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

Science.gov (United States)

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

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

Science.gov (United States)

Kowalewska, Zofia

2011-07-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-07-15

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

Spectral interferences in atomic absorption spectrometry, (5)

International Nuclear Information System (INIS)

Daidoji, Hidehiro

1979-01-01

Spectral interferences were observed in trace element analysis of concentrated solutions by atomic absorption spectrometry. Molecular absorption and emission spectra for strontium chloride and nitrate, barium chloride and nitrate containing 12 mg/ml of metal ion in airacetylene flame were measured in the wavelength range from 200 to 700 nm. The absorption and emission spectra of SrO were centered near 364.6 nm. The absorption spectra of SrOH around 606.0, 671.0 and 682.0 nm were very strong. And, emission spectrum of BaOH in the wavelength range from 480 to 550 nm was stronger. But, the absorption of this band spectrum was very weak. In the wavelength range from 200 to 400 nm, some unknown bands of absorption were observed for strontium and barium. Absorption spectra of SrCl and BaCl were observed in the argon-hydrogen flame. Also, in the carbon tube atomizer, the absorption spectra of SrCl and BaCl were detected clearly in the wavelength range from 185 to 400 nm. (author)

Molecular absorption spectrometry in flames and furnaces: A review

Energy Technology Data Exchange (ETDEWEB)

Butcher, David J., E-mail: butcher@email.wcu.edu

2013-12-04

Graphical abstract: -- Highlights: •Theory and analytical considerations for molecular absorption spectrometry (MAS). •Critical review of low resolution MAS. •Critical review of the analytical performance of high-resolution continuum source (HR-CS) flame MAS. •Critical review of the analytical performance of HR-CS graphite furnace MAS. •Current status of HR-CS MAS and its future prospects for elemental analysis. -- Abstract: Molecular absorption spectrometry (MAS), originally developed in the 1970s, is a technique to determine non-metals in flames and graphite furnaces by monitoring the absorbance of diatomic molecules. Early studies employed low resolution instruments designed for line source atomic absorption, which provided a limited choice of analytical wavelengths, insufficient spectral resolution, and spectral interferences. However, the development of high-resolution continuum source atomic absorption spectrometry (HR-CS AAS) instrumentation has allowed the analysis of challenging samples for non-metals as well as some difficult elements to determine by AAS, such as aluminum and phosphorus. In this review, theory and analytical considerations for MAS are discussed. The principles and limitations of low resolution MAS are described, along with its applications. HR-CS AAS instrumentation is reviewed, emphasizing performance characteristics most relevant for MAS. Applications of flame and HR-CS GFMAS are reviewed, highlighting the most significant work to date. The paper concludes with an evaluation of the enhanced analytical capabilities provided by HR-CS MAS.

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

International Nuclear Information System (INIS)

Sardans, Jordi; Montes, Fernando; Penuelas, Josep

2010-01-01

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 μg L -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 of

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

A self-sufficient and general method for self-absorption correction in gamma-ray spectrometry using GEANT4

International Nuclear Information System (INIS)

Hurtado, S.; Villa, M.; Manjon, G.; Garcia-Tenorio, R.

2007-01-01

This paper presents a self-sufficient and general method for measurement of the activity of low-level gamma-emitters in voluminous samples by gamma-ray spectrometry with a coaxial germanium detector. Due to self-absorption within the sample, the full-energy peak efficiency of low-energy emitters in semiconductor gamma-spectrometers depends strongly on a number of factors including sample composition, density, sample size and gamma-ray energy. As long as those commented factors are well characterized, the influence of self-absorption in the full-energy peak efficiency of low-energy emitters can be calculated using Monte Carlo method based on GEANT4 code for each individual sample. However this task is quite tedious and time consuming. In this paper, we propose an alternative method to determine this influence for voluminous samples of unknown composition. Our method combines both transmission measurements and Monte Carlo simulations, avoiding the application of Monte Carlo full-energy peak efficiency determinations for each individual sample. To test the accuracy and precision of the proposed method, we have calculated 210 Pb activity in sediments samples from an estuary located in the vicinity of several phosphates factories with the proposed method, comparing the obtained results with the ones determined in the same samples using two alternative radiometric techniques

Determination of technetium by graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Kaye, J.H.; Ballou, N.E.

1978-01-01

A detection limit of 6 x 10 -11 g has been achieved for measurement of technetium by graphite furnace atomic absorption spectrometry. A commercially available, demountable, hollow cathode lamp was used and both argon and neon were used as fill gases for the lamp. The range of applicability of the method, when the unresolved 2614.23 to 2615.87 A doublet is used for analysis, is from 60 pg to at least 3 ng of technetium per aliquot analyzed. 3 figures, 1 table

Determination of iron in seawater by electrothermal atomic absorption spectrometry and atomic fluorescence spectrometry: A comparative study

International Nuclear Information System (INIS)

Cabon, J.Y.; Giamarchi, P.; Le Bihan, A.

2010-01-01

Two methods available for direct determination of total Fe in seawater at low concentration level have been examined: electrothermal atomization atomic absorption spectrometry (ETAAS) and electrothermal atomization laser excited atomic fluorescence spectrometry (ETA-LEAFS). In a first part, we have optimized experimental conditions of ETAAS (electrothermal program, matrix chemical modification) for the determination of Fe in seawater by minimizing the chemical interference effects and the magnitude of the simultaneous background absorption signal. By using the best experimental conditions, a detection limit of 80 ng L -1 (20 μL, 3σ) for total Fe concentration was obtained by ETAAS. Using similar experimental conditions (electrothermal program, chemical modification), we have optimized experimental conditions for the determination of Fe by LEAFS. The selected experimental conditions for ETA-LEAFS: excitation wavelength (296.69 nm), noise attenuation and adequate background correction led to a detection limit (3σ) of 3 ng L -1 (i.e. 54 pM) for total Fe concentration with the use a 20 μL seawater sample. For the two methods, concentration values obtained for the analysis of Fe in a NASS-5 (0.2 μg L -1 ) seawater sample were in good agreement with the certified values.

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

Science.gov (United States)

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

2017-04-01

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

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

International Nuclear Information System (INIS)

Bye, R.

1986-01-01

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

Determination of iron in seawater by electrothermal atomic absorption spectrometry and atomic fluorescence spectrometry: a comparative study.

Science.gov (United States)

Cabon, J Y; Giamarchi, P; Le Bihan, A

2010-04-07

Two methods available for direct determination of total Fe in seawater at low concentration level have been examined: electrothermal atomization atomic absorption spectrometry (ETAAS) and electrothermal atomization laser excited atomic fluorescence spectrometry (ETA-LEAFS). In a first part, we have optimized experimental conditions of ETAAS (electrothermal program, matrix chemical modification) for the determination of Fe in seawater by minimizing the chemical interference effects and the magnitude of the simultaneous background absorption signal. By using the best experimental conditions, a detection limit of 80 ng L(-1) (20 microL, 3sigma) for total Fe concentration was obtained by ETAAS. Using similar experimental conditions (electrothermal program, chemical modification), we have optimized experimental conditions for the determination of Fe by LEAFS. The selected experimental conditions for ETA-LEAFS: excitation wavelength (296.69 nm), noise attenuation and adequate background correction led to a detection limit (3sigma) of 3 ng L(-1) (i.e. 54 pM) for total Fe concentration with the use a 20 microL seawater sample. For the two methods, concentration values obtained for the analysis of Fe in a NASS-5 (0.2 microg L(-1)) seawater sample were in good agreement with the certified values. Copyright 2010 Elsevier B.V. All rights reserved.

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…

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...

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.

[Determination of mercury in Boletus impolitus by flow injection-atomic absorption spectrometry].

Science.gov (United States)

Li, Tao; Wang, Yuan-Zhong

2008-04-01

Various test conditions and effect factors for the determination of mercury by flow injection-atomic absorption spectrometry were discussed, and a method for the determination of mercury in Boletus impolitus has been developed. The linear range for mercury is 0-60 microg x L(-1). The relative standard deviation is less than 3.0%, and the recovery is 96%-107%. This method is simple, rapid and has been applied to the determination of mercury in Boletus impolitus samples with satisfactory results.

Enhancement of the atomic absorbance of Cr, Zn, Cd, and Pb in metal furnace atomic absorption spectrometry using absorption tubes

Directory of Open Access Journals (Sweden)

Yuya Koike

2017-03-01

Full Text Available Trace amounts of Cr, Zn, Cd, and Pb were determined by metal furnace atomic absorption spectrometry using absorption tubes. Various absorption tubes were designed as roof- and tube-types, and fixed above the metal furnace in order to extend the light path length. Aqueous standards and samples were injected in the metal furnace and atomized in a metal atomizer with an absorption tube (6 cm length, 15.5 mm diameter. The used of an absorption tube resulted in an enhancement of the atomic absorbance. The ratios of absorbance values with and without the roof- and tube-type absorption tubes were 1.33 and 1.11 for Cr; 1.42 and 1.99 for Zn; 1.66 and 1.98 for Cd; and 1.31 and 1.16 for Pb, respectively. The use of an absorption tube was effective for Zn and Cd analysis, as the absorbance values for these low boiling point metals doubled. The proposed method was successfully applied in the determination of Zn in tap water.

Atomization mechanisms for barium in furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Styris, D.L.

1984-01-01

Atomic absorption spectrometry and mass spectrometry are used simultaneously in order to elucidate atomization mechanisms of barium dichloride in pyrolytic graphite, vitreous carbon, and tantalum furnaces. Gas-phase barium dicarbide is observed to appear concurrently with the free barium. Barium oxide and barium dihydroxide precursors appear with the chlorides. Surface reactions involving species that are absorbed on the various furnaces are postulated to explain the appearances of the species that are observed in the gas phase. 49 references, 4 figures, 1 table

Design considerations regarding an atomizer for multi-element electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Katskov, Dmitri A., E-mail: katskovda@tut.ac.za [Department of Chemistry, Tshwane University of Technology, Private Bag X680, Pretoria 0001 (South Africa); Sadagov, Yuri M. [All-Russian Scientific Research Institute of Optical and Physical Measurements (VNIIOFI), Ozernaya St. 46, Moscow 119361 (Russian Federation)

2011-06-15

The methodology of simultaneous multi-element electrothermal atomic absorption spectrometry (ETAAS-Electrothermal Atomic Absorption Spectrometry) stipulates rigid requirements to the design and operation of the atomizer. It must provide high degree of atomization for the group of analytes, invariant respective to the vaporization kinetics and heating ramp residence time of atoms in the absorption volume and absence of memory effects from major sample components. For the low resolution spectrometer with a continuum radiation source the reduced compared to traditional ETAAS (Electrothermal Atomic Absorption Spectrometry) sensitivity should be, at least partially, compensated by creating high density of atomic vapor in the absorption pulse. The sought-for characteristics were obtained for the 18 mm in length and 2.5 mm in internal diameter longitudinally heated graphite tube atomizer furnished with 2-4.5 mg of ring shaped carbon fiber yarn collector. The collector located next to the sampling port provides large substrate area that helps to keep the sample and its residue in the central part of the tube after drying. The collector also provides a 'platform' effect that delays the vaporization and stipulates vapor release into absorption volume having already stabilized gas temperature. Due to the shape of external surface of the tube, presence of collector and rapid (about 10 {sup o}C/ms) heating, an inverse temperature distribution along the tube is attained at the beginnings of the atomization and cleaning steps. The effect is employed for cleaning of the atomizer using the set of short maximum power heating pulses. Preparation, optimal maintenance of the atomizer and its compliance to the multi-element determination requirements are evaluated and discussed. The experimental setup provides direct simultaneous determination of large group of element within 3-4 order concentration range. Limits of detection are close to those for sequential single element

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

Science.gov (United States)

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

2014-06-11

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

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

Science.gov (United States)

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

2017-09-01

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

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

OpenAIRE

Abdollahi Atousa; Amirkavehei Mooud; Gheisari Mohammad Mehdi; Tadayon Fariba

2014-01-01

A novel dispersive liquid–liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for simultaneous separation/preconcentration of ultra trace amounts of mercury was used. A method based on amalgamation was used for collection of gaseous mercury on gold coated sand (Gold trap). The concentration of mercury was determined by cold vapor atomic absorption spectrometry (CV-AAS). The DLLME-SFO behavior of mercury by using dithizone as complexing agent was systematically ...

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

Science.gov (United States)

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

2017-08-01

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

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

Science.gov (United States)

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

2010-09-01

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

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

International Nuclear Information System (INIS)

Blecker, Carlo R.; Hermann, Gerd M.

2009-01-01

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

Study on aroma components of osmanthus by absorption wire gas chromatography/mass spectrometry

International Nuclear Information System (INIS)

Feng Janyue; Zhao Jing; Huang Qiaoqiao; Feng Lianmei

2001-01-01

The aroma components of fresh osmanthus are captured by absorption wires. The fragrant components absorbed in the wires are desorbed immediately at 358 degree C in Curie-point pyrolyzed, and then led into GC/MS to analyze. As a result, 41 aroma compounds such as β-linalool, linalooloxide, β-ocimene etc. in osmanthus are detected qualitatively by gas chromatography/mass spectrometry. This method can be used to analyze the change of aroma compounds of fresh flowers while blossoming

Atomic absorption spectrometry using tungsten and molybdenum tubes as metal atomizer

International Nuclear Information System (INIS)

Kaneco, Satoshi; Katsumata, Hideyuki; Ohta, Kiyohisa; Suzuki, Tohru

2007-01-01

We have developed a metal tube atomizer for the electrothermal atomization atomic absorption spectrometry (ETA-AAS). Tungsten, molybdenum, platinum tube atomizers were used as the metal atomizer for ETA-AAS. The atomization characteristics of various metals using these metal tube atomizers were investigated. The effects of heating rate of atomizer, atomization temperature, pyrolysis temperature, argon purge gas flow rate and hydrogen addition on the atomic absorption signal were investigated for the evaluation of atomization characteristics. Moreover, ETA-AAS with metal tube atomizer has been combined with the slurry-sampling techniques. Ultrasonic slurry-sampling ETA-AAS with metal tube atomizer were effective for the determination of trace metal elements in biological materials, calcium drug samples, herbal medicine samples, vegetable samples and fish samples. Furthermore, a preconcentration method of trace metals involving adsorption on a metal wire has been applied to ETA-AAS with metal tube atomizer. (author)

Development and Validation of a Sensitive Method for Trace Nickel Determination by Slotted Quartz Tube Flame Atomic Absorption Spectrometry After Dispersive Liquid-Liquid Microextraction.

Science.gov (United States)

Yolcu, Şükran Melda; Fırat, Merve; Chormey, Dotse Selali; Büyükpınar, Çağdaş; Turak, Fatma; Bakırdere, Sezgin

2018-05-01

In this study, dispersive liquid-liquid microextraction was systematically optimized for the preconcentration of nickel after forming a complex with diphenylcarbazone. The measurement output of the flame atomic absorption spectrometer was further enhanced by fitting a custom-cut slotted quartz tube to the flame burner head. The extraction method increased the amount of nickel reaching the flame and the slotted quartz tube increased the residence time of nickel atoms in the flame to record higher absorbance. Two methods combined to give about 90 fold enhancement in sensitivity over the conventional flame atomic absorption spectrometry. The optimized method was applicable over a wide linear concentration range, and it gave a detection limit of 2.1 µg L -1 . Low relative standard deviations at the lowest concentration in the linear calibration plot indicated high precision for both extraction process and instrumental measurements. A coal fly ash standard reference material (SRM 1633c) was used to determine the accuracy of the method, and experimented results were compatible with the certified value. Spiked recovery tests were also used to validate the applicability of the method.

The role of atomic absorption spectrometry in geochemical exploration

Science.gov (United States)

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

1992-01-01

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

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

International Nuclear Information System (INIS)

Bentlin, Fabrina R.S.; Pozebon, Dirce; Mello, Paola A.; Flores, Erico M.M.

2007-01-01

A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO 3 ) 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)

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

International Nuclear Information System (INIS)

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

2014-01-01

Highlights: • Single internal standard is commonly proposed for definite application in AAS. • Internal standard for general use in AAS techniques is original. • Bi showed efficiency as internal standard for Pb determinations by FAAS and GFAAS. • Assorted samples were analyzed and accurate results were found. - Abstract: Bismuth was evaluated as internal standard for Pb determination by line source flame atomic absorption spectrometry (LS FAAS), high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and line source graphite furnace atomic absorption spectrometry (LS GFAAS). Analysis of samples containing different matrices indicated close relationship between Pb and Bi absorbances. Correlation coefficients of calibration curves built up by plotting A Pb /A Bi versus Pb concentration were higher than 0.9953 (FAAS) and higher than 0.9993 (GFAAS). Recoveries of Pb improved from 52–118% (without IS) to 97–109% (IS, LS FAAS); 74–231% (without IS) to 96–109% (IS, HR-CS FAAS); and 36–125% (without IS) to 96–110% (IS, LS GFAAS). The relative standard deviations (n = 12) were reduced from 0.6–9.2% (without IS) to 0.3–4.3% (IS, LS FAAS); 0.7–7.7% (without IS) to 0.1–4.0% (IS, HR-CS FAAS); and 2.1–13% (without IS) to 0.4–5.9% (IS, LS GFAAS)

Working towards accreditation by the International Standards Organization 15189 Standard: how to validate an in-house developed method an example of lead determination in whole blood by electrothermal atomic absorption spectrometry.

Science.gov (United States)

Garcia Hejl, Carine; Ramirez, Jose Manuel; Vest, Philippe; Chianea, Denis; Renard, Christophe

2014-09-01

Laboratories working towards accreditation by the International Standards Organization (ISO) 15189 standard are required to demonstrate the validity of their analytical methods. The different guidelines set by various accreditation organizations make it difficult to provide objective evidence that an in-house method is fit for the intended purpose. Besides, the required performance characteristics tests and acceptance criteria are not always detailed. The laboratory must choose the most suitable validation protocol and set the acceptance criteria. Therefore, we propose a validation protocol to evaluate the performance of an in-house method. As an example, we validated the process for the detection and quantification of lead in whole blood by electrothermal absorption spectrometry. The fundamental parameters tested were, selectivity, calibration model, precision, accuracy (and uncertainty of measurement), contamination, stability of the sample, reference interval, and analytical interference. We have developed a protocol that has been applied successfully to quantify lead in whole blood by electrothermal atomic absorption spectrometry (ETAAS). In particular, our method is selective, linear, accurate, and precise, making it suitable for use in routine diagnostics.

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

Science.gov (United States)

Toya, Yusuke; Itagaki, Toshiko; Wagatsuma, Kazuaki

2017-01-01

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

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

Czech Academy of Sciences Publication Activity Database

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

2014-01-01

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

Determination of trace amounts of selenium in minerals and rocks by flemeless atomic-absorption spectrometry

International Nuclear Information System (INIS)

Capdevila, C.; Alduan, F.A.

1980-01-01

The determination of trace amounts of selenium in silicate rocks and feldspart by solvent extraction and graphite furnace atomic-absorption spectrometry has been studied. Sodium diethyl-ditiocarbamate and ammonium pyrrolidinedithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted into carbon tetrachloride as the sodium diethylditiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (author)

SOME SPECIATION STUDIES IN FOODSTUFF BY ATOMIC ABSORPTION SPECTROMETRY

OpenAIRE

Gücer, S

2000-01-01

There has been increasing interest in speciation studies of essentialelements in foods. The main limitation of this studies, their levels in foodsamples and the difficulties for the determination in their own differentforms without any changes in their original forms.Atomic Absorption Spectrometry (AAS) coupled with separation methodswould be outline in this presentation. Analytical scheme was given for tea, olive and garlic samples forManganese, Magnesium and Selenium respectively. Activated...

Investigation of chemical modifiers for phosphorus in a graphite furnace using high-resolution continuum source atomic absorption spectrometry

International Nuclear Information System (INIS)

Lepri, Fabio G.; Dessuy, Morgana B.; Vale, Maria Goreti R.; Borges, Daniel L.G.; Welz, Bernhard; Heitmann, Uwe

2006-01-01

Phosphorus is not one of the elements that are typically determined by atomic absorption spectrometry, but this technique nevertheless offers several advantages that make it attractive, such as the relatively great freedom from interferences. As the main resonance lines for phosphorus are in the vacuum-ultraviolet, inaccessible by conventional atomic absorption spectrometry equipment, L'vov and Khartsyzov proposed to use the non-resonance doublet at 213.5 / 213.6 nm. Later it turned out that with conventional equipment it is necessary to use a chemical modifier in order to get reasonable sensitivity, and lanthanum was the first one suggested for that purpose. In the following years more than 30 modifiers have been proposed for the determination of this element, and there is no consensus about the best one. In this work high-resolution continuum source atomic absorption spectrometry has been used to investigate the determination of phosphorus without a modifier and with the addition of selected modifiers of very different nature, including the originally recommended lanthanum modifier, several palladium-based modifiers and sodium fluoride. As high-resolution continuum source atomic absorption spectrometry is revealing the spectral environment of the analytical line at high resolution, it became obvious that without the addition of a modifier essentially no atomic phosphorus is formed, even at 2700 deg. C . The absorption measured with line source atomic absorption spectrometry in this case is due to the PO molecule, the spectrum of which is overlapping with the atomic line. Palladium, with or without the addition of calcium or ascorbic acid, was found to be the only modifier to produce almost exclusively atomic phosphorus. Lanthanum and particularly sodium fluoride produced a mixture of P and PO, depending on the atomization temperature. This fact can explain at least some of the discrepancies found in the literature and some of the phenomena observed in the

Measurements of sulfur compounds in CO2 by diode laser atomic absorption spectrometry

International Nuclear Information System (INIS)

Franzke, J.; Stancu, D.G.; Niemax, K.

2003-01-01

Two simple methods for the analysis of the total concentration of sulfur in CO 2 by diode laser atomic absorption spectrometry of excited, metastable sulfur atoms in a direct current discharge are presented. In the first method, the CO 2 sample gas is mixed with the plasma gas (Ar or He) while the second is based on reproducible measurements of the sulfur released from the walls in a helium discharge after being deposited as a result of operating the discharge in pure CO 2 sample gas. The detection limits obtained satisfy the requirements for the control of sulfur compounds in CO 2 used in the food and beverage industry

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

Science.gov (United States)

Ozbek, Nil; Akman, Suleyman

2016-07-20

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-10-17

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

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.

Methods of neutron spectrometry

International Nuclear Information System (INIS)

Doerschel, B.

1981-01-01

The different methods of neutron spectrometry are based on the direct measurement of neutron velocity or on the use of suitable energy-dependent interaction processes. In the latter case the measuring effect of a detector is connected with the searched neutron spectrum by an integral equation. The solution needs suitable unfolding procedures. The most important methods of neutron spectrometry are the time-of-flight method, the crystal spectrometry, the neutron spectrometry by use of elastic collisions with hydrogen nuclei, and neutron spectrometry with the aid of nuclear reactions, especially of the neutron-induced activation. The advantages and disadvantages of these methods are contrasted considering the resolution, the measurable energy range, the sensitivity, and the experimental and computational efforts. (author)

Critical evaluation of analytical performance of atomic absorption spectrometry and inductively coupled plasma mass spectrometry for mercury determination

International Nuclear Information System (INIS)

Krata, A.; Bulska, E.

2005-01-01

The analytical performance of cold vapor atomic absorption spectrometry (CV AAS), graphite furnace atomic absorption spectrometry (GF AAS) and inductively coupled plasma mass spectrometry (ICP-MS) for mercury determination have been investigated with the use of two reference materials SRM 2710 Montana I Soil and BCR-144R (sewage sludge from domestic origin). The digestion conditions and their influence on determination of mercury have been studied. Samples were decomposed by microwave digestion in closed vessels with the use of HCl alone or mixture of HCl+HNO 3 +HF. The digestion solutions were analyzed by CV AAS using NaBH 4 as a reducing agent, by GF AAS with Pd or mixture of Pd/Rh as modifiers and by ICP-MS with Rh as internal standard. In the case of CV AAS, results were not dependent on digestion conditions. In the case of GF AAS and ICP-MS, results depended significantly on digestion conditions; in both cases, the use of the mixture of acids as defined above suppressed the signal of mercury. Therefore, in those cases, the microwave digestion with HCl is recommended. Detection limits of 0.003, 0.01 and 0.2 μg g -1 were achieved by ICP-MS, CV AAS and GF AAS, respectively

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.

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.)

