA layer and Pb(2+) adsorption sites. A mini-column filled with RACNTs was used in an on-line solid phase extraction system coupled to a thermospray flame furnace atomic absorption spectrometry. At optimized experimental conditions, the method has a detection limit as low as 2.1µg L(-1), an enrichment factor of 5.5, and inter- and intra-day precisions (expressed as relative standard deviation) of <8.1%. Recoveries of the Pb(2+) spiked samples ranged from 89.4% to 107.3% for the extraction from untreated human blood serum. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

    Science.gov (United States)

    Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

    2016-08-15

    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

    2016-04-01

    High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. A new cloud point extraction procedure for determination of inorganic antimony species in beverages and biological samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan

    2015-05-15

    A new cloud-point extraction (CPE) for the determination of antimony species in biological and beverages samples has been established with flame atomic absorption spectrometry (FAAS). The method is based on the fact that formation of the competitive ion-pairing complex of Sb(III) and Sb(V) with Victoria Pure Blue BO (VPB(+)) at pH 10. The antimony species were individually detected by FAAS. Under the optimized conditions, the calibration range for Sb(V) is 1-250 μg L(-1) with a detection limit of 0.25 μg L(-1) and sensitive enhancement factor of 76.3 while the calibration range for Sb(III) is 10-400 μg L(-1) with a detection limit of 5.15 μg L(-1) and sensitive enhancement factor of 48.3. The precision as a relative standard deviation is in range of 0.24-2.35%. The method was successfully applied to the speciative determination of antimony species in the samples. The validation was verified by analysis of certified reference materials (CRMs). Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Indirect determination of the flavor enhancer maltol in foods and beverages through flame atomic absorption spectrometry after ultrasound assisted-cloud point extraction.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan; Orhan, Ulaş

    2017-11-15

    A simple ultrasound assisted-cloud point extraction (UA-CPE) method was developed and combined with flame atomic absorption spectrometry (FAAS) for pre-concentration and indirect determination of the flavor enhancer maltol in foods and beverages. The method is based on reduction of Cu(II) to Cu(I) by maltol at pH 6.5, and subsequent selective interaction of Cu(I) with bathocuproine (BCP) to form a ternary complex in presence of sodium dodecyl sulfate (SDS). Under the optimized conditions, pre-concentration of a 35mL sample solution allowed detection of 1.24µgL-1 maltol in a linear range of 4-230µgL-1. The method was validated by intra- and inter-day precision studies ranging from 2.1 to 3.4%, and recoveries ranged from 93.3% to 104.4% using standard addition method. After pretreatment with two different sample preparation steps assisted by ultrasound energy, the proposed method was applied successfully for determination of maltol in selected foods and beverages. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. One-step displacement dispersive liquid-liquid microextraction coupled with graphite furnace atomic absorption spectrometry for the selective determination of methylmercury in environmental samples.

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Mo, Yajun

    2016-01-01

    A novel method for the selective determination of methylmercury (MeHg) was developed by one-step displacement dispersive liquid-liquid microextraction (D-DLLME) coupled with graphite furnace atomic absorption spectrometry. In the proposed method, Cu(II) reacted with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which was used as the chelating agent instead of DDTC for the dispersive liquid-liquid microextraction (DLLME) of MeHg. Because the stability of MeHg-DDTC is higher than that of Cu-DDTC, MeHg can displace Cu from the Cu-DDTC complex and be preconcentrated in a single DLLME procedure. MeHg could be extracted into the extraction solvent phase at pH 6 while Hg(II) remained in the sample solution. Potential interference from co-existing metal ions with lower DDTC complex stability was largely eliminated without the need of any masking reagent. Under the optimal conditions, the limit of detection of this method was 13.6ngL(-1) (as Hg), and an enhancement factor of 81 was achieved with a sample volume of 5.0mL. The proposed method was successfully applied for the determination of trace MeHg in some environmental samples with satisfactory results. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Application of l-cystine modified zeolite for preconcentration and determination of ultra-trace levels of cadmium by flame atomic absorption spectrometry.

    Science.gov (United States)

    Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

    2016-03-04

    A very convenient, sensitive and precise solid phase extraction (SPE) system was developed for enrichment and determination of ultra-trace of cadmium ion in water and plant samples. This method was based on the retention of cadmium(II) ions by l-cystine adsorbed in Y-zeolite and carry out in a packed mini-column. The retained cadmium ions then were eluted and determined by flame atomic absorption spectrometry. The scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and Fourier Transform Infrared (FT-IR) spectroscopy techniques were applied for the characterization of cystine modified zeolite (CMZ). Some experimental conditions affecting the analytical performance such as pH, eluent type, concentration of sample, eluent flow rate and also the presence of interfering ions were investigated. The calibration graph was linear within the range of 0.1-7.5ngmL(-1) and limit of detection was obtained 0.04ngmL(-1) with the preconcentration factor of 400. The relative standard deviation (RSD) was obtained 1.4%, indicating the excellent reproducibility of this method. The proposed method was successfully applied for the extraction and determination of cadmium(II) ion in black tea, cigarette's tobacco and also various water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Development a novel supramolecular solvent microextraction procedure for copper in environmental samples and its determination by microsampling flame atomic absorption spectrometry.

    Science.gov (United States)

    Yilmaz, Erkan; Soylak, Mustafa

    2014-08-01

    A supramolecular solvent (Ss) made up of reverse micelles of 1-decanol in tetrahydrofuran (THF): water was used for the fast and selective microextraction of Cu(II) prior to its determination by microsampling flame atomic absorption spectrometry (FAAS). Cu(II) was complexed with dimethyl dithiocarbamate (DMDC) to obtain hydrophobic complex and extracted to supramolecular solvent phase. The influences of some analytical parameters including pH, type and volume of supramolecular solvent, amount of complexing agent, ultrasonication and centrifuge time and sample volume were investigated. The effects of matrix components were also examined. The detection limit (LOD) and the quantification limit (LOQ) were 0.52µg L(-1) and 1.71µg L(-1) respectively. An preconcentration factor was obtained as 60 and the relative standard deviation was <3%. The accuracy of the developed method was evaluated by the analysis of the certified reference materials (TMDA-64.2 water, SRM 1568A Rice Flour and 8433 Corn Bran) and addition-recovery tests. The presented supramolecular solvent based liquid-liquid microextraction (SsLLME) procedure was applied to the determination of copper in food and water samples with satisfactory results. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. A Green Preconcentration Method for Determination of Cobalt and Lead in Fresh Surface and Waste Water Samples Prior to Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Shah, Faheem; Afridi, Hassan Imran; Khan, Sumaira; Arian, Sadaf Sadia; Brahman, Kapil Dev

    2012-01-01

    Cloud point extraction (CPE) has been used for the preconcentration and simultaneous determination of cobalt (Co) and lead (Pb) in fresh and wastewater samples. The extraction of analytes from aqueous samples was performed in the presence of 8-hydroxyquinoline (oxine) as a chelating agent and Triton X-114 as a nonionic surfactant. Experiments were conducted to assess the effect of different chemical variables such as pH, amounts of reagents (oxine and Triton X-114), temperature, incubation time, and sample volume. After phase separation, based on the cloud point, the surfactant-rich phase was diluted with acidic ethanol prior to its analysis by the flame atomic absorption spectrometry (FAAS). The enhancement factors 70 and 50 with detection limits of 0.26 μg L−1 and 0.44 μg L−1 were obtained for Co and Pb, respectively. In order to validate the developed method, a certified reference material (SRM 1643e) was analyzed and the determined values obtained were in a good agreement with the certified values. The proposed method was applied successfully to the determination of Co and Pb in a fresh surface and waste water sample. PMID:23227429

  13. Evaluation of toxic metals in biological samples (scalp hair, blood and urine) of steel mill workers by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Afridi, Hassan I; Kazi, Tasneem G; Jamali, Mohammad K; Kazi, Gul H; Arain, Mohammad B; Jalbani, Nusrat; Shar, Ghulam Q; Sarfaraz, Raja A

    2006-10-01

    The determination of toxic metals in the biological samples of human beings is an important clinical screening procedure. This study aimed to assess the possible influence of environmental exposure on production workers (PW) and quality control workers (QCW) of a steel mill, all male subjects aged 25-55 years. In this investigation, the concentrations of Pb, Cd, Ni and Cr were determined in biological samples (blood, urine and scalp hair samples) from these steel mill workers in relation to controlled unexposed healthy subjects of the same age group. After pre-treatment with nitric acid-hydrogen peroxide, the samples were digested via a microwave oven, and for comparison purposes, the same samples were digested by the conventional wet acid digestion method. The samples digested were subjected to graphite furnace atomic absorption spectrometry (GFAAS). To assess the reliability of these methods, critical factors, such as detection limit(s), calibration range(s), accuracy and precision, were studied. Quality control for these procedures was established with certified sample of human hair, urine and whole blood. The results indicate that the level of lead, cadmium and nickel in scalp hair, blood and urine samples were significantly higher in both groups of exposed workers (QW and PW) than those of the controls. The possible connection of these elements with the etiology of disease is discussed. The results also show the need for immediate improvements in workplace ventilation and industrial hygiene practices.

  14. Ultrasound-assisted extraction for the determination of Cu, Mn, Ca, and Mg in alternative oilseed crops using flame atomic absorption spectrometry.

    Science.gov (United States)

    Peronico, Vanessa Cruz Dias; Raposo, Jorge Luiz

    2016-04-01

    An ultrasound-assisted extraction procedure was evaluated for the multi-element determination of Cu, Mn, Ca, and Mg in alternative oilseed crops using flame atomic absorption spectrometry. The best results were obtained when 0.3g of samples were used to extract the mineral content using 10 mL of a 1.40 mol L(-1) HNO3 solution for 10 min at 25 °C. The accuracy and precision of the analysis were evaluated using two oilseed reference materials, and the results were in agreement with reference values at 95% confidence level (paired t-test). The method was used to analyze five oilseed samples and the results were in agreement with those obtained using a closed-vessel microwave-assisted acid digestion system for sample preparation. The relative standard deviations were 0.52-6.13% for all of the standard and sample measurements, and the limits of detection were 666.7, 416.7, 333.4 μg g(-1), and 3.5 mg g(-1) for Cu, Mn, Ca, and Mg, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. A simple and selective approach for determination of trace Hg(II) using electromembrane extraction followed by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Kamyabi, Mohammad Ali; Aghaei, Ali

    2017-02-01

    The present study proposes the determination of trace Hg(II) using electromembrane extraction followed by graphite furnace atomic absorption spectrometry (GFAAS). Hg(II) migrated from 5 mL of an aqueous donor phase across a thin layer of supported liquid membrane, immobilized inside pores of a hollow fiber, into 10 μL of an acidic acceptor phase present inside the lumen of the fiber. The final analysis of the extracted Hg(II) performed using GFAAS (350 °C and 1400 °C for the ashing and atomization temperatures, respectively). Under optimal conditions, Hg(II) was effectively extracted with recoveries in the range of 41-43%, which corresponded to enrichment factors in the range of 102-108. The calibration curve was investigated in the range of 0.5-10 μg/L and a good linearity was achieved with a coefficient factor of 0.998. Detection limit (3σ) was found to be 0.5 μg/L and repeatability for 5 replicate determinations of three different concentration level of Hg(II) were found to be within the range of 6.2-7.1%. The reliability of the proposed method was examined by analyzing different real waters samples.

  16. Ultrasound-Assisted Emulsification Microextraction Based on Solidification Floating Organic Drop Trace Amounts of Manganese Prior to Graphite Furnace Atomic Absorption Spectrometry Determination

    Science.gov (United States)

    Mohadesi, Alireza; Falahnejad, Masoumeh

    2012-01-01

    In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn+2 at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50–10.0 ng mL−1 with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL−1 was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

  17. Combination of flotation and flame atomic absorption spectrometry for determination, preconcentration and separation of trace amounts of metal ions in biological samples.

    Science.gov (United States)

    Ghaedi, Mehrorang; Niknam, Khodabakhsh; Nasiri kokhdan, Syamak; Soylak, Mustafa

    2013-05-01

    An efficient enrichment procedure based on the combination of flame atomic absorption spectrometry (FAAS) and flotation for determination of Cd(2+), Ag(+) and Zn(2+) ions in various biological samples using new collector is studied. The influence of pH, amount of 2-(((1H-benzo[d]imidazol-2-yl)methoxy)methyl)-1H-benzo[d]imidazole (HBIMMHBI) as collector, sample matrix, type and amount of eluting agent, type and amount of surfactant as floating agent, ionic strength and air flow rates on the extraction efficiency were evaluated and optimized. It is ascertained that under study metal ions is preconcentrated simultaneously from matrix in the presence of 0.005 M HBIMMHBI, 0.085% (w/v) of SDS form 750 mL at pH 6.5. The floated complexes metal ions eluted quantitatively with 6 mL of 1.0 M HNO3 in methanol lead to achieve preconcentration factor of 125. The detection limits for analyte ions were in the range of 1.3-2.4 ng mL(-1), with recoveries more than 95% and relative SD lower than 4%.

  18. Determination of macro and trace elements in multivitamin dietary supplements by high-resolution continuum source graphite furnace atomic absorption spectrometry with slurry sampling.

    Science.gov (United States)

    Krawczyk, Magdalena

    2014-01-01

    In this research, three different commercially available multivitamin dietary supplements were analyzed by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) with slurry sampling. The concentrations of Cr, Cu, Fe, Mn, and Se were determined and compared to the amounts stated by producers. The safety of multivitamin dietary supplements depends on various factors including the manufacturing process and the purity and origins of the raw ingredients. For this reason, this research determined concentrations of several toxic elements (As, Cd, and Pb). Microwave-assisted high pressure Teflon bomb digestion was used to determine total amounts of elements in samples. Samples were prepared as slurries at a concentration of 0.1% (m/v) for macro elements (Cr, Cu, Fe, Mn, and Se) and at a concentration of % (m/v) for trace elements (As, Cd, and Pb) in acidic media (3M HNO3). The influence of acid concentration, Triton X-100 addition, sonication time, and sonication power on absorbance was investigated. The accuracy of this method was validated by analyses of NRCC LUTS-1 (Lobster hepatopancreas), NRCC DORM-1 (Dogfish Muscle), NRCC DOLT-2 (Dogfish Liver), NBS SRM 1570 (Spinach Leaves) and NBS SRM 1573 (Tomato Leaves) certified reference materials. The measured elements contents in these reference materials (except NRCC DOLT-2) were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Dispersive liquid-liquid microextraction based on solidification of floating organic drop for preconcentration and determination of trace amounts of copper by flame atomic absorption spectrometry.

    Science.gov (United States)

    Karadaş, Cennet; Kara, Derya

    2017-04-01

    A novel, simple, rapid, sensitive, inexpensive and environmentally friendly dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop (DLLME-SFO) was developed for the determination of copper by flame atomic absorption spectrometry (FAAS). N-o-Vanillidine-2-amino-p-cresol was used as a chelating ligand and 1-undecanol was selected as an extraction solvent. The main parameters affecting the performance of DLLME-SFO, such as sample pH, volume of extraction solvent, extraction time, concentration of the chelating ligand, salt effect, centrifugation time and sample volume were investigated and optimized. The effect of interfering ions on the recovery of copper was also examined. Under the optimum conditions, the detection limit (3σ) was 0.93μgL(-1) for Cu using a sample volume of 20mL, yielding a preconcentration factor of 20. The proposed method was successfully applied to the determination of Cu in tap, river and seawater, rice flour and black tea samples as well as certified reference materials. Copyright © 2016. Published by Elsevier Ltd.

  20. Synthesis, characterization and application of a new chelating resin for solid phase extraction, preconcentration and determination of trace metals in some dairy samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Daşbaşı, Teslima; Saçmacı, Şerife; Çankaya, Nevin; Soykan, Cengiz

    2016-11-15

    In this study, a simple and rapid solid phase extraction/preconcentration procedure was developed for determination of Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Pb(II), and Zn(II) trace metals by flame atomic absorption spectrometry (FAAS). A new chelating resin, poly(N-cyclohexylacrylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propanesulfonic acid) (NCA-co-DVB-co-AMPS) (hereafter CDAP) was synthesized and characterized. The influences of the analytical parameters such as pH of the sample solution, type and concentration of eluent, flow rates of the sample and eluent, volume of the sample and eluent, amount of chelating resin, and interference of ions were examined. The limit of detection (LOD) of analytes were found (3s) to be in the range of 0.65-1.90μgL(-1). Preconcentration factor (PF) of 200 and the relative standard deviation (RSD) of ⩽2% were achieved (n=11). The developed method was applied for determination of analytes in some dairy samples and certified reference materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

  1. Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

    Science.gov (United States)

    Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

    2017-06-01

    A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

  2. Determination of Lead in Water Samples Using a New Vortex-Assisted, Surfactant-Enhanced Emulsification Liquid-Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry.

    Science.gov (United States)

    Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Pan, Weiliang; Tang, Xiaohui; Zhou, Guangming; Mao, Yufeng; Su, Xaioxuan

    2016-04-01

    A low toxic solvent-based vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction (LT-VSLLME) combined with graphite furnace atomic absorption spectrometry was developed for the extraction and determination of lead (Pb) in water samples. In the LT-VSLLME method, the extraction solvent was dispersed into the aqueous samples by the assistance of vortex agitator. Meanwhile, the addition of a surfactant, which acted as an emulsifier, could enhance the speed of the mass-transfer from aqueous samples to the extraction solvent. The influences of analytical parameters, including extraction solvent type and its volume, surfactant type and its volume, pH, concentration of chelating agent, salt effect and extraction time were investigated. Under the optimized conditions, a good relative standard deviation of 3.69% at 10 ng L(-1) was obtained. The calibration graph showed a linear pattern in the ranges of 5-30 ngL(-1), with a limit of detection of 0.76 ng L(-1). The linearity was obtained by five points in the concentration range of 5-30 ngL(-1). The enrichment factor was 320. The procedure was applied to wastewater and river water, and the accuracy was assessed through the analysis of the recovery experiments.

  3. Determination of Cadmium by Electrothermal Atomic Absorption Spectrometry after its Separation and Preconcentration by Syringe to Syringe Dispersive Liquid Phase Microextraction-Solidified Floating Organic Drop

    Directory of Open Access Journals (Sweden)

    Mohammad Asadi

    2017-12-01

    Full Text Available The application of syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop was extended for the separation and preconcentration of trace amounts of cadmium ions from water and cereal samples. The extracted cadmium was quantified by electrothermal atomic absorption spectrometry. Factors affecting the complex formation as well as microextraction efficiency such as the concentration of dithizone as the chelating agent, sample pH, type and volume of the extractant, number of injections, ionic strength and sample volume were optimized. Under optimized conditions, the calibration curve was linear in the range of 1.0-14.0 ng L-1 with the coefficient of determination of 0.9994. The limit of detection and quantification were found to be 0.25 and 0.85 ng L-1, respectively. The inter-day and intra-day precision at two concentration levels (3.0 and 10.0 ng L-1 were in the range of 3.9-9.2%. The accuracy of the developed method was evaluated through recovery experiments and the analysis of certified reference material (SLRS-6.

  4. A novel separation/preconcentration technique based on ultrasonic dispersion liquid-liquid microextraction for determination of trace cobalt by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Jingci Li

    2012-12-01

    Full Text Available An improved method for the determination of trace cobalt in water samples has been developed using ultrasonic dispersion liquid-liquid microextraction (US-DLLME prior to flame atomic absorption spectrometry (FAAS analysis. In this method, cobalt was extracted into the fine droplets of carbon tetrachloride after chelate formation with the water soluble ligand, ammonium pyrrolidine dithiocarbamate (APDC. The fine droplets of carbon tetrachloride were formed and dispersed in the aqueous sample with the help of ultrasonic waves which accelerated the formation of the fine cloudy solution without using disperser solvents. Under optimum conditions, the calibration curve was linear in the range of 2.5-500 μg L-1, with a detection limit of 0.8 μg L-1. The relative standard deviation (RSD for ten replicate measurements of 20 and 500 μg L-1 of cobalt were 3.3 and 2.2%. This proposed method was successfully applied to tap water, river water, and sea water, and accuracy was assessed through the analysis of certified reference water or recovery experiments. Operation simplicity, low cost, high enrichment factor, and low consumption of the extraction solvent are the main advantages of the proposed method.DOI: http://dx.doi.org/10.4314/bcse.v26i1.2

  5. Cloud point extraction combined with electrothermal atomic absorption spectrometry for the speciation of antimony(III) and antimony(V) in food packaging materials.

    Science.gov (United States)

    Jiang, Xiuming; Wen, Shengping; Xiang, Guoqiang

    2010-03-15

    A simple, sensitive method for the speciation of inorganic antimony by cloud point extraction combined with electrothermal atomic absorption spectrometry (ETAAS) is presented and evaluated. The method based on the fact that formation of a hydrophobic complex of antimony(III) with ammonium pyrrolidine dithiocarbamate (APDC) at pH 5.0 and subsequently the hydrophobic complex enter into surfactant-rich phase, whereas antimony(V) remained in aqueous solutions. Antimony(III) in surfactant-rich phase was analyzed by ETAAS after dilution by 0.2 mL nitric acid in methanol (0.1M), and antimony(V) was calculated by subtracting antimony(III) from the total antimony after reducing antimony(V) to antimony(III) by l-cysteine. The main factors affecting the cloud point extraction, such as pH, concentration of APDC and Triton X-114, equilibrium temperature and incubation time, sample volume were investigated in detail. Under the optimum conditions, the detection limit (3 sigma) of the proposed method was 0.02 ng mL(-1) for antimony(III), and the relative standard deviation was 7.8% (c=1.0 ng mL(-1), n=7). The proposed method was successfully applied to speciation of inorganic antimony in the leaching solutions of different food packaging materials with satisfactory results. (c) 2009 Elsevier B.V. All rights reserved.

  6. Speciation of antimony(III) and antimony(V) by electrothermal atomic absorption spectrometry after ultrasound-assisted emulsification of solidified floating organic drop microextraction.

    Science.gov (United States)

    Wen, Shengping; Zhu, Xiashi

    2013-10-15

    A simple, sensitive and efficient method of ultrasound-assisted emulsification of solidified floating organic drop microextraction (USE-SFODME) coupled to electrothermal atomic absorption spectrometry for the speciation of antimony at different oxidation state Sb(III)/Sb(V) in environmental samples was established. In this method, the hydrophobic complex of Sb(III) with sodium diethyldithiocarbamate (DDTC) is extracted by 1-undecanol at pH 9.0, while Sb(V) remains in aqueous phase. Sb(V) content can be calculated by subtracting Sb(III) from the total antimony after reducing Sb(V) to Sb(III) by l-cysteine. Various factors affecting USE-SFODME including pH, extraction solvent and its volume, concentration of DDTC, sonication time, and extraction temperature were investigated. Under the optimized conditions, the calibration curve was linear in the range from 0.05 to 10.0 ng mL(-1), with the limit of detection (3σ) 9.89 ng L(-1) for Sb(III). The relative standard deviation for Sb(III) was 4.5% (n=9, c=1.0 ng mL(-1)). This method was validated against the certified reference materials (GSB 07-1376-2001, GBW07441), and applied to the speciation of antimony in environmental samples (soil and water samples) with satisfactory results. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Cloud point extraction combined with electrothermal atomic absorption spectrometry for the speciation of antimony(III) and antimony(V) in food packaging materials

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Xiuming; Wen Shengping [School of Chemistry and Chemical Engineering, Henan University of Technology, South Song Shan Road No. 140, Zhengzhou City 450001 (China); Xiang Guoqiang, E-mail: xianggq@haut.edu.cn [School of Chemistry and Chemical Engineering, Henan University of Technology, South Song Shan Road No. 140, Zhengzhou City 450001 (China)

    2010-03-15

    A simple, sensitive method for the speciation of inorganic antimony by cloud point extraction combined with electrothermal atomic absorption spectrometry (ETAAS) is presented and evaluated. The method based on the fact that formation of a hydrophobic complex of antimony(III) with ammonium pyrrolidine dithiocarbamate (APDC) at pH 5.0 and subsequently the hydrophobic complex enter into surfactant-rich phase, whereas antimony(V) remained in aqueous solutions. Antimony(III) in surfactant-rich phase was analyzed by ETAAS after dilution by 0.2 mL nitric acid in methanol (0.1 M), and antimony(V) was calculated by subtracting antimony(III) from the total antimony after reducing antimony(V) to antimony(III) by L-cysteine. The main factors affecting the cloud point extraction, such as pH, concentration of APDC and Triton X-114, equilibrium temperature and incubation time, sample volume were investigated in detail. Under the optimum conditions, the detection limit (3{sigma}) of the proposed method was 0.02 ng mL{sup -1} for antimony(III), and the relative standard deviation was 7.8% (c = 1.0 ng mL{sup -1}, n = 7). The proposed method was successfully applied to speciation of inorganic antimony in the leaching solutions of different food packaging materials with satisfactory results.

  8. Simultaneous determination of Cr, Ni and V in urine by electrothermal atomic absorption spectrometry (ET AAS); Determinacion simultanea de Cr, Ni y V en orina mediante et aas

    Energy Technology Data Exchange (ETDEWEB)

    Alvarez, Maria A.; Hermida, Jeymi [Universidad Central de Venezuela, Caracas (Venezuela, Bolivarian Republic of). Escuela de Quimica. Centro de Quimica Analitica

    2011-07-01

    A procedure for the simultaneous determination of Cr, Ni, and V in urine by electrothermal atomic absorption spectrometry (ET AAS) was optimized by factorial design, and performed at a pyrolysis and atomization temperatures of 1300 and 2500 deg C, respectively, using 15 {mu}g de Mg(NO{sub 3}){sub 2} as chemical modifier. Characteristics mass of 14, 6 and 220 {rho}g and detection limits of the method of 0.07, 0.38 and 0.75 {mu}g L{sup -1} were obtained for Cr, Ni and V respectively. The methodology was validated using a Liphochek Urine Metals Control sample (Bio-Rad) (P=0.05). The methodology was applied to samples of voluntary Venezuelan people, not environmentally exposed to specific emissions, and results ranging from < LOD-1.1 and 1.3-3.3 {mu}g L{sup -1} was observed for Cr and V, respectively, and not detectable levels for Ni. (author)

  9. Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Olmedo, P.; Pla, A.; Hernandez, A.F.; Lopez-Guarnido, O.; Rodrigo, L. [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain); Gil, F., E-mail: fgil@ugr.es [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain)

    2010-02-05

    For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

  10. On-line preconcentration of ultra-trace thallium(I in water samples with titanium dioxide nanoparticles and determination by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Saeid Asadpour

    2016-11-01

    Full Text Available A new method has been developed for the determination of Tl(I based on simultaneous sorption and preconcentration with a microcolumn packed with TiO2 nanoparticle with a high specific surface area prepared by Sonochemical synthesis prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS. The optimum experimental parameters for preconcentration of thallium, such as elution condition, pH, and sample volume and flow rate have been investigated. Tl(I can be quantitatively retained by TiO2 nanoparticles at pH 9.0, then eluted completely with 1.0 mol L−1 HCl. The adsorption capacity of TiO2 nanoparticles for Tl(I was found to be 25 mg g−1. Also detection limit, precision (RSD, n = 8 and enrichment factor for Tl(I were 87 ng L−1, 6.4% and 100, respectively. The method has been applied for the determination of trace amounts of Tl(I in some environmental water samples with satisfactory results.

