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Sample records for analytical atomic spectrometry

  1. Prospects in Analytical Atomic Spectrometry

    CERN Document Server

    Bolshakov, A A; Nemets, V M

    2006-01-01

    Tendencies in five main branches of atomic spectrometry (absorption, emission, mass, fluorescence and ionization spectrometry) are considered. The first three techniques are the most widespread and universal, with the best sensitivity attributed to atomic mass spectrometry. In the direct elemental analysis of solid samples, the leading roles are now conquered by laser-induced breakdown and laser ablation mass spectrometry, and the related techniques with transfer of the laser ablation products into inductively-coupled plasma. Advances in design of diode lasers and optical parametric oscillators promote developments in fluorescence and ionization spectrometry and also in absorption techniques where uses of optical cavities for increased effective absorption pathlength are expected to expand. Prospects for analytical instrumentation are seen in higher productivity, portability, miniaturization, incorporation of advanced software, automated sample preparation and transition to the multifunctional modular archite...

  2. A Thermo-Chemical Reactor for analytical atomic spectrometry

    International Nuclear Information System (INIS)

    A novel atomization/vaporization system for analytical atomic spectrometry is developed. It consists of two electrically and thermally separated parts that can be heated separately. Unlike conventional electrothermal atomizers in which atomization occurs immediately above the vaporization site and at the same instant of time, the proposed system allows analyte atomization via an intermediate stage of fractional condensation as a two stage process: Vaporization → Condensation → Atomization. The condensation step is selective since vaporized matrix constituents are mainly non-condensable gases and leave the system by diffusion while analyte species are trapped on the cold surface of a condenser. This kind of sample distillation keeps all the advantages of traditional electrothermal atomization and allows significant reduction of matrix interferences. Integration into one design a vaporizer, condenser and atomizer gives much more flexibility for in situ sample treatment and thus the system is called a Thermo-Chemical Reactor (TCR). Details of the design, temperature measurements, vaporization-condensation-atomization mechanisms of various elements in variety of matrices are investigated in the TCR with spectral, temporal and spatial resolution. The ability of the TCR to significantly reduce interferences and to conduct sample pyrolysis at much higher temperatures as compared to conventional electrothermal atomizers is demonstrated. The analytical potential of the system is shown when atomic absorption determination of Cd and Pb in citrus leaves and milk powder without the use of any chemical modification

  3. A Thermo-Chemical Reactor for analytical atomic spectrometry

    Science.gov (United States)

    Gilmutdinov, A. Kh.; Nagulin, K. Yu.

    2009-01-01

    A novel atomization/vaporization system for analytical atomic spectrometry is developed. It consists of two electrically and thermally separated parts that can be heated separately. Unlike conventional electrothermal atomizers in which atomization occurs immediately above the vaporization site and at the same instant of time, the proposed system allows analyte atomization via an intermediate stage of fractional condensation as a two stage process: Vaporization → Condensation → Atomization. The condensation step is selective since vaporized matrix constituents are mainly non-condensable gases and leave the system by diffusion while analyte species are trapped on the cold surface of a condenser. This kind of sample distillation keeps all the advantages of traditional electrothermal atomization and allows significant reduction of matrix interferences. Integration into one design a vaporizer, condenser and atomizer gives much more flexibility for in situ sample treatment and thus the system is called a Thermo-Chemical Reactor (TCR). Details of the design, temperature measurements, vaporization-condensation-atomization mechanisms of various elements in variety of matrices are investigated in the TCR with spectral, temporal and spatial resolution. The ability of the TCR to significantly reduce interferences and to conduct sample pyrolysis at much higher temperatures as compared to conventional electrothermal atomizers is demonstrated. The analytical potential of the system is shown when atomic absorption determination of Cd and Pb in citrus leaves and milk powder without the use of any chemical modification.

  4. Theory of analytical curves in atomic fluorescence flame spectrometry

    NARCIS (Netherlands)

    Hooymayers, H.P.

    1968-01-01

    An explicit expression for the intensity of atomic resonance fluorescence as a function of atomic concentration in a flame is derived under certain idealized conditions. The expression is generally valid for a pure Doppler absorption line profile as well as for a combined Doppler and collisional bro

  5. Analytical control of wollastonite for biomedical applications by use of atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    De Aza, P N; Guitián, F; De Aza, S; Valle, F J

    1998-04-01

    Preliminary in vitro experiments revealed that wollastonite (CaSiO3) is a potentially highly bioactive material that forms a hyroxyapatite (HA) surface layer on exposure to simulated body fluid with an ion concentration, pH and temperature virtually identical with those of human blood plasma. The formation of the HA layer is an essential requirement for an artificial material to be used as bioactive bone substitute. This finding opens up a wide field for biomedical applications of wollastonite. Biomaterials used as implants in the human body require strict control of trace elements and of the toxic species specified in American Society for Testing and Materials F-1185-88 (As, Cd, Hg and Pb) in ceramic hydroxyapatite for surgical implantation. In this work, two types of pseudowollastonite, the high temperature form of wollastonite, were analysed by using cold vapour atomic absorption spectrometry and hydride generation atomic absorption spectrometry, in order to determine the elements stated in the above-mentioned norm, and inductively coupled plasma atomic emission spectrometry to establish the SiO2/CaO ratio of the two materials and analyse for all other impurities introduced by the raw materials and by the processes of synthesis, sintering and grinding. Barium and Mg were especially prominent in raw materials, and Zr, Y, Mg, W, Co and Ni come mainly from the processing. PMID:9684401

  6. Expressing self-absorption in the analytical function of inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Kántor, Tibor; Bartha, András

    2015-11-01

    The self-absorption of spectral lines was studied with up to date multi-element inductively coupled plasma atomic emission spectrometry (ICP-AES) instrumentation using radial and axial viewing of the plasma, as well, performing line peak height and line peak area measurements. Two resonance atomic and ionic lines of Cd and Mg were studied, the concentration range was extended up to 2000 mg/L. At the varying analyte concentration, constant matrix concentration of 10,000 mg/L Ca was ensured in the pneumatically nebulized solutions. The physical and the phenomenological formulation of the emission analytical function is overviewed and as the continuity of the earlier results the following equation is offered:

  7. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.

    1992-01-01

    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  8. Atomic spectrometry update : environmental analysis

    OpenAIRE

    Butler, Owen T.; Cairns, Warren R. L.; Cook, Jennifer M.; Davidson, Christine M.

    2012-01-01

    This is the 27th annual review published in Journal of Analytical Atomic Spectrometry of the application of atomic spectrometry to the chemical analysis of environmental samples. This Update refers to papers published approximately between September 2010 and August 2011 and continues the series of Atomic Spectrometry Updates (ASUs) in Environmental Analysis1 that should be read in conjunction with other related ASU reviews in the series, namely: clinical and biological materials, foods and be...

  9. Towards broadening thermospray flame furnace atomic absorption spectrometry: Influence of organic solvents on the analytical signal of magnesium

    OpenAIRE

    Ezequiel Morzan; Jorge Stripeikis; Mabel Tudino

    2015-01-01

    This study demonstrates the influence of the solvent when thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is employed for the determination of elements of low volatility, taking magnesium (Mg) as leading case. Several organic solvents/water solutions of different characteristics (density, surface tension, viscosity, etc.) and proportions were employed for the TS-FF-AAS analytical determination. To this end, solutions containing methanol, ethanol and isopropanol in water w...

  10. Three-dimensional time-dependent computer modeling of the electrothermal atomizers for analytical spectrometry

    Science.gov (United States)

    Tsivilskiy, I. V.; Nagulin, K. Yu.; Gilmutdinov, A. Kh.

    2016-02-01

    A full three-dimensional nonstationary numerical model of graphite electrothermal atomizers of various types is developed. The model is based on solution of a heat equation within solid walls of the atomizer with a radiative heat transfer and numerical solution of a full set of Navier-Stokes equations with an energy equation for a gas. Governing equations for the behavior of a discrete phase, i.e., atomic particles suspended in a gas (including gas-phase processes of evaporation and condensation), are derived from the formal equations molecular kinetics by numerical solution of the Hertz-Langmuir equation. The following atomizers test the model: a Varian standard heated electrothermal vaporizer (ETV), a Perkin Elmer standard THGA transversely heated graphite tube with integrated platform (THGA), and the original double-stage tube-helix atomizer (DSTHA). The experimental verification of computer calculations is carried out by a method of shadow spectral visualization of the spatial distributions of atomic and molecular vapors in an analytical space of an atomizer.

  11. Analytical mass spectrometry. Abstracts

    Energy Technology Data Exchange (ETDEWEB)

    1990-12-31

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  12. Analytical mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    1990-01-01

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  13. 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 ostatní: 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

  14. 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...

  15. Trends of investigations on atomic analytical emission spectrometry (AES) in Lithuania

    Science.gov (United States)

    Salkauskas, Julius

    2003-11-01

    The main trends, results and methods of the investigations in AES are reviewed. The majority of the papers were devoted to the regularities and processes in electric discharges applied as spectra excitation sources. For this task the methods of plasma diagnostics, computer simulation, Fourier analysis of the noises, fluctuation as well as the correlation methods were developed and applied in AES. Lately much attention was paid to the metrological problems in spectrochemistry and analytical chemistry. At present the methods of inductively coupled plasma mass spectroscopy are implemented.

  16. Development of an analytical method for antimony speciation in vegetables by HPLC-hydride generation-atomic fluorescence spectrometry.

    Science.gov (United States)

    Olivares, David; Bravo, Manuel; Feldmann, Jorg; Raab, Andrea; Neaman, Alexander; Quiroz, Waldo

    2012-01-01

    A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 microg/L and 5.0, 5.2, and 4.7%, respectively, for a 100 microL sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts. PMID:22970588

  17. Graphite filter atomizer in atomic absorption spectrometry

    Science.gov (United States)

    Katskov, Dmitri A.

    2007-09-01

    Graphite filter atomizers (GFA) for electrothermal atomic absorption spectrometry (ETAAS) show substantial advantages over commonly employed electrothermal vaporizers and atomizers, tube and platform furnaces, for direct determination of high and medium volatility elements in matrices associated with strong spectral and chemical interferences. Two factors provide lower limits of detection and shorter determination cycles with the GFA: the vaporization area in the GFA is separated from the absorption volume by a porous graphite partition; the sample is distributed over a large surface of a collector in the vaporization area. These factors convert the GFA into an efficient chemical reactor. The research concerning the GFA concept, technique and analytical methodology, carried out mainly in the author's laboratory in Russia and South Africa, is reviewed. Examples of analytical applications of the GFA in AAS for analysis of organic liquids and slurries, bio-samples and food products are given. Future prospects for the GFA are discussed in connection with analyses by fast multi-element AAS.

  18. Atomic spectrometry update : environmental analysis

    OpenAIRE

    Butler, Owen T.; Warren R. L. Cairns; Cook, Jennifer M.; Davidson, Christine M.

    2013-01-01

    This is the 28th annual review published in JAAS on the application of atomic spectrometry to the chemical analysis of environmental samples. This Update refers to papers published approximately between September 2011 and August 2012 and continues the series of Atomic Spectrometry Updates (ASUs) in Environmental Analysis1 that should be read in conjunction with other related ASUs in the series, namely: clinical and biological materials, foods and beverages2; advances in atomic spectrometry an...

  19. Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

    International Nuclear Information System (INIS)

    Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system (ii) mineralization in a closed microwave system (iii) combustion in hydrogen-oxygen flame in the Wickbold's apparatus (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g-1 in procedures i-v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g-1 in procedures i-iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50-110 ng g-1 in crude oil, -1 in gasoline, -1 in atmospheric oil, -1 in heavy vacuum oil and 140-300 ng g-1 in distillation residue

  20. Analytical performance of a low-gas-flow torch optimized for inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Montaser, A.; Huse, G.R.; Wax, R.A.; Chan, S.-K.; Golightly, D.W.; Kane, J.S.; Dorrzapf, A.F., Jr.

    1984-01-01

    An inductively coupled Ar plasma (ICP), generated in a lowflow torch, was investigated by the simplex optimization technique for simultaneous, multielement, atomic emission spectrometry (AES). The variables studied included forward power, observation height, gas flow (outer, intermediate, and nebulizer carrier) and sample uptake rate. When the ICP was operated at 720-W forward power with a total gas flow of 5 L/min, the signal-to-background ratios (S/B) of spectral lines from 20 elements were either comparable or inferior, by a factor ranging from 1.5 to 2, to the results obtained from a conventional Ar ICP. Matrix effect studies on the Ca-PO4 system revealed that the plasma generated in the low-flow torch was as free of vaporizatton-atomizatton interferences as the conventional ICP, but easily ionizable elements produced a greater level of suppression or enhancement effects which could be reduced at higher forward powers. Electron number densities, as determined via the series until line merging technique, were tower ht the plasma sustained in the low-flow torch as compared with the conventional ICP. ?? 1984 American Chemical Society.

  1. Noise-immune cavity-enhanced analytical atomic spectrometry — NICE-AAS — A technique for detection of elements down to zeptogram amounts

    International Nuclear Information System (INIS)

    Noise-immune cavity-enhanced optical heterodyne molecular spectroscopy (NICE-OHMS) is a powerful technique for detection of molecular compounds in gas phase that is based on a combination of two important concepts: frequency modulation spectroscopy (FMS) for reduction of noise, and cavity enhancement, for prolongation of the interaction length between the light and the sample. Due to its unique properties, it has demonstrated unparalleled detection sensitivity when it comes to detection of molecular constituents in the gas phase. However, despite these, it has so far not been used for detection of atoms, i.e. for elemental analysis. The present work presents an assessment of the expected performance of Doppler-broadened (Db) NICE-OHMS for analytical atomic spectrometry, then referred to as noise-immune cavity-enhanced analytical atomic spectrometry (NICE-AAS). After a description of the basic principles of Db-NICE-OHMS, the modulation and detection conditions for optimum performance are identified. Based on a previous demonstrated detection sensitivity of Db-NICE-OHMS of 5 × 10−12 cm−1 Hz−1∕2 (corresponding to a single-pass absorbance of 7 × 10−11 over 10 s), the expected limits of detection (LODs) of Hg and Na by NICE-AAS are estimated. Hg is assumed to be detected in gas phase directly while Na is considered to be atomized in a graphite furnace (GF) prior to detection. It is shown that in the absence of spectral interferences, contaminated sample compartments, and optical saturation, it should be feasible to detect Hg down to 10 zg/cm3 (10 fg/m3 or 10−5 ng/m3), which corresponds to 25 atoms/cm3, and Na down to 0.5 zg (zg = zeptogram = 10−21 g), representing 50 zg/mL (parts-per-sextillion, pps, 1:1021) in liquid solution (assuming a sample of 10 μL) or solely 15 atoms injected into the GF, respectively. These LODs are several orders of magnitude lower (better) than any previous laser-based absorption technique previously demonstrated under

  2. A novel analytical system involving hydride generation and gold-coated W-coil trapping atomic absorption spectrometry for selenium determination at ng l-1 level

    International Nuclear Information System (INIS)

    A novel analytical technique was developed where gaseous hydrogen selenide formed by sodium tetrahydroborate reduction is transported to and trapped on a resistively heated gold-coated W-coil atom trap for in situ preconcentration. Gold coating on W-coil was prepared by using an organic solution of Au. The atom trap is held at 165 oC during the collection stage and is heated up to 675 deg. C for revolatilization; analyte species formed are transported to an externally heated quartz T-tube where the atomization takes place and the transient signal is obtained. The carrier gas consisted of 112.5 ml min-1 Ar with 75 ml min-1 H2 during the collection step and 112.5 ml min-1 Ar with 450 ml min-1 H2 in the revolatilization step. The half width of the transient signal obtained is less than 0.5 s. The RSD for the measurements was found to be 3.9% (n = 11) for 0.10 μg l-1 Se using peak height measurements. The calibration plot for 27.0 ml of sample collected in 4.0 min using a flow rate of 6.75 ml min-1 was linear between 0.13 and 2.0 μg l-1 of Se. The limit of detection (3 s) is 39 ng l-1. The enhancement factor for the characteristic concentration (Co) was found to be 20.1 when compared to conventional hydride generation atomic absorption spectrometry system without trap. In order to check the accuracy of the method, standard reference material, natural water NIST 1640 was employed; the result was found to be in good agreement with the certified value at the 95% confidence level

  3. Automatic gamma spectrometry analytical apparatus

    International Nuclear Information System (INIS)

    This invention falls within the area of quantitative or semi-quantitative analysis by gamma spectrometry and particularly refers to a device for bringing the samples into the counting position. The purpose of this invention is precisely to provide an automatic apparatus specifically adapted to the analysis of hard gamma radiations. To this effect, the invention relates to a gamma spectrometry analytical device comprising a lead containment, a detector of which the sensitive part is located inside the containment and additionally comprising a transfer system for bringing the analyzed samples in succession to a counting position inside the containment above the detector. A feed compartment enables the samples to be brought in turn one by one on to the transfer system through a duct connecting the compartment to the transfer system. Sequential systems for the coordinated forward feed of the samples in the compartment and the transfer system complete this device

  4. Heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel and its application to a flow analytical system using flame atomic absorption spectrometry.

    Science.gov (United States)

    Mori, Masanobu; Suzuki, Toshinobu; Sugita, Tsuyoshi; Nagai, Daisuke; Hirayama, Kazuo; Onozato, Makoto; Itabashi, Hideyuki

    2014-08-20

    This study aimed to evaluate the heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel (CaAD) and incorporate this biosorbent into a flow analytical system for heavy metal ions using flame atomic absorption spectrometry (FAAS). The biosorbent was synthesized by electrostatically coating calcium alginate onto diethylenetriamine (dien)-silica gel. Copper ion adsorption tests by a batch method showed that CaAD exhibited a higher adsorption rate compared with other biosorbents despite its low maximum adsorption capacity. Next, CaAD was packed into a 1mL microcolumn, which was connected to a flow analytical system equipped with an FAAS instrument. The flow system quantitatively adsorbed heavy metals and enriched their concentrations. This quantitative adsorption was achieved for pH 3-4 solutions containing 1.0×10(-6) M of heavy metal ions at a flow rate of 5.0 mL min(-1). Furthermore, the metal ions were successfully desorbed from CaAD at low nitric acid concentrations (0.05-0.15 M) than from the polyaminecarboxylic acid chelating resin (Chelex 100). Therefore, CaAD may be considered as a biosorbent that quickly adsorbs and easily desorbs analyte metal ions. In addition, the flow system enhanced the concentrations of heavy metals such as Cu(2+), Zn(2+), and Pb(2+) by 50-fold. This new enrichment system successfully performed the separation and determination of Cu(2+) (5.0×10(-8)M) and Zn(2+) (5.7×10(-8) M) in a river water sample and Pb(2+) (3.8×10(-9) M) in a ground water sample. PMID:25086892

  5. Heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel and its application to a flow analytical system using flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Highlights: • Calcium-alginate-modified dien-silica gel adsorbed multivalent metal ions. • Metal ions adsorbed on CaAD were eluted using low acidic concentrations. • Flow system with CaAD-packed column enriched metal concentrations up to 50-fold. - Abstract: This study aimed to evaluate the heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel (CaAD) and incorporate this biosorbent into a flow analytical system for heavy metal ions using flame atomic absorption spectrometry (FAAS). The biosorbent was synthesized by electrostatically coating calcium alginate onto diethylenetriamine (dien)-silica gel. Copper ion adsorption tests by a batch method showed that CaAD exhibited a higher adsorption rate compared with other biosorbents despite its low maximum adsorption capacity. Next, CaAD was packed into a 1 mL microcolumn, which was connected to a flow analytical system equipped with an FAAS instrument. The flow system quantitatively adsorbed heavy metals and enriched their concentrations. This quantitative adsorption was achieved for pH 3–4 solutions containing 1.0 × 10−6 M of heavy metal ions at a flow rate of 5.0 mL min−1. Furthermore, the metal ions were successfully desorbed from CaAD at low nitric acid concentrations (0.05–0.15 M) than from the polyaminecarboxylic acid chelating resin (Chelex 100). Therefore, CaAD may be considered as a biosorbent that quickly adsorbs and easily desorbs analyte metal ions. In addition, the flow system enhanced the concentrations of heavy metals such as Cu2+, Zn2+, and Pb2+ by 50-fold. This new enrichment system successfully performed the separation and determination of Cu2+ (5.0 × 10−8 M) and Zn2+ (5.7 × 10−8 M) in a river water sample and Pb2+ (3.8 × 10−9 M) in a ground water sample

  6. Zeeman atomic absorption spectrometry

    International Nuclear Information System (INIS)

    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

  7. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry. Progress report, January 1, 1990--December 31, 1992

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.

    1992-09-01

    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  8. The chemical speciation and analysis of trace elements in sediment with Neutron Activation Analytical method(NAA) and atomic mass spectrometry

    International Nuclear Information System (INIS)

    In this research, first of all, the analytical methods for the determination of major elements in sediment have been developed with ICP-MS (Inductively Coupled Plasma Mass Spectrometry). The analytical results of major elements (Al, Ca, K, Fe, Mg) with Cool ICP-MS were much better than those with normal ICP-MS. The analytical results were compared with those of NAA (Neutron Activation Analysis). NAA were a little superior to ICP-MS for the determination of major elements in sediment as a non-destructive trace analytical trace analytical method. The analytical methods for the determination of minor elements (Cr, Ce, U, Co, Pb, As, Se) have been also developed with ICP-MS. The analytical results by standard calibration curve with ICP-MS were not accurate due to the matrix interferences. Thus, the internal standard method was applied, then the analytical results for minor elements with ICP-MS were greatly improved. The analytical results obtained by ICP-MS were compared with those obtained by NAA. It showed that the two analytical methods have great capabilities for the determination of minor elements in sediments. Accordingly, the NAA will plan an important role in analysis of environment sample with complex matrix. ICP-MS also will play an important role because it has a great capability for the determination of Pb that could not be determined by NAA

  9. Ultratrace determination of lead by hydride generation in-atomizer trapping atomic absorption spectrometry: Optimization of plumbane generation and analyte preconcentration in a quartz trap-and-atomizer device

    Czech Academy of Sciences Publication Activity Database

    Kratzer, Jan

    71-72, MAY-JUN (2012), s. 40-47. ISSN 0584-8547 R&D Projects: GA ČR(CZ) GPP206/11/P002 Institutional support: RVO:68081715 Keywords : hydride generation AAS * lead determination * trap-and-atomizer device Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.141, year: 2012

  10. Development of an analytical method for the determination of arsenic in gasoline samples by hydride generation–graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The purpose of the present work was to optimize the conditions for the determination of arsenic in gasoline with hydride generation–graphite furnace atomic absorption spectrometry after acid digestion using a full two-level factorial design with center point. The arsine was generated in a batch system and collected in a graphite tube coated with 150 μg Ir as a permanent modifier. The sample volume, the pre-reduction conditions, the temperature program and modifier mass were kept fixed for all experiments. The estimated main effects were: reducing agent concentration (negative effect), acid concentration (negative effect) and trapping temperature (positive effect). It was observed that there were interactions between the variables. Moreover, the curvature was significant, indicating that the best conditions were at the center point. The optimized parameters for arsine generation were 2.7 mol L−1 hydrochloric acid and 1.6% (w/v) sodium tetrahydroborate. The optimized conditions to collect arsine in the graphite furnace were a trapping temperature of 250 °C and a collection time of 30 s. The limit of detection was 6.4 ng L−1 and the characteristic mass was 24 pg. Two different systems for acid digestion were used: a digester block with cold finger and a microwave oven. The concentration of arsenic found with the proposed method was compared with that obtained using a detergentless microemulsion and direct graphite furnace determination. The results showed that the factorial design is a simple tool that allowed establishing the appropriate conditions for sample preparation and also helped in evaluating the interaction between the factors investigated. - Highlights: ► We determined As in gasoline using hydride generation–graphite furnace AAS. ► We compared three sample preparation procedures. ► A multivariate approach was used to optimize the conditions. ► Analytical performance was best for semi-open digestion.

  11. Development of an analytical method for the determination of arsenic in gasoline samples by hydride generation-graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Becker, Emilene M. [Universidade Federal do Pampa, Bage, RS (Brazil); Universidade Federal de Pelotas, Pelotas, RS (Brazil); Dessuy, Morgana B.; Boschetti, Wiliam [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Ferreira, Sergio L.C. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil)

    2012-05-15

    The purpose of the present work was to optimize the conditions for the determination of arsenic in gasoline with hydride generation-graphite furnace atomic absorption spectrometry after acid digestion using a full two-level factorial design with center point. The arsine was generated in a batch system and collected in a graphite tube coated with 150 {mu}g Ir as a permanent modifier. The sample volume, the pre-reduction conditions, the temperature program and modifier mass were kept fixed for all experiments. The estimated main effects were: reducing agent concentration (negative effect), acid concentration (negative effect) and trapping temperature (positive effect). It was observed that there were interactions between the variables. Moreover, the curvature was significant, indicating that the best conditions were at the center point. The optimized parameters for arsine generation were 2.7 mol L{sup -1} hydrochloric acid and 1.6% (w/v) sodium tetrahydroborate. The optimized conditions to collect arsine in the graphite furnace were a trapping temperature of 250 Degree-Sign C and a collection time of 30 s. The limit of detection was 6.4 ng L{sup -1} and the characteristic mass was 24 pg. Two different systems for acid digestion were used: a digester block with cold finger and a microwave oven. The concentration of arsenic found with the proposed method was compared with that obtained using a detergentless microemulsion and direct graphite furnace determination. The results showed that the factorial design is a simple tool that allowed establishing the appropriate conditions for sample preparation and also helped in evaluating the interaction between the factors investigated. - Highlights: Black-Right-Pointing-Pointer We determined As in gasoline using hydride generation-graphite furnace AAS. Black-Right-Pointing-Pointer We compared three sample preparation procedures. Black-Right-Pointing-Pointer A multivariate approach was used to optimize the conditions. Black

  12. Atomic spectrometry update : environmental analysis

    OpenAIRE

    Butler, Owen T.; Cook, Jennifer; Davidson, Christine M.; Harrington, Chris F.; Miles, Douglas

    2009-01-01

    This is the twenty-forth annual review published in JAAS of the application of atomic spectrometry to the chemical analysis of environmental samples. This Update refers to papers published approximately between September 2007 and August 2008. In the analysis of air, work is focused on the need to collect and characterise ultrafines, i.e. particles below 100 nm in size, and such research is being facilitated through the development of air sampler technologies for subsequent off-line analysis o...

  13. Atomic spectrometry update : environmental analysis

    OpenAIRE

    Butler, O.T.; Cook, Jennifer; Harrington, C.F.; Hill, S. J.; Rieuwerts, J.; Miles, Douglas

    2007-01-01

    This is the twenty-second annual review published in JAAS of the application of atomic spectrometry to the chemical analysis of environmental samples. In the analysis of air, there is ongoing use of XRF techniques for the measurement of particles collected on filters. There is continuing interest in the determination of trace levels of mercury species in the atmosphere. Isotope ratio measurement protocols are attracting wider interest as a potential tool for source apport...

  14. Atomic spectrometry update : environmental analysis

    OpenAIRE

    Butler, Owen T.; Cairns, Warren; Cook, Jennifer M.; Davidson, Christine M.

    2010-01-01

    This is the twenty-fifth annual review published in JAAS on the application of atomic spectrometry to the chemical analysis of environmental samples. This Update refers to papers published approximately between September 2008 and August 2009. In the analysis of air, work has focused on: the need to collect and characterise ultrafines; determination of elements such as Be, Hg and PGEs in air samples; application of SRXRF techniques and advances in the development of field deployable aerosol ma...

  15. Analytical aspects of hydrogen exchange mass spectrometry

    Science.gov (United States)

    Engen, John R.; Wales, Thomas E.

    2016-01-01

    The analytical aspects of measuring hydrogen exchange by mass spectrometry are reviewed. The nature of analytical selectivity in hydrogen exchange is described followed by review of the analytical tools required to accomplish fragmentation, separation, and the mass spectrometry measurements under restrictive exchange quench conditions. In contrast to analytical quantitation that relies on measurements of peak intensity or area, quantitation in hydrogen exchange mass spectrometry depends on measuring a mass change with respect to an undeuterated or deuterated control, resulting in a value between zero and the maximum amount of deuterium that could be incorporated. Reliable quantitation is a function of experimental fidelity and to achieve high measurement reproducibility, a large number of experimental variables must be controlled during sample preparation and analysis. The method also reports on important qualitative aspects of the sample, including conformational heterogeneity and population dynamics. PMID:26048552

  16. Economical Alternatives for High Sensitivity in Atomic Spectrometry Laboratory

    Directory of Open Access Journals (Sweden)

    O. Yavuz Ataman

    2007-12-01

    Full Text Available The most commonly used analytical tools for determination of elements at trace levels are atomic absorption spectrometry (AAS, inductively coupled plasma, optical emission and mass spectrometry (ICP-OES and ICP-MS and atomic fluorescence spectrometry (AFS. Although sensitive plasma techniques are becoming predominant in most of the western laboratories, AAS keeps its importance in developing countries. Simple and inexpensive ways of enhancing sensitivity will be described for laboratories equipped with only a flame AA spectrometer. Although there are many chemical preconcentration procedures to improve sensitivity of flame AAS, only some atom trapping techniques will be included here. One kind of atom trapping device is a slotted quartz tube (SQT used for in situ preconcentration of analyte species followed by a rapid revolatilization cycle to obtain an enhanced signal. These devices provide limits of detection at a level of µg L-1. Another kind of atom trapping involves use of vapor generation technique and quartz or tungsten atom trapping surfaces. The analytical steps consist of the generation of volatile species, usually by hydride formation using NaBH4, trapping these species at the surface of an atom trap held at an optimized temperature and finally re-volatilizing analyte species by rapid heating of trap. These species are transported using a carrier gas to an externally heated quartz tube as commonly used in hydride generation AAS systems; a transient signal is formed and measured. These traps have limits of detection in the order of ng L-1.

  17. Recent developments in generation of volatile species and in their atomization for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Dědina, Jiří; Arslan, Y.; Mester, Z.; Sturgeon, R. E.; Kratzer, Jan; Matoušek, Tomáš; Musil, Stanislav; Svoboda, Milan

    2014. s. 221-221. [Rio Symposium on Atomic Spectrometry /13./. 19.10.2014-24.10.2014, Merida, Yucatan] R&D Projects: GA AV ČR(CZ) M200311202; GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : Arsenic * speciation analysis * sapphire tube atomizer Subject RIV: CB - Analytical Chemistry, Separation

  18. Fish and chips: Analytical applications of resonance ionization mass spectrometry

    International Nuclear Information System (INIS)

    Resonance ionization mass spectrometry is becoming recognized as an analytical technique for a wide range of applications. The extremely high element specificity and sensitivity of the resonance ionization (RI) process is especially valuable for ultratrace element analysis in samples where the complexity of the matrix is frequently a serious source of interferences. In this paper, we will describe the implementation of sputter-initiated resonance ionization microprobe (SIRIMP) and laser atomization RIMP (LARIMP) to solve a number of analytical problems and illustrate the technique's salient characteristics with applications ranging from environmental monitoring using fish scales to semiconductor device and DNA diagnostics chips

  19. Quantification of steroid conjugates using fast atom bombardment mass spectrometry

    International Nuclear Information System (INIS)

    Fast atom bombardment/mass spectrometry or liquid secondary ion mass spectrometry provides the capability for direct analysis of steroid conjugates (sulfates, glucuronides) without prior hydrolysis or derivatization. During the analysis of biologic extracts, limitations on the sensitivity of detection arise from the presence of co-extracted material which may suppress or obscure the analyte signal. A procedure is described for the quantitative determination of dehydroepiandrosterone sulfate in serum which achieved selective isolation of the analyte using immunoadsorption extraction and highly specific detection using tandem mass spectrometry. A stable isotope-labeled analog [( 2H2]dehydroepiandrosterone sulfate) was used as internal standard. Fast atom bombardment of dehydroepiandrosterone sulfate yielded abundant [M-H]- ions that fragmented following collisional activation to give HSO4-; m/z 97. During fast atom bombardment/tandem mass spectrometry of serum extracts, a scan of precursor ions fragmenting to give m/z 97 detected dehydroepiandrosterone sulfate and the [2H2]-labeled analog with a selectivity markedly superior to that observed using conventional mass spectrometry detection. Satisfactory agreement was observed between quantitative data obtained in this way and data obtained by gas chromatography/mass spectrometry of the heptafluorobutyrates of dehydroepiandrosterone sulfate and [2H2]dehydroepiandrosterone sulfate obtained by direct derivatization. 21 refs

  20. 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...

  1. Single atom electrochemical and atomic analytics

    Science.gov (United States)

    Vasudevan, Rama

    In the past decade, advances in electron and scanning-probe based microscopies have led to a wealth of imaging and spectroscopic data with atomic resolution, yielding substantial insight into local physics and chemistry in a diverse range of systems such as oxide catalysts, multiferroics, manganites, and 2D materials. However, typical analysis of atomically resolved images is limited, despite the fact that image intensities and distortions of the atoms from their idealized positions contain unique information on the physical and chemical properties inherent to the system. Here, we present approaches to data mine atomically resolved images in oxides, specifically in the hole-doped manganite La5/8Ca3/8MnO3, on epitaxial films studied by in-situ scanning tunnelling microscopy (STM). Through application of bias to the STM tip, atomic-scale electrochemistry is demonstrated on the manganite surface. STM images are then further analyzed through a suite of algorithms including 2D autocorrelations, sliding window Fourier transforms, and others, and can be combined with basic thermodynamic modelling to reveal relevant physical and chemical descriptors including segregation energies, existence and strength of atomic-scale diffusion barriers, surface energies and sub-surface chemical species identification. These approaches promise to provide tremendous insights from atomically resolved functional imaging, can provide relevant thermodynamic parameters, and auger well for use with first-principles calculations to yield quantitative atomic-level chemical identification and structure-property relations. This research was sponsored by the Division of Materials Sciences and Engineering, BES, DOE. Research was conducted at the Center for Nanophase Materials Sciences, which also provided support and is a DOE Office of Science User Facility.

  2. An effective analytical system based on a pulsed direct current microplasma source for ultra-trace mercury determination using gold amalgamation cold vapor atomic emission spectrometry

    International Nuclear Information System (INIS)

    A novel analysis system based on a low power atmospheric pressure pulsed direct current (Pdc) microplasma is described for the determination of ultra-trace mercury in natural water by cold vapor generation atomic emission spectrometry (CV-AES). The plasma was generated with a miniaturized home-built high-voltage Pdc power supply which decreased the volume and weight of the whole experiment setup. The CV-Pdc-AES system is based on the preconcentration of mercury vapor on a gold filament trapping micro-column prior to detection that provides fast, reproducible absorption and desorption of mercury. The micro-column is produced by winding 30 μm diameter 100 m long gold filament to a small ball and then insert it into a quartz tube of 6 mm i.d, 8 mm o.d. Under the optimized experimental conditions, the new system provides high sensitivity (detection limit: 0.08 pg mL−1) and good reproducibility (RSD 3.0%, [Hg] = 20 pg mL−1, n = 11). The calibration curve is linear at levels near the detection limit up to at least 200 pg mL−1 and the accuracy is on the order of 1–4%. The proposed method was applied to 5 real water samples for mercury ultra-trace analysis. The advantages and features of the newly developed system include high sensitivity, simple structure, low cost, and compact volume with field portable potential. - Highlights: • A novel system based on a low power pulsed dc microplasma for mercury detection. • A small home-built pulsed dc power supply was used to ignite the microplasma. • A gold filament preconcentrator followed by thermal desorption was used. • A detection limit of 0.08 pg mL−1 was achieved for sensitive mercury detection. • The system is compact, low power, and has potential for field portable application

  3. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS)

    International Nuclear Information System (INIS)

    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-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 10μg.L-1. The obtained results fall into a range

  4. 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 ostatní: 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: 3.176, year: 2014

  5. An analytical method for hydrogeochemical surveys: Inductively coupled plasma-atomic emission spectrometry after using enrichment coprecipitation with cobalt and ammonium pyrrolidine dithiocarbamate

    Science.gov (United States)

    Hopkins, D.M.

    1991-01-01

    Trace metals that are commonly associated with mineralization were concentrated and separated from natural water by coprecipitation with ammonium pyrollidine dithiocarbamate (APDC) and cobalt and determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The method is useful in hydrogeochemical surveys because it permits preconcentration near the sample sites, and selected metals are preserved shortly after the samples are collected. The procedure is relatively simple: (1) a liter of water is filtered; (2) the pH is adjusted; (3) Co chloride and APDC are added to coprecipitate the trace metals; and (4) later, the precipitate is filtered, dissolved, and diluted to 10 ml for a 100-fold concentration enrichment of the separated metals. Sb(III), As(III), Cd, Cr, Cu, Fe, Pb, Mo, Ni, Ag, V, and Zn can then be determined simultaneously by ICP-AES. In an experiment designed to measure the coprecipitation efficiency, Sb(III), Cd and Ag were recovered at 70 to 75% of their original concentration. The remaining metals were recovered at 85 to 100% of their original concentrations, however. The range for the lower limits of determination for the metals after preconcentration is 0.1 to 3.0 ??g/l. The precision of the method was evaluated by replicate analyses of a Colorado creek water and two simulated water samples. The accuracy of the method was estimated using a water reference standard (SRM 1643a) certified by the U.S. National Bureau of Standards. In addition, the method was evaluated by analyzing groundwater samples collected near a porphyry copper deposit in Arizona and by analyzing meltwater from glacier-covered areas favorable for mineralization in south-central Alaska. The results for the ICP-AES analyses compared favorably with those obtained using the sequential technique of GFAAS on the acidified but unconcentrated water samples. ICP-AES analysis of trace-metal preconcentrates for hydrogeochemical surveys is more efficient than GFAAS because a

  6. New cryogenic trap design for speciation analysis of arsenic by hydride generation-atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Kratzer, Jan; Dědina, Jiří

    Praha, 2014. s. 240-240. ISBN 978-80-905704-1-2. [European Symposium on Atomic Spectrometry ESAS 2014 & Czech-Slovak Spectroscopic Conference /15./. 16.03.2014-21.03.2014, Praha] R&D Projects: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : atomic absorption spectrometry * hydride generation * cryogenic trapping Subject RIV: CB - Analytical Chemistry, Separation

  7. Slurry sampling hydride generation-cryotrapping-atomic absorption spectrometry for arsenic speciation analysis in baby food

    Czech Academy of Sciences Publication Activity Database

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

    Hungarian Chemical Society, 2016 - (Mihucz, V.). s. 165 ISBN 978-963-9970-65-6. [European Symposium on Atomic Spectrometry /ESAS 2016/ & Hungarian Spectrochemical Conference /59./. 31.03.2016-02.04.2016, Eger] Institutional support: RVO:68081715 Keywords : arsenic speciation * atomic spectrometry * hydride generation Subject RIV: CB - Analytical Chemistry, Separation

  8. 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 ostatní: 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: 3.176, year: 2014

  9. Study on Atomic Fluorescence Spectrometry Excited by Synchrotron Radiation

    Institute of Scientific and Technical Information of China (English)

    Jia-jia Guo; Wu-er Gan; Guo-bin Zhang; Qing-de Su

    2008-01-01

    A novel analysis approach using atomic fluorescence excited by synchrotron radiation is presented. A system for synchrotron radiation-atomic fluorescence spectrometry is developed, and experimental conditions such as flow rate, analyte acidity, concentration of pre-reducing and hydrogenation system are optimized. The proposed method is successfully applied to get an excitation spectrum of arsenic. Seven of ten primary spectral lines, four of which have never been reported by means of atomic fluorescence spectrometry, agree well with the existing reports. The other three are proposed for the first time. Excitation potentials and possible transitions are investigated. Especially for the prominent line at 234.99 nm, the mechanism of generation is discussed and a model of energy transition processes is proposed.

  10. Using simple instrumentation to solve complex analytical problems: advanced AAS atomizers for volatile compounds and analyte trapping techniques

    Czech Academy of Sciences Publication Activity Database

    Dědina, Jiří; de Moraes, D. P.; Dessuy, M. B.; Kratzer, Jan; Řezáčová, Olga; Svoboda, Milan; Matoušek, Tomáš; de Moraes Flores, E. M.; Vale, M. G. R.

    2010. s. 59. [Rio Symposium on Atomic Spectrometry /11./. 24.10.2010-29.10.2010, Mar del Plata] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : AAS * volatile compounds * analyte trapping techniques Subject RIV: CB - Analytical Chemistry, Separation http://www.11thriosymposium.com.ar/index.htm

  11. Principle and analytical applications of resonance ionization mass spectrometry

    International Nuclear Information System (INIS)

    Resonance ionization mass spectrometry (RIMS) is a very sensitive analytical technique for the detection of trace elements. This method is based on the excitation and ionization of atoms with resonant laser light followed by mass analysis. It allows element and, in some cases, isotope selective ionization and is applicable to most of the elements of the periodic table. A high selectivity can be achieved by applying three step photoionization of the elements under investigation and an additional mass separation for an unambiguous isotope assignment. An effective facility for resonance ionization mass spectrometry consists of three dye lasers which are pumped by two copper vapor lasers and of a linear time-of-flight spectrometer with a resolution better than 2500. Each copper vapor laser has a pulse repetition rate of 6,5 kHz and an average output power of 30 W. With such an apparatus measurements with lanthanide-, actinide-, and technetium-samples have been performed. By saturating the excitation steps and by using autoionizing states for ionization step a detection efficiency of 4 x 10-6 and 2,5 x 10-6 has been reached for plutonium and technetium, respectively, leading to a detection limit of less than 107 atoms in the sample. Measurements of isotope ratios of plutonium samples were in good agreement with mass-spectrometric data. The high elemental selectivity of the resonance ionization spectrometry could be demonstrated. (Authors)

  12. CANAS '01 - Colloquium analytical atomic spectroscopy; CANAS '01 - Colloquium Analytische Atomspektroskopie. Programm. Kurzfassungen der Vortraege und Poster

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2001-07-01

    The main topics of the meeting on analytical atom spectroscopy were: optical atom spectrometry, x-ray fluorescence analysis, absorption spectroscopy, icp mass spectroscopy, trace analysis, sampling, sample preparation and quality assurance.

  13. Comparison of electrothermal atomization diode laser Zeeman- and wavelength-modulated atomic absorption and coherent forward scattering spectrometry

    International Nuclear Information System (INIS)

    Atomic absorption and coherent forward scattering spectrometry by using a near-infrared diode laser with and without Zeeman and wavelength modulation were carried out with graphite furnace electrothermal atomization. Analytical curves and limits of detection were compared. The magnetic field was modulated with 50 Hz, and the wavelength of the diode laser with 10 kHz. Coherent forward scattering was measured with crossed and slightly uncrossed polarizers. The results show that the detection limits of atomic absorption spectrometry are roughly the same as those of coherent forward scattering spectrometry with crossed polarizers. According to the theory with bright flicker noise limited laser sources the detection limits and linear ranges obtained with coherent forward scattering spectrometry with slightly uncrossed polarizers are significantly better than those obtained with crossed polarizers and with atomic absorption spectrometry. This is due to the fact that employing approaches of polarization spectroscopy reduce laser intensity fluctuations to their signal carried fractions

  14. The Rewards of Fundamental Atomic Spectrometry Research

    Institute of Scientific and Technical Information of China (English)

    Walter Slavin

    2000-01-01

    Atomic spectrometry research is the life-blood of the atomic spectrometry instrument industry.The instrument designer can be expected to innovate in the execution of instrumentation and should be expected to be the expert in optical,electronic and software engineering.Fundamentally new technology has required too long a period of gestation to be compatible with commercial time scales and budgets.But in the past decade,the pressure from stockholders for increased return on investments has put increasingly strong pressure on management to reduce expenses and focus increasingly on projects that guarantee a fast payback.This pressure falls particularly heavily on the larger companies;the same companies that a decade or more ago were the ones that brought the more far-reaching and expensive new concepts to market. Fundamental research in atomic spectrometry has been accomplished in the past several decades mostly in the academic environment and in research institutions that are Federally funded.All of the Federally funded research institutions have been forced to alter their missions to more tangible and immediate goals,and many have also seen severe financial reductions.

  15. Determination of cadmium in aluminium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A direct method for the determination of cadmium in elemental aluminium is described. Metal samples are dissolved in diluted hydrochloric acid and cadmium is determined by atomic absorption spectrometry in an air-acetylene flame. Interference by non-specific absorption observed at the analytical wavelength incorrected for by means of a non-absorbing line emitted by the hollow-cathode lamp. Relatively large amounts of arsenic do not interfere. The minimun determinable concentration of cadmium for this procedure is 2-3 ppm, expressed on aluminium basis. (author)

  16. Flame-in-gas-shield and miniature diffusion flame hydride atomizers for atomic fluorescence spectrometry: optimization and comparison

    International Nuclear Information System (INIS)

    A detailed optimization of relevant experimental parameters of two hydride atomizers for atomic fluorescence spectrometry: flame-in-gas-shield atomizer with a two-channel shielding unit and a standard atomizer for atomic fluorescence spectrometry, miniature diffusion flame, was performed. Arsine, generated by the reaction with NaBH4 in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were compared. Under optimum conditions sensitivity obtained with flame-in-gas-shield atomizer was approximately twice higher than with miniature diffusion flame. The additional advantage of flame-in-gas-shield atomizer is significantly lower flame emission resulting in a better signal to noise ratio. The resulting arsenic limits of detection for miniature diffusion flame and flame-in-gas-shield atomizer were 3.8 ng l−1 and 1.0 ng l−1, respectively. - Highlights: • We optimized and compared two hydride atomizers for atomic fluorescence spectrometry. • Miniature diffusion flame and flame-in-gas-shield atomizer were optimized. • The limit of detection for arsenic was 1.0 ng l−1

  17. Flame-in-gas-shield and miniature diffusion flame hydride atomizers for atomic fluorescence spectrometry: optimization and comparison

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2015-01-01

    Roč. 109, JUL (2015), s. 16-23. ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant ostatní: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : hydride generation * arsenic * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.176, year: 2014

  18. Excimer laser-ablated plasma atomic spectrometry

    International Nuclear Information System (INIS)

    The characterization and evaluation of a new kind of excimer laser-ablated plasma and applications for direct spectrochemical analysis were investigated through time- and space-resolved spectroscopy. The shape, size, emission spectra, and excitation temperatures of the plasma are largely department on the atmospheric surroundings, the ambient gas composition, the pressure, and laser energy. Spatial discrimination may be desirable to increase the line-to-background (L/B) ratio in atomic emission spectroscopy. A direct spectrochemical analytical method for solid samples with good linearity was developed using the excimer laser-AES. The sensitivity of the analytical signal varied depending on the chemical matrix of the solid samples. A typical detection limit for potassium in a glass matrix was 0.13 μg/g.

  19. Preconcentration and Atomization of Arsane in a Dielectric Barrier Discharge with Detection by Atomic Absorption Spectrometry.

    Science.gov (United States)

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-06-01

    Atomization of arsane in a 17 W planar quartz dielectric barrier discharge (DBD) atomizer was optimized, and its performance was compared to that of a multiple microflame quartz tube atomizer (MMQTA) for atomic absorption spectrometry (AAS). Argon, at a flow rate of 60 mL min(-1), was the best DBD discharge gas. Free As atoms were also observed in the DBD with nitrogen, hydrogen, and helium discharge gases but not in air. A dryer tube filled with NaOH beads placed downstream from the gas-liquid separator to prevent residual aerosol and moisture transport to the atomizer was found to improve the response by 25%. Analytical figures of merit were comparable, reaching an identical sensitivity of 0.48 s ng (-1) As in both atomizers and limits of detection (LOD) of 0.15 ng mL(-1) As in MMQTA and 0.16 ng mL(-1) As in DBD, respectively. Compared to MMQTA, DBD provided 1 order of magnitude better resistance to interference from other hydride-forming elements (Sb, Se, and Bi). Atomization efficiency in DBD was estimated to be 100% of that reached in the MMQTA. A simple procedure of lossless in situ preconcentration of arsane was developed. Addition of 7 mL min(-1) O2 to the Ar plasma discharge resulted in a quantitative retention of arsane in the optical arm of the DBD atomizer. Complete analyte release and atomization was reached as soon as oxygen was switched off. Preconcentration efficiency of 100% was observed, allowing a decrease of the LOD to 0.01 ng mL(-1) As employing a 300 s preconcentration period. PMID:27159266

  20. Arsenic speciation analysis by hydride generation – cryotrapping – atomic fluorescence spectrometry with flame-in-gas-shield atomizer

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Musil, Stanislav; Matoušek, Tomáš; Rychlovský, P.; Dědina, Jiří

    Prague: Charles University in Prague, Faculty of Science, 2010 - (Nesměrák, K.), s. 19-22. (1). ISBN 978-80-7444-005-2. [International Students Conference "Modern Analytical Chemistry" /6./. Praha (CZ), 23.09.2010-24.09.2010] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation * cryogenic trapping * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  1. Characterization and mutual comparison of new electrolytic cell designs for hydride generation-atomic absorption spectrometry with a quartz tube atomizer using Se as a model analyte and Se-75 as a radioactive indicator

    Czech Academy of Sciences Publication Activity Database

    Hraníček, J.; Červený, V.; Kratzer, Jan; Vobecký, Miloslav; Rychlovský, P.

    2012-01-01

    Roč. 27, č. 10 (2012), s. 1761-1771. ISSN 0267-9477 R&D Projects: GA ČR GA203/09/1783 Institutional support: RVO:68081715 Keywords : electrochemical hydride generation AAS * selenium hydride * radiotracer study Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.155, year: 2012

  2. Vapor generation and atom traps: Atomic absorption spectrometry at the ng/L level

    International Nuclear Information System (INIS)

    Atom-trapping atomic absorption spectrometry is a technique that allows detection at the ng/L level for several analytes such as As, Se, Sb, Pb, Bi, Cd, In, Tl, Te, Sn and Hg. The principle involves generation of volatile species, usually hydrides, trapping these species on the surface of an atom trap held at an optimized temperature and, finally, revolatilizing the analyte species by rapid heating of the trap and transporting them in a carrier gas to a heated quartz tube, as commonly used with hydride generation AAS systems. A transient signal having, in most cases, a full width at half maximum of less than 1 s is obtained. The atom trap may be a quartz surface or a W-coil; the former is heated externally and the latter is heated resistively. Both collection and revolatilization temperatures are optimized. In some cases, the W-coil itself is used as an electrothermal atomizer and a heated quartz tube is then not needed. The evolution of these traps starts with the well-known Watling's slotted quartz tube (SQT), continues with atom trapping SQT and finally reaches the present traps mentioned above. The analytical figures of merit for these traps need to be standardized. Naturally, enhancement is on characteristic concentration, C0, where the change in characteristic mass, m0, can be related to trapping efficiency. Novel terms are suggested for E, enhancement factor; such as Emax, maximum enhancement factor; Et, enhancement for 1.0 minute sampling and Ev, enhancement for 1.0 mL of sample. These figures will allow easy comparison of results from different laboratories as well as different analytes and/or traps

  3. Vapor generation and atom traps: Atomic absorption spectrometry at the ng/L level

    Energy Technology Data Exchange (ETDEWEB)

    Ataman, O. Yavuz [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey)], E-mail: ataman@metu.edu.tr

    2008-08-15

    Atom-trapping atomic absorption spectrometry is a technique that allows detection at the ng/L level for several analytes such as As, Se, Sb, Pb, Bi, Cd, In, Tl, Te, Sn and Hg. The principle involves generation of volatile species, usually hydrides, trapping these species on the surface of an atom trap held at an optimized temperature and, finally, revolatilizing the analyte species by rapid heating of the trap and transporting them in a carrier gas to a heated quartz tube, as commonly used with hydride generation AAS systems. A transient signal having, in most cases, a full width at half maximum of less than 1 s is obtained. The atom trap may be a quartz surface or a W-coil; the former is heated externally and the latter is heated resistively. Both collection and revolatilization temperatures are optimized. In some cases, the W-coil itself is used as an electrothermal atomizer and a heated quartz tube is then not needed. The evolution of these traps starts with the well-known Watling's slotted quartz tube (SQT), continues with atom trapping SQT and finally reaches the present traps mentioned above. The analytical figures of merit for these traps need to be standardized. Naturally, enhancement is on characteristic concentration, C{sub 0}, where the change in characteristic mass, m{sub 0}, can be related to trapping efficiency. Novel terms are suggested for E, enhancement factor; such as E{sub max}, maximum enhancement factor; E{sub t}, enhancement for 1.0 minute sampling and E{sub v}, enhancement for 1.0 mL of sample. These figures will allow easy comparison of results from different laboratories as well as different analytes and/or traps.