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

Science.gov (United States)

Nerdy

2018-01-01

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

Quantification of the fluorine containing drug 5-fluorouracil in cancer cells by GaF molecular absorption via high-resolution continuum source molecular absorption spectrometry

Science.gov (United States)

Krüger, Magnus; Huang, Mao-Dong; Becker-Roß, Helmut; Florek, Stefan; Ott, Ingo; Gust, Ronald

The development of high-resolution continuum source molecular absorption spectrometry made the quantification of fluorine feasible by measuring the molecular absorption as gallium monofluoride (GaF). Using this new technique, we developed on the example of 5-fluorouracil (5-FU) a graphite furnace method to quantify fluorine in organic molecules. The effect of 5-FU on the generation of the diatomic GaF molecule was investigated. The experimental conditions such as gallium nitrate amount, temperature program, interfering anions (represented as corresponding acids) and calibration for the determination of 5-FU in standard solution and in cellular matrix samples were investigated and optimized. The sample matrix showed no effect on the sensitivity of GaF molecular absorption. A simple calibration curve using an inorganic sodium fluoride solution can conveniently be used for the calibration. The described method is sensitive and the achievable limit of detection is 0.23 ng of 5-FU. In order to establish the concept of "fluorine as a probe in medicinal chemistry" an exemplary application was selected, in which the developed method was successfully demonstrated by performing cellular uptake studies of the 5-FU in human colon carcinoma cells.

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

Directory of Open Access Journals (Sweden)

Man Xiao

2017-01-01

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

Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

International Nuclear Information System (INIS)

Godoi Pereira, M. de; Arruda, M.A.Z.

2003-01-01

Methods for metal preconcentration are often described in the literature. However, purposes are often different, depending on whether the methods are applied in environmental, clinical or technological fields. The respective method needs to be efficient, give high sensitivity, and ideally also is selective which is useful when used in combination with atomic spectroscopy. This review presents the actual tendencies in metal preconcentration using techniques such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), hydride generation atomic absorption spectrometry (HGAAS), inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). Procedures based on related to electrochemical, coprecipitation/precipitation, liquid-liquid and solid-liquid extraction and atom trapping mechanisms are presented. (author)

The application of atomic absorption spectrometry to chemical analysis

International Nuclear Information System (INIS)

Walsh, A.

1980-01-01

YhThe history of the development of atomic absorption methods of elemental analysis is outlined. The theoretical basis of atomic absorption methods is discussed and the principle of modern methods of atomic absorption measurements is described. The advantages, scope and limations of these methods are discussed. Related methods based on the measurement of atomic fluorescence are also described

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

Science.gov (United States)

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

2018-02-01

A new and simple flow injection method followed by atomic absorption spectrometry was developed for indirect determination of sulfite. The proposed method is based on the oxidation of sulfite to sulphate ion using solid-phase manganese dioxide (30% W/W suspended on silica gel beads) reactor. MnO 2 will be reduced to Mn(II) by sample injection in to the column under acidic carrier stream of HNO 3 (pH 2) with flow rate of 3.5mLmin -1 at room temperature. Absorption measurement of Mn(II) which is proportional to the concentration of sulfite in the sample was carried out by atomic absorption spectrometry. The calibration curve was linear up to 25mgL -1 with a detection limit (DL) of 0.08mgL -1 for 400µL injection sample volume. The presented method is efficient toward sulfite determination in sugar and water samples with a relative standard deviation (RSD) less than 1.2% and a sampling rate of about 60h -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

Energy Technology Data Exchange (ETDEWEB)

Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

2015-03-01

The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration.

Determination of Mercury in an Assortment of Dietary Supplements Using an Inexpensive Combustion Atomic Absorption Spectrometry Technique

OpenAIRE

Levine, Keith E.; Levine, Michael A.; Weber, Frank X.; Hu, Ye; Perlmutter, Jason; Grohse, Peter M.

2005-01-01

The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a res...

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

International Nuclear Information System (INIS)

Alduan, F. A.; Capdevilla, C.

1980-01-01

The determination of trace amounts of selenium In silicate rocks and feldspar by solvent extraction and graphite furnace atomic-absorption spectrometry has been stu- died. Sodium diethyl-ditio carbamate and ammonium pyrrolidine dithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted Into carbon tetrachloride as the sodium diethyldithiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (Author) 7 refs

Combination of solid phase extraction and flame atomic absorption spectrometry for trace analysis of cadmium

OpenAIRE

Ensafi, Ali A.; Shiraz, Ameneh Zendegi

2008-01-01

A new selective method was developed for the separation and preconcentration of Cd(II) ions based on its complex formation with Xylenol orange loaded on activated carbon as a solid support in a mini-column. The preconcentrated ions were eluted by passing 5.0 mL 0.5 mol L-1 HNO3 solution through the solid support and then the Cd(II) contents was measured by flame atomic absorption spectrometry. Conditions for preparation of the modified activated carbon, pH and flow variables were studied, as ...

Determination of cobalt in human liver by atomic absorption spectrometry with electrothermal atomization

International Nuclear Information System (INIS)

Caldas, E.D.; Gine-Rosias, M.F.; Dorea, J.G.

1991-01-01

A detailed study of the use of electrothermal atomic absorption spectrometry for the determination of cobalt in human liver is described. Comparisons of sample digestion using nitric acid or nitric acid plus perchloric acid, atomization procedures and the application of palladium and magnesium nitrate chemical modifiers were studied using NBS SRM 1577a Bovine Liver. The best results were achieved with sample decomposition in nitric acid, atomization from the tube wall and no chemical modifier. Cobalt was determined in 90 samples of livers from foetuses and deceased newborns using the standard addition method with an average recovery of 99.8%. (author). 30 refs.; 4 figs.; 2 tabs

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

International Nuclear Information System (INIS)

Fernandes, E.A.N.

1981-01-01

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) [pt

Determination of cadmium in human urine by graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Shimizu, Tokuo; Shijo, Yoshio; Sakai, Kaoru

1981-01-01

A trace amount of cadmium in human urine was determined by graphite furnace atomic absorption spectrometry. A urine sample (25 ml) was digested with 5 ml of HNO 3 and 30 ml of H 2 O 2 in a long-neck flask on a hot-plate (200 0 C), then diluted to 50 ml. The standard addition method was carried out before digesting. Ten μl of the resulted solution was injected into a tube treated with tungsten carbide, and the cadmium signal was measured with the ramp mode atomization. Interference induced by organic materials in urine was avoided by HNO 3 -H 2 O 2 digestion. Interference induced by inorganic salts could be reduced by 2-fold dilution and tungsten carbide treatment. The cadmium signal was separated sufficiently from the molecular absorption due to NaCl etc. by the ramp mode atomization. Since the blank level of H 2 O 2 was relatively high, the determination was limited to about 0.1 μg/l. The coefficient of variation was 1.76% at 0.36 μg/l in 24 h human urine (n = 4). The time required was (8 -- 10)h. The precision of this method was higher than those of direct methods, and the reasonable values of urine levels of cadmium were obtained. (author)

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.

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...

A method optimization study for atomic absorption ...

African Journals Online (AJOL)

Sadia Ata

2014-04-24

Apr 24, 2014 ... Manufacturer brand Win 2.1 software was used for data inte- gration and processing. ... reagents and analyst) is suitable for the intended application. The % relative standard deviation for absorbance ... flame atomic absorption spectrometry. Table 2 Linearity data for analysis of zinc in insulin using AAS.

Method Comparison of Neutron Activation Analysis and Atomic Absorption Spectrometry for Determination of Zinc in Food Samples

International Nuclear Information System (INIS)

Endah Damastuti; Syukria Kurniawati; Natalia Adventini

2009-01-01

Zinc as a micro nutrient, has important roles in human metabolism system. It is required by the body in appropriate amount from food intake. Due to the very low concentration of Zinc in food, high selectivity and sensitivity analysis technique is required for the determination, such as Neutron Activation Analysis (NAA) and Atomic Absorption Spectrometry (AAS). In this experiment, both methods were compared in zinc analysis of food samples. The subject of this experiment is to examine of those methods conformity and improving the technique capability in zinc analysis in food sample. Those methods were validated by analyzing zinc in SRM NIST 1548a Typical Diet and were tested its accuracy and precision. The results of Zn concentration were 25.1 ± 2.14 mg/kg by NAA and 24.1 ± 1.40 mg/kg by AAS while the certificate value was 24.6 ± 1.80 mg/kg. Percentage of relative bias, %CV, μ-test score and HORRAT(Horwitz ratio) value given by NAA were 2%, 8.5%, 0.18 and 0.9 respectively, while %relative bias, %CV, μ-test score and HORRAT value given by AAS were 2%, 5.8 %, 0.20 and 0.6 respectively. The result obtained for Zn concentration in various food samples by NAA and AAS were varied from 13.7 – 29.3 mg/kg with mean value 19.8 mg/kg and 11.2 – 26.0 mg/kg with mean value 17.3 mg/kg (author)

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

Science.gov (United States)

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

2015-10-01

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

Quantification of the fluorine containing drug 5-fluorouracil in cancer cells by GaF molecular absorption via high-resolution continuum source molecular absorption spectrometry

International Nuclear Information System (INIS)

Krüger, Magnus; Huang, Mao-Dong; Becker-Roß, Helmut; Florek, Stefan; Ott, Ingo; Gust, Ronald

2012-01-01

The development of high-resolution continuum source molecular absorption spectrometry made the quantification of fluorine feasible by measuring the molecular absorption as gallium monofluoride (GaF). Using this new technique, we developed on the example of 5-fluorouracil (5-FU) a graphite furnace method to quantify fluorine in organic molecules. The effect of 5-FU on the generation of the diatomic GaF molecule was investigated. The experimental conditions such as gallium nitrate amount, temperature program, interfering anions (represented as corresponding acids) and calibration for the determination of 5-FU in standard solution and in cellular matrix samples were investigated and optimized. The sample matrix showed no effect on the sensitivity of GaF molecular absorption. A simple calibration curve using an inorganic sodium fluoride solution can conveniently be used for the calibration. The described method is sensitive and the achievable limit of detection is 0.23 ng of 5-FU. In order to establish the concept of “fluorine as a probe in medicinal chemistry” an exemplary application was selected, in which the developed method was successfully demonstrated by performing cellular uptake studies of the 5-FU in human colon carcinoma cells. - Highlights: ► Development of HR-CS MAS for quantification of fluorine bound to organic molecules ► Measuring as molecular absorption of gallium monofluoride ► Quantification of organic-bound fluorine in biological material ► The concept of “fluorine as a probe in medicinal chemistry” could be established

Determination of hafnium by atomic absorption spectrometry

International Nuclear Information System (INIS)

Yoshida, Isao; Kobayashi, Hiroshi; Ueno, Keihei.

1977-01-01

Optimum conditions for atomic absorption spectrophotometric determination of hafnium were investigated by use of a Jarrel-Ash AA-1 instrument which was equipped with a premixed gas burner slotted 50 mm in length and 0.4 mm in width. Absorption of hafnium, which was atomized in an nitrous oxide-acetylene flame, was measured on a resonance line at 307.29 nm. The absorption due to hafnium was enhanced in the presence of ammonium fluoride and iron(III) ion, as shown in Figs. 2 and 3, depending on their concentration. The highest absorption was attained by the addition of (0.15 -- 0.3)M ammonium fluoride, 0.07 M of iron(III) ion and 0.05 M of hydrochloric acid. An excess of the additives decreased the absorption. The presence of zirconium, which caused a significant interference in the ordinary analytical methods, did not affect the absorption due to hafnium, if the zirconium concentration is less than 0.2 M. A standard procedure was proposed; A sample containing a few mg of hafnium was dissolved in a 25-ml volumetric flask, and ammonium fluoride, ferric nitrate and hydrochloric acid were added so that the final concentrations were 0.3, 0.07 and 0.05 M, respectively. Atomic absorption was measured on the aqueous solution in a nitrous oxide-acetylene flame and the hafnium content was calculated from the absorbance. Sensitivity was as high as 12.5 μg of Hf/ml/l% absorption. The present method is especially recommendable to the direct determination of hafnium in samples containing zirconium. (auth.)

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.

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

Science.gov (United States)

Zhang, Q L; Gao, G

2016-04-20

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

Solid phase extraction method for the determination of lead, nickel, copper and manganese by flame atomic absorption spectrometry using sodium bispiperdine-1,1'-carbotetrathioate (Na-BPCTT) in water samples

International Nuclear Information System (INIS)

Rekha, D.; Suvardhan, K.; Kumar, J. Dilip; Subramanyam, P.; Prasad, P. Reddy; Lingappa, Y.; Chiranjeevi, P.

2007-01-01

A novel column solid phase extraction procedure was developed for the determination of lead, nickel, copper and manganese in various water samples by flame atomic absorption spectrometry (FAAS) after preconcentration on sodium bispiperdine-1,1'-carbotetrathioate (Na-BPCTT) supported by Amberlite XAD-7. The sorbed element was subsequently eluted with 1 M nitric acid and the acid eluates are analysed by Flame atomic absorption spectrometry (FAAS). Various parameters such as pH, amount of adsorbent, eluent type and volume, flow-rate of the sample solution, volume of the sample solution and matrix interference effect on the retention of the metal ions have been studied. The optimum pH for the sorption of above mentioned metal ions was about 6.0 ± 0.2. The loading capacity of adsorbent for Pb, Cu, Ni and Mn were found to 28, 26, 22 and 20 x 10 -6 g/mL, respectively. The recoveries of lead, copper, nickel and manganese under optimum conditions were found to be 96.7-99.2 at the 95% confident level. The limit of detection was 3.0, 3.2, 2.8 and 3.6 x 10 -6 g/mL for lead, copper, nickel and manganese, respectively by applying a preconcentration factor 50. The proposed enrichment method was applied for metal ions in various water samples. The results were obtained are good agreement with reported method

Quantification of the fluorine containing drug 5-fluorouracil in cancer cells by GaF molecular absorption via high-resolution continuum source molecular absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Krueger, Magnus [Freie Universitaet Berlin, Institut fuer Pharmazie, Pharmazeutische Chemie, Koenigin-Luise-Str. 2-4, 14195 Berlin (Germany); Huang, Mao-Dong; Becker-Ross, Helmut; Florek, Stefan [Leibniz Institut fuer Analytische Wissenschaften, ISAS-e.V., Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany); Ott, Ingo [Technische Universitaet Carolo Wilhelmina zu Braunschweig, Institut fuer Medizinische und Pharmazeutische Chemie, Beethovenstr. 55, 38106 Braunschweig (Germany); Gust, Ronald, E-mail: ronald.gust@uibk.ac.at [Universitaet Innsbruck, Institut fuer Pharmazie, Pharmazeutische Chemie, Innrain 80/82, 6020 Innsbruck (Austria)

2012-03-15

The development of high-resolution continuum source molecular absorption spectrometry made the quantification of fluorine feasible by measuring the molecular absorption as gallium monofluoride (GaF). Using this new technique, we developed on the example of 5-fluorouracil (5-FU) a graphite furnace method to quantify fluorine in organic molecules. The effect of 5-FU on the generation of the diatomic GaF molecule was investigated. The experimental conditions such as gallium nitrate amount, temperature program, interfering anions (represented as corresponding acids) and calibration for the determination of 5-FU in standard solution and in cellular matrix samples were investigated and optimized. The sample matrix showed no effect on the sensitivity of GaF molecular absorption. A simple calibration curve using an inorganic sodium fluoride solution can conveniently be used for the calibration. The described method is sensitive and the achievable limit of detection is 0.23 ng of 5-FU. In order to establish the concept of 'fluorine as a probe in medicinal chemistry' an exemplary application was selected, in which the developed method was successfully demonstrated by performing cellular uptake studies of the 5-FU in human colon carcinoma cells. - Highlights: Black-Right-Pointing-Pointer Development of HR-CS MAS for quantification of fluorine bound to organic molecules Black-Right-Pointing-Pointer Measuring as molecular absorption of gallium monofluoride Black-Right-Pointing-Pointer Quantification of organic-bound fluorine in biological material Black-Right-Pointing-Pointer The concept of 'fluorine as a probe in medicinal chemistry' could be established.

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

Science.gov (United States)

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

Determination of gold in copper-bearing sulphide ores and metallurgical flotation products by atomic-absorption spectrometry.

Science.gov (United States)

Strong, B; Murray-Smith, R

1974-12-01

A method is described which is specific for the determination of gold in sulphide copper ores and concentrates. Direct decomposition with aqua regia was found to be incomplete. A carefully controlled roasting stage followed by treatment with hydrochloric acid and then aqua regia was effective for dissolving all the gold. The gold is extracted into 4-methylpentan-2-one (methyli-sobutylketone) then aspirated into a very lean air-acetylene flame and the gold determined by atomic-absorption spectrometry. No interferences were observed from large concentrations of copper, iron or nickel.

Determination of silver in fresh water by atomic absorption spectrometry following flotation preconcentration by iron(III) collectors

Energy Technology Data Exchange (ETDEWEB)

Cundeva, K.; Stafilov, T. [Institute of Chemistry, Faculty of Science, St. Cyril and Methodius University, Skopje (Yugoslavia)

1997-08-01

Colloid precipitate flotation of silver from fresh water is applied for preconcentration and separation. Optimal conditions using hydrated iron(III) oxide and iron(III) tetramethylenedithiocarbamate as collectors were investigated. Various factors affecting the silver recovery, including collector mass, nature of the supporting electrolyte, pH of the working medium, electrokinetic potential of the collector particle surfaces, type of surfactant, induction time etc., were checked. Within the optimal pH range (5.5-6.5) silver was separated quantitatively (94.9- 100.0%) with 30 mg Fe(III) as collector. The content of silver was determined by electrothermal atomic absorption spectrometry and compared to that from inductively coupled plasma-atomic emission spectrometry. The detection limit of silver by the method described is 0.01 {mu}g/L. (orig.) With 2 figs., 3 tabs.

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

Science.gov (United States)

Ieggli, C. V. S.; Bohrer, D.; Noremberg, S.; do Nascimento, P. C.; de Carvalho, L. M.; Vieira, S. L.; Reis, R. N.

2009-06-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-06-15

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

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

Science.gov (United States)

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

2014-09-01

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

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

Czech Academy of Sciences Publication Activity Database

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

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

Optimization of trace elements determination (Arsenic and chromium) in blood and serum of human by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Ahmadi Faghih, M. A.; Aflaki, F.

2003-01-01

Trace elements play an important role in the bio physiology of cells by affecting their growth and contributions to various biological processes such as wound healing. Determination of toxic trace elements in biological fluids is an important subject of interest for toxicological purposes. Increasing the concentration of these elements in the blood levels, cause serious diseases in patients. Recently instrumental analysis procedures such as atomic absorption spectrometry have been used in clinical measurements for determination of many toxic trace elements in the biological samples. In this paper we are reporting the study of various methods of blood and serum samples preparation for determining the toxic trace elements of Arsenic and Chromium. The measurement of this elements performed by using electrothermal atomic absorption spectrometry. The best and reliable results for Chromium analysis was achieved by injection of diluted serum samples, where the samples were diluted with H CI 0.1N. In Arsenic analysis, the best results obtained by extraction with aqueous solution of TCA. For determining all of these elements the RSD% was less than 5%

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

Science.gov (United States)

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

2017-01-01

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

Determination of molybdenum in human urine by electrothermal atomization atomic absorption spectrometry

International Nuclear Information System (INIS)

Pita Calvo, C.; Bermejo Barrera, P.; Bermejo Barrera, A.

1995-01-01

Various matrix modifiers were investigated for the determination of molybdenum in human urine samples by electrothermal atomization atomic absorption spectrometry. Methods with nitric acid, barium difluoride, magnesium nitrate, palladium-magnesium nitrate and palladium-hydroxylamine hydrochloride were studied by introducing the urine samples directly into the graphite furnace with 0.3% Triton X-100. The charring and atomization curves, the amount of modifier and the calibration and addition graphs were studied in all instances. The precision, accuracy and chemical interferences of the methods were also investigated. The matrix interferences have been removed with the modifiers barium difluoride, palladium-magnesium nitrate and palladium-hydroxylamine hydrochloride. The limits of detection and quantification were 0.2 and 0.7 μg l -1 , respectively, for these modifiers. The characteristic masses were 14.1, 18.0 and 14.9 pg of Mo for palladium-magnesium nitrate, palladium-hydroxylamine hydrochloride and barium difluoride, respectively. The method with palladium-magnesium nitrate has been applied to the study of the amount of molybdenum in human urine samples. The molybdenum levels found lie between 4.8-205.6 μg l -1

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

Directory of Open Access Journals (Sweden)

Abdollahi Atousa

2014-07-01

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

Determination of metals in atmospheric particulates using atomic absorption spectrometry

International Nuclear Information System (INIS)

Alduan, F.A.; Capdevila, C.

1979-01-01

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 HN0 3 HCl solution. The sensitivities achieved are in the range of 2,5.10 -5 and 6,3.10 -3 μg/m 3 , for an air volume of 2000 m 3 . (author)

Determination of lead in water by electrothermal atomic absorption spectrometry with a nickel(II)-ammonium tartrate modifier

International Nuclear Information System (INIS)

Sekerka, I.; Lechner, J.F.

1991-01-01

A method is described for the determination of low concentrations of lead in water samples. Atomic absorption spectrometry is used with a tungsten ribbon furnace and Zeeman background correction. Interferences are eliminated by the addition of ammonium tartrate and nickel(II) nitrate to the samples to act as a matrix modifier and adjust the pH. The results show the superior performance of this modifier over other types used conventionally. The detection limit is 1 μg l -1 relative standard deviation of -1 can be obtained. The instrumentation is simple and the method is efficient for the determination of lead in various water samples. 25 refs.; 7 figs.; 6 tabs

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

International Nuclear Information System (INIS)

Wen, X.; Deng, Q.; Guo, J.; Zhao, X.; Zhao, Y.; Ji, S.

2012-01-01

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)

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

Science.gov (United States)

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

2016-12-15

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

Determination of microquantities of cesium in leaching tests by atomic absorption spectrometry with electrothermal atomization

International Nuclear Information System (INIS)

Crubellati, R.O.; Di Santo, N.R.

1988-01-01

An original method for cesium determinations by atomic absorption spectrometry with electrothermal atomization is described. The effect of foreign ions (alkali and earth alkaline metals) present in leaching test of glasses with incorporated radioactive wastes was studied. The effect of different mineral acids was also investigated. A comparison between the flame excitation method and the electrothermal atomization one was made. Under optimum conditions, cesium in quantities down to 700 ng in 1000 ml of sample could be determined. The calibration curve was linear in the range of 0.7 - 15 ng/mL. The fact that the proposed determinations can be performed in a short time and that a small sample volume is required are fundamental advantages of this method, compared with the flame excitation procedure. Besides, it is adaptable to be applied in hot cells and glove boxes. (Author) [es

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

Czech Academy of Sciences Publication Activity Database

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

2015-01-01

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

High-resolution continuum-source atomic absorption spectrometry: what can we expect?

Directory of Open Access Journals (Sweden)

Welz Bernhard

2003-01-01

Full Text Available A new instrumental concept has been developed for atomic absorption spectrometry (AAS, using a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator and a CCD array detector, providing a resolution of ~2 pm per pixel. Among the major advantages of the system are: i an improved signal-to-noise ratio because of the high intensity of the radiation source, resulting in improved photometric precision and detection limits; ii for the same reason, there are no more 'weak' lines, i.e. secondary lines can be used without compromises; iii new elements might be determined, for which no radiation source has been available; iv the entire spectral environment around the analytical line becomes 'visible', giving a lot more information than current AAS instruments; v the CCD array detector allows a truly simultaneous background correction close to the analytical line; vi the software is capable of storing reference spectra, e.g. of a molecular absorption with rotational fine structure, and of subtracting such spectra from the spectra recorded for a sample, using a least squares algorithm; vii although not yet realized, the system makes possible a truly simultaneous multi-element AAS measurement when an appropriate two-dimensional detector is used, as is already common practice in optical emission spectrometry; vii preliminary experiments have indicated that the instrumental concept could result in a more rugged analytical performance in the determination of trace elements in complex matrices.

Determination of calcium in Mashhad city tap water by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Mashhadian, N.V.