  11. Study of the roles of chemical modifiers in determining boron using graphite furnace atomic absorption spectrometry and optimization of the temperature profile during atomization.

    Science.gov (United States)

    Yamamoto, Yuhei; Shirasaki, Toshihiro; Yonetani, Akira; Imai, Shoji

    2015-01-01

    The measurement conditions for determining boron using graphite furnace-atomic absorption spectrometry (GF-AAS) were investigated. Differences in the boron absorbance profiles were found using three different commercially available GF-AAS instruments when the graphite atomizers in them were not tuned. The boron absorbances found with and without adjusting the graphite atomizers suggested that achieving an adequate absorbance for the determination of boron requires a sharp temperature profile that overshoots the target temperature during the atomization process. Chemical modifiers that could improve the boron absorbance without the need for using coating agents were tested. Calcium carbonate improved the boron absorbance but did not suppress variability in the peak height. Improvement of boron absorbance was comparatively less using iron nitrate or copper nitrate than using calcium carbonate, but variability in the peak height was clearly suppressed using iron nitrate or copper nitrate. The limit of detection was 0.0026 mg L(-1) when iron nitrate was used. It appears that iron nitrate is a useful new chemical modifier for the quick and simple determination of boron using GF-AAS.

  12. Direct determination of arsenic and antimony in naphtha by electrothermal atomic absorption spectrometry with microemulsion sample introduction and iridium permanent modifier.

    Science.gov (United States)

    Cassella, Ricardo J; Barbosa, Bruno Alberto R S; Santelli, Ricardo E; Rangel, Alessandra T

    2004-05-01

    This paper reports the determination of arsenic and antimony in naphtha by employing electrothermal atomic absorption spectrometry (ETAAS) as the analytical technique. In order to promote the direct determination of the analytes in the very volatile naphtha, the formation of a microemulsion with different surfactants (Triton X-100 and Brij-35) and different chemical modification strategies were tested. The results indicated that Triton X-100 is the best emulsification agent for naphtha in both As and Sb determination when it is employed at a concentration of 1% w/v in the microemulsion. Under these conditions, the microemulsion was stabile for at least 2 h. By using Brij-35 it was possible to achieve good stability only in the first 15 min. Among all chemical modification approaches investigated (Ir permanent modifier, W-Ir permanent modifier, and Pd modifier), the Ir permanent modifier provided better sensitivity for both analytes and allowed a higher pyrolysis temperature, which decreased the background signals at lower levels. Under the best conditions established in this work, an RSD of 4.6% (20 microg L(-1)) and a detection limit of 2.7 microg L(-1) were observed for arsenic. For antimony, an RSD of 4.0% (20 microg L(-1)) and a detection limit of 2.5 microg L(-1) were obtained. The accuracy of the procedure was assessed by analyzing spiked samples of naphtha from different origins.

  13. Distribution of heavy metals in Lumbricus terrestris, Aporrectodea longa and A. rosea measured by atomic absorption and X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Andersen, C.; Laursen, J. (Kongelige Veterinaer- og Landbohoejskole, Copenhagen (Denmark))

    1982-01-01

    Distribution of Ca, Pb, Cd, Zn, Fe and Mn has been investigated in the earthworm species Lumbricus terrestris, Aporectodea longa and A. rosea by atomic absorption and X-ray fluorescence spectrometry measurements. The material of L. terrestris originated from the garden of the Royal Veterinary and Agricultural University in central Copenhagen. Material of the other two species was sampled in sewage sludge treated plots. It was found that lead and cadmium are accumulated in the gut wall and from here transferred to waste nodules (brown bodies). In L. terrestris more lead was transferred to waste nodules than cadmium. Also large amounts of zinc were accumulated in the gut wall. Analyses of L. terrestris calciferous glands showed that these take part in regulation and excretion of a number of heavy metals. Lead and cadmium content was low in the ventral nerve chord and seminal vesicles. A. longa with poorly developed calciferous glands seems to rely more on waste nodule formation in the ultimate immobilization of lead.

  14. Determination of trace amounts of lead in mussels by flow-injection flame atomic-absorption spectrometry coupled with on-line minicolumn preconcentration

    Energy Technology Data Exchange (ETDEWEB)

    Yebra, M.C.; Enriquez, M.F.; Garcia, A.; Moreno-Cid, A. [Dept. of Analytical Chemistry, Nutrition and Bromatology, Chemistry Faculty, Santiago Univ., Santiago de Compostela (Spain)

    2001-05-01

    A minicolumn packed with poly(aminophosphonic acid) chelating resin incorporated in an on-line preconcentration system for flame atomic-absorption spectrometry was used to determine ultratrace amounts of lead in mussel samples at {mu}g L{sup -1} level. The preconcentrated lead was eluted with hydrochloric acid and injected directly into the nebulizer for atomization in an air-acetylene flame for measurement. The performance characteristics of the determination of lead were: preconcentration factor 26.8 for 1 min preconcentration time, detection limit (3{sigma}) in the sample digest was 0.25 {mu}g g{sup -1} (dry weight) for a sample volume of 3.5 mL and 0.2 g sample (preconcentration time 1 min), precision (RSD) 2.3% for 25 {mu}g L{sup -1} and 2.0% for 50 {mu}g L{sup -1}. The sampling frequency was 45 h{sup -1}. The method was highly tolerant of interferences, and the results obtained for the determination of lead in a reference material testify to the applicability of the proposed procedure to the determination of lead at ultratrace level in biological materials such as mussel samples. (orig.)

  15. RAPID AND SENSITIVE DETERMINATION OF PALLADIUM USING HOMOGENEOUS LIQUID-LIQUID MICROEXTRACTION VIA FLOTATION ASSISTANCE FOLLOWED BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Mohammad Rezaee

    2015-05-01

    Full Text Available A method for the determination of trace amounts of palladium was developed using homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA followed by graphite furnace atomic absorption spectrometry (GFAAS. Ammonium pyrrolidine dithiocarbamate (APDC was used as a complexing agent. This was applied to determine palladium in three types of water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added to the extraction cell which contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Parameters affecting extraction efficiency were investigated and optimized. Under the optimum conditions, the calibration graph was linear in the range of 1.0-200 µg L-1 with a limit of detection of 0.3 µg L-1. The performance of the method was evaluated for the extraction and determination of palladium in water samples and satisfactory results were obtained. In order to verify the accuracy of the approach, the standard addition method was applied for the determination of palladium in spiked synthetic samples and satisfactory results were obtained.

  16. Preconcentration of trace amounts of lead in water samples with cetyltrimethylammonium bromide coated magnetite nanoparticles and its determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mohammad Faraji

    2016-11-01

    Full Text Available A sensitive and simple magnetic solid phase extraction procedure was presented for the preconcentration of lead ions in environmental water samples. In the present study, lead ions form complexes with 1-(2-pyridilazo-2-naphthol reagent (PAN in basic medium, and then are quantitatively extracted to the surface of cetyltrimethylammonium bromide (CTAB-coated magnetite nanoparticles (Fe3O4 NPs. After magnetic separation of adsorbent, the adsorbent was eluted with 0.5% (v/v HCl in methanol prior to its analysis by flame atomic absorption spectrometry (FAAS. The pH of sample, concentrations of PAN, amounts of CTAB and Fe3O4 NPs, sample volume and desorption conditions were optimized. Under optimum conditions, the calibration curve was linear in the range of 0.05–100 ng mL−1 with R2 = 0.9996. Detection and quantification limits of the proposed method were 0.005 and 0.05 ng mL−1, respectively. Enhancement factor of 1050 was achieved using this method to extract 1000 mL of different environmental water samples. Compared with conventional solid phase extraction methods, the advantages of this method still include easy preparation of sorbents, short times of sample pre-treatment, high extraction yield, and high breakthrough volume. It shows great analytical potential in preconcentration of lead from large volume water samples.

  17. A Green Preconcentration Method for Determination of Cobalt and Lead in Fresh Surface and Waste Water Samples Prior to Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Naeemullah

    2012-01-01

    Full Text Available Cloud point extraction (CPE has been used for the preconcentration and simultaneous determination of cobalt (Co and lead (Pb in fresh and wastewater samples. The extraction of analytes from aqueous samples was performed in the presence of 8-hydroxyquinoline (oxine as a chelating agent and Triton X-114 as a nonionic surfactant. Experiments were conducted to assess the effect of different chemical variables such as pH, amounts of reagents (oxine and Triton X-114, temperature, incubation time, and sample volume. After phase separation, based on the cloud point, the surfactant-rich phase was diluted with acidic ethanol prior to its analysis by the flame atomic absorption spectrometry (FAAS. The enhancement factors 70 and 50 with detection limits of 0.26 μg L−1 and 0.44 μg L−1 were obtained for Co and Pb, respectively. In order to validate the developed method, a certified reference material (SRM 1643e was analyzed and the determined values obtained were in a good agreement with the certified values. The proposed method was applied successfully to the determination of Co and Pb in a fresh surface and waste water sample.

  18. Selective determination of antimony(III) and antimony(V) in liver tissue by microwave-assisted mineralization and hydride generation atomic absorption spectrometry.

    Science.gov (United States)

    Rondón, C; Burguera, J L; Burguera, M; Brunetto, M R; Gallignani, M; De Peña, Y P

    1995-09-01

    Antimony(III) and antimony(V) species have been selectively determined in liver tissues by optimizing the acidic conditions for the evolution of stibine using the reduction with sodium borohydride. The results show that a response for Sb(III) of 0.5 to 20 microg l(-1) was selectively obtained from samples in a 1 mol l(-1) acetic acid medium. The best response for total antimony from 1 to 20 microg l(-1) is obtained after sample treatment with a 0.5 mol l(-1) sulfuric acid and 10% w/v potassium iodide. Microwave digestion has been necessary to release quantitatively antimony species from sample slurries. The amount of Sb(V) was calculated from the difference between the value for total antimony and Sb(III) concentrations. A relative standard deviation from 2.9 to 3.1% and a detection limit of 0.15 and 0.10 microg l(-1) for Sb(III) and total Sb has been obtained. The average accuracy exceeded 95% in all cases comparing the results obtained from recovery studies, electrothermal atomic absorption spectrometry and the analysis of certified reference materials.

  19. Development of a simple method for the determination of lead in lipstick using alkaline solubilization and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Soares, Aline Rodrigues; Nascentes, Clésia Cristina

    2013-02-15

    A simple method was developed for determining the total lead content in lipstick samples by graphite furnace atomic absorption spectrometry (GFAAS) after treatment with tetramethylammonium hydroxide (TMAH). Multivariate optimization was used to establish the optimal conditions of sample preparation. The graphite furnace heating program was optimized through pyrolysis and atomization curves. An aliquot containing approximately 50mg of the sample was mixed with TMAH and heated in a water bath at 60°C for 60 min. Using Nb as the permanent modifier and Pd as the chemical modifier, the optimal temperatures were 900°C and 1800°C for pyrolysis and atomization, respectively. Under optimum conditions, the working range was from 1.73 to 50.0 μg L(-1), with detection and quantification limits of 0.20 and 0.34 μg g(-1), respectively. The precision was evaluated under conditions of repeatability and intermediate precision and showed standard deviations of 2.37%-4.61% and 4.93%-9.75%, respectively. The % recovery ranged from 96.2% to 109%, and no significant differences were found between the results obtained using the proposed method and the microwave decomposition method for real samples. Lead was detected in 21 tested lipstick samples; the lead content in these samples ranged from 0.27 to 4.54 μg g(-1). Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Investigation of chemical modifiers for sulfur determination in diesel fuel samples by high-resolution continuum source graphite furnace molecular absorption spectrometry using direct analysis

    Energy Technology Data Exchange (ETDEWEB)

    Huber, Charles S. [Instituto Federal Sul-rio-grandense, Câmpus Pelotas, Pelotas, RS (Brazil); Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Universidade Federal de Santa Catarina, Departamento de Química, Florianópolis, SC (Brazil); Andrade, Jailson B. [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2015-06-01

    High-resolution continuum source graphite furnace molecular absorption spectrometry has been applied for sulfur determination in diesel fuel. The sharp rotational lines of the carbon monosulfide molecule (formed during the vaporization step) were used to measure the absorbance. The analytical line at 258.056 nm was monitored using the sum of three pixels. Different chemical modifiers were investigated and the mixture of palladium and magnesium was used as chemical modifier in combination with iridium as permanent modifier. L-Cysteine was chosen as sulfur standard and the calibration was done against aqueous standard solutions. The proposed method was applied for the analyses of four diesel samples: two S10 samples and two S500 samples. The trueness of the method was checked with a certified reference material (CRM) of sulfur in diesel fuel (NIST 2724b). Accurate results, for samples and CRM, were achieved after a dilution with propan-1-ol. The following figures of merit were obtained: characteristic mass of 17 ± 3 ng, limit of detection and limit of quantification of 1.4 mg kg{sup −1} and 4.7 mg kg{sup −1}, respectively. - Highlights: • Ir, Ru and Zr were investigated as permanent modifiers. • Ca, Mg, Pd and Pd/Mg were investigated as modifiers in solution. • Indirect determination of sulfur monitoring the molecular absorbance of the CS • Direct analysis of diesel samples using a dilution in propan-1-ol.

  1. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    Energy Technology Data Exchange (ETDEWEB)

    Virgilio, Alex; Nobrega, Joaquim A. [Department of Chemistry, Federal University of Sao Carlos, Post Office Box 676, 13560-970, Sao Carlos-SP (Brazil); Rego, Jardes F. [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil); Neto, Jose A. Gomes, E-mail: anchieta@iq.unesp.br [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil)

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 Degree-Sign C and 2400 Degree-Sign C, respectively. Slopes of calibration curves (50-750 pg Cr, R{sup 2} > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 {mu}g g{sup -1} Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 {+-} 2.1 {mu}g g{sup -1} Cr. The limit of detection was 3.3 ng g{sup -1} Cr. - Highlights: Black-Right-Pointing-Pointer Direct solid sampling is first time employed for Cr in plant materials. Black-Right-Pointing-Pointer Calibration curves with liquids and solids are coincident. Black-Right-Pointing-Pointer Microanalysis of plants for Cr is validated by reference materials. Black-Right-Pointing-Pointer The proposed HR-CS GF AAS method is environmental friendly.

  2. Determination of cadmium and lead in mussels by electrothermal atomic absorption spectrometry using an ultrasound-assisted extraction method optimized by factorial design

    Energy Technology Data Exchange (ETDEWEB)

    Lavilla, I.; Capelo, J.L.; Bendicho, C. [Departamento de Quimica Analitica y Alimentaria, Universidad de Vigo, Facultad de Ciencias (Quimicas), As Lagoas - Marcosende s/n. E-36200 Vigo (Spain)

    1999-02-01

    A simple and rapid method is described for the quantitative extraction and determination of Cd and Pb in mussel tissue (Mytilus edulis). The method is based on the quantitative ultrasound-assisted extraction (i.e. sample mass at mg level) of the two metals using diluted nitric acid as extractant. The extraction procedure is carried out in autosampler cups of the graphite furnace (typically, less than 20 mg). A two-level full factorial design (2{sup 4}) was applied to optimize the variables influencing the ultrasound extraction process. These variables were: extraction time, ultrasound amplitude, nitric acid concentration and particle size. Optimization results showed that acid concentration and particle size were the more significant variables. Determination of Cd and Pb in extracts obtained after ultrasound treatment was carried out by Electrothermal Atomic Absorption Spectrometry. The method was validated by statistically comparing the metal contents found with the certified ones corresponding to the BCR 278 mussel tissue. No significant differences were observed for P= 0.05. LODs for Cd and Pb in mussel tissue were 0.019 and 0.37 {mu}g g{sup -1}. RSDs values (corresponding to between-batch precision for n= 5) were 2.2 and 6.7% for Cd and Pb, respectively. The method was applied to measure the contents of Cd and Pb in mussels used as pollution bioindicators from the Galician coast (Ria de Vigo, Spain). (orig.) With 2 figs., 9 tabs., 6 refs.

  3. Removal, preconcentration and determination of Ni(II from different environmental samples using modified magnetite nanoparticles prior to flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mohammad Ali Karimi

    2015-11-01

    Full Text Available In this paper, a simple, fast and reliable solid phase extraction (SPE method to determine Ni(II using dimethylglyoxim/sodium dodecyl sulfate-immobilized on alumina-coated magnetite nanoparticles (DMG/SDS-ACMNPs as a new adsorbent prior to its determination by flame atomic absorption spectrometry (FAAS is described. Under the optimal experimental conditions, the preconcentration factor, detection limit, linear range and relative standard deviation (RSD of nickel(II ions were 320 (for 800 mL of sample solution, 4.6 ng mL−1, 10.0–100.0 ng mL−1 and 1.9% (for 50.0 ng mL−1, n = 7, respectively. This method avoided the time-consuming column-passing process of loading large volume samples in traditional SPE through the rapid isolation of DMG/SDS-ACMNPs with an adscititious magnet. The proposed method was successfully applied to determine the content of Ni(II in soil, spinach, tomato, black tea, tobacco and different water samples and suitable recoveries were obtained.

  4. Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

    Science.gov (United States)

    de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

    2017-08-15

    Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl(-1), respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl(-1). Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Application of high-resolution continuum source flame atomic absorption spectrometry to reveal, evaluate and overcome certain spectral effects in Pb determination of unleaded gasoline

    Science.gov (United States)

    Kowalewska, Zofia; Laskowska, Hanna; Gzylewski, Michał

    2017-06-01

    High-resolution continuum source and line source flame atomic absorption spectrometry (HR-CS FAAS and LS FAAS, respectively) were applied for Pb determination in unleaded aviation or automotive gasoline that was dissolved in methyl-isobutyl ketone. When using HR-CS FAAS, a structured background (BG) was registered in the vicinity of both the 217.001 nm and 283.306 nm Pb lines. In the first case, the BG, which could be attributed to absorption by the OH molecule, directly overlaps with the 217 nm line, but it is of relatively low intensity. For the 283 nm line, the structured BG occurs due to uncompensated absorption by OH molecules present in the flame. BG lines of relatively high intensity are situated at a large distance from the 283 nm line, which enables accurate analysis, not only when using simple variants of HR-CS FAAS but also for LS FAAS with a bandpass of 0.1 nm. The lines of the structured spectrum at 283 nm can have ;absorption; (maxima) or ;emission; (minima) character. The intensity of the OH spectra can significantly depend on the flame character and composition of the investigated organic solution. The best detection limit for the analytical procedure, which was 0.01 mg L- 1 for Pb in the investigated solution, could be achieved using HR-CS FAAS with the 283 nm Pb line, 5 pixels for the analyte line measurement and iterative background correction (IBC). In this case, least squares background correction (LSBC) is not recommended. However, LSBC (available as the ;permanent structures; option) would be recommended when using the 217 nm Pb line. In LS FAAS, an additional phenomenon related to the nature of the organic matrix (for example, isooctane or toluene) can play an important role. The effect is of continuous character and probably due to the simultaneous efficient correction of the continuous background (IBC) it is not observed in HR-CS FAAS. The fact that the effect does not depend on the flame character indicates that it is not radiation

  6. Fast heating induced impulse halogenation of refractory sample components in electrothermal atomic absorption spectrometry by direct injection of a liquid halogenating agent.

    Science.gov (United States)

    György, Krisztina; Ajtony, Zsolt; Van Meel, Katleen; Van Grieken, René; Czitrovszky, Aladár; Bencs, László

    2011-09-15

    A novel electrothermal atomic absorption spectrometry (ETAAS) method was developed for the halogenation of refractory sample components (Er, Nd and Nb) of lithium niobate (LiNbO(3)) and bismuth tellurite (Bi(2)TeO(5)) optical single crystals to overcome memory effects and carry-over. For this purpose, the cleaning step of a regular graphite furnace heating program was replaced with a halogenation cycle. In this cycle, after the graphite tube cooled to room temperature, a 20 μL aliquot of liquid carbon tetrachloride (CCl(4)) was dispensed with a conventional autosampler into the graphite tube. The CCl(4) was partially dried at 80°C under the mini-flow (40 cm(3) min(-1)) condition of the Ar internal furnace gas (IFG), then the residue was decomposed (pyrolyzed) by fast furnace heating at 1900-2100°C under interrupted flow of the IFG. This step was followed by a clean-out stage at 2100°C under the maximum flow of the IFG. The advantage of the present method is that it does not require any alteration to the graphite furnace gas supply system in contrast to most of the formerly introduced halogenation techniques. The effectiveness of the halogenation method was verified with the determination of Er and Nd dopants in the optical crystals. In these analyses, a sensitivity decrease was observed, which was likely due to the enhanced deterioration of the graphite tube surface. Therefore, the application of mathematical correction (resloping) of the calibration was also required. The calibration curves were linear up to 1.5 and 10 μmol L(-1) for Er and Nd, respectively. Characteristic masses of 18 and 241 pg and the limit of detection (LOD) values of 0.017 and 0.27 μmol L(-1) were found for Er and Nd, respectively. These LOD data correspond to 0.68 μmol mol(-1) Er and 11 μmol mol(-1) Nd in solid bismuth tellurite samples. The analytical results were compared with those obtained by a conventional ETAAS method and validated with X-ray fluorescence spectrometry analysis

  7. Determination of trace amounts of selenium in minerals and rocks by flame less atomic-absorption spectrometry; Determinacion de selinio en minerales y rocas por espectrometria de absorcion atomica

    Energy Technology Data Exchange (ETDEWEB)

    Alduan, F. A.; Capdevilla, C.

    1980-07-01

    The determination of trace amounts of selenium In silicate rocks and feldspar by solvent extraction and graphite furnace atomic-absorption spectrometry has been stu- died. Sodium diethyl-ditio carbamate and ammonium pyrrolidine dithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted Into carbon tetrachloride as the sodium diethyldithiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (Author) 7 refs.

  8. Determination of Cd, Co, Cu, Mn, Ni, Pb, and Zn by Inductively Coupled Plasma Mass Spectroscopy or Flame Atomic Absorption Spectrometry after On-line Preconcentration and Solvent Extraction by Flow Injection System

    Science.gov (United States)

    Bortoli; Gerotto; Marchiori; Mariconti; Palonta; Troncon

    1996-11-01

    The concentrations of Cd, Co, Cu, Mn, Ni, Pb, and Zn in natural and sea waters are too low to be directly determined with by flame atomic absorption spectrometry (FAAS) or graphite furnace atomic absorption spectrometry (GFAAS). Specific sample preparations are requested that make possible the determination of these analytes by preconcentration or extraction. These techniques are affected by severe problems of sample contamination. In this work Cd, Co, Cu, Mn, Ni, Pb, and Zn were determined by inductively coupled plasma mass spectroscopy (ICP-MS) or by atomic absorption spectrometry, in fresh and seawater samples, after on-line preconcentration and following solvent elution with a flow injection system. Bonded silica with octadecyl functional group C18, packed in a microcolumn of 100-μl capacity, was used to collect diethyldithiocarbamate complexes of the heavy metals in aqueous solutions. The metals are complexed with a chelating agent, adsorbed on the C18 column, and eluted with methanol directly in the flow injection system. The methanolic stream can be addressed to FAAS for direct determination of Cu, Ni, and Zn, or collected in a vial for successive analysis by GFAAS. The eluted samples can be also dried in a vacuum container and restored to a little volume with concentrated HNO3 and Milli-Q water for analysis by ICP-MS or GFAAS.

  9. Preconcentration and determination of vanadium and molybdenum in milk, vegetables and foodstuffs by ultrasonic-thermostatic-assisted cloud point extraction coupled to flame atomic absorption spectrometry.

    Science.gov (United States)

    Gürkan, Ramazan; Korkmaz, Sema; Altunay, Nail

    2016-08-01

    A new ultrasonic-thermostatic-assisted cloud point extraction procedure (UTA-CPE) was developed for preconcentration at the trace levels of vanadium (V) and molybdenum (Mo) in milk, vegetables and foodstuffs prior to determination via flame atomic absorption spectrometry (FAAS). The method is based on the ion-association of stable anionic oxalate complexes of V(V) and Mo(VI) with [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) at pH 4.5, and then extraction of the formed ion-association complexes into micellar phase of polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5). The UTA-CPE is greatly simplified and accelerated compared to traditional cloud point extraction (CPE). The analytical parameters optimized are solution pH, the concentrations of complexing reagents (oxalate and Nile blue A), the PONPE 7.5 concentration, electrolyte concentration, sample volume, temperature and ultrasonic power. Under the optimum conditions, the calibration curves for Mo(VI) and V(V) are obtained in the concentration range of 3-340µgL(-1) and 5-250µgL(-1) with high sensitivity enhancement factors (EFs) of 145 and 115, respectively. The limits of detection (LODs) for Mo(VI) and V(V) are 0.86 and 1.55µgL(-1), respectively. The proposed method demonstrated good performances such as relative standard deviations (as RSD %) (≤3.5%) and spiked recoveries (95.7-102.3%). The accuracy of the method was assessed by analysis of two standard reference materials (SRMs) and recoveries of spiked solutions. The method was successfully applied into the determination of trace amounts of Mo(VI) and V(V) in milk, vegetables and foodstuffs with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.; Teixeira, Leonardo S. G.

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box-Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L- 1 HNO3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg- 1. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method.

  11. Ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry for a sensitive determination of cadmium in water samples

    Science.gov (United States)

    Li, Shengqing; Cai, Shun; Hu, Wei; Chen, Hao; Liu, Hanlan

    2009-07-01

    A new method was developed for the determination of cadmium in water samples using ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (IL-based USA-DLLME) followed by electrothermal atomic absorption spectrometry (ETAAS). The IL-based USA-DLLME procedure is free of volatile organic solvents, and there is no need for a dispersive solvent, in contrast to conventional DLLME. The ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate (HMIMPF 6), was quickly disrupted by an ultrasonic probe for 1 min and dispersed in water samples like a cloud. At this stage, a hydrophobic cadmium-DDTC complex was formed and extracted into the fine droplets of HMIMPF 6. After centrifugation, the concentration of the enriched cadmium in the sedimented phase was determined by ETAAS. Some effective parameters of the complex formation and microextraction, such as the concentration of the chelating agent, the pH, the volume of the extraction solvent, the extraction time, and the salt effect, have been optimized. Under optimal conditions, a high extraction efficiency and selectivity were reached for the extraction of 1.0 ng of cadmium in 10.0 mL of water solution employing 73 µL of HMIMPF 6 as the extraction solvent. The enrichment factor of the method is 67. The detection limit was 7.4 ng L - 1 , and the characteristic mass ( m0, 0.0044 absorbance) of the proposed method was 0.02 pg for cadmium (Cd). The relative standard deviation (RSD) for 11 replicates of 50 ng L - 1 Cd was 3.3%. The method was applied to the analysis of tap, well, river, and lake water samples and the Environmental Water Reference Material GSBZ 50009-88 (200921). The recoveries of spiked samples were in the range of 87.2-106%.