  4. Vapor generation and atom traps: Atomic absorption spectrometry at the ng/L level

    Science.gov (United States)

    Ataman, O. Yavuz

    2008-08-01

    Atom-trapping atomic absorption spectrometry is a technique that allows detection at the ng/L level for several analytes such as As, Se, Sb, Pb, Bi, Cd, In, Tl, Te, Sn and Hg. The principle involves generation of volatile species, usually hydrides, trapping these species on the surface of an atom trap held at an optimized temperature and, finally, revolatilizing the analyte species by rapid heating of the trap and transporting them in a carrier gas to a heated quartz tube, as commonly used with hydride generation AAS systems. A transient signal having, in most cases, a full width at half maximum of less than 1 s is obtained. The atom trap may be a quartz surface or a W-coil; the former is heated externally and the latter is heated resistively. Both collection and revolatilization temperatures are optimized. In some cases, the W-coil itself is used as an electrothermal atomizer and a heated quartz tube is then not needed. The evolution of these traps starts with the well-known Watling's slotted quartz tube (SQT), continues with atom trapping SQT and finally reaches the present traps mentioned above. The analytical figures of merit for these traps need to be standardized. Naturally, enhancement is on characteristic concentration, C0, where the change in characteristic mass, m0, can be related to trapping efficiency. Novel terms are suggested for E, enhancement factor; such as Emax, maximum enhancement factor; Et, enhancement for 1.0 minute sampling and Ev, enhancement for 1.0 mL of sample. These figures will allow easy comparison of results from different laboratories as well as different analytes and/or traps.

  5. Atomization of volatile compounds for atomic absorption and atomic fluorescence spectrometry: On the way towards the ideal atomizer

    International Nuclear Information System (INIS)

    This review summarizes and discusses the individual atomizers of volatile compounds. A set of criteria important for analytical praxis is used to rank all the currently existing approaches to the atomization based on on-line atomization for atomic absorption (AAS) and atomic fluorescence spectrometry (AFS) as well as on in-atomizer trapping for AAS. Regarding on-line atomization for AAS, conventional quartz tubes are currently the most commonly used devices. They provide high sensitivity and low baseline noise. Running and investment costs are low. The most serious disadvantage is the poor resistance against atomization interferences and often unsatisfactory linearity of calibration graphs. Miniature diffusion flame (MDF) is extremely resistant to interferences, simple, cheap and user-friendly. Its essential disadvantage is low sensitivity. A novel device, known as a multiatomizer, was designed to overcome disadvantages of previous atomizers. It matches performance of conventional quartz tubes in terms of sensitivity and baseline noise as well as in running and investment costs. The multiatomizer, however, provides much better (i) resistance against atomization interferences and (ii) linearity of calibration graphs. In-atomizer trapping enhances the sensitivity of the determination and eliminates the effect of the generation kinetics and of surges in gas flow on the signal shape. This is beneficial for the accuracy of the determination. It could also be an effective tool for reducing some interferences in the liquid phase. In-situ trapping in graphite furnaces (GF) is presently by far the most popular approach to the in-atomizer trapping. Its resistance against interferences is reasonably good and it can be easily automated. In-situ trapping in GF is a mature method well established in various application fields. These are the reasons to rank in-situ trapping in GF as currently the most convenient approach to hydride atomization for AAS. The recently suggested

  6. Method of trivalent chromium concentration determination by atomic spectrometry

    Science.gov (United States)

    Reheulishvili, Aleksandre N.; Tsibakhashvili, Neli Ya.

    2006-12-12

    A method is disclosed for determining the concentration of trivalent chromium Cr(III) in a sample. The addition of perchloric acid has been found to increase the atomic chromium spectrometric signal due to Cr(III), while leaving the signal due to hexavalent chromium Cr(VI) unchanged. This enables determination of the Cr(III) concentration without pre-concentration or pre-separation from chromium of other valences. The Cr(III) concentration may be measured using atomic absorption spectrometry, atomic emission spectrometry or atomic fluorescence spectrometry.

  7. Miniaturized analytical systems for mass spectrometry-based protein studies

    OpenAIRE

    Abonnenc, Mélanie

    2009-01-01

    Current proteomic strategies depend strongly on the development of analytical methodologies and instrumentation. In parallel to the development of mass spectrometry (MS) - based proteomic workflows, microfluidic devices emerged in this field as a flexible tool for rapid and sensitive protein studies. In this context, the present work focuses on the development of miniaturized analytical systems for protein studies, especially by electrospray ionization mass spectrometric detection. Several ap...

  8. Determination of trace impurities in titanium dioxide by direct solid sampling electrothermal atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vojtková, Blanka; Dočekal, Bohumil

    2005-01-01

    Roč. 99, S (2005), s489-s491. ISSN 0009-2770. [Meeting on Chemistry and Life /3./. Brno, 20.09.2005-22.09.2005] Institutional research plan: CEZ:AV0Z40310501 Keywords : solid sampling * electrothermal atomic absorption spectrometry * trace analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.445, year: 2005

  9. Arsenic speciation analysis by HPLC postcolumn hydride generation and detection by atomic fluorescence spectrometry

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Rychlovský, P.; Dědina, Jiří

    Prague: Charles University in Prague, Faculty of Science, 2014 - (Nesměrák, K.), s. 74-77 ISBN 978-80-7444-030-4. [International Students Conference "Modern Analytical Chemistry" /10./. Prague (CZ), 22.09.2014-23.09.2014] R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation http://www.natur.cuni.cz/isc-mac/

  10. Determination of gold by chemical hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. The chemical vapour generation (CVG) of transition and noble metals opens a novel route for introduction of these elements into atomic spectrometric sources. It can be accomplished by merging an acidic sample with tetrahydroborate reductant solution (Y. L. Feng et al., J. of Anal. At. Spectrom., 20 (2005) 255-265). There have been some studies for determination of Au; however, only mg L-1 levels of gold have been determined by CVG - Atomic Absorption Spectrometry (AAS) (G. Ertas et al., Applied Spectroscopy, 60 (2006) 423-429). Volatile Au species were generated in flow injection arrangement from acid environment in presence of surfactants. The core of the system is a mixing manifold based on 3 concentric capillaries (T. Matousek et al., J. of Anal. At. Spectrom., 18 (2003) 487-494) protruding into the glass gas-liquid separator (glass, volume 3 ml). Optimum flow rate of Ar as a carrier gas was found at 240 mL/min. The study of generation parameters as well as the use of reaction modifiers-surfactants and dithiocarbamate- will be presented. Quartz tube multiatomizer for AAS was employed for atomization. Atomization conditions including composition of carrier gases and their flow rates and atomization temperature were optimized. 900 deg C was found as the optimum atomization temperature; over 900 deg C, peak area of Au signal decreased; in addition, peak shape was altered. A sharp maximum of 6 mL/min oxygen as the outer gas was observed. Another important point was that hydrogen-rich atmosphere caused signal depression. Analytical performance of this approach to generation and atomization will be discussed and perspectives of its future will be outlined. This work was supported by the GA ASCR (grant No. A400310507 and IAA400310704) and Institute of Analytical Chemistry of the ASCR, v.v.i. (project no. AV0Z40310501). This work also was supported from OYP (Faculty Development Program) from the Middle East Technical University

  11. Analytical evaluation of atomic form factors: application to Rayleigh scattering

    CERN Document Server

    Safari, L; Amaro, P; Jänkälä, K; Fratini, F

    2014-01-01

    Atomic form factors are widely used for the characterization of targets and specimens, from crystallography to biology. By using recent mathematical results, here we derive an analytical expression for the atomic form factor within the independent particle model constructed from nonrelativistic screened hydrogenic wavefunctions. The range of validity of this analytical expression is checked by comparing the analytically obtained form factors with the ones obtained within the Hartee-Fock method. As an example, we apply our analytical expression for the atomic form factor to evaluate the differential cross section for Rayleigh scattering off neutral atoms.

  12. Analytical evaluation of atomic form factors: Application to Rayleigh scattering

    Energy Technology Data Exchange (ETDEWEB)

    Safari, L., E-mail: laleh.safari@ist.ac.at [IST Austria (Institute of Science and Technology Austria), Am Campus 1, 3400 Klosterneuburg (Austria); Department of Physics, University of Oulu, Box 3000, FI-90014 Oulu (Finland); Santos, J. P. [Laboratório de Instrumentação, Engenharia Biomédica e Física da Radiação (LIBPhys-UNL), Departamento de Física, Faculdade de Ciências e Tecnologia, FCT, Universidade Nova de Lisboa, 2829-516 Caparica (Portugal); Amaro, P. [Laboratório de Instrumentação, Engenharia Biomédica e Física da Radiação (LIBPhys-UNL), Departamento de Física, Faculdade de Ciências e Tecnologia, FCT, Universidade Nova de Lisboa, 2829-516 Caparica (Portugal); Physikalisches Institut, Universität Heidelberg, D-69120 Heidelberg (Germany); Jänkälä, K. [Department of Physics, University of Oulu, Box 3000, FI-90014 Oulu (Finland); Fratini, F. [Department of Physics, University of Oulu, Box 3000, FI-90014 Oulu (Finland); Institute of Atomic and Subatomic Physics, TU Wien, Stadionallee 2, 1020 Wien (Austria); Departamento de Física, Instituto de Ciências Exatas, Universidade Federal de Minas Gerais, 31270-901 Belo Horizonte, MG (Brazil)

    2015-05-15

    Atomic form factors are widely used for the characterization of targets and specimens, from crystallography to biology. By using recent mathematical results, here we derive an analytical expression for the atomic form factor within the independent particle model constructed from nonrelativistic screened hydrogenic wave functions. The range of validity of this analytical expression is checked by comparing the analytically obtained form factors with the ones obtained within the Hartee-Fock method. As an example, we apply our analytical expression for the atomic form factor to evaluate the differential cross section for Rayleigh scattering off neutral atoms.

  13. High sensitivity detection of selenium by laser excited atomic fluorescence spectrometry using electrothermal atomization

    International Nuclear Information System (INIS)

    The high sensitivity detection of the trace element selenium is reported. The analytical method applied is Laser Excited Atomic Fluorescence Spectrometry using Electrothermal Atomization within a graphite furnace atomizer. For the production of tunable laser radiation in the VUV spectral region a laser system was developed which consists of two dye lasers pumped by a Nd:YAG laser. The laser radiations are subsequently frequency doubled and sum frequency mixed by nonlinear optical KDP or BBO crystals, respectively. The system works with a repetition rate of 20 Hz and provides output energies of up to 100 μJ in the VUV at a pulse duration of 5 ns. The analytical investigations were focused on the detection of selenium in aqueous solutions and samples of human whole blood. From measurements on aqueous standards detection limits of 1.5 ng/l for selenium were obtained, with corresponding absolute detected masses of only 15 fg. The linear dynamic range spanned six orders of magnitude and good precision was achieved. In case of human whole blood samples the recovery was found to be within the range of 96% to 104%. The determination of the selenium content yielded medians of [119.5 ± 17.3] μg/l for 200 frozen blood samples taken in 1988 and [109.1 ± 15.6] μg/l for 103 fresh blood samples. (author)

  14. Analytical relativistic self-consistent-field calculations for atoms

    International Nuclear Information System (INIS)

    A new second-order representation of the Dirac equation is presented. This representation which is exact for a hydrogen atom is applied to approximate analytical self-consistent-field calculations for atoms. Results are given for the rare-gas atoms from helium to radon and for lead. The results compare favorably with numerical Dirac-Hartree-Fock solutions

  15. Evaluation of electrochemical generation of volatile zinc hydride by heated quartz tube atomizer atomic absorption spectrometry.

    Science.gov (United States)

    Arbab-Zavar, Mohammad-Hossein; Chamsaz, Mahmoud; Youssefi, Abbas; Aliakbari, Mostafa

    2012-01-01

    Electrochemical hydride generation (EcHG) as a sample introduction system for determination of zinc was developed. It was directly coupled to an electrically heated quartz tube atomizer (QTA) atomic absorption spectrometry (AAS) system. The hydride generator is a laboratory-made semi-batch electrolytic cell that consists of a lead-tin alloy cathode and a platinum anode. The effects of typical parameters on the generation efficiency of the technique, such as types of cathode material and catholyte and anolyte solutions, were studied. The influences of numerical experimental operating parameters on the analytical signal were evaluated in detail and optimum conditions were obtained. The analytical figures of merit for the developed method were determined. The calibration curve was linear up to 300 ng mL(-1) of Zn. A concentration detection limit (3σ, n = 9) of 11 ng mL(-1) Zn and a relative standard deviation of 5.0% (RSD, n = 9) for 200 ng mL(-1) Zn were accessed. In addition, the susceptibility of interference from various ions was evaluated. The accuracy of the method was verified by determination of Zn in a certified reference material and in tap water. The achieved concentrations were found to be in good agreement with both the certified value and the data obtained using flame AAS. PMID:22790376

  16. Atomic spectrometry methods for wine analysis: A critical evaluation and discussion of recent applications

    Energy Technology Data Exchange (ETDEWEB)

    Grindlay, Guillermo, E-mail: guillermo.grindlay@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, PO Box 99, 03080 Alicante (Spain); Mora, Juan; Gras, Luis [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, PO Box 99, 03080 Alicante (Spain); Loos-Vollebregt, Margaretha T.C. de [Delft University of Technology, Faculty of Applied Sciences, Analytical Biotechnology, Julianalaan 67, 2628 BC Delft (Netherlands)

    2011-04-08

    The analysis of wine is of great importance since wine components strongly determine its stability, organoleptic or nutrition characteristics. In addition, wine analysis is also important to prevent fraud and to assess toxicological issues. Among the different analytical techniques described in the literature, atomic spectrometry has been traditionally employed for elemental wine analysis due to its simplicity and good analytical figures of merit. The scope of this review is to summarize the main advantages and drawbacks of various atomic spectrometry techniques for elemental wine analysis. Special attention is paid to interferences (i.e. matrix effects) affecting the analysis as well as the strategies available to mitigate them. Finally, latest studies about wine speciation are briefly discussed.

  17. Atomic spectrometry methods for wine analysis: A critical evaluation and discussion of recent applications

    International Nuclear Information System (INIS)

    The analysis of wine is of great importance since wine components strongly determine its stability, organoleptic or nutrition characteristics. In addition, wine analysis is also important to prevent fraud and to assess toxicological issues. Among the different analytical techniques described in the literature, atomic spectrometry has been traditionally employed for elemental wine analysis due to its simplicity and good analytical figures of merit. The scope of this review is to summarize the main advantages and drawbacks of various atomic spectrometry techniques for elemental wine analysis. Special attention is paid to interferences (i.e. matrix effects) affecting the analysis as well as the strategies available to mitigate them. Finally, latest studies about wine speciation are briefly discussed.

  18. Neutron activation spectrometry and neutron activation analysis in analytical geochemistry

    International Nuclear Information System (INIS)

    The present report is to show the geochemists who are interested in neutron activation spectrometry (NAS) and neutron activation analysis (NAA) which analytical possibilities these methods offer him. As a review of these analytical possibilities, a lieterature compolation is given which is subdivided into two groups: 1) rock (basic, intermediary, acid, sediments, soils and nuds, diverse minerals, tectites, meteorites and lunar material). 2) ore (Al, Au, Be, Cr, Cu, Mn, Mo, Fe, Pb, Pt, Sn, Ti, W, Zn, Zr, U and phosphate ore, polymetallic ores, fluorite, monazite and diverse ores). The applied methods as well as the determinable elements in the given materials can be got from the tables. On the whole, the literature evaluation carried out makes it clear that neutron activation spectrometry is a very useful multi-element method for the analysis of rocks. The analysis of ores, however, is subjected to great limitations. As rock analysis is very frequently of importance in prospecting for ore deposits, the NAS proves to be extremely useful for this very field of application. (orig./LH)

  19. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Determination of low or trace-level amounts of metals by electrothermal atomic absorption spectrometry (ETAAS) often requires the use of suitable preconcentration and/or separation procedures in order to attain the necessary sensitivity and selectivity. Such schemes are advantageously executed in...... compensated by superior performance and versatility. In fact, two approaches are conceivable: The analyte-loaded ion-exchange beads might either be transported directly into the graphite tube where they are pyrolized and the measurand is atomized and quantified; or the loaded beads can be eluted and the...

  20. Glass frit nebulizer for atomic spectrometry

    Science.gov (United States)

    Layman, L.R.

    1982-01-01

    The nebuilizatlon of sample solutions Is a critical step In most flame or plasma atomic spectrometrlc methods. A novel nebulzatlon technique, based on a porous glass frit, has been Investigated. Basic operating parameters and characteristics have been studied to determine how thte new nebulizer may be applied to atomic spectrometrlc methods. The results of preliminary comparisons with pneumatic nebulizers Indicate several notable differences. The frit nebulizer produces a smaller droplet size distribution and has a higher sample transport efficiency. The mean droplet size te approximately 0.1 ??m, and up to 94% of the sample te converted to usable aerosol. The most significant limitations In the performance of the frit nebulizer are the stow sample equMbratton time and the requirement for wash cycles between samples. Loss of solute by surface adsorption and contamination of samples by leaching from the glass were both found to be limitations only In unusual cases. This nebulizer shows great promise where sample volume te limited or where measurements require long nebullzatlon times.

  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. Speciation analysis of arsenic by selective hydride generation- cryotrapping-atomic fluorescence spectrometry with flame-in-gas- shield atomizer: Achieving extremely low detection limits with inexpensive instrumentation

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Currier, J. M.; Stýblo, M.; Dědina, Jiří

    2014-01-01

    Roč. 86, č. 20 (2014), s. 10422-10428. ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S; GA MŠk LH12040 Institutional support: RVO:68081715 Keywords : speciation analysis of arsenic * selective hydride generation * flame-in-gas-shield atomizer * cryotrapping-atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

  3. Arsenic speciation in drugs by selective hydride generation-cryotrapping-gas chromatography-atomic absorption spectrometry with the multiatomizer

    Czech Academy of Sciences Publication Activity Database

    de Moraes, D. P.; Dědina, Jiří; Matoušek, Tomáš; de Moraes Flores, E. M.

    2010. s. 183. [Rio Symposium on Atomic Spectrometry /11./. 24.10.2010-29.10.2010, Mar del Plata] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic * HG-CT-AAS * multiatomizer Subject RIV: CB - Analytical Chemistry, Separation http://www.11thriosymposium.com.ar/index.htm

  4. New cryogenic trap design for speciation analysis of Arsenic by generation of substituted hydrides-atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Kratzer, Jan; Dědina, Jiří

    2014. s. 196-196. [Rio Symposium on Atomic Spectrometry /13./. 19.10.2014-24.10.2014, Merida, Yucatan] R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : cryotrapping * hydride generation * arsenic speciation analysis Subject RIV: CB - Analytical Chemistry, Separation

  5. Analytic Solutions of Three-Level Dressed-Atom Model

    Institute of Scientific and Technical Information of China (English)

    WANG Zheng-Ling; YIN Jian-Ping

    2004-01-01

    On the basis of the dressed-atom model, the general analytic expressions for the eigenenergies, eigenstates and their optical potentials of the A-configuration three-level atom system are derived and analysed. From the calculation of dipole matrix element of different dressed states, we obtain the spontaneous-emission rates in the dressed-atom picture. We find that our general expressions of optical potentials for the three-level dressed atom can be reduced to the same as ones in previous references under the approximation of a small saturation parameter. We also analyse the dependences of the optical potentials of a three-level 85Rb atom on the laser detuning and the dependences of spontaneous-emission rates on the radial position in the dark hollow beam, and discuss the probability (population) evolutions of dressed-atomic eigenstates in three levels in the hollow beam.

  6. Arsenic speciation analysis by cryogenic trapping – hydride generation – atomic absorption spectrometry; Investigation of water vapour dryers

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Taurková, Petra; Matoušek, Tomáš; Rychlovský, P.; Dědina, Jiří

    Prague: Charles University in Prague, Faculty of Science, 2010 - (Nesměrák, K.), s. 15-18. (1). ISBN 978-80-7444-005-2. [International Students Conference "Modern Analytical Chemistry" /6./. Praha (CZ), 23.09.2010-24.09.2010] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation * cryogenic trapping * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  7. COMPARISON OF SECONDARY ION MASS SPECTROMETRY (SIMS) WITH ELECTRON MICROPROBE ANALYSIS (EPMA) AND OTHER THIN FILM ANALYTICAL METHODS

    OpenAIRE

    Werner, H.; Von Rosenstiel, A.

    1984-01-01

    Different modes of SIMS for thin film analysis and the principle of SIMS will be discussed; this will be followed by a discussion of some features related to instrumentation: types of ion sources and their characteristics ; ion microprobe versus ion microscope ; special modes of SIMS : sputter neutral mass spectrometry (SNMS) and fast atom bombardment. (FAB). The discussion of analytical features will include : element range, quantitative analysis, depth profiling, two-dimensional and three-d...

  8. 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.

  9. Evaluation of quartz tubes as atomization cells for gold determination by thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    This work describes the development of a new analytical procedure able to determine gold by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) using nickel tubes (NiT) and quartz tubes (QT) as atomization cells. Experiments involving changes in the flow injection operational parameters, reagent concentrations and sizes of the QT were performed in order to optimize sensitivity. Under the same operational conditions, it was observed that the employment of QT increases the sensitivity of gold determination when compared to the nickel tube. Since solutions of highly concentrated hydrochloric acid showed the best performance as carriers, quartz tubes were also preferred due to its greater tolerance to corrosion by mineral acids in comparison to NiT. In addition, changes in the internal diameter of the QT revealed an important improvement in sensitivity for smaller tubes. Under optimized conditions the main figures of merit showed values close to that of graphite furnace atomic absorption spectrometry with the addition of an excellent improvement of the sample throughput. They are: LOD (3 s): 0.004 μg mL−1, sensitivity: 0.306 (μg mL−1)−1, RSD% (n = 10, 1 μg mL−1): 2.5, linear range: 0.01–4 μg mL−1 and sample throughput: 72 h−1. This new method was employed for the determination of gold in homeopathic medicines with no need of sample digestion. Validation of the analytical results will be shown. A full discussion of the most relevant findings regarding the role of the atomization cell as a strategic key for improving sensitivity will be also provided. - Highlights: ► Quartz tubes as furnaces in TS-FFAAS. ► Small tubes for controlling radial dispersion. ► Improved figures of merit for gold determination. ► Analysis of homeopathic medicines.

  10. Formulating analytic expressions for atomic collision cross sections

    International Nuclear Information System (INIS)

    Methods to formulate analytic expression for atomic collision cross sections as a function of projectile energy are described on the basis of the experiences of the data compilation work for more than 20 years. Topics considered are the choice of appropriate functional forms for the expressions and optimization of adjustable parameters. To make extrapolation possible, functions to be used should have the form with reasonable asymptotic behavior. In this respect, modified Green-McNeal formulas have been found useful for various atomic collision cross sections. For ionization processes, a modified Lotz formula has often given a good fit. The ALESQ code for least-squares fits has been convenient to optimize adjustable parameters in analytic expressions. (author)

  11. Determination of metals in atmospheric particulates using atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Nineteen trace metals in atmospheric samples have been determined by atomic absorption spectrometry, using a graphite furnace for most elements. Paper filters have been used to collect air samples. The sample preparation procedure involves the removal of organic matter and the conversion of the metals to soluble salts by ashing the filters in an oxygen plasma at 125 deg C for 6 h. and by subsequent dissolution in HN03HCl solution. The sensitivities achieved are in the range of 2,5.10-5 and 6,3.10-3 μg/m3, for an air volume of 2000 m3. (author)

  12. 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......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...

  13. Analytical conditions for field ionization mass spectrometry of diesel fuel

    Energy Technology Data Exchange (ETDEWEB)

    Tadao Ogawa [Toyota Central R& amp; D Labs., Inc., Aichi-ken (Japan). Materials Analysis and Evaluation Division

    2005-11-01

    Field ionization mass spectrometry (FIMS) was investigated to establish a method for clarifying the compositions of hydrocarbons in diesel fuels. Firstly, the influences of reservoir temperature, ion source temperature, emitter current, cathode voltage and ion focusing mode on ion intensities and double bond equivalence value (DBE) distributions were examined to define the analytical conditions for obtaining almost the same carbon number distribution of n-paraffins (DBE=0) as that obtained by gas chromatography. Secondly, the origin of the memory background and the measures to minimize it were examined to obtain the ion intensities of high reproducibility. As a result, variation coefficients of less than 6.4 and 5.1% were obtained for the ion intensity of each hydrocarbon and the sums of the ion intensities of the hydrocarbons with the same DBE, respectively. Finally, two fuels, which were similar in H/C but considerably different in the backend fraction at a distillation temperature of 290{sup o}C (R{sub 290}), were analyzed by FIMS established in this study, to explain the reasons why these fuels yielded nearly the same particulate emissions. FIMS results showed that a fuel with low R{sub 290} consisted of low carbon number aliphatic hydrocarbons and high carbon number aromatic hydrocarbons, both of which have low inflammability. The fuel was found to yield more HC emission than another fuel with high R{sub 290}. The amount of the particulate emission was larger than that expected from R{sub 290}. 14 refs., 14 figs., 3 tabs.

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

    International Nuclear Information System (INIS)

    The on-line atomization of gold volatile species was studied and the results were compared with thermodynamic calculations in several quartz atomizers, namely: diffusion flame, flame-in-gas-shield, flame-in-plain-tube, externally heated T-tube and externally heated flame-in-T-tube. Atomization mechanism in the explored devices is proposed, where volatile species are converted to thermodynamically stable AuH at elevated temperature over 500 °C and then atomized by an interaction with a cloud of hydrogen radicals. Because of its inherent simplicity and robustness, diffusion flame was employed as a reference atomizer. It yielded atomization efficiency of 70 to 100% and a very good long time reproducibility of peak area sensitivity: 1.6 to 1.8 s μg−1. Six and eleven times higher sensitivity, respectively, was provided by atomizers with longer light paths in the observation volume, i.e. externally heated T-tube and externally heated flame-in-T-tube. The latter one, offering limit of detection below 0.01 μg ml−1, appeared as the most prospective for on-line atomization. Insight into the mechanism of atomization of gold volatile species, into the fate of free atoms and into subsequent analyte transfer allowed to assess possibilities of in-atomizer preconcentration of gold volatile species: it is unfeasible with quartz atomizers but a sapphire tube atomizer could be useful in this respect. - Highlights: • On-line atomization of gold volatile species for AAS in quartz devices was studied. • Atomization mechanism was proposed and atomization efficiency was estimated. • Possibilities of in-atomizer preconcentration of gold volatile species were assessed

  15. Determination of lead traces in water and liqueurs by derivative atom trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun, H. [Department of Chemistry, Hebei University, Baoding, 071002 (China); Yang Lili [Department of Chemistry, Hebei University, Baoding, 071002 (China); Zhang Deqiang [Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing (China); Wang Weixiao [Department of Chemistry, Hebei University, Baoding, 071002 (China); Sun Jianmin [Department of Chemistry, Hebei University, Baoding, 071002 (China)

    1997-07-01

    A new method for the direct determination of lead traces using derivative atom trapping flame atomic absorption spectrometry (DAT-FAAS) with an improved water-cooled stainless steel trapping equipment in an air-acetylene flame was investigated. The optimum conditions concerning the sensitivity were studied. For a 1 min collection, the characteristic concentration (given as derivative absorbance of 0.0044) and the detection limit (3s) were 1.4 ng/mL and 0.27 ng/mL, respectively. This is 361 and 74-fold better than those of the conventional flame atomic absorption spectrometry (FAAS) and comparable to those of graphite furnace atomic absorption spectrometry (GFAAS). The detection limit and sensitivity of DAT-FAAS for a 3 min collection time were 2 and 3 orders of magnitude higher than those of conventional FAAS. The present method was applied to the determination of lead in water and liqueur samples with a recovery range of 94-108% and a relative standard deviation of 3.5-5.6%. (orig.). With 5 figs., 5 tabs.

  16. 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…

  17. 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.

  18. 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.

  19. Cooperative analysis of alloying elements in zirconium alloys using inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    The Second Sub-Committee on Zircaloy Analysis, under Committee on Analytical Chemistry of Nuclear Fuels and Reactor Materials, JAERI, carried out a cooperative analysis with the nine laboratories on the determination of tin, iron, nickel and chromium in zirconium alloys to evaluate the practical applicability of inductively coupled plasma (ICP) atomic emission spectrometry. This report describes the sample decomposition procedures, determination conditions and procedures, and analytical results. The results obtained for alloying elements in samples for cooperative analysis (JAERI CRMs Z11 to Z14 and others) were compared with certified values or those obtained by X-ray fluorescence method, and were in good agreement with those values. ICP atomic emission spectrometry were shown to be an effective field method for determining alloying elements (C.V. % 2 to 7 for 0.5 to 1.90 % Sn, C.V. % 2 to 3 for 0.093 to 0.130 % Fe, C.V. % 3 to 6 for 0.095 to 0.110 % Ni and C.V. % 2 to 7 for 0.01 to 0.150 % Cr) in zirconium alloys. (author)

  20. In situ atom trapping of Bi on W-coated slotted quartz tube flame atomic absorption spectrometry and interference studies

    International Nuclear Information System (INIS)

    Analytical performances of metal coated slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) and slotted quartz tube in situ atom trapping flame atomic absorption spectrometry (SQT-AT-FAAS) systems were evaluated for determination of Bi. Non-volatile elements such as Mo, Zr, W and Ta were tried as coating materials. It was observed that W-coated SQT gave the best sensitivity for the determination of Bi for SQT-FAAS and SQT-AT-FAAS. The parameters for W-coated SQT-FAAS and W-coated SQT-AT-FAAS were optimized. Sensitivity of FAAS for Bi was improved as 4.0 fold by W-coated SQT-FAAS while 613 fold enhancement in sensitivity was achieved by W-coated SQT-AT-FAAS using 5.0 min trapping with respect to conventional FAAS. MIBK was selected as organic solvent for the re-atomization of Bi from the trapping surface. Limit of detection values for W-coated SQT-FAAS and W-coated SQT-AT-FAAS was obtained as 0.14 μg mL−1 and 0.51 ng mL−1, respectively. Linear calibration plot was obtained in the range of 2.5–25.0 ng mL−1 for W-coated SQT-AT-FAAS. Accuracy of the W-coated SQT-AT-FAAS system was checked by analyzing a standard reference material, NIST 1643e. - Highlights: • Further increasing in sensitivity of SQT-AT-FAAS was obtained by using a W coated SQT. • 613 fold sensitivity enhancement was achieved by W coated SQT-AT-FAAS versus FAAS. • A sensitive, rapid and simple technique for Bi was developed with an LOD of 0.51 ng mL−1. • The technique is suggested for laboratories equipped with only a flame AA spectrometer

  1. The direct determination of HgS by thermal desorption coupled with atomic absorption spectrometry

    Science.gov (United States)

    Coufalík, Pavel; Zvěřina, Ondřej; Komárek, Josef

    2016-04-01

    This research was aimed at the direct determination of HgS in environmental samples by means of thermal desorption coupled with atomic absorption spectrometry. Operating parameters of the apparatus used for thermal desorption (including a prototype desorption unit) are described in this work, as well as the procedure for measuring mercury release curves together with an evaluation of the analytical signal including two methods of peak integration. The results of thermal desorption were compared with HgS contents obtained by sequential extraction. The limits of quantification of the proposed method for the selective determination of the black and red forms of HgS were 4 μg kg- 1 and 5 μg kg- 1, respectively. The limit of quantification of red HgS in soils was 35 μg kg- 1. The developed analytical procedure was applied to soil and sediment samples from historical mining areas.

  2. Organic solvents as interferents in arsenic determination by hydride generation atomic absorption spectrometry with flame atomization

    Science.gov (United States)

    Karadjova, Irina B.; Lampugnani, Leonardo; Dědina, Jiri; D'Ulivo, Alessandro; Onor, Massimo; Tsalev, Dimiter L.

    2006-05-01

    Interference effects of various organic solvents miscible with water on arsenic determination by hydride generation atomic absorption spectrometry have been studied. Arsine was chemically generated in continuous flow hydride generation system and atomized by using a flame atomizer able to operate in two modes: miniature diffusion flame and flame-in-flame. The effects of experimental variables and atomization mode were investigated: tetrahydroborate and hydrochloric acid concentrations, argon, hydrogen and oxygen supply rates for the microflame, and the distance from the atomization region to the observation zone. The nature of the species formed in the flame due to the pyrolysis of organic solvent vapors entering the flame volume together with arsine is discussed. The observed signal depression in the presence of organic solvents has been mainly attributed to the atomization interference due to heterogeneous gas-solid reaction between the free arsenic atoms and finely dispersed carbon particles formed by carbon radicals recombination. The best tolerance to interferences was obtained by using flame-in-flame atomization (5-10 ml min - 1 of oxygen flow rate), together with higher argon and hydrogen supply rates and elevated observation heights.

  3. Analytical strategies in mass spectrometry-based phosphoproteomics

    DEFF Research Database (Denmark)

    Rosenqvist, Heidi; Ye, Juanying; Jensen, Ole N

    2011-01-01

    discuss various tandem mass spectrometry approaches for phosphopeptide sequencing and quantification, and we consider aspects of phosphoproteome data analysis and interpretation. Efficient integration of these stages of phosphoproteome analysis is highly important to ensure a successful outcome of large...

  4. Determination of lithium in coloured alcoholic beverages by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. Lithium was first found in ashes from wine in 1878, and its presence was later confirmed by spectroscopy, but its determination in wine and beverages is not well documented, unlike the extensive research reported on other metals. Several methods can be implemented for determination of lithium, involving the use of atomic spectroscopy techniques. This paper reports on an analytical optimization to determine lithium by atomic absorption spectrometry (AAS). Good results in reproducibility, accuracy and precision were obtained. No significant interference was found. The method was applied for determination of lithium in six rum samples, eight brandy samples, four vermouth samples, eight whisky samples and two bourbon samples. The value of lithium content in samples ranges from 0,33 to 1,48 μg/ml. Recovery experiments were carried out in order to evaluate the accuracy of the method in samples determination. The values obtained ranges from 95,71% to 98%. The precision of the method in that samples determination was evaluated through variation coefficients. The values obtained ranges from 7,2% to 2,5%. The results have been statistically compared with those obtained using the Inductively Coupled Plasma Atomic Emission Spectrometry (ICP/AES) and reaches a 95% level of significance.

  5. Speciation analysis of arsenic by hydride generation-cryotrapping-atomic fluorescence spectrometry: achieving extremely low detection limits with inexpensive instrumentation

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Svoboda, Milan; Selecká, Anna; Rychlovský, P.; Dědina, Jiří

    Buzios, Rio de Janeiro, 2011. TH43. ISBN 978-85-8006-046-1. [Colloquium Spectroscopicum Internationale /37./. 28.08.2011-02.09.2011, Buzios, Rio de Janeiro] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation analysis * hydride generation * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  6. Speciation analysis of arsenic by hydride generation-cryotrapping-atomic fluorescence spectrometry: achieving extremely low detection limits with inexpensive instrumentation

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Svoboda, Milan; Selecká, Anna; Rychlovský, P.; Dědina, Jiří

    Münster, 2011. FTM 17. [International Symposium on Metallomics /3./. 15.06.2011-18.06.2011, Münster] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation analysis * hydride generation * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation http://www.metallomics2011.org/event/Metallomics2011/Scientific_program.html

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

    OpenAIRE

    Teslima Daşbaşı; Şenol Kartal; Şerife Saçmacı; Ahmet Ülgen

    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 ...

  8. Determination of Arsenic in Palm Kernel Expeller using Microwave Digestion and Graphite Furnace Atomic Absorption Spectrometry Method

    OpenAIRE

    Abdul Niefaizal Abdul Hammid; Ainie Kuntom; RazaIi Ismail; Norazilah Pardi

    2013-01-01

    A study on the method to determine arsenic in palm kernel expeller wascarried out. Microwave digestion technique is widely applied in the analytical chemistry field. In comparison to conventional sample digestion method, the microwave technique is simple, reduced contamination, usage of safe reagent and matrix completely digested. A graphite furnace atomic absorption spectrometry method was used for the total determination of arsenic in palm kernel expeller. Arsenic was extracted from palm ke...

  9. A comparative study of inductively coupled plasma optical emission spectrometry and microwave plasma atomic emission spectrometry for the direct determination of lanthanides in water and environmental samples

    International Nuclear Information System (INIS)

    A new instrumental technique – Microwave Plasma Atomic Emission Spectrometry (MP - AES) is compared to conventional Inductively Coupled Plasma Optical Emission Spectrometry (ICP - OES) for direct determination of lanthanides. Estimation of both methods is done using standard measurement conditions. The present study includes spectral and non- spectral matrix effect evaluation. Tested analytical wavelengths of lanthanides are divided into three groups: 1) relatively free, 2) interfered by other lanthanides and 3) interfered by concomitant elements. Non spectral effect on analytes is examined in two typical real matrices – acidic plant digests and saline water. The capabilities of both plasma methods for quantitative determination of La, Ce, Sm, Eu, Gd and Er are compared. The interference - free emission lines are selected; appropriate background correction is proposed and the corresponding instrumental detection limits are calculated. Key words: lanthanides, ICP -OES, MP -AES, spectral and non-spectral interference

  10. Development of an automated sequential injection on-line solvent extraction-back extraction procedure as demonstrated for the determination of cadmium with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium...

  11. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    with an aqueous solution of 6 mmol L-1 of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass...... spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 sigma) achieved by the HPLC-FAAS system was 1 mg L-1 of selenium (100 mu L injections) for each of the four...

  12. Quantitative determination of impurities in nuclear grade aluminum by Flame-Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    The paper deals with quantitative determination of impurity elements in nuclear grade aluminum, used as fin tubes in research reactors, by Flame-Atomic Absorption Spectrometry (F-AAS). The results have been compared with those obtained by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) method. Experimental conditions used in both the methods are given in the paper. (author)

  13. Determination of antimony by using tungsten trap atomic absorption spectrometry

    International Nuclear Information System (INIS)

    An electrically heated tungsten coil was used as a trap in the determination of antimony. The technique consists of three steps. Initially, SbH3 is formed by hydride generation procedure; then the analyte species in vapor form are transported to W-coil trap heated at 370 deg. C. Following the preconcentration step, the trap is heated to 895 deg. C; analyte species are revolatilized and transported to the flame-heated quartz atom cell where atomization and the formation of signal take place. The experimental parameters were optimized both for trap and no-trap studies. The most important experimental parameters are concentrations of HCl and NaBH4 solutions, H2 and Ar gas flow rates, and collection and revolatilization temperatures of W-coil. Accuracy was tested using a certified reference material, waste water EU-L-1. Limit of detection for the system is 16 ng l-1 using a sample of 36 ml collected in 4.0 min. Enhancement factor in sensitivity was 17

  14. Advances in metallomics by atomic and molecular spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. The scope of research in the field of elemental speciation has considerably evolved during the last decade. The analysis of specific metal-containing contaminants reached the maturity and has given way to the development of analytical methods to describe interactions of metals with biomolecules which are constituents of the genome, proteome, metabolome and other -omes in a cell, tissue or organism. The entirety of metal-biomolecule species has been termed the 'metallome' which gave rise to an emerging discipline: metallomics. Advances of trace element analysis in life sciences resulted in the proliferation of new terms related to the description of metal-interactions with biomolecules, such as, e.g. ionome, metalloproteome, metallogenome, metallometabolome, heteroatom-tagged proteome, single element proteomes (e.g., selenoproteome) and the corresponding -omics. The analytical chemistry challenges in the area metallomics include the detection, quantification, identification and characterization of complexes of metals (metalloids) at trace levels in an environment rich in biomolecules often having similar physicochemical properties. In the past, the only way to access to this information was modelling using stability constants. Today, hyphenated techniques based on the coupling of a high resolution separation technique with sensitive elemental (ICP MS) and molecular (ES MS/MS) mass spectrometry offer the possibility of high-throughput acquisition of metallomics information in many biological systems. The lecture discusses advances in analytical techniques in the field of metallomics. Particular attention will be to developments in multidimensional nanoHPLC with the parallel ICP MS and ESI MS detection and the sensitive spotting of heteroelement-containing proteins in 2D gels, accompanied by advances in MALDI TOF MS. Potential for medical research (e.g., characterization for selenoproteins as new biomarkers of clinical utility

  15. Study on the application of cold vapor atomic absorption spectrometry and hydride generation atomic absorption spectrometry for the determination of Hg and As traces in sea water samples

    International Nuclear Information System (INIS)

    The trace amount of total mercury (Hg) and arsenic (As) in sea water samples were quantitatively determined by using the Atomic Absorption Spectrometry connected with the hydride generation technique (HG-AAS) for As, and with the cold vapour technique (CV-AAS) for Hg. The experiments were carried out at room temperature on a Hydride System Module (HS55) combined with an Atomic Absorption Spectrometer (VARIO 6, Analytik Jena AG). The effect of reductants concentration, and that of matrix on the absorption intensity of each analyzed element was studied in details. The sea water sample after fitrating through a membrane with 0.45(μm-hole size was pre-treated with an oxidant or an reductant to obtain the identical medium. The absorption intensity of each element was then measured on the VARIO-6 under the optimum parameters for spectrometer such as: maximum wavelength, current of hollow cathode lamp, and that for hydride system such as cell temperature, speed of peristaltic pump, pump time, reaction time and rewash time, ect. The analytical procedures were set-up and applied for the determination of these above mentioned elements in the synthesized sea water sample and in the real sea water samples with high precision and accuracy. (author)

  16. Atomic force microscopy fishing and mass spectrometry identification of gp120 on immobilized aptamers

    Directory of Open Access Journals (Sweden)

    Ivanov YD

    2014-10-01

    Full Text Available Yuri D Ivanov,1 Natalia S Bukharina,1 Tatyana O Pleshakova,1 Pavel A Frantsuzov,1 Elena Yu Andreeva,1 Anna L Kaysheva,1,2 Victor G Zgoda,1 Alexander A Izotov,1 Tatyana I Pavlova,1 Vadim S Ziborov,1 Sergey P Radko,1 Sergei A Moshkovskii,1 Alexander I Archakov1 1Department of Personalized Medicine, Orekhovich Institute of Biomedical Chemistry of the Russian Academy of Medical Sciences, Moscow, Russia; 2PostgenTech Ltd., Moscow, Russia Abstract: Atomic force microscopy (AFM was applied to carry out direct and label-free detection of gp120 human immunodeficiency virus type 1 envelope glycoprotein as a target protein. This approach was based on the AFM fishing of gp120 from the analyte solution using anti-gp120 aptamers immobilized on the AFM chip to count gp120/aptamer complexes that were formed on the chip surface. The comparison of image contrasts of fished gp120 against the background of immobilized aptamers and anti-gp120 antibodies on the AFM images was conducted. It was shown that an image contrast of the protein/aptamer complexes was two-fold higher than the contrast of the protein/antibody complexes. Mass spectrometry identification provided an additional confirmation of the target protein presence on the AFM chips after biospecific fishing to avoid any artifacts. Keywords: gp120 HIV-1 envelope glycoprotein, aptamer, atomic force microscopy, mass spectrometry

  17. Innovative mass spectrometry-based analytical strategies in proteomics

    OpenAIRE

    Milioli, Marco

    2015-01-01

    This PhD thesis was divided in four main sections. In particular, the first section is composed by fourth chapters showing the main components of a mass spectrometer such as sources, analyzers and detectors followed by a brief introduction of mass spectrometry-based proteomics. In the second chapter, the proteomics analysis of platelet-derived microparticles under different agonist stimulations has been described. In the third chapter, the PTMs analysis of platelet-derived microparticles has ...

  18. Study on the GaAs(110) surface using emitted atom spectrometry

    International Nuclear Information System (INIS)

    The facilities implemented at Bariloche for the ion scattering spectrometry is described, and recent examples of the technique application to determine the atomic structure and the composition of metallic and semiconductor surfaces, pure and with different adsorbates. The surface analysis technique using emitted atom spectrometry is discussed. The sensitivity to the GaAs(110) surface atomic relaxation is presented, and the kinetic of hydrogen adsorption by the mentioned surface is studied

  19. Mass and emission spectrometry in the Analytical Chemistry Division of Oak Ridge National Laboratory

    International Nuclear Information System (INIS)

    The capabilities of the Mass and Emission Spectrometry Section of the Analytical Chemistry Division of Oak Ridge National Laboratory are described. Many different areas of mass spectrometric expertise are represented in the section: gas analysis, high abundance sensitivity measurements, high- and low-resolution organic analyses, spark source trace constituent analysis, and ion microprobe analysis of surfaces. These capabilities are complemented by emission spectrometry. The instruments are described along with a few applications, some of which are unique

  20. Determination of molybdenum in silicates through atomic absorption spectrometry using pre-concentration by active carbon

    International Nuclear Information System (INIS)

    An analytical procedure for molybdenum determination in geological materials through Atomic Absorption Spectrometry, after pre-concentration of the Mo-APDC complex in activated carbon, has been developed, which is needed in order to reduce the dilution effect in the sample decomposition. During the development of this method the influence of pH, the amount of APDC for complexation of Mo and the interference of Fe, Ca, Mn, Al, K, Na, Mg and Ti were tested. It was shown that none of these causes any significant effect on the Mo determination proposed. The results of the analysis at the international geochemical reference samples JB-1 (basalt) and GH (granite) were very accurate and showed that the detection limit in rocks (1,00g) is 0,6 ppm, when using sample dilution of 1 ml and microinjection techniques. (author)

  1. Preconcentration of Vanadium(Ⅴ) on Crosslinked Chitosan and Determination by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol*L-1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0-12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg*L-1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.

  2. Determination of mineral elements in fresh olive fruits by flame atomic spectrometry

    International Nuclear Information System (INIS)

    The mineral element characterisation of olive fruits is acquiring interest to evaluate the link between their nutritional status and the olive oil quality. A method for the analysis of mineral elements in fresh olive fruits is proposed. The presence of mineral elements such as potassium, sodium, calcium, magnesium, zinc, copper, iron, and manganese in olive fruits was quantified by flame atomic absorption spectrometry. The limits of quantification were (expressed in mg kg.1 of dry weight) 1.266, 1.569, 0.272, 0.172, 0.268, 0.316, 1.017 and 0.513 for K, Na, Ca, Mg, Zn, Cu, Fe and Mn, respectively. The results showed the method is a robust, reliable, and simple analytical procedure for the mineral element characterisation of olive fruit. (Author).

  3. Analytical calculations of scattering lengths in atomic physics

    International Nuclear Information System (INIS)

    We describe a method for evaluating analytical long-range contributions to scattering lengths for some potentials used in atomic physics. We assume that an interaction potential between colliding particles consists of two parts. The form of a short-range component, vanishing beyond some distance from the origin (a core radius), need not be given. Instead, we assume that a set of short-range scattering lengths due to that part of the interaction is known. A long-range tail of the potential is chosen to be an inverse power potential, a superposition of two inverse power potentials with suitably chosen exponents or the Lent potential. For these three classes of long-range interactions a radial Schrodinger equation at zero energy may be solved analytically with solutions expressed in terms of the Bessel, Whittaker and Legendre functions, respectively. We utilize this fact and derive exact analytical formulae for the scattering lengths. The expressions depend on the short-range scattering lengths, the core radius and parameters characterizing the long-range part of the interaction. Cases when the long-range potential (or its part) may be treated as a perturbation are also discussed and formulae for scattering lengths linear in strengths of the perturbing potentials are given. It is shown that for some combination of the orbital angular momentum quantum number and an exponent of the leading term of the potential the derived formulae, exact or approximate, take very simple forms and contain only polynomial and trigonometric functions. The expressions obtained in this paper are applicable to scattering of charged particles by neutral targets and to collisions between neutrals. The results are illustrated by accelerating convergence of scattering lengths computed for e--Xe and Cs-Cs systems. (author)

  4. 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...

  5. Determination of various extracted Al species and their fractions by atomic spectrometry techniques

    International Nuclear Information System (INIS)

    Complete text of publication follows. During the last few decades aluminium and its distribution in the environment has attracted much attention because of Al toxic effects to the plants, animals and humans. Its concentration in different environmental samples varies widely. While determination of high Al concentrations can be realized with no serious problem, reliable determination of its trace and ultratrace concentrations requires the development of enrichment techniques capable of improving both, the selectivity and also sensitivity for this analyte. Two extraction methods were used for selective separation and preconcentration of aluminium trace concentrations from model solutions. Solid phase extraction (SPE) using nanometer-sized titanium dioxide as a solid sorbent and cloud point extraction (CPE) using nonionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) were utilized. Spectrometry techniques such as flame (F AAS) and electrothermal (ET AAS) atomic absorption spectrometry, inductively coupled plasma optical emission spectrometry (ICP OES) or inductively coupled plasma mass spectrometry (ICP MS) were applied for the determination of aluminium. Direct TiO2-slurry sampling was used for sample injection into the graphite furnace of ET AAS in SPE. Optimized procedures were used for the determination of trace and ultratrace amounts of total aluminium and various aluminium species and their fractions in speciation analysis and fractionation studies using environmental samples such as natural waters, soils and sediments. The work was supported by Slovak Research and Development Agency under the contracts No. APVT-20-010204, LPP-0038-06, LPP-0146-09 and SK-CZ-0044-07, by Scientific Grant Agency of Ministry of Education of Slovak Republic and the Slovak Academy of Sciences under the contracts No. VEGA 1/4464/07 and VEGA 1/0272/08 and by Ministry of Education, Youth and Sports of Czech Republic under the contract No. MEB 080813.

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

    International Nuclear Information System (INIS)

    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

  7. Fast atom bombardment tandem mass spectrometry of carotenoids

    Energy Technology Data Exchange (ETDEWEB)

    van Breeman, R.B. [Univ. of Illinois, Chicago, IL (United States); Schmitz, H.H.; Schwartz, S.J. [North Carolina State Univ., Raleigh, NC (United States)

    1995-02-01

    Positive ion fast atom bombardment (FAB) tandem mass spectrometry (MS-MS) using a double-focusing mass spectrometer with linked scanning at constant B/E and high-energy collisionally activated dissociation (CAD) was used to differentiate 17 different cartenoids, including {beta}-apo-8{prime}- carotenal, astaxanthin, {alpha}-carotene, {beta}-carotene, {gamma}-carotene, {zeta}-carotene, canthaxanthin, {beta}-cryptoxanthin, isozeaxanthin bis (pelargonate), neoxanthin, neurosporene, nonaprene, lutein, lycopene, phytoene, phytofluene, and zeaxanthin. The carotenoids were either synthetic or isolated from plant tissues. The use of FAB ionization minimized degradation or rearrangement of the carotenoid structures due to the inherent thermal instability generally ascribed to these compounds. Instead of protonated molecules, both polar xanthophylls and nonpolar carotenes formed molecular ions, M{sup {center_dot}+}, during FAB ionization. Following collisionally activated dissociation, fragment ions of selected molecular ion precursors showed structural features indicative of the presence of hydroxyl groups, ring systems, ester groups, and aldehyde groups and the extent of aliphatic polyene conjugation. The fragmentation patterns observed in the mass spectra herein may be used as a reference for the structural determination of carotenoids isolated from plant and animal tissues. 18 refs., 4 figs.

  8. In situ atom trapping of Bi on W-coated slotted quartz tube flame atomic absorption spectrometry and interference studies

    Energy Technology Data Exchange (ETDEWEB)

    Kılınç, Ersin, E-mail: kilincersin@gmail.com [Medical Laboratory Techniques, Vocational Higher School of Healthcare Studies, Mardin Artuklu University, 47200 Mardin (Turkey); Bakırdere, Sezgin [Yıldız Technical University, Art and Science Faculy, Department of Chemistry, Esenler, TR 34220 İstanbul (Turkey); Aydın, Fırat [Dicle University, Faculty of Science, Department of Chemistry, Laboratory of Chemical Analysis, TR 21280 Diyarbakır (Turkey); Ataman, O. Yavuz [Middle East Technical University, Faculty of Arts and Sciences, Department of Chemistry, 06800 Ankara (Turkey)

    2013-11-01

    Analytical performances of metal coated slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) and slotted quartz tube in situ atom trapping flame atomic absorption spectrometry (SQT-AT-FAAS) systems were evaluated for determination of Bi. Non-volatile elements such as Mo, Zr, W and Ta were tried as coating materials. It was observed that W-coated SQT gave the best sensitivity for the determination of Bi for SQT-FAAS and SQT-AT-FAAS. The parameters for W-coated SQT-FAAS and W-coated SQT-AT-FAAS were optimized. Sensitivity of FAAS for Bi was improved as 4.0 fold by W-coated SQT-FAAS while 613 fold enhancement in sensitivity was achieved by W-coated SQT-AT-FAAS using 5.0 min trapping with respect to conventional FAAS. MIBK was selected as organic solvent for the re-atomization of Bi from the trapping surface. Limit of detection values for W-coated SQT-FAAS and W-coated SQT-AT-FAAS was obtained as 0.14 μg mL{sup −1} and 0.51 ng mL{sup −1}, respectively. Linear calibration plot was obtained in the range of 2.5–25.0 ng mL{sup −1} for W-coated SQT-AT-FAAS. Accuracy of the W-coated SQT-AT-FAAS system was checked by analyzing a standard reference material, NIST 1643e. - Highlights: • Further increasing in sensitivity of SQT-AT-FAAS was obtained by using a W coated SQT. • 613 fold sensitivity enhancement was achieved by W coated SQT-AT-FAAS versus FAAS. • A sensitive, rapid and simple technique for Bi was developed with an LOD of 0.51 ng mL{sup −1}. • The technique is suggested for laboratories equipped with only a flame AA spectrometer.