2012-01-01

Summary: Calcium in drinking water is one of the sources of calcium that may contribute significantly to the daily calcium intake. In this study, the samples of tap water were randomly taken from five zones of Mashhad city. Calcium concentration was determined by flame atomic absorption spectrometry (FAAS) technique. The precision of the method was evaluated. The CV% of 6 replicate determinations at 5 macro g/ml Ca was 4.2 in one day and 4.5, among 6 consecutive days. The recovery of spiked samples (98.7%) also showed that the proposed method is reliable for the determination of amounts of calcium in water samples. The mean of calcium in tap water in the city of Mashhad was 52.61+-12.91 (SD) macro g/ml. At present, the amount of calcium in Mashhad tap waters is within the national standard. However, due to the climate and environmental changes, determination of calcium in tap water of Mashhad in different seasons is recommended. (author)

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)

Ribeiro, Anderson Schwingel; Vieira, Mariana Antunes; Furtado da Silva, Alessandra; Borges, Daniel L. Gallindo; Welz, Bernhard; Heitmann, Uwe; Curtius, Adilson Jose

2005-01-01

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

Determination of chlorine in coal by X-ray fluorescence spectrometry method

Energy Technology Data Exchange (ETDEWEB)

Marek, S.; Bojarska, K. [Central Mining Institute, Katowice (Poland). Dept. of Environmental Monitoring

1997-12-31

Determination of chlorine contents in coal is essential for both environmental protection and its technological use. The existing method of chlorine determination in coal are titration methods which have considerable errors particularly in the low concentration range. The elaborated method with the use of X-ray fluorescence spectrometry in a comparison to the other methods is much faster and has better precision and accuracy. The principle of the method lies in the measurement of X-ray fluorescence radiation intensity which is emitted by chlorine in a sample and its comparison with standards. The calibration of the elaborated XRF method is based on natural coals having various concentrations of chlorine within the whole range of its occurrence in Polish coals. Concentrations for the calibration purpose were obtained by the determination of chlorine contents in selected coals by atomic absorption spectrometry method. The procedure of sample preparation for direct X-ray measurements, instrumental measuring conditions and the way of calibration curve preparation are described in the paper. All X-ray measurements were done with a Phillips sequential X-ray fluorescence spectrometer. A double anode Cr-Au X-ray tube with maximum power 3000 MW was used as the excitation source. 5 figs., 4 tabs.

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

Science.gov (United States)

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

2017-10-01

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

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

Science.gov (United States)

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

2014-10-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Dragan, Felicia [University of Oradea, Faculty of Medicine and Pharmacy, 29 N Jiga, 410028 Oradea (Romania); HIncu, Lucian [University of Medicine and Pharmacy ' Carol Davila' , Faculty of Pharmacy, 6 Traian Vuia, 020956 Bucuresti (Romania); Bratu, Ioan, E-mail: fdragan@uoradea.r [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania)

2009-08-01

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

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

Liquid-Liquid Extraction and Determination of Trace Elements in Iron Minerals by Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Taseska, Milena; Stafilov, Trajche; Makreski, Petre; Jacimovic, Radojko; Jovanovski, Gligor

2006-01-01

Various trace elements (cadmium, chromium, cobalt, nickel, manganese) in some iron minerals were determined by flame (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). The studied minerals were chalcopyrite (CuFeS 2 ), hematite (Fe 2 O 3 ) and pyrite (FeS 2 ). To avoid the interference of iron, a method for liquid-liquid extraction of iron and determination of investigated elements in the inorganic phase was proposed. Iron was extracted by diisopropyl ether in hydrochloride acid solution and the extraction method was optimized. Some parameters were obtained to be significantly important: Fe mass in the sample should not exceed 0.3 g, the optimal concentration of HCI should be 7.8 mol 1 -1 and ratio of the inorganic and organic phase should be 1: 1. The procedure was verified by the method of standard additions and by its applications to reference standard samples. The investigated minerals originate from various mines in the Republic of Macedonia. (Author)

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

Czech Academy of Sciences Publication Activity Database

Karadjova, I.B.; Lampugnani, L.; Dědina, Jiří; D'Ulivo, A.; Onor, M.; Tsalev, D.L.

2006-01-01

Roč. 61, č. 5 (2006), s. 525-531 ISSN 0584-8547 R&D Projects: GA AV ČR IAA400310507 Institutional research plan: CEZ:AV0Z40310501 Keywords : hydride generation * atomic absorption spectrometry * interferences Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.092, year: 2006

The determination of magnesium in simulated PWR coolant by graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Gatford, C.; Torrance, K.

1988-06-01

The determination of magnesium in simulated PWR coolant has been investigated by graphite furnace atomic absorption spectrometry with atomization from a L'vov platform. The presence of boric acid in the coolant suppresses the magnesium absorption to such an extent that removal of the boron is necessary and three variations of a methyl borate volatilization technique for the in situ removal of boron from the sample platform were investigated. This work has shown that dilution of the sample with an equal volume of acidified methanol and volatilization of the methyl borate was adequate for the determination of magnesium in coolant samples containing up to 2000 mg 1 -1 of boron. In simulated coolant samples containing 25 and 4 μg 1 -1 of magnesium, positive biases of about 2 and 0.5 μg 1 -1 were measured and these errors were considered to be due to contamination. The limit of detection in the presence of 100 and 2000 mg 1 -1 boron were 0.14 and 0.93 μg 1 -1 respectively. These performance characteristics suggest the method is completely acceptable for monitoring the chemical purity of PWR coolant and associated waters containing boric acid. If, however, more precise analyses were to be required for research purposes then any significant improvement in the above figures would require increased purity of reagents, clean-room conditions to reduce contamination and a more versatile atomic absorption spectrophotometer. (author)

Determination of lead and cadmium in urine by electrothermal atomization atomic absorption spectrometry

International Nuclear Information System (INIS)

Vasil'eva, L.A.; Grinshtejn, I.L.; Gucher, Sh.; Izgi, B.

2008-01-01

The applicability of a DETATA sorbent to the preconcentration of lead and cadmium followed by the determination of these elements in urine using atomic absorption spectrometry with electrothermal atomization was demonstrated. After preconcentration by a factor of 10, the limits of detection were 0.01 and 0.2 μg/l for cadmium and lead, respectively. The accuracy of the results was supported by the analysis of Seronorm TM Trace Elements Urine Batch no.101021 [ru

Reduction of interferences in graphite furnace atomic absorption spectrometry by multiple linear regression modelling

Science.gov (United States)

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Tiberiade, Christian; Frache, Roberto

2000-12-01

The multivariate effects of Na, K, Mg and Ca as nitrates on the electrothermal atomisation of manganese, cadmium and iron were studied by multiple linear regression modelling. Since the models proved to efficiently predict the effects of the considered matrix elements in a wide range of concentrations, they were applied to correct the interferences occurring in the determination of trace elements in seawater after pre-concentration of the analytes. In order to obtain a statistically significant number of samples, a large volume of the certified seawater reference materials CASS-3 and NASS-3 was treated with Chelex-100 resin; then, the chelating resin was separated from the solution, divided into several sub-samples, each of them was eluted with nitric acid and analysed by electrothermal atomic absorption spectrometry (for trace element determinations) and inductively coupled plasma optical emission spectrometry (for matrix element determinations). To minimise any other systematic error besides that due to matrix effects, accuracy of the pre-concentration step and contamination levels of the procedure were checked by inductively coupled plasma mass spectrometric measurements. Analytical results obtained by applying the multiple linear regression models were compared with those obtained with other calibration methods, such as external calibration using acid-based standards, external calibration using matrix-matched standards and the analyte addition technique. Empirical models proved to efficiently reduce interferences occurring in the analysis of real samples, allowing an improvement of accuracy better than for other calibration methods.

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-07-01

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

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

International Nuclear Information System (INIS)

Tran Bang Diep; Tran Dai Nghiep

2005-01-01

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

Sequential determination of arsenic, selenium, antimony, and tellurium in foods via rapid hydride evolution and atomic absorption spectrometry

International Nuclear Information System (INIS)

Fiorino, J.A.; Jones, J.W.; Capar, S.G.

1976-01-01

Analysis of acid digests of foods for As, Se, Sb, and Te was semiautomated. Hydrides generated by controlled addition of base stabilized NaBH 4 solution to acid digests are transported directly into a shielded, hydrogen (nitrogen diluted), entrained-air flame for atomic absorption spectrophotometric determination of the individual elements. The detection limits, based on 1 g of digested sample, are approximately 10 to 20 ng/g for all four elements. Measurement precision is 1 to 2 percent relative standard deviation for each element measured at 0.10 μg. A comparison is made of results of analysis of lyophilized fish tissues for As and Se by instrumental neutron activation (INAA), hydride generation with atomic absorption spectrometry, fluorometry, and spectrophotometry. NBS standard reference materials (orchard leaves and bovine liver) analyzed for As, Se, and Sb by this method show excellent agreement with certified values and with independent NAA values

Investigation of phosphorus atomization using high-resolution continuum source electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Dessuy, Morgana B.; Vale, Maria Goreti R.; Lepri, Fabio G.; Welz, Bernhard; Heitmann, Uwe

2007-01-01

The atomization of phosphorus in electrothermal atomic absorption spectrometry has been investigated using a high-resolution continuum source atomic absorption spectrometer and atomization from a graphite platform as well as from a tantalum boat inserted in a graphite tube. A two-step atomization mechanism is proposed for phosphorus, where the first step is a thermal dissociation, resulting in a fast atomization signal early in the atomization stage, and the second step is a slow release of phosphorus atoms from the graphite tube surface following the adsorption of molecular phosphorus at active sites of the graphite surface. Depending on experimental conditions only one of the mechanisms or both might be active. In the absence of a modifier and with atomization from a graphite or tantalum platform the second mechanism appears to be dominant, whereas in the presence of sodium fluoride as a modifier both mechanisms are observed. Intercalation of phosphorus into the graphite platform in the condensed phase has also been observed; this phosphorus, however, appears to be permanently trapped in the structure of the graphite and does not contribute to the absorption signal

Investigation of artifacts caused by deuterium background correction in the determination of phosphorus by electrothermal atomization using high-resolution continuum source atomic absorption spectrometry

International Nuclear Information System (INIS)

Dessuy, Morgana B.; Vale, Maria Goreti R.; Lepri, Fabio G.; Borges, Daniel L.G.; Welz, Bernhard; Silva, Marcia M.; Heitmann, Uwe

2008-01-01

The artifacts created in the measurement of phosphorus at the 213.6-nm non-resonance line by electrothermal atomic absorption spectrometry using line source atomic absorption spectrometry (LS AAS) and deuterium lamp background correction (D 2 BC) have been investigated using high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). The absorbance signals and the analytical curves obtained by LS AAS without and with D 2 BC, and with HR-CS AAS without and with automatic correction for continuous background absorption, and also with least-squares background correction for molecular absorption with rotational fine structure were compared. The molecular absorption due to the suboxide PO that exhibits pronounced fine structure could not be corrected by the D 2 BC system, causing significant overcorrection. Among the investigated chemical modifiers, NaF, La, Pd and Pd + Ca, the Pd modifier resulted in the best agreement of the results obtained with LS AAS and HR-CS AAS. However, a 15% to 100% higher sensitivity, expressed as slope of the analytical curve, was obtained for LS AAS compared to HR-CS AAS, depending on the modifier. Although no final proof could be found, the most likely explanation is that this artifact is caused by a yet unidentified phosphorus species that causes a spectrally continuous absorption, which is corrected without problems by HR-CS AAS, but which is not recognized and corrected by the D 2 BC system of LS AAS

In-situ gamma spectrometry method for determination of environmental gamma dose

International Nuclear Information System (INIS)

Conti, Claudio de Carvalho

1995-07-01

This work tries to establish a methodology for germanium detectors calibration, normally used for in situ gamma ray spectrometry, for determining the environmental exposure rate in function of the energy of the incident photons. For this purpose a computer code has been developed, based on the stripping method, for the computational spectra analysis to calculate the contribution of the partial absorption of the gamma rays (Compton effect) in the active and nonactive parts of the detector. The resulting total absorption spectrum is then converted to fluence distribution in function of the energy for the photons reaching the detector, which is then used to calculate the exposure rate or kerma in air. The unfolding and fluency convention parameters are determined by detector calibration using point gamma sources. The method is validated by comparison of the results against the calculated exposure rate at a point of interest for the standards. This method is used for the direct measurement of the exposure rate distribution in function of the energy at the site, in situ measurement technic, leading to rapid results during an emergency situation and also used for indoor measurements. (author)

Determination of sulfur in coal and ash slurry by high-resolution continuum source electrothermal molecular absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Nakadi, Flávio V.; Rosa, Lilian R.; Veiga, Márcia A.M.S. da, E-mail: mamsveiga@ffclrp.usp.br

2013-10-01

We propose a procedure for the determination of sulfur in coal slurries by high resolution continuum source electrothermal molecular absorption spectrometry. The slurry, whose concentration is 1 mg mL{sup −1}, was prepared by mixing 50 mg of the sample with 5% v/v nitric acid and 0.04% m/v Triton X-100 and was homogenized manually. It sustained good stability. The determination was performed via CS molecular absorption at 257.592 nm, and the optimized vaporization temperature was 2500 °C. The accuracy of the method was ensured by analysis of certified reference materials SRM 1632b (trace elements in coal) and SRM 1633b (coal fly ash) from the National Institute of Standards and Technology, using external calibration with aqueous standards prepared in the same medium and used as slurry. We achieved good agreement with the certified reference materials within 95% confidence interval, LOD of 0.01% w/w, and RSD of 6%, which confirms the potential of the proposed method. - Highlights: • HR-CS ET MAS as a technique to determine sulfur in coal and ash • Utilization of (coal and coal fly ash) slurry as a sample preparation • Simple and fast method, which uses external calibration with aqueous standards without chemical modifier.

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

Science.gov (United States)

Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata

2014-11-01

In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L- 1 HNO3 solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L- 1 and 36.4 mg L- 1, respectively. The repeatability of the results expressed as relative standard deviation was typically beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93-105% with the repeatability in the range of 4.1-5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg- 1), egg white (2188 ± 29 mg kg- 1), mineral water (31.0 ± 0.9 mg L- 1), white wine (260 ± 4 mg L- 1) and red wine (82 ± 2 mg L- 1), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L- 1).

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.

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

International Nuclear Information System (INIS)

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

2009-01-01

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

Proton Induced X-Rays Emission (PIXE) and Atomic Absorption Spectrometry (AAS) applied in the environmental sample analysis

International Nuclear Information System (INIS)

Popescu, Ion V.; Iordan, M.; Stihi, C.; Bancuta, A.; Dima, G.; Busuioc, G.; Ciupina, V.; Belc, M.; Badica, T.

2003-01-01

The aim of this work is to determine the elemental composition of tree leaves using Proton-Induced X-Rays Emission (PIXE) and Atomic Absorption Spectrophotometry (AAS) methods. By PIXE Spectrometry we identified and determined the concentration of S, Cl, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu Zn, As, Br, Sr and by AAS method the concentration of elements: Cr, Mn, Fe, Co, Cu, Zn, Se, Cd. Pb was identified in only 2 samples from 29. For tree leave samples collected at a large distance to the polluting source the Sr concentration decreased and the Mg, Ca, Se, Zn and Fe concentrations increased. Also, we can observe a small affinity of these leaves for the environmental Pb which was detected for two samples at a small distance to polluting source. (authors)

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.

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)

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

2014-01-01

The determination of N, P, and K in fertilizers by high-resolution continuum source flame atomic and molecular absorption spectrometry is proposed. Under optimized conditions, measurements of the diatomic molecules NO and PO at 215.360 and 247.620 nm, respectively, and K using the wing of the alternative line at 404.722 nm allowed calibration curves to be constructed in the ranges 500–5000 mg L −1 N (r = 0.9994), 100–2000 mg L −1 P (r = 0.9946), and 100–2500 mg L −1 K (r = 0.9995). Commercial fertilizers were analyzed by the proposed method and the concentrations of N, P, and K were found to be in agreement with those obtained by Kjeldahl, spectrophotometric, and flame atomic emission spectrometry methods, respectively, at a 95% confidence level (paired t-test). A phosphate rock certified reference material (CRM) was analyzed and the results for P and K were in agreement with the reference values. Recoveries from spiked CRM were in the ranges 97–105% (NO 3 − -N), 95–103% (NH 4 + -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 2 O 2 allows analysis of fertilizers with different nitrogen species. • Proposal provides advantages over traditional methods in terms of cost and time

Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Olmedo, P.; Pla, A.; Hernandez, A.F.; Lopez-Guarnido, O.; Rodrigo, L. [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain); Gil, F., E-mail: fgil@ugr.es [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain)

2010-02-05

For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Olmedo, P.; Pla, A.; Hernandez, A.F.; Lopez-Guarnido, O.; Rodrigo, L.; Gil, F.

2010-01-01

For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

Graphene oxide sheets immobilized polystyrene for column preconcentration and sensitive determination of lead by flame atomic absorption spectrometry.

Science.gov (United States)

Islam, Aminul; Ahmad, Hilal; Zaidi, Noushi; Kumar, Suneel

2014-08-13

A novel solid-phase extractant was synthesized by coupling graphene oxide (GO) on chloromethylated polystyrene through an ethylenediamine spacer unit to develop a column method for the preconcentration/separation of lead prior to its determination by flame atomic absorption spectrometry. It was characterized by Fourier transform infrared spectroscopy, far-infrared spectroscopy, thermogravimetric analysis/differential thermal analysis, scanning electron microscopy, energy-dispersive spectrometry, and transmission electron microscopy. The abundant oxygen-containing surface functional groups form a strong complex with lead, resulting in higher sorption capacity (227.92 mg g(-1)) than other nanosorbents used for sorption studies of the column method. Using the column procedure here is an alternative to the direct use of GO, which restricts irreversible aggregation of GO and its escape into the ecosystem, making it an environmentally sustainable method. The column method was optimized by varying experimental variables such as pH, flow rate for sorption/desorption, and elution condition and was observed to exhibit a high preconcentration factor (400) with a low preconcentration limit (2.5 ppb) and a high degree of tolerance for matrix ions. The accuracy of the proposed method was verified by determining the Pb content in the standard reference materials and by recovery experiments. The method showed good precision with a relative standard deviation <5%. The proposed method was successfully applied for the determination of lead in tap water, electroplating wastewater, river water, and food samples after preconcentration.

Paleodiet characterisation of an Etrurian population of Pontecagnano (Italy) by Isotope Ratio Mass Spectrometry (IRMS) and Atomic Absorption Spectrometry (AAS)(#).

Science.gov (United States)

Scarabino, Carla; Lubritto, Carmine; Proto, Antonio; Rubino, Mauro; Fiengo, Gilda; Marzaioli, Fabio; Passariello, Isabella; Busiello, Gaetano; Fortunato, Antonietta; Alfano, Davide; Sabbarese, Carlo; Rogalla, Detlef; De Cesare, Nicola; d'Onofrio, Antonio; Terrasi, Filippo

2006-06-01

Human bones recovered from the archaeological site of Pontecagnano (Salerno, Italy) have been studied to reconstruct the diet of an Etrurian population. Two different areas were investigated, named Library and Sant' Antonio, with a total of 44 tombs containing human skeletal remains, ranging in age from the 8th to the 3rd century B.C. This time span was confirmed by 14C dating obtained using Accelerator Mass Spectrometry (AMS) on one bone sample from each site. Atomic Absorption Spectrometry (AAS) was used to extract information about the concentration of Sr, Zn, Ca elements in the bone inorganic fraction, whilst stable isotope ratio measurements (IRMS) were carried out on bone collagen to obtain the delta13C and delta15N. A reliable technique has been used to extract and separate the inorganic and organic fractions of the bone remains. Both IRMS and AAS results suggest a mixed diet including C3 plant food and herbivore animals, consistent with archaeological indications.

Speciation of iron (II) and (III) by using solvent extraction and flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Yaman, Mehmet; Kaya, Gokce

2005-01-01

A method for speciation, preconcentration and separation of Fe 2+ and Fe 3+ in different matrices was developed using solvent extraction and flame atomic absorption spectrometry. PAN as complexing reagent for Fe 2+ and chloroform as organic solvent were used. The complex of Fe 2+ -PAN was extracted into chloroform phase in the pH range of 0.75-4.0 and Fe 3+ remains in water phase in the pH range 0.75-1.25. The optimum conditions for maximum recovery of Fe 2+ and minimum recovery of Fe 3+ were determined as pH = 1, the stirring time of 20 min, the PAN amount of 0.5 mg and chloroform volume of 8 mL. The developed method was applied to the determination of Fe 2+ and Fe 3+ in tea infusion, fruit juice, cola and pekmez. It is seen that there is high bioavailable iron (Fe 2+ ) in pekmez. The developed method is sensitive, simple and need the shorter time in comparison with other similar studies

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

International Nuclear Information System (INIS)

Mandiwana, Khakhathi L.; Panichev, Nikolay

2010-01-01

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 Na 2 CO 3 . 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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-11-01

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

Direct determination of Cu, Mn, Pb, and Zn in beer by thermospray flame furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Nascentes, Clesia C.; Kamogawa, Marcos Y.; Fernandes, Kelly G.; Arruda, Marco A.Z.; Nogueira, Ana Rita A.; Nobrega, Joaquim A.

2005-01-01

In this work, thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was employed for Cu, Mn, Pb, and Zn determination in beer without any sample digestion. The system was optimized and calibration was based on the analyte addition technique. A sample volume of 300 μl was introduced into the hot Ni tube at a flow-rate of 0.4 ml min -1 using 0.14 mol l -1 nitric acid solution or air as carrier. Different Brazilian beers were directly analyzed after ultrasonic degasification. Results were compared with those obtained by graphite furnace atomic absorption spectrometry (GFAAS). The detection limits obtained for Cu, Mn, Pb, and Zn in aqueous solution were 2.2, 18, 1.6, and 0.9 μg l -1 , respectively. The relative standard deviations varied from 2.7% to 7.3% (n=8) for solutions containing the analytes in the 25-50 μg l -1 range. The concentration ranges obtained for analytes in beer samples were: Cu: 38.0-155 μg l -1 ; Mn: 110-348 μg l -1 , Pb: 13.0-32.9 μg l -1 , and Zn: 52.7-226 μg l -1 . Results obtained by TS-FF-AAS and GFAAS were in agreement at a 95% confidence level. The proposed method is fast and simple, since sample digestion is not required and sensitivity can be improved without using expensive devices. The TS-FF-AAS presented suitable sensitivity for determination of Cu, Mn, Pb, and Zn in the quality control of a brewery

Determination of mercury in an assortment of dietary supplements using an inexpensive combustion atomic absorption spectrometry technique.

Science.gov (United States)

Levine, Keith E; Levine, Michael A; Weber, Frank X; Hu, Ye; Perlmutter, Jason; Grohse, Peter M

2005-01-01

The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a result, manufacturers and regulatory agencies concerned with monitoring lot-to-lot product quality may find this approach an attractive alternative to the more classical acid-decomposition, cold vapor atomic absorption methodology. Dietary supplement samples analyzed included astragalus, calcium, chromium picolinate, echinacea, ephedra, fish oil, ginger, ginkgo biloba, ginseng, goldenseal, guggul, senna, St John's wort, and yohimbe products. Quality control samples analyzed with the dietary supplements indicated a high level of method accuracy and precision. Ten replicate preparations of a standard reference material (NIST 1573a, tomato leaves) were analyzed, and the average mercury recovery was 109% (2.0% RSD). The method quantitation limit was 0.3 ng, which corresponded to 1.5 ng/g sample. The highest found mercury concentration (123 ng/g) was measured in a concentrated salmon oil sample. When taken as directed by an adult, this product would result in an approximate mercury ingestion of 7 mug per week.

Gamma spectrometry of infinite 4Π geometry

International Nuclear Information System (INIS)

Nordemann, D.J.R.

1987-07-01

Owing to the weak absorption og gamma radiation by matter, gamma-ray spectrometry may be applied to samples of great volume. A very interesting case is that of the gamma-ray spectrometry applied with 4Π geometry around the detector on a sample assumed to be of infinite extension. The determination of suitable efficiencies allows this method to be quantitative. (author) [pt

Elemental characterization of herbal medicines used in Ghana by instrumental neutron activation analysis and atomic absorption spectrometry and multivariate statistical analysis

International Nuclear Information System (INIS)

Ayivor, J.E.; Nyarko, B.J.B.; Dampare, S.B.; Okine, L.K.