  12. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Jorge S.; Anunciação, Taiana A. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Brandão, Geovani C. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); INCT de Energia e Ambiente, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Dantas, Alailson F. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Lemos, Valfredo A. [Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, Jequié, Bahia 45506-191 (Brazil); and others

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO{sub 3} gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L{sup −1} HNO{sub 3} as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg{sup −1}. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and

  13. Trace determination of lead, chromium and cadmium in herbal medicines using ultrasound-assisted emulsification microextraction combined with graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Aghamohammadi, Mohammad; Faraji, Mahya; Shahdousti, Parvin; Kalhor, Hamideh; Saleh, Abolfazl

    2015-01-01

    The World Health Organization (WHO) recommends that medicinal plants should be checked for the presence of heavy metals. A preconcentration and separation technique for trace amounts of heavy metals from plant matrix is necessary in order to increase the sensitivity and precision of their determination. Lead, chromium and cadmium contaminations in herbal medicines were monitored using ultrasound-assisted emulsification microextraction (USAEME) combined with graphite furnace atomic absorption spectrometry (GF-AAS). In this work, the metal ions in the aqueous solution were complexed with ammonium pyrrolidine dithiocarbamate (APDC) and were extracted into 45 μL of toluene that was sonically dispersed in the aqueous phase. The emulsion formed was centrifuged and 20 μL of separated toluene was injected into a GF-AAS for analysis. Several factors including the kind of extraction solvent and its volume, sample pH, ionic strength and concentration of APDC were optimised. The linear dynamic range (LDR) values were in the range of 0.05 to 20 µg/L and the limit of detection values were in the range of 0.002-0.03 µg/L for target heavy metals. Enrichment factors were obtained in the range of 70-500. The precision of the proposed method was ≤ 8% (n = 5). The obtained amounts of Pb, Cr and Cd in selected herbal medicines were in the standard range, according to the WHO reports. The USAEME with GF-AAS procedure was shown to be an efficient, rapid, inexpensive and eco-friendly method for the determination of lead, chromium and cadmium in herbal medicines. Application of the USAEME method leads to an increased extraction efficiency with satisfactory precision in a short time using an extraction solvent volume at the microlitre level. Copyright © 2015 John Wiley & Sons, Ltd.

  14. Simultaneous determination of antimony and boron in beverage and dairy products by flame atomic absorption spectrometry after separation and pre-concentration by cloud-point extraction.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan

    2016-01-01

    A new cloud-point extraction (CPE) method was developed for the pre-concentration and simultaneous determination of Sb(III) and B(III) by flame atomic absorption spectrometry (FAAS). The method was based on complexation of Sb(III) and B(III) with azomethine-H in the presence of cetylpyridinium chloride (CPC) as a signal-enhancing agent, and then extraction into the micellar phase of Triton X-114. Under optimised conditions, linear calibration was obtained for Sb(III) and B(III) in the concentration ranges of 0.5-180 and 2.5-600 μg l(-1) with LODs of 0.15 and 0.75 μg l(-1), respectively. Relative standard deviations (RSDs) (25 and 100 μg l(-1) of Sb(III) and B(III), n = 6) were in a range of 2.1-3.8% and 1.9-2.3%, respectively. Recoveries of spiked samples of Sb(III) and B(III) were in the range of 98-103% and 99-102%, respectively. Measured values for Sb and B in three standard reference materials were within the 95% confidence limit of the certified values. Also, the method was used for the speciation of inorganic antimony. Sb(III), Sb(V) and total Sb were measured in the presence of excess boron before and after pre-reduction with an acidic mixture of KI-ascorbic acid. The method was successfully applied to the simultaneous determination of total Sb and B in selected beverage and dairy products.

  15. Speciation analysis of volatile and non-volatile vanadium compounds in Brazilian crude oils using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lepri, Fabio G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil)]. E-mail: welz@qmc.ufsc.br; Borges, Daniel L.G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Silva, Alessandra F. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Vale, Maria Goreti R. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Heitmann, Uwe [ISAS - Institute of Analytical Sciences, Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany)

    2006-02-03

    A method is proposed that makes possible determining total and 'thermally stable' vanadium in crude oil without prior separation, and to calculate 'volatile' vanadium by difference. The volatile fraction is believed to be largely vanadyl porphyrine complexes. The method is based on the unsurpassed background correction capability of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS), which allows pyrolysis temperatures as low as 300 deg. C to be used. The samples were prepared as oil-in-water emulsions, and aqueous standards emulsified in the same way were used for calibration. Total vanadium has been determined using a pyrolysis temperature of 400 deg. C, and 'thermally stable' vanadium using a pyrolysis temperature of 800 deg. C. The content of total vanadium in 12 Brazilian crude oil samples was found to be between less than 0.04 and about 30 mg kg{sup -1}. The volatile fraction was between 5 and 51% of the total content, and there was no correlation between the total and the volatile vanadium content. The limits of detection and quantification were 0.04 and 0.12 mg kg{sup -1} of V in crude oil, respectively, based on a mass of 2 g of oil in 10 mL of emulsion. The precision was better than 4% at the 3 mg kg{sup -1} level and better than 1.5% at the 30 mg kg{sup -1} level of V in crude oil.

  16. Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mirabi, Ali; Dalirandeh, Zeinab [Department of Chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of); Rad, Ali Shokuhi, E-mail: a.shokuhi@qaemshahriau.ac.ir [Department of Chemical Engineering, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of)

    2015-05-01

    A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe{sub 3}O{sub 4} as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L{sup −1} HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml{sup −1} and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results. - Highlights: • MNPs method is economical, simple, rapid and sensitive for trace analysis of Cd. • High preconcentration factor was obtained easily through this method. • A detection limit at ng mL{sup −1} level was achieved with 100.0 mL of sample. • This method provides good repeatability and extraction efficiency in a short time.

  17. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Martinis, Estefanía M. [Laboratory of Analytical Chemistry for Research and Development (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo, Padre J. Contreras 1300, (5500) Mendoza (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina); Lascalea, Gustavo E. [Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Laboratory of Analytical Chemistry for Research and Development (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo, Padre J. Contreras 1300, (5500) Mendoza (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina)

    2015-01-01

    A flow injection system based on a modified polytetrafluoroethylene (PTFE) knotted reactor (KR) was developed for arsenite [As(III)] and arsenate [As(V)] species preconcentration and determination by electrothermal atomic absorption spectrometry (ETAAS). Activated carbon (AC) was immobilized on the inner walls of a PTFE KR by a thermal treatment. A significant increase in analyte retention was obtained with the AC-modified KR (100%) as compared to the regular PTFE KR (25%). The preconcentration method involved the on-line formation of As(III)-ammonium pyrrolidinedithiocarbamate (As-APDC) complex, followed by its adsorption onto the inner walls of the AC-modified KR. After analyte retention, the complex was eluted with acetone directly into the graphite furnace of ETAAS. The parameters affecting the flow injection system were evaluated with a full central composite face centered design with three center points. Under optimum conditions, a preconcentration factor of 200 was obtained with 10 ml of sample. The detection limit was 4 ng L{sup −1} and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L{sup −1} of As were 4.3% and 4.7% for As(III) and As(V), respectively. The developed methodology was highly selective towards As(III), while As(V), monomethylarsonic acid [MMA(V)] and dimethylarsinic [DMA(V)] were not retained in the AC-modified KR. The proposed method was successfully applied for As speciation analysis in infusions originated from medicinal herbs and tea. - Highlights: • We report an efficient method for As speciation. • We have modified a knotted reactor with activated carbon for high sorption capacity. • We provide a simple procedure for surface modification of a PTFE knotted reactor. • We have selectively separated inorganic As species from complex matrix samples. • We have implemented a modified KR in a flow injection system coupled to ETAAS.

  18. Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

    2018-03-01

    A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Trace determination of lead in lipsticks and hair dyes using microwave-assisted dispersive liquid-liquid microextraction and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Sharafi, K; Fattahi, N; Pirsaheb, M; Yarmohamadi, H; Fazlzadeh Davil, M

    2015-10-01

    A novel microwave-assisted dispersive liquid-liquid microextraction (MADLLME) technique according to the solidification of a floating organic droplet (SFO) and graphite furnace atomic absorption spectrometry (GFAAS) used for the extraction and determination of lead ions in lipsticks and hair dyes made in different countries. Lipstick and hair dye samples of different brands and colours were collected from local market in Kermanshah, Iran. After sample treatment with microwave-assisted acid digestion, an appropriate mixture of acetone, 1-undecanol and diethyl dithiophosphoric acid was injected rapidly into the aqueous sample containing lead ions, and as a result, cloudy mixture was formed. After centrifugation, the test tube was cooled for few minutes. The solidified 1-undecanol on top of the solution was transferred into a suitable vial and injected into the analytical instrument. Under the optimum experimental conditions (extraction solvent: 30 μL of 1-undecanol; disperser solvent: 500 μL of acetone; ligand concentration: 0.15% (v/v); pH: ~1.5 and without salt added), the enhancement factor of 96 was obtained. The calibration graphs were linear in the range of 0.3-50 μg kg(-1) with a correlation coefficient (r(2) ) more than 0.995. The detection limit was 0.1 μg kg(-1) . Consequently, the developed method was successfully applied to extract and determine lead ions in the lipsticks and hair dyes, and favourable results were obtained. The proposed method which applied in cosmetics showed excellent relative recoveries (90-109.7%) with relative standard deviations market is far below the recommended limits as applied in Germany (20 mg kg(-1) ) and Canada (10 mg kg(-1) ) and confirmed that very low levels of lead are technically available in the final cosmetic products. © 2015 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

  20. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    Science.gov (United States)

    Brum, Daniel M.; Lima, Claudio F.; Robaina, Nicolle F.; Fonseca, Teresa Cristina O.; Cassella, Ricardo J.

    2011-05-01

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO 3, the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO 3 medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  1. Determination of Pb (Lead), Cd (Cadmium), Cr (Chromium), Cu (Copper), and Ni (Nickel) in Chinese tea with high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Zhong, Wen-Si; Ren, Ting; Zhao, Li-Jiao

    2016-01-01

    The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5%) and recoveries (98.91-101.32%). The lead contents in tea leaves were 0.48-10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73-63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea. Copyright © 2015. Published by Elsevier B.V.

  2. Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

    2016-02-05

    An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be <5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L(-1) and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Optimization of a novel setup for an on-line study of elemental mercury adsorption by cold-vapor atomic absorption spectrometry.

    Science.gov (United States)

    Assari, Mohammad Javad; Rezaee, Abbas; Jonidi Jafari, Ahmad; Bahrami, Abdolrahman

    2013-05-29

    The objective of this work was developing a simple and stable time-based on-line setup for assessing the potential of mercury (Hg) vapor adsorption of the commercial sorbents used in air sampling and control operation followed by cold vapor atomic absorption spectrometry (CVAAS). A special designed separation chamber was used where reduction of the injected Hg (II) solution took place. Purge gas passes through this chamber resulting to a prompt release of mercury vapor, purging into the adsorbent that regulated at the desired adsorption temperature. After sorbent saturation, in order to study the adsorption parameters of sorbents (activated carbon and bone char) such as breakthrough time (BTT), and adsorptive capacity, mercury gas stream was passed through the sorbents, directly transport to the CVAAS. Preliminary experiments concerning the reductant solution showed that SnCl2 offers higher stability than NaBH4. Around the loading range 0.125-2.5 ml min⁻¹ of 100 µg l⁻¹ Hg(II) solution, a linear calibration curve with the equation peak area=0.134; loading flow=-0.017 and a correlation coefficient r=0.996 was obtained, and the detection limit was improved up to c(L)=1 µg l⁻¹. The relative standard deviation of five measurements of lowest flow loading of Hg (II) was RSD=2.8%. The significant differences were observed in the breakthrough time and mercury adsorptive capacity between activated carbon and bone char (P=0.010). This novel setup is suitable for an on-line study of elemental mercury adsorption, determination of breakthrough time and adsorption capacity, and because of its stable performance during all experiments; it can be applied to the time based studies.

  4. Cloud point extraction-flame atomic absorption spectrometry for pre-concentration and determination of trace amounts of silver ions in water samples.

    Science.gov (United States)

    Yang, Xiupei; Jia, Zhihui; Yang, Xiaocui; Li, Gu; Liao, Xiangjun

    2017-03-01

    A cloud point extraction (CPE) method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS) The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I)/diethyldithiocarbamate (DDTC) complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I)/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL-1 Ag+ in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL-1 for both Zn2+ and Cu2+, 80 μg·mL-1 for Pb2+, 1000 μg·mL-1 for Mn2+, and 100 μg·mL-1 for both Cd2+ and Ni2+. The calibration curve was linear in the range of 1-500 ng·mL-1 with a limit of detection (LOD) at 0.3 ng·mL-1. The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.

  5. Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

    Science.gov (United States)

    Sadeghi, Susan; Ashoori, Vahid

    2017-10-01

    The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL-1 , respectively, with a detection limit of 6.9 ng mL-1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  6. Coupling of non-selective adsorption with selective elution for novel in-line separation and detection of cadmium by vapour generation atomic absorption spectrometry.

    Science.gov (United States)

    Zhang, Yanlin; Adeloju, Samuel B

    2015-05-01

    Non-selective adsorption of Cd(2+) ions on a cation exchange fiber and subsequent selective elution with a KI solution has been strategically utilized to develop a highly selective in-line separation of Cd(2+) ions from other metal ions for its rapid and reliable quantification by cold vapour-atomic absorption spectrometry. After retention of Cd(2+) with a high efficiency on cation exchange fiber, selective elution of the retained Cd(2+) was subsequently accomplished with 0.3M KI. Vapour generation of Cd for in-line CV-AAS determination was then achieved by merging the eluate with HCl and NaBH4. Interferences from most base metals with the vapour generation of Cd were eliminated by this approach, with the exception of Pb(2+)ions which was removed by co-precipitation with BaSO4 prior to the in-line separation. Substantial improvement in sensitivity of the in-line CV-AAS determination of Cd was achieved by increasing the sample loading time. A detection limit of 0.6 ng L(-1) (3σ) was obtained with sample loading time of 120 s, corresponding to a consumption of 24 mL of sample solution. Application of the method to the determination of Cd in certified sediment and fish samples gave a good agreement with the certified values. Further validation by recovery study in real fish sample digests and water gave average Cd recoveries of 98.7±1.0% for fish and 92±3% for water with RSD of 1.5% for fish and 4% for water, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. A new supramolecular based liquid solid microextraction method for preconcentration and determination of trace bismuth in human blood serum and hair samples by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Kahe, Hadi; Chamsaz, Mahmoud

    2016-11-01

    A simple and reliable supramolecule-aggregated liquid solid microextraction method is described for preconcentration and determination of trace amounts of bismuth in water as well as human blood serum and hair samples. Catanionic microstructures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) surfactants, dissolved in deionized water/propanol, are used as a green solvent to extract bismuth (III)-diethyldithiocarbamate complexes by dispersive microextraction methodology. The extracted solid phase is easily removed and dissolved in 50 μL propanol for subsequent measurement by electrothermal atomic absorption spectrometry (ET-AAS). The procedure benefits the merits of supramolecule aggregates' properties and dispersive microextraction technique using water as the main component of disperser solvent, leading to direct interaction with analyte. Phase separation behavior of extraction solvent and different parameters influencing the extraction efficiency of bismuth ion such as salt concentration, pH, centrifugation time, amount of chelating agent, SDS:CTAB mole ratio, and solvent amounts were thoroughly optimized. Under the optimal experimental conditions, the calibration curve was linear in the range of 0.3-6 μg L-1 Bi (III) with a limit of detection (LOD) of 0.16 μg L-1 (S/N = 3). The relative standard deviations (RSD) of determination were obtained to be 5.1 and 6.2 % for 1 and 3 μg L-1 of Bi (III), respectively. The developed method was successfully applied as a sensitive and accurate technique for determination of bismuth ion in human blood serum, hair samples, and a certified reference material.

  8. Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by flame atomic absorption spectrometry.

    Science.gov (United States)

    Carletto, Jeferson Schneider; Luciano, Raquel Medeiros; Bedendo, Gizelle Cristina; Carasek, Eduardo

    2009-04-06

    A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML(2)). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5x10(-2) mol L(-1), extraction temperature 40 degrees C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 microL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 microL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 microg L(-1), relative standard deviation (RSD) 5.5% and the working linear range 2-30 microg L(-1).

  9. Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

    Science.gov (United States)

    Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

    2013-11-15

    A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. A sensitive magnetic nanoparticle-based immunoassay of phosphorylated acetylcholinesterase using protein cage templated lead phosphate for signal amplification with graphite furnace atomic absorption spectrometry detection.

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Yang, Enjian; Ge, Xiaoxiao; Du, Dan; Lin, Yuehe

    2016-04-07

    We developed a new magnetic nanoparticle sandwich-like immunoassay using protein cage nanoparticles (PCN) for signal amplification together with graphite furnace atomic absorption spectrometry (GFAAS) for the quantification of an organophosphorylated acetylcholinesterase adduct (OP-AChE), the biomarker of exposure to organophosphate pesticides (OPs) and nerve agents. OP-AChE adducts were firstly captured by titanium dioxide coated magnetic nanoparticles (TiO2-MNPs) from the sample matrixes through metal chelation with phospho-moieties, and then selectively recognized by anti-AChE antibody labeled on PCN which was packed with lead phosphate in its cavity (PCN-anti-AChE). The sandwich-like immunoreaction was performed among TiO2-MNPs, OP-AChE and PCN-anti-AChE to form a TiO2-MNP/OP-AChE/PCN-anti-AChE immunocomplex. The complex could be easily isolated from the sample solution with the help of magnet, and the released lead ions from PCN were detected by GFAAS for the quantification of OP-AChE. Greatly enhanced sensitivity was achieved because PCN increased the amount of metal ions in the cavity of each apoferritin. The proposed immunoassay yielded a linear response over a broad range of OP-AChE concentrations from 0.01 nM to 2 nM, with a detection limit of 2 pM, which has enough sensitivity for monitoring of low-dose exposure to OPs. This new method showed an acceptable stability and reproducibility and was validated with OP-AChE spiked human plasma.

  11. Hollow fiber liquid phase microextraction combined with electrothermal atomic absorption spectrometry for the speciation of arsenic (III) and arsenic (V) in fresh waters and human hair extracts

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Hongmei [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn; Chen Beibei; Xia Linbo [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2009-02-16

    A new method of hollow fiber liquid phase microextraction (HF-LPME) using ammonium pyrrolidine dithiocarbamate (APDC) as extractant combined with electrothermal atomic absorption spectrometry (ETAAS) using Pd as permanent modifier has been described for the speciation of As(III) and As(V). In a pH range of 3.0-4.0, the complex of As(III)-APDC complex can be extracted using toluene as the extraction solvent leaving As(V) in the aqueous layer. The post extraction organic phase was directly injected into ETAAS for the determination of As(III). To determine total arsenic in the samples, first As(V) was reduced to As(III) by L-cysteine, and then a microextraction method was performed prior to the determination of total arsenic. As(V) assay was based on subtracting As(III) form the total arsenic. All parameters, such as pH of solution, type of organic solvent, the amount of APDC, stirring rate and extraction time, affecting the separation of As(III) from As(V) and the extraction efficiency of As(III) were investigated, and the optimized extraction conditions were established. Under optimized conditions, a detection limit of 0.12 ng mL{sup -1} with enrichment factor of 78 was achieved. The relative standard deviation (R.S.D.) of the method for five replicate determinations of 5 ng mL{sup -1} As(III) was 8%. The developed method was applied to the speciation of As(III) and As(V) in fresh water and human hair extracts, and the recoveries for the spiked samples are 86-109%. In order to validate the developed method, three certified reference materials such as GBW07601 human hair, BW3209 and BW3210 environmental water were analyzed, and the results obtained were in good agreement with the certified values provided.

  12. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    Science.gov (United States)

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

  13. Fast determination of trace elements in organic fertilizers using a cup-horn reactor for ultrasound-assisted extraction and fast sequential flame atomic absorption spectrometry.

    Science.gov (United States)

    Teixeira, Leonel Silva; Vieira, Heulla Pereira; Windmöller, Cláudia Carvalhinho; Nascentes, Clésia Cristina

    2014-02-01

    A fast and accurate method based on ultrasound-assisted extraction in a cup-horn sonoreactor was developed to determine the total content of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn in organic fertilizers by fast sequential flame atomic absorption spectrometry (FS FAAS). Multivariate optimization was used to establish the optimal conditions for the extraction procedure. An aliquot containing approximately 120 mg of the sample was added to a 500 µL volume of an acid mixture (HNO3/HCl/HF, 5:3:3, v/v/v). After a few minutes, 500 µL of deionized water was added and eight samples were simultaneously sonicated for 10 min at 50% amplitude, allowing a sample throughput of 32 extractions per hour. The performance of the method was evaluated with a certified reference material of sewage sludge (CRM 029). The precision, expressed as the relative standard deviation, ranged from 0.58% to 5.6%. The recoveries of analytes were found to 100%, 109%, 96%, 92%, 101%, 104% and 102% for Cd, Cr, Cu, Mn, Ni, Pb and Zn, respectively. The linearity, limit of detection and limit of quantification were calculated and the values obtained were adequate for the quality control of organic fertilizers. The method was applied to the analysis of several commercial organic fertilizers and organic wastes used as fertilizers, and the results were compared with those obtained using the microwave digestion procedure. A good agreement was found between the results obtained by microwave and ultrasound procedures with recoveries ranging from 80.4% to 117%. Two organic waste samples were not in accordance with the Brazilian legislation regarding the acceptable levels of contaminants. © 2013 Published by Elsevier B.V.

  14. Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry.

    Science.gov (United States)

    Torres, Daiane Placido; Martins-Teixeira, Maristela Braga; Cadore, Solange; Queiroz, Helena Müller

    2015-01-01

    A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg(-1) (square regression) and 250.0 and 2000.0 μg kg(-1) (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg(-1), respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.

  15. Determination of Pb (Lead, Cd (Cadmium, Cr (Chromium, Cu (Copper, and Ni (Nickel in Chinese tea with high-resolution continuum source graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Wen-Si Zhong

    2016-01-01

    Full Text Available The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5% and recoveries (98.91–101.32%. The lead contents in tea leaves were 0.48–10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73–63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea.

  16. L-Tyrosine immobilized on multiwalled carbon nanotubes: A new substrate for thallium separation and speciation using stabilized temperature platform furnace-electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pacheco, Pablo H.; Gil, Raul A. [Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, P.O. Box 375, 5700 San Luis (Argentina); Instituto de Quimica de San Luis (INQUISAL-CONICET), Chacabuco y Pedernera, CP 5700, San Luis (Argentina); Smichowski, Patricia, E-mail: smichows@cnea.gov.ar [Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Rivadavia 1917, CP C1033 AAJ, Ciudad de Buenos Aires (Argentina); Comision Nacional de Energia Atomica, Gerencia Quimica, Av. Gral. Paz 1499, B1650KNA San Martin (Argentina); Polla, Griselda [Comision Nacional de Energia Atomica, Gerencia de Investigacion y Aplicaciones, Av.Gral. Paz 1499, B1650KNA San Martin (Argentina); Martinez, Luis D., E-mail: ldm@unsl.edu.ar [Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, P.O. Box 375, 5700 San Luis (Argentina); Instituto de Quimica de San Luis (INQUISAL-CONICET), Chacabuco y Pedernera, CP 5700, San Luis (Argentina)

    2009-12-10

    An approach for the separation and determination of inorganic thallium species is described. A new sorbent, L-tyrosine-carbon nanotubes (L-tyr-CNTs), was used and applied to the analysis of tap water samples. At pH 5.0, L-tyr was selective only towards Tl(III), while total thallium was determined directly by stabilized temperature platform furnace-electrothermal atomic absorption spectrometry (STPF-ETAAS). The Tl(III) specie, which was retained by L-tyrosine, was quantitatively eluted from the column with 10% of nitric acid. An on-line breakthrough curve was used to determine the column capacity, which resulted to be 9.00 {mu}mol of Tl(III) g{sup -1} of L-tyr-CNTs with a molar ratio of 0.14 (moles of Tl bound to moles of L-tyr at pH 5). Transient peak areas revealed that Tl stripping from the column occurred instantaneously. Effects of sample flow rate, concentration and flow rate of the eluent, and interfering ions on the recovery of the analyte were systematically investigated. The detection limit for the determination of total thallium (3{sigma}) by STPF-ETAAS was 150 ng L{sup -1}. The detection limit (3{sigma}) for Tl(III) employing the separation system was 3 ng L{sup -1}, with an enrichment factor of 40. The precision of the method expressed as the relative standard deviation (RSD) resulted to be 3.4%. The proposed method was applied to the speciation and determination of inorganic thallium in tap water samples. The found concentrations were in the range of 0.88-0.91 {mu}g L{sup -1} of Tl(III), and 3.69-3.91 {mu}g L{sup -1} of total thallium.

  17. Direct determination of bromine in plastic materials by means of solid sampling high-resolution continuum source graphite furnace molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Flórez, M.R.; Resano, M., E-mail: mresano@unizar.es

    2013-10-01

    This work investigates the potential of high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers, which could be interesting in view of the current regulations restricting the use of organobrominated compounds. The method developed is based on the addition of Ca (300 μg) and Pd (30 μg) to favor the formation of CaBr, which is monitored at the main molecular “lines” (rotational spectra) found in the vicinity of 625.315 nm. It was found that accurate results could be obtained for all the samples investigated (polyethylene, polypropylene and acrylonitrile butadiene styrene certified reference materials) using any of the lines studied and constructing the calibration curve with aqueous standards. Furthermore, the combined use of the main four CaBr lines available in the spectral area simultaneously monitored permits to easily expand the linear range up to 2000 ng, provides a limit of detection of 1.8 ng (1.8 μg g{sup −1} for a mass of 1 mg) and further improves precision to values between 3–7% RSD. Overall, the method proposed seems suited for the fast and simple control of these types of samples (approximately 10 min for sample are required), circumventing the traditional problems associated with sample digestion (e.g., losses of volatile compounds), and providing sufficient sensitivity to easily comply with regulations. - Highlights: • Owing to the extended use of BFRs, Br determination in plastics is of great interest. • Solid sampling HR CS GFMAS permits the direct determination of Br, as CaBr, in plastics. • A fast and simple methodology with aqueous standards for calibration is proposed. • A LOD of 1.8 μg g{sup −1} and precision values in the 3–7% RSD range are achieved.