  9. Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry

    Science.gov (United States)

    Chan, George C. Y.; Hieftje, Gary M.

    2010-08-03

    A method for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry (ICP-AES). ICP-AES analysis is performed across a plurality of selected locations in the plasma on an unknown sample, collecting the light intensity at one or more selected wavelengths of one or more sought-for analytes, creating a first dataset. The first dataset is then calibrated with a calibration dataset creating a calibrated first dataset curve. If the calibrated first dataset curve has a variability along the location within the plasma for a selected wavelength, errors are present. Plasma-related errors are then corrected by diluting the unknown sample and performing the same ICP-AES analysis on the diluted unknown sample creating a calibrated second dataset curve (accounting for the dilution) for the one or more sought-for analytes. The cross-over point of the calibrated dataset curves yields the corrected value (free from plasma related errors) for each sought-for analyte.

  10. New analytical tools combining gel electrophoresis and mass spectrometry

    OpenAIRE

    Tobolkina, Elena

    2014-01-01

    Proteomics has been one of the main projects challenging biological and analytical chemists for many years. The separation, identification and quantification of all the proteins expressed within biological systems remain the main objectives of proteomics. Due to sample complexity, the development of fractionation, separation, purification and detection techniques that possess appropriate resolution to separate a large number of proteins, as well as being sensitive and fast enough for high thr...

  11. Mass spectrometry-based hepcidin measurements in serum and urine: analytical aspects and clinical implications.

    OpenAIRE

    Kemna, E.; Tjalsma, H.; Podust, V N; Swinkels, D. W.

    2007-01-01

    BACKGROUND: Discovery of the central role of hepcidin in body iron regulation has shed new light on the pathophysiology of iron disorders. Information is lacking on newer analytical approaches to measure hepcidin in serum and urine. Recent reports on the measurement of urine and serum hepcidin by surface-enhanced laser-desorption/ionization time-of-flight mass spectrometry (SELDI-TOF MS) necessitate analytical and clinical evaluation of MS-based methodologies. METHODS: We used SELDI-TOF MS, i...

  12. On the structural denaturation of biological analytes in trapped ion mobility spectrometry - mass spectrometry.

    Science.gov (United States)

    Liu, Fanny C; Kirk, Samuel R; Bleiholder, Christian

    2016-06-01

    Key to native ion mobility/mass spectrometry is to prevent the structural denaturation of biological molecules in the gas phase. Here, we systematically assess structural changes induced in the protein ubiquitin during a trapped ion mobility spectrometry (TIMS) experiment. Our analysis shows that the extent of structural denaturation induced in ubiquitin ions is largely proportional to the amount of translational kinetic energy an ion gains from the applied electric field between two collisions with buffer gas particles. We then minimize the efficiency of the structural denaturation of ubiquitin ions in the gas phase during a TIMS experiment. The resulting "soft" TIMS spectra of ubiquitin are found largely identical to those observed on "soft" elevated-pressure ion mobility drift tubes and the corresponding calibrated cross sections are consistent with structures reported from NMR experiments for the native and A-state of ubiquitin. Thus, our analysis reveals that TIMS is useful for native ion mobility/mass spectrometry analysis. PMID:26998732

  13. Advances with tungsten coil atomizers: Continuum source atomic absorption and emission spectrometry

    International Nuclear Information System (INIS)

    Two new tungsten coil spectrometers are described: a continuum source tungsten coil atomic absorption spectrometer and a tungsten coil atomic emission spectrometer. Both devices use a 150 W tungsten coil extracted from a slide projector bulb. The power is provided by a computer-controlled, solid state, constant current 0-10 A supply. The heart of the optical system is a high-resolution spectrometer with a multi-channel detector. The continuum source system employs xenon or deuterium lamps, and is capable of multi-element analyses of complex samples like engine oil, urine, and polluted water. Spiked engine oil samples give mean percent recoveries of 98 ± 9, 104 ± 9, and 93 ± 0.8 for Al, V, and Ni, respectively. Copper, Zn, and Cd are determined in urine samples; while Cd, Co, Yb, and Sr are determined in water samples. Detection limits for Cd, Zn, Cu, Yb, Sr, and Co are: 8, 40, 1, 4, 1, and 4 μg l-1. The technique of tungsten coil atomic emission spectrometry using a 150 W commercial projector bulb is reported for the first time. Calcium, Ba, and Sr are determined with detection limits of 0.01, 0.5, and 0.1 μg l-1. Relative standard deviations are lower than 10% in each case, and Sr is determined in two water standard reference materials

  14. 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.

  15. Identification of Synthetic Polymers and Copolymers by Analytical Pyrolysis-Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Kusch, Peter

    2014-01-01

    An experiment for the identification of synthetic polymers and copolymers by analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was developed and performed in the polymer analysis courses for third-year undergraduate students of chemistry with material sciences, and for first-year postgraduate students of polymer sciences. In…

  16. Determination of daily intake of elements from Philippine total diet samples using inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Total diet samples were analyzed for major elements (Na, K, Ca, Mg, P) and some minor trace elements (Fe, Zn, Mn, Al, Sr, Cu, Ba, Yt) using inductively coupled plasma-atomic emission spectrometry (ICP-AES). Samples analyzed were classified into sex and age groups. Results for some elements (Na, K, Mg, Zn, Cu, Mn) were compared with values from Bataan dietary survey calculated using the Philippine composition table. Exceot for Na, analytical results were similar to calculated values. Analytical results for Ca and Fe were also compared with the values from Food and Nutrition Research Institute. In general, values obtained in the study were lower than the FNRI values. Comparison of the analytical and calculated results with the Japanese and ICRP data showed that Philippine values were lower than foreign values. (Auth.). 22 refs., 9 tabs

  17. 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

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

    International Nuclear Information System (INIS)

    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(NO3)2 and (NH4)H2PO4-Mg(NO3)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 μg L-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 -1

  19. Atomic and Nuclear Analytical Methods XRF, Mössbauer, XPS, NAA and Ion-Beam Spectroscopic Techniques

    CERN Document Server

    Verma, H R

    2007-01-01

    This book is a blend of analytical methods based on the phenomenon of atomic and nuclear physics. It comprises comprehensive presentations about X-ray Fluorescence (XRF), Mössbauer Spectroscopy (MS), X-ray Photoelectron Spectroscopy (XPS), Neutron- Activation Analysis (NAA), Particle Induced X-ray Emission Analysis (PIXE), Rutherford Backscattering Analysis (RBS), Elastic Recoil Detection (ERD), Nuclear Reaction Analysis (NRA), Particle Induced Gamma-ray Emission Analysis (PIGE), and Accelerator Mass Spectrometry (AMS). These techniques are commonly applied in the fields of medicine, biology, environmental studies, archaeology or geology et al. and pursued in major international research laboratories.

  20. Methylmercury determination in biological samples using electrothermal atomic absorption spectrometry after acid leaching extraction

    Energy Technology Data Exchange (ETDEWEB)

    Saber-Tehrani, Mohammad; Hashemi-Moghaddam, Hamid; Givianrad, Mohammad Hadi; Abroomand-Azar, Parviz [Islamic Azad University, Department of Chemistry, Science and Research Branch, Tehran (Iran)

    2006-11-15

    An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 {mu}g g{sup -1} and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%. (orig.)

  1. Shape, size, and atomic composition analysis of nanostructures in 3D by Rutherford backscattering spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zolnai, Zsolt, E-mail: zolnai.zsolt@ttk.mta.hu

    2013-09-15

    The emergence of novel micro- and nanofabrication tools lead to the targeted research of highly ordered three-dimensional nanosystems, constructed from regular building blocks like spheres, cylinders, bricks, pyramids, which can be used in a wide range of applications. As a consequence, the exploration of the potential and limits of efficient analytical techniques to characterize structured nanosystems became a significant task. In this work the scope of conventional Rutherford backscattering spectrometry (RBS) analysis is extended to investigate highly ordered periodic nanostructures in three dimensions. Hexagonally arranged spherical and ellipsoidal silica particles, rectangular gold nano-arrays, and embedded structures in Si substrates and silica particles are analyzed. It is shown that the shape of the measured spectra can be correlated with the shape of individual nano-objects through geometrical considerations. The evaluation of the recorded data for different sample tilt angles can be carried out with the Monte-Carlo type 3D simulation model cell concept considering the details of the applied measurement geometry. It is demonstrated that macrobeam 3D-RBS can provide valuable information on the shape, size, spacing, and atomic composition of nanostructured samples as well as on nanoscale atomic transport processes and consequently, it can be utilized as a highly precise, non-destructive characterization tool for nanotechnology.

  2. Air quality status in Kinshasa as determined by instrumental neutron activation analysis, atomic absorption spectrometry and ion-exchange chromatography

    International Nuclear Information System (INIS)

    Three independent analytical techniques - instrumental neutron activation analysis. Atomic absorption spectrometry and ion-exchange chromatography - were applied to airborne particulate collected on filters and to atmospheric acid gases collected in carbonate buffer solutions. 20 trace elements and 7 acid gases and acid aerosols were determined. Results were compared with those observed elsewhere and showed that air pollution is low in Kinshasa and does not give rise to anxieties. The main known sources of pollutants are: vehicle exhaust and aeolian process on stripped soils. (author). 13 refs, 2 figs, 6 tabs

  3. A simple analytical model for electronic conductance in a one dimensional atomic chain across a defect

    Energy Technology Data Exchange (ETDEWEB)

    Khater, Antoine; Szczesniak, Dominik [Laboratoire de Physique de l' Etat Condense UMR 6087, Universite du Maine, 72085 Le Mans (France)

    2011-04-01

    An analytical model is presented for the electronic conductance in a one dimensional atomic chain across an isolated defect. The model system consists of two semi infinite lead atomic chains with the defect atom making the junction between the two leads. The calculation is based on a linear combination of atomic orbitals in the tight-binding approximation, with a single atomic one s-like orbital chosen in the present case. The matching method is used to derive analytical expressions for the scattering cross sections for the reflection and transmission processes across the defect, in the Landauer-Buttiker representation. These analytical results verify the known limits for an infinite atomic chain with no defects. The model can be applied numerically for one dimensional atomic systems supported by appropriate templates. It is also of interest since it would help establish efficient procedures for ensemble averages over a field of impurity configurations in real physical systems.

  4. Determination of cadmium in biodiesel using microemulsion and electrothermal atomization atomic absorption spectrometry.

    Science.gov (United States)

    Lima, Adriana S; Silva, Deise G; Teixeira, Leonardo S G

    2015-01-01

    This work aimed to prepare biodiesel microemulsions for the subsequent quantification of cadmium via graphite furnace atomic absorption spectrometry (GFAAS). The biodiesel samples were prepared using n-propanol as an emulsifier, 10% (v/v) nitric acid as the aqueous phase, and biodiesel. Pseudoternary phase diagrams were constructed to determine the microemulsion region with the specified components. The optimized conditions for microemulsion formation were 57.6% (v/v) n-propanol, 21.2% (v/v) biodiesel, and 21.2% (v/v) nitric acid solution. The stability of the microemulsified system was investigated using aqueous and organic standards, and the system was found to be stable for at least 240 min. The applied pyrolysis and atomization temperatures were 800 and 2000 °C, respectively, and 5 μg of aluminum was used as the chemical modifier. The obtained limits of detection and quantification were 0.2 and 0.5 μg kg(-1), respectively, and the characteristic mass was 1.6 pg. The precision, expressed as the relative standard deviation (% R.S.D., n = 10), was 2.5% for a sample with a cadmium concentration of 6.5 μg kg(-1). The accuracy was determined from addition and recovery experiments, with results varying from 93 to 108% recovery. This study demonstrates that the proposed method based on the use of a microemulsion formation in sample preparation can be applied as an efficient alternative for the determination of cadmium in biodiesel by GFAAS. Cadmium determination in biodiesel samples of different origins (soybean, corn, cotton, and sunflower) was evaluated after acid digestion using the inductively coupled plasma-mass spectrometry (ICP-MS) technique, and the obtained results were compared to the results obtained using the proposed method. The paired t test (95% confidence level) did not show significant differences. The concentrations of cadmium found ranged from 5.3 to 8.0 μg kg(-1). PMID:25381584

  5. Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jesus, Alexandre de; Zmozinski, Ariane Vanessa [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Damin, Isabel Cristina Ferreira [Faculdade Dom Bosco de Porto Alegre, 90520-280, Porto Alegre, RS (Brazil); Silva, Marcia Messias, E-mail: mmsilva@iq.ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (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 Rodrigues [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2012-05-15

    In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 {mu}g kg{sup -1} for arsenic and 0.2 {mu}g kg{sup -1} for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a 'cold finger' was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis. - Highlights: Black-Right-Pointing-Pointer A direct sampling GF AAS method to determine As and Cd in crude oil was proposed. Black-Right-Pointing-Pointer The conventional chemical modifier Pd/Mg has been used to stabilize As and Cd. Black

  6. 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

  7. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pedersen, G.A. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark); Larsen, E.H. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark)

    1997-07-01

    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination with an aqueous solution of 6 mmol L{sup -1} of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 {sigma}) achieved by the HPLC-FAAS system was 1 mg L{sup -1} of selenium (100 {mu}L injections) for each of the four selenium species. More powerful selenium detection was achieved using an ELAN 5000 ICP-MS instrument. Selenium was measured at m/z = 82. The ICP-MS signal intensity was enhanced by a factor of 3-4 after addition of 3% methanol to the chromatographic mobile phase and by using an increased plasma power input of 1300 W. The limit of detection achieved under these conditions was 1 {mu}g L{sup -1} (100 {mu}L injections). The HPLC-ICP-MS system was used for selenium speciation of selenite and selenate in aqueous solutions during a BCR certification exercise and for selenium speciation in the certified reference material, BCR No. 402 White Clover. Extraction experiments revealed that the selenium species in the biological material were extractable only in the presence of water in the extraction medium. The results indicated that selenate and a compound of unknown identity U were present in the plant sample. (orig.). With 5 figs., 5 tabs.

  8. Padronização interna em espectrometria de absorção atômica Internal standardization in atomic absorption spectrometry

    OpenAIRE

    Kelly G. Fernandes; Mercedes de Moraes; José A. Gomes Neto; Joaquim A. Nóbrega; Pedro V. Oliveira

    2003-01-01

    This paper describes a review on internal standardization in atomic absorption spectrometry with emphasis to the systematic and random errors in atomic absorption spectrometry and applications of internal standardization in flame atomic absorption spectrometry and electrothermal atomic absorption spectrometry. The rules for selecting an element as internal standard, limitations of the method, and some comments about the application of internal standardization in atomic absorption spectrometry...

  9. Simultaneous determination of cadmium and lead in wine by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Freschi, Gian P. G.; Dakuzaku, Carolina S.; de Moraes, Mercedes; Nóbrega, Joaquim A.; Gomes Neto, José A.

    2001-10-01

    A method has been developed for the direct simultaneous determination of Cd and Pb in white and red wine by electrothermal atomic absorption spectrometry (ET-AAS) using a transversely heated graphite tube atomizer (THGA) with longitudinal Zeeman-effect background correction. The thermal behavior of both analytes during pyrolysis and atomization stages were investigated in 0.028 mol l -1 HNO 3 and in 1+1 v/v diluted wine using mixtures of Pd(NO 3) 2+Mg(NO 3) 2 and NH 4H 2PO 4+Mg(NO 3) 2 as chemical modifiers. With 5 μg Pd+3 μg Mg as the modifiers and a two-step pyrolysis (10 s at 400°C and 10 s at 600°C), the formation of carbonaceous residues inside the atomizer was avoided. For 20 μl of sample (wine+0.056 mol l -1 HNO 3, 1+1, v/v) dispensed into the graphite tube, analytical curves in the 0.10-1.0 μg l -1 Cd and 5.0-50 μg l -1 Pb ranges were established. The characteristic mass was approximately 0.6 pg for Cd and 33 pg for Pb, and the lifetime of the tube was approximately 400 firings. The limits of detection (LOD) based on integrated absorbance (0.03 μg l -1 for Cd, 0.8 μg l -1 for Pb) exceeded the requirements of Brazilian Food Regulations (decree #55871 from Health Department), which establish the maximum permissible level for Cd at 200 μg l -1 and for Pb at 500 μg l -1. The relative standard deviations ( n=12) were typically <8% for Cd and <6% for Pb. The recoveries of Cd and Pb added to wine samples varied from 88 to 107% and 93 to 103%, respectively. The accuracy of the direct determination of Cd and Pb was checked for 10 table wines by comparing the results with those obtained for digested wine using single-element ET-AAS, which were in agreement at the 95% confidence level.

  10. Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry

    OpenAIRE

    Ornatsky, Olga I.; Kinach, Robert; Bandura, Dmitry R.; Lou, Xudong; Tanner, Scott D; Baranov, Vladimir I.; Nitz, Mark; Mitchell A. Winnik

    2008-01-01

    Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for...

  11. Liquid sample introduction in inductively coupled plasma atomic emission and mass spectrometry — Critical review

    International Nuclear Information System (INIS)

    Inductively coupled plasma optical emission spectroscopy (ICP-OES) and mass spectrometry (ICP-MS) can be considered as the most important tools in inorganic analytical chemistry. Huge progress has been made since the first analytical applications of the ICP. More stable RF generators, improved spectrometers and detection systems were designed along with the achievements gained from advanced microelectronics, leading to overall greatly improved analytical performance of such instruments. In contrast, for the vast majority of cases liquid sample introduction is still based on the pneumatic principle as described in the late 19th century. High flow pneumatic nebulizers typically demand the use of spray chambers as “aerosol filters” in order to match the prerequisites of an ICP. By this, only a small fraction of the nebulized sample actually contributes to the measured signal. Hence, the development of micronebulizers was brought forward. Those systems produce fine aerosols at low sample uptake rates, but they are even more prone for blocking or clogging than conventional systems in the case of solutions containing a significant amount of total dissolved solids (TDS). Despite the high number of publications devoted to liquid sample introduction, it is still considered the Achilles' heel of atomic spectrometry and it is well accepted, that the technology used for liquid sample introduction is still far from ideal, even when applying state-of-the-art systems. Therefore, this review is devoted to offer an update on developments in the field liquid sample introduction that had been reported until the year 2013. The most recent and noteworthy contributions to this field are discussed, trends are highlighted and future directions are outlined. The first part of this review provides a brief overview on theoretical considerations regarding conventional pneumatic nebulization, the fundamentals on aerosol generation and discusses characteristics of aerosols ideally

  12. Column system using diaion HP-2MG for determination of some metal ions by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa; Soylak, Mustafa

    2004-02-23

    A column solid-phase extraction method for the preconcentration and determination of cadmium(II), copper(II), cobalt(II), iron(III), lead(II), nickel(II) and zinc(II) dithizone chelates by atomic absorption spectrometry has been described. Diaion HP-2MG was used as adsorbent for column studies. The influences of the various analytical parameters including pH of the aqueous solutions, amounts of ligand and resin were investigated for the retentions of the analyte ions. The recovery values are ranged from 95 to 102%. The influences of alkaline and earth alkaline ions were also discussed. The preconcentration factor was 375, when the sample volume and final volume are 750 and 2 ml, respectively. The detection limits of the analyte ions (k=3, N=21) were varying 0.08 {mu}g/l for cadmium to 0.25 {mu}g/l for lead. The relative standard deviations of the determinations at the concentration range of 1.8x10{sup -4} to 4.5x10{sup -5} mmol for the investigated elements were found to be lower than 9%. The proposed solid-phase extraction procedure were applied to the flame atomic absorption spectrometric determinations of analyte ions in natural waters (sea, tap, river), microwave digested samples (milk, red wine and rice) and two different reference standard materials (SRM1515 apple leaves and NRCC-SLRS-4 riverine water)

  13. Analytical theory for the nuclear level shift of hadronic atoms

    International Nuclear Information System (INIS)

    The spectrum problem in the Coulomb potential distorted at small distances is considered. Nuclear shifts of 3-levels in p anti p and Σ-p atoms are calculated. The probabilities of radiative transitions from p-states to the shifted s-states in hadronic atom are also given. It is shown that the reconstruction of atomic levels switches to oscillation regime when absorption increases. The limits of applicability of the perturbation theory in terms of the scattering length for different values of absorption is discussed. An exactly solvable model, Coulomb plus Yamaguchi potential, is considered

  14. Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes (MWCNTs) and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity (R2=0.9992)over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%,respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

  15. Electrospray ionization and matrix assisted laser desorption/ionization mass spectrometry: powerful analytical tools in recombinant protein chemistry

    DEFF Research Database (Denmark)

    Andersen, Jens S.; Svensson, B; Roepstorff, P

    1996-01-01

    Electrospray ionization and matrix assisted laser desorption/ionization are effective ionization methods for mass spectrometry of biomolecules. Here we describe the capabilities of these methods for peptide and protein characterization in biotechnology. An integrated analytical strategy is...

  16. Assessment of the analytical capabilities of inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Taylor, H.E.; Garbarino, J.R.

    1988-01-01

    A thorough assessment of the analytical capabilities of inductively coupled plasma-mass spectrometry was conducted for selected analytes of importance in water quality applications and hydrologic research. A multielement calibration curve technique was designed to produce accurate and precise results in analysis times of approximately one minute. The suite of elements included Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Hg, Li, Mn, Mo, Ni, Pb, Se, Sr, V, and Zn. The effects of sample matrix composition on the accuracy of the determinations showed that matrix elements (such as Na, Ca, Mg, and K) that may be present in natural water samples at concentration levels greater than 50 mg/L resulted in as much as a 10% suppression in ion current for analyte elements. Operational detection limits are presented.

  17. Determination of cadmium in real water samples by flame atomic absorption spectrometry after cloud point extraction

    International Nuclear Information System (INIS)

    Water pollution is a global threat and it is the leading world wide cause of death and diseases. The awareness of the potential danger posed by heavy metals to the ecosystems and in particular to human health has grown tremendously in the past decades. Separation and preconcentration procedures are considered of great importance in analytical and environmental chemistry. Cloud point is one of the most reliable and sophisticated separation methods for determination of traces quantities of heavy metals. Cloud point methodology was successfully employed for preconcentration of trace quantities of cadmium prior to their determination by flame atomic absorption spectrometry (FAAS). The metals react with 8-hydroxquinoline in a surfactant Triton X-114 medium. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation and the cadmium content was measured by FAAS. The validation of the procedure was carried out by spiking addition methods. The method was applied for determination of Cd in water samples of different ecosystems (lake and river). (author)

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

    International Nuclear Information System (INIS)

    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% SnCl2 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-1. The detection limit (3σ b/S) achieved is 5 ng L-1. The relative standard deviation (R.S.D.) was 1.4%, evaluated from 16 successive injections of 250 ng L-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

  19. Determination of myo-inositol hexakisphosphate (phytate) in urine by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grases, F.; Perello, J.; Isern, B.; Prieto, R.M

    2004-05-10

    Myo-inositol hexakisphosphate (phytate) is a substance present in urine with an important role in preventing calcium renal calculi development. In spite of this, the use of urinary phytate levels on stone-formers' evaluation and treatment is still notably restricted as a consequence of the enormous difficulty to analyze this substance in urine. In this paper, a simple procedure for routinary urinary phytate determination based on phosphorus determination through inductively coupled plasma atomic emission spectrometry is described. The method only requires a previous separation of phytate from other components by column anion exchange chromatography. The working linear range used was 0-2 mg l{sup -1} phosphorus (0-7 mg l{sup -1} phytate). The limit of detection was 64 {mu}g l{sup -1} of phytate and the limit of quantification was 213 {mu}g l{sup -1}. The relative standard deviation (R.S.D.) for 1.35 mg l{sup -1} phytate was 2.4%. Different urine samples were analyzed using an alternative analytical methodology based on gas chromatography (GC)/mass detection used for inositol determination (phytate was previously hydrolyzed), resulting both methods comparable using as criterion to assess statistical significance P<0.05.

  20. Chemical vapor generation of silver for atomic absorption spectrometry with the multiatomizer: Radiotracer efficiency study and characterization of silver species

    International Nuclear Information System (INIS)

    Volatile Ag species were generated in flow injection arrangement from nitric acid environment in the presence of surfactants (Triton X-100 and Antifoam B) and permanent Pd deposits as the reaction modifiers. Atomic absorption spectrometry (AAS) with multiple microflame quartz tube atomizer heated to 900 deg. C was used for atomization; evidence was found for thermal mechanism of atomization. Relative and absolute limits of detection (3σ, 250 μl sample loop) measured under optimized conditions were: 1.4 μg l-1 and 0.35 ng, respectively. The efficiency of chemical vapor generation (CVG) as well as spatial distribution of residual analyte in the apparatus was studied by 111Ag radioactive indicator (half-life 7.45 days) of high specific activity. It was found out that 23% of analyte was released into the gaseous phase. However, only 8% was found on filters placed at the entrance to the atomizer due to transport losses. About 40% of analyte remained in waste liquid, whereas the rest was found deposited over the CVG system. Presented study follows the hypothesis that the 'volatile' Ag species are actually metallic nanoparticles formed upon reduction in liquid phase and then released with good efficiency to the gaseous phase. Number/charge size distributions of dry aerosol were determined by Scanning Mobility Particle Sizer. Ag was detected in 40-45 nm particles holding 10 times more charge if compared to Boltzmann equilibrium. At the same time, Ag was also present on 150 nm particles, the main size mode of the CVG generator. The increase of Ag in standards was reflected by proportional increase in particle number/charge for 40-45 nm size particles only. Transmission electron microscopy revealed particles of 8 ± 2 nm sampled from the gaseous phase, which were associated in isolated clusters of few to few tens of nanometres. Ag presence in those particles was confirmed by Energy Dispersive X-ray Spectroscopy (EDS) analysis.

  1. A NEW GENERATION OF INSTRUMENTATION AND CAPABILITIES FOR ATOMIC MASS SPECTROMETRY

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    @@ Atomic mass spectrometry,embodied usually as inductively coupled plasma mass spectrometry (ICPMS) or glow-discharge mass spectrometry (GDMS),has become a widely accepted tool for trace and ultra-trace elemental analysis.ICPMS offers detection limits below 1 ppt in solution,a dynamic concentration levels,isotope-analysis and isotope-dilution capabilities,modest matrix interferences,understandable spectral interferences (isobaric overlaps),precision in range of 2—5%,and rapid measurements (typically 10 seconds per isotope).

  2. Considerations of particle vaporization and analyte diffusion in single-particle inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    The intensity of individual gold nanoparticles with nominal diameters of 80, 100, 150, and 200 nm was measured using single-particle inductively coupled plasma-mass spectrometry (ICP-MS). Since the particles are not perfectly monodisperse, a distribution of ICP-MS intensity was obtained for each nominal diameter. The distribution of particle mass was determined from the transmission electron microscopy (TEM) image of the particles. The distribution of ICP-MS intensity and the distribution of particle mass for each nominal diameter were correlated to give a calibration curve. The calibration curves are linear, but the slope decreases as the nominal diameter increases. The reduced slope is probably due to a smaller degree of vaporization of the large particles. In addition to the degree of particle vaporization, the rate of analyte diffusion in the ICP is an important factor that determines the measured ICP-MS intensity. Simulated ICP-MS intensity versus particle size was calculated using a simple computer program that accounts for the vaporization rate of the gold nanoparticles and the diffusion rate and degree of ionization of the gold atoms. The curvature of the simulated calibration curves changes with sampling depth because the effects of particle vaporization and analyte diffusion on the ICP-MS intensity are dependent on the residence time of the particle in the ICP. Calibration curves of four hypothetical particles representing the four combinations of high and low boiling points (2000 and 4000 K) and high and low analyte diffusion rates (atomic masses of 10 and 200 Da) were calculated to further illustrate the relative effects of particle vaporization and analyte diffusion. The simulated calibration curves show that the sensitivity of single-particle ICP-MS is smaller than that of the ICP-MS measurement of continuous flow of standard solutions by a factor of 2 or more. Calibration using continuous flow of standard solution is semi-quantitative at best. An

  3. A geração química de vapor em espectrometria atômica Chemical vapor generation in atomic spectrometry

    OpenAIRE

    Iracema Takase; Hugo Borges Pereira; Aderval S. Luna; Patrícia Grinberg; Reinaldo Calixto de Campos

    2002-01-01

    The historical development of atomic spectrometry techniques based on chemical vapor generation by both batch and flow injection sampling formats is presented. Detection via atomic absorption spectrometry (AAS), microwave induced plasma optical emission spectrometry (MIP-OES), inductively coupled plasma optical emission spectrometry (ICP-OES) , inductively coupled plasma mass spectrometry (ICP-MS) and furnace atomic nonthermal excitation spectrometry (FANES) are considered. Hydride generation...

  4. 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

  5. Generation of Volatile Compounds for Analytical Atomic Spectroscopy

    Czech Academy of Sciences Publication Activity Database

    Dědina, Jiří

    Chichester: John Wiley & Sons Ltd, 2011 - (Meyers, R.), s. 897-936 ISBN 978-0-470-97333-2 R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : VCs * AAS * AES * AFS Subject RIV: CB - Analytical Chemistry, Separation

  6. On-line preconcentration and determination of mercury in biological and environmental samples by cold vapor-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    An on-line procedure for the determination of traces of total mercury in environmental and biological samples is described. The present methodology combines cold vapor generation associated to atomic absorption spectrometry (CV-AAS) with preconcentration of the analyte on a minicolumn packed with activated carbon. The retained analyte was quantitatively eluted from the minicolumn with nitric acid. After that, volatile specie of mercury was generated by merging the acidified sample and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the atomizer device. Optimizations of both, preconcentration and mercury volatile specie generation variables were carried out using two level full factorial design (23) with 3 replicates of the central point. Considering a sample consumption of 25 mL, an enrichment factor of 13-fold was obtained. The detection limit (3σ) was 10 ng L-1 and the precision (relative standard deviation) was 3.1% (n = 10) at the 5 μg L-1 level. The calibration curve using the preconcentration system for mercury was linear with a correlation coefficient of 0.9995 at levels near the detection limit up to at least 1000 μg L-1. Satisfactory results were obtained for the analysis of mercury in tap water and hair samples

  7. 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. PMID:23708618

  8. Evaluation of a method for the determination of chromium in urine by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A method for the determination of chromium in urine by atomic absorption spectrometry, using electrothermic atomization with pyrolytic graphite tubes, is proposed. The determinations are performed by standard addition. The method is applicable to biologic monitoring of populations with different degrees of exposition. It is also used in the analysis of chromium in sediments. Results of chromium in urine of a population group non-exposed to the metal are presented. 11 refs

  9. Model calculation of the characteristic mass for convective and diffusive vapor transport in graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Bencs, László; Laczai, Nikoletta; Ajtony, Zsolt

    2015-07-01

    A combination of former convective-diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass - m0) in graphite furnace atomic absorption spectrometry (GFAAS). This approach encompasses the influence of forced convection of the internal furnace gas (mini-flow) combined with concentration diffusion of the analyte atoms on the residence time in a spatially isothermal furnace, i.e., the standard design of the transversely heated graphite atomizer (THGA). A couple of relationships for the diffusional and convectional residence times were studied and compared, including in factors accounting for the effects of the sample/platform dimension and the dosing hole. These model approaches were subsequently applied for the particular cases of Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn analytes. For the verification of the accuracy of the calculations, the experimental m0 values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm3 min- 1) of the internal sheath gas during atomization. The theoretical and experimental ratios of m0(mini-flow)-to-m0(stop-flow) were closely similar for each study analyte. Likewise, the calculated m0 data gave a fairly good agreement with the corresponding experimental m0 values for stopped and mini-flow conditions, i.e., it ranged between 0.62 and 1.8 with an average of 1.05 ± 0.27. This indicates the usability of the current model calculations for checking the operation of a given GFAAS instrument and the applied methodology.

  10. Direct microcomputer controlled determination of zinc in human serum by flow injection atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Nielsen, Bent; Jensen, Arne;

    1986-01-01

    A procedure is described for the direct determination of zinc in human serum by fully automated, microcomputer controlled flow injection atomic absorption spectrometry (Fl-AAS). The Fl system is pumpless, using the negative pressure created by the nebuliser. It only consists of a three-way valve...

  11. 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.

  12. Precise atomic mass measurements by deflection mass spectrometry

    CERN Document Server

    Barber, R C

    2003-01-01

    Since its inception nearly 90 years ago by J.J. Thomson, the precise determination of atomic masses by the classical technique of deflecting charged particles in electric and magnetic fields has provided a large body of data on naturally occurring nuclides. Currently, such measurements on stable nuclides have frequently achieved a precision of better than two parts in 10 sup 9 of the mass. A review of the technique, together with a brief summary of the important historical developments in the field of precise atomic mass measurements, will be given. The more recent contributions to this field by the deflection mass spectrometer at the University of Manitoba will be provided as illustrations of the culmination of the techniques used and the applications that have been studied. A brief comparison between this and newer techniques using Penning traps will be presented.

  13. Precise atomic mass measurements by deflection mass spectrometry

    Science.gov (United States)

    Barber, R. C.; Sharma, K. S.

    2003-05-01

    Since its inception nearly 90 years ago by J.J. Thomson, the precise determination of atomic masses by the classical technique of deflecting charged particles in electric and magnetic fields has provided a large body of data on naturally occurring nuclides. Currently, such measurements on stable nuclides have frequently achieved a precision of better than two parts in 10 9 of the mass. A review of the technique, together with a brief summary of the important historical developments in the field of precise atomic mass measurements, will be given. The more recent contributions to this field by the deflection mass spectrometer at the University of Manitoba will be provided as illustrations of the culmination of the techniques used and the applications that have been studied. A brief comparison between this and newer techniques using Penning traps will be presented.

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

    International Nuclear Information System (INIS)

    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.

  15. Evaluation of the effect of wavelength poisitioning errors on Kalman filtering results in inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    This work evaluates the effect of wavelength positioning errors in spectral scans on analytical results when the Kalman filtering technique is used for the correction of line interferences in inductively coupled plasma atomic emission spectrometry (ICP-AES). The results show that a positioning accuracy of 0.1 pm is required in order to obtain accurate and precise estimates for analyte concentrations. The positioning error in sample scans is more crucial than that in model scans. The relative bias in measured analyte concentration originating from a positioning error in a sample scan increases linearly with an increase in the magnitude of the error and the peak distance of the overlapping lines, but is inversely proportional to the signal-to-background ratio. By the use of an optimization procedure for the positions of scans with the innovations number as the criterion, the wavelength positioning error can be reduced and, correspondingly, the accuracy and precision of analytical results improved. 19 refs., 4 figs., 2 tabs

  16. In situ collection of volatile silver species in a new modular quartz tube atomizer for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Kratzer, Jan; Vobecký, Miloslav; Matoušek, Tomáš

    2012-01-01

    Roč. 27, č. 9 (2012), s. 1382-1390. ISSN 0267-9477 R&D Projects: GA ČR GA203/09/1783 Institutional support: RVO:68081715 Keywords : volatile species generation * in-situ collection * quartz tube atomizer Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.155, year: 2012

  17. Sapphire: a better material for atomization and in situ collection of silver volatile species for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Dědina, Jiří

    2015-01-01

    Roč. 108, JUN (2015), s. 61-67. ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant ostatní: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : silver * volatile species generation * sapphire tube atomizer Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.176, year: 2014

  18. On-Line Preconcentration and Speciation of Chromium by an 8-Hydroxyquinoline Microcolumn Immobilized on Surfactant-Coated Alumina and Flow Injection Atomic Absorption Spectrometry

    OpenAIRE

    AHMADI, Seyyed Hamid; SHABANI, Ali Mohammad HAJI

    2007-01-01

    An on-line technique for the determination of chromium species with atomic absorption spectrometry is described. The method is based on separation and preconcentration of Cr(III) on a microcolumn of immobilized 8-hydroxyquinoline on surfactant-coated alumina. The adsorbed analyte is then eluted with 400 m L of 20% ethanolic solution of 1.5 mol L-1 hydrochloric acid and is transported to a flame atomic absorption spectrometer for quantification. The effects of pH, sample and eluent f...

  19. Hydride generation for arsenic speciation analysis by atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Matoušek, Tomáš; Dědina, Jiří; Stýblo, M.

    Bratislava: Comenius University, 2006 - (Kubová, J.; Hagarová, I.). s. 119 ISBN 80-223-2244-X. [Slovak Spectroscopic Conference /18./. 15.10.2006-18.10.2006, Spišská Nová Ves] R&D Projects: GA AV ČR IAA400310507 Grant ostatní: NIH-FIRCA(US) 1 R03 TW007057-01 Institutional research plan: CEZ:AV0Z40310501 Keywords : HG-AAS * multiatomizer * arsenic Subject RIV: CB - Analytical Chemistry, Separation

  20. MERCURY QUANTIFICATION IN SOILS USING THERMAL DESORPTION AND ATOMIC ABSORPTION SPECTROMETRY: PROPOSAL FOR AN ALTERNATIVE METHOD OF ANALYSIS

    Directory of Open Access Journals (Sweden)

    Liliane Catone Soares

    2015-08-01

    Full Text Available Despite the considerable environmental importance of mercury (Hg, given its high toxicity and ability to contaminate large areas via atmospheric deposition, little is known about its activity in soils, especially tropical soils, in comparison with other heavy metals. This lack of information about Hg arises because analytical methods for determination of Hg are more laborious and expensive compared to methods for other heavy metals. The situation is even more precarious regarding speciation of Hg in soils since sequential extraction methods are also inefficient for this metal. The aim of this paper is to present a technique of thermal desorption associated with atomic absorption spectrometry, TDAAS, as an efficient tool for quantitative determination of Hg in soils. The method consists of the release of Hg by heating, followed by its quantification by atomic absorption spectrometry. It was developed by constructing calibration curves in different soil samples based on increasing volumes of standard Hg2+ solutions. Performance, accuracy, precision, and quantification and detection limit parameters were evaluated. No matrix interference was detected. Certified reference samples and comparison with a Direct Mercury Analyzer, DMA (another highly recognized technique, were used in validation of the method, which proved to be accurate and precise.

  1. Laser resonance ionization mass spectrometry as a sensitive analytical method for actinides and technetium

    International Nuclear Information System (INIS)

    Laser resonance ionization mass spectrometry has been investigated as a method for the determination of trace amounts of actinides and technetium. A high sensitivity and selectivity have been achieved by three-step photoionization of the elements in the atomic state followed by time-of-flight measurement for mass analysis. The system for photoionization consists of three dye lasers which are pumped simultaneously by a copper vapour laser of 30 W average power at a pulse repetition rate of 6.5 KHz. The time-of-flight spectrometer has a mass resolution better than 2500. By ionization via autoionization states and by saturation in each excitation step a detection limit of less than 108 atoms of actinides or of technetium in the sample can be reached. (author)

  2. A geração química de vapor em espectrometria atômica Chemical vapor generation in atomic spectrometry

    Directory of Open Access Journals (Sweden)

    Iracema Takase

    2002-12-01

    Full Text Available The historical development of atomic spectrometry techniques based on chemical vapor generation by both batch and flow injection sampling formats is presented. Detection via atomic absorption spectrometry (AAS, microwave induced plasma optical emission spectrometry (MIP-OES, inductively coupled plasma optical emission spectrometry (ICP-OES , inductively coupled plasma mass spectrometry (ICP-MS and furnace atomic nonthermal excitation spectrometry (FANES are considered. Hydride generation is separately considered in contrast to other methods of generation of volatile derivatives. Hg ¾ CVAAS (cold vapor atomic absorption spectrometry is not considered here. The current state-of-the-art, including extension, advantages and limitations of this approach is discussed.

  3. Pulse nebulization atomic absorption spectrometry after preconcentration from acidic media

    International Nuclear Information System (INIS)

    The possible advantages of the combination: chlorinated solvent extraction - pulse nebulization, abomic absorption spectrometry (AAS), as well as application of this method to multi-element determination of several important trace elements in biological samples is investigated. Hexamethyleneammonium hexamethylenedithiocarbamate (HMA-HMDTC) and ammonium pyrrolidinedithiocarbamate (APDC) as regents and CCl4, CHCl3, butylacetate (BuOAc) and methylisobutyl ketone (MIBK) as organic solvents are utilized. There is a tendency that CCl4 is the best solvent and MIBK - the worst. The study of extraction efficiency versus the ratio of aqueous-to-organic phase also shows the advantages of chlorinated solvents for extraction from acidic media. Better results are obtained with HMA-HMDTC as a reagent for Cu and Pb, whereas, for Cd extraction APDC gave a more efficient extraction. Chloroform shows a higher sensitivity enhancement factor, especially for volatile and/or chloride-forming elements. The extraction is successfully applied to determination of Cd, Cu and Pb in tissues of alfalfa, cabbage, carrots, onions, potatoes and wheat, as well as two standard reference materials. The results are in good agreement with the certified values

  4. Bromine and bromide content in soils: Analytical approach from total reflection X-ray fluorescence spectrometry.

    Science.gov (United States)

    Gallardo, Helena; Queralt, Ignasi; Tapias, Josefina; Candela, Lucila; Margui, Eva

    2016-08-01

    Monitoring total bromine and bromide concentrations in soils is significant in many environmental studies. Thus fast analytical methodologies that entail simple sample preparation and low-cost analyses are desired. In the present work, the possibilities and drawbacks of low-power total reflection X-ray fluorescence spectrometry (TXRF) for the determination of total bromine and bromide contents in soils were evaluated. The direct analysis of a solid suspension using 20 mg of fine ground soil (water soil extracts. In this case, the TXRF analysis can be directly performed by depositing 10 μL of the internal standardized soil extract sample on a quartz glass reflector in a measuring time of 1500 s. The bromide limit of detection by this approach was 10 μg L(-1). Good agreement was obtained between the TXRF results for the total bromine and bromide determinations in soils and those obtained by other popular analytical techniques, e.g. energy dispersive X-ray fluorescence spectrometry (total bromine) and ionic chromatography (bromide). As a study case, the TXRF method was applied to study bromine accumulation in two agricultural soils fumigated with a methyl bromide pesticide and irrigated with regenerated waste water. PMID:27179429

  5. Micro-determination of ytterbium with electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    This communication reports the use of a pyrolytic graphite coated tube, lined with tantalum-tungsten, and a local made atomic absorption spectrometer (Model WFD-Y3) for the determination of small amount Yb in pure Y2O3 and mixed rare earth oxides. It is found that the method proposed is sensitive, reproducible and simple in manipulation. Even as low as 0.2 μg Yb in one gram sample (n x 10-7) can be determined directly without pre-concentration. It is found experimentally that the optimum condition for drying is at 150 deg C. for 20 sec, ashing at 1000 deg C. for 20 sec and atomization at 2770 deg C. for 12 sec. Within the range 1.0-18ng Yb/ml the calibration curve of Yb is linear. Before injecting into the tube, the acidity of the sample solution should be ajusted to 0.1 to 2 M with nitric or hydrochloric acid. For 5ng Yb/ml, Al(III), Ca(II) and La(III) interference, when their amount present is 50 μg/ml or more. On the other hand, Cu(II), Fe(III), Mg(II), K(I) and Y(III) in amount up to 1 mg/ml do not interfere

  6. 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. PMID:15910814

  7. Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

    International Nuclear Information System (INIS)

    Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level)

  8. Behaviour of the thermospray nebulizer as a system for the introduction of organic solutions in flame atomic absorption spectrometry

    Science.gov (United States)

    Mora, Juan; Canals, Antonio; Hernandis, Vicente

    1996-10-01

    The results obtained in the evaluation of the thermospray nebulizer for the introduction of organic solutions in atomic spectrometry are described. To this end, the influence of the nebulization variables (i.e., liquid flow, control temperature and inner diameter of the capillary) and of the nature of the solvent on the fraction of solvent vaporized, on the drop size distribution of the primary aerosol, on the rates of analyte and solvent transport to the atomization cell and on the analytical signal has been studied. Experimental fraction of solvent vaporized values obtained under different nebulization conditions are reported for the first time. The results show that the characteristics of the aerosol generated strongly depend on the nebulization variables since they determine the amount of energy available for surface generation. The median of the volume drop size distribution of the primary aerosol decreases when the control temperature or the liquid flow is increased or when the inner diameter of the capillary is decreased. As regards the physical properties of the solvent, the so-called expansion factor (i.e., the volume of vapour produced per unit volume of liquid solvent) is the most influential. Surface tension and viscosity are much less significant here than in ordinary pneumatic nebulization. The volatility of the solvent and the characteristics of the primary aerosol determine the solvent transport efficiency which reaches values close to 100% in many cases. The analytical signal is mainly determined by the analyte transport rate, although a severe negative effect appears which is related to the high solvent load to the flame. Due to this fact, the use of organic solvents instead of water in thermospray nebulization for Flame Atomic Absorption Spectrometry does not provide clear advantages, at least without desolvation. A new modified Nukiyama-Tanasawa equation has been presented and evaluated in order to predict the Sauter mean diameter of the thermal

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

    International Nuclear Information System (INIS)

    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 μL 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-1, the detection limit was 0.37 ng mL-1 (3Sb/m, n = 7) and the relative standard deviation was ±1.63% (n = 7, C = 200 ng mL-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.

  10. Simple analysis of total mercury and methylmercury in seafood using heating vaporization atomic absorption spectrometry.

    Science.gov (United States)

    Yoshimoto, Keisuke; Anh, Hoang Thi Van; Yamamoto, Atsushi; Koriyama, Chihaya; Ishibashi, Yasuhiro; Tabata, Masaaki; Nakano, Atsuhiro; Yamamoto, Megumi

    2016-01-01

    This study aimed to develop a simpler method for determining total mercury (T-Hg) and methylmercury (MeHg) in biological samples by using methyl isobutyl ketone (MIBK) in the degreasing step. The fat in the samples was extracted by MIBK to the upper phase. T-Hg transferred into the water phase. This was followed by the extraction of MeHg from the water phase using HBr, CuCl2 and toluene. The MeHg fraction was reverse-extracted into L-cysteine-sodium acetate solution from toluene. The concentrations of T-Hg and MeHg were determined by heating vaporization atomic absorption spectrometry. Certified reference materials for T-Hg and MeHg in hair and fish were accurately measured using this method. This method was then applied to determine T-Hg and MeHg concentrations in the muscle, liver and gonads of seafood for the risk assessment of MeHg exposure. The mean T-Hg and MeHg concentrations in squid eggs were 0.023 and 0.022 µg/g, and in squid nidamental glands 0.052 and 0.049 µg/g, respectively. The MeHg/T-Hg ratios in the eggs and nidamental glands of squid were 94.4% and 96.5%, respectively. The mean T-Hg and MeHg concentrations in the gonads of sea urchins were 0.043 and 0.001 µg/g, respectively, with a MeHg/T-Hg ratio of 3.5%. We developed an efficient analytical method for T-Hg and MeHg using MIBK in the degreasing step. The new information on MeHg concentration and MeHg/T-Hg ratios in the egg or nidamental glands of squid and gonads of sea urchin will also be useful for risk assessment of mercury in seafood. PMID:27432235

  11. Development of an axially viewed inductively coupled plasma for atomic emission spectrometry and comparison between the detection limits of lead

    International Nuclear Information System (INIS)

    An ICP(Inductively Coupled plasma) emission spectrometer was developed with an axially viewed ICP source incorporated by a 5-turned induction coil and a torch, outer quartz tube of which was 50 mm longer than that used in conventional ICP/AES(Inductively Coupled Plasma Atomic Emission Spectrometry). The optimization of the system has been performed in terms of the determination of signal-to-noise ratio and background intensity at various rf powers, sample flow rates, argon gas flow rates and cut-off gas flow rates. The spectro-analytical characteristics of the spectrum obtained between 200 and 500 nm was revealed to be similar compared with a vertically viewed ICP source. The detection limit of Pb(II) at 220.35 nm was 11 ppb which was 5 times lower than that obtained with a vertically viewed ICP source. (author)

  12. Solid phase microextraction capillary gas chromatography combined with furnace atomization plasma emission spectrometry for speciation of mercury in fish tissues

    International Nuclear Information System (INIS)

    The use of solid phase microextraction in conjunction with tandem gas chromatography-furnace atomization plasma emission spectrometry (SPME-GC-FAPES) was evaluated for the determination of methylmercury and inorganic mercury in fish tissue. Samples were digested with methanolic potassium hydroxide, derivatized with sodium tetraethylborate and extracted by SPME. After the SPME extraction, species were separated by GC and detected by FAPES. All experimental parameters were optimized for best separation and analytical response. A repeatability precision of typically 2% can be achieved with long-term (3 months) reproducibility precision of 4.3%. Certified Reference Materials DORM-2, DOLT-2 and TORT-2 from the National Research Council of Canada were analyzed to verify the accuracy of this technique. Detection limits of 1.5 ng g-1 for methylmercury and 0.7 ng g-1 for inorganic mercury in biological tissues were obtained

  13. Optimization of conditions for the determination of Eu, Gd and Sm by atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES)

    International Nuclear Information System (INIS)

    The possibilities of the determination of Sm, Eu and Gd by atomic absorption and emission spectrometry were investigated. Measurement parameters on a Varian atomic absorption spectrometer were optimized (the height of the measurement above the nozzle of the burner, stoichiometry of the dinitrogen oxide-acetylene flame by statistical evaluation of the signals). The following optimal conditions were found for the Sm, Eu and Gd determinations: Samarium - measurement under the emission arrangement at 476.1 nm wavelength, slit width 0.05 nm, in reduction flame close to the outlet slit of the flame (at the lowest part of the flame). Europium - measurement under the absorption arrangement at 459.4 nm wavelength, slit width 1 nm, in reduction flame at the lowest part of the flame. Gadolinium - measurement under the emission arrangement at 461.7 nm wavelength, slit width 0.05 nm, at the lowest part of the flame. (author). 2 figs., 3 tabs., 2 refs

  14. Determination of antimony in sediments and soils by slurry sampling graphite furnace atomic absorption spectrometry using a permanent chemical modifier

    Energy Technology Data Exchange (ETDEWEB)

    Dobrowolski, Ryszard, E-mail: rdobrow@poczta.umcs.lublin.pl; Adamczyk, Agnieszka; Otto, Magdalena; Dobrzynska, Joanna

    2011-07-15

    For comparison of action of mixed permanent modifiers Ir/Nb and Ir/W, the influence of the amounts of modifier components was studied and the atomic absorption pyrolysis and atomization curves were determined with different modifiers. The optimum amounts of modifier components were 30 {mu}g Ir and 40 {mu}g of Nb that were deposited onto the L'vov platform in advance to analytical measurements. The long-term performance of the Ir and Nb permanent modifiers was derived from the investigations by scanning electron microscopy and energy dispersive X-ray spectrometry. The soil and sediment slurries were prepared in 4% hydrofluoric acid and 6% suspension of polytetrafluoroethylene in order to remove the high concentration of silica during the pyrolysis step of 900 deg. C. The calibration was made by using aqueous standards. The analysis of certified reference materials confirmed the accuracy and reliability of the proposed analytical approach. The precision of Sb determination was characterized with less than 6% RSD.