2010-01-01

k 0 instrumental neutron activation analysis and atomic absorption spectrometry were applied to determine multi elements in thirteen Ghanaian herbal medicines used for the management of various diseases. Concentrations of AI, Cu, Mg, Mn and Na were determined. As, Br, K, CI, and Na were determined by short and medium irradiations at a thermal neutron flux of 5x10ncm -2 s -1 . Fe, Cr, Pb, Co, Ni, Sn, Ca, Ba, Li and Sb were determined using atomic absorption spectrometry. Ba, Cu, Li and V were present at trace levels whereas AI, CI, Na, Ca were present at major levels. K, Br, Mg, Mn, Co, Ni, Fe and Sb were also present at minor levels. The precision and accuracy of the method using real samples and standard reference materials were within ±10% of the reported value. Multivariate analytical techniques, such as cluster analysis and principal component analysis (PCA)/factor analysis (FA), have been applied to evaluate the chemical variations in the herbal medicine dataset. All the 13 samples may be grouped into two statistically significant clusters, reflecting the different chemical compositions. The concentrations of elements were within the recommended daily allowances or maximum permissible levels posing no adverse effects on human health.

Noise-Immune Cavity-Enhanced Optical Heterodyne Molecular Spectrometry Modelling Under Saturated Absorption

Science.gov (United States)

Dupré, Patrick

2015-06-01

The Noise-Immune Cavity-Enhanced Optical Heterodyne Molecular Spectrometry (NICE-OHMS) is a modern technique renowned for its ultimate sensitivity, because it combines long equivalent absorption length provided by a high finesse cavity, and a detection theoretically limited by the sole photon-shot-noise. One fallout of the high finesse is the possibility to accumulating strong intracavity electromagnetic fields (EMF). Under this condition, molecular transitions can be easy saturated giving rise to the usual Lamb dips (or hole burning). However, the unusual shape of the basically trichromatic EMF (due to the RF lateral sidebands) induces nonlinear couplings, i.e., new crossover transitions. An analytical methodology will be presented to calculate spectra provided by NICE-OHMS experiments. It is based on the solutions of the equations of motion of an open two-blocked-level system performed in the frequency-domain (optically thin medium). Knowing the transition dipole moment, the NICE-OHMS signals (``absorption-like'' and ``dispersion-like'') can be simulated by integration over the Doppler shifts and by paying attention to the molecular Zeeman sublevels and to the EMF polarization The approach has been validated by discussion experimental data obtained on two transitions of {C2H2} in the near-infrared under moderated saturation. One of the applications of the saturated absorption is to be able to simultaneously determine the transition intensity and the density number while only one these 2 quantities can only be assessed in nonlinear absorption. J. Opt. Soc. Am. B 32, 838 (2015) Optics Express 16, 14689 (2008)

Determination of trace elements in soy milk using ICP atomic emission spectrometry

International Nuclear Information System (INIS)

Tanaka, Satoko; Chayama, Kenji

2009-01-01

The present study investigated the optimal method for the multi-element quantification of 9 elements in soy milk: calcium, copper, iron, potassium, magnesium, manganese, sodium, phosphorus, and zinc. Results obtained using ICP atomic emission spectrometry were compared with those obtained by atomic absorption spectrometry, which is the standard method. The same sample was measured using both ICP atomic emission spectrometry and atomic absorption spectrometry. The percentage of minerals recovered by ICP atomic emission spectrometry ranged from 99.3% to 102%, which was equivalent to that by atomic absorption spectrometry. Therefore, a good result with standard deviation was obtained. The mineral contents of 16 samples of commercially-available soy milk products were measured. The Cu content was significantly proportional to the amount of soybean solids (P < 0.001). Moreover, although relation-ships did not attain statistical significance, the consents of Fe, Zn, K, Mg and P were proportional to the amount of soybean solids, and were highest in soy milk, followed by prepared soy milk and so milk beverage. The Ca content of modified soy milk was significantly higher than that of soy milk and soy milk-based beverages (P < 0.001). Furthermore, the Na content in soy milk was significantly lower. (author)

Investigation of ultraviolet photolysis vapor generation with in-atomizer trapping graphite furnace atomic absorption spectrometry for the determination of mercury

Energy Technology Data Exchange (ETDEWEB)

Madden, Jeremy T. [Department of Chemistry, Biochemistry, and Physics, Marist College, 3399 North Road, Poughkeepsie, NY 12601 (United States); Fitzgerald, Neil [Department of Chemistry, Biochemistry, and Physics, Marist College, 3399 North Road, Poughkeepsie, NY 12601 (United States)], E-mail: neil.fitzgerald@marist.edu

2009-09-15

Generation of mercury vapor by ultraviolet irradiation of mercury solutions in low molecular weight organic acid solutions prior to measurement by Atomic Absorption Spectrometry is a cheap, simple and green method for determination of trace concentrations of mercury. In this work mercury vapor generated by ultraviolet photolysis was trapped onto a palladium coated graphite furnace significantly improving the detection limit of the method. The system was optimized and a detection limit of 0.12 {mu}g L{sup - 1} (compared to 2.1 {mu}g L{sup - 1} for a previously reported system in the absence of trapping) with a precision of 11% for a 10 {mu}g L{sup - 1} mercury standard (RSD, N = 5)

Recent advances in on-line coupling of capillary electrophoresis to atomic absorption and fluorescence spectrometry for speciation analysis and studies of metal-biomolecule interactions

International Nuclear Information System (INIS)

Li Yan; Yin Xuebo; Yan Xiuping

2008-01-01

Speciation information is vital for the understanding of the toxicity, mobility and bioavailability of elements in environmental or biological samples. Hyphenating high resolving power of separation techniques and element-selective detectors provides powerful tools for studying speciation of trace elements in environmental and biological systems. During the last five years several novel hybrid techniques based on capillary electrophoresis (CE) and atomic spectrometry have been developed for speciation analysis and metal-biomolecule interaction study in our laboratory. These techniques include CE on-line coupled with atomic fluorescence spectrometry (AFS), chip-CE on-line coupled with AFS, CE on-line coupled with flame heated quartz furnace atomic absorption spectrometry (FHF-AAS), and CE on-line coupled with electrothermal atomic absorption spectrometry (ETAAS). The necessity for the development of these techniques, their interface design, and applications in speciation analysis and metal-biomolecule interaction study are reviewed. The advantages and limitations of the developed hybrid techniques are critically discussed, and further development is also prospected

Sample Preprocessing For Atomic Spectrometry

International Nuclear Information System (INIS)

Kim, Sun Tae

2004-08-01

This book gives descriptions of atomic spectrometry, which deals with atomic absorption spectrometry such as Maxwell-Boltzmann equation and Beer-Lambert law, atomic absorption spectrometry for solvent extraction, HGAAS, ETASS, and CVAAS and inductively coupled plasma emission spectrometer, such as basic principle, generative principle of plasma and device and equipment, and interferences, and inductively coupled plasma mass spectrometry like device, pros and cons of ICP/MS, sample analysis, reagent, water, acid, flux, materials of experiments, sample and sampling and disassembling of sample and pollution and loss in open system and closed system.

Determination of Inorganic Arsenic in a Wide Range of Food Matrices using Hydride Generation - Atomic Absorption Spectrometry.

Science.gov (United States)

de la Calle, Maria B; Devesa, Vicenta; Fiamegos, Yiannis; Vélez, Dinoraz

2017-09-01

The European Food Safety Authority (EFSA) underlined in its Scientific Opinion on Arsenic in Food that in order to support a sound exposure assessment to inorganic arsenic through diet, information about distribution of arsenic species in various food types must be generated. A method, previously validated in a collaborative trial, has been applied to determine inorganic arsenic in a wide variety of food matrices, covering grains, mushrooms and food of marine origin (31 samples in total). The method is based on detection by flow injection-hydride generation-atomic absorption spectrometry of the iAs selectively extracted into chloroform after digestion of the proteins with concentrated HCl. The method is characterized by a limit of quantification of 10 µg/kg dry weight, which allowed quantification of inorganic arsenic in a large amount of food matrices. Information is provided about performance scores given to results obtained with this method and which were reported by different laboratories in several proficiency tests. The percentage of satisfactory results obtained with the discussed method is higher than that of the results obtained with other analytical approaches.

Speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Li Xun [Department of Chemistry, Beijing Normal University, Beijing 100875 (China); Department of Chemistry and Life Science, Gannan Teachers College, Ganzhou 341000 (China); Jia Jing [Department of Chemistry, Beijing Normal University, Beijing 100875 (China); Wang Zhenghao [Department of Chemistry, Beijing Normal University, Beijing 100875 (China)]. E-mail: zhwang@bnu.edu.cn

2006-02-23

A simple procedure was developed for the speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS), without pre-reduction of As(V). Glassy carbon was selected as cathode material in the flow cell. An optimum catholyte concentration for simultaneous generation of arsine from As(III) and As(V) was 0.06 mol l{sup -1} H{sub 2}SO{sub 4}. Under the optimized conditions, adequate sensitivity and difference in ratio of slopes of the calibration curves for As(III) and As(V) can be achieved at the electrolytic currents of 0.6 and 1 A. The speciation of inorganic arsenic can be performed by controlling the electrolytic currents, and the concentration of As(III) and As(V) in the sample can be calculated according to the equations of absorbance additivity obtained at two selected electrolytic currents. The calibration curves were linear up to 50 ng ml{sup -1} for both As(III) and As(V) at 0.6 and 1 A. The detection limits of the method were 0.2 and 0.5 ng ml{sup -1} for As(III) and As(V) at 0.6 A, respectively. The relative standard deviations were of 2.1% for 20 ng ml{sup -1} As(III) and 2.5% for 20 ng ml{sup -1} As(V). The method was validated by the analysis of human hair certified reference material and successfully applied to speciation of soluble inorganic arsenic in Chinese medicine.

Speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry

International Nuclear Information System (INIS)

Li Xun; Jia Jing; Wang Zhenghao

2006-01-01

A simple procedure was developed for the speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS), without pre-reduction of As(V). Glassy carbon was selected as cathode material in the flow cell. An optimum catholyte concentration for simultaneous generation of arsine from As(III) and As(V) was 0.06 mol l -1 H 2 SO 4 . Under the optimized conditions, adequate sensitivity and difference in ratio of slopes of the calibration curves for As(III) and As(V) can be achieved at the electrolytic currents of 0.6 and 1 A. The speciation of inorganic arsenic can be performed by controlling the electrolytic currents, and the concentration of As(III) and As(V) in the sample can be calculated according to the equations of absorbance additivity obtained at two selected electrolytic currents. The calibration curves were linear up to 50 ng ml -1 for both As(III) and As(V) at 0.6 and 1 A. The detection limits of the method were 0.2 and 0.5 ng ml -1 for As(III) and As(V) at 0.6 A, respectively. The relative standard deviations were of 2.1% for 20 ng ml -1 As(III) and 2.5% for 20 ng ml -1 As(V). The method was validated by the analysis of human hair certified reference material and successfully applied to speciation of soluble inorganic arsenic in Chinese medicine

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,…

Zeeman atomic absorption spectrometry

International Nuclear Information System (INIS)

Hadeishi, T.; McLaughlin, R.

1978-08-01

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

Integration of Solid-phase Extraction with Electrothermal Atomic Absorption Spectrometry for Determination of Trace Elements

OpenAIRE

NUKATSUKA, Isoshi; OHZEKI, Kunio

2006-01-01

An enrichment step in a sample treatment is essential for trace analysis to improve the sensitivity and to eliminate the matrix of the sample. Solid-phase extraction (SPE) is one of the widely used enrichment technique. Electrothermal atomic absorption spectrometry (ETAAS) is a well-established determination technique for trace elements. The integration of SPE with ETAAS leads to further improvement of sensitivity, an automation of the measurement and the economy in the sample size, amounts o...

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......, programmable from the microcomputer, to control the sample volume. No pre-treatment of the samples is necessary. The limit of detection is 0.14 mg l–1, and only small amounts of serum (

Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry.

Science.gov (United States)

Torres, Daiane Placido; Martins-Teixeira, Maristela Braga; Cadore, Solange; Queiroz, Helena Müller

2015-01-01

A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg(-1) (square regression) and 250.0 and 2000.0 μg kg(-1) (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg(-1), respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.

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

Science.gov (United States)

Kowalewska, Zofia; Ruszczyńska, Anna; Bulska, Ewa

2005-03-01

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, oil, oil and 140-300 ng g - 1 in distillation residue.

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

Science.gov (United States)

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

2014-12-01

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

Self-absorption corrections of various sample-detector geometries in gamma-ray spectrometry using sample Monte Carlo Simulations

International Nuclear Information System (INIS)

Ahmad Saat; Appleby, P.G.; Nolan, P.J.

1997-01-01

Corrections for self-absorption in gamma-ray spectrometry have been developed using a simple Monte Carlo simulation technique. The simulation enables the calculation of gamma-ray path lengths in the sample which, using available data, can be used to calculate self-absorption correction factors. The simulation was carried out on three sample geometries: disk, Marinelli beaker, and cylinder (for well-type detectors). Mathematical models and experimental measurements are used to evaluate the simulations. A good agreement of within a few percents was observed. The simulation results are also in good agreement with those reported in the literature. The simulation code was carried out in FORTRAN 90,

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

DEFF Research Database (Denmark)

Larsen, Erik Huusfeldt; Ekelund, J.

1989-01-01

A method for the determination of total selenium in nutritional supplements and selenised yeast is described. The samples were ashed in nitric acid. Hydrochloric acid was used to prevent precipitation of, in particular, iron salts. After appropriate dilutions, the selenium was determined by Zeeman......-effect background corrected graphite furnace atomic absorption spectrometry. A furnace ashing step at 1100 °C was necessary in order to obtain a total recovery of selenium when present in the organic form. Palladium nitrate-magnesium nitrate was used as a matrix modifier. Independent methods were used to determine...... the content of selenium in a selenised yeast check sample. Accuracy was assured using this sample and by recovery experiments. Between-day random error showed a coefficient of variation of 4.2%. Results from the analysis of eight different commercial supplements were in good agreement with declared contents....

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

Energy Technology Data Exchange (ETDEWEB)

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

2003-07-01

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

[A comparative study of cadmium, lead, mercury, arsenic, selenium, manganese, copper and zinc in brown rice and fish by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic absorption spectrometry].

Science.gov (United States)

Oshima, Harumi; Ueno, Eiji; Saito, Isao; Matsumoto, Hiroshi

2004-10-01

A study was conducted to evaluate the applicability of ICP-MS techniques for determination of metals in brown rice and fish. Cadmium, lead, mercury, arsenic, selenium, manganese, copper and zinc were determined by this method. An open digestion with nitric acid (Method A) and a rapid open digestion with nitric acid and hydrochloric acid (Method B) were used to solubilize analytes in samples, and these procedures were followed by ICP-MS analysis. Recovery of certified elements from standard reference materials by Method A and Method B ranged from 92 to 110% except for mercury (70 to 100%). Analytical results of brown rice and fish samples obtained by this ICP-MS agreed with those obtained by atomic absorption spectrometry (AAS). The results of this study demonstrate that quadrupole ICP-MS provides precise and accurate measurements of the elements tested in brown rice and fish samples.

A preconcentration method for indirect determination of acrylamide from chips, crackers and cereal-based baby foods using flame atomic absorption spectrometry.

Science.gov (United States)

Altunay, Nail; Gürkan, Ramazan; Orhan, Ulaş

2016-12-01

Acrylamide is a toxic species for human health, and is a Maillard reaction product which forms spontaneously in heat treatment process of foods. Therefore, a simple, fast and cost-effective method was developed for the indirect determination of acrylamide in processed foods particularly consumed by children. The method is based on ion-pairing of acrylamide with fluorescein (F 2- ) in presence of Ni(II) ions at pH 9.0, and then extraction of the formed ternary complex into micellar phase of poly(ethyleneglycol-mono-p-nonylphenylether) (PONPE 7.5) before analysis by flame atomic absorption spectrometry (FAAS). The ultrasonic-assisted cloud point extraction (UA-CPE) has been used for the preconcentration of acrylamide in the samples prior to its FAAS detection. The matrix matched calibration curve is linear in range of 0.3-150µgkg -1 under optimal reagent conditions (1.75mL of 0.1molL -1 ammonia buffer at pH 9.0, 2.2mgL -1 Ni(II), 4.0×10 -4 molL -1 F 2- , 0.4% (w/v) NH 4 Cl and 0.7% (v/v) PONPE 7.5) with sensitivity enhancement of 160-fold. The proposed method has been validated by assessment of the following parameters; the limits of detection (LOD) and quantification (LOQ) (0.08µgkg -1 and 0.28µgkg -1 , respectively) with a relative standard deviation (RSD%) lower than 6.3%, and extractive recovery higher than 95% for acrylamide spiked at levels of 5 and 25µgkg -1 . The method was successfully applied to the indirect determination of acrylamide in the processed foods and two CRMs with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of phosphorus, sulfur and the halogens using high-temperature molecular absorption spectrometry in flames and furnaces-A review

International Nuclear Information System (INIS)

Welz, Bernhard; Lepri, Fabio G.; Araujo, Rennan G.O.; Ferreira, Sergio L.C.; Huang Maodong; Okruss, Michael; Becker-Ross, Helmut

2009-01-01

The literature about the investigation of molecular spectra of phosphorus, sulfur and the halogens in flames and furnaces, and the use of these spectra for the determination of these non-metals has been reviewed. Most of the investigations were carried out using conventional atomic absorption spectrometers, and there were in essence two different approaches. In the first one, dual-channel spectrometers with a hydrogen or deuterium lamp were used, applying the two-line method for background correction; in the second one, a line source was used that emitted an atomic line, which overlapped with the molecular spectrum. The first approach had the advantage that any spectral interval could be accessed, but it was susceptible to spectral interference; the second one had the advantage that the conventional background correction systems could be used to minimize spectral interferences, but had the problem that an atomic line had to be found, which was overlapping sufficiently well with the maximum of the molecular absorption spectrum. More recently a variety of molecular absorption spectra were investigated using a low-resolution polychromator with a CCD array detector, but no attempt was made to use this approach for quantitative determination of non-metals. The recent introduction and commercial availability of high-resolution continuum source atomic absorption spectrometers is offering completely new possibilities for molecular absorption spectrometry and its use for the determination of non-metals. The use of a high-intensity continuum source together with a high-resolution spectrometer and a CCD array detector makes possible selecting the optimum wavelength for the determination and to exclude most spectral interferences.

Standard test methods for arsenic in uranium hexafluoride

CERN Document Server

American Society for Testing and Materials. Philadelphia

2005-01-01

1.1 These test methods are applicable to the determination of total arsenic in uranium hexafluoride (UF6) by atomic absorption spectrometry. Two test methods are given: Test Method A—Arsine Generation-Atomic Absorption (Sections 5-10), and Test Method B—Graphite Furnace Atomic Absorption (Appendix X1). 1.2 The test methods are equivalent. The limit of detection for each test method is 0.1 μg As/g U when using a sample containing 0.5 to 1.0 g U. Test Method B does not have the complete collection details for precision and bias data thus the method appears as an appendix. 1.3 Test Method A covers the measurement of arsenic in uranyl fluoride (UO2F2) solutions by converting arsenic to arsine and measuring the arsine vapor by flame atomic absorption spectrometry. 1.4 Test Method B utilizes a solvent extraction to remove the uranium from the UO2F2 solution prior to measurement of the arsenic by graphite furnace atomic absorption spectrometry. 1.5 Both insoluble and soluble arsenic are measured when UF6 is...

Atomic absorption spectrometry of the leaves of Newbouldia Laevis (Bignoniaceae)

International Nuclear Information System (INIS)

Mohammed, L.; Musa, A.; Isma'il, M. B.; Ahmed, Y. A.; Okunade, I.O.; Garba, M. A.

2011-01-01

In this study, fresh leaves samples of Newbouldia laevis, a medicinal plant, popularly known as African Border tree used traditionally for the treatment of a number of diseases, were collected in Dakace, (Lat. 11degree05'N Long. 7degree46'E) Zaria, Kaduna State, North-Central Nigeria, during the wet season (October to November) of 2008. The samples were digested using a tri-acid mixture (HNO 3 , HCIO 4 , and H 2 SO 4 ) in the ratio of 25:4:2 respectively. The concentrations of essential trace elements including magnesium, copper, iron, zinc, and cobalt in the samples were determined by Atomic Absorption Spectrometry (AAS). The results obtained showed that Fe has the highest mean concentration of 8.2481±3.689μg/g; whereas Co has the least mean concentration of 0.111±0.055μg/g. The study also revealed that the mean concentrations of Mg, Cu and Zn exceed the recommended limit set by FAO.

Quantitative Determination of Arsenic in Bottled Drinking Water Using Atomic Absorption Spectroscopy

Directory of Open Access Journals (Sweden)

Maria Guţu Claudia

2013-10-01

Full Text Available Background: Many studies have been performed in the past few years, to determine arsenic speciation in drinking water, food chain and environment, arsenic being a well-recognized carcinogenic and toxic agent mainly in its inorganic species. The instrumental techniques used for arsenic determination, such as hydride generation atomic absorption spectrometry (HGAAS, graphite furnace atomic absorption spectrometry (GFAAS and inductively coupled plasma mass spectrometry (ICP-MS, can provide a great sensitivity only on the total amount. Objective: The aim of this study was to develop a simple and rapid method and to analyze the concentration of total inorganic arsenic in bottled drinking water. Methods: Total arsenic was determined in samples from six different types of commercially available bottled drinking water using atomic absorption spectrometry with electrothermal or hydride generation vaporisation. All drinking water samples were acidified with 0.1M nitric acid to match the acidity of the standards. Results: The method was linear within the studied range (1-5 μg/L, R = 0.9943. The quantification limits for arsenic determination were 0.48 μg/L (HGAAS and 0.03 μg/L (GFAAS. The evaluated arsenic content in drinking water was within the accepted limits provided by law. Conclusions: A simple and sensitive method for the quantification of arsenic in drinking water using atomic absorbtion spectroscopy was described, which can be further used in toxicological studies. As an additional advantage, the system is very fast, efficient and environmental friendly

CaI and SrI molecules for iodine determination by high-resolution continuum source graphite furnace molecular absorption spectrometry: Greener molecules for practical application.

Science.gov (United States)

Zanatta, Melina Borges Teixeira; Nakadi, Flávio Venâncio; da Veiga, Márcia Andreia Mesquita Silva

2018-03-01

A new method to determine iodine in drug samples by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) has been developed. The method measures the molecular absorption of a diatomic molecule, CaI or SrI (less toxic molecule-forming reagents), at 638.904 or 677.692nm, respectively, and uses a mixture containing 5μg of Pd and 0.5μg of Mg as chemical modifier. The method employs pyrolysis temperatures of 1000 and 800°C and vaporization temperatures of 2300 and 2400°C for CaI and SrI, respectively. The optimized amounts of Ca and Sr as molecule-forming reagents are 100 and 150µg, respectively. On the basis of interference studies, even small chlorine concentrations reduce CaI and SrI absorbance significantly. The developed method was used to analyze different commercial drug samples, namely thyroid hormone pills with three different iodine amounts (15.88, 31.77, and 47.66µg) and one liquid drug with 1% m v -1 active iodine in their compositions. The results agreed with the values informed by the manufacturers (95% confidence level) regardless of whether CaI or SrI was determined. Therefore, the developed method is useful for iodine determination on the basis of CaI or SrI molecular absorption. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods.

Science.gov (United States)

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto

2003-01-01

A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min(-1), elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L(-1) using ETAAS and 12, 122, 3.4, 17, and 21 ng L(-1) using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-microg L(-1) concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater).

Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods

Energy Technology Data Exchange (ETDEWEB)

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto [Department of Chemistry and Industrial Chemistry, University of Genoa, Via Dodecaneso, 31-16146, Genoa (Italy)

2003-01-01

A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min{sup -1}, elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L{sup -1} using ETAAS and 12, 122, 3.4, 17, and 21 ng L{sup -1} using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-{mu}g L{sup -1} concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater). (orig.)

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

Czech Academy of Sciences Publication Activity Database

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

2017-01-01

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

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

Czech Academy of Sciences Publication Activity Database

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

2017-01-01

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

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)

Kowalewska, Zofia; Ruszczynska, Anna; Bulska, Ewa

2005-01-01

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

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

Science.gov (United States)

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

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

Science.gov (United States)

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

2017-03-01

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

Determination of five trace elements in leaves in Nanfang sweet orange by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Li Fangqing

2006-01-01

The five trace elements of copper, zinc, manganese, iron and cobalt in leaves of Nanfang sweet orange are determined by flame atomic absorption spectrometry. The technique is simple, precise and sensitive. The effect of the type of digesting solution (mixed acid), the ratio of mixed acid, the volume of digesting solution and the time of digesting are investigated in details. The results show that leaves of Nanfang sweet orange contain higher amount of iron and zinc. (authors)

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

Science.gov (United States)

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

1984-01-01

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

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

Science.gov (United States)

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

2014-12-10

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

Determination of phospholipids in soybean lecithin samples via the phosphorus monoxide molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry.