  18. Quality assessment of trace Cd and Pb contaminants in Thai herbal medicines using ultrasound-assisted digestion prior to flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Watsaka Siriangkhawut

    2017-10-01

    Full Text Available A simple, efficient, and reliable ultrasound-assisted digestion (UAD procedure was used for sample preparation prior to quantitative determination of trace Cd and Pb contaminants in herbal medicines using flame atomic absorption spectrometry. The parameters influencing UAD such as the solvent system, sample mass, presonication time, sonication time, and digestion temperature were evaluated. The efficiency of the proposed UAD procedure was evaluated by comparing with conventional acid digestion (CAD procedure. Under the optimum conditions, linear calibration graphs in a range of 2–250 μg/L for Cd, and 50–1000 μg/L for Pb were obtained with detection limits of 0.56 μg/L and 10.7 μg/L for Cd and Pb, respectively. The limit of quantification for Cd and Pb were 1.87 μg/L and 40.3 μg/L, respectively. The repeatability for analysis of 10 μg/L for Cd and 100 μg/L for Pb was 2.3% and 2.6%, respectively. The accuracy of the proposed method was evaluated by rice flour certified reference materials. The proposed method was successfully applied for analysis of trace Cd and Pb in samples of various types of medicinal plant and traditional medicine consumed in Thailand. Most herbal medicine samples were not contaminated with Cd or Pb. The contaminant levels for both metals were still lower than the maximum permissible levels of elements in medicinal plant materials and finished herbal products sets by the Ministry of Public Health of Thailand. The exception was the high level of Cd contamination found in two samples of processed medicinal plants.

  19. On-line determination of antimony(III) and antimony(V) in liver tissue and whole blood by flow injection - hydride generation - atomic absorption spectrometry.

    Science.gov (United States)

    Petit de Peña, Y; Vielma, O; Burguera, J L; Burguera, M; Rondón, C; Carrero, P

    2001-10-31

    A new analytical procedure for the speciation of antimony in liver tissues is presented here. For this purpose, a flow injection system has been developed for the treatment of samples and the determination of antimony by hydride generation - atomic absorption spectrometry. The method involves the sequential and the on-line extraction of antimony(III) and antimony(V) from solid lyophilized blood and hamsters liver tissues, with 1.5 mol l(-1) acetic acid and 0.5 mol l(-1) sulfuric acid for Sb(III) and Sb(V), respectively. Reduction of Sb(V) to Sb(III) for stibine generation is effected by the on-line pre-reduction with l-cysteine. The linear ranges were 2.5-20 and 1.0-25 mug l(-1) of Sb(III) and Sb(V), respectively. The detection limits (3sigma) were 1.0 mug l(-1) for Sb(III) and 0.5 mug l(-1) for Sb(V). The relative standard deviation values for fifteen independent measurements were 2.1 and 1.8% for Sb(III) and Sb(V), respectively. The recovery studies performed with samples of cattle liver provided results from 98 to 100% for Sb(III) and from 100 to 103% for Sb(V) for samples spiked with single species. For samples spiked with both Sb(III) and Sb(V), the recovery varied from 97 to 103% for Sb(III) and from 101 to 103% for Sb(V).

  20. Cloud point extraction-flame atomic absorption spectrometry for pre-concentration and determination of trace amounts of silver ions in water samples

    Directory of Open Access Journals (Sweden)

    Xiupei Yang

    2017-03-01

    Full Text Available A cloud point extraction (CPE method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I/diethyldithiocarbamate (DDTC complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL−1 Ag+ in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL−1 for both Zn2+ and Cu2+, 80 μg·mL−1 for Pb2+, 1000 μg·mL−1 for Mn2+, and 100 μg·mL−1 for both Cd2+ and Ni2+. The calibration curve was linear in the range of 1–500 ng·mL−1 with a limit of detection (LOD at 0.3 ng·mL−1. The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.

  1. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    Energy Technology Data Exchange (ETDEWEB)

    Brum, Daniel M.; Lima, Claudio F. [Departamento de Quimica, Universidade Federal de Vicosa, A. Peter Henry Rolfs s/n, Vicosa/MG, 36570-000 (Brazil); Robaina, Nicolle F. [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil); Fonseca, Teresa Cristina O. [Petrobras, Cenpes/PDEDS/QM, Av. Horacio Macedo 950, Ilha do Fundao, Rio de Janeiro/RJ, 21941-915 (Brazil); Cassella, Ricardo J., E-mail: cassella@vm.uff.br [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil)

    2011-05-15

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO{sub 3}, the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO{sub 3} medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  2. Determination of nickel in blood and serum samples of oropharyngeal cancer patients consumed smokeless tobacco products by cloud point extraction coupled with flame atomic absorption spectrometry.

    Science.gov (United States)

    Arain, Sadaf Sadia; Kazi, Tasneem Gul; Arain, Jamshed Bashir; Afridi, Hassan Imran; Kazi, Atif Gul; Nasreen, Syeda; Brahman, Kapil Dev

    2014-10-01

    Oropharyngeal cancer is a significant public health issue in the world. The incidence of oropharyngeal cancer has been increased among people who have habit of chewing smokeless tobacco (SLT) in Pakistan. The aim of present study was to evaluate the concentration of nickel (Ni) in biological samples (whole blood, serum) of oral (n = 95) and pharyngeal (n = 84) male cancer patients. For comparison purposes, the biological samples of healthy age-matched referents (n = 150), who consumed and did not consumed SLT products, were also analyzed for Ni levels. As the Ni level is very low in biological samples, a preconcentration procedure has been developed, prior to analysis of analyte by flame atomic absorption spectrometry (FAAS). The Ni in acid-digested biological samples was complexed with ammonium pyrrolidinedithio carbamate (APDC), and a resulted complex was extracted in a surfactant Triton X-114. Acidic ethanol was added to the surfactant-rich phase prior to its analysis by FAAS. The chemical variables, such as pH, amounts of reagents (APDC, Triton X-114), temperature, incubation time, and sample volume were optimized. The resulted data indicated that concentration of Ni was higher in blood and serum samples of cancer patients as compared to that of referents who have or have not consumed different SLT products (p = 0.012-0.001). It was also observed that healthy referents who consumed SLT products have two to threefold higher levels of Ni in both biological samples as compared to those who were not chewing SLT products (p < 0.01).

  3. Lead determination at ng/mL level by flame atomic absorption spectrometry using a tantalum coated slotted quartz tube atom trap.

    Science.gov (United States)

    Demirtaş, İlknur; Bakırdere, Sezgin; Ataman, O Yavuz

    2015-06-01

    Flame atomic absorption spectrometry (FAAS) still keeps its importance despite the relatively low sensitivity; because it is a simple and economical technique for determination of metals. In recent years, atom traps have been developed to increase the sensitivity of FAAS. Although the detection limit of FAAS is only at the level of µg/mL, with the use of atom traps it can reach to ng/mL. Slotted quartz tube (SQT) is one of the atom traps used to improve sensitivity. In atom trapping mode of SQT, analyte is trapped on-line in SQT for few minutes using ordinary sample aspiration, followed by the introduction of a small volume of organic solvent to effect the revolatilization and atomization of analyte species resulting in a transient signal. This system is economical, commercially available and easy to use. In this study, a sensitive analytical method was developed for the determination of lead with the help of SQT atom trapping flame atomization (SQT-AT-FAAS). 574 Fold sensitivity enhancement was obtained at a sample suction rate of 3.9 mL/min for 5.0 min trapping period with respect to FAAS. Organic solvent was selected as 40 µL of methyl isobutyl ketone (MIBK). To obtain a further sensitivity enhancement inner surface of SQT was coated with several transition metals. The best sensitivity enhancement, 1650 fold enhancement, was obtained by the Ta-coated SQT-AT-FAAS. In addition, chemical nature of Pb species trapped on quartz and Ta surface, and the chemical nature of Ta on quartz surface were investigated by X-ray photoelectron spectroscopy (XPS) and Raman Spectroscopy. Raman spectrometric results indicate that tantalum is coated on SQT surface in the form of Ta2O5. XPS studies revealed that the oxidation state of Pb in species trapped on both bare and Ta coated SQT surfaces is +2. For the accuracy check, the analyses of standard reference material were performed by use of SCP SCIENCE EnviroMAT Low (EU-L-2) and results for Pb were to be in good agreement with

  4. Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

    Science.gov (United States)

    Orani, Anna Maria; Han, Eunmi; Mandjukov, Petko; Vassileva, Emilia

    2015-01-01

    Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine sediment samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS AAS) and direct solid sample analysis has been developed. The application of fast programs in combination with direct solid sampling allows to eliminate the drying and pretreatment steps, however makes impossible the use of liquid standards for calibration. Iridium treated platforms were applied throughout the present study. Calibration technique based on the use of solid certified reference materials (marine sediments) similar to the nature of the analyzed sample and statistics of regression analysis were applied to the real sediment samples. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signals. The ISO-17025 requirements and Eurachem guidelines were followed in the validation of the proposed analytical procedure. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability reproducibility, limits of detection and quantification and expanded uncertainty (k = 2) for all investigated elements were assessed. Two different approaches for the estimation of measurement uncertainty were applied and obtained results compared. The major contributors to the combined uncertainty of the analyte mass fraction were found to be the homogeneity of the samples and the microbalance precision. The influence of sample particle sizes on the total combined uncertainty was also evaluated. Traceability to SI system of units of the obtained by the proposed analytical procedure results was demonstrated. Additionally, validation of the methodology developed was effectuated by the comparison of the obtained results with independent method e.g. ICP-MS with external calibration. The use of solid sampling HR CS AAS for the determination of trace elements in marine sediment matrix gives significant advantages

  5. Selenium speciation using capillary electrophoresis coupled with modified electrothermal atomic absorption spectrometry after selective extraction with 5-sulfosalicylic acid functionalized magnetic nanoparticles.

    Science.gov (United States)

    Yan, Lizhen; Deng, Biyang; Shen, Caiying; Long, Chanjuan; Deng, Qiufen; Tao, Chunyao

    2015-05-22

    A new method for selenium speciation in fermented bean curd wastewater and juice was described. This method involved sample extraction with 5-sulfosalicylic acid (SSA)-functionalized silica-coated magnetic nanoparticles (SMNPs), capillary electrophoresis (CE) separation, and online detection with a modified electrothermal atomic absorption spectrometry (ETAAS) system. The modified interface for ETAAS allowed for the introduction of CE effluent directly through the end of the graphite tube. Elimination of the upper injection hole of the graphite tube reduced the loss of the anlayte and enhanced the detection sensitivity. The SSA-SMNPs were synthesized and used to extract trace amounts of selenite [Se(IV)], selenite [Se(VI)], selenomethionine (SeMet), and selenocystine (SeCys2) from dilute samples. The concentration enrichment factors for Se(VI), Se(IV), SeMet, and SeCys2 were 21, 29, 18, and 12, respectively, using the SSA-SMNPs extraction. The limits of detection for Se(VI), Se(IV), SeMet, and SeCys2 were 0.18, 0.17, 0.54, 0.49ngmL(-1), respectively. The RSD values (n=6) of method for intraday were observed between 0.7% and 2.9%. The RSD values of method for interday were less than 3.5%. The linear range of Se(VI) and Se(IV) were in the range of 0.5-200ngmL(-1), and the linear ranges of SeMet and SeCys2 were 2-500 and 2-1000ngmL(-1), respectively. The detection limits of this method were improved by 10 times due to the enrichment by the SSA-SMNP extraction. The contents of Se(VI) and Se(IV) in fermented bean curd wastewater were measured as 3.83 and 2.62ngmL(-1), respectively. The contents of Se(VI), Se(IV), SeMet, and SeCys2 in fermented bean curd juice were determined as 6.39, 4.08, 2.77, and 4.00ngmL(-1), respectively. The recoveries were in the range of 99.14-104.5% and the RSDs (n=6) of recoveries between 0.82% and 3.5%. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. A solid phase extraction procedure for the determination of Cd(II) and Pb(II) ions in food and water samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Daşbaşı, Teslima; Saçmacı, Şerife; Ülgen, Ahmet; Kartal, Şenol

    2015-05-01

    A relatively rapid, accurate and precise solid phase extraction method is presented for the determination of cadmium(II) and lead(II) in various food and water samples. Quantitation is carried out by flame atomic absorption spectrometry (FAAS). The method is based on the retention of the trace metal ions on Dowex Marathon C, a strong acid cation exchange resin. Some important parameters affecting the analytical performance of the method such as pH, flow rate and volume of the sample solution; type, concentration, volume, flow rate of the eluent; and matrix effects on the retention of the metal ions were investigated. Common coexisting ions did not interfere on the separation and determination of the analytes. The detection limits (3 σb) for Cd(II) and Pb(II) were found as 0.13 and 0.18 μg L(-1), respectively, while the limit of quantification values (10 σb) were computed as 0.43 and 0.60 μg L(-1) for the same sequence of the analytes. The precision (as relative standard deviation was lower than 4% at 5 μg L(-1) Cd(II) and 10 μg L(-1) Pb(II) levels, and the preconcentration factor was found to be 250. The accuracy of the proposed procedure was verified by analysing the certified reference materials, SPS-WW2 Batch 108 wastewater level 2 and INCT-TL-1 tea leaves, with the satisfactory results. In addition, for the accuracy of the method the recovery studies (⩾ 95%) were carried out. The method was applied to the determination of the analytes in the various natural waters (lake water, tap water, waste water with boric acid, waste water with H2SO4) and food samples (pomegranate flower, organic pear, radish leaf, lamb meat, etc.), and good results were obtained. While the food samples almost do not contain cadmium, they have included lead at low levels of 0.13-1.12 μg g(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

  7. Magnetic solid-phase extraction combined with graphite furnace atomic absorption spectrometry for speciation of Cr(III) and Cr(VI) in environmental waters.

    Science.gov (United States)

    Jiang, Hong-mei; Yang, Ting; Wang, Yan-hong; Lian, Hong-zhen; Hu, Xin

    2013-11-15

    A new approach of magnetic solid phase extraction (MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) has been developed for the speciation of Cr(III) and Cr(VI) using zincon-immobilized silica-coated magnetic Fe3O4 nanoparticles (Zincon-Si-MNPs) as the MSPE absorbent. Cr(III) was quantitatively reserved on the absorbent at pH 9.1 while total Cr was reserved at pH 6.5. The absorbed Cr species were eluted by using 2 mol/L HCl and detected by GFAAS. The concentration of Cr(VI) could be calculated by subtracting Cr(III) from total Cr. All the parameters affecting the separation and extraction efficiency of Cr species such as pH, extraction time, concentration and volume of eluent, sample volume and influence of co-existing ions were systematically examined and the optimized conditions were established accordingly. The detection limit (LOD) of the method was 0.016 and 0.011 ng mL(-1) for Cr(III) and Cr(VI), respectively, with the enrichment factor of 100 and 150. The precisions of this method (Relative standard deviation, RSD, n=7) for Cr(III) and Cr(VI) at 0.1 ng mL(-1) were 6.0% and 6.2%, respectively. In order to validate the proposed method, a certified reference material of environmental water was analyzed, and the result of Cr speciation was in good agreement with the certified value. This MSPE-GFAAS method has been successfully applied for the speciation of Cr(III) and Cr(VI) in lake and tap waters with the recoveries of 88-109% for the spiked samples. Moreover, the MSPE separation mechanism of Cr(III) and Cr(VI) based on their adsorption-desorption on Zincon-Si-MNPs has been explained through various spectroscopic characterization. © 2013 Elsevier B.V. All rights reserved.

  8. Graphene oxide-TiO2 composite solid phase extraction combined with graphite furnace atomic absorption spectrometry for the speciation of inorganic selenium in water samples.

    Science.gov (United States)

    Zhang, Yanan; Chen, Beibei; Wu, Shaowei; He, Man; Hu, Bin

    2016-07-01

    In this paper, a method of graphene oxide (GO)-TiO2 composite solid phase extraction followed by graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the speciation of inorganic selenium in environmental waters. The adsorption behavior of inorganic Se(IV) and Se(VI) on the GO-TiO2(1:1) composite was investigated. It was found that Se(IV) was quantitatively retained on the GO-TiO2 composites within a wide pH range of 0.5-10, while Se(VI) was quantitatively adsorbed on GO-TiO2(1:1) composite at pH 0.5-2, and no obvious adsorption of Se(VI) within the pH range of 4-10 was found. By selecting pH 6.0, Se(IV) could be easily determined. After reduction of Se(VI), total Se was determined by the proposed method, and Se(VI) was calculated as the difference between the total Se and Se(IV). The factors affecting the separation/preconcentration of Se(IV) and Se(VI) were studied. Under the optimum conditions, the isothermal adsorption of Se(IV) on the GO-TiO2(1:1) composite fitted Langmuir model; a linear range over 0.1-12ngmL(-1) was obtained. The limit of detection (LOD) and precision of the method for Se(IV) was 0.04ngmL(-1) and 9.4% (cSe(IV)=0.5ngmL(-1), n=7), respectively. In order to verify the accuracy of the method, a standard water sample (GSBZ50031-94) was analyzed, and the determined value was in a good agreement to the certified value. The established method was applied to inorganic Se speciation in environmental water samples and the recovery of 87.4-102% was obtained for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Metal interferences and their removal prior to the determination of As(T) and As(III) in acid mine waters by hydride generation atomic absorption spectrometry

    Science.gov (United States)

    McCleskey, R. Blaine; Nordstrom, D. Kirk; Ball, James W.

    2003-01-01

    Hydride generation atomic absorption spectrometry (HGAAS) is a sensitive and selective method for the determination of total arsenic (arsenic(III) plus arsenic(V)) and arsenic(III); however, it is subject to metal interferences for acid mine waters. Sodium borohydride is used to produce arsine gas, but high metal concentrations can suppress arsine production. This report investigates interferences of sixteen metal species including aluminum, antimony(III), antimony(V), cadmium, chromium(III), chromium(IV), cobalt, copper(II), iron(III), iron(II), lead, manganese, nickel, selenium(IV), selenium(VI), and zinc ranging in concentration from 0 to 1,000 milligrams per liter and offers a method for removing interfering metal cations with cation exchange resin. The degree of interference for each metal without cation-exchange on the determination of total arsenic and arsenic(III) was evaluated by spiking synthetic samples containing arsenic(III) and arsenic(V) with the potential interfering metal. Total arsenic recoveries ranged from 92 to 102 percent for all metals tested except antimony(III) and antimony(V) which suppressed arsine formation when the antimony(III)/total arsenic molar ratio exceeded 4 or the antimony(V)/total arsenic molar ratio exceeded 2. Arsenic(III) recoveries for samples spiked with aluminum, chromium(III), cobalt, iron(II), lead, manganese, nickel, selenium(VI), and zinc ranged from 84 to 107 percent over the entire concentration range tested. Low arsenic(III) recoveries occurred when the molar ratios of metals to arsenic(III) were copper greater than 120, iron(III) greater than 70, chromium(VI) greater than 2, cadmium greater than 800, antimony(III) greater than 3, antimony(V) greater than 12, or selenium(IV) greater than 1. Low recoveries result when interfering metals compete for available sodium borohydride, causing incomplete arsine production, or when the interfering metal oxidizes arsenic(III). Separation of interfering metal cations using

  10. Determination of sub-ng g-1levels of total inorganic arsenic and selenium in foods by hydride-generation atomic absorption spectrometry after pre-concentration.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan

    2017-03-01

    A new and simple ultrasonic-assisted extraction (UAE) procedure was developed for the determination of inorganic arsenic and selenium in foods by hydride-generation atomic absorption spectrometry (HG-AAS). The various analytical variables affecting complex formation and extraction efficiency were investigated and optimised. The method is based on selective complex formation of As(III) and Se(IV) in the presence of excess As(V) and Se(VI) with toluidine red in the presence of tartaric acid at pH 4.5, and then extraction of the resulting condensation products into the micellar phase of non-ionic surfactant, polyethylene glycol dodecyl ether, Brij 35. Under optimised conditions, good linear relationships were obtained in the ranges of 4-225 and 12-400 ng l - 1 with limits of detection of 1.1 and 3.5 ng l - 1 for As(III) and Se(IV), respectively. The repeatability was better than 3.9% for both analytes (n = 10, 25 ng l - 1 ) while reproducibility ranged from 4.2% to 4.8%. The recoveries of As(III) and Se(IV) spiked at 25-100 ng l - 1 were in the range of 94.2-104.8%. After pre-concentration of a 5.0 ml sample, the sensitivity enhancement factors for As(III) and Se(IV) were 185 and 140, respectively. Accuracy was assessed by analysis of two standard reference materials (SRMs) and spiked recovery experiments. The method was successfully applied to the accurate and reliable determination of total As and total Se by HG-AAS after pre-reduction with a mixture of L-cysteine and tartaric acid. Finally, the method was shown to be rapid and sensitive, with good results for extraction, pre-concentration and determination of total As and Se contents (as As(III) and Se(IV)) from food samples.

  11. Investigation of chemical modifiers for the determination of lead in fertilizers and limestone using graphite furnace atomic absorption spectrometry with Zeeman-effect background correction and slurry sampling

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; Dessuy, Morgana B. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil)

    2014-02-01

    In this work, chemical modifiers in solution (Pd/Mg, NH{sub 4}H{sub 2}PO{sub 4} and NH{sub 4}NO{sub 3}/Pd) were compared with permanent modifiers (Ir and Ru) for the determination of lead in fertilizer and limestone samples using slurry sampling and graphite furnace atomic absorption spectrometry with Zeeman-effect background correction. The analytical line at 283.3 nm was used due to some spectral interference observed at 217.0 nm. The NH{sub 4}H{sub 2}PO{sub 4} was abandoned due to severe spectral interference even at the 283.3-nm line. For Pd/Mg and NH{sub 4}NO{sub 3}/Pd the optimum pyrolysis and atomization temperatures were 900 °C and 1900 °C, respectively. For Ru and Ir, the integrated absorbance signal was stable up to pyrolysis temperatures of 700 °C and 900 °C, respectively, and up to atomization temperature of 1700 °C. The limit of detection (LOD) was 17 ng g{sup −1} using Pd/Mg and 29 ng g{sup −1} using NH{sub 4}NO{sub 3}/Pd. Among the permanent modifiers investigated, the LOD was 22 ng g{sup −1} Pb for Ir and 10 ng g{sup −1} Pb for Ru. The accuracy of the method was evaluated using the certified reference material NIST SRM 695. Although Ru provided lower LOD, which can be attributed to a lower blank signal, only the modifiers in solution showed concordant values of Pb concentration for the NIST SRM 695 and the most of analyzed samples. Moreover, the Pd/Mg modifier provided the highest sensitivity and for this reason it is more suitable for the determination of Pb in fertilizers samples in slurry; besides this it presented a better signal-to-noise ratio than NH{sub 4}NO{sub 3}/Pd. - Highlights: • Lead has been determined in fertilizers using slurry sampling GF AAS. • The mixture of palladium and magnesium nitrates was found to be the ideal chemical modifier. • Calibration could be carried out against aqueous standard solutions. • The proposed method is much faster than the EPA method, which includes sample digestion.

  12. Optimized procedure for the determination of antimony in lipid-rich environmental matrices by flow injection hydride generation atomic absorption spectrometry.

    Science.gov (United States)

    Krachler, M; Burow, M; Emons, H

    1999-06-01

    An analytical procedure for the reliable determination of Sb in digests of lipid-rich environmental matrices in the low ng l-1-range based on flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) has been developed. Prior to HG-AAS, aliquots (250 to 320 mg) of dry samples were mineralized with 3 ml nitric acid and 0.5 ml of each sulfuric and perchloric acids in open digestion vessels made of glassy carbon in a heating block. Procedure detection and quantification limits of a previously developed procedure for the determination of Sb in plant materials by FI-HG-AAS were decreased with respect to the lower Sb concentrations in animal tissues, the sensitivity of the instrumental response was increased, and the composition of the acid digestion mixture was re-optimized for lipid-rich samples. The accuracy and precision of the developed procedure was evaluated by the analysis of the two reference materials Bovine Liver 1577a and Pig Kidney CRM 186. These reference materials have been additionally spiked with appropriate amounts of Sb to obtain recovery data. The solution detection limit (3 sigma) in digested samples was 0.021 microgram l-1, the detection limit for the whole procedure based on the dry powders was 7 pg g-1, the method quantification limit for a reliable determination of Sb was 23 pg g-1. The reproducibility of repetitive measurements was 6.0% at 0.1 microgram Sb l-1 and 2.2% at 0.5 microgram Sb l-1. Calibration curves were linear from 0.05 to 3 micrograms Sb l-1. To demonstrate the suitability of the developed method, concentrations of Sb have been determined in pigeon eggs (approximately 2 ng Sb g-1), as well as in bream livers (approximately 4 ng g-1) and in deer livers (approximately 5 to 8 ng g-1) from animals living in remote and urban-industrialized areas of Germany, respectively.

  13. Ion Imprinted Polymer for Preconcentration and Determination of Ultra-Trace Cadmium, Employing Flow Injection Analysis with Thermo Spray Flame Furnace Atomic Absorption Spectrometry.

    Science.gov (United States)

    do Lago, Ayla Campos; Marchioni, Camila; Mendes, Tássia Venga; Wisniewski, Célio; Fadini, Pedro Sergio; Luccas, Pedro Orival

    2016-11-01

    This work proposes a preconcentration method using an ion imprinted polymer (IIP) for determination of cadmium, in several samples, employing a mini-column filled with the polymer coupled into a flow injection analysis system with detection by thermospray flame furnace atomic absorption spectrometry (FIA-TS-FF-AAS). The polymer was synthesized via bulk using methacrylic acid and vinylimidazole as a functional monomer. For the FIA system initial assessment, the variables: pH, eluent concentration and buffer concentration were studied, employing a 23 full factorial design. To obtain the optimum values for each significant variable, a Doehlert matrix was employed. After the optimization conditions as: pH 5.8, eluent (HNO3) concentration of 0.48 mol L-1 and buffer concentration of 0.01 mol L-1, were adopted. The proposed method showed a linear response in the range of 0.081-10.0 μg L-1, limits detection and quantification of 0.024 and 0.081 μg L-1, respectively; preconcentration factor of 165, consumptive index of 0.06 mL, concentration efficiency 132 min-1, and frequency of readings equal to 26 readings h-1 The accuracy was checked by analysis of certified reference materials for trace metals and recovery tests. The obtained results were in agreement with 95% confidence level (t-test). The method was adequate to apply in samples of: jewelry (earrings) (2.38 ± 0.28 μg kg-1), black tea (1.09 ± 0.15 μg kg-1), green tea (3.85 ± 0.13 μg kg-1), cigarette tobacco (38.27 ± 0.22 μg kg-1), and hair (0.35 ± 0.02 μg kg-1). © The Author(s) 2016.