  15. Chemometric extraction of analyte-specific chromatograms in on-line gradient LC-infrared spectrometry.

    Science.gov (United States)

    Kuligowski, Julia; Quintás, Guillermo; Garrigues, Salvador; de la Guardia, Miguel

    2009-12-01

    This work exploits the possibilities offered by the recently developed multivariate method named Science-Based Calibration (SBC), for the extraction of 'analyte-specific' chromatograms in on-line gradient reversed phase LC-infrared spectrometry (IR) in the presence of a high spectral and chromatographic overlapping between the analyte of interest, co-eluting sample matrix constituents and the mobile phase components. The SBC method uses an experimentally measured single response spectrum of the analyte of interest and representative noise to calculate an optimum regression vector (b(opt(1))). Then, the b(opt(1)) vector is used to predict the concentration of the analyte of interest in the spectra of the LC-IR sample chromatograms. To evaluate the advantages and pitfalls of the proposed approach, two different situations were analysed on real LC-IR data sets obtained from the injection of a series of standard solutions of four nitrophenols (p-nitrophenol, 3-methyl-4-nitrophenol, 2,4-dinitrophenol and 4-nitrophenol) in a reversed phase system under gradient conditions. In the first situation, the extraction of the 'analyte-specific' chromatogram was carried out without previous knowledge of the spectral features of other interferents present in the sample matrix. In a second situation evaluated, data obtained from the LC injection of a sample blank is available. Results show the potential applicability of this technique in a variety of situations and evidenced that the proposed chemometric approach improves the selectivity and sensitivity of the LC-IR hyphenation. PMID:19877149

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

    International Nuclear Information System (INIS)

    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(NO3)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 μg g-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)

  17. Determination of Ultra-trace Amounts of Arsenic(III) by Flow Injection Hydride Generation Atomic Absorption Spectrometry with On-line Preconcentration by Coprecipitation with Lanthanum Hydroxide or Hafnium Hydroxide

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Sloth, Jens Jørgen; Hansen, Elo Harald

    1996-01-01

    A time-based flow-injection (FI) procedure for the determination of ultra-trace amounts of inorganic arsenic(III) is described, which combines hydride generation atomic absorption spectrometry (HG-AAS) with on-line preconcentration of the analyte by inorganic coprecipitation-dissolution in a...

  18. Sequential injection on-line matrix removal and trace metal preconcentration using a PTFE beads packed column as demonstrated for the determination of cadmium by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    A sequential injection (SI) on-line matrix removal and trace metal preconcentration procedure by using a novel microcolumn packed with PTFE beads is described, and demonstrated for trace cadmium analysis with detection by electrothermal atomic absorption spectrometry (ETAAS). The analyte is...

  19. Determination of Ultra-Trace Amounts of Selenium(IV) by Flow Injection Hydride Generation Atomic Absorption Spectrometry with On-line Preconcentration by Co-precipitation with Lanthanium Hydroxide. Part II. On-line Addition of Coprecipating Agent

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Sloth, Jens Jørgen; Hansen, Elo Harald

    1996-01-01

    A flow injection procedure for the determination of ultra-trace amounts of selenium(IV) is described, which combines hydride generation atomic absorption spectrometry (HGAAS) with on-line preconcentration of the analyte by co-precipitation-dissolution in a filterless knotted Microline reactor...

  20. 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

    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-system and the...

  1. Mercury determination in non- and biodegradable materials by cold vapor capacitively coupled plasma microtorch atomic emission spectrometry

    International Nuclear Information System (INIS)

    Highlights: → Use of a miniaturized analytical system with microtorch plasma for Hg determination. → Determination of Hg in non- and biodegradable materials using cold vapor generation. → Figures of merit and advantages of the miniaturized system for Hg determination. - Abstract: A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min-1 Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl2 reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO3-H2SO4 mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml-1 or 0.08 μg g-1 in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg-1, while recovery in two polyethylene certified reference materials in the range 98.7 ± 4.5% (95% confidence level).

  2. Assessment of resonance ionization mass spectrometry for analytical chemistry and spectroscopy

    International Nuclear Information System (INIS)

    Resonance ionization mass spectrometry (RIMS) is a natural outgrowth of RIS. The result of an RIS process is an ion pair. The electron can be used to detect the process, and single atom detection has been demonstrated by this method. The cation resulting from the RIS process actually carries more easily accessible and useful information (i.e. the mass of the ion). RIMS is useful in mass analysis. The development of RIMS has proceeded along several different directions, using CW or pulsed lasers, narrow or wide band laser energies, different kinds of sample generation, and different kinds of mass separations. RIMS in various forms can be used to obtain either element or isotope selectivity. Even though the RIMS technique has developed along several lines, several things are common to all approaches. Ultimately RIMS requires gaseous, free, atoms. RIMS makes use of the photoionization of these atoms by absorption of photons through allowed transitions involving real energy levels. The ion once formed is detected by standard mass spectrometric techniques

  3. Speciation of mercury by chromatography coupled with atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Armstrong, H.E.L

    2000-03-01

    A commercial GC-AFS instrument has been developed and optimised for the speciation of organomercury. This instrument couples a GC oven to a modified atomic fluorescence detector via a ceramic pyrolyser. Organomercury compounds in dichloromethane solvent were directly injected through a Programmable Temperature Vaporiser Injector onto a DB1 Megabore column. Once separated, the compounds eluted from the column and were atomised in the pyrolyser then detected by AFS. The direct injection technique, ceramic pyrolysis design and argon purged detector have improved previous instrument designs by enhancing and maintaining sensitivity. The instrumental limit of detection was determined to be 0.25 pg Hg absolute. Methods were developed for the extraction of methylmercury from a variety of marine samples. The techniques were validated using mussel homogenate and dogfish liver (IAEA 142, SRM 8044 and DOLT-2) certified reference materials. An interlaboratory comparison exercise was participated in and a method was developed for the determination of methylmercury in Fucus sea plant (IAEA 140). A concentration of 0.63 {+-} 0.006 ng g{sup -1} was reported. The material is now certified at 0.626 {+-} 0.139 ng g{sup -1}. Of all the participating laboratories, this was the closest result to the certified value. The instrument and methods were also applied to soil and sediment samples. Once again validation was performed with a CRM sediment, IAEA 356. Although this material has been reported to give positive artifact formation when using a steam distillation sample preparation procedure, good agreement and no artifacts were observed upon analysis. A further contaminated land, an uncontaminated soil and sediment sample were also studied. For all the samples studied by GC-AFS total mercury measurements were also made following an appropriate digestion procedure and CV-AFS. A gas chromatograph was also coupled with ICP-MS and HPLC was coupled to CV-AFS as comparative techniques. Both

  4. Speciation of mercury by chromatography coupled with atomic spectrometry

    International Nuclear Information System (INIS)

    A commercial GC-AFS instrument has been developed and optimised for the speciation of organomercury. This instrument couples a GC oven to a modified atomic fluorescence detector via a ceramic pyrolyser. Organomercury compounds in dichloromethane solvent were directly injected through a Programmable Temperature Vaporiser Injector onto a DB1 Megabore column. Once separated, the compounds eluted from the column and were atomised in the pyrolyser then detected by AFS. The direct injection technique, ceramic pyrolysis design and argon purged detector have improved previous instrument designs by enhancing and maintaining sensitivity. The instrumental limit of detection was determined to be 0.25 pg Hg absolute. Methods were developed for the extraction of methylmercury from a variety of marine samples. The techniques were validated using mussel homogenate and dogfish liver (IAEA 142, SRM 8044 and DOLT-2) certified reference materials. An interlaboratory comparison exercise was participated in and a method was developed for the determination of methylmercury in Fucus sea plant (IAEA 140). A concentration of 0.63 ± 0.006 ng g-1 was reported. The material is now certified at 0.626 ± 0.139 ng g-1. Of all the participating laboratories, this was the closest result to the certified value. The instrument and methods were also applied to soil and sediment samples. Once again validation was performed with a CRM sediment, IAEA 356. Although this material has been reported to give positive artifact formation when using a steam distillation sample preparation procedure, good agreement and no artifacts were observed upon analysis. A further contaminated land, an uncontaminated soil and sediment sample were also studied. For all the samples studied by GC-AFS total mercury measurements were also made following an appropriate digestion procedure and CV-AFS. A gas chromatograph was also coupled with ICP-MS and HPLC was coupled to CV-AFS as comparative techniques. Both approaches were

  5. Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Liu Qingyang, E-mail: liuqingyang0807@yahoo.com.c [Beijing Center for Physical and Chemical Analysis, Beijing 100089 (China)

    2010-07-15

    This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg{sup 0}, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL{sup -1} for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury (n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).

  6. Ultratrace determination of tin by hydride generation in-atomizertrapping atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Průša, Libor; Dědina, Jiří; Kratzer, Jan

    2013-01-01

    Roč. 804, DEC (2013), s. 50-58. ISSN 0003-2670 R&D Projects: GA ČR(CZ) GPP206/11/P002 Grant ostatní: GA MŠk(CZ) MSM0021620857 Institutional support: RVO:68081715 Keywords : hydride generation * tin preconcentration * in-atomizer trapping * trap-and-atomizer device * stannane Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.517, year: 2013

  7. On the expression 'external calibration' in atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kantor, Tibor [Geological Institute of Hungary, Stefania Ave 14, 1143 Budapest (Hungary)], E-mail: kantib@t-online.hu

    2008-04-15

    The expressions 'calibration' and 'external calibration' appear together in the present literature of atomic spectrometry resulting in a dilemma of understanding and correct use. It is examined how the IUPAC can provide a guidance to the solution of this problem by recalling the definitions of related terms of optical, mass and X-ray atomic spectrometry techniques. The introduction and definition of these expressions in widely used text books are investigated and statistically evaluated for the articles published during the last 30 years in the periodical Spectrochimica Acta Part B. For the elimination of the literary difficulties with the use of the term 'calibration', attributes are proposed to express the degree of matrix matching of standards and samples.

  8. Analytical Solutions of Temporal Evolution of Populations in Optically-Pumped Atoms with Circularly Polarized Light

    Directory of Open Access Journals (Sweden)

    Heung-Ryoul Noh

    2016-03-01

    Full Text Available We present an analytical calculation of temporal evolution of populations for optically pumped atoms under the influence of weak, circularly polarized light. The differential equations for the populations of magnetic sublevels in the excited state, derived from rate equations, are expressed in the form of inhomogeneous second-order differential equations with constant coefficients. We present a general method of analytically solving these differential equations, and obtain explicit analytical forms of the populations of the ground state at the lowest order in the saturation parameter. The obtained populations can be used to calculate lineshapes in various laser spectroscopies, considering transit time relaxation.

  9. Two low-level gamma spectrometry systems of the IAEA Safeguards Analytical Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Parus, J.L. [IAEA, SAL, Vienna (Austria); Raab, W. [IAEA, SAL, Vienna (Austria); Donohue, D. [IAEA, SAL, Vienna (Austria); Jansta, V. [IAEA, SAL, Vienna (Austria); Kierzek, J. [IAEA, SAL, Vienna (Austria)

    1997-03-01

    A gamma spectrometry system designed for the measurement of samples with low and medium radioactivity (activity from a few to about 10{sup 4} Bq in the energy range from 25 to 2700 keV) has been installed at the IAEA Safeguards Analytical Laboratory in Seibersdorf. The system consists of 3 low level detectors: (1) n-type coaxial Ge with 42.4% relative efficiency, 1.85 keV FWHM at 1.33 MeV (2) planar Ge with 2000 mm{sup 2} area and 20 mm thickness, 562 eV FWHM at 122 keV (3) NaI(Tl) annulus of 25.4 cm diameter and 25.4 cm height, hole diameter 90 mm. (orig./DG)

  10. Analytical developments in thermal ionization mass spectrometry for the isotopic analysis of very small amounts

    International Nuclear Information System (INIS)

    In the framework of the French transmutation project of nuclear wastes, experiments consisted in the irradiation in a fast neutron reactor of few milligrams of isotopically enriched powders. Hence, the isotopic analysis of very small amount of irradiation products is one of the main issues. The aim of this study was to achieve analytical developments in thermal ionization mass spectrometry in order to accurately analyze these samples. Several axes were studied including the new total evaporation method, deposition techniques, electron multiplier potentialities and comparison between different isotope measurement techniques. Results showed that it was possible to drastically decrease the amounts needed for analysis, especially with Eu and Nd, while maintaining an uncertainty level in agreement with the project requirements. (author)

  11. 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

  12. 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 por 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)μg.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 10μg.L{sup −1}. The obtained

  13. 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 as...

  14. Analytical Validation of Accelerator Mass Spectrometry for Pharmaceutical Development: the Measurement of Carbon-14 Isotope Ratio.

    Energy Technology Data Exchange (ETDEWEB)

    Keck, B D; Ognibene, T; Vogel, J S

    2010-02-05

    Accelerator mass spectrometry (AMS) is an isotope based measurement technology that utilizes carbon-14 labeled compounds in the pharmaceutical development process to measure compounds at very low concentrations, empowers microdosing as an investigational tool, and extends the utility of {sup 14}C labeled compounds to dramatically lower levels. It is a form of isotope ratio mass spectrometry that can provide either measurements of total compound equivalents or, when coupled to separation technology such as chromatography, quantitation of specific compounds. The properties of AMS as a measurement technique are investigated here, and the parameters of method validation are shown. AMS, independent of any separation technique to which it may be coupled, is shown to be accurate, linear, precise, and robust. As the sensitivity and universality of AMS is constantly being explored and expanded, this work underpins many areas of pharmaceutical development including drug metabolism as well as absorption, distribution and excretion of pharmaceutical compounds as a fundamental step in drug development. The validation parameters for pharmaceutical analyses were examined for the accelerator mass spectrometry measurement of {sup 14}C/C ratio, independent of chemical separation procedures. The isotope ratio measurement was specific (owing to the {sup 14}C label), stable across samples storage conditions for at least one year, linear over 4 orders of magnitude with an analytical range from one tenth Modern to at least 2000 Modern (instrument specific). Further, accuracy was excellent between 1 and 3 percent while precision expressed as coefficient of variation is between 1 and 6% determined primarily by radiocarbon content and the time spent analyzing a sample. Sensitivity, expressed as LOD and LLOQ was 1 and 10 attomoles of carbon-14 (which can be expressed as compound equivalents) and for a typical small molecule labeled at 10% incorporated with {sup 14}C corresponds to 30 fg

  15. 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.

  16. Mineral Analysis the Infusion of Black Tea Samples by Atomic Absorption Spectrometry

    OpenAIRE

    Lahiji N.; Tadayon F.; Tamiji F.; Lahiji A. H.

    2013-01-01

    Tea infusion is one of the most popular drinks around the world. Since tea infusion is known to contain several essential nutrients, it is considered a healthy beverage. In this study eight different Iranian brands of tea infusion and eleven brands imported tea infusion samples from another country for Cu, Zn, Mn and Al were determined by flame atomic absorption spectrometry after wet digestion. The results of analysis showed that the extraction rates of minerals from dry black tea to infusio...

  17. Analytic method development to quantify by in-situ gamma spectrometry radionuclides in the ground

    International Nuclear Information System (INIS)

    This research thesis reports the development of an analytic method based on a Monte Carlo simulation to quantify radionuclides present in soils by means of in-situ gamma spectrometry, to understand physical phenomena involved before and after detection, and to improve and complement results after spectrum analysis. The first part describes the evolution of in-situ gamma spectrometry: sensor development, in-situ measurement principle, evolution of the analysis principle. The second part introduces the Monte Carlo simulation and describes the used models (sensor model using the stripping method, development of a new simulation model for the incident flow). The third part discusses the understanding of an in-situ spectrum with the localization of the origin of incident photons and the identification of measurement parameters. Modelling results are then presented, as well as the development of spectrum de-convolution method, and the calculation of dose factors. Finally, the use of the 'Peak-to-Valley' method completed by the Monte Carlo simulation results is explained and used to localize a source depth and to define the exponential distribution of Cs-137 in Orsay

  18. Determination of noble metals by Inductively Coupled Plasma Atomic Emission Spectrometry

    International Nuclear Information System (INIS)

    Full text: It is well known that significant quantities of soluble fission products such as La, Ce, Pr, Eu, Gd, Sm and noble metals such as Ag, Pt, Au, Ru, Rh, Pd are produced in the spent fuel dissolver solutions, in nuclear reactors. The recovery of noble metals from generated high level waste assumes importance in view of their usage in chemical and electronic industries. In the present work, Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) technique has been explored to determine six noble metals in aqueous solutions. Synthetic solution standards containing individually Ag, Au, Pt, Pd, Rh and Ru in the range of 1-500 μg/mL were prepared. Individual elemental solutions at 100μg/mL were fed in to the plasma. The instrumental parameters were obtained for positioning of the analytical line with appropriate sensitivity on the photomultiplier tube. The prominent ICP lines reported in literature in decreasing order of sensitivities for Au are 242.745, 267.895, 197.819, 208.219 nm; Ru are 240.272, 245.657, 267.876 nm; for Rh are 233.477, 249.077, 343.419, 252.053 nm and for Pt are 214.423, 203.646, 214.937 nm respectively. Of these the lines shown in bold are only accessible with the axial ICP unit used in these studies. In addition less sensitive lines in the polyscan mode were chosen, where one can access an elemental line 2.2 nm on either side of the analytical channel provided in polychromator of the instrument. The lines chosen in the polyscan are: Pt 306.471, Ru 249.877 and Rh at 343.489 nm. For Ag and Pd the lines at 328.068 nm and 340.458 nm available with the polychromator of the ICP unit were used. A three point standardization containing the analytes in the concentration range of 0.1 to 200 μg/mL was used. The detection limits determined as per the IUPAC convention for these elements are given. The analytical range for Ag and Pd were 0.05-200 μg/mL while for other elements viz: Au, Pt, Rh and Ru it was 0.5-500 μg/mL . Synthetic samples

  19. Model calculation of the characteristic mass for convective and diffusive vapor transport in graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A combination of former convective–diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass — m0) in graphite furnace atomic absorption spectrometry (GFAAS). This approach encompasses the influence of forced convection of the internal furnace gas (mini-flow) combined with concentration diffusion of the analyte atoms on the residence time in a spatially isothermal furnace, i.e., the standard design of the transversely heated graphite atomizer (THGA). A couple of relationships for the diffusional and convectional residence times were studied and compared, including in factors accounting for the effects of the sample/platform dimension and the dosing hole. These model approaches were subsequently applied for the particular cases of Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn analytes. For the verification of the accuracy of the calculations, the experimental m0 values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm3 min−1) of the internal sheath gas during atomization. The theoretical and experimental ratios of m0(mini-flow)-to-m0(stop-flow) were closely similar for each study analyte. Likewise, the calculated m0 data gave a fairly good agreement with the corresponding experimental m0 values for stopped and mini-flow conditions, i.e., it ranged between 0.62 and 1.8 with an average of 1.05 ± 0.27. This indicates the usability of the current model calculations for checking the operation of a given GFAAS instrument and the applied methodology. - Highlights: • A calculation scheme for convective–diffusive vapor loss in GFAAS is described. • Residence time (τ) formulas were compared for sensitivity (m0) in a THGA furnace. • Effects of the sample/platform dimension and dosing hole on τ were assessed. • Theoretical m0 of 18 analytes were calculated for stopped & mini furnace gas flows. • Experimental

  20. Model calculation of the characteristic mass for convective and diffusive vapor transport in graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bencs, László, E-mail: bencs.laszlo@wigner.mta.hu [Institute for Solid State Physics and Optics, Wigner Research Centre for Physics, Hungarian Academy of Sciences, P.O. Box 49, H-1525 Budapest (Hungary); Laczai, Nikoletta [Institute for Solid State Physics and Optics, Wigner Research Centre for Physics, Hungarian Academy of Sciences, P.O. Box 49, H-1525 Budapest (Hungary); Ajtony, Zsolt [Institute of Food Science, University of West Hungary, H-9200 Mosonmagyaróvár, Lucsony utca 15–17 (Hungary)

    2015-07-01

    A combination of former convective–diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass — m{sub 0}) in graphite furnace atomic absorption spectrometry (GFAAS). This approach encompasses the influence of forced convection of the internal furnace gas (mini-flow) combined with concentration diffusion of the analyte atoms on the residence time in a spatially isothermal furnace, i.e., the standard design of the transversely heated graphite atomizer (THGA). A couple of relationships for the diffusional and convectional residence times were studied and compared, including in factors accounting for the effects of the sample/platform dimension and the dosing hole. These model approaches were subsequently applied for the particular cases of Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn analytes. For the verification of the accuracy of the calculations, the experimental m{sub 0} values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm{sup 3} min{sup −1}) of the internal sheath gas during atomization. The theoretical and experimental ratios of m{sub 0}(mini-flow)-to-m{sub 0}(stop-flow) were closely similar for each study analyte. Likewise, the calculated m{sub 0} data gave a fairly good agreement with the corresponding experimental m{sub 0} values for stopped and mini-flow conditions, i.e., it ranged between 0.62 and 1.8 with an average of 1.05 ± 0.27. This indicates the usability of the current model calculations for checking the operation of a given GFAAS instrument and the applied methodology. - Highlights: • A calculation scheme for convective–diffusive vapor loss in GFAAS is described. • Residence time (τ) formulas were compared for sensitivity (m{sub 0}) in a THGA furnace. • Effects of the sample/platform dimension and dosing hole on τ were assessed. • Theoretical m{sub 0} of 18 analytes were

  1. Direct determination of sodium, potassium, chromium and vanadium in biodiesel fuel by tungsten coil atomic emission spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •Direct analysis of biodiesel on a tungsten coil atomizer. •Determination of Na, K, Cr and V by tungsten coil atomic emission spectrometry. •Sample dilution with methanol or ethanol. •Ten-microliter sample aliquots and limits of detection between 20 and 90 μg kg−1. •Low consumption of reagents, samples and gases in a 140 s per run procedure. -- Abstract: High levels of sodium and potassium can be present in biodiesel fuel and contribute to corrosion, reduced performance and shorter engine lifetime. On the other hand, trace amounts of chromium and vanadium can increase the emission of pollutants during biodiesel combustion. Sample viscosity, immiscibility with aqueous solutions and high carbon content can compromise biodiesel analyzes. In this work, tungsten filaments extracted from microscope light bulbs are used to successively decompose biodiesel's organic matrix, and atomize and excite the analytes to determine sodium, potassium, chromium and vanadium by tungsten coil atomic emission spectrometry (WCAES). No sample preparation other than simple dilution in methanol or ethanol is required. Direct analysis of 10-μL sample aliquots using heating cycles with less than 150 s results in limits of detection (LOD) as low as 20, 70, 70 and 90 μg kg−1 for Na, K, Cr and V, respectively. The procedure's accuracy is checked by determining Na and K in a biodiesel reference sample and carrying out spike experiments for Cr and V. No statistically significant differences were observed between reference and determined values for all analytes at a 95% confidence level. The procedure was applied to three different biodiesel samples and concentrations between 6.08 and 95.6 mg kg−1 for Na and K, and between 0.22 and 0.43 mg kg−1 for V were obtained. The procedure is simple, fast and environmentally friendly. Small volumes of reagents, samples and gases are used and no residues are generated. Powers of detection are comparable to

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

    Science.gov (United States)

    Duben, Ondřej; Boušek, Jaroslav; Dědina, Jiří; Kratzer, Jan

    2015-09-01

    Atomization of selenium hydride in a quartz dielectric barrier discharge (DBD) atomizer was optimized and its performance was compared to that of the externally heated quartz multiatomizer. Argon was found as the best DBD discharge gas employing a flow rate of 75 ml min- 1 Ar while the DBD power was optimized at 14 W. The detection limits reached 0.24 ng ml- 1 Se in the DBD and 0.15 ng ml- 1 Se in the multiatomizer. The tolerance of DBD to interferences is even better than with the multiatomizer.

  3. An Analytical Model for Adsorption and Diffusion of Atoms/Ions on Graphene Surface

    Directory of Open Access Journals (Sweden)

    Yan-Zi Yu

    2015-01-01

    Full Text Available Theoretical investigations are made on adsorption and diffusion of atoms/ions on graphene surface based on an analytical continuous model. An atom/ion interacts with every carbon atom of graphene through a pairwise potential which can be approximated by the Lennard-Jones (L-J potential. Using the Fourier expansion of the interaction potential, the total interaction energy between the adsorption atom/ion and a monolayer graphene is derived. The energy-distance relationships in the normal and lateral directions for varied atoms/ions, including gold atom (Au, platinum atom (Pt, manganese ion (Mn2+, sodium ion (Na1+, and lithium-ion (Li1+, on monolayer graphene surface are analyzed. The equilibrium position and binding energy of the atoms/ions at three particular adsorption sites (hollow, bridge, and top are calculated, and the adsorption stability is discussed. The results show that H-site is the most stable adsorption site, which is in agreement with the results of other literatures. What is more, the periodic interaction energy and interaction forces of lithium-ion diffusing along specific paths on graphene surface are also obtained and analyzed. The minimum energy barrier for diffusion is calculated. The possible applications of present study include drug delivery system (DDS, atomic scale friction, rechargeable lithium-ion graphene battery, and energy storage in carbon materials.

  4. Multielement analysis of Pakistan coal by X-ray fluorescence spectrometry and inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Major, minor and trace element concentration levels are determined for 21 tertiary lignites and sub-bituminous coal samples collected from seven major coal field in Pakistan. Samples are collected as channel samples and/or run of mine samples. All samples are analysed by the x-ray fluorescence spectrometry (XRFS) technique whereas samples from Cherat coal field and the Katha-Pale coal field are analysed by the inductively coupled plasma atomic emission spectrometry (ICP-AES). Significant concentrations of toxic elements such as S, Ce, Cd, Cr, Cu, Mn, Ni, P, Pb, U and V are found in these coal samples. Thus, continuous exposure to dust of these coals (by the mine workers and inhabitants of the nearby settlements) and their extensive use of domestic purpose (cooking/heating), or in brick kilns and in combustion chambers of thermal power plants may cause significant environmental pollution problems as well as health problems. Their use in the industrial and energy sectors will further pose engineering/operational problems in items of requirements of preventive measures against corrosion of the combustion units. (author) 8 tabs

  5. Preconcentration and atomization of arsane in a dielectric barrier discharge with detection by atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-01-01

    Roč. 88, - (2016), s. 6064-6070. ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation * arsenic preconcentration Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

  6. Speciation analysis of thallium using solid phase extraction and electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. Thallium is a heavy, very toxic metallic element, which occurs in earth's crust in an estimated abundance from 0.1 to 0.8 mg.kg-1. In the environment, it is mainly combined with other elements (primarily oxygen, sulfur, halogens, potassium and rubidium) in inorganic compounds. During the weathering processes it can be mobilized by aqueous media and accumulated in sediments and soils. The main sources of pollution nowadays come from anthropogenic emissions from refineries, coal-fired power stations, mining activities, metal smelters and the cement industry. Thallium exists in natural waters as either Tl(I) (thallous) or Tl(III) (thallic) species. The oxidation state of Tl affects its complexation and subsequent bioavailability and toxicity in the environment. Thallium content in surface waters is within the range 1-82 ng l-1. Due to this low contents of Tl in water samples, it is necessary to combine the laboratory separation, preconcentration and determination techniques for the purpose of Tl speciation analysis. The scope of the presented work was to use an solid phase extraction (SPE) for the separation and preconcentration of Tl species in water samples followed by the determination using electrothermal atomic absorption spectrometry (ET AAS). In this method, Tl(III) was stabilized by formation of a Tl(III)-DTPA complex. Tl(I) species remained in its original form. These two species were then separated by using a cation exchange resin Amberlite IR120 and nitric acid as the eluent in a batch SPE protocol. The potential interferences of Fe (III), Al, Ca, Mg and other metals were investigated. The optimized experimental conditions for separation/preconcentration step (pH 2-3, time 15 min, temperature 60 deg C) and Zeeman ET AAS determination (chemical modifier Pd + ascorbic acid, atomization temperature 2100 deg C) were used for the speciation analysis of thallium in filtered acid water samples from open quartzite mine in the

  7. An Advanced Analytical Chemistry Experiment Using Gas Chromatography-Mass Spectrometry, MATLAB, and Chemometrics to Predict Biodiesel Blend Percent Composition

    Science.gov (United States)

    Pierce, Karisa M.; Schale, Stephen P.; Le, Trang M.; Larson, Joel C.

    2011-01-01

    We present a laboratory experiment for an advanced analytical chemistry course where we first focus on the chemometric technique partial least-squares (PLS) analysis applied to one-dimensional (1D) total-ion-current gas chromatography-mass spectrometry (GC-TIC) separations of biodiesel blends. Then, we focus on n-way PLS (n-PLS) applied to…

  8. Analytical and processing methodologies for non-target screening by coupling passive sampling and high resolution mass spectrometry

    OpenAIRE

    Coralie, Soulier; Anne, Togola

    2015-01-01

    Nowadays with technological advances, the use of environmental forensic approaches could help to characterize the various sources of groundwater contamination. This implies the need of specific analytical methodology to identify micropollutants, emerging substances or transformation products present at low concentrations. The high resolution mass spectrometry (HRMS) has gained increasingly in importance for monitoring organic compounds. Its high resolving power, mass accuracy and the sensitiv...

  9. Analytical and processing methodologies for non-target screening by coupling passive sampling and high resolution mass spectrometry

    OpenAIRE

    Coralie, Soulier; Anne, Togola

    2015-01-01

    International audience Nowadays with technological advances, the use of environmental forensic approaches could help to characterize the various sources of groundwater contamination. This implies the need of specific analytical methodology to identify micropollutants, emerging substances or transformation products present at low concentrations. The high resolution mass spectrometry (HRMS) has gained increasingly in importance for monitoring organic compounds. Its high resolving power, mass...

  10. Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

    Science.gov (United States)

    Goudarzi, Nasser

    2009-02-11

    A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples. PMID:19138082

  11. Electrochemical preconcentration and hydride generation methods for trace determination of selenium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The use of atomic absorption spectrometry in combination with two different preconcentration/separation techniques for the determination of trace concentrations of selenium is described. Electrochemical preconcentration onto a platinum electrode with a subsequent atomization of selenium is discussed briefly. Several parameters are considered such as the presence of depolarizers, and the temperature of the electrolyzed solutions. Special attention is payed to the efficiency of the atomization step, and a method to improve this is proposed. Applications of the technique to real samples are also reported. Secondly, the separation of the selenium as the volatile selenium hydride from the sample solution is considered. Several papers in this thesis deal with commonly occurring interferants as nickel and copper and with ways of minimizing or avoiding the interferring effects, whereas other papers relate to more theoretical aspects of the hydride generation process. New methods for the determination of selenium in technical samples with high contents of nickel and copper are also presented

  12. Simultaneous flow injection preconcentration of lead and cadmium using cloud point extraction and determination by atomic absorption spectrometry.

    Science.gov (United States)

    Silva, Edson Luiz; Roldan, Paulo Dos Santos

    2009-01-15

    A flow injection (FI) micelle-mediated separation/preconcentration procedure for the determination of lead and cadmium by flame atomic absorption spectrometry (FAAS) has been proposed. The analytes reacted with 1-(2-thiazolylazo)-2-naphthol (TAN) to form hydrophobic chelates, which were extracted into the micelles of 0.05% (w/v) Triton X-114 in a solution buffered at pH 8.4. In the preconcentration stage, the micellar solution was continuously injected into a flow system with four mini-columns packed with cotton, glass wool, or TNT compresses for phase separation. The analytes-containing micelles were eluted from the mini-columns by a stream of 3molL(-1) HCl solution and the analytes were determined by FAAS. Chemical and flow variables affecting the preconcentration of the analytes were studied. For 15mL of preconcentrated solution, the enhancement factors varied between 15.1 and 20.3, the limits of detection were approximately 4.5 and 0.75microgL(-1) for lead and cadmium, respectively. For a solution containing 100 and 10microgL(-1) of lead and cadmium, respectively, the R.S.D. values varied from 1.6 to 3.2% (n=7). The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. The method was susceptible to matrix effects, but these interferences were minimized by adding barium ions as masking agent in the sample solutions, and recoveries from spiked sample varied in the range of 95.1-107.3%. PMID:18456398

  13. Analytical chemistry

    International Nuclear Information System (INIS)

    This book is comprised of nineteen chapters, which describes introduction of analytical chemistry, experimental error and statistics, chemistry equilibrium and solubility, gravimetric analysis with mechanism of precipitation, range and calculation of the result, volume analysis on general principle, sedimentation method on types and titration curve, acid base balance, acid base titration curve, complex and firing reaction, introduction of chemical electro analysis, acid-base titration curve, electrode and potentiometry, electrolysis and conductometry, voltammetry and polarographic spectrophotometry, atomic spectrometry, solvent extraction, chromatograph and experiments.

  14. Alternative approaches to correct interferences in the determination of boron in shrimps by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The aim of this study is to propose alternative techniques and methods in combination with the classical chemical modification to correct the major matrix interferences in the determination of boron in shrimps. The performance of an internal standard (Ge) for the determination of boron by the simultaneous multi-element atomic absorption spectrometry was tested. The use of internal standardization increased the recovery from 85.9% to 101% and allowed a simple correction of errors during sampling preparation and heating process. Furthermore, a new preparation procedure based on the use of citric acid during digestion and dilution steps improved the sensitivity of the method and decreased the limit of detection. Finally, a comparative study between the simultaneous multi-element atomic absorption spectrometry with a longitudinal Zeeman-effect background correction system, equipped with a transversely-heated graphite atomizer and the single element atomic absorption spectrometry with a D2 background correction system, equipped with an end-heated graphite atomizer was undertaken to investigate the different behavior of boron in both techniques. Different chemical modifiers for the determination of boron were tested with both techniques. Ni-citric acid and Ca were the optimal chemical modifiers when simultaneous multi-element atomic absorption spectrometry and single-element atomic absorption spectrometry were used, respectively. By using the single-element atomic absorption spectrometry, the calculated characteristic mass was 220 pg and the calculated limit of detection was 370 μg/kg. On the contrary, with simultaneous multi-element atomic absorption spectrometry, the characteristic mass was 2200 pg and the limit of detection was 5.5 mg/kg. - Highlights: • New approaches were developed to cope with interferences of B determination by ETAAS • Ge was used as internal standard for the determination of B by simultaneous ETAAS • Citric acid was used during digestion

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

    Energy Technology Data Exchange (ETDEWEB)

    Karadjova, Irina B.; Petrov, Panayot K. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria); Serafimovski, Ivan [Food Institute, Faculty of Veterinary Medicine, Sts. Cyril and Methodius University, P.O. Box 95, MK-1000, Skopje (Macedonia, The Former Yugoslav Republic of); Stafilov, Trajce [Institute of Chemistry, Faculty of Science, Sts. Cyril and Methodius University, P.O. Box 162, MK-1000, Skopje (Macedonia, The Former Yugoslav Republic of); Tsalev, Dimiter L. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria)], E-mail: tsalev@chem.uni-sofia.bg

    2007-03-15

    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 deg. 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 deg. C and atomization temperature 2100 deg. C) with 1.5 {mu}g Pd as modifier on Zr-Ir treated platform. Platforms have been pre-treated with 2.7 {mu}mol of zirconium and then with 0.10 {mu}mol 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

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

    International Nuclear Information System (INIS)

    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 deg. 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 deg. C and atomization temperature 2100 deg. 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

  17. In-situ vaporization and matrix removal for the determination of rare earth impurities in zirconium dioxide by electrothermal vaporization inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    A novel method for the determination of trace rare earth impurities in ZrO2 powder has been developed based on electrothermal vaporization inductively coupled plasma atomic emission spectrometry. A polytetrafluoroethylene slurry was used as a fluorinating reagent to convert both the matrix (Zr) and the analytes (rare earth elements) into fluorides with different volatilities at a high temperature in a graphite furnace. The more volatile ZrF4 was removed in-situ by selective vaporization prior to the determination of the analytes, removing matrix spectral interferences. Under optimum operating conditions, the absolute detection limits of the analytes varied from 0.04 ng (Yb) to 0.50 ng (Pr) with relative standard deviations less than 5%. The recommended approach has been successfully applied to the determination of trace rare earth impurities (La, Pr, Eu, Gd, Ho and Yb) in ZrO2 powder and the results were in good agreement with those obtained by pneumatic nebulization inductively coupled plasma atomic emission spectrometry after the separation of the matrix using a solvent extraction procedure

  18. Determination of platinum and palladium in road dust after their separation on immobilized fungus by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Woinska, Sylwia; Godlewska-Zylkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2011-07-15

    A flow solid phase extraction procedure based on biosorption of Pt(IV) and Pd(II) on Aspergillus sp. immobilized on cellulose resin Cellex-T was proposed for the separation and preconcentration of Pt and Pd before their determination by electrothermal atomic absorption spectrometry (ETAAS). The analytical conditions including sample pH, eluent type, flow rates of sample and eluent solutions were examined. The analytes were selectively retained on the biosorbent in acidic medium (pH 1) and subsequently eluted from the column with 1 mL of thiourea solution (0.25 mol L{sup -1} thiourea in 0.3 mol L{sup -1} HCl). The reproducibility of the procedure was below 5%. The limit of detection of the method was 0.020 ng mL{sup -1} for Pt and 0.012 ng mL{sup -1} for Pd. The method validation was performed by analysis of certified reference materials BCR-723 (tunnel dust) and SARM-76 (platinum ore). The developed separation procedure was applied to the determination of Pt and Pd in road dust samples by ETAAS. The applied biosorbent is characterized by high sorption capacity: 0.47 mg g{sup -1} for Pt and 1.24 mg g{sup -1} for Pd.

  19. 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.

  20. 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

  1. Observations on the quantitation of the phosphate content of peptides by fast-atom bombardment mass spectrometry.

    Science.gov (United States)

    Poulter, L; Ang, S G; Williams, D H; Cohen, P

    1987-07-29

    Equimolar mixtures of the phosphorylated and dephosphorylated forms of several peptides have been subjected to fast-atom bombardment mass spectrometry (FABMS), to investigate whether the stoichiometry of phosphorylation can be determined from the relative molecular-ion abundances of the phospho and dephospho derivatives. It is concluded that quantitation can be achieved for peptides with large positive or negative hydrophobicity/hydrophilicity indices (delta F values) where addition of a phosphate group does not alter the distribution of the peptide within the matrix significantly. For peptides with small positive or negative delta F values, phosphopeptides tend to be partially suppressed by their dephosphorylated counterparts. Suppression can be partially or totally overcome by conversion of the peptide to a hydrophobic derivative, and by the selection of an appropriate matrix. Alternatively, addition of a very strong acid, perchloric acid, can even reverse the original suppression effect. This last effect is believed to be due to the increased ionic strength in the matrix, which forces a relatively hydrophilic analyte to the matrix surface; and the ability of such a phosphorylated analyte to form a more stable gas-phase cation. PMID:3038197

  2. Possibilities for applying gamma-spectrometry software ANGLE in isotope hydrology analytical procedures

    International Nuclear Information System (INIS)

    ANGLE software for gamma-spectrometry (semiconductor detector gamma-efficiency calculations, in particular) in its various forms has been in use for 15 years in numerous gamma-spectrometry laboratories all around. ANGLE is basically a semi-empirical model for efficiency calculations, which combines the advantages of both absolute and relative approach, while attempting to minimize their drawbacks. The physical model behind is the concept of the effective solid angle, which is calculated upon the input data on the geometrical and physical characteristics of (1) the source (including the container vessel), (2) the detector and (3) the counting arrangement (including intercepting layers between the latter two). It was shown earlier that only the simultaneous differential treatment of gamma-attenuation, geometry and detector response, as in ANGLE, is essentially justified for this type of calculations. The program can be applied to practically all counting situations encountered in laboratory practice: point, disc, cylindrical or Marinelli sources and any matrix composition. No standards are required, but a so called 'reference efficiency curve' should be obtained ('once for ever') by measuring a set of calibrated point sources. As a summary, ANGLE is characterized by (1) a very broad application range, (2) satisfactory accuracy (of the order of a few percent), (3) easy data manipulation (under WINDOWS), (4) short computation times, (5) flexibility in respect with input parameters and (6) suitability for didactical purposes. Possibilities for applying ANGLE in isotope hydrology analytical procedures (e.g. with radioactive tracers involved), are discussed. Tracer techniques are of particular interest for water resources management in Mediterranean karstic regions, typically abundant with precipitation in winter, but scarce with ground waters in summer - like is the case with east coast of Adriatic, including the coastal part of Montenegro. (author)

  3. The determination of caesium and silver in soil and fungal fruiting bodies by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Methods have been developed for the determination of caesium and silver in soil and fungal samples by microwave-assisted aqua regia digestion, followed by electrothermal atomic absorption spectrometry. The procedure was found to be repeatable (for soil, RSD -1, respectively, and for fungi, RSD -1, respectively) and reasonably efficient. Silver was recovered quantitatively from reference soils, but only about 80-85% of the caesium present could be extracted. Poorer caesium recoveries (< 70%) were obtained if, as part of the sample preparation procedure, solutions were taken to dryness in glass beakers prior to analysis. The detection limits were 0.02 mg Ag and 0.09 mg Cs per gram of dry soil, which are adequate for the determination of the analytes at typical environmental levels. The methods were applied in the analysis of three types of soil, a peaty podzol, a clay loam and a sandy loam and no significant matrix interferences were observed except in the determination of caesium in the sandy loam. For caesium, non-linear response curves, thought to be due to ionisation interference, were encountered using one atomic absorption spectrometer, but were not observed with the other instrument

  4. Improvements in cobalt determination by thermospray flame furnace atomic absorption spectrometry using an on-line derivatization strategy.

    Science.gov (United States)

    Matos, Geraldo Domingues; Arruda, Marco Aurélio Zezzi

    2008-07-15

    An on-line derivatization strategy was developed for improving cobalt sensitivity using thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) as the analytical technique. This strategy involves the generation of a volatile cobalt compound, providing better sample vaporization efficiency. The effect of sodium diethyldithiocarbamate (DDTC) as complexing agent on the integrated absorbance signal was evaluated. Parameters including the pH of complex formation, complex concentration and volume, sample volume, flame gas composition and tube atomization configuration were optimized. A wide linear range (from 23 microg L(-1) to 3 mg L(-1); r(2)=0.9786) was obtained, with the best one (r(2)=0.9992) attained from 23 to 400 microg L(-1) with a sample throughput of 30 h(-1). The improvement in the detection power was 17-fold when compared to FAAS, which provides 7 microg L(-1) as the limit of detection when considered TS-FF-AAS technique. A relative standard deviation (n=10) of 4% for a cobalt solution containing 50 microg L(-1) was attained, and the accuracy of the procedure was evaluated through certified reference materials (IAEA-SL-1, lake sediment; and ISS-MURST-A1, Antarctic marine sediment). Good agreement between the results at the 95% confidence level was observed. PMID:18585309

  5. Trapping and diffusion of noble gas atoms in some off-stoichiometric ceramics studied by thermal desorption spectrometry. Doctoral thesis

    Energy Technology Data Exchange (ETDEWEB)

    Hoondert, W.H.B.

    1993-01-01

    The thesis deals with the mobility of small noble gas atoms, mainly helium, in ceramic materials with high defect concentrations. Hence, two subjects are covered: diffusion and defect physics. The experimental technique employed is Thermal Desorption Spectrometry (TDS). An introductory outline of TDS is given. The present study was initiated for various reasons. First of all, research on helium retention and mobility behavior, such as bubble nucleation and subsequent bubble migration, in potential fusion reactor wall materials (which some of the ceramics are) is of practical interest. Secondly, because the ceramic materials investigated in the present work have defect concentrations on the order of percents, and because they are binary compounds where in principle more defect types can be present than in pure materials, the defect physics is more complicated and diverse than e.g., in simple metals. Finally, high defective materials can serve as a model system for thin films produced by Ion Beam Assisted Deposition (IBAD). TDS as an analytical tool is of key importance to be able to control the IBAD process, and for the understanding of the atomic-scale phenomena involved.

  6. Determination of bismuth in environmental samples by slurry sampling graphite furnace atomic absorption spectrometry using combined chemical modifiers.

    Science.gov (United States)

    Dobrowolski, Ryszard; Dobrzyńska, Joanna; Gawrońska, Barbara

    2015-01-01

    Slurry sampling graphite furnace atomic absorption spectrometry technique was applied for the determination of Bi in environmental samples. The study focused on the effect of Zr, Ti, Nb and W carbides, as permanent modifiers, on the Bi signal. Because of its highest thermal and chemical stability and ability to substantially increase Bi signal, NbC was chosen as the most effective modifier. The temperature programme applied for Bi determination was optimized based on the pyrolysis and atomization curves obtained for slurries prepared from certified reference materials (CRMs) of the soil and sediments. To overcome interferences caused by sulfur compounds, Ba(NO₃)₂ was used as a chemical modifier. Calibration was performed using the aqueous standard solutions. The analysis of the CRMs confirmed the reliability of the proposed analytical method. The characteristic mass for Bi was determined to be 16 pg with the detection limit of 50 ng/g for the optimized procedure at the 5% (w/v) slurry concentration. PMID:25384374

  7. Plasma jet desorption atomization-atomic fluorescence spectrometry and its application to mercury speciation by coupling with thin layer chromatography.

    Science.gov (United States)

    Liu, Zhifu; Zhu, Zhenli; Zheng, Hongtao; Hu, Shenghong

    2012-12-01

    A novel plasma jet desorption atomization (PJDA) source was developed for atomic fluorescence spectrometry (AFS) and coupled on line with thin layer chromatography (TLC) for mercury speciation. An argon dielectric barrier discharge plasma jet, which is generated inside a 300 μm quartz capillary, interacts directly with the sample being analyzed and is found to desorb and atomize surface mercury species rapidly. The effectiveness of this PJDA surface sampling technique was demonstrated by measuring AFS signals of inorganic Hg(2+), methylmercury (MeHg), and phenylmercury (PhHg) deposited directly on TLC plate. The detection limits of the proposed PJDA-AFS method for inorganic Hg(2+), MeHg, and PhHg were 0.51, 0.29, and 0.34 pg, respectively, and repeatability was 4.7%, 2.2%, and 4.3% for 10 pg Hg(2+), MeHg, and PhHg. The proposed PJDA-AFS was also successfully coupled to TLC for mercury speciation. Under optimized conditions, the measurements of mercury dithizonate (Hg-D), methylmercury dithizonate (MeHg-D), and phenylmercury dithizonate (PhHg-D) could be achieved within 3 min with detection limits as low as 8.7 pg. The combination of TLC with PJDA-AFS provides a simple, cost-effective, relatively high-throughput way for mercury speciation. PMID:23153091

  8. 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

    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) are...

  9. 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) are...

  10. Analytic solution and pulse area theorem for three-level atoms

    Science.gov (United States)

    Shchedrin, Gavriil; O'Brien, Chris; Rostovtsev, Yuri; Scully, Marlan O.

    2015-12-01

    We report an analytic solution for a three-level atom driven by arbitrary time-dependent electromagnetic pulses. In particular, we consider far-detuned driving pulses and show an excellent match between our analytic result and the numerical simulations. We use our solution to derive a pulse area theorem for three-level V and Λ systems without making the rotating wave approximation. Formulated as an energy conservation law, this pulse area theorem can be used to understand pulse propagation through three-level media.

  11. Determination of the elemental composition of cyanobacteria cells and cell fractions by atomic emission and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    An approach to studying the elemental composition of cyanobacteria Spirulina platensis and Nostoc commune using a set of complementary analytical methods (ICP-AES, PAAS, and ETAAS) was proposed . The procedures were adapted for the determination of macro- and microelements (Na, K, Mg, Ca, Fe, Mn, Cu, Mo, Zn, B, and Se) in the biomass of cyanobacteria and separated cell fractions (chloroform and water-methanol extracts and precipitates). The conditions for the mineralization of biological materials were optimized for autoclave and microwave sample preparation procedures. The evaporation and atomization of Se and Mo in a graphite furnace in the presence of chloroform and methanol were studied

  12. Self-interstitial configuration in molybdenum studied by modified analytical embedded atom method

    Indian Academy of Sciences (India)

    Jian-Min Zhang; Zhang Fang Wang; Ke-Wei Xu

    2009-05-01

    The stability of various atomic configurations containing a self-interstitial atom (SIA) in a model representing Mo has been investigated using the modified analytical embedded atom method (MAEAM). The lattice relaxations are treated with the molecular dynamics (MD) simulation at absolute zero of temperature. Six relatively stable self-interstitial configurations and formation energies have been described and calculated. The results indicate that the [1 1 1] dumbbell interstitial S111 has the lowest formation energy, and in ascending order, the sequence of the configurations is predicted to be S111, C, S110, T, S001 and O. From relaxed displacement field up to the fifth-NN atoms of six configurations, we know that the relaxed displacements depend not only on separation distances of the NN atoms from the defect centre but also strongly on the direction of the connected line between the NN atoms and the defect centre. The equilibrium distances between two nearest atoms in the core of the S111, C, S110, T, S001 and O configurations are 0.72a, 0.72a, 0.71a, 0.72a, 0.70a and 0.70a, respectively.

  13. Fourier transform ion cyclotron resonance mass spectrometry: the analytical tool for heavy oil and bitumen characterization

    Energy Technology Data Exchange (ETDEWEB)

    Oldenburg, Thomas B.P; Brown, Melisa; Hsieh, Ben; Larter, Steve [Petroleum Reservoir Group (prg), Department of Geoscience, University of Calgary, Alberta (Canada)

    2011-07-01

    The Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FTICRMS), developed in the 1970's by Marshall and Comisarow at the University of British Columbia, has become a commercially available tool capable of analyzing several hundred thousand components in a petroleum mixture at once. This analytical technology will probably usher a dramatic revolution in geochemical capability, equal to or greater than the molecular revolution that occurred when GCMS technologies became cheaply available. The molecular resolution and information content given by the FTICRMS petroleum analysis can be compared to the information in the human genome. With current GCMS-based petroleum geochemical protocols perhaps a few hundred components can be quantitatively determined, but with FTICRMS, 1000 times this number of components could possibly be resolved. However, fluid and other properties depend on interaction of this multitude of hydrocarbon and non-hydrocarbon components, not the components themselves, and access to the full potential of this new petroleomics will depend on the definition of this interactome.

  14. Direct determination of selenium in rat blood plasma by Zeeman atomic absorption spectrometry.

    Science.gov (United States)

    Kabirov, K K; Kapetanovic, I M; Lyubimov, A V

    2008-01-30

    The method was developed to be applied for direct determination of selenium in rat plasma by graphite-furnace atomic absorption spectrometry with Zeeman background correction. Blood was obtained from CD rats of both sexes 2h after dosing in weeks 7 and 13 in order to acquire data on the levels of selenium in these animals during 13-week gavage administration of l-seleno-methylselenocysteine (SeMC), a new candidate chemopreventive agent under development. Application of the commonly used method of standard addition was found to be unsuitable to calculate the selenium content in rat plasma (within-run and between-run accuracy and precision parameters were less than 85%). Therefore, a new analytical method was developed. In this method, samples of rat plasma (50 microL) were diluted 10-fold with a reducing agent containing l-ascorbic acid, a modifier solution containing palladium chloride and Triton X-100. Samples were atomized in pyrolytically coated graphite tubes and peak height signals were measured. Selenium concentrations were determined by linear least squares regression analysis based on the standard curve generated in pooled rat blank plasma. Since selenium is normally present in plasma, a three-step approach was used to calculate selenium plasma levels. Initially selenium levels were determined based on the standard curve with selenium-spiked pool plasma. In the second step, background selenium levels in the pooled plasma were determined based on the same standard curve. In the third step, background level was added to the previously derived number. The relative errors were in the range from -4.6 to 11.4% (intra-day assay) and from -0.4 to 8.8% (inter-day assay) which proved good accuracy. The relative standard deviations were in the range from 1.88 to 4.70% (intra-day precision) and from 3.28 to 5.38% (inter-day precision). In rat plasma, the following dose-dependent selenium levels (mean+/-S.D.) in males and females, respectively, were observed at 13 weeks

  15. Inductively coupled plasma-atomic emission spectrometry (ICP-AES) in support of nuclear waste management

    International Nuclear Information System (INIS)

    Simulated complex nuclear waste solutions are characterized by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AEC). The system uses and ICP source focused on both a polychromator and a computer-controlled scanning monochromator for intensity measurements. This instrumentation allows for simultaneous and sequential measurements of liquid extraction distribution coefficients needed in the development of process flow sheets for component separations. A large number of elements are determined rapidly with adequate sensitivity and accuracy. The focus of this investigation centers on the analysis of nuclear fission products. 13 references, 13 tables

  16. Analysis of atmospheric aerosols by atomic emission spectrometry with electrical discharge sampling

    International Nuclear Information System (INIS)

    A procedure is developed for the determination of the concentration of heavy metals (Pb, Mn, Cu, Ni, Zn, and Cd) in atmospheric air by atomic emission spectrometry with gas-discharge sampling onto the end of a standard carbon electrode. A design of a two-section sampler is proposed; the sampler provides the rapid determination of deposition factors for the deposition of heavy metals contained in aerosol particles onto the end of a carbon electrode. Examples of determining metal concentrations in a model sample of air and in atmospheric air and determination limits of metals deposited onto the end of a carbon electrode are given

  17. Chloride isolation for accelerator mass spectrometry of 36Cl produced by atomic bomb neutrons

    International Nuclear Information System (INIS)

    Accelerator mass spectrometry was performed at the Munich tandem laboratory to determine the ratio of 36Cl/Cl in silicate rock samples exposed to neutrons of the Hiroshima atomic bomb. Chloride was chemically separated from silicate rock for this purpose. Five grams of silicate rock was fused with 30 g of sodium hydroxide and dissolved in 900 ml of water. The chloride in the resulting solution was spectrophotometrically determined. Chloride was precipitated as silver chloride by addition of appropriate amounts of silver nitrate, and silver chloride was then collected on a membrane filter. The chloride in the rock samples was thus isolated quantitatively. (author)

  18. 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.