Science.gov (United States)

Pires, Laís N; Brandão, Geovani C; Teixeira, Leonardo S G

2017-06-15

This paper presents a method for determining phospholipids in soybean lecithin samples by phosphorus determination using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) via molecular absorption of phosphorus monoxide. Samples were diluted in methyl isobutyl ketone. The best conditions were found to be 213.561nm with a pyrolysis temperature of 1300°C, a volatilization temperature of 2300°C and Mg as a chemical modifier. To increase the analytical sensitivity, measurement of the absorbance signal was obtained by summing molecular transition lines for PO surrounding 213nm: 213.561, 213.526, 213.617 and 213.637nm. The limit of detection was 2.35mgg -1 and the precision, evaluated as relative standard deviation (RSD), was 2.47% (n=10) for a sample containing 2.2% (w/v) phosphorus. The developed method was applied for the analysis of commercial samples of soybean lecithin. The determined concentrations of phospholipids in the samples varied between 38.1 and 45% (w/v). Copyright © 2017 Elsevier Ltd. All rights reserved.

Development of an in situ solvent formation microextraction and preconcentration method based on ionic liquids for the determination of trace cobalt (II in water samples by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Mohammad Reza Jamali

2017-02-01

Full Text Available A simple in situ solvent formation microextraction (ISFME methodology based on the application of ionic liquid (IL as an extractant solvent and sodium hexafluorophosphate (NaPF6 as an ion-pairing agent was proposed for the preconcentration of the trace levels of cobalt ions. In this method cobalt was complexed with 2-(5-bromo-2-pyridylazo-5-diethylaminophenol (5-Br-PADAP and extracted into an ionic liquid phase. After phase separation, the enriched analyte in the final solution is determined by flame atomic absorption spectrometry (FAAS. Some effective factors that influence the microextraction efficiency were investigated and optimized. Under the optimum experimental conditions, the limit of detection and the enrichment factor were 0.97 μg L−1 and 50, respectively. The relative standard deviation (R.S.D. was obtained as 2.4%. The proposed method was assessed through the analysis of certified reference water and recovery experiments.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of arsenic and selenium in water and sediment by graphite furnace atomic absorption spectrometry

Science.gov (United States)

Jones, Sandra R.; Garbarino, John R.

1999-01-01

Graphite furnace-atomic absorption spectrometry (GF-AAS) is a sensitive, precise, and accurate technique that can be used to determine arsenic and selenium in samples of water and sediment. The GF-AAS method has been developed to replace the hydride generation-atomic absorption spectrometry (HG-AAS) methods because the method detection limits are similar, bias and variability are comparable, and interferences are minimal. Advantages of the GF-AAS method include shorter sample preparation time, increased sample throughput from simultaneous multielement analysis, reduced amount of chemical waste, reduced sample volume requirements, increased linear concentration range, and the use of a more accurate digestion procedure. The linear concentration range for arsenic and selenium is 1 to 50 micrograms per liter in solution; the current method detection limit for arsenic in solution is 0.9 microgram per liter; the method detection limit for selenium in solution is 1 microgram per liter. This report describes results that were obtained using stop-flow and low-flow conditions during atomization. The bias and variability of the simultaneous determination of arsenic and selenium by GF-AAS under both conditions are supported with results from standard reference materials--water and sediment, real water samples, and spike recovery measurements. Arsenic and selenium results for all Standard Reference Water Samples analyzed were within one standard deviation of the most probable values. Long-term spike recoveries at 6.25, 25.0, 37.5 micrograms per liter in reagent-, ground-, and surface-water samples for arsenic averaged 103 plus or minus 2 percent using low-flow conditions and 104 plus or minus 4 percent using stop-flow conditions. Corresponding recoveries for selenium were 98 plus or minus 13 percent using low-flow conditions and 87 plus or minus 24 percent using stop-flow conditions. Spike recoveries at 25 micrograms per liter in 120 water samples ranged from 97 to 99 percent

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

Science.gov (United States)

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

2011-09-01

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

Applications of mass spectrometry in the trace element analysis of biological materials

International Nuclear Information System (INIS)

Moens, L.

1997-01-01

The importance of mass spectrometry for the analysis of biological material is illustrated by reviewing the different mass spectrometric methods applied and describing some typical applications published recently. Though atomic absorption spectrometry is used in the majority of analyses of biological material, most mass spectrometric methods have been used to some extent for trace element determination in biomedical research. The relative importance of the different methods is estimated by reviewing recent research papers. It is striking that especially inductively coupled plasma mass spectrometry is increasingly being applied, partly because the method can be used on-line after chromatographic separation, in speciation studies. Mass spectrometric methods prove to offer unique possibilities in stable isotope tracer studies and for this purpose also experimentally demanding methods such as thermal ionization mass spectrometry and accelerator mass spectrometry are frequently used. (orig.)

Standardization of digestion procedure for the determination of heavy metals in biological materials by atomic absorption spectrometry

International Nuclear Information System (INIS)

Khalid, N.; Chaudhri, S.A.

1999-01-01

Proper decomposition of the sample is one of the basic requirements of the atomic absorption spectroscopic analysis. In the present studies, heavy metals (Cu, Fe, Mn and Zn) were determined in biological samples by designating them in a mixture of nitric acid and perchloric acid. The quantification was made with atomic absorption spectrometry using an air-acetylene flame. The reliability of the procedure used was checked by analysing standard reference materials from NBS and IAEA, such as Rice flour (NBS-SRM-1568), Horse Kidney (IAEA H-8), Mixed Human diet(IAEA H-9), Copepod (IAEA MA-A-1) and fish flesh (IAEA MA-A-2) under identical conditions. A good agreement was observed between determined and the certified values reported by NBS and IAEA. (author)

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

Science.gov (United States)

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

2016-09-14

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

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.

Determination of trace amounts of impurities in molybdenum by spark source and glow discharge mass spectrometry

International Nuclear Information System (INIS)

Saito, Morimasa

1994-01-01

For the determination of trace and ultra-trace amounts of impurities in high-purity molybdenum, spark source mass spectrometry and glow discharge mass spectrometry were studied. In spark source mass spectrometry using the metal probe method, the liquid-helium cryogenic pump was used in order to protect the surface of the samples from oxidation. The theoretical relative sensitivity factors (Mo=1) calculated from physical properties were used. The analytical results obtained for molybdenum tablet and high-purity molybdenum were in good agreement with those obtained by other methods (atomic absorption spectrometry and others). In glow discharge mass spectrometry, the relative sensitivity factors were calculated by using the results obtained by spark source mass spectrometry and atomic absorption spectrometry, and this method was applied to the determination of ultra-trace amounts of impurities in ultra high-purity molybdenum and gave the satisfactory results. The detection limits (2σ, n=10) in the integration time of 600 s for U and Th were 0.6 ppb and 0.3 ppb, and the values for Al, Si, Cr, Mn and Cu were in the range of 10 ppb to 0.5 ppb. (author)

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

International Nuclear Information System (INIS)

Naeemullah, A.; Kazi, T.G.

2011-01-01

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)

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

International Nuclear Information System (INIS)

Sun Mei; Wu Qianghua

2010-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Sun Mei, E-mail: sunmei@ustc.edu.cn [Hefei National Laboratory for Physical Sciences on Microscale, University of Science and Technology of China, No. 96, Jinzhai Road, Hefei 230026 (China); Wu Qianghua [Department of Polymer Science and Engineering, University of Science and Technology of China, Hefei 230026 (China)

2010-04-15

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

Determination of vanadium in sea water by graphite furnace atomic absorption spectrometry with a tube coated with pyrolytic graphite

International Nuclear Information System (INIS)

Shimizu, Tokuo; Sakai, Kaoru

1981-01-01

The trace amount of vanadium in sea water was determined by graphite furnace atomic absorption spectrometry with a tube coated with pyrolytic graphite. To correct the background absorption, a deuterium lamp with a higher-brilliant thermal cathode was used. The sensitivity for vanadium increased 10 -- 20 fold by the use of the tube coated with pyrolytic graphite, and the utility lifetime of the tube was greatly extended. Vanadium(V) - 4-(2-pyridylazo)resorcinol (PAR) complexes were extracted into chloroform as an ion-pair with benzyldimethyltetradecylammonium (Zephiramine) cation alternatively. The sample of sea water, which was made to 0.1 N in sulfuric acid and 0.1% in hydrogen peroxide, was loaded onto the column of Dowex 1-X 4 resin (SO 4 2- -form). Vanadium was then eluted from the resin with 1 N sulfuric acid-0.1% hydrogen peroxide or 1 N hydrochloric acid-0.1% hydrogen peroxide evaporated to dry. After dissolution of the elute in 0.2 N nitric acid, vanadium was extracted. Secondly, the sample of sea water was adjusted to pH 5.0, and loaded onto the column of Chelex-100 resin. Vanadium was eluted from the resin with 2 N ammonia. The above two methods took much time, but the coprecipitation method was not so and recommended for the determination of vanadium in sea water. Vanadium was coprecipitated with iron(III) hydroxide-hydrous titanium(IV) oxide at pH 6.0. The precipitate was digested with nitric acid-hydrogen peroxide. The solution was diluted to 50 ml with water. The resulting solutions were employed to determine the vanadium concentration by the graphite furnace atomic absorption measurement. The trace amounts of vanadium in various kinds of the coastal sea water were determined by the coprecipitation method. (author)

Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Zeini Jahromi, Elham; Bidari, Araz; Assadi, Yaghoub; Milani Hosseini, Mohammad Reza; Jamali, Mohammad Reza

2007-01-01

Dispersive liquid-liquid microextraction (DLLME) technique was successfully used as a sample preparation method for graphite furnace atomic absorption spectrometry (GF AAS). In this extraction method, 500 μL methanol (disperser solvent) containing 34 μL carbon tetrachloride (extraction solvent) and 0.00010 g ammonium pyrrolidine dithiocarbamate (chelating agent) was rapidly injected by syringe into the water sample containing cadmium ions (interest analyte). Thereby, a cloudy solution formed. The cloudy state resulted from the formation of fine droplets of carbon tetrachloride, which have been dispersed, in bulk aqueous sample. At this stage, cadmium reacts with ammonium pyrrolidine dithiocarbamate, and therefore, hydrophobic complex forms which is extracted into the fine droplets of carbon tetrachloride. After centrifugation (2 min at 5000 rpm), these droplets were sedimented at the bottom of the conical test tube (25 ± 1 μL). Then a 20 μL of sedimented phase containing enriched analyte was determined by GF AAS. Some effective parameters on extraction and complex formation, such as extraction and disperser solvent type and their volume, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor 125 was obtained from only 5.00 mL of water sample. The calibration graph was linear in the rage of 2-20 ng L -1 with detection limit of 0.6 ng L -1 . The relative standard deviation (R.S.D.s) for ten replicate measurements of 20 ng L -1 of cadmium was 3.5%. The relative recoveries of cadmium in tap, sea and rivers water samples at spiking level of 5 and 10 ng L -1 are 108, 95, 87 and 98%, respectively. The characteristics of the proposed method have been compared with cloud point extraction (CPE), on-line liquid-liquid extraction, single drop microextraction (SDME), on-line solid phase extraction (SPE) and co-precipitation based on bibliographic data. Therefore, DLLME combined with

Analysis of nuclear grade uranium oxides by atomic absorption spectrometry with electrothermal atomization

International Nuclear Information System (INIS)

Batistoni, D.A.; Erlijman, L.H.; Pazos, A.L.

1986-01-01

The application of atomic absorption spectrometry for the determination of five trace impurities in nuclear grade uranium oxides is described. The elements were separated from the uranium matrix by extraction chromatography and determined in 5.5 M nitric acid by electrothermal atomization using pyrolytic graphite coated tubes. Two elements, cadmium and chromium, with different volatility characteristics were employed to investigate the operating conditions. Drying and ashing conditions were studied for both elements. Ramp and constant potential (step) heating modes have also been studied and compared. Good reproducibility and a longer life of graphite tubes were obtained with ramp atomization. Detection limits (in micrograms per gram of uranium) were: Cd 0.01; Cr 0.1; Cu 0.4; Mn 0.04 and Ni 0.2. (author) [es

Statistical methods for mass spectrometry-based clinical proteomics

NARCIS (Netherlands)

Kakourou, A.

2018-01-01

The work presented in this thesis focuses on methods for the construction of diagnostic rules based on clinical mass spectrometry proteomic data. Mass spectrometry has become one of the key technologies for jointly measuring the expression of thousands of proteins in biological samples.

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

Science.gov (United States)

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

2014-01-01

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

Examination of the Measurement of Absorption Using the Reverberant Room Method for Highly Absorptive Acoustic Foam

Science.gov (United States)

Hughes, William O.; McNelis, Anne M.; Chris Nottoli; Eric Wolfram

2015-01-01

The absorption coefficient for material specimens are needed to quantify the expected acoustic performance of that material in its actual usage and environment. The ASTM C423-09a standard, "Standard Test Method for Sound Absorption and Sound Absorption Coefficients by the Reverberant Room Method" is often used to measure the absorption coefficient of material test specimens. This method has its basics in the Sabine formula. Although widely used, the interpretation of these measurements are a topic of interest. For example, in certain cases the measured Sabine absorption coefficients are greater than 1.0 for highly absorptive materials. This is often attributed to the diffraction edge effect phenomenon. An investigative test program to measure the absorption properties of highly absorbent melamine foam has been performed at the Riverbank Acoustical Laboratories. This paper will present and discuss the test results relating to the effect of the test materials' surface area, thickness and edge sealing conditions. A follow-on paper is envisioned that will present and discuss the results relating to the spacing between multiple piece specimens, and the mounting condition of the test specimen.

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...... 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 eluate forwarded...

Gamow-Teller strength distribution in the beta-decay of 100Ag from total-absorption gamma spectrometry

International Nuclear Information System (INIS)

Batist, L.; Bykov, A.; Moroz, F.; Wittmann, V.; Alkhazov, G.D.; Keller, H.; Kirchner, R.; Klepper, O.; Roeckl, E.; Huyse, M.; Duppen, P. van; Reusen, G.; Plochocki, A.; Pfuetzner, M.; Rykaczewski, K.; Szerypo, J.; Zylicz, J.; Brown, B.A.

1994-10-01

The EC/β + -decay of the odd-odd nucleus 100 Ag was studied by means of total absorption γ-ray spectrometry. Most of the Gamow-Teller strength was found to be concentrated at an excitation energy of 5.6 MeV in 100 Pd, the FWHM of this resonance being 1.5 MeV. The measured strength distribution which is interpreted within the BCS approximation as being due to the dominant population of four-quasiparticle excitations, resembles the distribution predicted by an advanced shell-model calculation for the 98 Ag→ 98 Cd decay. (orig.)

Assessment of elemental pollution in soil of Islamabad city using instrumental neutron activation analysis and atomic absorption spectrometry techniques

International Nuclear Information System (INIS)

Daud, M.; Wasim, M.; Khalid, N.; Zaidi, J.H.; Iqbal, J.

2009-01-01

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.)

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

Science.gov (United States)

Sirirat, Natnicha; Tetbuntad, Kornrawee; Siripinyanond, Atitaya

2017-03-01

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

Selection of the optimal combination of water vapor absorption lines for detection of temperature in combustion zones of mixing supersonic gas flows by diode laser absorption spectrometry

International Nuclear Information System (INIS)

Mironenko, V.R.; Kuritsyn, Yu.A.; Bolshov, M.A.; Liger, V.V.

2017-01-01

Determination of a gas medium temperature by diode laser absorption spectrometry (DLAS) is based on the measurement of integral intensities of the absorption lines of a test molecule (generally water vapor molecule). In case of local thermodynamic equilibrium temperature is inferred from the ratio of the integral intensities of two lines with different low energy levels. For the total gas pressure above 1 atm the absorption lines are broadened and one cannot find isolated well resolved water vapor absorption lines within relatively narrow spectral interval of fast diode laser (DL) tuning range (about 3 cm"−"1). For diagnostics of a gas object in the case of high temperature and pressure DLAS technique can be realized with two diode lasers working in different spectral regions with strong absorption lines. In such situation the criteria of the optimal line selection differs significantly from the case of narrow lines. These criteria are discussed in our work. The software for selection the optimal spectral regions using the HITRAN-2012 and HITEMP data bases is developed. The program selects spectral regions of DL tuning, minimizing the error of temperature determination δT/T, basing on the attainable experimental error of line intensity measurement δS. Two combinations of optimal spectral regions were selected – (1.392 & 1.343 μm) and (1.392 & 1.339 μm). Different algorithms of experimental data processing are discussed.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-05-30

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

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

Science.gov (United States)

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

2013-12-01

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

Use of the helium-3 proportional counter for neutron spectrometry; Utilisation du compteur proportionnel a helium 3 pour la spectrometrie des neutrons

Energy Technology Data Exchange (ETDEWEB)

Vialettes, H; Le Thanh, P [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1967-07-01

Up to now, two methods have been mainly used for neutron spectrometry near nuclear installations: - photographic emulsion spectrometry - the so-called, 'multisphere' technique spectrometry. The first method, which is fairly difficult to apply, has a threshold energy of about 500 keV; this is a big disadvantage for an apparatus which has to be used for spectrometry around nuclear installations where the neutron radiation is very much degraded energetically. The second method does not suffer from this disadvantage but the results which it yields are only approximate. In order to extend the energy range of the neutron spectra studied with sufficient accuracy the use of a helium-3 proportional counter has been considered. This report presents the principles of operation of the helium-3 spectrometer, and the calculation methods which make it possible to take into account the two main effects tending to deform the spectra obtained: - energy absorption by the walls of the counter, - energy loss of the incident neutrons due to elastic collisions with helium-3 nuclei. As an example of the application, the shape of the neutron spectrum emitted by a polonium-lithium source is given; the results obtained are in excellent agreement with theoretical predictions. (authors) [French] Jusqu'ici deux methodes ont ete utilisees principalement pour la spectrometrie des neutrons autour des installations nucleaires: - la spectrometrie par emulsions photographiques - la spectrometrie par la technique dite des multispheres. La premiere methode, d'un emploi assez delicat presente un seuil en energie d'environ 500 keV qui est un obstacle serieux a la spectrometrie autour des installations nucleaires ou le rayonnement neutronique est tres degrade en energie. La deuxieme methode ne presente pas cet inconvenient mais les resultats qu'elle permet d'obtenir ne sont qu'approches. Pour etendre la gamme d'energie des spectres de neutrons etudies avec une precision suffisante, l'utilisation du

Determination of trace amounts of selenium in minerals and rocks by flame less atomic-absorption spectrometry; Determinacion de selinio en minerales y rocas por espectrometria de absorcion atomica

Energy Technology Data Exchange (ETDEWEB)

Alduan, F. A.; Capdevilla, C.

1980-07-01

The determination of trace amounts of selenium In silicate rocks and feldspar by solvent extraction and graphite furnace atomic-absorption spectrometry has been stu- died. Sodium diethyl-ditio carbamate and ammonium pyrrolidine dithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted Into carbon tetrachloride as the sodium diethyldithiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (Author) 7 refs.

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

Science.gov (United States)

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

2017-05-01

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

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

Science.gov (United States)

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

2017-12-01

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

Determination of total sulfur in agricultural samples by high-resolution continuum source flame molecular absorption spectrometry.

Science.gov (United States)

Virgilio, Alex; Raposo, Jorge L; Cardoso, Arnaldo A; Nóbrega, Joaquim A; Gomes Neto, José A

2011-03-23

The usefulness of molecular absorption was investigated for the determination of total sulfur (S) in agricultural samples by high-resolution continuum source flame molecular absorption spectrometry. The lines for CS at 257.595, 257.958, and 258.056 nm and for SH at 323.658, 324.064, and 327.990 nm were evaluated. Figures of merit, such as linear dynamic range, sensitivity, linear correlation, characteristic concentration, limit of detection, and precision, were established. For selected CS lines, wavelength-integrated absorbance equivalent to 3 pixels, analytical curves in the 100-2500 mg L(-1) (257.595 nm), 250-2000 mg L(-1) (257.958 nm), and 250-5000 mg L(-1) (258.056 nm) ranges with a linear correlation coefficient better than 0.9980 were obtained. Results were in agreement at a 95% confidence level (paired t test) with those obtained by gravimetry. Recoveries of S in fungicide and fertilizer samples were within the 84-109% range, and the relative standard deviation (n=12) was typically <5%.

High-resolution continuum source electrothermal atomic absorption spectrometry: Linearization of the calibration curves within a broad concentration range

Energy Technology Data Exchange (ETDEWEB)

Katskov, Dmitri, E-mail: katskovda@tut.ac.za [Tshwane University of Technology, Chemistry Department, Pretoria 0001 (South Africa); Hlongwane, Miranda [Tshwane University of Technology, Chemistry Department, Pretoria 0001 (South Africa); Heitmann, Uwe [German Aerospace Center, Rose-Luxemburg Str. 2, 10178 Berlin (Germany); Florek, Stefan [ISAS-Leibniz-Institut fuer Analytische Wissenschaften e.V., Albert-Einstein-Str. 9,12489 Berlin (Germany)

2012-05-15

The calculation algorithm suggested provides linearization of the calibration curves in high-resolution continuum source electrothermal atomic absorption spectrometry. The algorithm is based on the modification of the function wavelength-integrated absorbance vs. concentration of analyte vapor in the absorption volume. According to the suggested approach, the absorption line is represented by a triangle for low and trapezium for high analyte vapor concentration in the absorption volume. The respective semi-empirical formulas include two linearization parameters, which depend on properties of the absorption line and characteristics of the atomizer and spectrometer. The parameters can be approximately evaluated from the theory and determined in practice from the original broad-range calibration curve. The parameters were found and the proposed calculation algorithm verified in the experiments on direct determination of Ag, Cd, Cu, Fe, Mn and Pb in the solutions within a concentration ranges from 0.15 to 625 {mu}g{center_dot}L{sup -1} using tube, platform tube and filter furnace atomizers. The use of various atomizers, lines, elements and atomization temperatures made possible the simulation of various practical analytical conditions. It was found that the algorithm and optimal linearization parameters made it possible to obtain for each line and atomizer linear approximations of the calibration curves within 3-4 orders of magnitude with correlation coefficients close to 0.999. The algorithm makes possible to employ a single line for the direct element determination over a broad concentration range. The sources of errors and the possibility of a priori theoretical evaluation of the linearization parameters are discussed. - Highlights: Black-Right-Pointing-Pointer New calculation algorithm for HR-CS ET AAS measurements was proposed and applied. Black-Right-Pointing-Pointer The suggested formulas include two parameters to be determined experimentally. Black

Multielement preconcentration of trace heavy metals in seawater with an emulsion containing 8-quinolinol for graphite-furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Matsumiya, Hiroaki; Kageyama, Tomohiro; Hiraide, Masataka

2004-01-01

A water-in-oil type emulsion containing 8-quinolinol has been used for the concentration of traces of heavy metals from seawater prior to their determinations by graphite-furnace atomic absorption spectrometry. The emulsion used was prepared by dissolving 40 mg of 8-quinolinol and 60 mg of sorbitan monooleate (Span-80) in 3.0 ml of toluene and vigorously mixing with 0.70 ml of aqueous hydrochloric acid solution (1.5 mol l -1 ) by ultrasonic irradiation. The resulting emulsion was gradually injected into 100 ml of sample solution (pH 8.5) and dispersed by stirring as numerous tiny globules. Four heavy metals (Co, Ni, Cu, and Cd) in the sample solution were quantitatively transported through the organic layer into the acidic aqueous droplets encapsulated in the emulsion. After collecting the dispersed emulsion globules, they were demulsified by heating and the heavy metals in the segregated aqueous phase were determined by atomic absorption spectrometry. Owing to the highly efficient concentration (100-fold), these heavy metals at sub-ng ml -1 levels in seawater were determined with satisfactory accuracy and precision, being confirmed with certified reference samples

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

Science.gov (United States)

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

2016-05-01

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

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

Science.gov (United States)

Sun, Mei; Wu, Qianghua

2010-04-15

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

Atomic absorption spectrometry

International Nuclear Information System (INIS)

Haswell, S.J.