  14. Application of three-variables Doehlert matrix for optimisation of an on-line pre-concentration system for zinc determination in natural water samples by flame atomic absorption spectrometry

    OpenAIRE

    Santos, Walter N. L. dos; Santos, Carla M. C.; Ferreira, Sergio Luis Costa

    2003-01-01

    Texto completo: acesso restrito. p. 211-221 This article describes an on-line pre-concentration system for zinc determination in environmental samples by flame atomic absorption spectrometry (FAAS).It was based on the sorption of zinc(II) ions in a minicolumn of polyurethane foam loaded with 4-(2-pyridylazo)-resorcinol (PAR).The optimisation step was carried out using twolevel full factorial and a Doehlert design.Thr ee variables (sampling flow rate, buffer concentration and pH) were...

  15. Selective Flow-Injection Quantification of Ultra-trace Amounts of Cr(VI) via On-line Complexation and Preconcentration with APDC Followed by Determination by Electrothermal Atomic Absorption Spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Hansen, Elo Harald

    1998-01-01

    is effected by adsorption on the inner wall of a knotted reactor made from PTFE tubing. The complex is subsequently eluted with a monosegmented discrete zone of ethanol (55 mu l), and the analyte is quantified by electrothermal atomic absorption spectrometry (ETAAS). The operations of the FI...... of the retained analyte in order to remove possibly interfering matrix components; quantitative dissolution of the retained analyte in the smallest possible volume of eluent to satisfy the volumetric requirements of the graphite tube (platform); reproducible transport of the concentrate to the ETAAS instrument...

  16. Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

    Science.gov (United States)

    dos Santos, Lisia M G; Welz, Bernhard; Araujo, Rennan G O; Jacob, Silvana do C; Vale, Maria Goreti R; Martens, Andreas; Gonzaga Martens, Irland B; Becker-Ross, Helmut

    2009-11-11

    A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

  17. Direct sample introduction of wines in graphite furnace atomic absorption spectrometry for the simultaneous determination of arsenic, cadmium, copper and lead content.

    Science.gov (United States)

    Ajtony, Zsolt; Szoboszlai, Norbert; Suskó, Emoke Klaudia; Mezei, Pál; György, Krisztina; Bencs, László

    2008-07-30

    A multi-element graphite furnace atomic absorption spectrometry (GFAAS) method was elaborated for the simultaneous determination of As, Cd, Cu, and Pb in wine samples of various sugar contents using the transversally heated graphite atomizer (THGA) with end-capped tubes and integrated graphite platforms (IGPs). For comparative GFAAS analyses, direct injection (i.e., dispensing the sample onto the IGP) and digestion-based (i.e., adding oxidizing agents, such as HNO(3) and/or H(2)O(2) to the sample solutions) methods were optimized with the application of chemical modifiers. The mixture of 5 microg Pd (applied as nitrate) plus 3 microg Mg(NO(3))(2) chemical modifier was proven to be optimal for the present set of analytes and matrix, it allowing the optimal 600 degrees C pyrolysis and 2200 degrees C atomization temperatures, respectively. The IGP of the THGA was pre-heated at 70 degrees C to prevent the sputtering and/or foaming of sample solutions with a high organic content, dispensed together with the modifier solution, which method also improved the reproducibility of the determinations. With the digestion-based method, the recovery ranged between 87 and 122%, while with the direct injection method it was between 96 and 102% for Cd, Cu, and Pb, whereas a lower, compromise recovery of 45-85% was realized for As. The detection limits (LODs) were found to be 5.0, 0.03, 1.2, and 0.8 microg l(-1) for As, Cd, Cu, and Pb, respectively. The characteristic mass (m(0)) data were 24 pg As, 1.3 pg Cd, 13 pg Cu, and 35 pg Pb. The upper limits of the linear calibration range were 100, 2, 100, and 200 microg l(-1) for As, Cd, Cu, and Pb, respectively. The precisions were not worse than 4.8, 3.1, 3.7, and 2.3% for As, Cd, Cu, and Pb, respectively. For arsenic, a higher amount of the modifier (e.g., 20 microg Pd plus 12 microg Mg(NO(3))(2)) could be recommended to overcome the interference from the presence of sulphate and phosphate in wines. Although this method increased the

  18. Working towards accreditation by the International Standards Organization 15189 Standard: how to validate an in-house developed method an example of lead determination in whole blood by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Garcia Hejl, Carine; Ramirez, Jose Manuel; Vest, Philippe; Chianea, Denis; Renard, Christophe

    2014-09-01

    Laboratories working towards accreditation by the International Standards Organization (ISO) 15189 standard are required to demonstrate the validity of their analytical methods. The different guidelines set by various accreditation organizations make it difficult to provide objective evidence that an in-house method is fit for the intended purpose. Besides, the required performance characteristics tests and acceptance criteria are not always detailed. The laboratory must choose the most suitable validation protocol and set the acceptance criteria. Therefore, we propose a validation protocol to evaluate the performance of an in-house method. As an example, we validated the process for the detection and quantification of lead in whole blood by electrothermal absorption spectrometry. The fundamental parameters tested were, selectivity, calibration model, precision, accuracy (and uncertainty of measurement), contamination, stability of the sample, reference interval, and analytical interference. We have developed a protocol that has been applied successfully to quantify lead in whole blood by electrothermal atomic absorption spectrometry (ETAAS). In particular, our method is selective, linear, accurate, and precise, making it suitable for use in routine diagnostics.

  19. Combined discrete nebulization and microextraction process for molybdenum determination by flame atomic absorption spectrometry (FAAS); Avaliacao da combinacao da nebulizacao discreta e processos de microextracao aplicados a determinacao de molibdenio por espectrometria de absorcao atomica com chama (FAAS)

    Energy Technology Data Exchange (ETDEWEB)

    Oviedo, Jenny A.; Jesus, Amanda M.D. de; Fialho, Lucimar L.; Pereira-Filho, Edenir R., E-mail: erpf@ufscar.br [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Departamento de Quimica

    2014-04-15

    Simple and sensitive procedures for the extraction/preconcentration of molybdenum based on vortex-assisted solidified floating organic drop microextraction (VA-SFODME) and cloud point combined with flame absorption atomic spectrometry (FAAS) and discrete nebulization were developed. The influence of the discrete nebulization on the sensitivity of the molybdenum preconcentration processes was studied. An injection volume of 200 μ resulted in a lower relative standard deviation with both preconcentration procedures. Enrichment factors of 31 and 67 and limits of detection of 25 and 5 μ L{sup -1} were obtained for cloud point and VA-SFODME, respectively. The developed procedures were applied to the determination of Mo in mineral water and multivitamin samples. (author)

  20. Dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous separation/preconcentration of nickel, cobalt and copper prior to determination by electrothermal atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mooud Amirkavei

    2013-01-01

    Full Text Available A dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous extraction of trace amounts of nickel, cobalt and copper followed by their determination with electrothermal atomic absorption spectrometry was developed. 300 µL of acetone and 1-undecanol was injected into an aqueous sample containing diethyldithiocarbamate complexes of metal ions. For a sample volume of 10 mL, enrichment factors of 277, 270 and 300 and detection limits of 1.2, 1.1 and 1 ng L-1 for nickel, cobalt and copper were obtained, respectively. The method was applied to the extraction and determination of these metals in different water samples.

  1. Development of an in situ solvent formation microextraction and preconcentration method based on ionic liquids for the determination of trace cobalt (II in water samples by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Jamali

    2017-02-01

    Full Text Available A simple in situ solvent formation microextraction (ISFME methodology based on the application of ionic liquid (IL as an extractant solvent and sodium hexafluorophosphate (NaPF6 as an ion-pairing agent was proposed for the preconcentration of the trace levels of cobalt ions. In this method cobalt was complexed with 2-(5-bromo-2-pyridylazo-5-diethylaminophenol (5-Br-PADAP and extracted into an ionic liquid phase. After phase separation, the enriched analyte in the final solution is determined by flame atomic absorption spectrometry (FAAS. Some effective factors that influence the microextraction efficiency were investigated and optimized. Under the optimum experimental conditions, the limit of detection and the enrichment factor were 0.97 μg L−1 and 50, respectively. The relative standard deviation (R.S.D. was obtained as 2.4%. The proposed method was assessed through the analysis of certified reference water and recovery experiments.

  2. Analytical strategy for rapid identification and quantification of lubricant additives in mineral oil by high-performance thin-layer chromatography with UV absorption and fluorescence detection combined with mass spectrometry and infrared spectroscopy.

    Science.gov (United States)

    Dytkiewitz, Elisabeth; Morlock, Gertrud E

    2008-01-01

    A simple strategy for identification and quantification of lubricant additives in mineral oil was demonstrated by high-performance thin-layer chromatography with UV absorption and fluorescence detection using various coupling options, e.g., with attenuated total reflectance infrared (ATR-IR) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, electrospray ionization mass spectrometry (ESI-MS), and direct analysis in real-time mass spectrometry (DART-MS). For the additives zinc bis(O,O'-diisobutyl dithiophosphate), zinc bis(O,O'-didodecyl dithiophosphate), and Anglamol 99, 2 chromatographic systems were developed, i.e., a reversed-phase (RP) system on RP2 plates using an acetonitrile-based mobile phase and a normal-phase system on silica gel 60 plates using a toluene-based gradient. Densitometry was performed by absorption measurement at 220 nm. Repeatabilities (relative standard deviation, n = 6) between 2.2 and 5.5% and correlation coefficients >0.9973 were highly satisfactory for the analysis of these additives in the mineral oil. Primuline reagent was used to improve the detection limit of the lipophilic additives by a factor of 2, followed by fluorescence measurement at UV 366/>400 nm. For rapid identification by ATR-IR and FTIR, the respective additive zones on the plate were online extracted by an interface called ChromeXtract, concentrated, and directly applied for measurements in the wave number range of 4000-400 cm(-1). Identification was confirmed by online ESI-MS within a minute using ChromeXtract and by DART-MS within seconds.

  3. Slurry sampling high-resolution continuum source electrothermal atomic absorption spectrometry for direct beryllium determination in soil and sediment samples after elimination of SiO interference by least-squares background correction.

    Science.gov (United States)

    Husáková, Lenka; Urbanová, Iva; Šafránková, Michaela; Šídová, Tereza

    2017-12-01

    In this work a simple, efficient, and environmentally-friendly method is proposed for determination of Be in soil and sediment samples employing slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral effects originating from SiO species were identified and successfully corrected by means of a mathematical correction algorithm. Fractional factorial design has been employed to assess the parameters affecting the analytical results and especially to help in the development of the slurry preparation and optimization of measuring conditions. The effects of seven analytical variables including particle size, concentration of glycerol and HNO3 for stabilization and analyte extraction, respectively, the effect of ultrasonic agitation for slurry homogenization, concentration of chemical modifier, pyrolysis and atomization temperature were investigated by a 27-3 replicate (n = 3) design. Using the optimized experimental conditions, the proposed method allowed the determination of Be with a detection limit being 0.016mgkg-1 and characteristic mass 1.3pg. Optimum results were obtained after preparing the slurries by weighing 100mg of a sample with particle size samples by slurry sampling with those determined after microwave-assisted extraction by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS). The reported method has a precision better than 7%. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS).

    Science.gov (United States)

    Ciftci, Harun; Er, Cigdem

    2013-03-01

    In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L(-1) HNO(3) and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L(-1) and 3.91 μg L(-1), respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.

  5. Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Acar, O.

    2012-07-01

    The Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive) and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds) were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS) using an Sc + Ir + NH{sub 4}H{sub 2}PO{sub 4} chemical modifier mixture and flame atomic absorption spectrometer (FAAS) after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD) for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 {mu}g L{sup -}1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM) and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH{sub 4}H{sub 2}PO{sub 4} mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compared with international and national food quality guidelines as well as with literature values. (Author) 48 refs.

  6. Absolute number densities of helium metastable atoms determined by atomic absorption spectroscopy in helium plasma-based discharges used as ambient desorption/ionization sources for mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reininger, Charlotte; Woodfield, Kellie [Brigham Young University, Department of Chemistry and Biochemistry, Provo, UT 84602 (United States); Keelor, Joel D.; Kaylor, Adam; Fernández, Facundo M. [Georgia Institute of Technology, School of Chemistry and Biochemistry, Atlanta, GA 30332 (United States); Farnsworth, Paul B., E-mail: paul_farnsworth@byu.edu [Brigham Young University, Department of Chemistry and Biochemistry, Provo, UT 84602 (United States)

    2014-10-01

    The absolute number densities of helium atoms in the 2s {sup 3}S{sub 1} metastable state were determined in four plasma-based ambient desorption/ionization sources by atomic absorption spectroscopy. The plasmas included a high-frequency dielectric barrier discharge (HF-DBD), a low temperature plasma (LTP), and two atmospheric-pressure glow discharges, one with AC excitation and the other with DC excitation. Peak densities in the luminous plumes downstream from the discharge capillaries of the HF-DBD and the LTP were 1.39 × 10{sup 12} cm{sup −3} and 0.011 × 10{sup 12} cm{sup −3}, respectively. Neither glow discharge produced a visible afterglow, and no metastable atoms were detected downstream from the capillary exits. However, densities of 0.58 × 10{sup 12} cm{sup −3} and 0.97 × 10{sup 12} cm{sup −3} were measured in the interelectrode regions of the AC and DC glow discharges, respectively. Time-resolved measurements of metastable atom densities revealed significant random variations in the timing of pulsed absorption signals with respect to the voltage waveforms applied to the discharges. - Highlights: • We determine He metastable number densities for four plasma types • The highest number densities were observed in a dielectric barrier discharge • No helium metastable atoms were observed downstream from the exits of glow discharges.

  7. Determination of sulfur in human hair using high resolution continuum source graphite furnace molecular absorption spectrometry and its correlation with total protein and albumin

    Science.gov (United States)

    Ozbek, Nil; Baysal, Asli

    2017-04-01

    Human hair is a valuable contributor for biological monitoring. It is an information storage point to assess the effects of environmental, nutritional or occupational sources on the body. Human proteins, amino acids or other compounds are among the key components to find the sources of different effects or disorders in the human body. Sulfur is a significant one of these compounds, and it has great affinity to some metals and compounds. This property of the sulfur affects the human health positively or negatively. In this manuscript, sulfur was determined in hair samples of autistic and age-match control group children via molecular absorption of CS using a high-resolution continuum source graphite furnace atomic absorption spectrometer. For this purpose, hair samples were appropriately washed and dried at 75 °C. Then samples were dissolved in microwave digestion using HNO3 for sulfur determination. Extraction was performed with HCl hydrolysation by incubation for 24 h at 110 °C for total protein and albumin determination. The validity of the method for the sulfur determination was tested using hair standard reference materials. The results were in the uncertainty limits of the certified values at 95% confidence level. Finally correlation of sulfur levels of autistic children's hair with their total protein and albumin levels were done.

  8. Determination of essential elements in beverages, herbal infusions and dietary supplements using a new straightforward sequential approach based on flame atomic absorption spectrometry.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Procopio, Jesús R

    2017-03-15

    A simple method based on FAAS was developed for the sequential multi-element determination of Cu, Zn, Mn, Mg and Si in beverages and food supplements with successful results. The main absorption lines for Cu, Zn and Si and secondary lines for Mn and Mg were selected to carry out the measurements. The sample introduction was performed using a flow injection system. Using the choice of the absorption line wings, the upper limit of the linear range increased up to 110mgL-1 for Mg, 200mgL-1 for Si and 13mgL-1 for Zn. The determination of the five elements was carried out, in triplicate, without the need of additional sample dilutions and/or re-measurements, using less than 3.5mL of sample to perform the complete analysis. The LODs were 0.008mgL-1 for Cu, 0.017mgL-1 for Zn, 0.011mgL-1 for Mn, 0.16mgL-1 for Si and 0.11mgL-1 for Mg. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Evaluation of a novel PTFE material for use as a means for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems. Determination of cadmium (II) with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Hansen, Elo Harald

    2004-01-01

    with an external packed column and in a sequential injection lab-on-valve (SI-LOV) system. Employed for the determination of cadmium(II), complexed with diethyldithiophosphate (DDPA), and detection by electrothermal atomic absorption spectrometry (ETAAS), its performance was compared to that of a previously used...

  10. Separation of seven arsenic compounds by high performance liquid chromatography with on-line detection by hydrogen-argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, Erik Huusfeldt; Pritzl, G.

    1992-01-01

    the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs...... of mixtures of arsenic standards into the HPLC system were: arsenite, As(III) 1.1; arsenate, As(V) 1.4; MMA 1.4; DMA 0.7; AsB 0.3; AsC 0.5; and the TMAs 0.4. The HPLC-AAS system was used for the analysis of arsenic species in aqueous extracts of soil samples from a polluted land site. Only arsenate was found...

  11. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen–argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, E. H.; Pritzl, G.

    1992-01-01

    the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs...... of mixtures of arsenic standards into the HPLC system were: arsenite, As(III) 1.1; arsenate, As(V) 1.4; MMA 1.4; DMA 0.7; AsB 0.3; AsC 0.5; and the TMAs 0.4. The HPLC-AAS system was used for the analysis of arsenic species in aqueous extracts of soil samples from a polluted land site. Only arsenate was found...

  12. Determination of tin, vanadium, iron, and molybdenum in various matrices by atomic absorption spectrometry using a simultaneous liquid-liquid extraction procedure.

    Science.gov (United States)

    Sánchez-Viñas, M; Bagur, G M; Gázquez, D; Camino, M; Romero, R

    1999-01-01

    An atomic-absorption spectrometric method is described for the determination of tin, vanadium, iron, and molybdenum in two certified reference materials, food samples, and petroleum crude. After treatment with acids, these elements are separated from matrix elements by simultaneous solvent extraction of 5,5'-methylenedisalicylohydroxamic acid complexes from HCl/NaClO4 solution into an isobutyl methyl ketone/tributyl phosphate solution. The detection limits range from 0.018 to 0.19 microg/mL (n = 3), and the relative standard deviations do not exceed 2.0% at levels of 0.5, 0.6, 2.0, and 7.0 microg/mL of Fe, Mo, V, and Sn, respectively. The method is selective and suffers only from interference by Zr(IV), Ti(IV), Th(IV), W(VI), PO4(3-), and F-.

  13. Coprecipitation of trace elements with Ni2+/2-Nitroso-1-naphthol-4-sulfonic acid and their determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Uluozlu, Ozgür Dogan; Tuzen, Mustafa; Mendil, Durali; Soylak, Mustafa

    2010-04-15

    Ni(2+)/2-Nitroso-1-naphthol-4-sulfonic acid precipitate was used for the coprecipitation of Co, Pb, Cu, Fe and Zn prior to their flame atomic absorption spectrometric (FAAS) determinations in environmental samples. The precipitate could be easily dissolved with concentrated nitric acid. The recovery values for analyte ions were higher than 95%. The parameters including pH, sample volume, centrifuge time, amounts of nickel and matrix effects were optimized for the quantitative recoveries of the analytes. The relative standard deviations of cobalt, lead, copper, iron and zinc were found 4.5, 5.7, 3.8, 6.1 and 7.5%, respectively. The limit of detection was calculated as 1.05, 2.67, 1.30, 1.38, and 0.50 microg L(-1) for cobalt, lead, copper, iron and zinc. The validation of the procedure was checked by the analysis of IAEA 336 lichen and SLRS 4 Riverine water standard reference materials were analyzed with satisfactory results. The presented coprecipitation procedure was successfully applied to some environmental samples for determination of analyte ions. 2009 Elsevier B.V. All rights reserved.

  14. Flame atomic absorption spectrometry determination of trace amount of gold after separation and preconcentration onto ion-exchange polyethylenimine coated on Al2O3

    Directory of Open Access Journals (Sweden)

    Daryoush Afzali

    2014-11-01

    Full Text Available The object of this work is to develop a simple and selective method for efficient extraction of Au(III ions in aqueous solution using a new solid-phase extraction sorbent. Polyethylenimine (PEI ion-exchange polymer was coated on alumina in the presence of NaNO3. The method is based on sorption of Au3+ ions on 50 mg PEI/Al2O3. A solution of 0.5 M thiourea, then 1.0 M HCl effectively eluted the gold ion and then aspirated into flame atomic absorption spectroscopy (FAAS. The influence of flow rate of sample solution and eluent, the pH effect, eluent type and sorption capacity was investigated. The effects of various diverse ions for preconcentration and separation of the gold ion were investigated. Relative standard deviation of 4.0 μg mL−1 of gold was 1.46% (n = 10. The detection limit was 26.2 ng L−1 in original solution. The method has been applied successfully for the recovery of trace amount of Au(III ions from water samples.

  15. Application of chitosan and its N-heterocyclic derivatives for preconcentration of noble metal ions and their determination using atomic absorption spectrometry.

    Science.gov (United States)

    Azarova, Yu A; Pestov, A V; Ustinov, A Yu; Bratskaya, S Yu

    2015-12-10

    Chitosan and its N-heterocyclic derivatives N-2-(2-pyridyl)ethylchitosan (2-PEC), N-2-(4-pyridyl) ethylchitosan (4-PEC), and N-(5-methyl-4-imidazolyl) methylchitosan (IMC) have been applied in group preconcentration of gold, platinum, and palladium for subsequent determination by atomic absorption spectroscopy (AAS) in solutions with high background concentrations of iron and sodium ions. It has been shown that the sorption mechanism, which was elucidated by XPS, significantly influences the sorption capacity of materials, the efficiency of metal ions elution after preconcentration, and, as a result, the accuracy of metal determination by AAS. We have shown that native chitosan was not suitable for preconcentration of Au(III), if the elution step was used as a part of the analysis scheme. The group preconcentration of Au(III), Pd(II), and Pt(IV) with subsequent quantitative elution using 0.1M HCl/1M thiourea solution was possible only on IMC and 4-PEC. Application of IMC for analysis of the national standard quartz ore sample proved that gold could be accurately determined after preconcentration/elution with the recovery above 80%. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Solid sampling graphite furnace atomic absorption spectrometry for the direct analysis of microextraction solvent bars used for metal ultra-trace pre-concentration

    Science.gov (United States)

    González-Álvarez, Rafael Jesús; Pinto, Juan J.; Bellido-Milla, Dolores; Moreno, Carlos

    2017-09-01

    The potential applicability of the continuum source solid sampling graphite furnace atomic absorption spectroscopy (CS SS-GF AAS) technique has been studied to carry out the direct analysis of microextraction solvent bars used for metal ultra-trace pre-concentration in natural waters. An optimisation of the temperature program was developed for this purpose. Preliminary chamber furnace studies were performed in order to understand the behaviour of the bars with the increasing temperature. Solvent bars were filled with an acceptor solution, impregnated with an organic extractant and placed into the chamber furnace to carry out several temperature programs. Results led to perform a correct optimisation of the drying and pyrolysis steps of the furnace temperature program, which was tested with silver once completed. Blank solvent bars as well as standards containing silver were measured, obtaining a calibration curve with a correlation coefficient of 0.991. The results exhibited good repeatability and reproducibility, with relative standard deviations below 10% in both cases, indicating a promising applicability of the CS SS-GF AAS technique to directly determine metallic species in microextraction solvent bars.

  17. On-line preconcentration system using a microcolumn packed with Alizarin Red S-modified alumina for zinc determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    A.M. Haji Shabani

    2009-01-01

    Full Text Available A simple and sensitive on-line flow injection system for determination of zinc with FAAS has been described. The method is based on the separation and preconcentration of zinc on a microcolumn of immobilized Alizarin Red S on alumina. The adsorbed analyte is then eluted with 250 µL of nitric acid (1 mol L-1 and is transported to flame atomic absorption spectrometer for quantification. The effect of pH, sample and eluent flow rates and presence of various cations and anions on the retention of zinc was investigated. The sorption of zinc was quantitative in the pH range of 5.5-8.5. For a sample volume of 25 mL an enrichment factor of 144 and a detection limit (3S of 0.2 µg L-1 was obtained. The precision (RSD, n=7 was 3.0% at the 20 µg L-1 level. The developed system was successfully applied to the determination of zinc in water samples, hair, urine and saliva.

  18. A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    M. Carmen Yebra

    2012-01-01

    Full Text Available A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6% and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee and pharmaceutical preparations (multivitamin tablets. The ranges of concentrations found were 21.4–25.61 μg g-1 for iron, 5.74–18.30 μg g-1 for manganese, and 33.27–57.90 μg g-1 for zinc in soluble solid food samples and 3.75–9.90 μg g-1 for iron, 0.47–5.05 μg g-1 for manganese, and 1.55–15.12 μg g-1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors.

  19. Field sample preconcentration of copper in sea water using chelating minicolumns subsequently incorporated on a flow-injection-flame atomic absorption spectrometry system.

    Science.gov (United States)

    Yebra, M C; Carro, N; Enríquez, M F; Moreno-Cid, A; García, A

    2001-06-01

    A field flow preconcentration system for copper determination in seawater is described. Seawater samples are collected and preconcentrated in situ by passing them using a peristaltic pump through a minicolumn packed with Amberlite XAD-4 impregnated with the complexing agent 1-(2-pyridylazo)-2-naphthol. Thus, copper is preconcentrated without the interference of the saline matrix. Once in the laboratory, the minicolumns loaded with copper are incorporated on a flow injection system and eluted with a small volume of a 20% (v/v) ethanolic solution of 0.5 mol L-1 hydrochloric acid into the nebuliser-burner system of a flame atomic absorption spectrometer. The analytical figures of merit for the determination of copper are as follows: detection limit (3s), 0.06 microgram L-1; precision (RSD), 1.2% for 2 micrograms L-1; enrichment factor, 30 (using 25 mL of sample and 83 microL of eluent). Analysis of certified reference materials (SLEW-3 and NASS-5) showed good agreement with the certified value. This procedure was applied to the determination of copper in seawater samples from Galicia (Spain).

  20. Quantifying uncertainty in measurement of mercury in suspended particulate matter by cold vapor technique using atomic absorption spectrometry with hydride generator.