  19. Speciation of organometallic compounds by Zeeman atomic absorption spectrometry with liquid chromatography

    International Nuclear Information System (INIS)

    A method for the determination of organometallic compounds in the ppB range includes separation of the desired species with a high pressure liquid chromatograph and determination of the trace element by Zeeman atomic absorption spectrometry. The analysis of a mixture of vitamin B12 and Co(NO3)2 is described as a demonstration of the method. Determination of many enzymes and coenzymes having a metal ion in their functional center and of many toxic metals in environmental samples are other fields for application of this method

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

    International Nuclear Information System (INIS)

    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

  1. 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.)

  2. 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.

  3. Evaluation of the temporal profiles and the analytical features of a laser ablation - Pulsed glow discharge coupling for optical emission spectrometry

    Science.gov (United States)

    González de Vega, Claudia; Bordel, Nerea; Pereiro, Rosario; Sanz-Medel, Alfredo

    2016-07-01

    The coupling of a glow discharge (GD) in pulsed mode (PGD) as secondary source for excitation/ionization of the material provided by laser ablation (LA) has been investigated using optical emission spectrometry (OES). The variation of the laser pulse delay with respect to the GD pulse allows to producing the ablation process during prepeak, plateau or afterglow GD regions. Emission properties of the LA-PGD plasma in each temporal region of the GD pulse have been evaluated for analytical lines of different elements. Resonant atomic lines have shown higher emission intensity in the prepeak region compared to non-resonant lines. Non-resonant lines showed higher enhancement of the emission intensity in the afterglow region. Moreover, the coupled LA-PGD system offered better linear correlation coefficients using a set of glass standards for calibration as well as lower detection limits (by at least a factor of two) when compared to laser induced breakdown spectroscopy.

  4. Optimization of trace molybdenum content determination in human nails by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The accurate determination of molybdenum (Mo) in biological materials is of considerable importance in medical science because of the essential role played by this element in human metabolism. Molybdenum is a component of enzymes responsible for the initial stages of nitrogen, carbon and sulfur metabolism of plants, animals and humans. This element is usually determined by neutron activation analysis (NAA) in variety of samples, but direct measurement of low levels of molybdenum in biological samples by NAA is difficult. Recently instrumental analysis procedures such as atomic absorption spectrometry (AAS) have been used in clinical measurements for determination of many trace elements in the biological samples. These techniques are much simpler and cheaper than NAA. In this paper we are reporting a method of sample preparation for determining molybdenum by using graphite furnace atomic absorption spectrometry (GF-AAS). This method is the most readily available technique for determination of molybdenum at the ng/g level in biological samples. It can be used for the routine hospital laboratory determination of molybdenum and has appropriate sensitivity and simplicity. The best and reliable results for molybdenum analysis was achieved by digestion of nails in HNO3 2 N and was determined in the range from 0.11 to 5.10 μg/g

  5. Determination of trace elements in ground water by two preconcentration methods using atomic absorption spectrometry

    International Nuclear Information System (INIS)

    This is a comparative study between two different methods of preconcentration done to separate the trace elements cadmium, nickel. chromium, manganese, copper, zinc, and lead in drinking (ground) water samples taken from different locations in Gezira State, central Sudan (the map); these methods are (coprecipitation) with aluminium hydroxide and by Ammonium Pyrrolidine Dithiocarbamate (APDC) using Methyl Isobutyl Ketone (MIBK) as an organic solvent; and subsequent analysis by Atomic Absorption Spectrometry (AAS) for both methods. The result of comparison showed the superiority of the (APDC) coprecipitation method over the aluminium hydroxide coprecipitation method in the total percentage recoveries of the studied trace elements in drinking (ground) water samples, such results confirm previous studies. This study also involves direct analysis of these water samples by atomic absorption spectrometry to determine the concentrations of trace elements Cadmium, Nickel, Chromium, Manganese, Copper, Zinc and Lead and compare it to the corresponding guide line values described by the World Health Organization and the maximum concentrations of trace elements in drinking water permitted by the Sudanese Standards and Metrology Organizations (SSMO), where the concentrations of some elements in some samples were found to be different than the described values by both of the organizations. The study includes a trial to throw light on the effect of the proximity of the water samples sources to the Blue Nile river on its trace elements concentrations; no relation was proved to exist in that respect.(Author)

  6. Determination of Elements by Atomic Absorption Spectrometry in Medicinal Plants Employed to Alleviate Common Cold Symptoms

    Institute of Scientific and Technical Information of China (English)

    F Zehra Küçükbay; Ebru Kuyumcu

    2014-01-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of com-mon cold have been studied for their mineral contents .Eleven minor and major elements (essential ,non-essen-tial and toxic) were identified in the Asplenium adiantum-nigrum L .,Althaea of ficinalis L .,Verbascum phlomoides L .,Euphorbiachamaesyce L .,Zizyphus jujube Miller ,Peganum harmala L .,Arum dioscori-dis Sm .,Sambucus nigra L .,Piper longum L .,Tussilago farfara L .and Elettariacardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrom-etry .Microwave digestion procedure for total concentration was applied under optimized conditions for dissolu-tion 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 .

  7. Simultaneous determination of iron and nickel in fluoropolymers by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Soares, Bruno M; Santos, Rafael F; Bolzan, Rodrigo C; Muller, Edson I; Primel, Ednei G; Duarte, Fabio A

    2016-11-01

    This paper reports the development of a method of simultaneous determination of iron and nickel in fluoropolymers by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with direct solid sampling. In order to carry out simultaneous measurements, both the main resonance line of nickel (232.003nm) and the adjacent secondary line of iron (232.036nm) were monitored in the same spectral window. The proposed method was optimized with a perfluoroalkoxy (PFA) sample and was applied to the determination of iron and nickel in fluorinated ethylene propylene (FEP) and modified polytetrafluoroethylene (PTFE-TFM) samples. Pyrolysis and atomization temperatures, as well as the use of Pd and H2 (during pyrolysis) as chemical modifiers, were carefully investigated. Compromise temperatures for pyrolysis and atomization of both analytes were achieved at 800 and 2300°C, respectively, using only 0.5Lmin(-1) H2 as chemical modifier during pyrolysis. Calibration curves were performed with aqueous standards by using a single solution which contained both analytes. Limits of detection were 221 and 9.6ngg(-1) for iron and nickel, respectively. Analyte concentrations in all samples ranged from 3.53 to 12.4µgg(-1) for iron and from 37 to 78ngg(-1) for nickel, with relative standard deviation less than 19%. Accuracy was evaluated by comparing these results with those obtained by inductively coupled plasma mass spectrometry after sample digestion by microwave-induced combustion and no significant statistical difference was observed. PMID:27591638

  8. Direct determination of Cr and Cu in urine samples by electrothermal atomic absorption spectrometry using ruthenium as permanent modifier (R1)

    Energy Technology Data Exchange (ETDEWEB)

    Lelis, Katia Linces Alves; Rocha, Clelia Aparecida [Instituto de Patologia Clinica Hermes Pardini, 30140-070 Belo Horizonte, MG (Brazil); Magalhaes, Cristina Goncalves; Silva, Jose Bento Borba of [Departamento de Quimica, Universidade Federal de Minas Gerais, 31270-901 Belo Horizonte, MG (Brazil)

    2002-12-01

    In this study Ru, deposited thermally on an integrated platform pyrolytic graphite tube, is proposed as a permanent modifier for the determination of Cu and Cr in urine samples by electrothermal atomic absorption spectrometry. The samples were diluted 1:1 with nitric acid (1% v/v). Pyrolysis and atomization temperatures for spiked urine samples were 1,100 C and 1,900 C respectively for Cu, and 1,400 C and 2,500 C respectively for Cr. For comparison purposes, the conventional modification with Pd+Mg was also studied. The sensitivity for Ru as permanent modifier was higher for the two analytes. The characteristic masses were 7.3 and 17.7 for Cr and Cu. The detection limits (3{sigma}) were 0.22 and 0.32 {mu}g/L, for Cr and Cu, respectively. Good agreement was obtained with certified urine samples for the two elements. (orig.)

  9. Phonon dispersion on Ag (100) surface: A modified analytic embedded atom method study

    Science.gov (United States)

    Xiao-Jun, Zhang; Chang-Le, Chen

    2016-01-01

    Within the harmonic approximation, the analytic expression of the dynamical matrix is derived based on the modified analytic embedded atom method (MAEAM) and the dynamics theory of surface lattice. The surface phonon dispersions along three major symmetry directions , and X¯M¯ are calculated for the clean Ag (100) surface by using our derived formulas. We then discuss the polarization and localization of surface modes at points X¯ and M¯ by plotting the squared polarization vectors as a function of the layer index. The phonon frequencies of the surface modes calculated by MAEAM are compared with the available experimental and other theoretical data. It is found that the present results are generally in agreement with the referenced experimental or theoretical results, with a maximum deviation of 10.4%. The agreement shows that the modified analytic embedded atom method is a reasonable many-body potential model to quickly describe the surface lattice vibration. It also lays a significant foundation for studying the surface lattice vibration in other metals. Project supported by the National Natural Science Foundation of China (Grant Nos. 61471301 and 61078057), the Scientific Research Program Funded by Shaanxi Provincial Education Department, China (Grant No. 14JK1301), and the Specialized Research Fund for the Doctoral Program of Higher Education, China (Grant No. 20126102110045).

  10. Hydride generation in-atomizer collection atomic absorption spectrometry for the determination of antimony in acetic acid leachates from pewter cups

    Czech Academy of Sciences Publication Activity Database

    Dessuy, M. B.; Kratzer, Jan; Vale, M. G. R.; Welz, B.; Dědina, Jiří

    2011-01-01

    Roč. 87, - (2011), s. 255-261. ISSN 0039-9140 R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : in-atomizer trapping * in-atomizer trapping * tin interference Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.794, year: 2011

  11. 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. PMID:26946014

  12. Determination of toxic elements in different brands of cigarette by atomic absorption spectrometry using ultrasonic assisted acid digestion.

    Science.gov (United States)

    Kazi, Tasneem Gul; Jalbani, Nusrat; Arain, Muhammad Balal; Jamali, Muhammad Khan; Afridi, Hassan Imran; Shah, Abdul Qadir

    2009-07-01

    In this paper, a sample preparation method based on ultrasonic assisted acid extraction (UAE) of Al, As, Cd, Ni and Pb from filler tobacco (FT) of different local branded (LBCs) and imported branded cigarettes (IBCs) consumed in Pakistan. Acid extracts obtained upon sonication were determined by atomic absorption spectrometry. Parameters influencing extraction such as pre-sonication time 10-15 min, sonication time 2-10 min, mass of sample 0.1-0.5 g, particle size VTL-2), and also applied a conventional acid digestion method (CDM) on same CRM, for comparative purpose. The average relative standard deviation of UAE method of CRM, ranged as 1.64-8.42% for N = 6, depending on the analytes. Extraction efficiencies for CRM were close to 97.1, 97.5, 98.5, 97.8 and 96.7 for Al, As, Cd, Ni and Pb, respectively. The concentrations of Al, As, Cd, Ni and Pb in cigarettes were present in all branded cigarettes, there is no any significance difference among LBCs and IBCs, except in few cases of LBCs, have high level of Cd and Al. Our results were compared with other worldwide studies. PMID:18600465

  13. Slurry sampling for the determination of thallium in soils and sediments by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dobrowolski, R. [Analytical Laboratory, Faculty of Chemistry, Maria Curie-Sklodowska University, M.C. Sklodowska Sq.3, 20-031 Lublin (Poland)

    2002-12-01

    The analytical conditions for thallium determination in soils and sediments by slurry sampling graphite furnace atomic absorption spectrometry were studied and optimized. Elimination of a strong background for soils rich in organic materials by application of tungsten carbides coated graphite tubes/platforms was studied in detail. Tungsten carbides increased the maximum permissible pyrolysis temperature from 300 to 900 C. The mechanism of tungsten carbide formation on different graphite surfaces was proposed. Application of a strong basic anion-exchange resin for interference elimination in thallium determination in marine sediments was described. Calibration was performed directly using aqueous standards both for soil and sediment analysis. Analysis of CRM confirmed the reliability of the approach. The precision and accuracy of thallium determination by the described method for soils and sediments was acceptable. A characteristic mass of 13.8 pg was obtained and the limit of detection for the proposed method was around 0.06 {mu}g g{sup -1} Tl. (orig.)

  14. Unusual calibration curves observed for iron using high-resolution continuum source graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The simultaneous determination of cadmium and iron in plant and soil samples has been investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry. The primary cadmium resonance line at 228.802 nm and an adjacent secondary iron line at 228.726 nm, which is within the spectral interval covered by the charge-coupled device (CCD) array detector, have been used for the investigations. Due to the very high iron content in most of the soil samples the possibility has been investigated to reduce the sensitivity and extend the working range by using side pixels for measurement at the line wings instead of the line core. It has been found that the calibration curves measured at all the analytically useful pixels of this line consisted of two linear parts with distinctly different slopes. This effect has been independent of the positioning of the wavelength, i.e., if the Cd line or the Fe line was in the center of the CCD array. The most likely explanation for this unusual behavior is a significant difference between the instrument width ΔλInstr and the absorption line width ΔλAbs, which is quite pronounced in the case of Fe. Using both parts of the calibration curves and simultaneous measurement at the line center and at the wings made it possible to extend the working range for the iron determination to more than three orders of magnitude.

  15. Microwave digestion of sludge, soil and sediment samples for metal analysis by inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Three digestion programs for the Anton Paar multiwave microwave were investigated to obtain a simple, rapid method for the determination of metals in sludge, soil and sediment samples. The digests were subsequently analysed for metal content by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The trace metals determined were Mn, Ni, Zn, Pb, Cr, Cd, Cu and V, and the major elements determined were Mg, Ca, Fe and Al. In addition to the heating programs used, different combinations and volumes of hydrofluoric, nitric and hydrochloric acids were evaluated for digestion efficiency. Three standard reference materials (SRMs) were used in the comparison. From the results obtained, the fastest microwave program (36 min) provided the most consistent recovery data for all three SRMs. Six millilitres of HNO3 was the optimum acid mixture for the digestion of LGC6136 sewage sludge (with the exception of Al) and for LGC6138 coal carbonisation site soil. For PACS-1 marine sediment (and for the determination of Al in LGC6136), a mixture of 3 ml of HNO3+2 ml of HF produced the best analytical results. The experimental results were in agreement with the certified values and demonstrated that the proposed method was precise and accurate

  16. Determination of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid in cereals by hydride generation atomic fluorescence spectrometry

    Science.gov (United States)

    Matos Reyes, M. N.; Cervera, M. L.; Campos, R. C.; de la Guardia, M.

    2007-09-01

    A fast, sensitive and simple non-chromatographic analytical method was developed for the speciation analysis of toxic arsenic species in cereal samples, namely rice and wheat semolina. An ultrasound-assisted extraction of the toxic arsenic species was performed with 1 mol L - 1 H 3PO 4 and 0.1% (m/v) Triton XT-114. After extraction, As(III), As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) concentrations were determined by hydride generation atomic fluorescence spectrometry using a series of proportional equations corresponding to four different experimental reduction conditions. The detection limits of the method were 1.3, 0.9, 1.5 and 0.6 ng g - 1 for As(III), As(V), DMA and MMA, respectively, expressed in terms of sample dry weight. Recoveries were always greater than 90%, and no species interconversion occurred. The speciation analysis of a rice flour reference material certified for total arsenic led to coherent results, which were also in agreement with other speciation studies made on the same certified reference material.

  17. Permanent modification in electrothermal atomic absorption spectrometry — advances, anticipations and reality

    Science.gov (United States)

    Tsalev, Dimiter L.; Slaveykova, Vera I.; Lampugnani, Leonardo; D'Ulivo, Alessandro; Georgieva, Rositsa

    2000-05-01

    Permanent modification is an important recent development in chemical modification techniques which is promising in view of increasing sample throughput with 'fast' programs, reducing reagent blanks, preliminary elimination of unwanted modifier components, compatibility with on-line and in situ enrichment, etc. An overview of this approach based on the authors' recent research and scarce literature data is given, revealing both success and failure in studies with permanently modified surfaces (carbides, non-volatile noble metals, noble metals on carbide coatings, etc.), as demonstrated in examples of direct electrothermal atomic absorption spectrometric (ETAAS) applications to biological and environmental matrices and vapor generation (VG)-ETAAS coupling with in-atomizer trapping of hydrides and other analyte vapors. Permanent modifiers exhibit certain drawbacks and limitations such as: poorly reproducible treatment technologies — eventually resulting in poor tube-to-tube repeatability and double or multiple peaks; impaired efficiency compared with modifier addition to each sample aliquot; relatively short lifetimes; limitations imposed on temperature programs, the pyrolysis, atomization and cleaning temperatures being set somewhat lower to avoid excessive loss of modifier; applicability to relatively simple sample solutions rather than to high-salt matrices and acidic digests; side effects of overstabilization, etc. The most important niches of application appear to be the utilization of permanently modified surfaces in coupled VG-ETAAS techniques, analysis of organic solvents and extracts, concentrates and fractions obtained after enrichment and/or speciation separations and direct ETAAS determinations of highly volatile analytes in relatively simple sample matrices.

  18. Direct determination of lead in sweet fruit-flavored powder drinks by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Lima, Éder C.; Krug, Francisco José; Arruda, Marco A. Z.

    1998-04-01

    A simplified method for direct determination of lead in sweet fruit-flavored powder drinks, syrups and honeys by electrothermal atomic absorption spectrometry without sample digestion is proposed. Samples were dissolved in water, acidified to 0.2% (v/v) HNO 3, and directly injected into an end-capped transversely heated graphite atomizer (THGA). Building up of carbonaceous residue inside the atomizer was effectively precluded for sugar solutions not exceeding 8.0% (m/v) when a heating program with two pyrolysis steps (600 and 1000°C) was carried out without air-ashing. Under these conditions one atomizer supported about 250 firings. Among various chemical modifiers tested, better recovery and repeatability results were obtained with a 5 μg Pd + 3 μg Mg(NO 3) 2 mixture. Tests carried out with individual concomitants containing up to 1.0 μg Na, K, Ca or Cl, and up to 10.0 μg phosphate or sulphate, and several mixtures of these six concomitants, did not reveal significant interferences on lead atomization. Characteristic mass and detection limit based on integrated absorbance were 15 and 11 pg Pb, respectively. The relative standard deviation based on 10 measurements for typical samples (20-60 ng g -1 Pb) was always lower than 5.5%. The detection limit of 7.0 ng g -1 Pb attained the Codex recommendation for the maximum allowed lead contents in the sugar samples. Application of t-test to the results obtained by the proposed direct analysis, and the official method adopted by Food Chemical Codex, demonstrated that there were no significant differences at the 5% probability level.

  19. Comparative oxidation state specific analysis of arsenic species by high-performance liquid chromatography- inductively coupled plasma-mass spectrometry and hydride generation-cryotrapping-atomic absorption spectrometry

    OpenAIRE

    Currier, J. M.; Saunders, R J; Ding, L.; Bodnar, W.; Cable, P.; Matoušek, T. (Tomáš); Creed, J. T.; Stýblo, M.

    2013-01-01

    The formation of methylarsonous acid (MAsIII) and dimethylarsinous acid (DMAsIII) in the course of inorganic arsenic (iAs) metabolism plays an important role in the adverse effects of chronic exposure to iAs. High-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) and hydride generation-cryotrapping-atomic absorption spectrometry (HG-CT-AAS) have been frequently used for the analysis of MAsIII and DMAsIII in biological samples. While HG-CT-AAS has con...

  20. Determination of Cd, Pb and As in sediments of the Sava River by electrothermal atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    SIMONA MURKO

    2010-01-01

    Full Text Available The applicability of nitric acid, palladium nitrate and a mixture of palladium and magnesium nitrate as matrix modifiers were estimated for the accurate and reproducible determination of cadmium (Cd, lead (Pb and arsenic (As in sediments of the Sava River by electrothermal atomic absorption spectrometry, ETAAS. Decomposition of the samples was done in a closed vessel microwave-assisted digestion system using nitric, hydrochloric and hydrofluoric acids, followed by the addition of boric acid to convert the fluorides into soluble complexes. The parameters for the determination of Cd, Pb and As in sediments were optimised for each individual element and for each matrix modifier. In addition, two sediment reference materials were also analysed. In determination of Cd and Pb, nitric acid was found to be the most appropriate matrix modifier. The accurate and reliable determination of Cd and Pb in sediments was possible also in the presence of boric acid. The use of a mixture of palladium and magnesium nitrate efficiently compensated for matrix effects and enabled the accurate and reliable determination of As in the sediments. Quantification of Cd and As was performed by calibration using acid matched standard solutions, while the standard addition method was applied for the quantification of Pb. The repeatability of the analytical procedure for the determination of Cd, Pb and As in sediments was ±5 % for Cd, ±4 % for Pb and ±2 % for As. The LOD values of the analytical procedure were found to be 0.05 mg/kg for Cd and 0.25 mg/kg for Pb and As, while the LOQ values were 0.16 mg/kg for Cd and 0.83 mg/kg for Pb and As. Finally, Cd, Pb and As were successfully determined in sediments of the Sava River in Slovenia.

  1. Analytical estimation of the gravitational constant with atomic and nuclear physical constants

    International Nuclear Information System (INIS)

    If NA represents the Avogadro's number, gravitational constant associated with atomic electromagnetic interaction can be expressed as GE ≅ N2AG. With GE and with the assumed two new pseudo numbers x ≈ 38.725 and y ≈ 47.415, value of G can be fixed for 10 digits in a verifiable approach. (x, y) can be called as the back ground analytical numbers using by which micro-macro physical constants can be interlinked qualitatively and quantitatively

  2. EVALUATION OF CORROSION OF ENGINEERING CERAMICS BY ATOMIC EMISSION SPECTROMETRY IN INDUCTIVELY COUPLED PLASMA

    OpenAIRE

    DAGMAR GALUSKOVÁ; DUŠAN GALUSEK; PAVOL ŠAJGALÍK

    2014-01-01

    An analytical method has been developed and verified, facilitating chemical analysis of saline aqueous solutions from corrosion tests of two types of engineering ceramics, i.e. polycrystalline alumina, and silicon nitride. The method is capable of providing complementary information related to mechanisms of corrosion and kinetics of dissolution of the two main components of the ceramics, i.e. Al in α-Al2O3, and Si in Si3N4. A radially viewed inductively coupled plasma atomic emission spectros...

  3. Different platform and tube geometries and atomization temperatures in graphite furnace atomic absorption spectrometry: Cadmium determination in whole blood as a case study

    International Nuclear Information System (INIS)

    In the present work the performance of different platform and tube geometries and atomization temperatures in graphite furnace atomic absorption spectrometry was investigated, using the determination of Cd in whole blood as an example. Grooved, integrated and fork platforms as well as atomization temperatures between 1200 deg. C and 2200 deg. C were investigated in a longitudinally heated graphite atomizer and compared with the performance of a transversely heated furnace. In the longitudinally heated furnace the increase of the atomization temperature in the studied range resulted in an increase of matrix effects for all platform geometries. The integrated platform exhibited slightly lower sensitivity and increased multiplicative interferences in comparison to the other two platform designs. Interference-free Cd determination was possible with all types of platforms and 1200 deg. C as the atomization temperature as well as with grooved and fork platforms at 1700 deg. C. On the other hand, lower atomization temperatures resulted in poorer limits of detection, due to the longer integration time needed. No matrix effect was observed at any atomization temperature using the transversely heated atomizer; in addition, limits of detection were better than those observed with the longitudinally heated atomizer. Best values were around 0.02 μg L-1 with the latter atomizer compared to values around 0.02 μg L-1 with the former one

  4. 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

  5. Analysis of soil reference materials for vanadium(+5) species by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Solid Certified Reference Materials (CRMs) with known vanadium(+5) content are currently not commercially available. Because of this, vanadium species have been determined in solid CRMs of soil, viz. CRM023-50, CRM024-50, CRM049-50, SQC001 and SQC0012. These CRMs are certified with only total vanadium content. Vanadium(+5) was extracted from soil reference materials with 0.1 M Na2CO3. The quantification of V(+5) was carried out by electrothermal atomic absorption spectrometry (ET-AAS). The concentration of V(+5) in the analyzed CRMs was found to be ranging between 3.60 and 86.0 μg g-1. It was also found that SQC001 contains approximately 88% of vanadium as V(+5) species. Statistical evaluation of the results of the two methods by paired t-test was in good agreement at 95% level of confidence.

  6. The coupling of rapidly synergistic cloud point extraction with thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Rapidly synergistic cloud point extraction (RS-CPE) was coupled with thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to result in new CPE patterns and accelerated (1 min) protocols. It is demonstrated, for the case of copper (II) ion, that TS-FF-AAS improves the sampling efficiency and the sensitivity of FAAS determinations. Problems of nebulization associated with previous methods based on the coupling of FAAS and RS-CPE are overcome. TS-FF-AAS also improves sensitivity and gives a limit of detection for copper of 0.20 μg L-1, which is better by a factor of 32. Compared to direct FAAS, the factor is 114. (author)

  7. Determination of Trace Selenium in Electrolytic Manganese by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    YAO Jun; ZHOU Fang-qin; MA Cheng-jin; TUO Yong; LIU Jian-ben; WU Zhu-qin; TAN Zhu-zhong

    2003-01-01

    The effects of four types of graphite tube and five matrix modifiers on the determination of selenium by graphite furnace atomic absorption spectrometry were compared.The results show that platform thermolysis coat graphite tube and magnesium nitrate and cobaltco as matrix modifer can get a high sensitivity and a good recovery.The optimized working conditions and interference in the determination were invesigated.This result is consistent with that of XRF.The recovery is from 100.8 % to102.2 %,the relative standard deviation is from 3.47% to 5.56 % (n=9),and the detection limit of selenium is 378 pg (C=44.5μg/g to 97.3μg/g.).The proposed method can be applied to the rapid determination of selenium in electrolytic manganese.

  8. Some metals determination in beers by atomic emission spectrometry of induced argon plasma

    International Nuclear Information System (INIS)

    It was made the identification and determination of metals in brazilian bottled and canned beer, using atomic emission spectrometry with d.c. are and argon coupled plasma excitation sources. The elements Co, Cr, Cu, Fe, Pb and Zn were determined in beer samples, after treatment with HNO sub(3) conc. /H sub(2) O sub(2) (30%). In the determination of Co, Cr, Cu, Pb and Zn and alternative method using HNO sub(3) conc. /O sub(3) was proved be useful. The results obtained for Co, Cr, Cu, Fe, Pb and Zn were below the limits established by brazilian legislation, showing the good quality of the beer concerning the metals. The results of this work were requested by the previous Ministerio do Meio Ambiente e Urbanismo in order to contribute to review the brazilian legislation in foods and beverages about metals contents. (author)

  9. Determination of ultra trace amounts of bismuth in biological and water samples by electrothermal atomic absorption spectrometry (ET-AAS) after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Shemirani, Farzaneh; Baghdadi, Majid; Ramezani, Majid; Jamali, Mohammad Reza

    2005-04-04

    A new approach for a cloud point extraction electrothermal atomic absorption spectrometric method was used for determining bismuth. The aqueous analyte was acidified with sulfuric acid (pH 3.0-3.5). Triton X-114 was added as a surfactant and dithizone was used as a complexing agent. After phase separation at 50 deg. C based on the cloud point separation of the mixture, the surfactant-rich phase was diluted using tetrahydrofuran (THF). Twenty microliters of the enriched solution and 10 {mu}l of 0.1% (w/v) Pd(NO{sub 3}){sub 2} as chemical modifier were dispersed into the graphite tube and the analyte determined by electrothermal atomic absorption spectrometry. After optimizing extraction conditions and instrumental parameters, a preconcentration factor of 196 was obtained for a sample of only 10 ml. The detection limit was 0.02 ng ml{sup -1} and the analytical curve was linear for the concentration range of 0.04-0.60 ng ml{sup -1}. Relative standard deviations were <5%. The method was successfully applied for the extraction and determination of bismuth in tap water and biological samples (urine and hair)

  10. Speciation analysis of arsenic by hydride generation-cryotrapping-atomic fluorescence spectrometry: achieving extremely low detection limits with inexpensive instrumentation

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Svoboda, Milan; Selecká, Anna; Rychlovský, P.; Dědina, Jiří

    Münster, 2011. FTM17. [Internaional Symposium on Metallomics /3./. 15.06.2011-18.06.2011, Münster] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation analysis * hydride generation * atonmic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  11. Extraction and preconcentration of trace levels of cobalt using functionalized magnetic nanoparticles in a sequential injection lab-on-valve system with detection by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: An approach to performing extraction and preconcentration employing functionalized magnetic particles for the determination of cobalt in the sequential injection lab-on-valve system using detection by electrothermal atomic absorption spectrometry. Highlights: ► New SPE method for cobalt separation/preconcentration was reported. ► Functionalized magnetic nanoparticles were used as adsorbent. ► Extraction, elution, and detection procedures were performed in the LOV system. ► This automatic extraction technique provided a good platform for metal analysis. - Abstract: A new approach to performing extraction and preconcentration employing functionalized magnetic nanoparticles for the determination of trace metals is presented. Alumina-coated iron oxide nanoparticles were synthesized and used as the solid support. The nanoparticles were functionalized with sodium dodecyl sulfate and used as adsorbents for solid phase extraction of the analyte. Extraction, elution, and detection procedures were performed sequentially in the sequential injection lab-on-valve (SI-LOV) system followed by electrothermal atomic absorption spectrometry (ETAAS). Mixtures of hydrophobic analytes were successfully extracted from solution using the synthesized magnetic adsorbents. The potential use of the established scheme was demonstrated by taking cobalt as a model analyte. Under the optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 0.01–5 μg L−1, and the relative standard deviation was 2.8% at the 0.5 μg L−1 level (n = 11). The limit of detection was 6 ng L−1 with a sampling frequency of 18 h−1. The present method has been successfully applied to cobalt determination in water samples and two certified reference materials.

  12. 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,…

  13. Application of FTIR spectrometry to determine the atomic composition of submicron silicon nitride layers HxSirNzHy

    International Nuclear Information System (INIS)

    Authors presents the developed software that allows to use the data from Fourier transform infrared spectrometry to calculate atomic composition in the silicon nitride HxSirNzHy layers of the submicron thickness. Autonomous and rapid method for the quantitative analysis of the IR spectra does not require prior measurement of thickness and density of the layers

  14. SPECIATION OF SELENIUM(IV) AND SELENIUM(VI) USING COUPLED ION CHROMATOGRAPHY: HYDRIDE GENERATION ATOMIC ABSORPTION SPECTROMETRY

    Science.gov (United States)

    A simple method was developed to speciate inorganic selenium in the microgram per liter range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determination of the redox states selenite, Se(IV), and s...

  15. The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

    Science.gov (United States)

    Pfennig, Brian W.; Schaefer, Amy K.

    2011-01-01

    A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

  16. 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

    -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...

  17. Determination of tellurium in indium antimonide semiconductor material by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Shiue, M Y; Sun, Y C; Yang, M H

    2001-08-01

    A method for the determination of the dopant concentration of tellurium in dissolved indium antimonide semiconductor material by electrothermal atomic absorption spectrometry (ETAAS) was developed. Efforts were made to investigate the optimal conditions of the furnace heating program and the effect of palladium modifier on the variation of tellurium and the background absorbance. According to the results obtained, the presence of palladium chemical modifier in the analysis of indium antimonide allowed the successful retention of tellurium in the graphite tube, and the optimum mass of palladium modifier was found to be dependent on the sample matrix concentration. The absorbance profile of tellurium and the background level were significantly improved when a pyrolysis temperature of 1100 degrees C and an atomization temperature of 2200 degrees C were employed in the optimized heating program. With the use of this method, a detection limit of 0.8 microg g(-1) tellurium in indium antimonide could be achieved. The applicability of the proposed method was evaluated by comparison with two independent methods, i.e. slurry sampling-ETAAS and ICP-MS. From the good agreement between the results, it was demonstrated that the proposed method is suitable for the determination of typical dopant concentrations of tellurium in indium antimonide. PMID:11534624

  18. Test of the Pauli exclusion principle for nucleons and atomic electrons by accelerator mass spectrometry

    International Nuclear Information System (INIS)

    The Pauli exclusion principle was tested by searching with accelerator mass spectrometry for non-Paulian atoms with three electrons in the K-shell and for non-Paulian nuclei with three protons or three neutrons in the nuclear 1 s1/2 shell. For non-Paulian atoms of 20Ne and 36Ar the following limits have been obtained: N(20Ne)/N(20Ne)-21 and N(36Ar)/N(36Ar)-17. For non-Paulian nuclei of 5Li and 5He with three protons or three neutrons, respectively, in the nuclear 1 s1/2 shell the following limits have been measured: N(5Li)/N(6Li)-17 for a range of proton separation energies of 5Li between 0 and 50 MeV and N(5He)/N(4He)-15 for neutron separation energies between 0 and 32 MeV. The result for 5Li is used to deduce a limit for the probability β2/2 of finding two colliding protons in the symmetric state with respect to exchange to be β2/2-32. (orig.)

  19. A espectrometria atômica e a determinação de elementos metálicos em material polimérico Atomic spectrometry and the determination of metals in polymeric materials

    Directory of Open Access Journals (Sweden)

    Solange Cadore

    2008-01-01

    Full Text Available Polymeric materials are widely used in the chemical industry and are part of our daily lives. Inorganic species may be added to them as additives, anti-oxidizing agents, stabilizers, plasticizers, colorants and catalysts and may be present in a wide range of concentrations. Their determination demands the development of analytical methods considering different kinds of polymeric materials, their composition and the final use of the material. Although many different analytical techniques may be used, this review emphasizes those based on atomic absorption and emission spectrometry. Solid sampling techniques and digestion methods are described and discussed and compared considering published results.

  20. Slurry analysis of cadmium and copper collected on 11-mercaptoundecanoic acid modified TiO2 core-Au shell nanoparticles by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Separation/preconcentration of copper and cadmium using TiO2 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, 3σ) for copper and cadmium were 0.28 and 0.15 ng mL-1, respectively.

  1. A simple and fast procedure for the determination of Al, Cu, Fe and Mn in biodiesel using high-resolution continuum source electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A procedure for the determination of Al, Cu, Fe and Mn in biodiesel samples by high resolution continuum source electrothermal atomic absorption spectrometry is proposed. Sample preparation consists in simply diluting the biodiesel samples with ethanol at room temperature. For Al determination, a Zr-treated graphite tube was used as permanent modifier; for the other analytes no modifier was required. Calibration was carried out against aqueous standards, except for Al, for which calibration solutions were prepared using ethanol. Accuracy was verified by means of recovery tests and comparison with the results obtained using a different analytical procedure. The precision, expressed as the relative standard deviation, was typically better than 7%. Detection limits at ng g-1 levels for all analytes were obtained. The concentration of the analytes in biodiesel samples was generally very low, around a few tens of ng g-1, except for two samples for which the Fe concentrations were in the μg g-1 level. The proposed method has proved to be simple, precise and accurate.

  2. Nondestructive atomic compositional analysis of BeMgZnO quaternary alloys using ion beam analytical techniques

    Energy Technology Data Exchange (ETDEWEB)

    Zolnai, Z., E-mail: zolnai.zsolt@ttk.mta.hu [Research Centre for Natural Sciences, Institute of Technical Physics and Materials Science (MFA), Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary); Toporkov, M. [Department of Electrical and Computer Engineering, Virginia Commonwealth University, 601W Main St, Richmond, VA 23284 (United States); Volk, J. [Research Centre for Natural Sciences, Institute of Technical Physics and Materials Science (MFA), Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary); Department of Electrical and Computer Engineering, Virginia Commonwealth University, 601W Main St, Richmond, VA 23284 (United States); Demchenko, D.O. [Department of Physics, Virginia Commonwealth University, 701W. Grace St., Richmond, VA 23284 (United States); Okur, S. [Department of Electrical and Computer Engineering, Virginia Commonwealth University, 601W Main St, Richmond, VA 23284 (United States); Szabó, Z. [Research Centre for Natural Sciences, Institute of Technical Physics and Materials Science (MFA), Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary); Özgür, Ü.; Morkoç, H.; Avrutin, V. [Department of Electrical and Computer Engineering, Virginia Commonwealth University, 601W Main St, Richmond, VA 23284 (United States); Kótai, E. [Wigner Research Centre for Physics, Institute for Particle and Nuclear Physics, Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary)

    2015-02-01

    Highlights: • BeMgZnO thin layers were grown with plasma-assisted molecular beam epitaxy (MBE). • The Be contents were accurately measured with RBS and proton elastic backscattering. • The Tauc bandgap was measured from optical transmittance experiments. • The bandgap has been varied between 3.26 eV and 4.62 eV via the Be and Mg content. • Experimental and density functional theory calculated bandgaps were in good agreement. - Abstract: The atomic composition with less than 1–2 atom% uncertainty was measured in ternary BeZnO and quaternary BeMgZnO alloys using a combination of nondestructive Rutherford backscattering spectrometry with 1 MeV He{sup +} analyzing ion beam and non-Rutherford elastic backscattering experiments with 2.53 MeV energy protons. An enhancement factor of 60 in the cross-section of Be for protons has been achieved to monitor Be atomic concentrations. Usually the quantitative analysis of BeZnO and BeMgZnO systems is challenging due to difficulties with appropriate experimental tools for the detection of the light Be element with satisfactory accuracy. As it is shown, our applied ion beam technique, supported with the detailed simulation of ion stopping, backscattering, and detection processes allows of quantitative depth profiling and compositional analysis of wurtzite BeZnO/ZnO/sapphire and BeMgZnO/ZnO/sapphire layer structures with low uncertainty for both Be and Mg. In addition, the excitonic bandgaps of the layers were deduced from optical transmittance measurements. To augment the measured compositions and bandgaps of BeO and MgO co-alloyed ZnO layers, hybrid density functional bandgap calculations were performed with varying the Be and Mg contents. The theoretical vs. experimental bandgaps show linear correlation in the entire bandgap range studied from 3.26 eV to 4.62 eV. The analytical method employed should help facilitate bandgap engineering for potential applications, such as solar blind UV photodetectors and

  3. Nondestructive atomic compositional analysis of BeMgZnO quaternary alloys using ion beam analytical techniques

    International Nuclear Information System (INIS)

    Highlights: • BeMgZnO thin layers were grown with plasma-assisted molecular beam epitaxy (MBE). • The Be contents were accurately measured with RBS and proton elastic backscattering. • The Tauc bandgap was measured from optical transmittance experiments. • The bandgap has been varied between 3.26 eV and 4.62 eV via the Be and Mg content. • Experimental and density functional theory calculated bandgaps were in good agreement. - Abstract: The atomic composition with less than 1–2 atom% uncertainty was measured in ternary BeZnO and quaternary BeMgZnO alloys using a combination of nondestructive Rutherford backscattering spectrometry with 1 MeV He+ analyzing ion beam and non-Rutherford elastic backscattering experiments with 2.53 MeV energy protons. An enhancement factor of 60 in the cross-section of Be for protons has been achieved to monitor Be atomic concentrations. Usually the quantitative analysis of BeZnO and BeMgZnO systems is challenging due to difficulties with appropriate experimental tools for the detection of the light Be element with satisfactory accuracy. As it is shown, our applied ion beam technique, supported with the detailed simulation of ion stopping, backscattering, and detection processes allows of quantitative depth profiling and compositional analysis of wurtzite BeZnO/ZnO/sapphire and BeMgZnO/ZnO/sapphire layer structures with low uncertainty for both Be and Mg. In addition, the excitonic bandgaps of the layers were deduced from optical transmittance measurements. To augment the measured compositions and bandgaps of BeO and MgO co-alloyed ZnO layers, hybrid density functional bandgap calculations were performed with varying the Be and Mg contents. The theoretical vs. experimental bandgaps show linear correlation in the entire bandgap range studied from 3.26 eV to 4.62 eV. The analytical method employed should help facilitate bandgap engineering for potential applications, such as solar blind UV photodetectors and heterostructures

  4. Mass Spectrometry as a Powerful Analytical Technique for the Structural Characterization of Synthesized and Natural Products

    Science.gov (United States)

    Es-Safi, Nour-Eddine; Essassi, El Mokhtar; Massoui, Mohamed; Banoub, Joseph

    Mass spectrometry is an important tool for the identification and structural elucidation of natural and synthesized compounds. Its high sensitivity and the possibility of coupling liquid chromatography with mass spectrometry detection make it a technique of choice for the investigation of complex mixtures like raw natural extracts. The mass spectrometer is a universal detector that can achieve very high sensitivity and provide information on the molecular mass. More detailed information can be subsequently obtained by resorting to collision-induced dissociation tandem mass spectrometry (CID-MS/MS). In this review, the application of mass spectrometric techniques for the identification of natural and synthetic compounds is presented. The gas-phase fragmentation patterns of a series of four natural flavonoid glycosides, three synthesized benzodiazepines and two synthesized quinoxalinone derivatives were investigated using electrospray ionization mass spectrometry (ESI-MS) and tandem mass spectrometry techniques. Exact accurate masses were measured using a modorate resolution quadrupole orthogonal time-of-flight QqTOF-MS/MS hybrid mass spectrometer instrument. Confirmation of the molecular masses and the chemical structures of the studied compounds were achieved by exploring the gas-phase breakdown routes of the ionized molecules. This was rationalized by conducting low-energy collision CID-MS/MS analyses (product ion- and precursor ion scans) using a conventional quadrupole hexapole-quadrupole (QhQ) tandem mass spectrometer.

  5. Determination of lead in dolomite by Zeeman electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The mineral lorandite (TlAsS2), present in the Alshar deposit (Republic of Macedonia), is a possible solar neutrino detector (Freedman et al., 1976). As a result of nuclear reaction between the isotopes of thallium 205Tl and the solar neutrino, 205 Pb is produced. The aim of the idea is to determine the content of Pb in the lorandite, that could give information for the value of solar neutrino flux over extended time (Pavicevic, 1994). A method for the lead determination in dolomite by Zeeman electrothermal atomic absorption spectrometry, is presented. After the dissolution of samples, lead was extracted with sodium diethyldithio-carbamate. The lead-diethyldithiocarbamate complex was extracted into methylisobutyl ketone from a medium of pH 6.0-10.0. The procedure was verified by method of standard additions and by analyzing referent standard samples. A calibration curve (for organic solutions containing up to 1 ng Pb) was made using the proposed extraction procedure for standard solutions of lead. The standard deviation (SD) for 0.5 ng Pb is 0.01 ng and the relative standard deviation ranges from 2.5 to 3.5%. The detection limit of the method, calculated as 3 SD of the blank, was found to be 1.5 ng.g-1. The operation conditions in electrothermal atomic absorption measurements (temperature and time) were: drying - 90oC, 20 s; charring - 400oC, 20 s; atomizing - 1900oC, 3 s; cleaning - 2650oC, 3 s (Author)

  6. Electrochemical hydride generation atomic fluorescence spectrometry for detection of tin in canned foods using polyaniline-modified lead cathode

    International Nuclear Information System (INIS)

    An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH4 and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL-1 (3σ) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL-1 Sn(IV) standard solution.

  7. Validação de metodologia analítica para determinação de mercúrio total em amostras de urina por espectrometria de absorção atômica com geração de vapor frio (CV-AAS: estudo de caso Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS: case study

    Directory of Open Access Journals (Sweden)

    Sabine Neusatz Guilhen

    2010-01-01

    Full Text Available Mercury is a toxic metal used in a variety of substances over the course history. One of its more dubious uses is in dental amalgam restorations. It is possible to measure very small concentrations of this metal in the urine of exposed subjects by the cold vapor atomic absorption technique. The present work features the validation as an essential tool to confirm the suitability of the analytical method chosen to accomplish such determination. An initial analysis will be carried out in order to evaluate the environmental and occupational levels of exposure to mercury in 39 members of the auxiliary dental staff at public consulting rooms in the city of Araguaína (TO.

  8. Analytic Evaluation of some 2-, 3- and 4- Electron Atomic Integrals Containing Exponentially Correlated Functions of $r_{ij}$

    CERN Document Server

    Padhy, Bholanath

    2016-01-01

    A simple method is outlined for analytic evaluation of the basic 2-electron atomic integral with integrand containing products of atomic s-type Slater orbitals and exponentially correlated function of the form $r_{ij} exp(-\\lambda_{ij}r_{ij})$, by employing the Fourier representation of $exp(-\\lambda_{ij}r_{ij})/r_{ij}$ without the use of either the spherical harmonic addition theorem or the Feynman technique. This method is applied to obtain closed-form expressions, in a simple manner, for certain other 2-,3- and 4-electron atomic integrals with integrands which are products of exponentially correlated functions and atomic s-type Slater orbitals.

  9. Analytical method for parameterizing the random profile components of nanosurfaces imaged by atomic force microscopy

    CERN Document Server

    Mirsaidov, Utkur; Polyakov, Yuriy S; Misurkin, Pavel I; Musaev, Ibrahim; Polyakov, Sergey V

    2010-01-01

    The functional properties of many technological surfaces in biotechnology, electronics, and mechanical engineering depend to a large degree on the individual features of their nanoscale surface texture, which in turn are a function of the surface manufacturing process. Among these features, the surface irregularities and self-similarity structures at different spatial scales, especially in the range of 1 to 100 nm, are of high importance because they greatly affect the surface interaction forces acting at a nanoscale distance. An analytical method for parameterizing the surface irregularities and their correlations in nanosurfaces imaged by atomic force microscopy (AFM) is proposed. In this method, flicker noise spectroscopy - a statistical physics approach - is used to develop six nanometrological parameters characterizing the high-frequency contributions of jump- and spike-like irregularities into the surface texture. These contributions reflect the stochastic processes of anomalous diffusion and inertial e...

  10. Methods for the analysis of the overlapped peaks in analytical gamma-spectrometry

    International Nuclear Information System (INIS)

    A new simple method for the quantitative analysis of the doublet peaks in Ge(Li) or HPGe gamma-spectrometry is presented. No assumptions on the shape of the peaks in gamma-ray spectra being measured are required. Special feature of the method proposed is its usefulness for the analysis of closed doublets. 7 refs., 6 figs. (author)

  11. Mesoporous Silica Nanoparticles as an Adsorbent for Preconcentration and Determination of Trace Amount of Nickel in Environmental Samples by Atom Trap Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Shirkhanloo, H.; Falahnejad, M.; Zavvar Mousavi, H.

    2016-01-01

    A rapid enrichment method based on solid-phase extraction (SPE) has been established for preconcentration and separation of trace Ni(II) ions in water samples prior to their determination by atom trap flame atomic absorption spectrometry. A column filled with bulky NH2-UVM7 was used as the novel adsorbent. Under optimal conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were 3-92 μg/L, 0.8 μg/L, and 100, respectively. The validity of the method was checked by the standard reference material.

  12. 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.

  13. Determination of manganese in diesel, gasoline and naphtha by graphite furnace atomic absorption spectrometry using microemulsion medium for sample stabilization

    Science.gov (United States)

    Brandão, Geisamanda Pedrini; de Campos, Reinaldo Calixto; de Castro, Eustáquio Vinicius Ribeiro; de Jesus, Honério Coutinho

    2008-08-01

    The determination of Mn in diesel, gasoline and naphtha samples at µg L - 1 level by graphite furnace atomic absorption spectrometry, after sample stabilization in a three-component medium (microemulsion) was investigated. Microemulsions were prepared by mixing appropriate volumes of sample, propan-1-ol and nitric acid aqueous solution, and a stable system was immediately and spontaneously formed. After multivariate optimization by central composite design the optimum microemulsion composition as well as the temperature program was defined. In this way, calibration using aqueous analytical solution was possible, since the same sensitivity was observed in the optimized microemulsion media and 0.2% v/v HNO 3. The use of modifier was not necessary. Recoveries at the 3 µg L - 1 level using both inorganic and organic Mn standards spiked solutions ranged from 98 to 107% and the limits of detection were 0.6, 0.5 and 0.3 µg L - 1 in the original diesel, gasoline and naphtha samples, respectively. The Mn characteristic mass 3.4 pg. Typical relative standard deviation ( n = 5) of 8, 6 and 7% were found for the samples prepared as microemulsions at concentration levels of 1.3, 0.8, and 1.5 µg L - 1 , respectively. The total determination cycle lasted 4 min for diesel and 3 min for gasoline and naphtha, equivalent to a sample throughput of 7 h - 1 for duplicate determinations in diesel and 10 h - 1 for duplicate determinations in gasoline and naphtha. Accuracy was also assessed by using other method of analysis (ASTM D 3831-90). No statistically significant differences were found between the results obtained with the proposed method and the reference method in the analysis of real samples.

  14. Wall loss of atomic nitrogen determined by ionization threshold mass spectrometry

    International Nuclear Information System (INIS)

    In the afterglow of an inductively coupled N2 plasma, relative N atom densities are measured by ionization threshold mass spectrometry as a function of time in order to determine the wall loss time twN from the exponential decay curves. The procedure is performed with two mass spectrometers on different positions in the plasma chamber. twN is determined for various pressures, i.e., for 3.0, 5.0, 7.5, and 10 Pa. For this conditions also the internal plasma parameters electron density ne and electron temperature Te are determined with the Langmuir probe and the rotational temperature TrotN2 of N2 is determined with the optical emission spectroscopy. For TrotN2, a procedure is presented to evaluate the spectrum of the transition υ′=0→υ″=2 of the second positive system (C3Πu→B3Πg) of N2. With this method, a gas temperature of 610 K is determined. For both mass spectrometers, an increase of the wall loss times of atomic nitrogen with increasing pressure is observed. The wall loss time measured with the first mass spectrometer in the radial center of the cylindrical plasma vessel increases linearly from 0.31 ms for 3 Pa to 0.82 ms for 10 Pa. The wall loss time measured with the second mass spectrometer (further away from the discharge) is about 4 times higher. A model is applied to describe the measured twN. The main loss mechanism of atomic nitrogen for the considered pressure is diffusion to the wall. The surface loss probability βN of atomic nitrogen on stainless steel was derived from twN and is found to be 1 for the present conditions. The difference in wall loss times measured with the mass spectrometers on different positions in the plasma chamber is attributed to the different diffusion lengths

  15. Analytical Approaches Based on Gas Chromatography Mass Spectrometry (GC/MS) to Study Organic Materials in Artworks and Archaeological Objects.

    Science.gov (United States)

    Bonaduce, Ilaria; Ribechini, Erika; Modugno, Francesca; Colombini, Maria Perla

    2016-02-01

    Gas chromatography/mass spectrometry (GC/MS), after appropriate wet chemical sample pre-treatments or pyrolysis, is one of the most commonly adopted analytical techniques in the study of organic materials from cultural heritage objects. Organic materials in archaeological contexts, in classical art objects, or in modern and contemporary works of art may be the same or belong to the same classes, but can also vary considerably, often presenting different ageing pathways and chemical environments. This paper provides an overview of the literature published in the last 10 years on the research based on the use of GC/MS for the analysis of organic materials in artworks and archaeological objects. The latest progresses in advancing analytical approaches, characterising materials and understanding their degradation, and developing methods for monitoring their stability are discussed. Case studies from the literature are presented to examine how the choice of the working conditions and the analytical approaches is driven by the analytical and technical question to be answered, as well as the nature of the object from which the samples are collected. PMID:27572989

  16. Combination of cloud point extraction and flame atomic absorption spectrometry for preconcentration and determination of nickel and manganese ions in water and food samples

    International Nuclear Information System (INIS)

    A simple, rapid, inexpensive, and nonpolluting cloud point extraction (CPE) technique has been improved for the preconcentration and determination of nickel and manganese. After complexation with p-nitrophenylazoresorcinol (Magneson I), the analytes could be competitively extracted in a surfactant octylphenoxy polyethoxyethanol (Triton X-114), prior to determination by flame atomic absorption spectrometry (FAAS). The effects of experimental conditions such as pH, concentration of chelating agent and surfactant, equilibration temperature and time on CPE were studied. Under the optimum conditions, preconcentration of a 25 mL sample solution permitted the detection of 2.7 ng mL-1 Ni2+ and 2.9 ng mL-1 Mn2+ with enrichment factors of 17 and 19 for Ni2+ and Mn2+, respectively. The developed method was applied to the determination of trace nickel and manganese in water and food samples with satisfactory results.