1991-01-01

Atomic absorption spectroscopy is now well established and widely used technique for the determination of trace and major elements in a wide range analyte types. There have been many advances in the atomic spectroscopy over the last decade and for this reason and to meet the demand, it was felt that there was a need for an updated book. Whilst interest in instrumental design has tended to dominate the minds of the spectrocopist, the analyst concerned with obtaining reliable and representative data, in diverse areas of application, has been diligently modifying and developing sample treatment and instrumental introduction techniques. Such methodology is de fundamental part of analysis and form the basis of the fourteen application chapters of this book. The text focuses in the main on AAS; however, the sample handling techniques described are in many cases equally applicable to ICP-OES and ICP-MS analysis. (author). refs.; figs.; tabs

Strontium mono-chloride — A new molecule for the determination of chlorine using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

Energy Technology Data Exchange (ETDEWEB)

Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Lopez, Alfredo H.D.; Gois, Jefferson S. de; Caramori, Giovanni F. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Borges, Daniel L.G.; Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

2014-12-01

A new method has been developed for the determination of chlorine in biological reference materials using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) of the strontium mono-chloride (SrCl) molecule and direct solid sample analysis. The use of the SrCl molecule for high-temperature MAS was not described up to now in the literature. Preliminary time-dependent density functional theory calculations of the SrCl structure were carried out in order to obtain reasonable estimates of the absorption spectrum of the target molecule. The calculations, which were carried out at BHandHLyp/def2-QZVP level of theory, proved a very accurate and inexpensive way to get information about the spectrum of the SrCl molecule, which enabled us to perform the Cl determination with good sensitivity and specificity. The molecular absorption of the SrCl molecule has been measured using the wavelength at 635.862 nm, and zirconium and palladium have been evaluated as the chemical modifiers in order to increase the sensitivity of the gaseous SrCl molecule generated in the graphite furnace. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Accuracy and precision of the method have been evaluated using biological certified reference materials of both animal and plant origins, showing good agreement with the informed and certified values. Limit of detection and characteristic mass were 1.0 and 2.2 ng, respectively. The results found using HR-CS GF MAS were in agreement (95% confidence level) compared to those obtained by electrothermal vaporization-inductively coupled plasma mass spectrometry. - Highlights: • The spectrum of the SrCl molecule was calculated on a theoretical basis and found very close to the predicted wavelength. • It is the first time that the spectrum of the SrCl molecule is described and used analytically for the determination of Cl. • No spectral interferences were observed as the

Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

Science.gov (United States)

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

2009-11-11

A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

Preconcentration of lead using solidification of floating organic drop and its determination by electrothermal atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Mahmoud Chamsaz

2013-07-01

Full Text Available A simple microextraction method based on solidification of a floating organic drop (SFOD was developed for preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry (ETAAS. Ammonium pyrolidinedithiocarbamate (APDC was used as complexing agent, and the formed complex was extracted into a 20 μL of 1-undecanol. The extracted complex was diluted with ethanol and injected into a graphite furnace. An orthogonal array design (OAD with OA16 (45 matrix was employed to study the effects of different parameters such as pH, APDC concentration, stirring rate, sample solution temperature and the exposure time on the extraction efficiency. Under the optimized experimental conditions the limit of detection (based on 3 s and the enhancement factor were 0.058 μg L−1 and 113, respectively. The relative standard deviation (RSD for 8 replicate determinations of 1 μg L−1 of Pb was 8.8%. The developed method was validated by the analysis of certified reference materials and was successfully applied to the determination of lead in water and infant formula base powder samples.

Determination of trace concentrations of chlorine in aqueous solutions by high-resolution continuum source graphite furnace molecular absorption spectrometry

Science.gov (United States)

Machyňák, Ľubomír; Čacho, František; Němeček, Martin; Beinrohr, Ernest

2016-11-01

Trace concentrations of total chlorine were determined by means of molecular absorption of indium mono-chloride (InCl) at 267.217 nm using high-resolution continuum source graphite furnace molecular absorption spectrometry. The effects of chemical modifiers and the amount of In on the sensitivity and accuracy were investigated. The optimum pyrolysis and vaporization temperatures were 600 °C and 1400 °C, respectively. The limit of detection and characteristic mass were found to be 0.10 ng and 0.21 ng, respectively. Potential non-spectral and spectral interferences were tested for various metals and non-metals at concentrations up to 50 mg L- 1 and for phosphoric, sulphuric and nitric acids. No spectral interferences were observed. Significant non-spectral interferences were observed with F, Br, and I at concentrations higher than 1 mg L- 1, 5 mg L- 1 and 25 mg L- 1, respectively, which is probably caused by formation of competitive indium halogen molecules. Higher concentrations of mineral acids depressed the signal owing to the formation of volatile HCl. The calibration curve was linear in the range between 0.3 and 10 ng with a correlation coefficient of R = 0.993. The elaborated method was used for the chlorine determination in various waters and a drug sample.

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

Science.gov (United States)

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S; Korn, Maria G A; Bezerra, Marcos A

2009-03-15

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

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

International Nuclear Information System (INIS)

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria G.A.; Bezerra, Marcos A.

2009-01-01

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

Physical analytical methods for uranium hexafluoride; Methodes physiques d'analyse de l'hexafluorure d'uranium

Energy Technology Data Exchange (ETDEWEB)

Vandenbussche, G [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

1965-12-15

Various physical methods of analysis currently used or still under investigation such as: sound analysis, vapor pressure measurements, fractional distillation, cryogenics, micro-sublimation, ultra-violet, visible and infra-red absorption spectrophotometry, nuclear magnetic resonance and mass spectrometry are reviewed. For each method, principle and applications are given, and results obtained concerning reproducibility, application limits and rapidity are discussed. (author) [French] On passe en revue les differentes methodes physiques d'analyse utilisees ou en cours d'etude actuellement: par mesure de la vitesse du son, de la pression de vapeur, par distillation fractionnee, cryometrie, microsublimation, spectrometrie d'absorption dans l'ultraviolet, le visible et l'infrarouge, par resonance magnetique nucleaire et par spectrometrie de masse. Pour chaque methode, on donne le principe et son application et on examine les resultats obtenus concernant la reproductibilite, le domaine d'application et la duree des mesures. (auteur)

Determination of chlorine in food samples via the AlCl molecule using high-resolution continuum source molecular absorption spectrometry in a graphite furnace

Energy Technology Data Exchange (ETDEWEB)

Fechetia, Miriam; Tognon, Andre Luiz; Veiga, Marcia A.M.S. da, E-mail: mamsveiga@ffclrp.usp.br

2012-05-15

Determination of chlorine using the molecular absorption of aluminum mono-chloride (AlCl) at the 261.418 nm wavelength was accomplished by high-resolution continuum source molecular absorption spectrometry using a transversely heated graphite tube furnace with an integrated platform. For the analysis, 10 {mu}L of the sample followed by 10 {mu}L of a solution containing Al-Ag-Sr modifier, (1 g L{sup -1} each), were directly injected onto the platform. A spectral interference due to the use of Al-Ag-Sr as mixed modifier was easily corrected by the least-squares algorithm present in the spectrometer software. The pyrolysis and vaporization temperatures were 500 Degree-Sign C and 2200 Degree-Sign C, respectively. To evaluate the feasibility of a simple procedure for the determination of chlorine in food samples present in our daily lives, two different digestion methods were applied, namely (A) an acid digestion method using HNO{sub 3} only at room temperature, and (B) a digestion method with Ag, HNO{sub 3} and H{sub 2}O{sub 2}, where chlorine is precipitated as a low-solubility salt (AgCl), which is then dissolved with ammonia solution. The experimental results obtained with method B were in good agreement with the certified values and demonstrated that the proposed method is more accurate than method A. This is because the formation of silver chloride prevented analyte losses by volatilization. The limit of detection (LOD, 3{sigma}/s) for Cl in methods A and B was 18 {mu}g g{sup -1} and 9 {mu}g g{sup -1}, respectively, 1.7 and 3.3 times lower compared to published work using inductively coupled plasma optical emission spectrometry, and absolute LODs were 2.4 and 1.2 ng, respectively. - Highlights: Black-Right-Pointing-Pointer HR-CS MAS as technique for Cl determination via AlCl molecule Black-Right-Pointing-Pointer Spectral interference was corrected by the least-squares algorithm. Black-Right-Pointing-Pointer Chorine precipitation as AgCl prevents Cl losses during

Atomization in graphite-furnace atomic absorption spectrometry. Peak-height method vs. integration method of measuring absorbance: carbon rod atomizer 63

International Nuclear Information System (INIS)

Sturgeon, R.E.; Chakrabarti, C.L.; Maines, I.S.; Bertels, P.C.

1975-01-01

Oscilloscopic traces of transient atomic absorption signals generated during continuous heating of a Carbon Rod Atomizer model 63 show features which are characteristic of the element being atomized. This research was undertaken to determine the significance and usefulness of the two analytically significant parameters, absorbance maximum and integrated absorbance. For measuring integrated absorbance, an electronic integrating control unit consisting of a timing circuit, a lock-in amplifier, and a digital voltmeter, which functions as a direct absorbance x second readout, has been designed, developed, and successfully tested. Oscilloscopic and recorder traces of the absorbance maximum and digital display of the integrated absorbance are simultaneously obtained. For the elements studied, Cd, Zn, Cu, Al, Sn, Mo, and V, the detection limits and the precision obtained are practically identical for both methods of measurements. The sensitivities by the integration method are about the same as, or less than, those obtained by the peak-height method, whereas the calibration curves by the former are generally linear over wider ranges of concentrations. (U.S.)

Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of cyanide using cadmium carbonate as a new solid-phase reactor

International Nuclear Information System (INIS)

Noroozifar, M.; Khorasani-Motlagh, M.; Hosseini, S.-N.

2005-01-01

A new and simple flow injection system procedure has been developed for the indirect determination of cyanide. The method is based on insertion of aqueous cyanide solutions into an on-line cadmium carbonate packed column (25% m/m suspended on silica gel beads) and a sodium hydroxide with pH 10 is used as the carrier stream. The eluent containing the analyte as cadmiumcyanide complexes, produced from reaction between cadmium carbonate and cyanide, measured by flame atomic absorption spectrometry. The absorbance is proportional to the concentration of cyanide in the sample. The linear range of the system is up to 15 mg L -1 with a detection limit 0.2 mg L -1 and sampling rate 72 h -1 . The method is suitable for determination of cyanide in industrial waste waters with a relative standard deviation better than 1.22%

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.

Combined discrete nebulization and microextraction process for molybdenum determination by flame atomic absorption spectrometry (FAAS)

International Nuclear Information System (INIS)

Oviedo, Jenny A.; Jesus, Amanda M.D. de; Fialho, Lucimar L.; Pereira-Filho, Edenir R.

2014-01-01

Simple and sensitive procedures for the extraction/preconcentration of molybdenum based on vortex-assisted solidified floating organic drop microextraction (VA-SFODME) and cloud point combined with flame absorption atomic spectrometry (FAAS) and discrete nebulization were developed. The influence of the discrete nebulization on the sensitivity of the molybdenum preconcentration processes was studied. An injection volume of 200 μ resulted in a lower relative standard deviation with both preconcentration procedures. Enrichment factors of 31 and 67 and limits of detection of 25 and 5 μ L -1 were obtained for cloud point and VA-SFODME, respectively. The developed procedures were applied to the determination of Mo in mineral water and multivitamin samples. (author)

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)

Guilhen, Sabine Neusatz

2009-01-01

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 -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

Cloud point extraction of palladium in water samples and alloy mixtures using new synthesized reagent with flame atomic absorption spectrometry (FAAS)

International Nuclear Information System (INIS)

Priya, B. Krishna; Subrahmanayam, P.; Suvardhan, K.; Kumar, K. Suresh; Rekha, D.; Rao, A. Venkata; Rao, G.C.; Chiranjeevi, P.

2007-01-01

The present paper outlines novel, simple and sensitive method for the determination of palladium by flame atomic absorption spectrometry (FAAS) after separation and preconcentration by cloud point extraction (CPE). The cloud point methodology was successfully applied for palladium determination by using new reagent 4-(2-naphthalenyl)thiozol-2yl azo chromotropic acid (NTACA) and hydrophobic ligand Triton X-114 as chelating agent and nonionic surfactant respectively in the water samples and alloys. 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. The preconcentration factor was found to be (50-fold) for 250 ml of water sample. Under optimum condition the detection limit was found as 0.067 ng ml -1 for palladium in various environmental matrices. The present method was applied for the determination of palladium in various water samples, alloys and the result shows good agreement with reported method and the recoveries are in the range of 96.7-99.4%

Development of a new free radical absorption capacity assay method for antioxidants: aroxyl radical absorption capacity (ARAC).

Science.gov (United States)

Nagaoka, Shin-ichi; Nagai, Kanae; Fujii, Yuko; Ouchi, Aya; Mukai, Kazuo

2013-10-23

A new free radical absorption capacity assay method is proposed with use of an aroxyl radical (2,6-di-tert-butyl-4-(4'-methoxyphenyl)phenoxyl radical) and stopped-flow spectroscopy and is named the aroxyl radical absorption capacity (ARAC) assay method. The free radical absorption capacity (ARAC value) of each tocopherol was determined through measurement of the radical-scavenging rate constant in ethanol. The ARAC value could also be evaluated through measurement of the half-life of the aroxyl radical during the scavenging reaction. For the estimation of the free radical absorption capacity, the aroxyl radical was more suitable than the DPPH radical, galvinoxyl, and p-nitrophenyl nitronyl nitroxide. The ARAC value in tocopherols showed the same tendency as the free radical absorption capacities reported previously, and the tendency was independent of an oxygen radical participating in the scavenging reaction and of a medium surrounding the tocopherol and oxygen radical. The ARAC value can be directly connected to the free radical-scavenging rate constant, and the ARAC method has the advantage of treating a stable and isolable radical (aroxyl radical) in a user-friendly organic solvent (ethanol). The ARAC method was also successfully applied to a palm oil extract. Accordingly, the ARAC method would be useful in free radical absorption capacity assay of antioxidative reagents and foods.

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

Science.gov (United States)

Vassileva, E; Baeten, H; Hoenig, M

2001-01-02

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

Solid phase extraction of lead on octadecyl bonded silica membrane disk modified with Cyanex302 and determination by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Karve, Manjusha; Rajgor, Reeta V.

2007-01-01

A simple, reliable and rapid method for preconcentration and determination of lead using octadecyl bonded silica membrane disk impregnated with Cyanex302 and flame atomic absorption spectrometry is presented. The influence of aqueous phase pH, type of eluent, flow rates of sample solution and eluent, volume of eluent and amount of extractant has been investigated. The break through volume is greater than 4.0 dm 3 with an enrichment factor of more than 400 and a detection limit of 1.0 μg dm -3 . The method developed for determination of lead is good as six replicate determinations using 100 cm 3 solution containing lead in the range 1-4900 μg provides a relative standard deviation (R.S.D.) of 0.4%. The selectivity of the proposed method was confirmed from the interference studies. The developed procedure was successfully applied for the determination of lead in spiked sea water, USGS standard soil sample, sludge and industrial effluents, medicinal formulation, plant, some food products and wine

Cadmium and lead determination in foods by beam injection flame furnace atomic absorption spectrometry after ultrasound-assisted sample preparation

International Nuclear Information System (INIS)

Aleixo, Poliana Carolina; Junior, Dario Santos; Tomazelli, Andrea Cristina; Rufini, Iolanda A.; Berndt, Harald; Krug, Francisco Jose

2004-01-01

A simple method for cadmium and lead determination in foods by beam injection flame furnace atomic absorption spectrometry (BIFF-AAS) was proposed. Food slurries were prepared by transferring an exact amount of cryogenic-ground homogenized material (50-100 mg) to centrifuge tubes, followed by addition of 5 ml (up to 2.8 mol l -1 ) nitric acid solution and sonication in an ultrasonic bath during 5-10 min. Thereafter, slurries were diluted with water to 10 ml, centrifuged during 5 min at 5400 rpm and 400 μl aliquot of the supernatant was analyzed by BIFF-AAS. The detection limits based on peak height measurements were 0.03 μg g -1 Cd and 1.6 μg g -1 Pb for 2% (m/v) slurry (200 mg/10 ml). For method validation, the certified reference materials Pig Kidney (BCR 186) and Rice Flour (NIES 10) were used. Quantitative cadmium and lead recoveries were obtained and no statistical differences were found at 95% level by applying the t-test

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

Directory of Open Access Journals (Sweden)

Yukun Wang

2016-09-01

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

Determination of lead associated with airborne particulate matter by flame atomic absorption and wave-length dispersive x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Talebi, S.M.

1997-01-01

The lead content of airborne particulate matter was determined by flame atomic absorption spectrometry (FAAS) following digestion with a mixture of nitric acid and hydrogen peroxide and also by wave-length dispersive x-ray fluorescence (WDXRF). The extraction procedure was checked by analyzing a standard reference material of airborne particulate matter (NIST, SRM -1648). It was concluded that lead can quantitatively (98%) be extracted from airborne particulate matter by the leaching process. A five-stage sequential extraction was performed to assess the potential mobility of lead associated with airborne particulate matter. Comparison of the airborne particulate lead measured by WDXRF to that measured by FAAS showed good agreement. The WDXRF method requires no time-consuming sample preparation or use of environmentally unfriendly solvents. The technique is suggested for direct determination of lead in airborne particulate matter in air pollution studies. (author)

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

Science.gov (United States)

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

2018-03-01

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

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

Directory of Open Access Journals (Sweden)

Christophe Waterlot

2012-01-01

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

Analysis of aluminium by atomic absorption spectrometry and analysis of thorium and uranium by alpha spectrometry in the black sand of Egypt

International Nuclear Information System (INIS)

Hannachi, Dhouha; Mathlouthi, Nadia

2008-01-01

Throughout the period of our project of end of study carried out in the Center ; main road Sciences and Nuclear Engineering's CNSTN in one is tallied took one Egypt black sand simple with an aim has of knowing the activities of the existing radio elements and especially Uranium and Thorium. In the same mining, we try to take another Egypt black sand simple an aim has knowing the mass of aluminum by using a techniques in Atomique Absorption Spectrophotometer. After the radio chemical and Spectrometry analysis of the black sand sample we found the results following: - Egypt black sand is contains isotopes of Uranium such as 234 U and 238 U; - The Egypt black sand is contains isotopes of Thorium such as 230 Th and 232 Th. - L' Aluminum is a major. (Author)

Application of methane as a gaseous modifier for the determination of silicon using electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Heinrich, Hans-Joachim, E-mail: hans-joachim.heinrich@bam.de; Kipphardt, Heinrich

2012-04-15

For determination of silicon in aqueous solutions by electrothermal atomic absorption spectrometry methane/argon mixtures as a gaseous modifier were applied during the pyrolysis step to improve the analytical performance. The beneficial effects observed on thermal stabilization, signal enhancement and shape of absorbance signals were attributed to the thermal decomposition products of methane, which were hydrogen and carbon black (soot). Using a 5% CH{sub 4} mixture with argon, the optimized pyrolysis and atomization temperatures were 1350 Degree-Sign C and 2450 Degree-Sign C, respectively. A flushing step following the pyrolysis was mandatory to avoid background absorption and accelerated deposition of pyrolytic graphite. Characteristic masses of 50 and 30 pg were obtained for standard transversely heated graphite atomizer (THGA) tubes and end-capped THGA tubes, respectively, which were lower than with other previously applied modifiers. A limit of detection of 0.2 {mu}g L{sup -1} (3 s, n = 10) has been obtained. In addition, this gaseous modifier did not contribute to contamination which often was significant when a liquid modifier solution was co-injected. The proposed method has been applied to the determination of silicon in ultrapure water, nitric and hydrochloric acids. - Highlights: Black-Right-Pointing-Pointer CH{sub 4}/Ar gas mixtures act as new modifier in the determination of Si using ET AAS. Black-Right-Pointing-Pointer CH{sub 4} improved thermal stabilization, atomization efficiency and signal shape of Si. Black-Right-Pointing-Pointer Optimum performance by addition of 5% CH{sub 4} during pyrolysis at 1350 Degree-Sign C. Black-Right-Pointing-Pointer Gaseous modifier does not contribute to blank values. Black-Right-Pointing-Pointer Optimized method suitable for determination of Si in ultrapure reagents.

International comparison of Cd content in a quality control material of Navajuelas (Tagelus dombeii) determined by anodic stripping voltammetry, atomic absorption spectrometry and neutron activation analysis

International Nuclear Information System (INIS)

Queirolo, F.; Forschungszentrum Juelich GmbH; Universidad de Extremadura, Badajoz; Ostapczuk, P.; Valenta, P.; Stegen, S.; Universidad de Extremadura, Badajoz; Marin, C.; Vinagre, F.; Sanchez, A.

1991-01-01

The determination of Cd was performed by neutron activation analysis (NAA), atomic absorption spectrometry (AAS) with flame or in the electrothermal mode and anodic stripping voltammetry in the differential pulse mode (DPASV) and the square wave mode (SWASV). (orig./EF)

Determination of tellurium in lead and lead alloy using flow injection-hydride generation atomic absorption spectrometry

International Nuclear Information System (INIS)

Mesko, Marcia F.; Pozebon, Dirce; Flores, Erico M.M.; Dressler, Valderi L.

2004-01-01

A method based on flow injection-hydride generation atomic absorption spectrometry (FI-HG AAS) for the determination of trace amount of Te in lead and lead alloy is described. A flow injection system (FI) and related analytical parameters as well as Te determination and interference caused by Pb, Bi and Ag on Te were investigated. The Pb interference could be overcome by using a small sample volume, while the Bi interference could be overcome by thiourea. However, it was not possible to minimise the interference caused by Ag on Te. The optimised conditions for Te determination in the analysed samples were: 6 mol l -1 HCl as sample carrier solution, 0.75% (m/v) sodium tetrahydroborate as Te reductant, 40 μl of sample solution, and 200 ml min -1 Ar flow rate as carrier gas. The limit of quantification (LOQ) was 1.0 μg g -1 Te (using 250 mg of sample in 50 ml final solution), the limit of detection (LOD) was 2.5 μg l -1 and the relative standard deviation (RSD) was 6% for five consecutive measurements of sample solution. The standard addition calibration method was used. Relatively high sample throughput (ca. 45 sample runs can be performed in a working hour), reduced sample manipulation since matrix separation is not necessary, and minor waste generation are the main advantages of the proposed method for Te determination by FI-HG AAS

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-03-15

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

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

DEFF Research Database (Denmark)

Nielsen, Steffen; Hansen, Elo Harald

1997-01-01

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

Separation and determination of copper in bottled water samples by combination of dispersive liquid--liquid microextraction and microsample introduction flame atomic absorption spectrometry.

Science.gov (United States)

Citak, Demirhan; Tuzen, Mustafa

2013-01-01

A new and simple method for the determination of trace amounts of Cu(II) was developed by combination of dispersive liquid-liquid microextraction (DLLME) preconcentration and microsample introduction flame atomic absorption spectrometry. In this method, ethanol and chloroform were chosen as disperser and extraction solvents, respectively, and 1-nitroso-2-naphthol was used as the complexing agent. The factors affecting the extraction efficiency and determination of Cu(II), including extraction and disperser solvent nature and volume, concentration of the complexing agent, pH of the solution, extraction time, and matrix ions, were investigated. Under optimal conditions, the LOD for Cu(II) was 0.95 microg/L with a preconcentration factor of 70. The RSD was 1.9%. The accuracy of the developed DLLME method was verified by determination of Cu(II) in a certified reference material (NRCC-SLRS-4 river water). The relative error was -3.31%. The developed preconcentration procedure was successfully applied to the analysis of bottled drinking water samples.

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

Energy Technology Data Exchange (ETDEWEB)

Calle, Inmaculada de la; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos, E-mail: bendicho@uvigo.es

2016-09-14

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

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

International Nuclear Information System (INIS)

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

2016-01-01

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

Practical aspects of the uncertainty and traceability of spectrochemical measurement results by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Duta, S.; Robouch, P.; Barbu, L.; Taylor, P.