    Science.gov (United States)

    Singh, Nahar; Ahuja, Tarushee; Ojha, Vijay Narain; Soni, Daya; Tripathy, S Swarupa; Leito, Ivo

    2013-01-01

    As a result of rapid industrialization several chemical forms of organic and inorganic mercury are constantly introduced to the environment and affect humans and animals directly. All forms of mercury have toxic effects; therefore accurate measurement of mercury is of prime importance especially in suspended particulate matter (SPM) collected through high volume sampler (HVS). In the quantification of mercury in SPM samples several steps are involved from sampling to final result. The quality, reliability and confidence level of the analyzed data depends upon the measurement uncertainty of the whole process. Evaluation of measurement uncertainty of results is one of the requirements of the standard ISO/IEC 17025:2005 (European Standard EN IS/ISO/IEC 17025:2005, issue1:1-28, 2006). In the presented study the uncertainty estimation in mercury determination in suspended particulate matter (SPM) has been carried out using cold vapor Atomic Absorption Spectrometer-Hydride Generator (AAS-HG) technique followed by wet chemical digestion process. For the calculation of uncertainty, we have considered many general potential sources of uncertainty. After the analysis of data of seven diverse sites of Delhi, it has been concluded that the mercury concentration varies from 1.59 ± 0.37 to 14.5 ± 2.9 ng/m(3) with 95% confidence level (k = 2).

  1. A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Yebra, M. Carmen

    2012-01-01

    A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6%) and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4–25.61 μg g−1 for iron, 5.74–18.30 μg g−1 for manganese, and 33.27–57.90 μg g−1 for zinc in soluble solid food samples and 3.75–9.90 μg g−1 for iron, 0.47–5.05 μg g−1 for manganese, and 1.55–15.12 μg g−1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors. PMID:22567553

  2. Determination of Cu, Cd, Pb and Cr in yogurt by slurry sampling electrothermal atomic absorption spectrometry: A case study for Brazilian yogurt.

    Science.gov (United States)

    de Andrade, Camila Kulek; de Brito, Patrícia Micaella Klack; Dos Anjos, Vanessa Egéa; Quináia, Sueli Pércio

    2018-02-01

    A slurry sampling electrothermal atomic absorption spectrometric method is proposed for the determination of trace elements such as Cu, Cr, Cd and Pb in yogurt. The main factors affecting the slurry preparation were optimized: nature and concentration of acid solution and sonication time. The analytical method was validated in-house by calibration, linearity, limits of detection and quantification, precision and accuracy test obtaining satisfactory results in all cases. The proposed method was applied for the determination of Cd, Cr, Cu and Pb in some Brazilian yogurt samples. For these samples, the concentrations ranged from 2.5±0.2 to 12.4±0.2ngg-1; 34±3 to 899±7ngg-1; <8.3 to 12±1ngg-1; and <35.4 to 210±16ngg-1 for Cd, Cu, Cr and Pb, respectively. The daily intake of Cd, Cu, Cr and Pb via consumption of these samples was estimated. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Dried polyacrylamide gel absorption: a method for efficient elimination of the interferences from SDS-solubilized protein samples in mass spectrometry-based proteome analysis.

    Science.gov (United States)

    Zhou, Jian; Li, Jianglin; Li, Jianjun; Chen, Ping; Wang, Xianchun; Liang, Songping

    2010-12-01

    Sample preparation holds an important place in MS-based proteome analysis. For effective proteolysis and MS analysis, it is essential to eliminate the interferences while extracting the analytes of interest from complex mixtures. To address this, herein we describe a new dried polyacrylamide gel absorption method. In this method, the protein sample prepared using high concentration of SDS was directly and completely absorbed by vacuum-dried polyacrylamide gel, and then the interfering substances including SDS and some other salts were efficiently removed by in-gel washing steps while retaining the denatured proteins in the gel, thus offering a clean environment amenable to downstream buffer exchange, proteolytic digestion and digest recovery, etc. In combination with in-gel digestion and LC-MS/MS, the newly developed method was applied to the proteome analyses of membrane-enriched fraction and whole tissue homogenate. It was demonstrated that the method is suitable for the analysis of a complex biological sample and can be widely used for sample cleanup in shotgun proteome analyses.

  4. A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry in water samples

    Directory of Open Access Journals (Sweden)

    Arpa Şahin Ç.

    2013-04-01

    Full Text Available A simple, rapid and inexpensive solidified floating organic drop microextraction (SFODME and flow injection flame atomic absorption spectrometric determination (FI-FAAS method for copper was developed. 3-amino-7-dimethylamino-2-methylphenazine (Neutral red, NR was used as the complexing agent. Several factors affecting the microextraction efficiency, such as, pH, NR and sodium dodecylbenzenesulfonate (SDBS concentration, extraction time, stirring rate, and temperature were investigated and optimized. Under optimized experimental conditions an enrichment factor of 541 was obtained for 100 mL of sample solution. The calibration graph was linear in the range of 0.5 – 20.0 ng mL–1 and the limit of detection (3s was 0.18 ng mL–1, the limit of quantification (10s was 0.58 ng mL–1. The relative standard deviation (RSD for 10 replicate measurements of 10 ng mL–1 copper was 2.7%. The developed method was successfully applied to the extraction and determination of copper in different certified reference materials (Estuarine water, Slew 3 and fortified water, TM 23.2 and real water samples and satisfactory results were obtained.

  5. Medieval glass from the Cathedral in Paderborn: a comparative study using X-ray absorption spectroscopy, X-ray fluorescence, and inductively coupled laser ablation mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hormes, J. [University of Saskatchewan, Canadian Light Source Inc., Saskatoon, SK (Canada); Louisiana State University, CAMD, Baton Rouge, LA (United States); Roy, A.; Bovenkamp, G.L. [Louisiana State University, CAMD, Baton Rouge, LA (United States); Simon, K. [University of Goettingen, Geochemistry, Centre for Geosciences, Goettingen (Germany); Kim, C.Y. [University of Saskatchewan, Canadian Light Source Inc., Saskatoon, SK (Canada); Boerste, N. [Faculty for Theology Paderborn, Paderborn (Germany); Gai, S. [LWL - Archaeologie fuer Westfalen, Muenster (Germany)

    2013-04-15

    We have investigated four stained glass samples recovered from an archaeological excavation at the Cathedral in Paderborn (Germany) between 1978 and 1980. On two of the samples there are parts of paintings. Concentrations of major elements were determined using two independent techniques: LA-ICP-MS (a UV laser ablation microsampler combined with an inductively coupled plasma mass spectrometer) and synchrotron radiation X-ray excited X-ray fluorescence (SR-XRF). The SR-XRF data were quantified by using the program package PyMCA developed by the software group of the ESRF in Grenoble. Significant differences were found between the concentrations determined by the two techniques that can be explained by concentration gradients near the surface of the glasses caused, for example, by corrosion/leaching processes and the different surface sensitivities of the applied techniques. For several of the elements that were detected in the glass and in the colour pigments used for the paintings X-ray absorption near edge structure (XANES) spectra were recorded in order to determine the chemical speciation of the elements of interest. As was expected, most elements in the glass were found as oxides in their most stable form. Two notable exceptions were observed: titanium was not found as rutile - the most stable form of TiO{sub 2} - but in the form of anatase, and lead was not found in one defined chemical state but as a complex mixture of oxide, sulphate, and other compounds. (orig.)

  6. Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Acar, Orhan

    2012-10-01

    Full Text Available The Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS using an Sc + Ir + NH4H2PO4 chemical modifier mixture and flame atomic absorption spectrometer (FAAS after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 μg L–1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH4H2PO4 mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compared with international and national food quality guidelines as well as with literature values.

    Se han determinado los metales Cd, Cu, Pb, Fe y Zn en aceites vegetales comestibles (soja, girasol, flores, nueces, maíz y aceite de oliva y aceitunas (aceitunas-1, negra, verde, negra machacadas con semillas y verde machacadas con semillas mediante espectrometría de absorción atómica electrotérmica (ETAAS utilizando como modificador químico la mezcla Sc + Ir + NH4H2PO4 y mediante espectrometría de absorción atómica de llama (FAAS tras digestión con microondas. Se estudiaron las temperaturas de pirólisis y atomización para Cd

  7. Selective determination of inorganic cobalt in nutritional supplements by ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Berton, Paula; Martinis, Estefania M. [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Martinez, Luis D. [INQUISAL-CONICET, Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, San Luis (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

    2012-02-03

    Highlights: Black-Right-Pointing-Pointer Synergy of ultrasound energy and TILDLME technique for improved metal extraction. Black-Right-Pointing-Pointer Highly selective determination of inorganic Co species at trace levels. Black-Right-Pointing-Pointer Speciation analysis of Co in several nutritional supplements with highly complex matrices. Black-Right-Pointing-Pointer Development of an environmentally friendly microextraction technique with minimal waste production and sample consumption. - Abstract: In the present work, a simple and rapid analytical method based on application of ionic liquids (ILs) for inorganic Co(II) species (iCo) microextraction in a variety of nutrient supplements was developed. Inorganic Co was initially chelated with 1-nitroso-2-naphtol (1N2N) reagent followed by a modern technique named ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction (USA-TILDLME). The extraction was performed with 1-hexyl-3-methylimidazolium hexafluorophosphate [C{sub 6}mim][PF{sub 6}] with the aid of ultrasound to improve iCo recovery. Finally, the iCo-enriched IL phase was solubilized in methanol and directly injected into an electrothermal atomic absorption spectrometer (ETAAS). Several parameters that could influence iCo microextraction and detection were carefully studied. Since the main difficulty in these samples is caused by high concentrations of potential interfering ions, different approaches were evaluated to eliminate interferences. The limit of detection (LOD) was 5.4 ng L{sup -1}, while the relative standard deviation (RSD) was 4.7% (at 0.5 {mu}g L{sup -1} Co level and n = 10), calculated from the peak height of absorbance signals. Selective microextraction of iCo species was achieved only by controlling the pH value during the procedure. The method was thus successfully applied for determination of iCo species in nutritional supplements.

  8. Preconcentration and determination of boron in milk, infant formula, and honey samples by solid phase extraction-electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, I.; Vinas, P.; Romero-Romero, R. [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, M. [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain)], E-mail: hcordoba@um.es

    2009-02-15

    This work presents alternative procedures for the electrothermal atomic absorption spectrometric determination of boron in milk, infant formulas, and honey samples. Honey samples (10% m/v) were diluted in a medium containing 1% v/v HNO{sub 3} and 50% v/v H{sub 2}O{sub 2} and introduced in the atomizer. A mixture of 20 {mu}g Pd and 0.5 {mu}g Mg was used for chemical modification. Calibration was carried out using aqueous solutions prepared in the same medium, in the presence of 10% m/v sucrose. The detection limit was 2 {mu}g g{sup -1}, equivalent to three times the standard error of the estimate (s{sub y/x}) of the regression line. For both infant formulas and milk samples, due to their very low boron content, we used a procedure based on preconcentration by solid phase extraction (Amberlite IRA 743), followed by elution with 2 mol L{sup -1} hydrochloric acid. Detection limits were 0.03 {mu}g g{sup -1} for 4% m/v honey, 0.04 {mu}g g{sup -1} for 5% m/v infant formula and 0.08 {mu}g mL{sup -1} for 15% v/v cow milk. We confirmed the accuracy of the procedure by comparing the obtained results with those found via a comparable independent procedure, as well by the analysis of four certified reference materials.

  9. Method development for the control determination of mercury in seafood by solid-sampling thermal decomposition amalgamation atomic absorption spectrometry (TDA AAS).

    Science.gov (United States)

    Torres, D P; Martins-Teixeira, M B; Silva, E F; Queiroz, H M

    2012-01-01

    A very simple and rapid method for the determination of total mercury in fish samples using the Direct Mercury Analyser DMA-80 was developed. In this system, a previously weighted portion of fresh fish is combusted and the released mercury is selectively trapped in a gold amalgamator. Upon heating, mercury is desorbed from the amalgamator, an atomic absorption measurement is performed and the mercury concentration is calculated. Some experimental parameters have been studied and optimised. In this study the sample mass was about 100.0 mg. The relative standard deviation was lower than 8.0% for all measurements of solid samples. Two calibration curves against aqueous standard solutions were prepared through the low linear range from 2.5 to 20.0 ng of Hg, and the high linear range from 25.0 to 200.0 ng of Hg, for which a correlation coefficient better than 0.997 was achieved, as well as a normal distribution of the residuals. Mercury reference solutions were prepared in 5.0% v/v nitric acid medium. Lyophilised fish tissues were also analysed; however, the additional procedure had no advantage over the direct analysis of the fresh fish, and additionally increased the total analytical process time. A fish tissue reference material, IAEA-407, was analysed and the mercury concentration was in agreement with the certified value, according to the t-test at a 95% confidence level. The limit of quantification (LOQ), based on a mercury-free sample, was 3.0 µg kg(-1). This LOQ is in accordance with performance criteria required by the Commission Regulation No. 333/2007. Simplicity and high efficiency, without the need for any sample preparation procedure, are some of the qualities of the proposed method.

  10. Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sigrist, Mirna, E-mail: msigrist@fiq.unl.edu.ar [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Albertengo, Antonela; Beldomenico, Horacio [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Tudino, Mabel [Laboratorio de Analisis de Trazas, Departamento de Quimica Inorganica, Analitica y Quimica Fisica/INQUIMAE, Facultad de Ciencias Exactas y Naturales, Pabellon II, Ciudad Universitaria (1428), Buenos Aires (Argentina)

    2011-04-15

    A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH{sub 3} generation using 3.5 mol L{sup -1} HCl as carrier solution and 0.35% (m/v) NaBH{sub 4} in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl{sup -}, SO{sub 4}{sup 2-}, NO{sub 3}{sup -}, HPO{sub 4}{sup 2-}, HCO{sub 3}{sup -} on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C{sub 6}H{sub 8}O{sub 6} solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 {mu}g L{sup -1} and 0.6 {mu}g L{sup -1} for As(III) and inorganic total As, respectively, were obtained for a 500 {mu}L sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h{sup -1}. The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species

  11. Determination of V(IV) and V(V) by electrothermal atomic absorption spectrometry following selective solid-phase extraction and the study on the change in the oxidation state of vanadium species in seawater during the sample storage.

    Science.gov (United States)

    Nukatsuka, Isoshi; Shimizu, Yutaka; Ohzeki, Kunio

    2002-09-01

    The changes in the oxidation state of vanadium in artificial and natural seawater samples were studied by electrothermal atomic absorption spectrometry (ETAAS) with a direct injection of a resin suspension. V(IV) and V(V) were extracted as the complex with Chromazurol B and with N-cinnamoyl-N-2,3-xylylhydroxylamine, respectively, using a suspension of an anion-exchange resin and determined by ETAAS independently. The detection limits of both methods were 0.02 ng ml(-1) for 40 ml of a sample solution. The recovery tests for an artificial seawater sample spiked with V(IV) and/or V(V) were carried out carefully. The results showed that the recoveries of V(IV) or V(V) were 99.2-109% and the standard deviations were 1-6%. The total V was also determined after V(V) was reduced by ascorbic acid. In artificial seawater at pH 7.8, V(V) was stable but V(IV) was oxidized rapidly. In acidified artificial seawater (pH 2.0), V(IV) was oxidized slowly but only a small tendency of such reduction of V(V) was observed. In a natural seawater sample, V(IV) was not detected. The acidification of the natural seawater sample resulted in the reduction of V(V).

  12. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    Science.gov (United States)

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

  13. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

  14. Trace elements determination in high salinity petroleum produced formation water by high-resolution continuum source graphite furnace atomic absorption spectrometry after matrix separation using Chelex-100® resin

    Science.gov (United States)

    Freire, Aline Soares; Santelli, Ricardo Erthal

    2012-05-01

    This study describes a procedure used for the determination of trace metals (Co, Cu, Mn, Ni and Pb) in high salinity petroleum produced formation water (PFW) employing high-resolution continuum source graphite furnace atomic absorption spectrometry for detection and Chelex-100® resin for matrix elimination and analytes preconcentration. Using 15.0 mL of PFW for the separation/preconcentration, detection limits of 0.006, 0.07, 0.03, 0.08 and 0.02 μg L- 1 were obtained for Co, Cu, Mn, Ni and Pb, respectively. The accuracy of the proposed method was evaluated by analyzing three seawater certified reference materials and by recovery tests, and the data indicate that the methodology can be successfully applied to this kind of samples. The precision values, expressed as relative standard deviation (% RSD, n = 10) for 2.0 μg L- 1, were found to be 3.5, 4.0, 9.0, 5.3 and 5.9 for Co, Cu, Mn, Ni and Pb, respectively. The proposed procedure was applied for the determination of these metals in medium and high salinity PFW samples obtained from Brazilian offshore petroleum exploration platforms.

  15. Development of a new green non-dispersive ionic liquid microextraction method in a narrow glass column for determination of cadmium prior to couple with graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa; Shah, Faheem; Afridi, Hassan Imran; Citak, Demirhan

    2014-02-17

    Easy and innovative non-dispersive ionic liquid based microextraction (NDILME) has been developed for preconcentration of trace level of cadmium (Cd) in aqueous real surface water samples prior to couple with graphite furnace atomic absorption spectrometry (GFAAS). A 200 cm long narrow glass column containing aqueous solution of standard/sample was used to increase phase transfer ratio by providing more contact area between two medium (aqueous and extractive), which drastically improve the recoveries of labile hydrophobic chelate of Cd ammonium pyrrolidinedithiocarbamate (APDC), into ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6]. Different aspect of the desire method have been investigated and optimized. Under the optimized key experimental variables, limit of detection (LOD) and enhancement factor (EF) were achieved to be 0.5 ng L(-1) and 150, respectively. Reliability of the model method was checked by relative standard deviation (%RSD), which was found to be water samples (SLRS-4 Riverine water) using standard addition method. Application of the model method was productively performed by analysis of Cd in real surface water samples (tap and sea). Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Atmospheric Deposition of Heavy Metals around the Lead and Copper-Zinc Smelters in Baia Mare, Romania, Studied by the Moss Biomonitoring Technique, Neutron Activation Analysis and Flame Atomic Absorption Spectrometry

    CERN Document Server

    Culicov, O A; Steinnes, E; Okina, O S; Santa, Z; Todoran, R

    2002-01-01

    The mosses Pleurozium schreberi, Pseudoscleropodium purum and Rhytidiadelphus squarrosus were used as biomonitors to study the atmospheric deposition of heavy metals around the lead and copper-zinc smelters in Baia Mare. Samples representing the last three years' growth of moss or its green part, collected on the ground at 28 sites located 2-17 km from the source area, were analyzed by instrumental neutron activation analysis using epithermal neutrons and by flame atomic absorption spectrometry. A total of 31 elements were determined, including most of the heavy metals characteristic of emissions from this kind industry. The observed data for Pb, As, Cu, and Cd are all high compared with those observed in other regions of Europe with similar industries, but the concentrations in moss approach regional background levels at a distance of about 8 km from the main source area. Factor analysis of the data distinguishes two industrial components, one characterized by Pb, Cu, As, and Sb, and another one by Zn and Cd...

  17. Cobalt internal standard for Ni to assist the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis.

    Science.gov (United States)

    de Babos, Diego Victor; Bechlin, Marcos André; Barros, Ariane Isis; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta; de Oliveira, Silvana Ruella

    2016-05-15

    A new method is proposed for the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS), employing direct solid sample analysis (DSS) and internal standardization (IS). Cobalt was used as internal standard to minimize matrix effects during Ni determinations, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9937. The performance of the method was checked by analysis of six plant certified reference materials, and the results for Mo and Ni were in agreement with the certified values (95% confidence level, t-test). Analysis was made of different types of plant materials used as renewable sources of energy, including sugarcane leaves, banana tree fiber, soybean straw, coffee pods, orange bagasse, peanut hulls, and sugarcane bagasse. The concentrations found for Mo and Ni ranged from 0.08 to 0.63 ng mg(-1) and from 0.41 to 6.92 ng mg(-1), respectively. Precision (RSD) varied from 2.1% to 11% for Mo and from 3.7% to 10% for Ni. Limits of quantification of 0.055 and 0.074 ng were obtained for Mo and Ni, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Determination of arsenic in scalp hair samples from exposed subjects using microwave-assisted digestion with and without enrichment based on cloud point extraction by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Kazi, Tasneem Gul; Baig, Jameel Ahmad; Shah, Abdul Qadir; Kandhro, Ghulam Abbas; Khan, Sumaira; Afridi, Hassan Imran; Kolachi, Nida Fatima; Wadhwa, Sham Kumar; Shah, Faheem; Baig, Akhtar Mehmood

    2011-01-01

    A simple and rapid cloud point extraction (CPE) procedure was applied for preconcentration of trace quantities of arsenic (As) in scalp hair samples. The samples were subjected to microwave-assisted digestion in a mixture of nitric acid and hydrogen peroxide (2 + 1, v/v) prior to preconcentration by CPE. The As in digested samples was complexed with ammonium pyrrolidine dithiocarbamate (APDC), and the resultant As-PDC complex was extracted by a nonionic surfactant, octylphenoxypolyethoxyethanol (Triton X-114). After centrifugation, the surfactant-rich phase was diluted with 0.1 M HNO3 in methanol and analyzed by electrothermal atomic absorption spectrometry. The experimental parameters, i.e., amount of APDC, concentration of Triton X-114, equilibrium temperature and time, were optimized. For validation of the proposed method, a certified reference material (CRM) of human hair (BCR 397) was used. No significant difference (P > 0.05) was observed between the experimental results and certified values of the CRM (paired t-test). The LOD and LOQ obtained under the optimal conditions were 0.025 and 0.083 microg/kg, respectively. The developed method was applied for the determination of As in scalp hair samples from male and female subjects of two villages of Khairpur Mir's, Pakistan.

  19. Determination of essential and toxic elements in commercial baby foods by instrumental neutron activation analysis and atomic absorption spectrometry; Determinacao dos elementos essenciais e toxicos em alimentos comerciais infantis por analise por ativacao com neutrons e espectrometria de absorcao atomica

    Energy Technology Data Exchange (ETDEWEB)

    Vallinoto, Priscila

    2013-08-01

    The World Health Organization recommends that infants should be breast fed exclusively for at least six months after birth. After this period, it is recommended to start introducing complementary foods, in order to meet the child's nutritional, mineral and energy needs. Commercial food products for infants form an important part of the diet for many babies. Thus, it is very important that such food contains sufficient amounts of minerals. Inadequate complementary feeding is a major cause of high rates of infant malnutrition in developing countries. In this study, essential elements: Ca, Cl, Co, Cr, Fe, K, Mg, Mn, Na, Se and Zn and toxic elements: As, Cd, Hg levels were determined in twenty seven different commercial infant food product samples by Instrumental Neutron Activation Analysis (INAA) and Atomic Absorption Spectrometry (AAS). In order to validate both methodologies the reference material: INCT MPH-2 Mixed Polish Herbs and NIST - SRM 1577b Bovine Liver by INAA and NIST - SRM 1548th Typical Diet and NIST - SRM 1547 Peach Leaves by AAS were analyzed. The twenty seven baby food samples were acquired from Sao Paulo city supermarkets and stores. Essential and toxic elements were determined. Most of the essential element concentrations obtained were lower than the World Health Organization requirements, while concentrations of toxic elements were below the tolerable upper limit. These low essential element concentrations in these samples indicate that infants should not be fed only with commercial complementary foods. (author)

  20. Use of Doehlert and constrained mixture designs in the development of a photo-oxidation procedure using UV radiation/H₂O₂ for decomposition of landfill leachate samples and determination of metals by flame atomic absorption spectrometry.

    Science.gov (United States)

    Bezerra, Marcos A; Souza, Antônio D S; Oliveira, Rafael V; Oliveira, Djalma M; Cardoso, Luiz A M; Sousa Filho, Hélio R

    2015-03-01

    This work proposes the use of photo-oxidation degradation with UV radiation/H2O2 as sample treatment for the determination of Fe, Zn, Mn, Ni and Co in municipal solid waste landfill leachate by flame atomic absorption spectrometry (FAAS). Three variables (pH, irradiation time and buffer concentration) were optimized using Doehlert design and the proportions of mixture components submitted to UV radiation (leachate sample, buffer solution and H2O2 30%, v/v) were optimized using a constrained mixture design. Using the experimental conditions established, this procedure allows limits of detection of 0.075, 0.025, 0.010, 0.075 and 0.041 µg mL-1, and the precision levels expressed as relative standard (%RSD, 0.5 µg mL-1) were 3.6, 1.8, 1.3, 3.3 and 1.7%, for Fe, Mn, Zn, Ni and Co respectively. Recovery tests were carried out for evaluation of the procedure accuracy and recoveries were between 92 and 106% for the studied metals. This procedure has been applied for the analysis of the landfill leachate collected in Jequié, a city of the southwestern region of the State of Bahia, Brazil. The results were compared with those obtained by acid digestion. There was no significant difference between the results obtained by the two methods based on paired t-test at 95% confidence level.

  1. Use of Doehlert and constrained mixture designs in the development of a photo-oxidation procedure using UV radiation/H2O2 for decomposition of landfill leachate samples and determination of metals by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Marcos A. Bezerra

    2015-03-01

    Full Text Available This work proposes the use of photo-oxidation degradation with UV radiation/H2O2 as sample treatment for the determination of Fe, Zn, Mn, Ni and Co in municipal solid waste landfill leachate by flame atomic absorption spectrometry (FAAS. Three variables (pH, irradiation time and buffer concentration were optimized using Doehlert design and the proportions of mixture components submitted to UV radiation (leachate sample, buffer solution and H2O2 30%, v/v were optimized using a constrained mixture design. Using the experimental conditions established, this procedure allows limits of detection of 0.075, 0.025, 0.010, 0.075 and 0.041 µg mL-1, and the precision levels expressed as relative standard (%RSD, 0.5 µg mL-1 were 3.6, 1.8, 1.3, 3.3 and 1.7%, for Fe, Mn, Zn, Ni and Co respectively. Recovery tests were carried out for evaluation of the procedure accuracy and recoveries were between 92 and 106% for the studied metals. This procedure has been applied for the analysis of the landfill leachate collected in Jequié, a city of the southwestern region of the State of Bahia, Brazil. The results were compared with those obtained by acid digestion. There was no significant difference between the results obtained by the two methods based on paired t-test at 95% confidence level.

  2. Ligandless surfactant mediated solid phase extraction combined with Fe₃O₄ nano-particle for the preconcentration and determination of cadmium and lead in water and soil samples followed by flame atomic absorption spectrometry: multivariate strategy.

    Science.gov (United States)

    Jalbani, N; Soylak, M

    2014-04-01

    In the present study, a microextraction technique combining Fe3O4 nano-particle with surfactant mediated solid phase extraction ((SM-SPE)) was successfully developed for the preconcentration/separation of Cd(II) and Pb(II) in water and soil samples. The analytes were determined by flame atomic absorption spectrometry (FAAS). The effective variables such as the amount of adsorbent (NPs), the pH, concentration of non-ionic (TX-114) and centrifugation time (min) were investigated by Plackett-Burman (PBD) design. The important variables were further optimized by central composite design (CCD). Under the optimized conditions, the detection limits (LODs) of Cd(II) and Pb(II) were 0.15 and 0.74 µg/L, respectively. The validation of the proposed procedure was checked by the analysis of certified reference materials of TMDA 53.3 fortified water and GBW07425 soil. The method was successfully applied for the determination of Cd(II) and Pb(II) in water and soil samples. Copyright © 2014 Elsevier Inc. All rights reserved.