  17. Functionalization of cross linked chitosan with 2-aminopyridine-3-carboxylic acid for solid phase extraction of cadmium and zinc ions and their determination by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    We have developed a new method for solid phase extraction (SPE) and preconcentration of trace amounts of cadmium and zinc using cross linked chitosan that was functionalized with 2-aminopyridine-3-carboxy acid. Analytical parameters, sample pH, effect of flow rate, sample volume, and concentration of eluent on column SPE were investigated. The effect of matrix ions on the recovery of cadmium and zinc has been investigated and were found not to interfere with preconcentration. Under the optimum experimental conditions, the preconcentration factors for Cd(II) and Zn(II) were found to be 90. The two elements were quantified via atomic absorption spectrometry. The detection limits for cadmium and zinc are 21 and 65 ng L -1, respectively. The method was evaluated by analyzing a certified reference material (NIST 1643e; water) and has been successfully applied to the analysis of cadmium and zinc in environmental water samples. (author)

  18. Application of High Resolution-Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS): determination of trace elements in tea and tisanes.

    Science.gov (United States)

    Paz-Rodríguez, Beatriz; Domínguez-González, María Raquel; Aboal-Somoza, Manuel; Bermejo-Barrera, Pilar

    2015-03-01

    A new application of HR-CS FAAS (High Resolution-Continuum Source Flame Atomic Absorption Spectrometry) has been developed for the determination of several trace elements (Ca, Co, Cu, Fe, Mn, Ni, Na and Zn) in infusions made from tea, rooibos and tea with seaweed samples. The proposed methods are fast, inexpensive and show good performances: the mean analytical recovery was approximately 100%. The mean limit of detection was 29.4 μg/l, and the mean limit of quantification was 98.0 μg/l (both limits refer to the brewed samples). Due to the matrix effect observed, the standard addition method had to be applied. Preliminary classification (based on metal contents) using chemometric techniques such as PCA (Principal Component Analysis) and CA (Cluster Analysis), was successful for infusions made from rooibos and tea with seaweed, but inconclusive for black and green teas. PMID:25306375

  19. Solid sampling determination of lithium and sodium additives in microsamples of yttrium oxyorthosilicate by high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Laczai, Nikoletta; Kovács, László; Péter, Ágnes; Bencs, László

    2016-03-01

    Solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS-HR-CS-GFAAS) methods were developed and studied for the fast and sensitive quantitation of Li and Na additives in microsamples of cerium-doped yttrium oxyorthosilicate (Y2SiO5:Ce) scintillator materials. The methods were optimized for solid samples by studying a set of GFAAS conditions (i.e., the sample mass, sensitivity of the analytical lines, and graphite furnace heating programs). Powdered samples in the mass range of 0.099-0.422 mg were dispensed onto graphite sample insertion boats, weighed and analyzed. Pyrolysis and atomization temperatures were optimized by the use of single-element standard solutions of Li and Na (acidified with 0.144 mol/L HNO3) at the Li I 610.353 nm and Na I 285.3013 nm analytical lines. For calibration purposes, the method of standard addition with Li and Na solutions was applied. The correlation coefficients (R values) of the calibration graphs were not worse than 0.9678. The limit of detection for oxyorthosilicate samples was 20 μg/g and 80 μg/g for Li and Na, respectively. The alkaline content of the solid samples were found to be in the range of 0.89 and 8.4 mg/g, respectively. The accuracy of the results was verified by means of analyzing certified reference samples, using methods of standard (solution) addition calibration.

  20. 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. PMID:27260436

  1. Direct analysis of silica by means of solid sampling graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    This paper reports on the use of solid sampling-graphite furnace atomic absorption spectrometry for the direct analysis of synthetic amorphous silica. In particular, determination of hazardous elements such As, Cd, Cr, Cu, Pb and Sb is investigated, as required by regulations of the food industry. The conclusion of the work is that, after proper optimization of the working conditions, paying particular attention to the atomization temperature and the use of proper modifiers (graphite powder, HNO3 or Pd), it is possible to develop suitable procedures that rely on the use of aqueous standard solutions to construct the calibration curves for all the elements investigated. The proposed method shows important benefits for the cost-effective analysis of such difficult samples in routine labs, permitting fast screening of those elements that are very rarely present in this type of sample, but also accurate quantification of those often found, while offering low limits of detection (always below 0.1 mg g−1) that comply well with legal requirements, and precision levels that are fit for the purpose (approx. 6–9% R.S.D.). - Highlights: ► Solid sampling GFAAS is investigated for the direct analysis of silica samples; ► a fast and simple methodology with aqueous standards for calibration is proposed; ► this method permits accurate determination of As, Cd, Cr, Cu, Pb and Sb in the samples of interest; ► LODs below 100 ng g−1 and precision values in the 6–10% RSD range are achieved.

  2. EVALUATION OF CORROSION OF ENGINEERING CERAMICS BY ATOMIC EMISSION SPECTROMETRY IN INDUCTIVELY COUPLED PLASMA

    Directory of Open Access Journals (Sweden)

    DAGMAR GALUSKOVÁ

    2014-03-01

    Full Text Available An analytical method has been developed and verified, facilitating chemical analysis of saline aqueous solutions from corrosion tests of two types of engineering ceramics, i.e. polycrystalline alumina, and silicon nitride. The method is capable of providing complementary information related to mechanisms of corrosion and kinetics of dissolution of the two main components of the ceramics, i.e. Al in α-Al2O3, and Si in Si3N4. A radially viewed inductively coupled plasma atomic emission spectroscopy was used, and the operating conditions for the analysis were optimised. The method was validated. Internal standardisation, matrix matching, standard addition technique and direct measurement without matrix correction were applied, and the results were critically discussed. The technique of internal standard was shown to be the most sensitive. The method exhibited satisfactory precision (relative standard deviation up to 5 %, analytical recoveries from 95 to 100 %, and acceptable limits of detection based on 3σ criterion of 0.095 mg∙l-1 for Al (measured at 308.215 nm and 0.099 mg∙l-1 for Si (at 251.611 nm.

  3. 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

    vehicle for reproducible sample presentation to the AAS instrument, as a means for facilitating conversion techniques for determination of anions, for allowing on-line preconcentration procedures via incorporated column reactors or via (co)precipitation, for exploiting kinetic discrimination schemes in...

  4. Determination of inorganic species of Sb and Te in cereals by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reyes, Mariela N.M.; Cervera, Maria L.; Guardia, Miguel de la, E-mail: m.luisa.cervera@uv.e [University of Valencia, Valencia (Spain). Dept. of Analytical Chemistry

    2011-07-01

    A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L{sup -1} phosphoric acid, 1 mol L{sup -1} nitric acid, aqua regia, 1 mol L{sup -1} sulfuric acid and 6 mol L{sup -1} hydrochloric acid. The extraction with aqua regia showed a clear interconversion of the species during the process, being H{sub 2}SO{sub 4} the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g{sup -1} with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species. (author)

  5. Determination of inorganic species of Sb and Te in cereals by hydride generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L-1 phosphoric acid, 1 mol L-1 nitric acid, aqua regia, 1 mol L-1 sulfuric acid and 6 mol L-1 hydrochloric acid. The extraction with aqua regia showed a clear interconversion of the species during the process, being H2SO4 the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g-1 with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species. (author)

  6. Determination of cadmium in water samples by fast pyrolysis-chemical vapor generation atomic fluorescence spectrometry

    Science.gov (United States)

    Zhang, Jingya; Fang, Jinliang; Duan, Xuchuan

    2016-08-01

    A pyrolysis-vapor generation procedure to determine cadmium by atomic fluorescence spectrometry has been established. Under fast pyrolysis, cadmium ion can be reduced to volatile cadmium species by sodium formate. The presence of thiourea enhanced the efficiency of cadmium vapor generation and eliminated the interference of copper. The possible mechanism of vapor generation of cadmium was discussed. The optimization of the parameters for pyrolysis-chemical vapor generation, including pyrolysis temperature, amount of sodium formate, concentration of hydrochloric acid, and carrier argon flow rate were carried out. Under the optimized conditions, the absolute and concentration detection limits were 0.38 ng and 2.2 ng ml- 1, respectively, assuming that 0.17 ml of sample was injected. The generation efficiency of was 28-37%. The method was successfully applied to determine trace amounts of cadmium in two certified reference materials of Environmental Water (GSB07-1185-2000 and GSBZ 50009-88). The results were in good agreement with the certified reference values.

  7. Determination of nickel in active pharmaceutical ingredients by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Bubnič, Zoran; Urleb, Uroš; Kreft, Katjuša; Veber, Marjan

    2010-03-01

    An electrothermal atomic absorption spectrometric procedure for the determination of nickel in active pharmaceutical ingredients was developed. Since the recoveries of nickel by the direct dissolution of samples in diluted nitric acid were low and caused errors in the determination of Ni in pharmaceutical samples, different approaches for sample pre-treatment were examined. It was found that the microwave digestion was the most suitable way for sample preparation. Various combinations of digestion agents and different microwave conditions were tested. The combination of nitric acid and hydrogen peroxide was found to be the most appropriate. The validity of the method was evaluated by recovery studies of spiked samples and by the comparison of the results obtained by inductively coupled plasma mass spectrometry (ICP-MS). The recovery ranged from 87.5 to 104.0% and a good agreement was achieved between both methods. The detection limit and the limit of quantification were 0.6 and 2.1 µg g-1 respectively. The precision of the method was confirmed by the determination of Ni in the spiked samples and was below 4%, expressed in terms of a relative standard deviation. The method was applied to the determination of nickel in production samples of active pharmaceutical ingredients and intermediates. PMID:24061653

  8. Wet sample digestion for quantification of vanadium(V) in serum by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Three types of pressure digestion systems used prior to the determination of the ultratrace element vanadium by electrothermal atomic absorption spectrometry were evaluated: The high-pressure ashing (HPA) system, the DAB III pressure digestion system and the pressurized microwave digestion (PMD) system. Complete sample digestion and no loss of graphite tube sensitivity as well as reliable vanadium values could only be achieved with HPA digests of freeze-dried serum. The mean recovery rate was 98% and no loss of tube sensitivity could be observed. Using non-lyophilized serum the mean recovery rate was 70%. The DAB III digestion system, vicarious for closed pressure digestion in steel bombs with an allowable temperature up to about 200C, cannot be recommended to mineralize human biological material for vanadium determinations, because the remaining not completely decomposed organic compounds extracted together with the vanadium-cupferron complex caused a marked carbon-buildup and formation of carbides in the graphite tube were found to change the shape of the absorption signals distinctly, and to decline the tube sensitivity strongly (about 25%) so that reliable results cannot be achieved. The recovery rate was too low in general (about 50%). In addition, a subsequent treatment of the DAB III digests with perchloric acid was unsuccessful. The PMD system proved to be not suited, because the samples became highly contaminated by vanadium possibly from the titan seal. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  9. Use of Atomic Absorption Spectrometry in Assessment of Biomonitor Plants for Lead, Cadmium and Copper Pollution

    Institute of Scientific and Technical Information of China (English)

    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 · kg-1,respectively.Significantly increased lead concentration up to 2 750 mg · 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 angustifolia 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.

  10. 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. PMID:22497165

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

    Directory of Open Access Journals (Sweden)

    Hana Zelinková

    2012-01-01

    Full Text Available 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.

  12. Determination of eight trace elements in doped crystal ALN by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. In this paper, an accurate and simple method has been developed for the determination of trace Cr, Co, Cu, Fe, Mg, Mn ,Ni and Zn in doped AlN crystal using inductively coupled plasma atomic emission spectrometry (ICP-AES). AlN crystal becomes ideal substrate for the epitaxial growth of GaN, AlGaN with high Al ingredient and AlN which are used to fabricate ultraviolet LEDs, blue- ultraviolet solid state LDs, lasers, ultraviolet detectors. At present, It is a very important aspect for scientific workers to promote in the transition metals elements doped AlN showing ferromagne. Owing its low detection limits and multi-element capability, ICP-AES has been used in many fields.The optimum instrument working conditions are selected .AlN crystal was fused with KOH and the fusion product was dissolved in dilute aqua regia. Matrix effect from KOH and interference to the spectral lines of the elements to be determined were investigated and corrected by matrix matching and background correction method. Detection limits of elements were 0.01% to 0.0002% The recoveries for elements were 98% to 104%. The relative standard deviation was 0.5% to 4.0%.

  13. Direct solid soil analysis by laser ablation inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Determination of heavy metals in soils by inductively coupled plasma atomic emission spectrometry (ICP-AES) usually involves the time-consuming step of preparing a solution of the solid that is then nebulized into the plasma. According to regulations, digestion by aqua regia(hydrochloric acid + nitric acid, 3 + 1) should be carried out although it is known that this method is incomplete for silicate soils. The problem can be eliminated by introducing the solid directly into the plasma using the laser ablation technique for sampling. Results are described for a study of laser ablation using a Q-switched Nd: YAG laser coupled with a new échelle spectrometer which has a multichannel solid-state detector. The laser pulses were focused onto the solid surface of pressed soil samples to generate an aerosol which is entrained in a flowing Ar stream, transported through a tube and then introduced directly into the inductively coupled plasma. Some characteristics of the preparation technique, the selection of an internal standard and homogeneity tests of the elemental distribution are reported along with a comparison and evaluation of three methods of calibration. The criteria used to measure the performance of laser ablation ICP-AES are the relative standard deviations obtained of 4.9–12.7% and the accuracy, 0.3–12.4% for Fe, Mn, Cu, Pb, Cr, Zn and Ni

  14. 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.

  15. 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.

  16. Determination of manganese in thermoluminescent materials by inductively coupled plasma atomic emission spectrometry and spectrophotometry

    International Nuclear Information System (INIS)

    The content of manganese in the mixed fluorides CaF2: MnF2 and CaF2: Mn thermoluminophors was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and spectrophotometry. The various Mn emission lines were compared and the manganese emission line at 257.610 nm was used for ICP-AES analysis. For the spectrophotometric determination the manganese(II) ions were oxidized to intensively coloured permanganate ions using potassium periodate. No statistically significant differences were found between the results of ICP-AES and spectrophotometric methods of analysis. The thermoluminophors were synthesized by coprecipitation of manganese with CaF2, varying the concentration of manganese in the initial solutions in the range of 0.01 - 2.0 % (m/m). The coprecipitated mixed fluorides CaF2: MnF2 were heated at 1423 K. The glow curves of synthesized CaF2: Mn thermoluminophors were measured. (author)

  17. Speciation Analysis of Serum Copper by Ultrafiltration Com-bined with Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    WANG Zhi-Hua; MA Hui-Min; MA Quan-Li; LIANG Shu-Chuan

    2001-01-01

    UItrafiltration combined with graphite furnace atomic absorp-tion spectrometry(GFAAS)was used to study protein binding and speciation of copper in human serum..UItrafiltration was carried out using a cell unit ultrafiltration membraoes having a nominal cut-off of 10,000Dalton.The effects of var-ious experimental factors including the kind and concentration of electrolyte,sample storge,pH,pressure and the precon-ditioning of the membranes on the speciation analysis of serum copper by ultrafiltration were examined.It was observed that 4.5±2.3% of the total copper in serum was ultrafiltrable and this value did not seem to be influenced by the total serum ele-mental concentration,the PH (6.5——10) adn the pressure(≤1.5kg/cm2).the preconditioning of the ultrafiltration system with 0.1mol/L calcium nitrate can overcome the adsorption loss of copper effectively,and the addition of tris-HCI sohtion (pH 7.4)to serum accelerates the ultrafiltration.The present method was proved to be suitable for speciation analysis for its simplicity,rapidity,small sample reuqirement and easy con-trol.The results obtained with the method are accurate and reliable.

  18. Determination of mercury by intermittent flow electrochemical cold vapor generation coupled to atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    A novel method for determination of mercury was developed using an intermittent flow electrochemical cold vapor generation coupled to atomic fluorescence spectrometry (IF-ECVG-AFS). The mercury vapor was generated on the surface of glassy carbon cathode in the flow cell. The operating conditions for the electrochemical generation of mercury vapor were investigated in detail, and the interferences from various ions were evaluated. Under the optimized conditions, no evident memory effects of mercury were observed. The calibration curve was linear up to 5 μg L-1 Hg at 0.54 A cm-2. A detection limit of 1.2 ng L-1 Hg and a relative standard deviation of 1.8% for 1 μg L-1 Hg were obtained. The accuracy of method was verified by the determination of mercury in the certified reference human hair. The ECVG avoided the use of reductants, thereby greatly reducing the contamination sources. In addition, the manifold of IF-ECVG-AFS was simple and amenable to automation

  19. Analysis of the release characteristics of cu-treated antimicrobial implant surfaces using atomic absorption spectrometry.

    Science.gov (United States)

    Zietz, Carmen; Fritsche, Andreas; Finke, Birgit; Stranak, Vitezslav; Haenle, Maximilian; Hippler, Rainer; Mittelmeier, Wolfram; Bader, Rainer

    2012-01-01

    New developments of antimicrobial implant surfaces doped with copper (Cu) ions may minimize the risk of implant-associated infections. However, experimental evaluation of the Cu release is influenced by various test parameters. The aim of our study was to evaluate the Cu release characteristics in vitro according to the storage fluid and surface roughness. Plasma immersion ion implantation of Cu (Cu-PIII) and pulsed magnetron sputtering process of a titanium copper film (Ti-Cu) were applied to titanium alloy (Ti6Al4V) samples with different surface finishing of the implant material (polished, hydroxyapatite and corundum blasted). The samples were submersed into either double-distilled water, human serum, or cell culture medium. Subsequently, the Cu concentration in the supernatant was measured using atomic absorption spectrometry. The test fluid as well as the surface roughness can alter the Cu release significantly, whereby the highest Cu release was determined for samples with corundum-blasted surfaces stored in cell medium. PMID:22162672

  20. Determination of lead in croatian wines by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A method has been developed for direct determination of lead in wine by graphite furnace atomic absorption spectrometry (GFAAS) with Zeeman-effect background correction. The thermal behaviour of Pb during pyrolysis and atomisation stages was investigated without matrix modifier and in the presence of Pd(NO3)2, Pd(NO3)2 + Mg(NO3)2 x 6H2O, and NH4H2PO4 + Mg(NO3)2 x 6H2O as matrix modifiers. A simple 1:1 dilution of wine samples with Pd(NO3)2 as a matrix modifier proved optimal for accurate determination of Pb in wine. Mean recoveries were 106 % for red and 114 % for white wine, and the detection limit was 3 μg L-1. Within-run precision of measurements for red and white wine was 2.1 % and 1.8 %, respectively. The proposed method was applied for analysis of 23 Croatian wines. Median Pb concentrations were 33 μg L-1, range (16 to 49) μg L-1 in commercially available wines and 46 μg L-1, range (14 to 559) μg L-1 in home-made wines. There were no statistically significant differences (P<0.05) in Pb concentration between commercial and home-made wines or between red and white wines. (authors)

  1. Gas chromatography/plasma spectrometry - an important analytical tool for elemental speciation studies

    International Nuclear Information System (INIS)

    In this review, a full discussion and update of the state-of-the-art of gas chromatography (GC) coupled to all known plasma spectrometers is presented. A brief introductive discussion of the advantages and disadvantages of GC-plasma interfaces, as well as types of plasmas and mass spectrometers, is given. The plasma-based techniques covered include inductively coupled plasma mass spectrometry (ICP-MS) microwave-induced plasma optical emission spectrometry (MIP-OES), and inductively coupled plasma optical emission spectrometry (ICP-OES). Also, different variants of plasma sources, such as low power plasmas and glow discharge (GD) sources, are described and compared with respect to their capabilities in elemental speciation. Recent advances and alternative mass analyzers (collision/reaction cell; time-of-flight; double-focusing sector field) are also mentioned. Different aspects of the GC-plasma coupling are discussed with particular attention to the applications of these hyphenated techniques to the analysis of elemental species. Additionally, classical and modern sample preparation methods, including extraction and/or preconcentration and derivatization reactions, are presented and evaluated

  2. Method development for the determination of calcium, copper, magnesium, manganese, iron, potassium, phosphorus and zinc in different types of breads by microwave induced plasma-atomic emission spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

    A novel method was developed for the determination of calcium, magnesium, potassium, iron, copper, zinc, and manganese and phosphorous in various kinds of breads samples sold in Turkey by microwave plasma-atomic emission spectrometry (MIP-AES). Breads were dried at 100 °C for one day, ground thoroughly and then digested using nitric acid/hydrogen per oxide (3:1). The analytes in certified reference wheat flour and maize flour samples were determined in the uncertainty limits of the certified values as well as the analytes added to the mixture of ground bread and acid mixture prior to digestion were recovered quantitatively (>90%). Therefore, all determinations were made by linear calibration technique using aqueous standards. The LOD values for Ca, Cu, Fe, K, Mg, Mn, P and Zn were 13.1, 0.28, 4.47, 118, 1.10, 0.41, 7550 and 3.00 ng mL(-1), respectively. No spectral interference was detected at the working wavelengths of the analytes. PMID:26830585

  3. Direct determination of arsenic and antimony in naphtha by electrothermal atomic absorption spectrometry with microemulsion sample introduction and iridium permanent modifier

    Energy Technology Data Exchange (ETDEWEB)

    Cassella, Ricardo J. [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de Sao Joao Batista s/n, Centro, 24020-007, Niteroi/RJ (Brazil); Barbosa, Bruno Alberto R.S.; Santelli, Ricardo E. [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro de Sao Joao Batista s/n, Centro, 24020-007, Niteroi/RJ (Brazil); Rangel, Alessandra T. [PETROBRAS, CENPES, PDEDS/QM, Rio de Janeiro (Brazil)

    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 {mu}g L{sup -1}) and a detection limit of 2.7 {mu}g L{sup -1} were observed for arsenic. For antimony, an RSD of 4.0% (20 {mu}g L{sup -1}) and a detection limit of 2.5 {mu}g L{sup -1} were obtained. The accuracy of the procedure was assessed by analyzing spiked samples of naphtha from different origins. (orig.)

  4. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Cunha, Francisco Antônio S; Sousa, Rafael A; Harding, David P; Cadore, Solange; Almeida, Luciano F; Araújo, Mário César U

    2012-05-21

    The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0±3.5% for Pb in the naphtha samples, and 100.2±3.4% and 100.7±4.6% for Cu and Cr, respectively in gasoline samples. PMID:22541820

  5. 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. PMID:27283608

  6. Analytical procedure for characterization of medieval wall-paintings by X-ray fluorescence spectrometry, laser ablation inductively coupled plasma mass spectrometry and Raman spectroscopy

    International Nuclear Information System (INIS)

    Analytical procedure for the comprehensive chemical characterization of samples from medieval Nubian wall-paintings by means of portable X-ray fluorescence (pXRF), laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) and Raman spectroscopy (RS) was proposed in this work. The procedure was used for elemental and molecular investigations of samples from archeological excavations in Nubia (modern southern Egypt and northern Sudan). Numerous remains of churches with painted decorations dated back to the 7th–14th century were excavated in the region of medieval kingdoms of Nubia but many aspects of this art and its technology are still unknown. Samples from the selected archeological sites (Faras, Old Dongola and Banganarti) were analyzed in the form of transfers (n = 26), small fragments collected during the excavations (n = 35) and cross sections (n = 15). XRF was used to collect data about elemental composition, LA-ICPMS allowed mapping of selected elements, while RS was used to get the molecular information about the samples. The preliminary results indicated the usefulness of the proposed analytical procedure for distinguishing the substances, from both the surface and sub-surface domains of the wall-paintings. The possibility to identify raw materials from the wall-paintings will be used in the further systematic, archeometric studies devoted to the detailed comparison of various historic Nubian centers. - Highlights: • The analytical procedure for examination of unique wall paintings was proposed. • Identification of pigments and supporting layers of wall-paintings was obtained. • Heterogeneous samples were mapped with the use of LA-ICPMS. • Anatase in the sub-surface regions of samples was detected by Raman spectroscopy

  7. Analytical procedure for characterization of medieval wall-paintings by X-ray fluorescence spectrometry, laser ablation inductively coupled plasma mass spectrometry and Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Syta, Olga; Rozum, Karol; Choińska, Marta [Faculty of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warsaw (Poland); Zielińska, Dobrochna [Institute of Archaeology, University of Warsaw, Krakowskie Przedmieście 26/28, 00-927 Warsaw (Poland); Żukowska, Grażyna Zofia [Chemical Faculty, Warsaw University of Technology, Noakowskiego 3, 00-664 Warsaw (Poland); Kijowska, Agnieszka [National Museum in Warsaw, Aleje Jerozolimskie 3, 00-495 Warsaw (Poland); Wagner, Barbara, E-mail: barbog@chem.uw.edu.pl [Faculty of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warsaw (Poland)

    2014-11-01

    Analytical procedure for the comprehensive chemical characterization of samples from medieval Nubian wall-paintings by means of portable X-ray fluorescence (pXRF), laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) and Raman spectroscopy (RS) was proposed in this work. The procedure was used for elemental and molecular investigations of samples from archeological excavations in Nubia (modern southern Egypt and northern Sudan). Numerous remains of churches with painted decorations dated back to the 7th–14th century were excavated in the region of medieval kingdoms of Nubia but many aspects of this art and its technology are still unknown. Samples from the selected archeological sites (Faras, Old Dongola and Banganarti) were analyzed in the form of transfers (n = 26), small fragments collected during the excavations (n = 35) and cross sections (n = 15). XRF was used to collect data about elemental composition, LA-ICPMS allowed mapping of selected elements, while RS was used to get the molecular information about the samples. The preliminary results indicated the usefulness of the proposed analytical procedure for distinguishing the substances, from both the surface and sub-surface domains of the wall-paintings. The possibility to identify raw materials from the wall-paintings will be used in the further systematic, archeometric studies devoted to the detailed comparison of various historic Nubian centers. - Highlights: • The analytical procedure for examination of unique wall paintings was proposed. • Identification of pigments and supporting layers of wall-paintings was obtained. • Heterogeneous samples were mapped with the use of LA-ICPMS. • Anatase in the sub-surface regions of samples was detected by Raman spectroscopy.

  8. Hooke's Atom in an Arbitrary External Electric Field: Analytical Solutions of Two-Electron Problem by Path Integral Approach

    Institute of Scientific and Technical Information of China (English)

    CAI Liang; ZHANG Ping; YANG Tao; PAN Xiao-Yin

    2011-01-01

    By using the path integral approach, we investigate the problem of Hooke's atom (two electrons interacting with Coulomb potential in an external harmonic-oscillator potential) in an arbitrary time-dependent electric field. For a certain infinite set of discrete oscillator frequencies, we obtain the analytical solutions. The ground state polarization of the atom is then calculated. The same result is also obtained through linear response theory.

  9. In-situ determination of cross-over point for overcoming plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    A novel method is described for overcoming plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry (ICP-AES). The method is based on measurement of the vertically resolved atomic emission of analyte within the plasma and therefore requires the addition of no reagents to the sample solution or to the plasma. Plasma-related matrix effects enhance analyte emission intensity low in the plasma but depress the same emission signal at higher positions. Such bipolar behavior is true for all emission lines and matrices that induce plasma-related interferences. The transition where the enhancement is balanced by the depression (the so-called cross-over point) results in a spatial region with no apparent matrix effects. Although it would be desirable always to perform determinations at this cross-over point, its location varies between analytes and from matrix to matrix, so it would have to be found separately for every analyte and for every sample. Here, a novel approach is developed for the in-situ determination of the location of this cross-over point. It was found that the location of the cross-over point is practically invariant for a particular analyte emission line when the concentration of the matrix was varied. As a result, it is possible to determine in-situ the location of the cross-over point for all analyte emission lines in a sample by means of a simple one-step sample dilution. When the original sample is diluted by a factor of 2 and the diluted sample is analyzed again, the extent of the matrix effect is identical (zero) between the original sample and the diluted sample at one and only one location - the cross-over point. This novel method was verified with several single-element matrices (0.05 M Na, Ca, Ba and La) and some mixed-element matrices (mixtures of Na-Ca, Ca-Ba, and a plant-sample digest). The inaccuracy in emission intensity due to the matrix effect could be as large as - 30% for conventional measurements in the

  10. In-situ determination of cross-over point for overcoming plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Chan, George C.-Y. [Department of Chemistry, Indiana University, 800 E Kirkwood Avenue, Bloomington, IN 47405 (United States); Hieftje, Gary M. [Department of Chemistry, Indiana University, 800 E Kirkwood Avenue, Bloomington, IN 47405 (United States)], E-mail: hieftje@indiana.edu

    2008-03-15

    A novel method is described for overcoming plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry (ICP-AES). The method is based on measurement of the vertically resolved atomic emission of analyte within the plasma and therefore requires the addition of no reagents to the sample solution or to the plasma. Plasma-related matrix effects enhance analyte emission intensity low in the plasma but depress the same emission signal at higher positions. Such bipolar behavior is true for all emission lines and matrices that induce plasma-related interferences. The transition where the enhancement is balanced by the depression (the so-called cross-over point) results in a spatial region with no apparent matrix effects. Although it would be desirable always to perform determinations at this cross-over point, its location varies between analytes and from matrix to matrix, so it would have to be found separately for every analyte and for every sample. Here, a novel approach is developed for the in-situ determination of the location of this cross-over point. It was found that the location of the cross-over point is practically invariant for a particular analyte emission line when the concentration of the matrix was varied. As a result, it is possible to determine in-situ the location of the cross-over point for all analyte emission lines in a sample by means of a simple one-step sample dilution. When the original sample is diluted by a factor of 2 and the diluted sample is analyzed again, the extent of the matrix effect is identical (zero) between the original sample and the diluted sample at one and only one location - the cross-over point. This novel method was verified with several single-element matrices (0.05 M Na, Ca, Ba and La) and some mixed-element matrices (mixtures of Na-Ca, Ca-Ba, and a plant-sample digest). The inaccuracy in emission intensity due to the matrix effect could be as large as - 30% for conventional measurements in the

  11. 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). PMID:26838401

  12. Direct determination of selenium in whole blood by electrothermal atomic absorption spectrometry using W Rh-coated platform and co-injection of Rh as thermal stabilizer

    Science.gov (United States)

    Zanão, Renato A.; Barbosa, Fernando, Jr.; Souza, Samuel S.; Krug, Francisco J.; Abdalla, Adibe L.

    2002-02-01

    A W-Rh coating on the integrated platform of a transversely heated graphite atomizer (platform modifier) and a RhCl 3 solution (analyte/matrix modifier) were combined for the direct determination of selenium in whole blood by electrothermal atomic absorption spectrometry. Samples were diluted 1+4 v/v with a mixture of 0.2% v/v HNO 3 and 0.5% v/v Triton X-100. For the analysis, 12 μl of the resulting sample plus 6 μl of the Rh solution were delivered into the transversely heated graphite atomizer (THGA) platform modified with W-Rh. The combined use of Rh solution with the W-Rh coating was decisive in increasing the maximum pyrolysis temperature of blood selenium up to 1300 °C. Use of W-Rh as a platform modifier increased the tube useful lifetime up to 200% when compared to an untreated platform using a conventional [Pd+Mg(NO 3) 2] modifier. The accuracy and precision of the method proposed were verified by analyzing serum certified reference material (Seronorm™) and 20 whole blood samples using Pd/Mg(NO 3) 2 modifier in untreated platforms; no statistical differences were found between methods by applying the t-test at the 95% level.

  13. Non-chromatographic screening procedure for arsenic speciation analysis in fish-based baby foods by using electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    López-García, Ignacio; Briceño, Marisol; Hernández-Córdoba, Manuel

    2011-08-01

    A procedure for the speciation analysis of arsenic in fish-based baby foods is presented. Inorganic arsenic, methylarsonic acid (MA), dimethylarsinic acid (DMA) and arsenobetaine (AB) were determined by electrothermal atomic absorption spectrometry (ETAAS) using suspensions prepared in a 0.01 mol L(-1) tetramethylammonium hydroxide (TMAH) solution. Speciation is based on the use of three different chemically modified ETAAS atomizers to obtain the analytical signals. Using a palladium salt as the chemical modifier, the signal corresponding to the total arsenic concentration is obtained. When palladium is replaced by Ce(IV), the signal is solely due to inorganic arsenic (III and V)+MA. If no signal is obtained in this latter case, it is possible to distinguish between DMA and AB using a zirconium coated atomizer. The signal obtained in this way is due solely to DMA, and the concentration of AB can be obtained by the difference with the total arsenic content. Determinations by ETAAS require the use of the standard additions method. The limits of detection for the determination of AB, DMA and inorganic arsenic (+MA) are 15, 25 and 50 ng g(-1) expressed as arsenic, respectively. These detection limits are good enough for the procedure to be appropriate for the rapid determination of these compounds, avoiding extraction processes and/or chromatographic separations. Data for commercial samples, as well as for four standard reference materials, are given. PMID:21704752

  14. Present analytical possibilities in prompt γ-ray spectrometry with charged projectiles

    International Nuclear Information System (INIS)

    This review article deals with γ-rays following bombardment by charged projectiles and the use of this process as an analytical method. A general enumeration of analytical possibilities with expected sensitivities is given. The basic principles and the different possible productions are summarized. A discussion of the physical background is included. Methods for quantitative analysis are discussed. Experimental arrangements are indicated and factors affecting the accuracy of analysis are considered. A number of applications are briefly described and a comparison with X-ray emission (PIXE) is made

  15. Studies of ion-imprinted polymers for solid-phase extraction of ruthenium from environmental samples before its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zambrzycka, Elzbieta; Roszko, Dorota; Lesniewska, Barbara; Wilczewska, Agnieszka Z.; Godlewska-Zylkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2011-07-15

    The examination of the effect of interfering ions on the analytical signal of ruthenium measured by electrothermal atomic absorption spectrometry was initially performed in this work. The complexes of ruthenium(III) with thiosemicarbazide (TSd) and acetaldehyde thiosemicarbazone (AcTSn) were prepared and imprinted in polymeric network. The ion-imprinted polymers were synthesized by copolymerization of methacrylic acid, as functional monomer and ethylene glycol dimethacrylate, as crosslinking agent in the presence of 2,2-azobisisobutyronitrile as initiator. The effects of sample volume, pH, and flow rate on the extraction of analyte were studied in dynamic mode. The optimum pH for quantitative retention of ruthenium on each of the studied sorbents was 7.5 {+-} 0.5. The elution of analyte was completed with 0.2 mol L{sup -1} thiourea in 0.2 mol L{sup -1} HCl. The effect of matrix ions on ruthenium(III) separation process was studied. The analytical performance of the Ru-TSd polymer in the presence of competing ions was better than Ru-AcTSn polymer, considering recovery of analyte, reproducibility of results, selectivity coefficients, and sorbent capacity. The detection limit of the proposed method (0.16 ng mL{sup -1} on Ru-TSd and 0.25 ng mL{sup -1} on Ru-AcTSn) is lower in comparison with the previously published methods. The developed separation method was successfully applied to the determination of trace amounts of ruthenium in spiked water samples, sludge, grass, and human hair.

  16. Studies of ion-imprinted polymers for solid-phase extraction of ruthenium from environmental samples before its determination by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Zambrzycka, Elżbieta; Roszko, Dorota; Leśniewska, Barbara; Wilczewska, Agnieszka Z.; Godlewska-Żyłkiewicz, Beata

    2011-07-01

    The examination of the effect of interfering ions on the analytical signal of ruthenium measured by electrothermal atomic absorption spectrometry was initially performed in this work. The complexes of ruthenium(III) with thiosemicarbazide (TSd) and acetaldehyde thiosemicarbazone (AcTSn) were prepared and imprinted in polymeric network. The ion-imprinted polymers were synthesized by copolymerization of methacrylic acid, as functional monomer and ethylene glycol dimethacrylate, as crosslinking agent in the presence of 2,2-azobisisobutyronitrile as initiator. The effects of sample volume, pH, and flow rate on the extraction of analyte were studied in dynamic mode. The optimum pH for quantitative retention of ruthenium on each of the studied sorbents was 7.5 ± 0.5. The elution of analyte was completed with 0.2 mol L -1 thiourea in 0.2 mol L -1 HCl. The effect of matrix ions on ruthenium(III) separation process was studied. The analytical performance of the Ru-TSd polymer in the presence of competing ions was better than Ru-AcTSn polymer, considering recovery of analyte, reproducibility of results, selectivity coefficients, and sorbent capacity. The detection limit of the proposed method (0.16 ng mL -1 on Ru-TSd and 0.25 ng mL -1 on Ru-AcTSn) is lower in comparison with the previously published methods. The developed separation method was successfully applied to the determination of trace amounts of ruthenium in spiked water samples, sludge, grass, and human hair.

  17. Studies of ion-imprinted polymers for solid-phase extraction of ruthenium from environmental samples before its determination by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The examination of the effect of interfering ions on the analytical signal of ruthenium measured by electrothermal atomic absorption spectrometry was initially performed in this work. The complexes of ruthenium(III) with thiosemicarbazide (TSd) and acetaldehyde thiosemicarbazone (AcTSn) were prepared and imprinted in polymeric network. The ion-imprinted polymers were synthesized by copolymerization of methacrylic acid, as functional monomer and ethylene glycol dimethacrylate, as crosslinking agent in the presence of 2,2-azobisisobutyronitrile as initiator. The effects of sample volume, pH, and flow rate on the extraction of analyte were studied in dynamic mode. The optimum pH for quantitative retention of ruthenium on each of the studied sorbents was 7.5 ± 0.5. The elution of analyte was completed with 0.2 mol L-1 thiourea in 0.2 mol L-1 HCl. The effect of matrix ions on ruthenium(III) separation process was studied. The analytical performance of the Ru-TSd polymer in the presence of competing ions was better than Ru-AcTSn polymer, considering recovery of analyte, reproducibility of results, selectivity coefficients, and sorbent capacity. The detection limit of the proposed method (0.16 ng mL-1 on Ru-TSd and 0.25 ng mL-1 on Ru-AcTSn) is lower in comparison with the previously published methods. The developed separation method was successfully applied to the determination of trace amounts of ruthenium in spiked water samples, sludge, grass, and human hair.

  18. On-line characterization of gaseous and particulate organic analytes using atmospheric pressure chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    A modified atmospheric pressure chemical ionization ion source is applied for direct analysis of volatile or low volatile organic compounds in air. The method is based on the direct introduction of the analytes in the gas phase and/or particle phase into the ion source of a commercial ion-trap mass spectrometer. Two methods are employed for the production of primary ions at atmospheric pressure, photoionization and corona discharge. It is shown that in the presence of a dopant, photoionization can be a highly efficient ionization method also for real-time analysis with detection limits for selected analytes in the lower ppt-range. Using corona discharge for the production of primary ions, which is instrumentally easier since no additional chemicals have to be added to the sample flow, we demonstrate the analytical potential of on-line atmospheric pressure chemical ionization mass spectrometry for reaction monitoring experiments. To do so, an atmospherically relevant gas phase reaction is carried out in a 500 l reaction chamber and gaseous and particulate compounds are monitored in the positive and negative ion mode of the mass spectrometer

  19. Improved analytical sensitivity for uranium and plutonium in environmental samples: Cavity ion source thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    Following successful field trials, environmental sampling has played a central role as a routine part of safeguards inspections since early 1996 to verify declared and to detect undeclared activity. The environmental sampling program has brought a new series of analytical challenges, and driven a need for advances in verification technology. Environmental swipe samples are often extremely low in concentration of analyte (ng level or lower), yet the need to analyze these samples accurately and precisely is vital, particularly for the detection of undeclared nuclear activities. Thermal ionization mass spectrometry (TIMS) is the standard method of determining isotope ratios of uranium and plutonium in the environmental sampling program. TIMS analysis typically employs 1-3 filaments to vaporize and ionize the sample, and the ions are mass separated and analyzed using magnetic sector instruments due to their high mass resolution and high ion transmission. However, the ionization efficiency (the ratio of material present to material actually detected) of uranium using a standard TIMS instrument is low (0.2%), even under the best conditions. Increasing ionization efficiency by even a small amount would have a dramatic impact for safeguards applications, allowing both improvements in analytical precision and a significant decrease in the amount of uranium and plutonium required for analysis, increasing the sensitivity of environmental sampling

  20. Analytical characteristics of inductively coupled oxygen-plasma mass spectrometry assisted by adding argon to the outer gas

    International Nuclear Information System (INIS)

    An inductively coupled oxygen plasma (O2 ICP) using a 40.68 MHz generator with a maximum radio-frequency (RF) power of 4 kW was evaluated as an ion source for mass spectrometry (MS). Although the intermediate and central Ar flows are completely replaced with O2, a certain amount of Ar should be added to the outer gas for a stable plasma discharge. The proposed O2 ICP discharge is more stable than N2 ICP, because of the lower dissociation energy of O2. The sampling depth, RF power and carrier flow rate of O2 for maximum analyte signals were found to be 7 mm above the work coil, 2.4 kW and 1.41 min-1, respectively. Under the optimized conditions, O+ is strongly observed in the mass spectra. The sensitivity of the proposed O2 ICP is inferior to those of Ar and N2 ICPs, and decreases with increasing the mass number of the analyte. Although the average kinetic energy of the analyte ions in the O2 ICP is almost equivalent to that of the Ar ICP, its distribution is wider. A wide energy distribution seems to lead to a higher ratio of doubly charged ions to singly charged ions. The ratio of monoxide ions to singly charged ions is much higher than those in Ar and N2 ICPs. (author)

  1. Determination of cadmium, cobalt, manganese, copper, nickel, and chromium in concentrated solutions of calcium chloride by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A procedure is developed for the direct determination of Cd, Co, Cr, Cu, Mn, and Ni in concentrated solutions of calcium chloride by electrothermal atomic absorption spectrometry. Ascorbic and oxalic acids and magnesium nitrate were examined as chemical modifiers. Oxalic acid was found to be the best modifier. Although an atomic absorption spectrometer with a background correction system of relatively low efficiency (deuterium lamp) was used, elements under study can be reliably determined in the presence of oxalic acid at concentrations of calcium chloride in the solution up to 6%. Because cadmium is evaporated before the major part of the given matrix, it can be determined without modifier

  2. Sapphire: a better material for atomization and in situ collection of silver volatile species for atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Musil, Stanislav, E-mail: stanomusil@biomed.cas.cz; Matoušek, Tomáš; Dědina, Jiří

    2015-06-01

    Sapphire is presented as a high temperature and corrosion resistant material of an optical tube of an atomizer for volatile species of Ag generated by the reaction with NaBH{sub 4}. The modular atomizer design was employed which allowed to carry out the measurements in two modes: (i) on-line atomization and (ii) in situ collection (directly in the optical tube) by means of excess of O{sub 2} over H{sub 2} in the carrier gas during the trapping step and vice versa in the volatilization step. In comparison with quartz atomizers, the sapphire tube atomizer provides a significantly increased atomizer lifetime as well as substantially improved repeatability of the Ag in situ collection signals shapes. In situ collection of Ag in the sapphire tube atomizer was highly efficient (> 90%). Limit of detection in the on-line atomization mode and in situ collection mode, respectively, was 1.2 ng ml{sup −1} and 0.15 ng ml{sup −1}. - Highlights: • Sapphire was tested as a new material of an atomizer tube for Ag volatile species. • Two measurement modes were investigated: on-line atomization and in situ collection. • In situ collection of Ag was highly efficient (> 90%) with LOD of 0.15 ng ml{sup −1}. • No devitrification of the sapphire tube observed in the course of several months.

  3. Determination of trace amounts of selenium in minerals and rocks by flame less atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    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

  4. Determination of calcium, copper, chromium, iron, magnesium, manganese, potassium, sodium and zinc in ethanol by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The direct determinacao of calcium, copper, chomium, iron, magnesium, manganese, potassium, sodium and zinc in ethanol by atomic absorption spectrometry with, air-acetylene flame is proposed. Effects of fuel/oxidant ratio, burner height and water content in the samples were investigated in detail. The method allows the determition of the elements with good precision (r.s.d. -1 for the elements tested. (author)

  5. Elemental analysis using instrumental neutron activation analysis and inductively coupled plasma atomic emission spectrometry: a comparative study

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Yong Sam; Choi, Kwang Soon; Moon, Jong Hwa; Kim, Sun Ha; Lim, Jong Myoung; Kim, Young Jin [KAERI, Taejon (Korea, Republic of); Quraishi, Shamshad Begum [Bangladesh Atomic Energy Commission, Dhaka (Bangladesh)

    2003-05-01

    Elemental analyses for certified reference materials were carried out using instrumental neutron activation analysis and inductively coupled plasma-atomic emission spectrometry. Five Certified Reference Materials (CRM) were selected for the study on comparative analysis of environmental samples. The CRM are Soil (NIST SRM 2709), Coal fly ash (NIST SRM 1633a), urban dust (NIST SRM 1649a) and air particulate on filter media (NIST SRM 2783 and human hair (GBW 09101)

  6. Trace elements analysis by PIXE (particle induced x-ray excitation) and AAS (atomic absorption spectrometry) from environmental samples

    International Nuclear Information System (INIS)

    The aim of this work is the micro elemental analysis of environmental samples by PIXE (Particle Induced X-ray Excitation) method and AAS (Atomic Absrobtion Spectrometry). The samples were collected from neighborhood of Targoviste city (mulberry, apple, poplar, walnut, prune, maple). The concentration data have been obtain for the elements: S, Cl, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Br, Sr by PIXE method and Mn, Fe, Cu, Cr, Se, Zn by AAS method. A good correlation b

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

    OpenAIRE

    Jelena Milinović; Rada Đurović

    2007-01-01

    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 procedu...

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

    OpenAIRE

    Joyce Nunes Bianchin; Eduardo Carasek; Edmar Martendal

    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 precisio...

  9. Elemental analysis using instrumental neutron activation analysis and inductively coupled plasma atomic emission spectrometry: a comparative study

    International Nuclear Information System (INIS)

    Elemental analyses for certified reference materials were carried out using instrumental neutron activation analysis and inductively coupled plasma-atomic emission spectrometry. Five Certified Reference Materials (CRM) were selected for the study on comparative analysis of environmental samples. The CRM are Soil (NIST SRM 2709), Coal fly ash (NIST SRM 1633a), urban dust (NIST SRM 1649a) and air particulate on filter media (NIST SRM 2783 and human hair (GBW 09101)

  10. Model and real pollutant dispersion: concentration studies by conventional analytics and by laser spectrometry

    Czech Academy of Sciences Publication Activity Database

    Zelinger, Zdeněk; Střižík, Michal; Kubát, Pavel; Lang, Kamil; Bezpalcová, Klára; Jaňour, Zbyněk

    2006-01-01

    Roč. 86, č. 12 (2006), s. 889-903. ISSN 0306-7319 R&D Projects: GA MŠk OC 723.001; GA MŠk OC 723.002; GA MŠk 1P05ME766; GA AV ČR 1ET400400410 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z20760514; CEZ:AV0Z40320502 Keywords : air pollution * photoacoustic spectrometry * wind tunel * diffrential absorption LIDAR Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 0.917, year: 2006

  11. The use of nanomaterials for mass spectrometry can be uplifting for analyte detection

    Science.gov (United States)

    Li, J.; Lipson, R. H.

    2014-03-01

    Surface-Assisted Laser Desorption Ionization (SALDI) involves desorbing and ionizing analyte molecules from a nanoporous substrate by laser irradiation for detection in a mass spectrometer. In this work experiments were designed to better understand the mechanisms governing desorption and ionization for Desorption Ionization On Silicon (DIOS), a variant of SALDI which uses porous silicon (pSi) as a substrate. Experiments are also reported for other nanoporous semiconducting materials (WO3, TiO2) which exhibit very similar behaviors; specifically, that both protonated analyte ions and analyte radical cations can be generated with relative intensities that depend on the position of the incident laser focus relative to substrate surface. While thermal desorption appears to be important, preliminary evidence suggests that the ionization mechanism leading to protonated analytes involves in part electrons and holes formed when photoexciting the substrate above its electronic band gap, and the presence of defect states within the band gap. Radical cation formation appears to be driven in part by electron transfer due to the large electron affinity of each substrate used in this work.

  12. The use of nanomaterials for mass spectrometry can be uplifting for analyte detection

    Energy Technology Data Exchange (ETDEWEB)

    Li, J.; Lipson, R. H. [University of Victoria Department of Chemistry, P.O. Box 3065, STN CSC Victoria, BC V8W 3V6 (Canada)

    2014-03-31

    Surface-Assisted Laser Desorption Ionization (SALDI) involves desorbing and ionizing analyte molecules from a nanoporous substrate by laser irradiation for detection in a mass spectrometer. In this work experiments were designed to better understand the mechanisms governing desorption and ionization for Desorption Ionization On Silicon (DIOS), a variant of SALDI which uses porous silicon (pSi) as a substrate. Experiments are also reported for other nanoporous semiconducting materials (WO{sub 3}, TiO{sub 2}) which exhibit very similar behaviors; specifically, that both protonated analyte ions and analyte radical cations can be generated with relative intensities that depend on the position of the incident laser focus relative to substrate surface. While thermal desorption appears to be important, preliminary evidence suggests that the ionization mechanism leading to protonated analytes involves in part electrons and holes formed when photoexciting the substrate above its electronic band gap, and the presence of defect states within the band gap. Radical cation formation appears to be driven in part by electron transfer due to the large electron affinity of each substrate used in this work.

  13. Application of analytical pyrolysis-mass spectrometry in characterization of animal manures

    Science.gov (United States)

    Different analytical pyrolysis techniques have been used in characterizing natural organic matter and synthesized organic polymers. Most common ones are pyrolysis followed by direct detection using MS such as in Py-FIMS technique or pyrolysis followed by GC separation of pyrosates then detected by M...

  14. Dielectric barrier discharge: Critical evaluation of a novel AAS atomizer

    Czech Academy of Sciences Publication Activity Database

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

    Praha, 2014. s. 102-102. ISBN 978-80-905704-1-2. [European Symposium on Atomic Spectrometry ESAS 2014 & Czech-Slovak Spectroscopic Conference /15./. 16.03.2014-21.03.2014, Praha] R&D Projects: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * bismuthine * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  15. Advanced analytical techniques for the extraction and characterization of plant-derived essential oils by gas chromatography with mass spectrometry.