2007-01-01

The determination of trace elements concentration in water by electrothermal atomic absorption spectrometry (ETAAS) is a common and well established technique in many chemical testing laboratories. However, the evaluation of measurement uncertainty results is not systematically implemented. The paper presents an easy step-by-step example leading to the evaluation of the combined standard uncertainty of copper determination in water using ETAAS. The major contributors to the overall measurement uncertainty are identified due to amount of copper in water sample that mainly depends on the absorbance measurements, due to certified reference material and due to auto-sampler volume measurements. The practical aspects how the traceability of copper concentration in water can be established and demonstrated are also pointed out

Practical aspects of the uncertainty and traceability of spectrochemical measurement results by electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Duta, S. [Institute for Reference Materials and Measurements, Joint Research Centre, European Commission, Retieseweg 111, B-2440 Geel (Belgium); National Institute of Metrology, 042122 Vitan Barzesti 11, sector 4 Bucharest (Romania)], E-mail: steluta.duta@inm.ro; Robouch, P. [Institute for Reference Materials and Measurements, Joint Research Centre, European Commission, Retieseweg 111, B-2440 Geel (Belgium)], E-mail: Piotr.Robouch@ec.europa.eu; Barbu, L. [Coca-Cola Entreprise, Analytical Department, Bucharest (Romania); Taylor, P. [Institute for Reference Materials and Measurements, Joint Research Centre, European Commission, Retieseweg 111, B-2440 Geel (Belgium)], E-mail: Philip.Taylor@ec.europa.eu

2007-04-15

The determination of trace elements concentration in water by electrothermal atomic absorption spectrometry (ETAAS) is a common and well established technique in many chemical testing laboratories. However, the evaluation of measurement uncertainty results is not systematically implemented. The paper presents an easy step-by-step example leading to the evaluation of the combined standard uncertainty of copper determination in water using ETAAS. The major contributors to the overall measurement uncertainty are identified due to amount of copper in water sample that mainly depends on the absorbance measurements, due to certified reference material and due to auto-sampler volume measurements. The practical aspects how the traceability of copper concentration in water can be established and demonstrated are also pointed out.

Study to determine the content of vanadium, aluminum, nickel, sodium, iron and copper in a catalytic cracking catalyst, by using Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Gomez, J.; Alonso, A.; Tumbarell, O.; Bustanmete, E.

2003-01-01

Atomic Absorption Spectrometry (AAS), has the advantage of its simplicity, speed and low cost. All this, together with its high sensibility and selectivity, makes the AAS one the most widely used analytic techniques. The present work shows, the study to determine the content of vanadium, aluminum, nickel, sodium, iron and copper in a catalytic cracking catalyst of a refinery, by using this technique. The results are compared to those of two laboratories which use the ICP-AES and AAS techniques and shows the processing of the statistics with the use of the t of Student and the F of Snedecor. The results using different methods are also shown as well as the recommended application of this results in the chemical characterization of this type of catalysts

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

DEFF Research Database (Denmark)

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

1997-01-01

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

Water analysis. Determination of elements by atomic absorption

International Nuclear Information System (INIS)

Anon.

Analysis of homogeneous water solutions (plain water, polluted waters, effluents...) by atomic absorption spectrometry with correction for non specific absorption. The quantity ratio is determined by comparison with standard solutions, correction tables are given [fr

Cu,Cr and As determination in preserved woods (Eucalyptus ssp.) by X-ray fluorescence spectrometries

International Nuclear Information System (INIS)

Pereira Junior, Sergio Matias

2014-01-01

Brazil produces around 2.2 millions of cubic meters of treated wood to meet the annual demand of railway, electric, rural and construction sectors. The most used wood species are eucalyptus (Eucalyptus ssp.) and pine (Pinus ssp.).The treated woods used for poles, sleepers, fence posts and plywoods should be according to Brazilian norms requirements. The most usual wood preservative products used in Brazil are CCA (chromated copper arsenate) and CCB (copper chromium and boron salt). The analytical methods, such as flame atomic absorption spectrometry (FAAS), plasma inductively coupled optical emission spectrometry (ICPOES) and X-ray fluorescence spectrometry (XRFS) have been used for the analytical control of those treatment processes. In this work, the eucalyptus trees (Eucalyptus ssp) samples was obtained from Minas Gerais State, Brazil, cut plantation areas. Under pressure, eucalyptus wood samples were submitted to different concentration of CCA solution reaching 3.9, 6.7, 9.1, 12.4 and 14.0 kg of CCA by m-³ sapwood retentions. Samples in cylinders and sawdust forms were obtained from treated wood samples. Copper, chromium and arsenic determination was performed using the energy dispersive X-ray fluorescence spectrometry (EDXRFS), portable X-ray fluorescence spectrometry (PXRFS), flame atomic absorption spectrometry (FAAS) and instrumental neutron activation analysis. In this work, the method of analysis, sensitivity, precision and accuracy performances of the related techniques were outlined. (author)

Phytosterol glycosides reduce cholesterol absorption in humans

Science.gov (United States)

Lin, Xiaobo; Ma, Lina; Racette, Susan B.; Anderson Spearie, Catherine L.; Ostlund, Richard E.

2009-01-01

Dietary phytosterols inhibit intestinal cholesterol absorption and regulate whole body cholesterol excretion and balance. However, they are biochemically heterogeneous and a portion is glycosylated in some foods with unknown effects on biological activity. We tested the hypothesis that phytosterol glycosides reduce cholesterol absorption in humans. Phytosterol glycosides were extracted and purified from soy lecithin in a novel two-step process. Cholesterol absorption was measured in a series of three single-meal tests given at intervals of 2 wk to each of 11 healthy subjects. In a randomized crossover design, participants received ∼300 mg of added phytosterols in the form of phytosterol glycosides or phytosterol esters, or placebo in a test breakfast also containing 30 mg cholesterol-d7. Cholesterol absorption was estimated by mass spectrometry of plasma cholesterol-d7 enrichment 4–5 days after each test. Compared with the placebo test, phytosterol glycosides reduced cholesterol absorption by 37.6 ± 4.8% (P lecithin are bioactive in humans and should be included in methods of phytosterol analysis and tables of food phytosterol content. PMID:19246636

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 pyrrolidinedithioc......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....../preconcentration process of the ensuing sample. An enrichment factor of 21.4, a detection limit of 2.7 ng/l, along with a sampling frequency of 13s/h were obtained at a sample flow rate of 6.0mlmin/sup -1/. The precision (R.S.D.) at the 0.4 mug/l level was 1.8% as compared to 3.2% when quantifying the organic extractant...

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

International Nuclear Information System (INIS)

Vilar Farinas, M.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.; Herrero Latorre, C.

2007-01-01

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 3 ) 2 and (NH 4 )H 2 PO 4 -Mg(NO 3 ) 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

Sensitivity improvement for antimony determination by using in-situ atom trapping in a slotted quartz tube and flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Titretir, Serap, E-mail: serap.titretir@inonu.edu.tr [Department of Chemistry, Faculty of Arts and Sciences, Inoenue University, 44280 Malatya (Turkey); S Latin-Small-Letter-Dotless-I k, Ahmet Inanc [Department of Chemistry, Faculty of Arts and Sciences, Inoenue University, 44280 Malatya (Turkey); Arslan, Yasin [Department of Chemistry, Faculty of Arts and Sciences, Mehmet Akif Ersoy University, Istiklal Yerleskesi, 15030 Burdur (Turkey); Ataman, O. Yavuz [Department of Chemistry, Faculty of Arts and Sciences, Middle East Technical University, 06800 Ankara (Turkey)

2012-11-15

Significant improvement has been achieved for antimony determination using a slotted quartz tube (SQT) as an atom trap (AT) for in situ preconcentration and flame atomic absorption spectrometry (FAAS). The suggested technique consists of trapping analyte species during ordinary nebulization followed by releasing the collected analyte via introducing organic solvent. Procedures and analytical figures of merit have been presented for the techniques called FAAS, SQT-FAAS and finally SQT-AT-FAAS with the relevant comparisons. Analytical parameters, namely composition of the aqueous medium, sample flow rate, flame conditions, distance between burner head and SQT, sampling period and type of organic solvent and its volume have been optimized. Using SQT-AT-FAAS, a sensitivity enhancement of 369 fold has been obtained, 3 s limit of detection was 3.9 {mu}g L{sup -1} when 25.0 mL of sample was collected in 4.0 min. Interference effects of some elements on antimony signal were studied. - Highlights: Black-Right-Pointing-Pointer Atom trapping in a quartz tube was used for Sb with flame AAS. Black-Right-Pointing-Pointer An inexpensive, simple and sensitive analytical method was suggested for Sb. Black-Right-Pointing-Pointer Almost no background absorption was observed. Black-Right-Pointing-Pointer Range is in microgram per liter level.

Sensitivity improvement for antimony determination by using in-situ atom trapping in a slotted quartz tube and flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Titretir, Serap; Şık, Ahmet İnanç; Arslan, Yasin; Ataman, O. Yavuz

2012-01-01

Significant improvement has been achieved for antimony determination using a slotted quartz tube (SQT) as an atom trap (AT) for in situ preconcentration and flame atomic absorption spectrometry (FAAS). The suggested technique consists of trapping analyte species during ordinary nebulization followed by releasing the collected analyte via introducing organic solvent. Procedures and analytical figures of merit have been presented for the techniques called FAAS, SQT-FAAS and finally SQT-AT-FAAS with the relevant comparisons. Analytical parameters, namely composition of the aqueous medium, sample flow rate, flame conditions, distance between burner head and SQT, sampling period and type of organic solvent and its volume have been optimized. Using SQT-AT-FAAS, a sensitivity enhancement of 369 fold has been obtained, 3 s limit of detection was 3.9 μg L −1 when 25.0 mL of sample was collected in 4.0 min. Interference effects of some elements on antimony signal were studied. - Highlights: ► Atom trapping in a quartz tube was used for Sb with flame AAS. ► An inexpensive, simple and sensitive analytical method was suggested for Sb. ► Almost no background absorption was observed. ► Range is in microgram per liter level.

A novel 3D absorption correction method for quantitative EDX-STEM tomography

International Nuclear Information System (INIS)

Burdet, Pierre; Saghi, Z.; Filippin, A.N.; Borrás, A.; Midgley, P.A.

2016-01-01

This paper presents a novel 3D method to correct for absorption in energy dispersive X-ray (EDX) microanalysis of heterogeneous samples of unknown structure and composition. By using STEM-based tomography coupled with EDX, an initial 3D reconstruction is used to extract the location of generated X-rays as well as the X-ray path through the sample to the surface. The absorption correction needed to retrieve the generated X-ray intensity is then calculated voxel-by-voxel estimating the different compositions encountered by the X-ray. The method is applied to a core/shell nanowire containing carbon and oxygen, two elements generating highly absorbed low energy X-rays. Absorption is shown to cause major reconstruction artefacts, in the form of an incomplete recovery of the oxide and an erroneous presence of carbon in the shell. By applying the correction method, these artefacts are greatly reduced. The accuracy of the method is assessed using reference X-ray lines with low absorption. - Highlights: • A novel 3D absorption correction method is proposed for 3D EDX-STEM tomography. • The absorption of X-rays along the path to the surface is calculated voxel-by-voxel. • The method is applied on highly absorbed X-rays emitted from a core/shell nanowire. • Absorption is shown to cause major artefacts in the reconstruction. • Using the absorption correction method, the reconstruction artefacts are greatly reduced.

A novel 3D absorption correction method for quantitative EDX-STEM tomography

Energy Technology Data Exchange (ETDEWEB)

Burdet, Pierre, E-mail: pierre.burdet@a3.epfl.ch [Department of Materials Science and Metallurgy, University of Cambridge, Charles Babbage Road 27, Cambridge CB3 0FS, Cambridgeshire (United Kingdom); Saghi, Z. [Department of Materials Science and Metallurgy, University of Cambridge, Charles Babbage Road 27, Cambridge CB3 0FS, Cambridgeshire (United Kingdom); Filippin, A.N.; Borrás, A. [Nanotechnology on Surfaces Laboratory, Materials Science Institute of Seville (ICMS), CSIC-University of Seville, C/ Americo Vespucio 49, 41092 Seville (Spain); Midgley, P.A. [Department of Materials Science and Metallurgy, University of Cambridge, Charles Babbage Road 27, Cambridge CB3 0FS, Cambridgeshire (United Kingdom)

2016-01-15

This paper presents a novel 3D method to correct for absorption in energy dispersive X-ray (EDX) microanalysis of heterogeneous samples of unknown structure and composition. By using STEM-based tomography coupled with EDX, an initial 3D reconstruction is used to extract the location of generated X-rays as well as the X-ray path through the sample to the surface. The absorption correction needed to retrieve the generated X-ray intensity is then calculated voxel-by-voxel estimating the different compositions encountered by the X-ray. The method is applied to a core/shell nanowire containing carbon and oxygen, two elements generating highly absorbed low energy X-rays. Absorption is shown to cause major reconstruction artefacts, in the form of an incomplete recovery of the oxide and an erroneous presence of carbon in the shell. By applying the correction method, these artefacts are greatly reduced. The accuracy of the method is assessed using reference X-ray lines with low absorption. - Highlights: • A novel 3D absorption correction method is proposed for 3D EDX-STEM tomography. • The absorption of X-rays along the path to the surface is calculated voxel-by-voxel. • The method is applied on highly absorbed X-rays emitted from a core/shell nanowire. • Absorption is shown to cause major artefacts in the reconstruction. • Using the absorption correction method, the reconstruction artefacts are greatly reduced.

[Determination of trace cobalt in human urine by graphite furnace atomic absorption spectrometr].

Science.gov (United States)

Zhong, L X; Ding, B M; Jiang, D; Liu, D Y; Yu, B; Zhu, B L; Ding, L

2016-05-20

To establish a method to determine cobalt in human urine by graphite furnace atomic absorption spectrometry. Urine with 2% nitric acid diluted two-fold, to quantify the curve, graphite furnace atomic absorption spectrometric detection. Co was linear within 2.5~40.0 ng/ml with r>0.999. Spike experiment showed that Co received good recovery rate, which was 90.8%~94.8%. Intra-assay precisions were 3.2%~5.1% for Co, inter-assay precisions were 4.4%~5.2% for Co. The method by using graphite furnace atomic absorption spectrometr to determine urine Co was fast, accurate and with low matrix effect. It could meet the requirement in GBZ/T 210.5-2008.

Application of atomic absorption spectrophotometry to determine Cd, Cu, Pb, Zn,...in vegetable samples in Dalat

Energy Technology Data Exchange (ETDEWEB)

Giang, Nguyen; Tam, Nguyen Thanh; Ngoc Trinh, Le Thi; Mai, Truong Phuong; Minh, Nguyen Van [Nuclear Research Institute, Dalat (Viet Nam)

2004-08-01

Nowadays atomic absorption spectrometry has become valuable method for trace element analysis because high specificity; low detection litmus, easy to use; easy sample preparation, low investment and running costs... atomic absorption spectrometry is generally accepted as one the most suitable method for single - element analysis of trace elements in various kinds of materiel. In 2003, we applied flame - atomic absorption spectrometry for analyzing Ca, Cd, Cu, Pb, Zn...in vegetables and their extracted juices were collected form 11 locations of Dalat, including two kinds of vegetables (goods and safety) in both the summer and winter. Average concentration of Ca = 240 mg/kg wet, Cd = 0.035 mg/kg wet, Cu = 0.67 mg/kg wet, Mg = 131 mg/kg wet, Fe = 8.1/kg wet, Mn = 3.1/kg wet, Na = 3266 mg/kg wet, Pb = 0.345 mg/kg wet and Zn = 3.3 mg wet. In their extracted juices: Ca = 89 mg/kg wet, Cd = 0.008 mg/kg wet, Cu = 0.19 mg/kg wet, Mg = 43 mg/kg wet, Fe = 2.3 mg/kg wet, Mn = 0.61 mg/kg wet, Na = 971 mg/kg wet, Pb = 0.107 mg/kg wet and Zn = 0.65 mg/kg wet. (author)

Application of atomic absorption spectrophotometry to determine Cd, Cu, Pb, Zn,...in vegetable samples in Dalat

International Nuclear Information System (INIS)

Nguyen Giang; Nguyen Thanh Tam; Le Thi Ngoc Trinh; Truong Phuong Mai; Nguyen Van Minh

2004-01-01

Nowadays atomic absorption spectrometry has become valuable method for trace element analysis because high specificity; low detection litmus, easy to use; easy sample preparation, low investment and running costs... atomic absorption spectrometry is generally accepted as one the most suitable method for single - element analysis of trace elements in various kinds of materiel. In 2003, we applied flame - atomic absorption spectrometry for analyzing Ca, Cd, Cu, Pb, Zn...in vegetables and their extracted juices were collected form 11 locations of Dalat, including two kinds of vegetables (goods and safety) in both the summer and winter. Average concentration of Ca = 240 mg/kg wet, Cd = 0.035 mg/kg wet, Cu = 0.67 mg/kg wet, Mg = 131 mg/kg wet, Fe = 8.1/kg wet, Mn = 3.1/kg wet, Na = 3266 mg/kg wet, Pb = 0.345 mg/kg wet and Zn = 3.3 mg wet. In their extracted juices: Ca = 89 mg/kg wet, Cd = 0.008 mg/kg wet, Cu = 0.19 mg/kg wet, Mg = 43 mg/kg wet, Fe = 2.3 mg/kg wet, Mn = 0.61 mg/kg wet, Na = 971 mg/kg wet, Pb = 0.107 mg/kg wet and Zn = 0.65 mg/kg wet. (author)

Primary gas thermometry by means of laser-absorption spectroscopy: Determination of the Boltzmann constant

OpenAIRE

Casa, G.; Castrillo, A.; Galzerano, G.; Wehr, R.; Merlone, A.; Di Serafino, D.; Laporta, P.; Gianfrani, L.

2008-01-01

We report on a new optical implementation of primary gas thermometry based on laser absorption spectrometry in the near infrared. The method consists in retrieving the Doppler broadening from highly accurate observations of the line shape of the R(12) $\

Speciation and determination of ultra trace amounts of chromium by solidified floating organic drop microextraction (SFODME) and graphite furnace atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Moghadam, Masoud Rohani [Department of Chemistry, Faculty of Science, Yazd University, Yazd 89195-741 (Iran, Islamic Republic of); Dadfarnia, Shayessteh, E-mail: sdadfarnia@yazduni.ac.ir [Department of Chemistry, Faculty of Science, Yazd University, Yazd 89195-741 (Iran, Islamic Republic of); Haji Shabani, Ali Mohammad [Department of Chemistry, Faculty of Science, Yazd University, Yazd 89195-741 (Iran, Islamic Republic of)

2011-02-15

Solidified floating organic drop microextraction (SFODME) method in combination with graphite furnace atomic absorption spectrometry (GFAAS) has been used for the determination of chromium species in water and urine samples. 1-undecanol containing 2-thenoyltrifluoroacetone (TTA) was used as a selective chelating agent for the extraction of Cr(III). The total Cr was determined after the reduction of Cr(VI) to Cr(III) with hydroxylamine. The concentration of Cr(VI) was determined from the difference between the concentration of total chromium and the Cr(III). Several variables such as the sample pH, concentration of TTA, salt concentration, extraction time and the sample volume were investigated in detail. Under the optimum conditions, the limit of detection of the proposed method was 0.006 {mu}g l{sup -1} for Cr(III) and the relative standard deviation for six replicate determinations at 0.1 {mu}g l{sup -1} Cr(III) was 5.1%. The proposed method was successfully applied for the determination of chromium species in tap water, well water, mineral water, and urine samples.

A method optimization study for atomic absorption ...

African Journals Online (AJOL)

A sensitive, reliable and relative fast method has been developed for the determination of total zinc in insulin by atomic absorption spectrophotometer. This designed study was used to optimize the procedures for the existing methods. Spectrograms of both standard and sample solutions of zinc were recorded by measuring ...

Speciation of arsenic in water samples by high-performance liquid chromatography-hydride generation-atomic absorption spectrometry at trace levels using a post-column reaction system

Energy Technology Data Exchange (ETDEWEB)

Stummeyer, J. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany); Harazim, B. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany); Wippermann, T. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany)

1996-02-01

Anion-exchange HPLC has been combined with hydride generation - atomic absorption spectrometry (HG-AAS) for the routine speciation of arsenite, arsenate, monomethylarsenic acid and dimethylarsinic acid. The sensitivity of the AAS-detection was increased by a post-column reaction system to achieve complete formation of volatile arsines from the methylated species and arsenate. The system allows the quantitative determination of 0.5 {mu}g/l of each arsenic compound in water samples. The stability of synthetical and natural water containing arsenic at trace levels was investigated. To preserve stored water samples, a method for quantitative separation of arsenate at high pH-values with the basic anion-exchange resin Dowex 1 x 8 was developed. (orig.)

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

Directory of Open Access Journals (Sweden)

Şerife Tokalıoğlu

2017-01-01

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

Molecular absorption spectra of beryllium, cerium, lanthanum, iron, and platinum salts

International Nuclear Information System (INIS)

Daidoji, Hidehiro

1980-01-01

The absorption spectra of some salts of beryllium, cerium, lanthanum, iron and platinum in air-acetylene flame were measured in the wavelength range from 200 to 400 nm. A Hitachi 207 type atomic absorption spectrophotometer was used. A deuterium lamp, a home-made continuous radiation lamp and some hollow cathode lamps were used as light sources. The new molecular absorption spectra of cerium, lanthanum and platinum and the absorption spectra due to Be(OH) 2 , LaO, PtH, FeO and FeCl in 200-400 nm region were obtained. Emission spectra of CeO, LaO and FeOH were also obtained. These molecular absorption bands were estimated as absorption errors of maximum 15 times to the sensitivity of each elements in atomic absorption spectrometry. In addition, spectral line interferences of iron were observed in atomic absorption spectrometry of Zn, Cd, Ni, Cu and Cr. (author)

Utilization of electrodeposition for electrothermal atomic absorption spectrometry determination of gold

International Nuclear Information System (INIS)

Konecna, Marie; Komarek, Josef

2007-01-01

Gold was determined by electrothermal atomic absorption spectrometry after electrochemical preconcentration on the graphite ridge probe used as a working electrode and sample support. The probe surface was electrochemically modified with Pd, Re and the mixture of both. The electrolysis of gold was performed under galvanostatic control at 0.5 mA. Maximum pyrolysis temperature for the probe surface modified with Pd was 1200 deg. C, with Re 1300 deg. C. The relative standard deviation for the determination of 2 μg l -1 Au was not higher than 5.6% (n = 8) for 2 min electrodeposition. The sensitivity of gold determination was reproducible for 300 electrodeposition and atomization cycles. When the probe surface was modified with a mixture of Pd and Re the detection limit was 31 ng l -1 for 2 min electrodeposition, 3.7 ng l -1 for 30 min, 1.5 ng l -1 for 1 h and 0.4 ng l -1 for 4 h electrodeposition, respectively. The procedure was applied to the determination of gold in river water samples. The relative standard deviation for the determination of 2.5 ng l -1 Au at 4 h electrodeposition time at 0.5 mA was 7.5%

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)

Wang Yang; Luo Xiaoyu; Tang Jie; Hu Xiaoya; Xu Qin; Yang Chun

2012-01-01

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.

Analysis of metal-laden water via portable X-ray fluorescence spectrometry

Science.gov (United States)

Pearson, Delaina; Weindorf, David C.; Chakraborty, Somsubhra; Li, Bin; Koch, Jaco; Van Deventer, Piet; de Wet, Jandre; Kusi, Nana Yaw

2018-06-01

A rapid method for in-situ elemental composition analysis of metal-laden water would be indispensable for studying polluted water. Current analytical lab methods to determine water quality include flame atomic absorption spectrometry (FAAS), atomic absorption spectrophotometry (AAS), electrothermal atomic absorption spectrometry (EAAS), and inductively coupled plasma (ICP) spectroscopy. However only two field methods, colorimetry and absorptiometry, exist for elemental analysis of water. Portable X-ray fluorescence (PXRF) spectrometry is an effective method for elemental analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study sought to statistically establish PXRF's predictive ability for various elements in water at different concentrations relative to inductively coupled plasma atomic emission spectroscopy (ICP-AES). A total of 390 metal-laden water samples collected from leaching columns of mine tailings in South Africa were analyzed via PXRF and ICP-AES. The PXRF showed differential effectiveness in elemental quantification. For the collected water samples, the best relationships between ICP and PXRF elemental data were obtained for K and Cu (R2 = 0.92). However, when scanning ICP calibration solutions with elements in isolation, PXRF results indicated near perfect agreement; Ca, K, Fe, Cu and Pb produced an R2 of 0.99 while Zn and Mn produced an R2 of 1.00. The utilization of multiple PXRF (stacked) beams produced stronger correlation to ICP relative to the use of a single beam in isolation. The results of this study demonstrated the PXRF's ability to satisfactorily predict the composition of metal-laden water as reported by ICP for several elements. Additionally this study indicated the need for a "Water Mode" calibration for the PXRF and demonstrates the potential of PXRF for future study of polluted or contaminated waters.

Chemical methods of rock analysis

National Research Council Canada - National Science Library

Jeffery, P. G; Hutchison, D

1981-01-01

.... Such methods include those based upon spectrophotometry, flame emission spectrometry and atomic absorption spectroscopy, as well as gravimetry, titrimetry and the use of ion-selective electrodes...