  3. Determination of Ultra-trace Rhodium in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction Using 2-(5-Iodo-2-Pyridylazo)-5-Dimethylaminoaniline as a Chelating Agent.

    Science.gov (United States)

    Han, Quan; Huo, Yanyan; Wu, Jiangyan; He, Yaping; Yang, Xiaohui; Yang, Longhu

    2017-03-24

    A highly sensitive method based on cloud point extraction (CPE) separation/preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection has been developed for the determination of ultra-trace amounts of rhodium in water samples. A new reagent, 2-(5-iodo-2-pyridylazo)-5-dimethylaminoaniline (5-I-PADMA), was used as the chelating agent and the nonionic surfactant TritonX-114 was chosen as extractant. In a HAc-NaAc buffer solution at pH 5.5, Rh(III) reacts with 5-I-PADMA to form a stable chelate by heating in a boiling water bath for 10 min. Subsequently, the chelate is extracted into the surfactant phase and separated from bulk water. The factors affecting CPE were investigated. Under the optimized conditions, the calibration graph was linear in the range of 0.1-6.0 ng/mL, the detection limit was 0.023 ng/mL for rhodium and relative standard deviation was 3.67% (c = 1.0 ng/mL, n = 11).The method has been applied to the determination of trace rhodium in water samples with satisfactory results.

  4. Synthesis and application of a nanoporous ion-imprinted polymer for the separation and preconcentration of trace amounts of vanadium from food samples before determination by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Dehghanpoor Frashah, Shahab

    2016-04-01

    A vanadium ion-imprinted polymer was synthesized in the presence of V(V) and N-benzoyl-N-phenyl hydroxyl amine using 4-vinyl pyridine as the monomer, ethylene glycol dimethacrylate as the cross linker and 2,2'-azobis(isobutyronitrile) as the initiator. The imprinted V(V) ions were completely removed by leaching the polymer with 5 mol/L nitric acid, and the polymer structure was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The ion-imprinted polymer was used as the sorbent in the development of the solid-phase extraction method for V(V) prior to its determination by electrothermal atomic absorption spectrometry. The maximum sorption capacity for V(V) ions was 26.7 mg/g at pH 4.0. Under the optimum conditions, for a sample volume of 150.0 mL, an enrichment factor of 289.0 and a detection limit of 6.4 ng/L were obtained. The developed method was successfully applied to the determination of vanadium in parsley, zucchini, black tea, rice, and water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Simultaneous Preconcentration of Copper and Cadmium by Dispersive Liquid-Liquid Microextraction Using N,N'-Bis (2-Hydroxy-5-Bromo-Benzyl)1,2 Diaminopropane and Their Determination by Flame Atomic Absorption Spectrometry.

    Science.gov (United States)

    Arslan, Osman; Karadaş, Cennet; Kara, Derya

    2016-09-01

    In the present study, the simultaneous preconcentration of copper and cadmium based on dispersive liquid-liquid microextraction as a prior step to their determination using flame atomic absorption spectrometry was developed. Carbon tetrachloride and N,N'-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane were used as the extraction solvent and chelating ligand, respectively. Some parameters that influence the extraction efficiency-e.g., sample pH, volume of extraction solvent (carbon tetrachloride), concentration of the chelating ligand, effect of salt addition, and sample volume-were investigated and optimized. With a preconcentration factor of 10, the LODs (3σ) for Cd and Cu were 0.69 and 1.98 μg/L, respectively. The accuracy of the developed method was evaluated by analyzing SLRS-5 river water and SRM 1573a tomato leaves certified reference materials. Results obtained were in good agreement with the certified values. The proposed method was successfully applied to river water, seawater, and black tea samples. Good spike recoveries, varying within the range of 97.5 to 116.9%, confirmed the good performance of the method in real sample analysis.

  6. Biosorption using chitosan thiourea polymer as an extraction and preconcentration technique for copper prior to its determination in environmental and food samples by flame atomic absorption spectrometry: Synthesis, characterization and analytical applications.

    Science.gov (United States)

    Al-Saidi, H M

    2016-12-01

    The present work describes the synthesis and use of the chitosan thiourea polymer (CT polymer) as a novel biosorbent for copper preconcentration prior to its determination by flame atomic absorption spectrometry (FAAS). CT polymer submitted in the present study was synthesized by the direct reaction between chitosan isolated from penaeus monodon chitin and ammonium thiocyanate, then the chemical structure and morphology of polymer were investigated by spectroscopic measurements, thermal analysis, X-ray diffraction (XRD) and scanning electron microscope (SEM). The results of SEM and XRD show that the prepared CT polymer has rough and hard surface with pores and nanofibers structure in the α-form. The height equivalent to the theoretical plates (HETP), the plates number (N), LOD and LOQ of CT polymer packed column were calculated to be 0.10±0.04mm, 100±2.02, 0.3μgL(-1)and 0.99μgL(-1), respectively. The developed column was employed in combination with FAAS for the analysis of copper in a certified reference material (NRCC-SLRS-4 Riverine water), potato, tea, and rice. Furthermore, the structure of the copper complex with CT polymer was proven with the aid of different spectroscopic and magnetic measurements. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Determination of lead at trace levels in mussel and sea water samples using vortex assisted dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry.

    Science.gov (United States)

    Erarpat, Sezin; Özzeybek, Gözde; Chormey, Dotse Selali; Bakırdere, Sezgin

    2017-12-01

    In this study, dispersive liquid-liquid microextraction (DLLME) and slotted quartz tube (SQT) were coupled to flame atomic absorption spectrometry (FAAS) to increase the sensitivity of lead. Conditions such as the formation of the lead-dithizone complex, efficiency of the DLLME method and the output of the SQT were systematically optimized to improve the detection limit for the analyte. The conventional FAAS system was improved upon by about 3.0 times with SQT-FAAS, 32 times with DLLME-FAAS and 142 times with DLLME-SQT-FAAS. The method was applicable over a wide linear range (10-500 μg L -1 ). The limit of detection (LOD) determined by DLLME-SQT-FAAS for seawater and mussel were 2.7 μg L -1 and 270 μg kg -1 , respectively. The percent recoveries obtained for mussel and seawater samples (spiked at 20 and 50 μg L -1 ) were 95-96% and 98-110%, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Application of fractional factorial design and Doehlert matrix in the optimization of experimental variables associated with the ultrasonic-assisted acid digestion of chocolate samples for aluminum determination by atomic absorption spectrometry.

    Science.gov (United States)

    Jalbani, Nusrat; Kazi, Tasneem Gul; Jamali, Muhammad Khan; Arain, Muhammad Balal; Afridi, Hassan Imran; Sheerazi, Syed T; Ansari, Rehana

    2007-01-01

    A simple and rapid method based on ultrasound energy is described for the determination of aluminum (AI) in complex matrixes of chocolate and candy samples by electrothermal atomic absorption spectrometry. The optimization strategy was carried out using multivariate methodologies. Five variables (temperature of the ultrasonic bath; exposure time to ultrasound energy; volumes of 2 acid mixtures, HNO3-H2SO4-H2O2 (1 + 1 + 1) and HNO3-H2O2 (1 + 1); and sample mass) were considered as factors in the optimization process. Interactions between analytical factors and their optimal levels were investigated using fractional factorial and Doehlert matrix designs. Validation of the ultrasonic-assisted acid digestion procedure was performed against standard reference materials, milk powder (SRM 8435) and wheat flour (SRM 1567a). The proposed procedure allowed Al determination with a detection limit of 2.3 microg/L (signal-to-noise = 3) and a precision, calculated as relative standard deviation, of 2.2% for a set of 10 measurements of certified samples. The recovery of Al by the proposed procedure was close to 100%, and no significant difference at the 95% confidence level was found between determined and certified values of Al. The proposed procedure was applied to the determination of Al in chocolate and candy samples. The results indicated that cocoa-based chocolates have higher contents of Al than milk- and sugar-based chocolates and candies.

  9. Investigation of (235)U, (226)Ra, (232)Th, (40)K, (137)Cs, and heavy metal concentrations in Anzali international wetland using high-resolution gamma-ray spectrometry and atomic absorption spectroscopy.

    Science.gov (United States)

    Zare, Mohammad Reza; Kamali, Mahdi; Fallahi Kapourchali, Maryam; Bagheri, Hashem; Khoram Bagheri, Mahdi; Abedini, Ali; Pakzad, Hamid Reza

    2016-02-01

    Measurements of natural radioactivity levels and heavy metals in sediment and soil samples of the Anzali international wetland were carried out by two HPGe-gamma ray spectrometry and atomic absorption spectroscopy techniques. The concentrations of (235)U, (226)Ra, (232)Th, (40)K, and (137)Cs in sediment samples ranged between 1.05 ± 0.51-5.81 ± 0.61, 18.06 ± 0.63-33.36 ± .0.34, 17.57 ± 0.38-45.84 ± 6.23, 371.88 ± 6.36-652.28 ± 11.60, and 0.43 ± 0.06-63.35 ± 0.94 Bq/kg, while in the soil samples they vary between 2.36-5.97, 22.71-38.37, 29.27-42.89, 472.66-533, and 1.05-9.60 Bq/kg for (235)U, (226)Ra, (232)Th, (40)K, and (137)Cs, respectively. Present results are compared with the available literature data and also with the world average values. The radium equivalent activity was well below the defined limit of 370 Bq/kg. The external hazard indices were found to be less than 1, indicating a low dose. Heavy metal concentrations were found to decrease in order as Fe > Mn > Sr > Zn > Cu > Cr > Ni > Pb > Co > Cd. These measurements will serve as background reference levels for the Anzali wetland.

  10. Decomposição ácida assistida por ultrassom para a determinação de Cu, Fe, Mg e Zn por F AAS em cerâmicas de uso doméstico

    Directory of Open Access Journals (Sweden)

    Eliézer Quadro Oreste

    Full Text Available This paper describes a sample preparation method for domestic ceramics, based on the acid decomposition assisted by ultrasound for further determination of Cu, Fe, Mg and Zn by Flame Atomic Absorption Spectrometry technique. The main optimized conditions were: particle size (25 µm; sample mass (25 mg and the acid volume (0.5 mL of HNO3 and 0.5 mL of HF. The samples were placed in an ultrasonic bath for 2 hours at 40 ºC. The method was employed for eight commercial samples of domestic ceramic, which showed different concentrations for all analytes investigated, showing the existing variety of raw materials. The method showed good accuracy and precision, attested by the addition and recovery test, with values of 87 to 112% for all analytes and relative standard deviation lower than 3.0%.

  11. Decomposição de amostras de cerveja com sistema de refluxo para determinação monoelementar por F AAS/AES e determinação multielementar por MIP OES

    OpenAIRE

    Leão, Paulo Roberto Pereira de; Medina, Aline Lisbôa; Vieira, Mariana Antunes; Ribeiro,Anderson Schwingel

    2017-01-01

    Resumo Neste trabalho, é descrito o desenvolvimento de um método analítico para análise de amostras de cervejas por técnicas de espectrometria. As amostras foram preparadas por decomposição em meio ácido, em um sistema de refluxo, e as determinações foram realizadas por F AAS (Fe, Mg e Zn), F AES (Na) e MIP OES (Ca, Fe, K, Mg, Mn, Na, Ni e Zn). As melhores condições para a decomposição da amostra foram obtidas através de estudo com delineamento composto central rotacional: volume de 10,0 mL d...

  12. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of arsenic and selenium in water and sediment by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Jones, Sandra R.; Garbarino, John R.

    1999-01-01

    Graphite furnace-atomic absorption spectrometry (GF-AAS) is a sensitive, precise, and accurate technique that can be used to determine arsenic and selenium in samples of water and sediment. The GF-AAS method has been developed to replace the hydride generation-atomic absorption spectrometry (HG-AAS) methods because the method detection limits are similar, bias and variability are comparable, and interferences are minimal. Advantages of the GF-AAS method include shorter sample preparation time, increased sample throughput from simultaneous multielement analysis, reduced amount of chemical waste, reduced sample volume requirements, increased linear concentration range, and the use of a more accurate digestion procedure. The linear concentration range for arsenic and selenium is 1 to 50 micrograms per liter in solution; the current method detection limit for arsenic in solution is 0.9 microgram per liter; the method detection limit for selenium in solution is 1 microgram per liter. This report describes results that were obtained using stop-flow and low-flow conditions during atomization. The bias and variability of the simultaneous determination of arsenic and selenium by GF-AAS under both conditions are supported with results from standard reference materials--water and sediment, real water samples, and spike recovery measurements. Arsenic and selenium results for all Standard Reference Water Samples analyzed were within one standard deviation of the most probable values. Long-term spike recoveries at 6.25, 25.0, 37.5 micrograms per liter in reagent-, ground-, and surface-water samples for arsenic averaged 103 plus or minus 2 percent using low-flow conditions and 104 plus or minus 4 percent using stop-flow conditions. Corresponding recoveries for selenium were 98 plus or minus 13 percent using low-flow conditions and 87 plus or minus 24 percent using stop-flow conditions. Spike recoveries at 25 micrograms per liter in 120 water samples ranged from 97 to 99 percent

  13. Determination of diphenylarsinic acid, phenylarsonic acid and inorganic arsenic in drinking water by graphite-furnace atomic-absorption spectrometry after simultaneous separation and preconcentration with solid-phase extraction disks.

    Science.gov (United States)

    Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Nakamura, Toshihiro

    2013-01-01

    A simple method of graphite-furnace atomic-absorption spectrometry (GFAAS) after solid-phase extraction (SPE) was developed for the determination of diphenylarsinic acid (DPAA), phenylarsonic acid (PAA), and inorganic arsenic (iAs) in drinking water. This method involves the simultaneous collection of DPAA, PAA, and iAs using three stacked SPE disks, i.e., an Empore SDB-XD disk (the upper layer), an activated carbon disk (the middle layer), and a Cation-SR disk loaded with Zr and Ca (ZrCa-CED; the lower layer). A 200-mL aqueous sample was adjusted to pH 3 with nitric acid and passed through the SPE disks at a flow rate of 15 mL min(-1), to concentrate DPAA on the SDB-XD disk, PAA on the activated carbon disk, and iAs on the ZrCa-CED. The As compounds were eluted from the disks with 10 mL of ethanol containing 0.5 mol L(-1) ammonia solution for DPAA, 20 mL of 1 mol L(-1) ammonia solution for PAA, and 20 mL of 6 mol L(-1) hydrochloric acid for iAs. The eluates of DPAA, PAA, and iAs were diluted to 20, 25, and 25 mL, respectively, with deionized water, and then analyzed by GFAAS. The detection limits of As (three-times the standard deviation (n = 3) of the blank values) were 0.13 and 0.16 μg L(-1) at enrichment factors of 10 and 8, respectively, using a 200-mL water sample. Spike tests with 2 μg (10 μg L(-1)) of DPAA, PAA, and iAs in 200 mL of tap water and bottled drinking water showed good recoveries (96.1-103.8%).

  14. Effect of different precursors on generation of reference spectra for structural molecular background correction by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry: Determination of antimony in cosmetics.

    Science.gov (United States)

    Barros, Ariane Isis; Victor de Babos, Diego; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta

    2016-12-01

    Different precursors were evaluated for the generation of reference spectra and correction of the background caused by SiO molecules in the determination of Sb in facial cosmetics by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis. Zeolite and mica were the most effective precursors for background correction during Sb determination using the 217.581nm and 231.147nm lines. Full 2 3 factorial design and central composite design were used to optimize the atomizer temperature program. The optimum pyrolysis and atomization temperatures were 1500 and 2100°C, respectively. A Pd(NO 3 ) 2 /Mg(NO 3 ) 2 mixture was employed as the chemical modifier, and calibration was performed at 217.581nm with aqueous standards containing Sb in the range 0.5-2.25ng, resulting in a correlation coefficient of 0.9995 and a slope of 0.1548s ng -1 . The sample mass was in the range 0.15-0.25mg. The accuracy of the method was determined by analysis of Montana Soil (II) certified reference material, together with addition/recovery tests. The Sb concentration found was in agreement with the certified value, at a 95% confidence level (paired t-test). Recoveries of Sb added to the samples were in the range 82-108%. The limit of quantification was 0.9mgkg -1 and the relative standard deviation (n=3) ranged from 0.5% to 7.1%. From thirteen analyzed samples, Sb was not detected in ten samples (blush, eye shadow and compact powder); three samples (two blush and one eye shadow) presented Sb concentration in the 9.1-14.5mgkg -1 range. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Trace elements determination in high salinity petroleum produced formation water by high-resolution continuum source graphite furnace atomic absorption spectrometry after matrix separation using Chelex-100 Registered-Sign resin

    Energy Technology Data Exchange (ETDEWEB)

    Freire, Aline Soares [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Departamento de Quimica Analitica, Universidade Federal do Rio de Janeiro Av. Athos da Silveira Ramos 149, Centro de Tecnologia, Bloco A, Cidade Universitaria, Rio de Janeiro/RJ, 21941-909 (Brazil); Santelli, Ricardo Erthal, E-mail: santelli@iq.ufrj.br [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Departamento de Quimica Analitica, Universidade Federal do Rio de Janeiro Av. Athos da Silveira Ramos 149, Centro de Tecnologia, Bloco A, Cidade Universitaria, Rio de Janeiro/RJ, 21941-909 (Brazil)

    2012-05-15

    This study describes a procedure used for the determination of trace metals (Co, Cu, Mn, Ni and Pb) in high salinity petroleum produced formation water (PFW) employing high-resolution continuum source graphite furnace atomic absorption spectrometry for detection and Chelex-100 Registered-Sign resin for matrix elimination and analytes preconcentration. Using 15.0 mL of PFW for the separation/preconcentration, detection limits of 0.006, 0.07, 0.03, 0.08 and 0.02 {mu}g L{sup -1} were obtained for Co, Cu, Mn, Ni and Pb, respectively. The accuracy of the proposed method was evaluated by analyzing three seawater certified reference materials and by recovery tests, and the data indicate that the methodology can be successfully applied to this kind of samples. The precision values, expressed as relative standard deviation (% RSD, n = 10) for 2.0 {mu}g L{sup -1}, were found to be 3.5, 4.0, 9.0, 5.3 and 5.9 for Co, Cu, Mn, Ni and Pb, respectively. The proposed procedure was applied for the determination of these metals in medium and high salinity PFW samples obtained from Brazilian offshore petroleum exploration platforms. - Highlights: Black-Right-Pointing-Pointer Petroleum-produced formation water were analyzed for Co, Cu, Mn, Ni and Pb determination. Black-Right-Pointing-Pointer In batch analyte preconcentration/matrix separation using Chelex-100 Registered-Sign was used. Black-Right-Pointing-Pointer Detection limits between 0.006 and 0.08 {mu}g L{sup -1} were found by using HR-CS-GFAAS. Black-Right-Pointing-Pointer Trace elements characterization is possible using the developed method. Black-Right-Pointing-Pointer Maximum trace element concentrations found could support future Brazilian directives.

  16. Selective and sensitive speciation analysis of Cr(VI) and Cr(III), at sub-μgL-1 levels in water samples by electrothermal atomic absorption spectrometry after electromembrane extraction.

    Science.gov (United States)

    Tahmasebi, Zeinab; Davarani, Saied Saeed Hosseiny

    2016-12-01

    In this work, electromembrane extraction in combination with electrothermal atomic absorption spectrometry (ET-AAS) was investigated for speciation, preconcentration and quantification of Cr(VI) and Cr(III) in water samples through the selective complexation of Cr(VI) with 1,5-diphenylcarbazide (DPC) as a complexing agent. DPC reduces Cr(VI) to Cr(III) ions and then Cr(III) species are extracted based on electrokinetic migration of their cationic complex (Cr(III)-DPC) toward the negative electrode placed in the hollow fiber. Also, once oxidized to Cr(VI), Cr(III) ions in initial sample were determined by this procedure. The influence of extraction parameters such as pH, type of organic solvent, chelating agent concentration, stirring rate, extraction time and applied voltage were evaluated following a one-at-a-time optimization approach. Under optimized conditions, the extracted analyte was quantified by ETAAS, with an acceptable linearity in the range of 0.05-5ngmL-1 (R2 value=0.996), and a repeatability (%RSD) between 3.7% and 12.2% (n=4) for 5.0 and 1.0ngmL-1 of Cr(VI), respectively. Also, we obtained an enrichment factor of 110 that corresponded to the recovery of 66%. The detection limit (S/N ratio of 3:1) was 0.02ngmL-1. Finally, this new method was successfully employed to determine Cr(III) and Cr(VI) species in real water samples. Copyright © 2016. Published by Elsevier B.V.

  17. Speciation of As(III) and As(V) in water samples by graphite furnace atomic absorption spectrometry after solid phase extraction combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop.

    Science.gov (United States)

    Shamsipur, Mojtaba; Fattahi, Nazir; Assadi, Yaghoub; Sadeghi, Marzieh; Sharafi, Kiomars

    2014-12-01

    A solid phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, using diethyldithiphosphate (DDTP) as a proper chelating agent, has been developed as an ultra preconcentration technique for the determination of inorganic arsenic in water samples prior to graphite furnace atomic absorption spectrometry (GFAAS). Variables affecting the performance of both steps were thoroughly investigated. Under optimized conditions, 100mL of As(ΙΙΙ) solution was first concentrated using a solid phase sorbent. The extract was collected in 2.0 mL of acetone and 60.0 µL of 1-undecanol was added into the collecting solvent. The mixture was then injected rapidly into 5.0 mL of pure water for further DLLME-SFO. Total inorganic As(III, V) was extracted similarly after reduction of As(V) to As(III) with potassium iodide and sodium thiosulfate and As(V) concentration was calculated by difference. A mixture of Pd(NO3)2 and Mg(NO3)2 was used as a chemical modifier in GFAAS. The analytical characteristics of the method were determined. The calibration graph was linear in the rage of 10-100 ng L(-1) with detection limit of 2.5 ng L(-1). Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 80 ng L(-1) of As(ΙΙΙ) were 6.8% and 7.5%, respectively. The method was successfully applied to speciation of As(III), As(V) and determination of the total amount of As in water samples and in a certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop followed by electrothermal atomic absorption spectrometry for speciation of antimony (ΙΙΙ, V).

    Science.gov (United States)

    Eftekhari, Mohammad; Chamsaz, Mahmoud; Arbab-Zavar, Mohammad Hossein; Eftekhari, Ali

    2015-01-01

    Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop (VASEME-SFO) was used for preconcentration and speciation of antimony (ΙΙΙ, V) followed by electrothermal atomic absorption spectrometry (ETAAS). In this procedure, Triton X-114 was used as emulsifier and 1-undecanol was used as extraction solvent. This method is based on the complexation of Sb(ΙΙΙ) with dithizone (as complexing agent) at pH 2 and extraction of the resulting hydrophobic complex into the extraction solvent (1-undecanol) with vortex-assisted liquid phase microextraction, whereas Sb(V) remained in solution. Sb(ΙΙΙ) in extraction solvent was directly analyzed by ETAAS after dilution with ethanol, and Sb(V) was calculated by subtracting Sb(ΙΙΙ) from the total antimony after reducing Sb(V) to Sb(ΙΙΙ) by L-cysteine. Under the optimized condition, the calibration curve was linear in the range of 0.4-8 μg L(-1) of Sb(ΙΙΙ) with a correlation coefficient of 0.9995. The detection limit based on three times of the standard deviation of the blank (n = 8) was 0.09 μg L(-1). The validation and the recovery of the proposed method were performed by the analysis of a certified reference material and spike method. The obtained results were in very good agreements with certified values. The proposed method was successfully applied for the determination of antimony species at trace levels in different water samples.

  19. Doehlert matrix for optimisation of procedure for determination of nickel in saline oil-refinery effluents by use of flame atomic absorption spectrometry after preconcentration by cloud-point extraction.

    Science.gov (United States)

    Bezerra, Marcos de A; Conceição, André L B; Ferreira, Sérgio L C

    2004-02-01

    This paper proposes a preconcentration procedure for determination of nickel in saline aqueous waste samples by flame atomic absorption spectrometry (FAAS). It is based on cloud-point extraction of nickel(II) ions as 2-(5-bromo-2-pyridylazo)-5-diethilaminophenol (Br-PADAP) complexes using octylphenoxypolyethoxyethanol (Triton X-114) as surfactant. The optimisation step was performed using a four-variable Doehlert design, involving the factors centrifugation time (CT) of system after addition of surfactant, solution pH, methanol volume (MV) added at micellar phase, and buffer concentration (BC). The analytical response used was absorbance, after volume correction. Using the established experimental conditions in the optimisation step the procedure enables nickel determination with a detection limit (3 delta/ S) of 0.2 microg L(-1), quantification limit (10 delta/ S) of 0.7 microg L(-1), and precision, calculated as relative standard deviation ( RSD) of 4.7 ( n=8) and 3.5% ( n=8) for nickel concentration of 1 and 5 microg L(-1), respectively. The preconcentration factor, determined from the ratio of the slopes of the analytical curves with and without preconcentration, is 74. The recovery achieved for nickel determination in the presence of several cations demonstrated that this procedure could be applied for analysis of water samples. The robustness was checked by using saturated fractional factorial designs, centred on the established experimental conditions in the optimisation step. The results of these tests demonstrated that the variables centrifugation time and buffer concentration are robust for modification by 10% and that solution pH and methanol volume are robust for 5%. Accuracy was evaluated by using the certified material reference SLEW-3 estuarine water for trace metals. The procedure was used for determination of nickel in saline effluents from oil refinery samples. Recovery results (95-104%) indicate that the procedure has satisfactory accuracy for

  20. Speciation of As(ΙΙΙ)/As(V) and Total Inorganic Arsenic in Biological Fluids Using New Mode of Liquid-Phase Microextraction and Electrothermal Atomic Absorption Spectrometry.

    Science.gov (United States)

    Haghnazari, Lida; Mirzaei, Nezam; Arfaeinia, Hossein; Karimyan, Kamaladdin; Sharafi, Hooshmand; Fattahi, Nazir

    2017-08-12

    In this paper, a new extraction method based on countercurrent liquid-liquid microextraction (CLLME) has been developed for the extraction and preconcentration of inorganic arsenic (iAs) in plasma and urine samples prior to their analysis by electrothermal atomic absorption spectrometry (ETAAS). In this method, firstly, 5 ml of water is added to the extraction vessel. Then 30.0 μl of the extracting solvent is added to it in order for the extracting solvent to be placed in the narrow-necked vessel. In total, 10 ml of a standard solution or a pretreated real sample is added to the sample container and it is connected to the extraction vessel via a connector. While opening the embedded valve at the bottom of the sample container and the one in the extraction vessel, the sample solution flows into the extracting solvent with the same flow rate, leading to the successful extraction of metal ligand into the extracting organic solvent. Under the optimum conditions, calibration curves are linear in the range of 0.1-50 μg l -1 , and limit of detections (LODs) are in the range of 0.03-0.05 μg l -1 . The enhancement factor and enrichment factor were in the range of 220-240 and 198-212, respectively. Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 5.0 μg l -1 of arsenic were in the range of 2.3-3.5% and 4.0-5.7%, respectively. The applicability of the proposed CLLME and ETAAS methods was demonstrated by analyzing the iAs in spiked urine and plasma samples. The obtained recoveries of the arsenic in the range of 92-107% indicated the excellent capability of the developed method for speciation of arsenic from plasma and urine samples. Graphical Abstract ᅟ.