    Science.gov (United States)

    Waseem, Rabia; Low, Kah Hin

    2015-02-01

    In recent years, essential oils have received a growing interest because of the positive health effects of their novel characteristics such as antibacterial, antifungal, and antioxidant activities. For the extraction of plant-derived essential oils, there is the need of advanced analytical techniques and innovative methodologies. An exhaustive study of hydrodistillation, supercritical fluid extraction, ultrasound- and microwave-assisted extraction, solid-phase microextraction, pressurized liquid extraction, pressurized hot water extraction, liquid-liquid extraction, liquid-phase microextraction, matrix solid-phase dispersion, and gas chromatography (one- and two-dimensional) hyphenated with mass spectrometry for the extraction through various plant species and analysis of essential oils has been provided in this review. Essential oils are composed of mainly terpenes and terpenoids with low-molecular-weight aromatic and aliphatic constituents that are particularly important for public health. PMID:25403494

  16. Slurry sampling procedure for the determination of lead in human hair by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. Human hair is a stable matrix that presents numerous advantages for human biomonitoring, such as easy collection, low cost, easy transport and storage, information about short- and long-term exposure (Angerer J et al., Int. J. Hyg. Environ. Health, 2007, 201-228). The use of the slurry sampling procedure was applied for the determination of lead in human hair by electrothermal atomic absorption spectrometry (ETAAS). This technique presents high sensitivity, low cost and the possibility of direct determination. Hair samples were pulverized using a cryogenic mill. Ten milligrams of the hair powder were transferred into a polyethylene vial and 2 ml of 2.5% HNO3 and 1.5% H2O2 were added. The slurries were maintained homogeneous with air bubbling with an aquarium pump. Niobium and Rhodium were chosen from several potential permanent modifiers by evaluating the background and absorbance signals obtained under the conditions recommended by the manufacturer. A 23 factorial design and a central composite design (CCD) were realized to optimize permanent modifier and pyrolysis and atomization temperatures. The parameters of merit were obtained in the optimized conditions (Tp = 660 deg C, Ta = 1780 deg C and Rh), and they were as follows: linear working range up to 50 μg L-1; limit of detection (0.032 0.002) μg g-1; limit of quantification (0.106 0.005) μg g-1; matrix-matched calibration, with r2 > 0.99 and reproducibility ranged from 2.3 to 4.2 relative standard deviation (RSD). The accuracy was evaluated by recovery tests and comparing slurry sampling and microwave decomposition. The recovery values for different concentrations were in the range between 89 and 101% and non-significant differences were observed (t-test; p = 0.05) when comparing the average of lead values obtained from microwave decomposition method and proposed method. Lead concentrations in different samples ranged between 0.13 and 1.11 μg g-1. The authors kindly

  17. Determination of natural isotopic variation in antimony using inductively coupled plasma mass spectrometry for an uncertainty estimation of the standard atomic weight of antimony

    International Nuclear Information System (INIS)

    The isotopic variation of industrially produced antimony was estimated using multiple-collector inductively coupled plasma mass spectrometry. A reproducible 123Sb/121Sb ratio of ±0.004% (2 standard deviations) was routinely obtained using a Sn doping mass discrimination correction technique. Only a small isotopic variation of about 0.05% was observed among industrially important Sb materials (five commercially available reagents and two ore minerals). The degree of Sb isotopic variation to determine the uncertainty in Sb atomic weight can be reduced by this new analytical technique to 0.00025 compared to the currently accepted IUPAC isotopic variation determined by conventional mass spectrometry of ±0.001. Heavy isotope enrichment of Sb in a drainage water sample from a stibnite mining area was found. This heavy isotope enrichment tendency in an aqueous environment may be useful in detecting anthropogenic Sb input from industrial emission by the smelting process via air because Sb of anthropogenic origin will have lighter isotope enrichment features. (author)

  18. Ultratrace determination of mercury in water following EN and EPA standards using atomic fluorescence spectrometry.

    Science.gov (United States)

    Labatzke, Thomas; Schlemmer, Gerhard

    2004-02-01

    Chemical vapour generation has been used in combination with atomic fluorescence spectrometry to determine mercury at ultratrace concentrations down to 0.1 ng L(-1). A time-based injection of 1 mL of solution for measurement was sufficient to generate a steady-state detector response in the direct mode of measurement. The detection limit calculated from a ten-point calibration curve according to DIN 32645 was 0.26 ng L(-1). Instrument noise is limited by reflected radiation from the light source rather than by the dark current of the photomultiplier. The detection limit is directly influenced by the reagent blank which was 2 ng L(-1) in the experiments described. Focusing by amalgamation and subsequent thermal desorption generates a detector response which is about eight times higher in peak intensity and about twice as large in integrated intensity. The detection limit under these conditions is 0.09 ng L(-1) which can be further improved by preconcentration of larger volumes of solution for measurement. The cycle time for one individual reading is about 40 s without amalgamation and 125 s with amalgamation. The linear dynamic range of the system is five orders of magnitude with a single photomultiplier gain setting. The carry-over is less than 0.3% in direct measurement mode. Reference water samples and a surface water containing approximately 5 ng L(-1) were used to prove the validity of the method for real samples. Good accuracy and recoveries of 103% were calculated using the fast direct determination technique. PMID:14673566

  19. Gunshot residue testing in suicides: Part II: Analysis by inductive coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Molina, D Kimberley; Castorena, Joe L; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

    2007-09-01

    Several different methods can be employed to test for gunshot residue (GSR) on a decedent's hands, including scanning electron microscopy with energy dispersive x-ray (SEM/EDX) and inductive coupled plasma-atomic emission spectrometry (ICP-AES). In part I of this 2-part series, GSR results performed by SEM/EDX in undisputed cases of suicidal handgun wounds were studied. In part II, the same population was studied, deceased persons with undisputed suicidal handgun wounds, but GSR testing was performed using ICP-AES. A total of 102 cases were studied and analyzed for caliber of weapon, proximity of wound, and the results of the GSR testing. This study found that 50% of cases where the deceased was known to have fired a handgun immediately prior to death had positive GSR results by ICP/AES, which did not differ from the results of GSR testing by SEM/EDX. Since only 50% of cases where the person is known to have fired a weapon were positive for GSR by either method, this test should not be relied upon to determine whether someone has discharged a firearm and is not useful as a determining factor of whether or not a wound is self-inflicted or non-self-inflicted. While a positive GSR result may be of use, a negative result is not helpful in the medical examiner setting as a negative result indicates that either a person fired a weapon prior to death or a person did not fire a weapon prior to death. PMID:17721164

  20. Determination of Lead in Human Teeth by Hydride Generation Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Hassan T. Abdulsahib

    2011-01-01

    Full Text Available Problem statement: The determination of lead in human teeth at concentration levels of ìg/ml is proposed using Hydride Generation Atomic Absorption Spectrometry (HG-AAS. To do this, 2% (wv lanthanum chloride solution is employed as matrix modifying reagent to increase sensitivity and remove matrix interferences. Approach: About 100 µL of sample and 100 µL of 3.0% (m/v NaBH4 are simultaneously injected into carrier streams. The detection of limit of 0.46 µg L-1 for Pb was achieved and the relative standard deviation of 3.0% for 10 µg L-1 lead was obtained. The recovery percentage of the method has been found to be (92.8-100.5% for known quantities of lead added to teeth sample which were completely recovered. A comparison of the proposed method with standard addition method showed nearly results in the same samples of teeth and the results compared with other studies in the world. Results: The method was shown to be satisfactory for determination of traces of lead in teeth samples with excellent accuracy. Teeth analysis reveals that intact teeth contained the highest amounts of lead which provide an evidence that lead may reduce the prevalence of dantal caries. Statistically significant differences (pConclusion: Statistically significant difference between age groups were seen in the mean value of lead concentrations in human teeth, the concentration of lead increased with age. The differences may be due to the exposure of lead and others factors such as differences in diet and drinking water.

  1. Determination of nickel by flow injection nickel tetracarbonyl generation and in situ trapping graphite furnace atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Marek, P.; Dočekal, Bohumil

    Košice : Štroffek publishing, 1998, s. 60-66. [Seminar on Atomic Spectrochemistry /14./. Podbánske (SK), 07.09.1998-11.09.1998] R&D Projects: GA ČR GA203/98/0754 Subject RIV: CB - Analytical Chemistry, Separation

  2. Flow injection-chemical vapor generation atomic fluorescence spectrometry hyphenated system for organic mercury determination: A step forward

    Energy Technology Data Exchange (ETDEWEB)

    Angeli, Valeria [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Biagi, Simona [National Research Council of Italy, C.N.R., Istituto per i Processi Chimico-Fisici - IPCF-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Ghimenti, Silvia [University of Pisa, Department of Chemistry and Industrial Chemistry, Via Risorgimento 35, 56126 Pisa (Italy); Onor, Massimo; D' Ulivo, Alessandro [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Bramanti, Emilia, E-mail: bramanti@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2011-11-15

    Monomethylmercury and ethylmercury were determined on line using flow injection-chemical vapor generation atomic fluorescence spectrometry without neither requiring a pre-treatment with chemical oxidants, nor UV/MW additional post column interface, nor organic solvents, nor complexing agents, such as cysteine. Inorganic mercury, monomethylmercury and ethylmercury were detected by atomic fluorescence spectrometry in an Ar/H{sub 2} miniaturized flame after sodium borohydride reduction to Hg{sup 0}, monomethylmercury hydride and ethylmercury hydride, respectively. The effect of mercury complexing agent such as cysteine, ethylendiaminotetracetic acid and HCl with respect to water and Ar/H{sub 2} microflame was investigated. The behavior of inorganic mercury, monomethylmercury and ethylmercury and their cysteine-complexes was also studied by continuous flow-chemical vapor generation atomic fluorescence spectrometry in order to characterize the reduction reaction with tetrahydroborate. When complexed with cysteine, inorganic mercury, monomethylmercury and ethylmercury cannot be separately quantified varying tetrahydroborate concentration due to a lack of selectivity, and their speciation requires a pre-separation stage (e.g. a chromatographic separation). If not complexed with cysteine, monomethylmercury and ethylmercury cannot be separated, as well, but their sum can be quantified separately with respect to inorganic mercury choosing a suitable concentration of tetrahydroborate (e.g. 10{sup -5} mol L{sup -1}), thus allowing the organic/inorganic mercury speciation. The detection limits of the flow injection-chemical vapor generation atomic fluorescence spectrometry method were about 45 nmol L{sup -1} (as mercury) for all the species considered, a relative standard deviation ranging between 1.8 and 2.9% and a linear dynamic range between 0.1 and 5 {mu}mol L{sup -1} were obtained. Recoveries of monomethylmercury and ethylmercury with respect to inorganic mercury were

  3. Sensitivity enhancement of beryllium determination in graphite furnace-atomic absorption spectrometry by use of atomization under pressure

    International Nuclear Information System (INIS)

    Using pressurized atomization both peak height and area sensitivity of beryllium is considerably improved. The enhancement may probably be explained by the fact that the Lorentz broadening and shift is more than compensated for by the lower diffusion rate of atoms with increasing pressures. The alteration of peak shapes and parameters should result in a diminishment of vapor phase interferences with increasing pressure. The relative time resolution of the detection system also improves with increasing pressures, with a consequent improvement of precision and accuracy. In the absorbance domain calibration curves are more linear with pressurized atomization than at atmospheric pressure. (Author)

  4. Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza, E-mail: luis.claudio@ctmsp.mar.mil.br, E-mail: adriana@ctmsp.mar.mil.br, E-mail: gomide@ctmsp.mar.mil.br, E-mail: ieda@ctmsp.mar.mil.br [Centro Tecnologico da Marinha em Sao Paulo (CEA/CTMSP), Ipero, SP (Brazil). Centro Experimental Aramar

    2013-07-01

    A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

  5. Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

    International Nuclear Information System (INIS)

    A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

  6. Suspended nanoparticles in surfactant media as a microextraction technique for simultaneous separation and preconcentration of cobalt, nickel and copper ions for electrothermal atomic absorption spectrometry determination.

    Science.gov (United States)

    Dadfarnia, Shayessteh; Shakerian, Farid; Shabani, Ali Mohammad Haji

    2013-03-15

    The aim of this study was to describe a new method of microextraction based on the suspension of alumina nanoparticles in the surfactant media for simultaneous separation and preconcentration of the ultra-traces of cobalt, nickel and copper ions. In this technique, the alumina nanoparticles were suspended in the non-ionic surfactant solution of Triton X-114. The analytes in the sample solution were adsorbed onto the nanoparticles. After the phase separation based on the cloud point of the mixture at 40 °C, the nanoparticles settled down in the surfactant rich phase. Then 120 μL of nitric acid (3.0 mol L(-1)) was added to the surfactant rich phase which caused desorption of the analytes. Finally, the liquid phase was separated by centrifugation from the nanoparticles and was used for the quantification of the analytes by the electrothermal atomic absorption spectrometry (ETAAS). The parameters affecting the extraction and detection processes were optimized. Under the optimized experimental conditions (i.e. pH∼8, Triton X-114, 0.05% (v/v); temperature 40 °C), a sample volume of 25 mL resulted in the enhancement factors of 198, 205 and 206 and detection limits (defined as 3Sb/m) of 2.5, 2.8 and 2.6 ng L(-1) for Co(II), Ni(II) and Cu(II) respectively. The sorbent showed high capacity for these metal ions (30-40 mg g(-1) sorbent). The method was successfully applied to the determination of the analytes in natural water samples. PMID:23598108

  7. Label-Free and Separation-Free Atomic Fluorescence Spectrometry-Based Bioassay: Sensitive Determination of Single-Strand DNA, Protein, and Double-Strand DNA.

    Science.gov (United States)

    Chen, Piaopiao; Wu, Peng; Chen, Junbo; Yang, Peng; Zhang, Xinfeng; Zheng, Chengbin; Hou, Xiandeng

    2016-02-16

    Based on selective and sensitive determination of Hg(2+) released from mercury complex by cold vapor generation (CVG) atomic fluorescence spectrometry (AFS) using SnCl2 as a reductant, a novel label-free and separation-free strategy was proposed for DNA and protein bioassay. To construct the DNA bioassay platform, an Hg(2+)-mediated molecular beacon (hairpin) without labeling but possessing several thymine (T) bases at both ends was employed as the probe. It is well-known that Hg(2+) could trigger the formation of the hairpin structure through T-Hg(2+)-T connection. In the presence of a specific target, the hairpin structure could be broken and the captured Hg(2+) was released. Interestingly, it was found that SnCl2 could selectively reduce only free Hg(2+) to Hg(0) vapor in the presence of T-Hg(2+)-T complex, which could be separated from sample matrices for sensitive AFS detection. Three different types of analyte, namely, single-strand DNA (ssDNA), protein, and double-strand DNA (dsDNA), were investigated as the target analytes. Under the optimized conditions, this bioassay provided high sensitivity for ssDNA, protein, and dsDNA determination with the limits of detection as low as 0.2, 0.08, and 0.3 nM and the linear dynamic ranges of 10-150, 5-175, and 1-250 nM, respectively. The analytical performance for these analytes compares favorably with those by previously reported methods, demonstrating the potential usefulness and versatility of this new AFS-based bioassay. Moreover, the bioassay retains advantages of simplicity, cost-effectiveness, and sensitivity compared to most of the conventional methods. PMID:26781421

  8. 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.

  9. 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

    International Nuclear Information System (INIS)

    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. - 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

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

    International Nuclear Information System (INIS)

    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 NH4H2PO4 at 217.001 nm, and a mixture of H2SO4 + Ca and HNO3 + 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 eliminated spectral interferences for most of

  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. 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.

  13. 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

    International Nuclear Information System (INIS)

    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. - 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 H2O2 allows analysis of fertilizers with different nitrogen species. • Proposal provides advantages over traditional methods in terms of cost and time

  14. 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. PMID:25952852

  15. Preconcentration of uranium, thorium, zirconium, titanium, molybdenum and vanadium with oxine supported on microcrystalline naphthalene and their determinations by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    A sensitive and rapid method for the determination of uranium, thorium, zirconium, titanium, molybdenum and vanadium by inductively coupled plasma atomic emission spectrometry (ICP-AES) after solid-liquid extraction with microcrystalline naphthalene is developed. Analytes were quantitatively adsorbed as their oxinate complexes on naphthalene and determined by ICP-AES after stripping with 2 M HCl. The effect of various experimental parameters such as pH, reagent amounts, naphthalene amount and stripping conditions on the determination of these elements was investigated in detail. Under the optimized experimental conditions, the detection limits of this method for U (VI), Th (IV), Zr (IV), Ti (IV), Mo (VI) and V (V) were 20.0 ng mL-1 and the relative standard deviations obtained for three replicate determinations at a concentration of 1.0 µg mL-1 were 1.5-3.0%. The proposed method has been applied in the analysis of SY-2, SY-3 and pre-analysed samples for U, Th, Zr, Ti, Mo and V the analytical results are in good agreement with recommended values. (author)

  16. Flagging and correcting non-spectral matrix interferences with spatial emission profiles and gradient dilution in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Matrix interference remains one of the most daunting challenges commonly encountered in inductively coupled plasma-atomic emission spectrometry (ICP-AES). In the present study, a method is described that enables identification and correction of matrix interferences in axial-viewed ICP-AES through a combination of spatial mapping and on-line gradient dilution. Cross-sectional emission maps of the plasma are used to indicate the presence of non-spectral (plasma-related and sample-introduction-related) matrix interferences. In particular, apparent concentrations of an analyte species determined at various radial locations in the plasma differ in the presence of a matrix interference, which allows the interference to be flagged. To correct for the interference, progressive, on-line dilution of the sample, performed by a gradient high-performance liquid-chromatograph pump, is utilized. The spatially dependent intensities of analyte emission are monitored at different levels of sample dilution. As the dilution proceeds, the matrix-induced signal variation is reduced. At a dilution where the determined concentrations become independent of location in the plasma, the matrix interference is minimized. - Highlights: • Non-spectral matrix interference in ICP-AES is flagged and minimized. • Emission from different locations of the plasma are collected simultaneously. • Spatially dependent determined concentrations indicate the presence of interference. • Gradient dilution is performed on both calibration standards and sample. • Optimal dilution factor to minimize interference is found as dilution increases

  17. Determination of rare earth elements, thorium, and uranium in mussel, ark shell, and coral by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    The determination of rare earth elements, thorium, and uranium in mussel, ark shell, and coral was made by inductively coupled plasma atomic emission spectrometry(ICP-AES). Four samples of mussels, original mussles, and mussels powdered by the original standard method, were dissolved with a mixture of HNO3 and HClO4. For one part of the sample solution, coprecipitation by ferric hydroxide was applied. Analytical values obtained with and without coprecipitation showed good agreement. The sample solutions for shells and coral were prepared by acid decomposition, and the elements to be determined were separated from calcium by coprecipitation to eliminate spectral interference by calcium. Analytical values were obtained from the calibration curves made with standard solutions containing matrix components at concentrations similar to those for real samples solutions. The concentrations of rare earth elements, Th and U in sample solutions of mussel ranged from 0.001 μg/g to 0.2 μg/g. The concentrations of rare earth elements and Th in mussel, shells, and coral are 2000 -- 15000 times higher than those in sea water. (author)

  18. Use of High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS) for Sequential Multi-Element Determination of Metals in Seawater and Wastewater Samples

    Science.gov (United States)

    Peña-Vázquez, E.; Barciela-Alonso, M. C.; Pita-Calvo, C.; Domínguez-González, R.; Bermejo-Barrera, P.

    2015-09-01

    The objective of this work is to develop a method for the determination of metals in saline matrices using high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Module SFS 6 for sample injection was used in the manual mode, and flame operating conditions were selected. The main absorption lines were used for all the elements, and the number of selected analytical pixels were 5 (CP±2) for Cd, Cu, Fe, Ni, Pb and Zn, and 3 pixels for Mn (CP±1). Samples were acidified (0.5% (v/v) nitric acid), and the standard addition method was used for the sequential determination of the analytes in diluted samples (1:2). The method showed good precision (RSD(%) < 4%, except for Pb (6.5%)) and good recoveries. Accuracy was checked after the analysis of an SPS-WW2 wastewater reference material diluted with synthetic seawater (dilution 1:2), showing a good agreement between certified and experimental results.

  19. 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. PMID:24645524

  20. Rapid diagnosis of Zellweger syndrome and infantile Refsum's disease by fast atom bombardment-mass spectrometry of urine bile salts

    International Nuclear Information System (INIS)

    A method is described for the rapid determination of urinary bile salt profiles by fast atom bombardment-mass spectrometry (FAB-MS). Negative ion FAB spectra could be obtained from the equivalent of 10 μl of urine loaded onto the target probe with glycerol as matrix. In samples from infants and children with cholestasis the major peaks were produced by the taurine and glycine conjugates of di-, tri- and tetrahydroxycholanoic acids. In samples from patients with Zellweger syndrome and infantile Refsum's disease, a unique ion at m/z 572 indicated the presence of taurine-conjugated tetrahydroxycholestanoic acid(s). Capillary gas chromatography-mass spectrometry (GC-MS) of the bile acids liberated by alkaline hydrolysis indicated the presence of at least two nuclear-tetrahydroxylated cholestanoic acids, probably the 6α- and 1β-hydroxylated derivatives of 3α, 7α, 12α-trihydroxy-5β-cholestan-26-oic acid. (Auth.)

  1. Study of the roles of chemical modifiers in determining boron using graphite furnace atomic absorption spectrometry and optimization of the temperature profile during atomization

    International Nuclear Information System (INIS)

    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. (author)

  2. Continuous-flow determination of aqueous sulfur by atmospheric-pressure helium microwave-induced plasma atomic emission spectrometry with gas-phase sample introduction

    Science.gov (United States)

    Nakahara, Taketoshi; Mori, Toshio; Morimoto, Satoru; Ishikawa, Hiroshi

    1995-06-01

    A simple continuous-flow generation of volatile hydrogen sulfide and sulfur dioxide by acidification of aqueous sulfide and sulfite ions, respectively, is described for the determination of low concentrations of sulfur by atmospheric-pressure helium microwave-induced plasma atomic emission spectrometry (MIP-AES) in the normal ultraviolet (UV) and vacuum ultraviolet (VUV) regions of the spectrum. For measuring spectral lines in the VUV region, the monochromator and the enclosed external optical path between the MIP source and the entrance slit of the monochromator have both been purged with nitrogen to minimize oxygen absorption below 190 nm. Sulfur atomic emission lines at 180.73, 182.04 and 217.05 nm have been selected as the analytical lines. Of the various acids examined, 1.0 M hydrochloric acid is the most favorable for both the generation of hydrogen sulfide from sulfide ions and sulfur dioxide from sulfite ions. Either generated hydrogen sulfide or sulfur dioxide is separated from the solution in a simple gas-liquid separator and swept into the helium stream of a microwave-induced plasma for analysis. The best attainable detection limits (3 σ criterion) for sulfur at 180.73 nm were 0.13 and 1.28 ng ml -1 for the generation of hydrogen sulfide and sulfur dioxide, respectively, with the corresponding background equivalent concentrations of 20.9 and 62.2 ng ml -1 in sulfur concentration. The typical analytical working graphs obtained under the optimized experimental conditions were rectilinear over approximately four orders of magnitude in sulfur concentration. The present method has been successfully applied to the recovery test of the sulfide spiked to waste water samples and to the determination of sulfite in some samples of commercially available wine.

  3. Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

    2015-12-01

    The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

  4. Determination of Heavy Metals in Meat, Intestine, Liver, Eggs, and Chicken Using Neutron Activation Analysis and Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    The elements As, Cd, Co, Cr, Fe, Hg, Ni, Pb, Sb, se and Zn in meat, intestine, and liver of cow and goat, as well as in broiler, local breed chicken and eggs have been determined using Neutron Activation Analysis and Atomic Absorption Spectrometry. Mercury was determined after being separated radiochemically. The results showed that concentration of the essential elements studied i.e. Cr, Cu, Fe, Zn, Co, and Ni were higher in liver and intestine than in the meat, but still in the normal range, while toxic elements As, Cd, and Pb were undetectable in all samples. (author). 8 refs., 6 tabs

  5. ANALYSES OF QUINOLONE ANTIMICROBIALS IN HUMAN PLASMA BY CAPILLARY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/FAST ATOM BOMBARDMENT MASS SPECTROMETRY

    OpenAIRE

    Hattori, Hideki; Suzuki, Osamu; Seno, Hiroshi; Ishii, Akira; Yamada, Takamichi

    1993-01-01

    Capillary high-performance liquid chromatography (HPLC) was combined with frit fast atom bombardment (FAB)-mass spectrometry (MS) , and a detailed procedure has been established for on-line analysis of ten quinolone antimicrobials in human plasma by the HPLC/FAB-MS. A special column switching device for concentration enabled injection of as large as a 500 μl sample; and the capillary column (0.5 mm i. d.) enabled introduction of its entire effluent to the frit interface of FAB-MS. These condi...

  6. Flow injection sorbent extraction of metals with activated carbon and its application to flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    In the present study activated carbon was used as a sorbent material for the flow injection on-line sorbent extraction of metal ions combined with atomic absorption spectrometry. On-line chelation of zinc was performed with 8-Hydroxyquinoline and the resultant metal chelate was adsorbed on the activated carbon, then adsorbed with zinc acid and on-line detected with flame AAS. Various parameters affecting the zinc enrichment were optimized and the method was applied for the determination of zinc in tap water, natural water, boiled and tea samples. The results obtained with the present method were compared with those obtained by the ICP-AES. (author)

  7. LASER-ENHANCED IONIZATION SPECTROMETRY WITH A TOTAL CONSUMPTION BURNER

    OpenAIRE

    Green, R; Hall, Janet

    1983-01-01

    This paper describes the use of a total consumption burner as an analytical atom reservoir for laser-enhanced ionization spectrometry. A total consumption burner and premixed burner are compared for limits of detection and matrix interferences. These results demonstrate that high sensitivity laser-enhanced ionization measurements are possible in adverse sample environments where traditional methods of optical spectrometry have proven inadequate.

  8. 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.

  9. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    International Nuclear Information System (INIS)

    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 HNO3, 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 HNO3 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.

  10. Determination of lead and nickel in environmental samples by flame atomic absorption spectrometry after column solid-phase extraction on Ambersorb-572 with EDTA

    International Nuclear Information System (INIS)

    Lead and nickel were preconcentrated as their ethylenediaminetetraacedic acid (EDTA) complexes from aqueous sample solutions using a column containing Ambersorb-572 and determined by flame atomic absorption spectrometry (FAAS). pH values, amount of solid phase, elution solution and flow rate of sample solution have been optimized in order to obtain quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of Pb and Ni under the optimum conditions were 99 ± 2 and 97 ± 3%, respectively, at 95% confidence level. Seventy-five-fold (using 750 mL of sample solution and 10 mL of eluent) and 50-fold (using 500 mL of sample solution and 10 mL of eluent) preconcentration was obtained for Pb and Ni, respectively. Time of analysis is about 4.5 h (for obtaining enrichment factor of 75). By applying these enrichment factors, the analytical detection limits of Pb and Ni were found as 3.65 and 1.42 ng mL-1, respectively. The capacity of the sorbent was found as 0.17 and 0.21 mmol g-1 for Pb and Ni, respectively. The interferences of some cations, such as Mn2+, Co2+, Fe3+, Al3+, Zn2+, Cd2+, Ca2+, Mg2+, K+ and Na+ usually present in water samples were also studied. This procedure was applied to the determination of lead and nickel in parsley, green onion, sea water and waste water samples. The accuracy of the procedure was checked by determining Pb and Ni in standard reference tea leaves sample (GBW-07605). The results demonstrated good agreement with the certified values

  11. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Highlights: ► Micro-emulsion composition phase study to obtain low fuel dilutions. ► Automated and instantaneous in-line preparation of micro-emulsions for metals determinations. ► A versatile piston-driven form of “Flow-batch Analysis”. ► Rheological considerations explored including a mathematical derivation of flow parameters. - Abstract: The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0 ± 3.5% for Pb in the naphtha samples, and 100.2 ± 3.4% and 100.7 ± 4.6% for Cu and Cr, respectively in gasoline samples.

  12. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Cunha, Francisco Antonio S. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Sousa, Rafael A. [Institute of Chemistry-University of Campinas, P.O. Box 6154, 13083-970, Campinas, SP (Brazil); Harding, David P. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Cadore, Solange [Institute of Chemistry-University of Campinas, P.O. Box 6154, 13083-970, Campinas, SP (Brazil); Almeida, Luciano F. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Araujo, Mario Cesar U., E-mail: laqa@quimica.ufpb.br [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil)

    2012-05-21

    Highlights: Black-Right-Pointing-Pointer Micro-emulsion composition phase study to obtain low fuel dilutions. Black-Right-Pointing-Pointer Automated and instantaneous in-line preparation of micro-emulsions for metals determinations. Black-Right-Pointing-Pointer A versatile piston-driven form of 'Flow-batch Analysis'. Black-Right-Pointing-Pointer Rheological considerations explored including a mathematical derivation of flow parameters. - Abstract: The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0 {+-} 3.5% for Pb in the naphtha samples, and 100.2 {+-} 3.4% and 100.7 {+-} 4.6% for Cu and Cr, respectively in gasoline samples.

  13. Comprehensive analytical strategy for biomarker identification based on liquid chromatography coupled to mass spectrometry and new candidate confirmation tools.

    Science.gov (United States)

    Mohamed, Rayane; Varesio, Emmanuel; Ivosev, Gordana; Burton, Lyle; Bonner, Ron; Hopfgartner, Gérard

    2009-09-15

    A comprehensive analytical LC-MS(/MS) platform for low weight biomarkers molecule in biological fluids is described. Two complementary retention mechanisms were used in HPLC by optimizing the chromatographic conditions for a reversed-phase column and a hydrophilic interaction chromatography column. LC separation was coupled to mass spectrometry by using an electrospray ionization operating in positive polarity mode. This strategy enables us to correctly retain and separate hydrophobic as well as polar analytes. For that purpose artificial model study samples were generated with a mixture of 38 well characterized compounds likely to be present in biofluids. The set of compounds was used as a standard aqueous mixture or was spiked into urine at different concentration levels to investigate the capability of the LC-MS(/MS) platform to detect variations across biological samples. Unsupervised data analysis by principal component analysis was performed and followed by principal component variable grouping to find correlated variables. This tool allows us to distinguish three main groups whose variables belong to (a) background ions (found in all type of samples), (b) ions distinguishing urine samples from aqueous standard and blank samples, (c) ions related to the spiked compounds. Interpretation of these groups allows us to identify and eliminate isotopes, adducts, fragments, etc. and to generate a reduced list of m/z candidates. This list is then submitted to the prototype MZSearcher software tool which simultaneously searches several lists of potential metabolites extracted from metabolomics databases (e.g., KEGG, HMDB, etc) to propose biomarker candidates. Structural confirmation of these candidates was done off-line by fraction collection followed by nanoelectrospray infusion to provide high quality MS/MS data for spectral database queries. PMID:19702294

  14. Non-chromatographic screening procedure for arsenic speciation analysis in fish-based baby foods by using electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Highlights: → Arsenic in fish-based food samples can be determined without the need of a dissolution stage. → Speciation of the main forms of arsenic in fish-based baby foods does not require chromatography. → The behavior of arsenic compounds in ETAAS strongly depends on the chemical modifier used. - Abstract: A procedure for the speciation analysis of arsenic in fish-based baby foods is presented. Inorganic arsenic, methylarsonic acid (MA), dimethylarsinic acid (DMA) and arsenobetaine (AB) were determined by electrothermal atomic absorption spectrometry (ETAAS) using suspensions prepared in a 0.01 mol L-1 tetramethylammonium hydroxide (TMAH) solution. Speciation is based on the use of three different chemically modified ETAAS atomizers to obtain the analytical signals. Using a palladium salt as the chemical modifier, the signal corresponding to the total arsenic concentration is obtained. When palladium is replaced by Ce(IV), the signal is solely due to inorganic arsenic (III and V) + MA. If no signal is obtained in this latter case, it is possible to distinguish between DMA and AB using a zirconium coated atomizer. The signal obtained in this way is due solely to DMA, and the concentration of AB can be obtained by the difference with the total arsenic content. Determinations by ETAAS require the use of the standard additions method. The limits of detection for the determination of AB, DMA and inorganic arsenic (+MA) are 15, 25 and 50 ng g-1 expressed as arsenic, respectively. These detection limits are good enough for the procedure to be appropriate for the rapid determination of these compounds, avoiding extraction processes and/or chromatographic separations. Data for commercial samples, as well as for four standard reference materials, are given.

  15. Non-chromatographic screening procedure for arsenic speciation analysis in fish-based baby foods by using electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, Ignacio; Briceno, Marisol [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, Manuel, E-mail: hcordoba@um.es [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain)

    2011-08-05

    Highlights: {yields} Arsenic in fish-based food samples can be determined without the need of a dissolution stage. {yields} Speciation of the main forms of arsenic in fish-based baby foods does not require chromatography. {yields} The behavior of arsenic compounds in ETAAS strongly depends on the chemical modifier used. - Abstract: A procedure for the speciation analysis of arsenic in fish-based baby foods is presented. Inorganic arsenic, methylarsonic acid (MA), dimethylarsinic acid (DMA) and arsenobetaine (AB) were determined by electrothermal atomic absorption spectrometry (ETAAS) using suspensions prepared in a 0.01 mol L{sup -1} tetramethylammonium hydroxide (TMAH) solution. Speciation is based on the use of three different chemically modified ETAAS atomizers to obtain the analytical signals. Using a palladium salt as the chemical modifier, the signal corresponding to the total arsenic concentration is obtained. When palladium is replaced by Ce(IV), the signal is solely due to inorganic arsenic (III and V) + MA. If no signal is obtained in this latter case, it is possible to distinguish between DMA and AB using a zirconium coated atomizer. The signal obtained in this way is due solely to DMA, and the concentration of AB can be obtained by the difference with the total arsenic content. Determinations by ETAAS require the use of the standard additions method. The limits of detection for the determination of AB, DMA and inorganic arsenic (+MA) are 15, 25 and 50 ng g{sup -1} expressed as arsenic, respectively. These detection limits are good enough for the procedure to be appropriate for the rapid determination of these compounds, avoiding extraction processes and/or chromatographic separations. Data for commercial samples, as well as for four standard reference materials, are given.

  16. Analytical Model of the Nonlinear Dynamics of Cantilever Tip-Sample Surface Interactions for Various Acoustic-Atomic Force Microscopies

    Science.gov (United States)

    Cantrell, John H., Jr.; Cantrell, Sean A.

    2008-01-01

    A comprehensive analytical model of the interaction of the cantilever tip of the atomic force microscope (AFM) with the sample surface is developed that accounts for the nonlinearity of the tip-surface interaction force. The interaction is modeled as a nonlinear spring coupled at opposite ends to linear springs representing cantilever and sample surface oscillators. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a standard iteration procedure. Solutions are obtained for the phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) techniques including force modulation microscopy, atomic force acoustic microscopy, ultrasonic force microscopy, heterodyne force microscopy, resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), and the commonly used intermittent contact mode (TappingMode) generally available on AFMs. The solutions are used to obtain a quantitative measure of image contrast resulting from variations in the Young modulus of the sample for the amplitude and phase images generated by the A-AFM techniques. Application of the model to RDF-AFUM and intermittent soft contact phase images of LaRC-cp2 polyimide polymer is discussed. The model predicts variations in the Young modulus of the material of 24 percent from the RDF-AFUM image and 18 percent from the intermittent soft contact image. Both predictions are in good agreement with the literature value of 21 percent obtained from independent, macroscopic measurements of sheet polymer material.

  17. Characterization of Arsenic Biotransformation Products from an Open Anaerobic Degradation of Fucus distichus by Hydride Generation Gas Chromatography Atomic Absorption Spectrometry and High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Abiodun A. Ojo; Onasanya, Amos

    2013-01-01

    This work reports on the isolation and determination of biotransformation products obtained from the organoarsenic compounds that are present in Fucus distichus when it was subjected to an open anaerobic decomposition by using the Hydride Generation Gas Chromatography Atomic Absorption Spectrometry (HG-GC-AAS) and High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS). The seaweed and filtrate residues obtained from the open anaerobic degradation pro...

  18. Atomization in graphite-furnace atomic absorption spectrometry. Peak-height method vs. integration method of measuring absorbance: heated graphite atomizer 2100

    International Nuclear Information System (INIS)

    The signal integration technique developed and reported earlier has been used for measuring atomic absorption signals generated by the Heated Graphite Atomizer 2100. Cd, Zn, Al, Sn, Cu, Mo, and V have been selected for this study. In theory, the integration method of measuring absorbance is superior to the conventional peak-height as the measure of absorbance. In practice, integration does offer some advantages over the peak-height method of measurement; absolute sensitivity is increased by a factor of 2- to 8-fold and the linear range of the working curves is increased by a factor of up to 2. This study shows the effect of the better cell geometry of the HGA 2100 (as opposed to the Carbon Rod Atomizer 63) on the integrated absorbance signals. Modifications to the Heated Graphite Atomizer 2100 which would improve the atomization conditions beneficial to the integration method of measuring are suggested. (U.S.)

  19. Determination of Mercury in Aqueous and Geologic Materials by Continuous Flow-Cold Vapor-Atomic Fluorescence Spectrometry (CVAFS)

    Science.gov (United States)

    Hageman, Philip L.

    2007-01-01

    New methods for the determination of total mercury in geologic materials and dissolved mercury in aqueous samples have been developed that will replace the methods currently (2006) in use. The new methods eliminate the use of sodium dichromate (Na2Cr2O7 ?2H2O) as an oxidizer and preservative and significantly lower the detection limit for geologic and aqueous samples. The new methods also update instrumentation from the traditional use of cold vapor-atomic absorption spectrometry to cold vapor-atomic fluorescence spectrometry. At the same time, the new digestion procedures for geologic materials use the same size test tubes, and the same aluminum heating block and hot plate as required by the current methods. New procedures for collecting and processing of aqueous samples use the same procedures that are currently (2006) in use except that the samples are now preserved with concentrated hydrochloric acid/bromine monochloride instead of sodium dichromate/nitric acid. Both the 'old' and new methods have the same analyst productivity rates. These similarities should permit easy migration to the new methods. Analysis of geologic and aqueous reference standards using the new methods show that these procedures provide mercury recoveries that are as good as or better than the previously used methods.

  20. Enhancement reagents for simultaneous vapor generation of zinc and cadmium with intermittent flow system coupled to atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Simultaneous vapor generation of zinc (Zn) and cadmium (Cd) was evaluated by atomic fluorescence spectrometry coupled with an intermittent flow vapor generation system. Some complexing reagents, surfactant and transition metal ions were respectively tested as enhancement reagents. Experiments showed that an appropriate amount of 8-hydroxyquinoline or phenanthroline and nickel ion simultaneously, effectively improved the vapor generation efficiency of Zn and Cd. The volatile species generation was presumed to be a hydrogenation process interpreting how the enhancement reagents played an important role in vapor generation. Additionally, due to the instability of volatile species, reaction temperature, rapid and sufficient mixing of reagents and rapid separation of the volatile species from liquid phase were also crucial. The method of simultaneous determination of Zn and Cd by intermittent flow vapor generation led to the development of atomic fluorescence spectrometry. The detection limits (3σb) were 1.6 μg l-1 for Zn and 0.01 μg l-1 for Cd and the relative standard deviations were 3.6% for Zn (50 μg l-1, n=11) and 1.7% for Cd (2 μg l-1, n=11) respectively. Results for the determination of Zn and Cd have been confirmed by the analysis of CRMs with good agreement between the certified and found values

  1. 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. PMID:25632445

  2. Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Peng, Jin-feng; Liu, Rui; Liu, Jing-fu; He, Bin; Hu, Xia-lin; Jiang, Gui-bin

    2007-05-01

    A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO 3 that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L - 1 ) and a relative standard deviation (2.5% at 50 ng L - 1 level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L - 1 and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples.

  3. Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Peng Jinfeng; Liu Rui [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P. O. Box 2871, Beijing 100085 (China); Liu Jingfu [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P. O. Box 2871, Beijing 100085 (China)], E-mail: jfliu@rcees.ac.cn; He Bin; Hu Xialin; Jiang Guibin [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P. O. Box 2871, Beijing 100085 (China)

    2007-05-15

    A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO{sub 3} that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L{sup -1}) and a relative standard deviation (2.5% at 50 ng L{sup -1} level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L{sup -1} and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples.

  4. Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO3 that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L-1) and a relative standard deviation (2.5% at 50 ng L-1 level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L-1 and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples

  5. 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.

  6. Feasibility of internal standardization in the direct and simultaneous determination of As, Cu and Pb in sugar-cane spirits by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Bismuth and Sb were evaluated as internal standards (IS) to minimize matrix effects on the direct and simultaneous determination of As, Cu, and Pb in cachaca by graphite furnace atomic absorption spectrometry using W-coated platform plus Pd-Mg(NO3)2 as modifier. For 20 μL injected sample, calibration within the 0.5-10 μg L-1 As, 100-1000 μg L-1 Cu and 0.5-30 μg L-1 Pb intervals were established using the ratios As absorbance to Sb absorbance, Cu absorbance to Bi absorbance and Pb absorbance to Bi absorbance versus analytes concentration, respectively. Typical linear correlations of 0.998, 0.999 and 0.999 were, respectively, obtained. The proposed method was applied for direct determination of As, Cu and Pb in 10 commercial cachaca samples and results were in agreement with those obtained by inductively coupled plasma mass spectrometry at 95% confidence level. The found characteristic masses were 30 pg As, 274 pg Cu and 39 pg Pb. The useful lifetime of the graphite tube was around 760 firings. Recoveries of As, Cu and Pb added to cachaca samples varied, respectively, from 98% to 109%, 97% to 108% and 98% to 104% with internal standards and from 48% to 54%, 53% to 92% and 62% to 97% without internal standards. The limits of detection were 0.13 μg L-1 As, 22 μg L-1 Cu and 0.05 μg L-1 Pb. The relative standard deviations (n = 12) for a spiked sample containing 20 μg L-1 As, Pb and 500 μg L-1 Cu were 1.6%, 1.0%, and 1.8% with IS and 4.3%, 5.2%, and 5.5% without IS

  7. 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

    International Nuclear Information System (INIS)

    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 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

  8. Nonstationary structure of atomic and molecular layers in electrothermal. Atomic absorption spectrometry: formation of atomic and molecular absorbing layers of gallium and indium

    International Nuclear Information System (INIS)

    The dynamics of the formation of absorbing layers of gallium and indium atoms and their compounds in a graphite tubular atomizer was investigated by the shadow spectral filming method. These compounds are localozed in the central part of the furnace over the platform and dissapear ay the hotter walls. It the case of gallium and indium atomization, the effects of chemical reactions between the vapor and the walls of the furnace on the formation of absorbing layers are stronger than that of diffusion and convective mass-transfer processes, which are common to all of the elements. Atom propagation from the center to the stomizer ends proceeds through the cascade mechanism because of its relatively low rate of warming up and strong longitudinal anisothermicity

  9. Green method for ultrasensitive determination of Hg in natural waters by electrothermal-atomic absorption spectrometry following sono-induced cold vapor generation and 'in-atomizer trapping'

    International Nuclear Information System (INIS)

    Sono-induced cold vapor generation (SI-CVG) has been used for the first time in combination with a graphite furnace atomizer for determination of Hg in natural waters by electrothermal-atomic absorption spectrometry after in situ trapping onto a noble metal-pretreated platform (Pd, Pt or Rh) inserted into a graphite tube. The system allows 'in-atomizer trapping' of Hg without the use of conventional reduction reactions based on sodium borohydride or tin chloride in acid medium for cold vapor generation. The sono-induced reaction is accomplished by applying ultrasound irradiation to the sample solution containing Hg(II) in the presence of an organic compound such as formic acid. As this organic acid is partly degraded upon ultrasound irradiation to yield CO, CO2, H2 and H2O, the amount of lab wastes is minimized and a green methodology is achieved. For this purpose, experimental variables influencing the generation/trapping process are fully investigated. The limit of detection for a 10 min trapping time and 10 mL sample volume was 0.03 μg L-1 (Integrated absorbance) and the repeatability expressed as relative standard deviation was about 3%. Carbonates and chlorides at 100 mg L-1 level caused a signal depression by 20-30%. The enhanced trapping efficiency observed with the sono-induced cold vapor generation as compared with 'in-atomizer trapping' methods employing chemical vapor generation is discussed. A reaction pathway for SI-CVG is proposed on the basis of the current knowledge for synthesis of noble metal nanoparticles by ultrasound

  10. Method development for the determination of manganese, cobalt and copper in green coffee comparing direct solid sampling electrothermal atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Oleszczuk, Nédio; Castro, Jacira T; da Silva, Márcia M; Korn, Maria das Graças A; Welz, Bernhard; Vale, Maria Goreti R

    2007-10-31

    A method has been developed for the determination of cobalt, copper and manganese in green coffee using direct solid sampling electrothermal atomic absorption spectrometry (SS-ET AAS). The motivation for the study was that only a few elements might be suitable to determine the origin of green coffee so that the multi-element techniques usually applied for this purpose might not be necessary. The three elements have been chosen as test elements as they were found to be significant in previous investigations. A number of botanical certified reference materials (CRM) and pre-analyzed samples of green coffee have been used for method validation, and inductively coupled plasma optical emission spectrometry (ICP OES) after microwave-assisted acid digestion of the samples as reference method. Calibration against aqueous standards could be used for the determination of Mn and Co by SS-ET AAS, but calibration against solid CRM was necessary for the determination of Cu. No significant difference was found between the results obtained with the proposed method and certified or independently determined values. The limits of detection for Mn, Cu and Co were 0.012, 0.006 and 0.004mugg(-1) using SS-ET AAS and 0.015, 0.13 and 0.10mugg(-1) using ICP OES. Seven samples of Brazilian green coffee have been analyzed, and there was no significant difference between the values obtained with SS-ET AAS and ICP OES for Mn and Cu. ICP OES could not be used as a reference method for Co, as essentially all values were below the limit of quantification of this technique. PMID:19073113

  11. A sapphire tube atomizer for on-line atomization and in situ collection of bismuthine and volatile species of silver

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Dědina, Jiří

    Praha, 2014. s. 209-209. ISBN 978-80-905704-1-2. [European Symposium on Atomic Spectrometry ESAS 2014 & Czech-Slovak Spectroscopic Conference /15./. 16.03.2014-21.03.2014, Praha] R&D Projects: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : volatile species * sapphire tube atomizer * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  12. Arsenic speciation analysis by post-separation hydride generation and atomic fluorescence detection

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Rychlovský, P.; Dědina, Jiří

    2014. s. 133-133. [Rio Symposium on Atomic Spectrometry /13./. 19.10.2014-24.10.2014, Merida, Yucatan] R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  13. The case of gold: How to atomize (and preconcentrate) its volatile species

    Czech Academy of Sciences Publication Activity Database

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

    Praha, 2014. s. 48-48. ISBN 978-80-905704-1-2. [European Symposium on Atomic Spectrometry ESAS 2014 & Czech-Slovak Spectroscopic Conference /15./. 16.03.2014-21.03.2014, Praha] R&D Projects: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : atomic absorption spectrometry * volatile compound generation * gold Subject RIV: CB - Analytical Chemistry, Separation

  14. Atomic Mineral Characteristics of Indonesian Osteoporosis by High-Resolution Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Zairin Noor; Sutiman Bambang Sumitro; Mohammad Hidayat; Agus Hadian Rahim; Akhmad Sabarudin; Tomonari Umemura

    2012-01-01

    Clinical research indicates that negative calcium balance is associated with low bone mass, rapid bone loss, and high fracture rates. However, some studies revealed that not only calcium is involved in bone strengthening as risk factor of fracture osteoporosis. Thus, in this report, the difference of metallic and nonmetallic elements in osteoporosis and normal bones was studied by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). The influence of these elements on bone...

  15. New analytical LC-mass spectrometry methodologies for the quali-quantitative determination of natural substances and drugs in complex matrices

    OpenAIRE

    Spinozzi, Silvia

    2015-01-01

    This thesis reports an integrated analytical and physicochemical approach for the study of natural substances and new drugs based on mass spectrometry techniques combined with liquid chromatography. In particular, Chapter 1 concerns the study of Berberine a natural substance with pharmacological activity for the treatment of hepatobiliary and intestinal diseases. The first part focused on the relationships between physicochemical properties, pharmacokinetics and metabolism of Berberine and...

  16. Development of bio-analytical methods for the quantitative and qualitative analysis of labelled peptides and proteins via hyphenation of chromatography and mass spectrometry

    OpenAIRE

    Holste, Angela Sarah

    2014-01-01

    This PhD thesis was a Cotutelle between the Université de Pau et des Pays de l’Adour (UPPA) in Pau, France and the Christian-Albrechts University (CAU) in Kiel, Germany. In the course of this international collaboration, bio-analytical methods for the quantitative and qualitative analysis of labelled peptides and proteins were developed, which were based on the hyphenation of chromatography with mass spectrometry. Peptides and protein digests were lanthanide labelled using DOTA-based comp...

  17. Ultrasound-assisted extraction technique for establishing selenium contents in breast cancer biopsies by Zeeman-electrothermal atomic absorption spectrometry using multi-injection

    International Nuclear Information System (INIS)

    A solid-liquid extraction method is developed to establish the contents of selenium in breast cancer biopsies. The method is based on the ultrasound-assisted extraction of selenium from pretreated biopsies prior to Se determination by atomic absorption spectrometry with longitudinal-Zeeman background correction. Fifty-one breast biopsies were collected from the Cies Hospital (Vigo, Spain), 32 of which correspond to tumor tissue and 19 to normal tissue (parenchyma). Difficulties arising from the samples analyzed, i.e. small samples mass (50-100 mg), extremely low Se contents and sample texture modification including tissue hardening due to formaldehyde preservation are addressed and overcome. High intensity sonication using a probe together with addition of hydrogen peroxide succeeded in completely extracting Se from biopsies. The multiple injection technique was useful to tackle the low Se contents present in some biopsies. The detection limit was 25 ng g-1 of Se and the precision, expressed as relative standard deviation, was less than 10%. Se contents ranged from 0.08 to 0.4 μg g-1 for parenchyma samples and from 0.09 to 0.8 μg g-1 for tumor samples. In general, Se levels in tumor biopsies were higher as compared with the adjacent normal tissue in 19 patients by a factor of up to 6. Analytical data confirmed Se accumulation in the breast tumors

  18. Use of gradient dilution to flag and overcome matrix interferences in axial-viewing inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Despite the undisputed power of inductively coupled plasma-atomic emission spectrometry (ICP-AES), its users still face serious challenges in obtaining accurate analytical results. Matrix interference is perhaps the most important challenge. Dilution of a matrix-containing sample is a common practice to reduce matrix interference. However, determining the optimal dilution factor requires tedious and time-consuming offline sample preparation, since emission lines and the effect of matrix interferences are affected differently by the dilution. The current study exploits this difference by employing a high-performance liquid chromatography gradient pump prior to the nebulizer to perform on-line mixing of a sample solution and diluent. Linear gradient dilution is performed on both the calibration standard and the matrix-containing sample. By ratioing the signals from two emission lines (from the same or different elements) as a function of dilution factor, the analyst can not only identify the presence of a matrix interference, but also determine the optimal dilution factor needed to overcome the interference. A ratio that does not change with dilution signals the absence of a matrix interference, whereas a changing ratio indicates the presence of an interference. The point on the dilution profile where the ratio stabilizes indicates the optimal dilution factor to correct the interference. The current study was performed on axial-viewing ICP-AES with o-xylene as the solvent

  19. Separation and preconcentration of trace quantities of copper ion using modified alumina nanoparticles, and its determination by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    We report on a sensitive, reliable and relatively fast method for separation, preconcentration and determination of trace quantities of copper(II) ion. It is making use of nanometer-sized γ-alumina nanoparticles modified with sodium dodecyl sulfate (SDS). The adsorptive potential was assessed via a Langmuir isotherm and the maximal sorption capacity was found to be 138 mg g-1. The effects of pH values, amount of ligand, flow rate, type of eluting agent, volume of eluent, and the volume of sample were examined. The effects of interfering ions on the recovery of the analyte were also investigated. Copper ion was then determined by flame atomic absorption spectrometry. The relative standard deviation for five replicate determinations (at 50 μg L-1 of copper) is 3.3%. The detection limit (at 3 s) is 2.5 μg L-1. This method was validated with a certified reference material of oyster tissue (NIST SRM 1566b) and the results coincided well with the certified values. The procedure was successfully applied to the determination of Cu in water and food samples. (author)

  20. Graphene-based solid-phase extraction combined with flame atomic absorption spectrometry for a sensitive determination of trace amounts of lead in environmental water and vegetable samples.

    Science.gov (United States)

    Wang, Yukun; Gao, Shutao; Zang, Xiaohuan; Li, Jingci; Ma, Jingjun

    2012-02-24

    Graphene, a novel class of carbon nanostructures, has great promise for use as sorbent materials because of its ultrahigh specific surface area. A new method using a column packed with graphene as sorbent was developed for the preconcentration of trace amounts of lead (Pb) using dithizone as chelating reagent prior to its determination by flame atomic absorption spectrometry. Some 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 10.0-600.0 μg L(-1) with a detection limit of 0.61 μg L(-1). The relative standard deviation for ten replicate measurements of 20.0 and 400.0 μg L(-1) of Pb were 3.56 and 3.25%, 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 Pb. The proposed method was successfully applied in the analysis of environmental water and vegetable samples. Good spiked recoveries over the range of 95.3-100.4% were obtained. This work not only proposes a useful method for sample preconcentration, but also reveals the great potential of graphene as an excellent sorbent material in analytical processes. PMID:22284885

  1. 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. PMID:25442538

  2. 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.

  3. Photoassisted vapor generation in the presence of organic acids for ultrasensitive determination of Se by electrothermal-atomic absorption spectrometry following headspace single-drop microextraction

    International Nuclear Information System (INIS)

    A method is described for the determination of selenium at the pg/mL level by electrothermal-atomic absorption spectrometry using in situ photogeneration of Se vapors, headspace sequestration onto an aqueous microdrop containing Pd(II) and subsequent injection in a graphite tube. Several organic acids (formic, oxalic, acetic, citric and ethylenediaminetetraacetic) have been tried for photoreduction of Se(IV) into volatile Se compounds under UV irradiation. Experimental variables such as UV irradiation time, organic acid concentration, Pd(II) concentration in the drop, sample and drop volumes, extraction time and pH were fully optimized. Low-molecular weight acids such as formic and acetic provided optimal photogeneration of volatile Se species at a 0.6 mol/L concentration. Citric and ethylenediaminetetraacetic acid allowed to use a concentration as low as 1 mmol/L, but extraction times were longer than for formic and acetic acids. Photogeneration of (CH3)2Se from Se(IV) in the presence of acetic acid provided a detection limit of 20 pg/mL, a preconcentration factor of nearly 285 and a precision, expressed as relative standard deviation, of 4%. Analytical performance seemed to depend not only on the photogeneration efficiency obtained with each acid but also on the stability of the vapors in the headspace. The method showed a high freedom from interferences caused by saline matrices, but interferences were observed for transition metals at a relatively low concentration

  4. Determination of total Sb,Se Te, and Bi and evaluation of their inorganic species in garlic by hydride-generation-atomic-fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matos Reyes, M.N.; Cervera, M.L.; Guardia, M. de la [University of Valencia, Department of Analytical Chemistry, Burjassot, Valencia (Spain)

    2009-07-15

    A sensitive and simple analytical method has been developed for determination of Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), Te(VI), and Bi(III) in garlic samples by using hydride-generation-atomic-fluorescence spectrometry (HG-AFS). The method is based on a single extraction of the inorganic species by sonication at room temperature with 1 mol L{sup -1} H{sub 2}SO{sub 4} and washing of the solid phase with 0.1% (w/v) EDTA, followed by measurement of the corresponding hydrides generated under two different experimental conditions directly and after a pre-reduction step. The limit of detection of the method was 0.7 ng g{sup -1} for Sb(III), 1.0 ng g{sup -1} for Sb(V), 1.3 ng g{sup -1} for Se(IV), 1.0 ng g{sup -1} for Se(VI), 1.1 ng g{sup -1} for Te(IV), 0.5 ng g{sup -1} for Te(VI), and 0.9 ng g{sup -1} for Bi(III), in all cases expressed in terms of sample dry weight. (orig.)

  5. Effect of surfactant addition on ultrasonic leaching of trace elements from plant samples in inductively coupled plasma-atomic emission spectrometry

    Science.gov (United States)

    Borkowska-Burnecka, Jolanta; Jankowiak, Urszula; Zyrnicki, Wieslaw; Anna Wilk, Kazimiera

    2004-04-01

    The applicability of surfactants in sample preparation of plant materials followed by analysis by inductively coupled plasma atomic emission spectrometry has been examined. Reference materials (INCT-MPH-2-Mixed Polish Herbs, INCT-TL-1 black tea leaves and CTA-VTL-2 -Virginia tobacco leaves) and commercially available tea leaves were analyzed. Effects of addition surfactants (Triton X-100, didodecyldimethylammonium bromide and cetyltrimethylammonium bromide) on efficiency of ultrasonic leaching of elements from the plant samples and on plasma parameters were investigated. Low concentrations of the surfactants in solutions did not affect, in practice, analytical line intensities and the nebulization process. Quantitative recovery of some elements could be obtained by ultrasonic diluted acid leaching with the aid of surfactants. However, the element recovery depended on type of surfactant, as well as element and sample material. Plasma parameters, i.e. the excitation temperatures of Ar I, Fe II and Ca II as well as the electron number density and the Mg II/Mg I intensity ratio did not vary significantly due to the surfactants in solutions.

  6. Effect of surfactant addition on ultrasonic leaching of trace elements from plant samples in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    The applicability of surfactants in sample preparation of plant materials followed by analysis by inductively coupled plasma atomic emission spectrometry has been examined. Reference materials (INCT-MPH-2-Mixed Polish Herbs, INCT-TL-1 black tea leaves and CTA-VTL-2 -Virginia tobacco leaves) and commercially available tea leaves were analyzed. Effects of addition surfactants (Triton X-100, didodecyldimethylammonium bromide and cetyltrimethylammonium bromide) on efficiency of ultrasonic leaching of elements from the plant samples and on plasma parameters were investigated. Low concentrations of the surfactants in solutions did not affect, in practice, analytical line intensities and the nebulization process. Quantitative recovery of some elements could be obtained by ultrasonic diluted acid leaching with the aid of surfactants. However, the element recovery depended on type of surfactant, as well as element and sample material. Plasma parameters, i.e. the excitation temperatures of Ar I, Fe II and Ca II as well as the electron number density and the Mg II/Mg I intensity ratio did not vary significantly due to the surfactants in solutions

  7. Analysis of Si3N4 ultra fine powder using high-pressure acid digestion and slurry injection in inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Si3N4 powder has been analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sample was dissolved by high-pressure acid digestion with HF, H2SO4 (1+1), and HNO3 mixture. This technique is well suited for the impurity analysis of Si3N4 because the matrix interference is eliminated. A round robin samples trace elements, such as Ca, W, Co, Al, Fe, Mg, and Na, were determined. For the direct analysis, slurry nebulization of 0.96 mm Si3N4 powder also has been studied by ICP-AES. Emission intensities of Fe were measure as ICP operational conditions were changed. Significant signal difference between slurry particles and aqueous solution was observed in the present experiment. Analytical results of slurry injection and high-pressure acid digestion were compared. For the use of aqueous standard solution for calibration, k-factor was determined to be 1.71 for further application

  8. Evaluation of two atomisation modes for direct determination of molybdenum in complex matrices by ultrasonic slurry sampling-electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Tube wall (TWA) and L'vov platform (LPA) atomisations were compared for the direct determination of molybdenum (Mo) in coal fly ash by slurry sampling-electrothermal atomic absorption spectrometry (ETAAS). For both atomisation modes eight chemical modifiers were tested, namely HNO3, Pd(NO3)2, Mg(NO3)2, Pd + Mg(NO3)2, reduced Pd, BaF2, Ir and HF. The interfering effects of major and minor concomitants of samples on Mo signals and memory effects were also evaluated. BaF2 and Pd(NO3)2 + Mg(NO3)2 mixture were selected for TWA and LPA, respectively. Standard addition calibration is needed in both cases. The best peak performance, memory effect reduction, within-run precision (6% versus 9% R.S.D.), and sensitivity (mo 7.5 pg versus 15.2 pg) were achieved with TWA compared to LPA. Both atomisation modes gave good analytical recoveries (94-102%), but the analysis of a certified coal fly ash (NIST SRM 1633a) only was accurate using TWA. Additionally, the urban dust NIST SRM 1629a was analysed

  9. 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

    2016-03-01

    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. PMID:26852265

  10. Immobilized salen (N,N'-bis (salicylidene) ethylenediamine) as a complexing agent for on-line sorbent extraction/preconcentration and flow injection-flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The microcolumn of salen I (N,N'-bis (salicylidene) ethylenediamine) immobilized on surfactant-coated alumina has been used for on-line preconcentration of copper and lead with a flow injection-flame atomic absorption spectrometry (FI-AAS). Various parameters affecting the deposition/elution processes in the FI-AAS system was optimized. Deposition of analytes was affected at pH of ∼9, and injection of nitric acid (250 μl 2 mol l-1) served to elute retained species to AAS. A good relative standard deviation of 4.5 and 3.8% at 30 μg l-1(n = 7), high enrichment factors of 100 and 75, and detection limits of 0.3, 2.6 μg l-1 (3S) for Cu(II) and Pb(II) were obtained, respectively. The method was applied to water samples, multivitamin tablet and standard reference alloys (C12E41 and C12X3500) and accuracy was assessed through recovery experiment and independent analysis by furnace AAS, or comparing the results with the accepted values

  11. 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%. PMID:27451169

  12. Analytical Method for Pu-239, Pu-240, Np-237 and Tc-99 using Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    An efficient analytical method for Pu isotopes (Pu-239 and Pu-240), Np-237 and Tc-99 in environmental samples has been developed using sector field inductively coupled plasma mass spectrometry (SF-ICPMS) detection. The chemical separation of Pu in terrestrial samples, soil, and sediment was carried out on two extraction resins, Sr-Spec and TEVA, which were sequentially combined in PrepLab, an integrated liquid handing device. By reducing the final eluent volume to 2.4 mL, directly injecting it to SF-ICPMS, and employing MCN-6000, a membrane desolvating sample introduction system, the analysis of Pu isotopes was found to be feasible in 1 g of soil. The detection limits of Pu-239, Pu-240, and Pu-242 were approximately 4 fg mL-1 (9.2 Bq mL-1), 3 fg mL-1 (25 Bq mL-1), and 6 fg mL-1 (0.87 Bq mL-1), which represent total amounts of 9.6, 7.2, and 14 fg, respectively, in the final eluent. Chemical separation and measurement were fully automated by a sequential injection (SI) program in an on-line system, and the analysis could thereby be completed within roughly 5 hours. The reliability of this method was confirmed by a validity test with several certified standard reference materials (NIST-4350b, IAEA-6, IAEA-300, IAEA-367, IAEA-368, IAEA-375). The analytical method for Pu in environmental seawater is different from that of terrestrial samples owing to the strong interference effect of U as well as ultra-low level Pu. Although the principle of chemical separation is nearly the same as in soil, seawater was co-precipitated with Fe(OH)2 in the pre-treatment step and a micro TEVA column (50 L) was used in the on-line system to improve precision and the lower detection limit. With this method, it was possible to analyze ultra-trace level Pu isotopes in only 5 L of surface seawater within 1 day, and the precision for Pu-239 and Pu-240 was less than 3.4% (n=7) and 5% (n=7), respectively. The accuracy of this method was verified by analysis of reference seawater (IAEA-381) as

  13. Analytical Method for Pu-239, Pu-240, Np-237 and Tc-99 using Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Cheol Su

    2007-02-15

    An efficient analytical method for Pu isotopes (Pu-239 and Pu-240), Np-237 and Tc-99 in environmental samples has been developed using sector field inductively coupled plasma mass spectrometry (SF-ICPMS) detection. The chemical separation of Pu in terrestrial samples, soil, and sediment was carried out on two extraction resins, Sr-Spec and TEVA, which were sequentially combined in PrepLab, an integrated liquid handing device. By reducing the final eluent volume to 2.4 mL, directly injecting it to SF-ICPMS, and employing MCN-6000, a membrane desolvating sample introduction system, the analysis of Pu isotopes was found to be feasible in 1 g of soil. The detection limits of Pu-239, Pu-240, and Pu-242 were approximately 4 fg mL-1 (9.2 Bq mL-1), 3 fg mL-1 (25 Bq mL-1), and 6 fg mL-1 (0.87 Bq mL-1), which represent total amounts of 9.6, 7.2, and 14 fg, respectively, in the final eluent. Chemical separation and measurement were fully automated by a sequential injection (SI) program in an on-line system, and the analysis could thereby be completed within roughly 5 hours. The reliability of this method was confirmed by a validity test with several certified standard reference materials (NIST-4350b, IAEA-6, IAEA-300, IAEA-367, IAEA-368, IAEA-375). The analytical method for Pu in environmental seawater is different from that of terrestrial samples owing to the strong interference effect of U as well as ultra-low level Pu. Although the principle of chemical separation is nearly the same as in soil, seawater was co-precipitated with Fe(OH)2 in the pre-treatment step and a micro TEVA column (50 L) was used in the on-line system to improve precision and the lower detection limit. With this method, it was possible to analyze ultra-trace level Pu isotopes in only 5 L of surface seawater within 1 day, and the precision for Pu-239 and Pu-240 was less than 3.4% (n=7) and 5% (n=7), respectively. The accuracy of this method was verified by analysis of reference seawater (IAEA-381) as

  14. 原子荧光光谱法测定土壤中的砷含量%Determination of Arsenic in Soil by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘燕芬

    2015-01-01

    通过结合具体的试验对运用原子荧光光谱法测定土壤中的砷含量进行了探讨,以期能为有关方面的需要提供有益的参考和借鉴。%In order to provide a useful reference for the relevant aspects of the arsenic content in soil by atomic fluorescence spectrometry, the method of atomic fluorescence spectrometry was used to determine the arsenic content in soil.

  15. Graphite furnace atomic absorption spectrometry as a routine method for the quantification of beryllium in blood and serum

    Directory of Open Access Journals (Sweden)

    Brousseau Pauline

    2008-07-01

    Full Text Available Abstract Background A routine method for the quantification of beryllium in biological fluids is essential for the development of a chelation therapy for Chronic Beryllium Disease (CBD. We describe a procedure for the direct determination of beryllium in undigested micro quantities of human blood and serum using graphite furnace atomic absorption spectrometry. Blood and serum samples are prepared respectively by a simple 8-fold and 5-fold dilution with a Nash Reagent. Three experimental setups are compared: using no modifier, using magnesium nitrate and using palladium/citric acid as chemical modifiers. Results In serum, both modifiers did not improve the method sensitivity, the optimal pyrolysis and atomization temperatures are 1000°C and 2900°C, respectively. In blood, 6 μg of magnesium nitrate was found to improve the method sensitivity. The optimal pyrolysis and atomization temperatures were 800°C and 2800°C respectively. Conclusion In serum, the method detection limit was 2 ng l-1, the characteristic mass was 0.22 (± 0.07 pg and the accuracy ranged from 95 to 100%. In blood, the detection limit was 7 ng l-1, the characteristic mass was 0.20 (± 0.02 pg and the accuracy ranged from 99 to 101%.

  16. A highly sensitive method for the determination of mercury using vapor generation gold wire microextraction and electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The study introduces a new simple and highly sensitive method for headspace solid phase microextraction (HS-SPME) coupled with electrothermal atomic absorption spectrometric determination of mercury. In the proposed method, a gold wire, mounted in the headspace of a sample solution in a sealed bottle, is used for collection of mercury vapor generated by addition of sodium tetrahydroborate. The gold wire is then simply inserted in the sample introduction hole of a graphite furnace of an electrothermal atomic absorption spectrometry instrument. By applying an atomization temperature of 600 deg. C, mercury is rapidly desorbed from the wire and determined with high sensitivity. Factorial design and response surface analysis methods were used for optimization of the effect of five different variables in order to maximize the mercury signal. By using a 0.75 mm diameter gold wire, a sample volume of about 8 ml and an extraction time of 11 min, the sensitivity of mercury determination was enhanced up to 104 times in comparison to its ordinary ETAAS determination with direct injection of 10 μl sample solutions. A detection limit of 0.006 ng ml-1 and a precision better than 4.6% (relative standard deviation) were obtained. The method was successfully applied to the determination of mercury in industrial wastewaters and tuna fish samples

  17. A highly sensitive method for the determination of mercury using vapor generation gold wire microextraction and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hashemi, Payman [Department of Chemistry, Lorestan University, Khorram Abad (Iran, Islamic Republic of)], E-mail: payman_hashemi@yahoo.com; Rahimi, Akram [Department of Chemistry, Lorestan University, Khorram Abad (Iran, Islamic Republic of)

    2007-04-15

    The study introduces a new simple and highly sensitive method for headspace solid phase microextraction (HS-SPME) coupled with electrothermal atomic absorption spectrometric determination of mercury. In the proposed method, a gold wire, mounted in the headspace of a sample solution in a sealed bottle, is used for collection of mercury vapor generated by addition of sodium tetrahydroborate. The gold wire is then simply inserted in the sample introduction hole of a graphite furnace of an electrothermal atomic absorption spectrometry instrument. By applying an atomization temperature of 600 deg. C, mercury is rapidly desorbed from the wire and determined with high sensitivity. Factorial design and response surface analysis methods were used for optimization of the effect of five different variables in order to maximize the mercury signal. By using a 0.75 mm diameter gold wire, a sample volume of about 8 ml and an extraction time of 11 min, the sensitivity of mercury determination was enhanced up to 10{sup 4} times in comparison to its ordinary ETAAS determination with direct injection of 10 {mu}l sample solutions. A detection limit of 0.006 ng ml{sup -1} and a precision better than 4.6% (relative standard deviation) were obtained. The method was successfully applied to the determination of mercury in industrial wastewaters and tuna fish samples.

  18. [Determination of aluminum in wheat flour food by microwave digestion-high resolution continuum source graphite furnace atomic absorption spectrometry].

    Science.gov (United States)

    Ren, Ting; Zhao, Li-jiao; Zhong, Ru-gang

    2011-12-01

    The contents of aluminum (Al) in four kinds of wheat flour food (noodle, dumpling wrapper, twisted cruller and soda biscuit) were determined by high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) combined with microwave digestion. The samples were completely digested by the mixture of HNO3 and H2O2 in closed polytetrafluoroethylene (PTFE) vessels. The conditions for microwave digestion, pyrolysis temperature and atomization temperature were optimized. The optimum experimental conditions were determined as follows. The microwave digestion was performed with HNO3/H2O2 7:1 (volume ratio), microwave power 1000 W and 190 degrees C for 40 minutes. The optimum pyrolysis temperature was 1350 degrees C and the optimum atomization temperature was 2400 degrees C. Magnesium nitrate solution with the concentration of 1 g x L(-1) was used as the matrix modifier. The correlation coefficient for the standard curve was 0.9999, the relative standard deviation (RSD) was from 1.7% to 2.4%, and the recovery for the samples was from 98.16% to 102.67%. The assay method for the determination of Al in wheat flour food established in this study has referential importance for the constituent of the correlated food standards. PMID:22295801

  19. Direct determination of P in biodiesel by high-resolution continuum source graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The direct determination of P in biodiesel by high-resolution continuum source graphite furnace atomic absorption spectrometry has been investigated. A slow drying stage proved to be essential for good repeatability. Optimization was performed by a D optimal planning. The atomization temperature and modifier composition were the most relevant parameters. Thus, using a mixture of Pd (30 μg) and Mg(NO3)2 (20 μg) as the modifier, previously deposited onto the platform of the graphite tube and dried, a five step drying stage, and pyrolysis and atomization temperatures of 1000 and 2700 deg. C, respectively, a limit of detection of 0.5 μg g-1 was obtained. The analysis of biodiesel of different origins confirmed that external calibration with organic P standard solutions, diluted in P-free biodiesel, could be used. In this way, excellent agreement between the found and expected results was observed in the analysis of an ANP interlaboratorial exercise sample.

  20. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    International Nuclear Information System (INIS)

    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−1 and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L−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

  1. Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Brombach, Christoph-Cornelius [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Chen, Bin; Corns, Warren T. [PS Analytical, Arthur House, Crayfields Industrial Estate, Main Road, Orpington, Kent BR5 3HP (United Kingdom); Feldmann, Jörg [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Krupp, Eva M., E-mail: e.krupp@abdn.ac.uk [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom)

    2015-03-01

    Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography–cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation. - Highlights: • We demonstrate that a novel mixture of thiourea-thiolsilica shows an excellent trapping of MeHg between a broad pH range 1–6. • We develop the method so that it can potentially be automated for inorganic and methyl-mercury. • The method is matrix independent with highly accurate results for MeHg in hair CRM extracts and spiked water samples • The limit of detection is around 40 pg/L when just 200 mL sample is used, without any intensive preparation.

  2. Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography–cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation. - Highlights: • We demonstrate that a novel mixture of thiourea-thiolsilica shows an excellent trapping of MeHg between a broad pH range 1–6. • We develop the method so that it can potentially be automated for inorganic and methyl-mercury. • The method is matrix independent with highly accurate results for MeHg in hair CRM extracts and spiked water samples • The limit of detection is around 40 pg/L when just 200 mL sample is used, without any intensive preparation

  3. Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    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 (ML2). 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 1.5 x 10-2 mol L-1, extraction temperature 40 deg. C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 μL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 μL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 μg L-1, relative standard deviation (RSD) 5.5% and the working linear range 2-30 μg L-1.

  4. Assessment of cadmium and iron adsorption in sediment, employing a flow injection analysis system with on line filtration and detection by flame atomic absorption spectrometry and thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •A FIA system with on-line filtration for isotherms adsorption studies was proposed. •Isotherms for iron and cadmium elements in bottom lake sediment were done. •Inferences about adsorption/desorption mechanisms were feasible. •The proposed method turns the isotherm studies fast and reliable. -- Abstract: This work presents an evaluation of iron and cadmium adsorption in sediment of the Furnas Hydroelectric Plant Reservatory located in Alfenas, Minas Gerais (Brazil). The metal determination was done employing a flow injection analysis (FIA) with an on-line filtering system. As detection techniques, flame atomic absorption spectrometry (FAAS) for iron and thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) for cadmium determinations were used. The developed methodology presented good limits of detection, being 190 μg L−1 for iron and 1.36 μg L−1 for cadmium, and high sampling frequency for both metals 144 and 60 readings h−1 for iron and cadmium, respectively. Both metals obey the Langmuir model, with maximum adsorptive capacity of 0⋅169 mg g−1 for iron and 7⋅991 mg g−1 for cadmium. For iron, a pseudo-first-order kinetic model was obtained with a theoretical Qe = 9⋅8355 mg g−1 (experimental Qe = 9⋅5432 mg g−1), while for cadmium, a pseudo-second-order kinetic model was obtained, with a theoretical Qe = 0.3123 mg g−1 (experimental Qe = 0⋅3052 mg g−1)

  5. 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.

  6. Ambient-Temperature Trap/Release of Arsenic by Dielectric Barrier Discharge and Its Application to Ultratrace Arsenic Determination in Surface Water Followed by Atomic Fluorescence Spectrometry.

    Science.gov (United States)

    Mao, Xuefei; Qi, Yuehan; Huang, Junwei; Liu, Jixin; Chen, Guoying; Na, Xing; Wang, Min; Qian, Yongzhong

    2016-04-01

    A novel dielectric barrier discharge reactor (DBDR) was utilized to trap/release arsenic coupled to hydride generation atomic fluorescence spectrometry (HG-AFS). On the DBD principle, the precise and accurate control of trap/release procedures was fulfilled at ambient temperature, and an analytical method was established for ultratrace arsenic in real samples. Moreover, the effects of voltage, oxygen, hydrogen, and water vapor on trapping and releasing arsenic by DBDR were investigated. For trapping, arsenic could be completely trapped in DBDR at 40 mL/min of O2 input mixed with 600 mL/min Ar carrier gas and 9.2 kV discharge potential; prior to release, the Ar carrier gas input should be changed from the upstream gas liquid separator (GLS) to the downstream GLS and kept for 180 s to eliminate possible water vapor interference; for arsenic release, O2 was replaced by 200 mL/min H2 and discharge potential was adjusted to 9.5 kV. Under optimized conditions, arsenic could be detected as low as 1.0 ng/L with an 8-fold enrichment factor; the linearity of calibration reached R(2) > 0.995 in the 0.05 μg/L-5 μg/L range. The mean spiked recoveries for tap, river, lake, and seawater samples were 98% to 103%; and the measured values of the CRMs including GSB-Z50004-200431, GBW08605, and GBW(E)080390 were in good agreement with the certified values. These findings proved the feasibility of DBDR as an arsenic preconcentration tool for atomic spectrometric instrumentation and arsenic recycling in industrial waste gas discharge. PMID:26976077

  7. Determination of Mercury in Milk by Cold Vapor Atomic Fluorescence: A Green Analytical Chemistry Laboratory Experiment

    Science.gov (United States)

    Armenta, Sergio; de la Guardia, Miguel

    2011-01-01

    Green analytical chemistry principles were introduced to undergraduate students in a laboratory experiment focused on determining the mercury concentration in cow and goat milk. In addition to traditional goals, such as accuracy, precision, sensitivity, and limits of detection in method selection and development, attention was paid to the…

  8. Simultaneous determination of cadmium, iron and tin in canned foods using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Leao, Danilo J; Junior, Mario M S; Brandao, Geovani C; Ferreira, Sergio L C

    2016-06-01

    A method was established to simultaneously determine cadmium, iron and tin in canned-food samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). The quantification step has been performed using the primary line (228.802nm) for cadmium and the adjacent secondary lines (228.725nm and 228.668nm) for iron and tin, respectively. The selected chemical modifier was an acid solution that contained a mixture of 0.1% (w/v) Pd and 0.05% (w/v) Mg. The absorbance signals were measured based on the peak area using 3 pixels for cadmium and 5 pixels for iron and tin. Under these conditions, cadmium, iron and tin have been determined in canned-food samples using the external calibration technique based on aqueous standards, where the limits of quantification were 2.10ngg(-1) for cadmium, 1.95mgkg(-1) for iron and 3.00mgkg(-1) for tin, and the characteristic masses were 1.0pg for cadmium, 0.9ng for iron and 1.1ng for tin. The precision was evaluated using two solutions of each metal ion, and the results, which were expressed as the relative standard deviation (RSD%), were 3.4-6.8%. The method accuracy for cadmium and iron was confirmed by analyzing a certified reference material of apple leaves (NIST 1515), which was supplied by NIST. However, for tin, the accuracy was confirmed by comparing the results of the proposed method and another analytical technique (inductively coupled plasma optical emission spectrometry). The proposed procedure was applied to determine cadmium, iron and tin in canned samples of peeled tomato and sardine. Eleven samples were analyzed, and the analyte concentrations were 3.57-62.9ngg(-1), 2.68-31.48mgkg(-1) and 4.06-122.0mgkg(-1) for cadmium, iron and tin, respectively. In all analyzed samples, the cadmium and tin contents were lower than the permissible maximum levels for these metals in canned foods in the Brazilian legislation. PMID:27130088

  9. Electron impact ionization and excitation of laser-excited atoms: investigation by means of electron spectrometry

    International Nuclear Information System (INIS)

    We have measured the electron spectra following the excitation and ionization of laser-excited atoms by impact of 1.5 keV electrons: 2p excitation and 2s ionization of Na(3p3/2), 1s excitation of Li(2p3/2) and 5p ionization of Ba(6s5d 1,3D). Except for Ba the intensities of ejected electrons are directly proportional to the cross sections of Auger and autoionizing states. Theoretical excitation cross sections (Na 2p, Li 1s) are obtained in first Born approximation including the full relaxation of the atomic electrons. Relative ionization cross sections (Na 2s, Ba 5p) are evaluated in sudden approximation as a two-step process: pure 2s(5p) ionization plus relaxation of the rest of the atomic electrons. The experimental spectra are compared to theoretical spectra

  10. Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

    International Nuclear Information System (INIS)

    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

  11. Determination of PASHs by various analytical techniques based on gas chromatography-mass spectrometry: application to a biodesulfurization process.

    Science.gov (United States)

    Mezcua, Milagros; Fernández-Alba, Amadeo R; Boltes, Karina; Alonso Del Aguila, Raul; Leton, Pedro; Rodríguez, Antonio; García-Calvo, Eloy

    2008-06-15

    . Recoveries of the selected compound in both media were studied. They were in the range of 80-100% for the watery and in the range of 40-60% for the organic phase, respectively. Gas chromatography coupled to mass spectrometry (GC-MS) has been employed for the identification of these selected compounds. Three different ionization modes were applied: conventional electron impact (EI); positive chemical ionization (PCI), using methane as the reagent gas; and a recently developed ionization mode known as hybrid chemical ionization (HCI), using perfluorotri-n-butylamine as the reagent gas. Limits of detection and identification capabilities have been compared between the three analytical techniques. The sensitivity of the three analytical techniques was studied and LOD between 0.05 and 1, between 0.09 and 2 and between 0.001 and 0.043 were achieved for PCI, EI and HCI, respectively. The developed method was applied in samples from a biodesulfurization process. The biodesulfurization reactions were conducted in resting cell operation mode, using Erlenmeyer flasks or an agitated tank bioreactor. The microorganism employed was Pseudomonas putida CECT 5279. The reaction was performed under controlled air flow, stirring and temperature conditions. PMID:18585197

  12. Analysis of neodymium oxide for rare earth impurities by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    A procedure for the determination of the rare earths elements in neodymium oxide with purity grade above 99% by inductively coupled plasma optical emission spectrometry is described. Determination limits were 0,005% for the elements Eu, Dy, Gd, Tb, Ho and Y and 0,01% for Sm and La. The precision of the method was evaluated through the relative standard deviation (RSD) for individual rare earth elements. The values lies in the range of 3 -7% for most of them but lanthanum, has shown 13% RSD. (author)

  13. Feasibility guidelines for kaonic-atom experiments with ultra-high-resolution X-ray spectrometry

    CERN Document Server

    Friedman, E

    2013-01-01

    Recent studies of strong interaction effects in kaonic atoms suggest that analysing so-called `lower' and `upper' levels in the same atom could separate one-nucleon absorption from multinucleon processes. The present work examines the feasibility of direct measurements of upper level widths in addition to lower level widths in future experiments, using superconducting microcalorimeter detectors. About ten elements are identified as possible candidates for such experiments, all of medium-weight and heavy nuclei. New experiments focused on achieving good accuracy for widths of such pairs of levels could contribute significantly to our knowledge of the $K^-$-nucleon interaction in the nuclear medium.

  14. Assessment of elemental pollution in soil of Islamabad city using instrumental neutron activation analysis and atomic absorption spectrometry techniques

    Energy Technology Data Exchange (ETDEWEB)

    Daud, M.; Wasim, M.; Khalid, N.; Zaidi, J.H. [Pakistan Institute of Nuclear Science and Technology, Islamabad (Pakistan). Chemistry Div.; Iqbal, J. [University of the Punjab, Lahore (Pakistan). Inst. of Chemistry

    2009-07-01

    The soil samples of nine different sites in Islamabad were studied for their elemental composition. Instrumental neutron activation analysis and atomic absorption spectrometry were employed and 33 elements were determined. The acquired data were analyzed using descriptive statistics, principal component analysis, cluster analysis, pollution level index and enrichment factor. A perusal of results shows a distribution of elemental concentration in two major groups, one along the highway and the other in industrial area of Islamabad. The soil along the highway sites was found to be relatively less polluted than at the sites in the industrial area. The enrichment factor indicates the presence of As, Pb, Sb, Se and Sn at higher levels. The method validation was done by analyzing IAEA reference materials SL-1 (lake sediment) and S7 (soil). (orig.)

  15. Determination of boron in the waters of Troia by inductively coupled plasma-atomic emission spectrometry (ICP-AES

    Directory of Open Access Journals (Sweden)

    HASAN OZCAN

    2005-10-01

    Full Text Available The inductively coupled plasma-atomic emission spectrometry method (ICP-EAS is proposed for the determination of boron in Troia water sources. In this study, boron samples were taken from 25 different locations during November 2002 and May 2003. The 249.773 nm boron emmision line was not affected by the samplematrix. The boron content was determined without further pretreatment of samples proposed ICP-AES method. An analysis of a given sample was completed in about 15 min. The determined boron concentrations in surface and ground water sources were between 0.00444–1.11200mgl-1. Inorder to compare the results obtained by the proposed method, selected water samples were also analysed titrimetically. Pearson correlation coefficient analysis showed that there is a close relationship between the ICP-AES and the titrimetric method and the determination coefficient (R2 was calculated to be 91.34 %.

  16. Atmospheric deposition of heavy metals studied by analysis of moss samples using neutron activation analysis and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    In a study of the atmospheric deposition of trace elements in different parts of Norway samples of the moss Hylocomium splendens were analyzed with respect to 26 elements. The determination of Cu, Zn, Pb, Cd and Ni was carried out by flame atomic absorption spectrometry, while an additional 21 elements were determined by instrumental neutron activation analysis. Several elements showed a substantially higher deposition in the southernmost parts of Norway than in places located farther north. As regards Pb, As and Sb, the difference amounted to a factor of ten or more. A similar but less pronounced trend was evident for elements such as V, Zn, Cd, Se and Ag. In some cases local pollution sources or marine aerosols had a significant effect on the results. For several heavy metals however long-distance transport from areas to the south and the south west of Norway was responsible for a major part of the air pollution

  17. Acid dissolution of soils and rocks for the determination of boron by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    The boron concentration in rocks, soils and standard reference materials was determined using hydrofluoric acid-aqua regia dissolution followed by inductively coupled plasma atomic emission spectrometry (ICP-AES) using the B 1 249.773 -nm line, corrected for spectral interference by iron. An excess of fluoride was complexed with aluminium to release boron from the stable fluoroborate ion and to protect the borosilicate and quartz components of the instrument. Boron was not lost by volatilisation during volume reduction. Soil and rock boron values determined using the recommended dissolution procedures were comparable to those obtained using the accepted sodium carbonate fusion procedure and by d.c. arc emission spectrophotometry, and those for standard reference materials showed good agreement and precision with the literature values. (author)

  18. Rapid determination of major and minor elements in rare earth-cobalt magnets by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Major and minor constituents, Sm, Ce, Y, Co, Fe, Mn, Cu, Zr and Hf, in typical rare earth-cobalt magnets were determined sequentially by inductively coupled plasma atomic emission spectrometry. Sample solutions were prepared by dissolving the magnets with aqua regia followed by dilution with 1.2 M HCl to suitable concentration. Beryllium was added as an internal standard in order to improved experimental accuracy and precision, and the emission intensity of Be was measured by using an additional small monochromator attached to the original instrument system. Cobalt, Fe, Cu and Zr in the magnets were also determined by conventional spectrophotometry. The results obtained by both methods were in good agreement with each other. (author)

  19. Determination of mercury by electrochemical cold vapor generation atomic fluorescence spectrometry using polyaniline modified graphite electrode as cathode

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Xianjuan [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Gan Wuer, E-mail: wgan@ustc.edu.c [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Wan Lingzhong; Zhang Hanchang; He Youzhao [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China)

    2010-02-15

    An electrochemical cold vapor generation system with polyaniline modified graphite electrode as cathode material was developed for Hg (II) determination by coupling with atomic fluorescence spectrometry. This electrochemical cold vapor generation system with polyaniline/graphite electrode exhibited higher sensitivity; excellent stability and lower memory effect compared with graphite electrode electrochemical cold vapor generation system. The relative standard deviation was 2.7% for eleven consecutive measurements of 2 ng mL{sup -1} Hg (II) standard solution and the mercury limit of detection for the sample blank solution was 1.3 rg mL{sup -1} (3sigma). The accuracy of the method was evaluated through analysis of the reference materials (GBW09101) (Human hair) and GBW (08517) (Laminaria Japonica Aresch) and the proposed method was successfully applied to the analysis of human hairs.

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

    International Nuclear Information System (INIS)

    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)

  1. Achieving 100% Efficient Postcolumn Hydride Generation for As Speciation Analysis by Atomic Fluorescence Spectrometry

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2016-01-01

    Roč. 88, APR (2016), s. 4041-4047. ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * HPLC Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

  2. The direct determination of HgS by thermal desorption coupled with atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Coufalík, Pavel; Zvěřina, O.; Komárek, J.

    2016-01-01

    Roč. 118, APR (2016), s. 1-5. ISSN 0584-8547 R&D Projects: GA ČR GAP503/12/0682 Institutional support: RVO:68081715 Keywords : mercury * HgS * thermal desorption Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.176, year: 2014

  3. Achieving 100% Efficient Postcolumn Hydride Generation for As Speciation Analysis by Atomic Fluorescence Spectrometry

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2016-01-01

    Roč. 88, - (2016), s. 4041-4047. ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * HPLC Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 5.636, year: 2014

  4. UV-assisted Fenton digestion of rice for the determination of trace cadmium by hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Yu, Huimin; Ai, Xi; Xu, Kailai; Zheng, Chengbin; Hou, Xiandeng

    2016-02-21

    A new digestion method using UV-assisted Fe(0) Fenton reaction was developed for the determination of trace Cd in rice by hydride generation atomic fluorescence spectrometry. The proposed method integrated the advantages of simplicity, small dose of reagents, low cost and moderate reaction conditions, and was successfully utilized to analyze a Certified Reference Material (CRM) and real rice samples. A 1 mL mixture of the sample and reagents (0.0500 g rice powder, 0.2% (m/v) Fe(0), 0.75% (v/v) HNO3 and 18% (v/v) H2O2) was irradiated by UV-light for 50 min and then a clear solution was obtained by separating excess Fe(0) with a magnet prior to spectral analysis. The limit of detection (LOD) for Cd was found to be 0.02 mg kg(-1) and the relative standard deviation was better than 5.0% at a concentration level of 0.40 mg kg(-1). The recovery obtained by analyzing the CRM was 103% and spiked recoveries with 0.40 mg kg(-1) Cd in rice samples were 93% and 101%. The t-test proved that there is no significant difference between the certified value and the determined value of the CRM, and between the proposed method and microwave-assisted digestion coupled with inductively coupled plasma mass spectrometry (MWD-ICP-MS) at 95% confidence level. PMID:26759832

  5. Analytical approach for the determination of steroid profile of humans by gas chromatography isotope ratio mass spectrometry aimed at distinguishing between endogenous and exogenous steroids.

    Science.gov (United States)

    Bulska, Ewa; Gorczyca, Damian; Zalewska, Izabela; Pokrywka, Andrzej; Kwiatkowska, Dorota

    2015-03-15

    The contamination of commonly used supplements by unknown steroids as well as their metabolites (parent compounds) become a challenge for the analytical laboratories. Although the determination of steroids profile is not trivial because of the complex matrix and low concentration of single compound, one of the most difficult current problem is to distinguish, during analytical procedure, endogenous androgens such as testosterone, dehydrotestosterone or dehydroepiandrosterone from their synthetic equivalents. The aim of this work was to develop and validate an analytical procedure for determination of the steroid profile in human urine by gas chromatography-combustion-isotope ratio mass spectrometry (GC/C/IRMS) toward distinguishing between endogenous and exogenous steroids. Beside the optimization of the experimental parameters for gas chromatography separation and mass spectrometry, attention was focused on urine sample preparation. Using an optimized sample preparation protocol it was possible to achieve better chromatographic resolutions and better sensitivity enabling the determination of 5 steroids, androsterone, etiocholanolone, testosterone, 5-androstandiol, 11-hydroxyandrdostane, pregnandiol, with the expanded uncertainty (k=2) below 1‰. This enable to evaluate the significant shift of the δ(13)C/(12)C [‰] values for each of examined steroids (excluding ERC). The analytical protocol described in this work was successfully used for the confirmation of positive founding urine by evaluation T/E ratio after GC/C/IRMS analysis. PMID:25498150

  6. Flotation separation of iron, copper and lead in environmental samples and their determination by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. Some of the heavy metals are among the most harmful of the elemental pollutants and are of particular concern because of their toxicities to humans. Heavy metals include essential elements like iron as well as toxic metals like cadmium and mercury. Direct determination of trace heavy metals, by flame atomic absorption spectrometry (FAAS) or electrothermal atomic spectrometry (ETAAS) is not possible, because of their low concentrations and matrix effects. In order to know the accurate concentrations of trace heavy metals, enrichment processes are necessary. The most common, simple, rapid, low cost and effective method used for preconcentration is flotation. Only a small amount of surfactant, collector agent and tiny air bubbles is required to perform the proper flotation. Most of them have a tremendous affinity for sulfur and disrupt enzyme function by forming bonds with sulfur groups in enzymes. In this work a simple, sensitive and accurate procedure for flotation separation followed by ETAAS determination of Fe, Cu and Pb is proposed. 2-(2-methoxy phenyl) benzimidazole was used as the new collector agent. The optimum conditions of flotation were studied and important parameters were optimized. The experiment was done at pH =5. The linear ranges are 0-58, 0.350, 0-28 μg L-1 for Fe, Cu, and Pb respectively. The detection limits of the method for Fe, Cu and Pb are 0.08, 0.001, 0.08 μg L-1 respectively. This method was successfully applied for separation and determination of Cu, Pb and Fe in some environmental samples.

  7. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    International Nuclear Information System (INIS)

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 deg. C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 deg. C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g-1

  8. Nonthermal Optical Emission Spectrometry: Direct Atomization and Excitation of Cadmium for Highly Sensitive Determination.

    Science.gov (United States)

    Cai, Yi; Zhang, Ya-Jie; Wu, De-Fu; Yu, Yong-Liang; Wang, Jian-Hua

    2016-04-19

    The low atomization and excitation capability of nonthermal microplasma, e.g., dielectric barrier discharge (DBD), has greatly hampered its potential applications for the determination of metals in solution. In the present work, an inspiring development is reported for direct atomization and excitation of cadmium in aqueous solution by DBD and facilitates highly sensitive determination. A DBD microplasma is generated on the nozzle of a pneumatic micronebulizer to focus the DBD energy on a confined space and atomize/excite metals in the spray. Meanwhile, an appropriate sample matrix and nebulization in helium further improves the atomization and excitation capability of DBD. With cadmium as a model, its emission is recorded by a CCD spectrometer at 228.8 nm. By using an 80 μL sample solution nebulized at 3 μL s(-1), a linear range of 5-1000 μg L(-1) along with a detection limit of 1.5 μg L(-1) is achieved, which is comparable to those obtained by commercial bulky inductively coupled plasma (ICP)-based instrumentations. PMID:27030025

  9. Analytical procedure for mapping the distribution of 10B and 99Tc markers in cryo-sections of animal tissue samples by secondary ion mass spectrometry

    International Nuclear Information System (INIS)

    The development of a complete, standard analytical procedure for a quantitative use of secondary ion mass spectrometry to map the distribution in animal tissues of exogenous isotopes presents difficulties inherently related to sample preparation and preservation, as well as to the specific application being considered. We have tested in two very different cases a procedure based on the cryo-preparation of samples and calibration standards. The applications under investigation were the mapping of 10B in mouse brain tissue, with relevance to the boron neutron capture therapy, and of the perfusion tracer 99Tc in mouse heart tissue, with relevance to the study of microcirculation and cardiovascular pathologies. Scanning electron microscopy and inductively coupled mass spectrometry analysis were used as reference techniques for secondary ion mass spectrometry images and analyte measurements, respectively. Cryo-preparation of tissue sections for ion microscopy proved to be simple and efficient (in terms of structural and chemical integrity) for both brain and heart samples derived from fresh organs. This technique, however, turned out to be reliable only on the brain tissue when applied to the preparation of standards, which required chemical fixation of portions of organs. Brain and heart tissues showed a totally different response to chemical fixation, from both a structural and an analytical point of view. On the one hand, we were able to estimate a relative sensitivity factor for 10B in the cryo-sectioned brain matrix; on the other hand, even without the possibility of an absolute quantification of the 99Tc signal and notwithstanding the presence of an isobaric interference, secondary ion mass spectrometry mapping however proved to be capable to resolve the specific response of the cardiac tissue to the perfusion mechanism.

  10. Analytical procedure for mapping the distribution of 10B and 99Tc markers in cryo-sections of animal tissue samples by secondary ion mass spectrometry

    Science.gov (United States)

    Marchetti, Ilaria; Menichetti, Luca; Kusmic, Claudia; de las Heras, Laura Aldave; Salvadori, Piero; Fuoco, Roger; Belloni, Fabio; L'Abbate, Antonio; Betti, Maria

    2009-09-01

    The development of a complete, standard analytical procedure for a quantitative use of secondary ion mass spectrometry to map the distribution in animal tissues of exogenous isotopes presents difficulties inherently related to sample preparation and preservation, as well as to the specific application being considered. We have tested in two very different cases a procedure based on the cryo-preparation of samples and calibration standards. The applications under investigation were the mapping of 10B in mouse brain tissue, with relevance to the boron neutron capture therapy, and of the perfusion tracer 99Tc in mouse heart tissue, with relevance to the study of microcirculation and cardiovascular pathologies. Scanning electron microscopy and inductively coupled mass spectrometry analysis were used as reference techniques for secondary ion mass spectrometry images and analyte measurements, respectively. Cryo-preparation of tissue sections for ion microscopy proved to be simple and efficient (in terms of structural and chemical integrity) for both brain and heart samples derived from fresh organs. This technique, however, turned out to be reliable only on the brain tissue when applied to the preparation of standards, which required chemical fixation of portions of organs. Brain and heart tissues showed a totally different response to chemical fixation, from both a structural and an analytical point of view. On the one hand, we were able to estimate a relative sensitivity factor for 10B in the cryo-sectioned brain matrix; on the other hand, even without the possibility of an absolute quantification of the 99Tc signal and notwithstanding the presence of an isobaric interference, secondary ion mass spectrometry mapping however proved to be capable to resolve the specific response of the cardiac tissue to the perfusion mechanism.

  11. Analytical procedure for mapping the distribution of {sup 10}B and {sup 99}Tc markers in cryo-sections of animal tissue samples by secondary ion mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Marchetti, Ilaria [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany); Menichetti, Luca [National Research Council, Institute of Clinical Physiology, via G. Moruzzi, 1, 56124 Pisa (Italy)], E-mail: luca.m@ifc.cnr.it; Kusmic, Claudia [National Research Council, Institute of Clinical Physiology, via G. Moruzzi, 1, 56124 Pisa (Italy); Aldave de las Heras, Laura [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany); Salvadori, Piero [National Research Council, Institute of Clinical Physiology, via G. Moruzzi, 1, 56124 Pisa (Italy); Fuoco, Roger [University of Pisa, Department of Chemistry and Industrial Chemistry, via Risorgimento, 35, 56126 Pisa (Italy); Belloni, Fabio [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany)], E-mail: fabio.belloni@ec.europa.eu; L' Abbate, Antonio [Scuola Superiore Sant' Anna, P.zza Martiri della Liberta, 33, 56127 Pisa (Italy); Betti, Maria [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany); International Atomic Energy Agency, IAEA-MEL Laboratories, MC 98000 Montecarlo, Principality of Monaco (Monaco)

    2009-09-15

    The development of a complete, standard analytical procedure for a quantitative use of secondary ion mass spectrometry to map the distribution in animal tissues of exogenous isotopes presents difficulties inherently related to sample preparation and preservation, as well as to the specific application being considered. We have tested in two very different cases a procedure based on the cryo-preparation of samples and calibration standards. The applications under investigation were the mapping of {sup 10}B in mouse brain tissue, with relevance to the boron neutron capture therapy, and of the perfusion tracer {sup 99}Tc in mouse heart tissue, with relevance to the study of microcirculation and cardiovascular pathologies. Scanning electron microscopy and inductively coupled mass spectrometry analysis were used as reference techniques for secondary ion mass spectrometry images and analyte measurements, respectively. Cryo-preparation of tissue sections for ion microscopy proved to be simple and efficient (in terms of structural and chemical integrity) for both brain and heart samples derived from fresh organs. This technique, however, turned out to be reliable only on the brain tissue when applied to the preparation of standards, which required chemical fixation of portions of organs. Brain and heart tissues showed a totally different response to chemical fixation, from both a structural and an analytical point of view. On the one hand, we were able to estimate a relative sensitivity factor for {sup 10}B in the cryo-sectioned brain matrix; on the other hand, even without the possibility of an absolute quantification of the {sup 99}Tc signal and notwithstanding the presence of an isobaric interference, secondary ion mass spectrometry mapping however proved to be capable to resolve the specific response of the cardiac tissue to the perfusion mechanism.

  12. Analytical investigation of the feasibility of sacrificial microchannel sealing for Chip-Scale Atomic Magnetometers

    OpenAIRE

    Tsujimoto, Kazuya; Hirai, Yoshikazu; Sugano, Koji; Tsuchiya, Toshiyuki; TABATA, Osamu

    2014-01-01

    An alkali metal vapor cell is a crucial component of the highly sensitive Chip Scale Atomic Magnetometers (CSAMs) that are increasingly deployed in a variety of electronic devices. Herein, we propose a novel microfabrication technique utilizing an array of microchannels at a bonded interface, to enable gas feedthrough for evacuation of unwanted gases from a vapor cell and subsequent introduction of an inert gas, followed by permanent sealing of the microchannels by reflow of a glass frit. The...

  13. Sputtering of copper atoms by keV atomic and molecular ions A comparison of experiment with analytical and computer based models

    CERN Document Server

    Gillen, D R; Goelich,

    2002-01-01

    Non-resonant multiphoton ionisation combined with quadrupole and time-of-flight analysis has been used to measure energy distributions of sputtered copper atoms. The sputtering of a polycrystalline copper target by 3.6 keV Ar sup + , N sup + and CF sub 2 sup + and 1.8 keV N sup + and CF sub 2 sup + ion bombardment at 45 deg. has been investigated. The linear collision model in the isotropic limit fails to describe the high energy tail of the energy distributions. However the TRIM.SP computer simulation has been shown to provide a good description. The results indicate that an accurate description of sputtering by low energy, molecular ions requires the use of computer simulation rather than analytical approaches. This is particularly important when considering plasma-surface interactions in plasma etching and deposition systems.

  14. Use of atomic absorption spectrometry to determine metallic impurities in coal

    International Nuclear Information System (INIS)

    The Brazilian Energetic Alternative Program expects the reduction of our dependence on foreign energy sources, by replacing fuel oil by mineral coal. Its gasification by means of nuclear energy must be also considered. However, the intensive burning of coal leads to serious environmental problems. During its combustion the release to atmosphere of toxic elements such as As, Hg, Pb, Zn and others is of great concern. Hence, it is important to have reliable analytical methods which can monitor inorganic constituents at various stages of coal production and utilization. The AAS is a suitable analytical technique to determine pollutants in coal because it is sensitive, simple, economic and cover a large range of concentration. The need of a previous treatment of sample is overcome by using an acid attack (HNO3 + HClO4 + HF) which has been proved to be rapid and efficient. (Author)

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

    International Nuclear Information System (INIS)

    Soybean hull was chemically modified with citric acid and used as a solid phase extraction adsorbent for the determination of trace amounts of Cu2+ 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 Cu2+ could be adsorbed on the modified soybean hull at pH 8.0 and eluted by 2.0 mL of 1.0 mol L-1 HCl. Under the optimized conditions, the adsorption capacity of modified soybean hull was found to be 18.0 mg g-1 for Cu2+. The detection limit of the proposed method was 0.8 ng mL-1 for Cu2+ 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 Cu2+ in dried sweet potato, lake water and milk powder, the recovery of Cu2+ for spiked samples was between 91% and 109.6%.

  16. 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%.

  17. Minimization of detection limits in arsenic speciation analysis by hydride generation - cryogenic trapping - atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Matoušek, Tomáš; Stýblo, M.; Rychlovský, P.; Dědina, Jiří

    Xiamen: Xiamen University Press, 2007. s. 77. [Colloquium Spectroscopicum Internationale /35./. 23.09.2007-27.09.2007, Xiamen] R&D Projects: GA AV ČR IAA400310507 Grant ostatní: NIH-FIRCA(US) 1 R03 TW007057-01 Institutional research plan: CEZ:AV0Z40310501 Keywords : cryogenic trapping * arsenic speciation * hydride generation Subject RIV: CB - Analytical Chemistry, Separation

  18. Arsenic speciation analysis by hydride generation - cryogenic trapping - atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Matoušek, Tomáš; Stýblo, M.; Rychlovský, P.; Dědina, Jiří

    Lednice: Spektroskopická společnost Jana Marka Marci, 2007. s. 80. ISBN 80-903732-2-4. [Spektroskopická konference /13./. 18.06.2007-21.06.2007, Lednice] R&D Projects: GA AV ČR IAA400310507 Grant ostatní: NIH-FIRCA(US) 1 R03 TW007057-01 Institutional research plan: CEZ:AV0Z40320502 Keywords : cryogenic trapping * arsenic speciation * hydride generation Subject RIV: CB - Analytical Chemistry, Separation

  19. Determination of trace elements in heroin by inductively coupled plasma atomic emission spectrometry using ultrasonic nebulization

    Science.gov (United States)

    Budič, Bojan; Klemenc, Sonja

    2000-06-01

    A method for the determination of Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Ni, P, S, Sr and Zn in heroin samples by ICP-AES using ultrasonic nebulization is described. The samples were microwave digested with HNO 3. To improve the detection limits and minimise the matrix interferences the experimental parameters were optimised by variation of the operating power, carrier gas flow rate and observation height above the load coil. Optimum operating conditions for most of the analytes were at operating power 1550 W, carrier gas flow rate between 0.8 and 1.0 l min -1 and observation height between 10 and 12 mm above load coil. The limits of detection were below 0.5 μg g -1 (dry mass) for most of the elements investigated. The analytical recoveries of spiked samples were in the range between 94 and 103% and precision was on average better than 6%. The analysis of heroin samples shows that the method is simple, rapid and capable of providing accurate results for all the analytes investigated with the exception of nickel which was below the limit of detection in the analyzed samples.

  20. X-Ray Microanalysis and Electron Energy Loss Spectrometry in the Analytical Electron Microscope: Review and Future Directions

    Science.gov (United States)

    Goldstein, J. I.; Williams, D. B.

    1992-01-01

    This paper reviews and discusses future directions in analytical electron microscopy for microchemical analysis using X-ray and Electron Energy Loss Spectroscopy (EELS). The technique of X-ray microanalysis, using the ratio method and k(sub AB) factors, is outlined. The X-ray absorption correction is the major barrier to the objective of obtaining I% accuracy and precision in analysis. Spatial resolution and Minimum Detectability Limits (MDL) are considered with present limitations of spatial resolution in the 2 to 3 microns range and of MDL in the 0.1 to 0.2 wt. % range when a Field Emission Gun (FEG) system is used. Future directions of X-ray analysis include improvement in X-ray spatial resolution to the I to 2 microns range and MDL as low as 0.01 wt. %. With these improvements the detection of single atoms in the analysis volume will be possible. Other future improvements include the use of clean room techniques for thin specimen preparation, quantification available at the I% accuracy and precision level with light element analysis quantification available at better than the 10% accuracy and precision level, the incorporation of a compact wavelength dispersive spectrometer to improve X-ray spectral resolution, light element analysis and MDL, and instrument improvements including source stability, on-line probe current measurements, stage stability, and computerized stage control. The paper reviews the EELS technique, recognizing that it has been slow to develop and still remains firmly in research laboratories rather than in applications laboratories. Consideration of microanalysis with core-loss edges is given along with a discussion of the limitations such as specimen thickness. Spatial resolution and MDL are considered, recognizing that single atom detection is already possible. Plasmon loss analysis is discussed as well as fine structure analysis. New techniques for energy-loss imaging are also summarized. Future directions in the EELS technique will be