  1. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L{sup −1} and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L{sup −1} of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic.

  2. Combination of flame atomic absorption spectrometry with ...

    African Journals Online (AJOL)

    The accuracy was checked by analyzing a certified reference material from the National Institute of Standard and Technology, Trace elements in water (NIST CRM 1643e). KEY WORDS: Dispersive liquid–liquid microextraction, Lead determination, Preconcentration, Ligandless, Water analysis. Bull. Chem. Soc. Ethiop. 2013 ...

  3. optimization of flame atomic absorption spectrometry

    African Journals Online (AJOL)

    unesco

    cost-effective and routine analysis, who can not afford the expensive methods such as ICP-MS,. ICP-AES, ICP-OES etc. The study finally suggests the implications of the findings to chemical education. [AJCE, 2(3) .... findings of this study in teaching-learning program, because our optimized method is a rapid, cost-effective, ...

  4. LIMS for Lasers 2015 for achieving long-term accuracy and precision of δ2H, δ17O, and δ18O of waters using laser absorption spectrometry

    Science.gov (United States)

    Coplen, Tyler B.; Wassenaar, Leonard I

    2015-01-01

    RationaleAlthough laser absorption spectrometry (LAS) instrumentation is easy to use, its incorporation into laboratory operations is not easy, owing to extensive offline manipulation of comma-separated-values files for outlier detection, between-sample memory correction, nonlinearity (δ-variation with water amount) correction, drift correction, normalization to VSMOW-SLAP scales, and difficulty in performing long-term QA/QC audits.MethodsA Microsoft Access relational-database application, LIMS (Laboratory Information Management System) for Lasers 2015, was developed. It automates LAS data corrections and manages clients, projects, samples, instrument-sample lists, and triple-isotope (δ17O, δ18O, and δ2H values) instrumental data for liquid-water samples. It enables users to (1) graphically evaluate sample injections for variable water yields and high isotope-delta variance; (2) correct for between-sample carryover, instrumental drift, and δ nonlinearity; and (3) normalize final results to VSMOW-SLAP scales.ResultsCost-free LIMS for Lasers 2015 enables users to obtain improved δ17O, δ18O, and δ2H values with liquid-water LAS instruments, even those with under-performing syringes. For example, LAS δ2HVSMOW measurements of USGS50 Lake Kyoga (Uganda) water using an under-performing syringe having ±10 % variation in water concentration gave +31.7 ± 1.6 ‰ (2-σ standard deviation), compared with the reference value of +32.8 ± 0.4 ‰, after correction for variation in δ value with water concentration, between-sample memory, and normalization to the VSMOW-SLAP scale.ConclusionsLIMS for Lasers 2015 enables users to create systematic, well-founded instrument templates, import δ2H, δ17O, and δ18O results, evaluate performance with automatic graphical plots, correct for δ nonlinearity due to variable water concentration, correct for between-sample memory, adjust for drift, perform VSMOW-SLAP normalization, and perform long-term QA/QC audits

  5. Fluorine speciation analysis using reverse phase liquid chromatography coupled off-line to continuum source molecular absorption spectrometry (CS-MAS): identification and quantification of novel fluorinated organic compounds in environmental and biological samples.

    Science.gov (United States)

    Qin, Zhiwei; McNee, David; Gleisner, Heike; Raab, Andrea; Kyeremeh, Kwaku; Jaspars, Marcel; Krupp, Eva; Deng, Hai; Feldmann, Jörg

    2012-07-17

    Driven by increasing demand for the monitoring of industrial perfluorinated compounds (PFCs), the identification of novel fluorine containing compounds (FOCs) and the tracking of organofluorine drugs and their degradation products, there is a clear need for sensitive, fluorine-specific detection of unknown FOCs. Here we report the first ever direct fluorine-specific (speciation) method; capable of individually detecting untargeted FOCs in environmental and biological samples through the application of continuum source molecular absorption spectrometry (CS-MAS) using a commercial CS-AAS. Two model FOCs (2,4,6, trifluorobenzoic acid (TFBA) and 5-fluoroindol-5-carboxylic acid (FICA)) were used, achieving fluorine-specific detection across a range of 0.1 to 300 ng/mL fluorine, corresponding to a limit of detection of 4 pg F and 5.26 nM for both compounds. Both TFBA and FICA showed a similar response to CS-MAS detection, potentially enabling the quantification of fluorine content in novel FOCs without having molecular standards available. This paper also reports the use of reverse-phase high performance liquid chromatography (RP-HPLC) coupled off-line with CS-MAS for the identification of single organofluorines in a mixture of FOCs via fraction collection. The linear range of both FOCs was determined to be from 1 to 500 ng/mL. The limits of detection of those species were just above 1 ng/mL (100 pg) and can therefore compete with targeted analytical methods such as ESI-MS. Finally, as a proof of principle the analysis of a fluoride-containing groundwater sample from Ghana demonstrated that this method can be used in the detection of novel FOCs, with identification achieved through parallel ESI-MS. Coupled HPLC-CS-MAS/ESI-MS is the first analytical methodology capable of selectively detecting and identifying novel FOCs, making possible the quantification of all fluorine containing compounds in one sample. This is the necessary analytical requirement to perform

  6. Separation and preconcentration of platinum-group metals from spent autocatalysts solutions using a hetero-polymeric S, N-containing sorbent and determination by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Eskina, Vasilina V; Dalnova, Olga A; Filatova, Daria G; Baranovskaya, Vasilisa B; Karpov, Yuri A

    2016-10-01

    This paper describes the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for determination of Pt, Pd and Rh after separation and concentration by original in-house developed heterochain polymer S, N-containing sorbent. The methods of sample preparation of spent ceramic-based autocatalysts were considered, two of which were used: autoclave decomposition in mixture of acids HCl:HNO3 (3:1) and high-temperature melting with K2S2O7. Both methods anyway limit the direct determination of analytes by HR CS GFAAS. Using the first method it is an incomplete digestion of spent autocatalysts samples, since the precipitate is Si, and the rhodium metal dissolves with difficulty and partially passes into solution. In contrast to the first method, the second method allow to completely transfer analytes into solution, however, the background signal produced by the chemical composition of the flux, overlaps the analytical zone. It was found, that Pt, Pd and Rh contained in the spent ceramic automotive catalysts could be effectively separated and concentrated by heterochain polymer S, N-containing sorbent, which has high sorption capacity, selectivity and resistant to dilute acids. The chosen HR CS GFAAS analysis conditions enable us to determine Pt, Pd and Rh with good metrological characteristics. The concentrations of Pt, Pd and Rh in two samples of automobile exhaust catalysts were found in range of 0.00015-0.00050; 0.170-0.189; 0.0180-0.0210wt%, respectively. The relative standard deviation obtained by HR CS GFAAS was not more than 5%. Limits of detection by HR CS GFAAS achieved were 6.2·10(-6)wt% for Pt, 1.8·10(-6)wt% for Pd, and 3.4·10(-6)wt% for Rh. Limits of determination achieved by HR CS GFAAS were 1.1·10(-5)wt% for Pt, 6.9·10(-5)wt% for Pd, and 8.3·10(-5)wt% for Rh. To control the accuracy of PGM in sorption concentrates by HR CS GFAAS method, it was appropriate to conduct an inter-method comparative experiment. The

  7. Narrative absorption

    DEFF Research Database (Denmark)

    Narrative Absorption brings together research from the social sciences and Humanities to solve a number of mysteries: Most of us will have had those moments, of being totally absorbed in a book, a movie, or computer game. Typically we do not have any idea about how we ended up in such a state. No...

  8. Prediction of Molar Extinction Coefficients of Proteins and Peptides Using UV Absorption of the Constituent Amino Acids at 214 nm To Enable Quantitative Reverse Phase High-Performance Liquid Chromatography-Mass Spectrometry Analysis

    NARCIS (Netherlands)

    Kuipers, B.J.H.; Gruppen, H.

    2007-01-01

    The molar extinction coefficients of 20 amino acids and the peptide bond were measured at 214 nm in the presence of acetonitrile and formic acid to enable quantitative comparison of peptides eluting from reversed-phase high-performance liquid chromatography, once identified with mass spectrometry

  9. (EDXRF) spectrometry

    Indian Academy of Sciences (India)

    Unknown

    house developed CATXRF program. (Tiwari and Sawhney 2000), which is based on FP method and corrects for both absorption and enhancement effects. The peak areas have been determined by the use of non-. *Author for correspondence ...

  10. Mass spectrometry

    DEFF Research Database (Denmark)

    Nyvang Hartmeyer, Gitte; Jensen, Anne Kvistholm; Böcher, Sidsel

    2010-01-01

    Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) is currently being introduced for the rapid and accurate identification of bacteria. We describe 2 MALDI-TOF MS identification cases - 1 directly on spinal fluid and 1 on grown bacteria. Rapidly obtained r...

  11. Separation and preconcentration of ultratrace levels of cadmium(II) in a sequential injection (SI) system with a PTFE packed column as a mimic sequential injection lab-on-valve (SI-LOV) system with renewable column employing detection by electrothermal atomic absorption spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Gała, Piotr

    A sequential injection (SI) on-line separation and preconcentration system furnished with an external column packed with PTFE beads, serving as a mimic renewable microcolumn used in a sequential injection lab-on-valve (SI-LOV) system, was investigated for the determination of ultratrace levels...... of cadmium(II) by detection with electrothermal atomic absorption spectrometry (ETAAS). The non-charged complex formed between the analyste and the chelating reagent diethyldithiophosphate (DDPA) was selectively adsorbed on the surface of the PTFE beads and eluted by ethanol before being directed...... to the ETAAS. Two kinds of sorbents were investigated, that is, granular Algoflon® PTFE and Aldrich PTFE. A mimic external packed column was employed since difficulties of aspirating and discarding beads plus a high background signal were encountered in the renewable microcolumn SI-LOV system. As compared...

  12. Application of total reflection X-ray fluorescence spectrometry for ...

    Indian Academy of Sciences (India)

    in rainwater are, inductively coupled plasma-mass spectrometry (ICPMS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), atomic absorption spectrom- etry (AAS), X-ray fluorescence (XRF), total reflection X-ray fluorescence (TXRF), neu- tron activation analysis (NAA), electroanalytical techniques, etc.

  13. Speciation analysis of calcium, iron, and zinc in casein phosphopeptide fractions from toddler milk-based formula by anion exchange and reversed-phase high-performance liquid chromatography-mass spectrometry/flame atomic-absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Miquel, Esther; Alegria, Amparo; Barbera, Reyes; Farre, Rosaura [University of Valencia, Nutrition and Food Chemistry, Faculty of Pharmacy, Burjassot, Valencia (Spain)

    2005-03-01

    Casein phosphopeptides (CPP) are phosphorylated casein-derived peptides that can be released by in-vitro or in-vivo enzymatic hydrolysis of {alpha}{sub s1}-casein, {alpha}{sub s2}-casein, and {beta}-casein (CN). Many of these peptides contain a highly polar acidic sequence of three phosphoseryl groups followed by two glutamic acid residues. These domains are binding sites for minerals such as calcium, iron, and zinc and play an important role in mineral bioavailability. The aim of this study was speciation analysis of calcium, iron, and zinc in CPP fractions from the soluble fraction of a toddler milk-based formula. Methods for CPP separation by anion-exchange high-performance liquid chromatography (AE-HPLC) were combined with CPP identification by reversed-phase high performance liquid chromatography-electrospray ionization mass spectrometry and determination of the calcium, iron, zinc, and phosphorus content of the fractions obtained by AE-HPLC. Calcium and phosphorus were detected in all the analyzed AE-HPLC fractions. Calcium and zinc could be bound to CPP derived from {alpha}{sub s1}-CN and {alpha}{sub s2}-CN in fraction 3. Iron could be bound to CPP in fraction 4 in which {beta}-CN(15-34)4P was present with the cluster sequence S(P)S(P)S(P)EE. The results obtained prove the different distribution of calcium, iron, and zinc in heterogeneous CPP fractions. (orig.)

  14. Determination of Pb(II), Zn(II), Cd(II), and Co(II) ions by flame atomic absorption spectrometry in food and water samples after preconcentration by coprecipitation with Mo(VI)-diethyldithiocarbamate.

    Science.gov (United States)

    Tufekci, Mehmet; Bulut, Volkan Numan; Elvan, Hamide; Ozdes, Duygu; Soylak, Mustafa; Duran, Celal

    2013-02-01

    A new, simple, and rapid separation and preconcentration procedure, for determination of Pb(II), Cd(II), Zn(II), and Co(II) ions in environmental real samples, has been developed. The method is based on the combination of coprecipitation of analyte ions by the aid of the Mo(VI)-diethyldithiocarbamate-(Mo(VI)-DDTC) precipitate and flame atomic absorption spectrometric determinations. The effects of experimental conditions like pH of the aqueous solution, amounts of DDTC and Mo(VI), standing time, centrifugation rate and time, sample volume, etc. and also the influences of some foreign ions were investigated in detail on the quantitative recoveries of the analyte ions. The preconcentration factors were found to be 150 for Pb(II), Zn(II) and Co(II), and 200 for Cd(II) ions. The detection limits were in the range of 0.1-2.2 μg L(-1) while the relative standard deviations were found to be lower than 5 % for the studied analyte ions. The accuracy of the method was checked by spiked/recovery tests and the analysis of certified reference material (CRM TMDW-500 Drinking Water). The procedure was successfully applied to seawater and stream water as liquid samples and baby food and dried eggplant as solid samples in order to determine the levels of Pb(II), Cd(II), Zn(II), and Co(II) ions.

  15. Speciation of Tl(III and Tl(I in hair samples by dispersive liquid–liquid microextraction based on solidification of floating organic droplet prior to flame atomic absorption spectrometry determination

    Directory of Open Access Journals (Sweden)

    S.Z. Mohammadi

    2016-11-01

    Full Text Available Dispersive liquid–liquid microextraction based on solidification of floating organic droplet was successfully used as a sample preparation method prior to flame atomic absorption determination of trace amounts of Tl(III and Tl(I in hair samples. In the proposed method, 1-(2-pyridylazo-2-naphthol, 1-dodecanol and ethanol were used as chelating agent, extraction and dispersive solvent, respectively. Several factors that may be affected in the extraction process, such as type and volume of extraction and disperser solvents, pH, salting out effect, ionic strength and extraction time were studied. Under the optimal conditions, linearity was maintained between 6.0 and 900.0 ng mL−1 for Tl(III. The relative standard deviation for seven replicate determinations of 0.2 μg mL−1 Tl(III was 2.5%. The detection limit based on 3Sb for Tl(III in the original solution was 2.1 ng mL−1. The proposed method has been applied for the determination of trace amounts of thallium in hair samples and satisfactory results were obtained.

  16. Development of ultralow energy (1-10 eV) ion scattering spectrometry coupled with reflection absorption infrared spectroscopy and temperature programmed desorption for the investigation of molecular solids.

    Science.gov (United States)

    Bag, Soumabha; Bhuin, Radha Gobinda; Methikkalam, Rabin Rajan J; Pradeep, T; Kephart, Luke; Walker, Jeff; Kuchta, Kevin; Martin, Dave; Wei, Jian

    2014-01-01

    Extremely surface specific information, limited to the first atomic layer of molecular surfaces, is essential to understand the chemistry and physics in upper atmospheric and interstellar environments. Ultra low energy ion scattering in the 1-10 eV window with mass selected ions can reveal extremely surface specific information which when coupled with reflection absorption infrared (RAIR) and temperature programmed desorption (TPD) spectroscopies, diverse chemical and physical properties of molecular species at surfaces could be derived. These experiments have to be performed at cryogenic temperatures and at ultra high vacuum conditions without the possibility of collisions of neutrals and background deposition in view of the poor ion intensities and consequent need for longer exposure times. Here we combine a highly optimized low energy ion optical system designed for such studies coupled with RAIR and TPD and its initial characterization. Despite the ultralow collision energies and long ion path lengths employed, the ion intensities at 1 eV have been significant to collect a scattered ion spectrum of 1000 counts/s for mass selected CH2(+).

  17. Modified Activated Carbon Prepared from Acorn Shells as a New Solid-Phase Extraction Sorbent for the Preconcentration and Determination of Trace Amounts of Nickel in Food Samples Prior to Flame Atomic Absorption Spectrometry.

    Science.gov (United States)

    Ebrahimi, Bahram

    2017-03-01

    A new solid-phase extraction (SPE) sorbent was introduced based on acidic-modified (AM) activated carbon (AC) prepared from acorn shells of native oak trees in Kurdistan. Hydrochloric acid (15%, w/w) and nitric acid (32.5%, w/w) were used to condition and modify AC. The IR spectra of AC and AM-AC showed that AM lead to the formation of increasing numbers of acidic functional groups on AM-AC. AM-AC was used in the SPE method for the extraction and preconcentration of Ni+2 prior to flame atomic absorption spectrometric determination at ng/mL levels in model and real food samples. Effective parameters of the SPE procedure, such as the pH of the solutions, sorbent dosage, extraction time, sample volume, type of eluent, and matrix ions, were considered and optimized. An enrichment factor of 140 was obtained. The calibration curve was linear with an R2 of 0.997 in the concentration range of 1-220 ng/mL. The RSD was 5.67% (for n = 7), the LOD was 0.352 ng/mL, and relative recoveries in vegetable samples ranged from 96.7 to 103.7%.

  18. Fast sequential multi-element determination of Ca, Mg, K, Cu, Fe, Mn and Zn for foliar diagnosis using high-resolution continuum source flame atomic absorption spectrometry: Feasibility of secondary lines, side pixel registration and least-squares background correction

    Science.gov (United States)

    de Oliveira, Silvana Ruella; Raposo, Jorge Luiz, Jr.; Gomes Neto, José Anchieta

    2009-06-01

    The fast sequential multi-element determination of Ca, Mg, K, Cu, Fe, Mn and Zn in plant tissues by high-resolution continuum source flame atomic absorption spectrometry is proposed. For this, the main lines for Cu (324.754 nm), Fe (248.327 nm), Mn (279.482 nm) and Zn (213.857 nm) were selected, and the secondary lines for Ca (239.856 nm), Mg (202.582 nm) and K (404.414 nm) were evaluated. The side pixel registration approach was studied to reduce sensitivity and extend the linear working range for Mg by measuring at wings (202.576 nm; 202.577 nm; 202.578 nm; 202.580 nm; 202.585 nm; 202.586 nm; 202.587 nm; 202.588 nm) of the secondary line. The interference caused by NO bands on Zn at 213.857 nm was removed using the least-squares background correction. Using the main lines for Cu, Fe, Mn and Zn, secondary lines for Ca and K, and line wing at 202.588 nm for Mg, and 5 mL min - 1 sample flow-rate, calibration curves in the 0.1-0.5 mg L - 1 Cu, 0.5-4.0 mg L - 1 Fe, 0.5-4.0 mg L - 1 Mn, 0.2-1.0 mg L - 1 Zn, 10.0-100.0 mg L - 1 Ca, 5.0-40.0 mg L - 1 Mg and 50.0-250.0 mg L - 1 K ranges were consistently obtained. Accuracy and precision were evaluated after analysis of five plant standard reference materials. Results were in agreement at a 95% confidence level (paired t-test) with certified values. The proposed method was applied to digests of sugar-cane leaves and results were close to those obtained by line-source flame atomic absorption spectrometry. Recoveries of Ca, Mg, K, Cu, Fe, Mn and Zn in the 89-103%, 84-107%, 87-103%, 85-105%, 92-106%, 91-114%, 96-114% intervals, respectively, were obtained. The limits of detection were 0.6 mg L - 1 Ca, 0.4 mg L - 1 Mg, 0.4 mg L - 1 K, 7.7 µg L - 1 Cu, 7.7 µg L - 1 Fe, 1.5 µg L - 1 Mn and 5.9 µg L - 1 Zn.

  19. Comparison of 4 analytical techniques based on atomic spectrometry for the determination of total tin in canned foodstuffs

    OpenAIRE

    2011-01-01

    Abstract Different techniques for the determination of total tin in beverage and canned food by atomic spectrometry were compared. The performance characteristics of Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry (HG-ICP-AES), Electrothermal Atomization Atomic Absorption Spectrometry (ETA-AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) were determined in term of linearity, ...

  20. D-xylose absorption

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003606.htm D-xylose absorption To use the sharing features on this page, please enable JavaScript. D-xylose absorption is a laboratory test to determine ...

  1. Development of an analytical model for the determination of {sup 60}Co in aqueous samples by atomic absorption and gamma spectrometry techniques; Elaboracion de un modelo analitico para la determinacion de {sup 60}Co en muestras acuosas mediante tecnicas de absorcion atomica y espectrometria gamma

    Energy Technology Data Exchange (ETDEWEB)

    Solis A, N. A.

    2015-07-01

    The applications of the nuclear energy in industry and medicine generate radioactive wastes that must be isolated and confined in order to limit its spread in the biosphere. These types of wastes are generated in hospitals, industry, research centers and nuclear power plants (during de fuel cycle). The radioactive elements (radionuclides) cannot be destroyed by any known method, either chemical or mechanical. Its final destruction is produced by radioactive decay, which makes them stable isotopes, or nuclear transmutation being bombarded with atomic particles. Consequently, the radioactive waste management is to control the radioactive discharges and reduce to tolerable limits, eliminating of effluents and wastes the radionuclides of interest, concentrating them so they can be stored or evacuated so that later not appear in dangerous concentration in the biosphere. In Mexico, the main generators of radioactive wastes are the nuclear power plant of Laguna Verde in Veracruz, Hospitals of the public and private sector, in addition Instituto Nacional de Investigaciones Nucleares (ININ) some institutes and facilities of the UNAM and Instituto Politecnico Nacional (IPN) and industries among others. The aqueous radioactive wastes, particularly those from the nuclear power plants contain traces of cobalt-60. Currently there is no model or analytical technique for the separation of this radionuclide, so it became necessary to develop an analytical model for separation and facilitate their disposal. In this paper was shown that atomic absorption and gamma spectrometry techniques can separate the active concentration of the inactive, which is important because the total concentration can be associated through direct relationships with the wear of metal parts of the nuclear reactor, since the metal alloys of the same reactor containing a fraction of cobalt. Also this analytical and mathematical model that can be reproducible and applicable to full sets of samples and that this

  2. Determination of VOCs in traffic exhaust by FTIR absorption spectrometry

    Science.gov (United States)

    Sedlmaier, Achim; Schaefer, Klaus; Becker, K. H.; Brockmann, Klaus; Heland, Joerg; Kurtenbach, Ralf; Loerzer, J.; Wiesen, Peter

    1999-09-01

    Infrared spectral features of organic hydrocarbons were investigated with respect to single compounds. A separation and consequently a quantitative concentration determination is possible for ethane, ethene, ethyne, propene, iso-butene, benzene, toluene, o-xylene, m-xylene and p-xylene using a MCT detector with a cut-off frequency below 660 cm-1. The spectral features of propane, butane, pentane and hexane cannot be separated. In order to be able to derive parameters, such as detection limits, accuracy, precision and the influence of interfering species or different reference data, validation measurements were carried out in a road tunnel and in the laboratory using an open White mirror compartment and closed White cells. FTIR spectra were collected with two spectrometers at different spectral resolutions. Parallel GC measurements were made for comparison.

  3. combination of flame atomic absorption spectrometry with ligandless

    African Journals Online (AJOL)

    Preferred Customer

    The high efficiency of dispersive liquid-liquid microextraction to carry out the determination of trace amounts of lead in complex ... KEY WORDS: Dispersive liquid–liquid microextraction, Lead determination, Preconcentration, Ligandless,. Water analysis .... Mineral water samples were acquired from a local market. The only ...

  4. Combination of Flow Injection and Electrothermal Atomic Absorption Spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Nielsen, Steffen

    1999-01-01

    The paper discusses the advantages gained by exploiting this combination, FI-ETAAS. Emphasis is placed on illlustrating various avenues to perform on-line preconcentration of metal ions in order to obtain very low limits of detection of the measurand, and ways and means to enhance the selectivity...

  5. The Determination of Lead in Gasoline by Atomic Absorption Spectrometry.

    Science.gov (United States)

    Coleman, M. F. M.

    1985-01-01

    Describes an experiment that involves the extraction of lead from gasoline into an aqueous solvent using iodine monochloride reagent. This method (which avoids the aspiration of organic solvents) also illustrates the use of wavelengths other than the most sensitive wavelength and effects of flame stoichiometry and burner height upon absorbance.…

  6. [Study on lead absorption in pumpkin by atomic absorption spectrophotometry].

    Science.gov (United States)

    Li, Zhen-Xia; Sun, Yong-Dong; Chen, Bi-Hua; Li, Xin-Zheng

    2008-07-01

    A study was carried out on the characteristic of lead absorption in pumpkin via atomic absorption spectrophotometer. The results showed that lead absorption amount in pumpkin increased with time, but the absorption rate decreased with time; And the lead absorption amount reached the peak in pH 7. Lead and cadmium have similar characteristic of absorption in pumpkin.

  7. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina para espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method's performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 +- 11,70)mug.L{sup -1} with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10{mu}g.L{sup -1}. The

  8. Membrane Gas Absorption

    NARCIS (Netherlands)

    Jansen, A.E.; Klaassen, R.; Feron, P.H.M.

    1995-01-01

    Membrane gas absorption processes are absorption processes utilising hollow fibre membranes as contacting media for gas and liquid flows. The principle of operation and engineering aspects are discussed, followed by discussion of a number of typical applications. Benefits in terms of operation,

  9. Nutrition and magnesium absorption

    NARCIS (Netherlands)

    Brink, E.J.

    1992-01-01

    The influence of various nutrients present in dairy products and soybean-based products on absorption of magnesium has been investigated. The studies demonstrate that soybean protein versus casein lowers apparent magnesium absorption in rats through its phytate component. However, true

  10. Solar absorption surface panel

    Science.gov (United States)

    Santala, Teuvo J.

    1978-01-01

    A composite metal of aluminum and nickel is used to form an economical solar absorption surface for a collector plate wherein an intermetallic compound of the aluminum and nickel provides a surface morphology with high absorptance and relatively low infrared emittance along with good durability.