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-02-15

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

Determination of Hg(II) in waters by on-line preconcentration using Cyanex 923 as a sorbent - Cold vapor atomic absorption spectrometry

International Nuclear Information System (INIS)

Duan Taicheng; Song Xuejie; Xu Jingwei; Guo Pengran; Chen Hangting; Li Hongfei

2006-01-01

Using a solid phase extraction mini-column home-made from a neutral extractant Cyanex 923, inorganic Hg could be on-line preconcentrated and simultaneously separated from methyl mercury. The preconcentrated Hg (II) was then eluted with 10% HNO 3 and subsequently reduced by NaBH 4 to form Hg vapor before determination by cold vapor atomic absorption spectrometry (CVAAS). Optimal conditions for and interferences on the Hg preconcentration and measurement were at 1% HCl, for a 25 mL sample uptake volume and a 10 mL min -1 sample loading rate. The detection limit was 0.2 ng L -1 and much lower than that of conventional method (around 15.8 ng L -1 ). The relative standard deviation (RSD) is 1.8% for measurements of 40 ng L -1 of Hg and the linear working curve is from 20 to 2000 ng L -1 (with a correlation coefficient of 0.9996). The method was applied in determination of inorganic Hg in city lake and deep well water (from Changchun, Jilin, China), and recovery test results for both samples were satisfactory

Validation of a hydride generation atomic absorption spectrometry methodology for determination of mercury in fish designed for application in the Brazilian national residue control plan.

Science.gov (United States)

Damin, Isabel C F; Santo, Maria A E; Hennigen, Rosmari; Vargas, Denise M

2013-01-01

In the present study, a method for the determination of mercury (Hg) in fish was validated according to ISO/IEC 17025, INMETRO (Brazil), and more recent European recommendations (Commission Decision 2007/333/EC and 2002/657/EC) for implementation in the Brazilian Residue Control Plan (NRCP) in routine applications. The parameters evaluated in the validation were investigated in detail. The results obtained for limit of detection and quantification were respectively, 2.36 and 7.88 μg kg(-1) of Hg. While the recovery varies between 90-96%. The coefficient of variation was of 4.06-8.94% for the repeatability. Furthermore, a comparison using an external proficiency testing scheme was realized. The results of method validated for the determination of the mercury in fish by Hydride generation atomic absorption spectrometry were considered suitable for implementation in routine analysis.

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

Directory of Open Access Journals (Sweden)

Prkić Ante

2017-08-01

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

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...

Liquid scintillation alpha spectrometry techniques

International Nuclear Information System (INIS)

McKlveen, J.W.; McDowell, W.J.

1984-01-01

Accurate, quantitative determinations of alpha emitting nuclides by conventional plate counting methods are difficult, because of sample self-absorption problems in counting and because of non-reproducible losses in conventional sample separation methods. Liquid scintillation alpha spectrometry offers an attractive alternative with no sample self-absorption or geometry problems and with 100% counting efficiency. Sample preparation may include extraction of the alpha emitter of interest by a specific organic phase-soluble compound directly into the liquid scintillation counting medium. Detection electronics use energy and pulse-shape discrimination, to yield alpha spectra without beta and gamma background interference. Specific procedures have been developed for gross alpha, uranium, plutonium, thorium and colonium assay. Possibilities for a large number of other applications exist. Accuracy and reproducibility are typically in the 1% range. Backgrounds of the order of 0.01 cpm are readily achievable. The paper will present an overview of liquid scintillation alpha counting techniques and some of the results achieved for specific applications. (orig.)

Development of a High-Resolution Laser Absorption Spectroscopy Method with Application to the Determination of Absolute Concentration of Gaseous Elemental Mercury in Air.

Science.gov (United States)

Srivastava, Abneesh; Hodges, Joseph T

2018-05-07

Isotope dilution-cold-vapor-inductively coupled plasma mass spectrometry (ID-CV-ICPMS) has become the primary standard for measurement of gaseous elemental mercury (GEM) mass concentration. However, quantitative mass spectrometry is challenging for several reasons including (1) the need for isotopic spiking with a standard reference material, (2) the requirement for bias-free passive sampling protocols, (3) the need for stable mass spectrometry interface design, and (4) the time and cost involved for gas sampling, sample processing, and instrument calibration. Here, we introduce a high-resolution laser absorption spectroscopy method that eliminates the need for sample-specific calibration standards or detailed analysis of sample treatment losses. This technique involves a tunable, single-frequency laser absorption spectrometer that measures isotopically resolved spectra of elemental mercury (Hg) spectra of 6 1 S 0 ← 6 3 P 1 intercombination transition near λ = 253.7 nm. Measured spectra are accurately modeled from first-principles using the Beer-Lambert law and Voigt line profiles combined with literature values for line positions, line shape parameters, and the spontaneous emission Einstein coefficient to obtain GEM mass concentration values. We present application of this method for the measurement of the equilibrium concentration of mercury vapor near room temperature. Three closed systems are considered: two-phase mixtures of liquid Hg and its vapor and binary two-phase mixtures of Hg-air and Hg-N 2 near atmospheric pressure. Within the experimental relative standard uncertainty, 0.9-1.5% congruent values of the equilibrium Hg vapor concentration are obtained for the Hg-only, Hg-air, Hg-N 2 systems, in confirmation with thermodynamic predictions. We also discuss detection limits and the potential of the present technique to serve as an absolute primary standard for measurements of gas-phase mercury concentration and isotopic composition.

Use of electrothermal atomic absorption spectrometry for size profiling of gold and silver nanoparticles.

Science.gov (United States)

Panyabut, Teerawat; Sirirat, Natnicha; Siripinyanond, Atitaya

2018-02-13

Electrothermal atomic absorption spectrometry (ETAAS) was applied to investigate the atomization behaviors of gold nanoparticles (AuNPs) and silver nanoparticles (AgNPs) in order to relate with particle size information. At various atomization temperatures from 1400 °C to 2200 °C, the time-dependent atomic absorption peak profiles of AuNPs and AgNPs with varying sizes from 5 nm to 100 nm were examined. With increasing particle size, the maximum absorbance was observed at the longer time. The time at maximum absorbance was found to linearly increase with increasing particle size, suggesting that ETAAS can be applied to provide the size information of nanoparticles. With the atomization temperature of 1600 °C, the mixtures of nanoparticles containing two particle sizes, i.e., 5 nm tannic stabilized AuNPs with 60, 80, 100 nm citrate stabilized AuNPs, were investigated and bimodal peaks were observed. The particle size dependent atomization behaviors of nanoparticles show potential application of ETAAS for providing size information of nanoparticles. The calibration plot between the time at maximum absorbance and the particle size was applied to estimate the particle size of in-house synthesized AuNPs and AgNPs and the results obtained were in good agreement with those from flow field-flow fractionation (FlFFF) and transmission electron microscopy (TEM) techniques. Furthermore, the linear relationship between the activation energy and the particle size was observed. Copyright © 2017 Elsevier B.V. All rights reserved.

Modular L-design of hydride atomizers for atomic absorption spectrometry

International Nuclear Information System (INIS)

Rezacova, Olga; Dedina, Jiri

2009-01-01

A novel modular L-shaped design of hydride atomizer for atomic absorption spectrometry is described. It makes it possible to replace the optical tube of the atomizer and, mainly, to employ optical tubes made also from other materials than fused quartz. The design is useful mainly for further improvement of hydride atomizers based on the multiatomizer concept. Employing selenium hydride as the analyte and arsine as the interferent, a preliminary evaluation of performance of three types of L-shaped multiatomizers based on various optical tubes in terms of sensitivity, linearity of calibration graph and resistance to atomization interferences is made. The 'classical' T-shaped multiatomizer was employed as a reference. The L-shaped multiatomizer with the optical tube analogous to that employed in the 'classical' T-shaped multiatomizer offers virtually the same performance as the reference multiatomizer. Optical tube made of fused quartz with holes with smaller diameters does not offer significantly better performance compared to the reference T-shaped multiatomizer. However, the L-shaped multiatomizer with optical tube fabricated from porous quartz glass overpowers all the other multiatomizers substantially in terms of the resistance against interferences: even the maximum As interferent concentration of 5 μg ml - 1 does not significantly influence the observed signal. This should be compared with multiatomizers based on plain fused quartz tubes with holes: tolerance limit around 0.5 μg ml - 1 ; interferent concentration of 1 μg ml - 1 causing 20% signal depression.

Development of a new green non-dispersive ionic liquid microextraction method in a narrow glass column for determination of cadmium prior to couple with graphite furnace atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Naeemullah, E-mail: naeemullah433@yahoo.com [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Kazi, Tasneem Gul [National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Tuzen, Mustafa [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Shah, Faheem; Afridi, Hassan Imran [National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Citak, Demirhan [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey)

2014-02-17

Graphical abstract: -- Highlights: •A novel and rapid non-dispersive ionic liquid based microextractions. •We used a long narrow glass column to provide more contact area between two media (aqueous and extractive). •APDC using as complexing agent and analyzed by GFAAS. •Introduced a novel approach that reduced solvent consumption, effort, time. •It was applied for determination of understudy analytes in real water sample. -- Abstract: Easy and innovative non-dispersive ionic liquid based microextraction (NDILME) has been developed for preconcentration of trace level of cadmium (Cd) in aqueous real surface water samples prior to couple with graphite furnace atomic absorption spectrometry (GFAAS). A 200 cm long narrow glass column containing aqueous solution of standard/sample was used to increase phase transfer ratio by providing more contact area between two medium (aqueous and extractive), which drastically improve the recoveries of labile hydrophobic chelate of Cd ammonium pyrrolidinedithiocarbamate (APDC), into ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate [C{sub 4}mim][PF{sub 6}]. Different aspect of the desire method have been investigated and optimized. Under the optimized key experimental variables, limit of detection (LOD) and enhancement factor (EF) were achieved to be 0.5 ng L{sup −1} and 150, respectively. Reliability of the model method was checked by relative standard deviation (%RSD), which was found to be < 5%. Validity and accuracy of the developed method was checked by analysis of certified reference water samples (SLRS-4 Riverine water) using standard addition method. Application of the model method was productively performed by analysis of Cd in real surface water samples (tap and sea)

Estimation of water absorption coefficient using the TDR method

Science.gov (United States)

Suchorab, Zbigniew; Majerek, Dariusz; Brzyski, Przemysław; Sobczuk, Henryk; Raczkowski, Andrzej

2017-07-01

Moisture accumulation and transport in the building barriers is an important feature that influences building performance, causing serious exploitation problems as increased energy use, mold and bacteria growth, decrease of indoor air parameters that may lead to sick building syndrome (SBS). One of the parameters that is used to describe moisture characteristic of the material is water absorption coefficient being the measure of capillary behavior of the material as a function of time and the surface area of the specimen. As usual it is determined using gravimetric methods according to EN 1925:1999 standard. In this article we demonstrate the possibility of determination of water absorption coefficient of autoclaved aerated concrete (AAC) using the Time Domain Reflectometry (TDR) method. TDR is an electric technique that had been adopted from soil science and can be successfully used for real-time monitoring of moisture transport in building materials and envelopes. Data achieved using TDR readouts show high correlation with standard method of moisture absorptivity coefficient determination.

Phytosterol glycosides reduce cholesterol absorption in humans.

Science.gov (United States)

Lin, Xiaobo; Ma, Lina; Racette, Susan B; Anderson Spearie, Catherine L; Ostlund, Richard E

2009-04-01

Dietary phytosterols inhibit intestinal cholesterol absorption and regulate whole body cholesterol excretion and balance. However, they are biochemically heterogeneous and a portion is glycosylated in some foods with unknown effects on biological activity. We tested the hypothesis that phytosterol glycosides reduce cholesterol absorption in humans. Phytosterol glycosides were extracted and purified from soy lecithin in a novel two-step process. Cholesterol absorption was measured in a series of three single-meal tests given at intervals of 2 wk to each of 11 healthy subjects. In a randomized crossover design, participants received approximately 300 mg of added phytosterols in the form of phytosterol glycosides or phytosterol esters, or placebo in a test breakfast also containing 30 mg cholesterol-d7. Cholesterol absorption was estimated by mass spectrometry of plasma cholesterol-d7 enrichment 4-5 days after each test. Compared with the placebo test, phytosterol glycosides reduced cholesterol absorption by 37.6+/-4.8% (Pphytosterol esters 30.6+/-3.9% (P=0.0001). These results suggest that natural phytosterol glycosides purified from lecithin are bioactive in humans and should be included in methods of phytosterol analysis and tables of food phytosterol content.

The Determination of Composite Elements in Zircaloy-2 by X-Ray Fluorescence and Emission Spectrometry Method

International Nuclear Information System (INIS)

Dian Anggraini; Rosika Kriswarini; Yusuf N

2007-01-01

Analysis of composing elements in zircaloy-2 has been done by Emission Spectrometry method and X-Ray Fluorescence (XRF). The aim of the analysis is to verify conformity between composing elements in zircaloy-2 and the material certificate. Spectrometry Emission method has higher sensitivity in element determination of a material than that of XRF method, so can be estimated that emission spectrometry method has higher accuracy than that of XRF method. The result of qualitative analysis by Emission Spectrometry indicate that the composing elements in zircaloy-2 were Sn, Cr and Ni. However, the qualitative analysis result by XRF method indicated that the composing elements in zircaloy 2 were Sn, Cr, Ni and Fe. Fe element can not be analysed by Emission Spectrometry method because Emission Spectrometer did not equipped with Fe detector. The quantitative analysis result of the composing elements in the material with both methods showed that Sn, Cr and Ni concentration of zircaloy 2 existed in concentration ranges of the material certificate. Result of statistical test (F and t-test) of analysis result of both methods can be used for analyzing composing elements in zircaloy 2. Emission Spectrometry method was more sensitive and accurate for determining Cr and Ni element in zircaloy 2 than that of emission Spectrometry method but both methods had same accuracy. The precision of measurement of Sn, Cr and Ni element using XRF method was better than that of Emission spectrometry method. (author)

Pre-analytic evaluation of volumetric absorptive microsampling and integration in a mass spectrometry-based metabolomics workflow.

Science.gov (United States)

Volani, Chiara; Caprioli, Giulia; Calderisi, Giovanni; Sigurdsson, Baldur B; Rainer, Johannes; Gentilini, Ivo; Hicks, Andrew A; Pramstaller, Peter P; Weiss, Guenter; Smarason, Sigurdur V; Paglia, Giuseppe

2017-10-01

Volumetric absorptive microsampling (VAMS) is a novel approach that allows single-drop (10 μL) blood collection. Integration of VAMS with mass spectrometry (MS)-based untargeted metabolomics is an attractive solution for both human and animal studies. However, to boost the use of VAMS in metabolomics, key pre-analytical questions need to be addressed. Therefore, in this work, we integrated VAMS in a MS-based untargeted metabolomics workflow and investigated pre-analytical strategies such as sample extraction procedures and metabolome stability at different storage conditions. We first evaluated the best extraction procedure for the polar metabolome and found that the highest number and amount of metabolites were recovered upon extraction with acetonitrile/water (70:30). In contrast, basic conditions (pH 9) resulted in divergent metabolite profiles mainly resulting from the extraction of intracellular metabolites originating from red blood cells. In addition, the prolonged storage of blood samples at room temperature caused significant changes in metabolome composition, but once the VAMS devices were stored at - 80 °C, the metabolome remained stable for up to 6 months. The time used for drying the sample did also affect the metabolome. In fact, some metabolites were rapidly degraded or accumulated in the sample during the first 48 h at room temperature, indicating that a longer drying step will significantly change the concentration in the sample. Graphical abstract Volumetric absorptive microsampling (VAMS) is a novel technology that allows single-drop blood collection and, in combination with mass spectrometry (MS)-based untargeted metabolomics, represents an attractive solution for both human and animal studies. In this work, we integrated VAMS in a MS-based untargeted metabolomics workflow and investigated pre-analytical strategies such as sample extraction procedures and metabolome stability at different storage conditions. The latter revealed that

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

Energy Technology Data Exchange (ETDEWEB)

Surtipanti, S; Suwirma, S; Yumiarti, S; Mellawati, Yune [National Atomic Energy Agency, Jakarta (Indonesia), Center for the Application of Isotopes Radiation

1995-01-01

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.

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

International Nuclear Information System (INIS)

Surtipanti, S.; Suwirma, S.; Yumiarti, S.; Mellawati, Yune

1995-01-01

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

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

A pre-concentration procedure using coprecipitation for determination of lead and iron in several samples using flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Saracoglu, S.; Soylak, M.; Peker, D.S. Kacar; Elci, L.; Santos, W.N.L. dos; Lemos, V.A.; Ferreira, S.L.C.

2006-01-01

The present paper proposes a pre-concentration procedure for determination of lead and iron in several samples by flame atomic absorption spectrometry. In it, lead(II) and iron(III) ions are coprecipitated using the violuric acid-copper(II) system as collector. Afterwards, the precipitate is dissolved with 1 M HNO 3 solution and the metal ions are determined. The optimization step was performed using factorial design involving the variables: pH, violuric acid mass (VA) and copper concentration (Cu). Using the optimized experimental conditions, the proposed procedure allows the determination these metals with detection limits of 0.18 μg L -1 for iron and 0.16 μg L -1 for lead. The effects of foreign ions on the pre-concentration procedure were also evaluated and the results demonstrated that this method could be applied for determination of iron and lead in several real samples. The proposed method was successfully applied to the analysis of seawater, urine, mineral water, soil and physiological solution samples. The concentrations of lead and iron achieved in these samples agree well with others data reported in the literature

Determination of trace amounts of rare earth elements in samarium, terbium and disprosium oxides by graphite furnace atomic-absorption spectrometry

International Nuclear Information System (INIS)

Dantas, E.S.K.

1990-01-01

A graphite furnace atomic-absorption spectrometry method for the determination of neodymium, europium, terbium, dysprosium and yttrium at trace level in samarium oxide; of samarium, europium, dysprosium, holmium, erbium and yttrium in terbium oxide and of europium, terbium, holmium, erbium and yttrium in dysprosium oxide was established. The best pyrolysis and atomization temperatures were determined for each lanthanide considered. Calibration curves were obtained for the pure elements, for binary mixtures formed by the matrix and each of the lanthanides studied and, finally, for the complex mixtures constituted by the matrix and all the other lanthanide of the group under scrutiny. This study has been carried out to examine the interference of the presence of one lanthanide on the behaviour of the other, since a lack of linearity on the calibration curves has been observed in some cases. Detection and determination limits have been determined as well. The detection limits encountered were within the range 0.002 to 0.3% for different elements. The precision of the method expressed as the relative standard deviation was calculated for each element present in each of the matrices studied. The conclusion arrived at is that the method can be applied for determining the above mentioned lanthanides present in the matrices studied with purity up to 99.50%. (author)

A new supramolecular based liquid solid microextraction method for preconcentration and determination of trace bismuth in human blood serum and hair samples by electrothermal atomic absorption spectrometry.

Science.gov (United States)

Kahe, Hadi; Chamsaz, Mahmoud

2016-11-01

A simple and reliable supramolecule-aggregated liquid solid microextraction method is described for preconcentration and determination of trace amounts of bismuth in water as well as human blood serum and hair samples. Catanionic microstructures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) surfactants, dissolved in deionized water/propanol, are used as a green solvent to extract bismuth (III)-diethyldithiocarbamate complexes by dispersive microextraction methodology. The extracted solid phase is easily removed and dissolved in 50 μL propanol for subsequent measurement by electrothermal atomic absorption spectrometry (ET-AAS). The procedure benefits the merits of supramolecule aggregates' properties and dispersive microextraction technique using water as the main component of disperser solvent, leading to direct interaction with analyte. Phase separation behavior of extraction solvent and different parameters influencing the extraction efficiency of bismuth ion such as salt concentration, pH, centrifugation time, amount of chelating agent, SDS:CTAB mole ratio, and solvent amounts were thoroughly optimized. Under the optimal experimental conditions, the calibration curve was linear in the range of 0.3-6 μg L -1 Bi (III) with a limit of detection (LOD) of 0.16 μg L -1 (S/N = 3). The relative standard deviations (RSD) of determination were obtained to be 5.1 and 6.2 % for 1 and 3 μg L -1 of Bi (III), respectively. The developed method was successfully applied as a sensitive and accurate technique for determination of bismuth ion in human blood serum, hair samples, and a certified reference material.

Analytical methods applied to water pollution

International Nuclear Information System (INIS)

Baudin, G.

1977-01-01

A comparison of different methods applied to water analysis is given. The discussion is limited to the problems presented by inorganic elements, accessible to nuclear activation analysis methods. The following methods were compared: activation analysis: with gamma-ray spectrometry, atomic absorption spectrometry, fluorimetry, emission spectrometry, colorimetry or spectrophotometry, X-ray fluorescence, mass spectrometry, voltametry, polarography or other electrochemical methods, activation analysis-beta measurements. Drinking-water, irrigation waters, sea waters, industrial wastes and very pure waters are the subjects of the investigations. The comparative evaluation is made on the basis of storage of samples, in situ analysis, treatment and concentration, specificity and interference, monoelement or multielement analysis, analysis time and accuracy. The significance of the neutron analysis is shown. (T.G.)

Flow analysis-hydride generation-gas phase derivative molecular absorption spectrophotometric determination of antimony in antileishmanial drugs

Directory of Open Access Journals (Sweden)

Máximo Gallignani

2009-01-01

Full Text Available In the present work, the development of a method based on the coupling of flow analysis (FA, hydride generation (HG, and derivative molecular absorption spectrophotometry (D-EAM in gas phase (GP, is described in order to determine total antimony in antileishmanial products. Second derivative order (D²224nm of the absorption spectrum (190 - 300 nm is utilized as measurement criterion. Each one of the parameters involved in the development of the proposed method was examined and optimized. The utilization of the EAM in GP as detection system in a continuous mode instead of atomic absorption spectrometry represents the great potential of the analytic proposal.

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

The determination of trace elements in uranium ores by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

De Villiers, W. van Z.

1983-11-01

The determination of 17 trace elements (As, Ba, Co, Cr, Cu, Mo, Nb, Ni, Pb, Rb, Sr, Th, U, V, Y, Zn and Zr) in uranium ores by x-ray fluorescence spectrometry was investigated in this study. The determination of major elements was also necessary for the calculation of mass absorption coefficients. Initially a method was developed for the determination of the elements of interest in unmineralised silicates. Correction for absorption of radiation by the sample were made by means of mass absorption coefficients which were obtained from the relation between the inverse of the mass absorption coefficient and the intensity of the Compton scattering peak. The Feather and Willis method was used for determining the background intensity at the peak positions as well as for mass absorption coefficients. It was observed that the background intensity in the region of the uranium lines increases with increasing uranium content of the sample

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous separation/preconcentration of nickel, cobalt and copper prior to determination by electrothermal atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Mooud Amirkavei

2013-01-01

Full Text Available A dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous extraction of trace amounts of nickel, cobalt and copper followed by their determination with electrothermal atomic absorption spectrometry was developed. 300 µL of acetone and 1-undecanol was injected into an aqueous sample containing diethyldithiocarbamate complexes of metal ions. For a sample volume of 10 mL, enrichment factors of 277, 270 and 300 and detection limits of 1.2, 1.1 and 1 ng L-1 for nickel, cobalt and copper were obtained, respectively. The method was applied to the extraction and determination of these metals in different water samples.

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

Science.gov (United States)

Altunay, Nail; Gürkan, Ramazan

2015-05-15

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

Use of the helium-3 proportional counter for neutron spectrometry

International Nuclear Information System (INIS)

Vialettes, H.; Le Thanh, P.

1967-01-01

Up to now, two methods have been mainly used for neutron spectrometry near nuclear installations: - photographic emulsion spectrometry - the so-called, 'multisphere' technique spectrometry. The first method, which is fairly difficult to apply, has a threshold energy of about 500 keV; this is a big disadvantage for an apparatus which has to be used for spectrometry around nuclear installations where the neutron radiation is very much degraded energetically. The second method does not suffer from this disadvantage but the results which it yields are only approximate. In order to extend the energy range of the neutron spectra studied with sufficient accuracy the use of a helium-3 proportional counter has been considered. This report presents the principles of operation of the helium-3 spectrometer, and the calculation methods which make it possible to take into account the two main effects tending to deform the spectra obtained: - energy absorption by the walls of the counter, - energy loss of the incident neutrons due to elastic collisions with helium-3 nuclei. As an example of the application, the shape of the neutron spectrum emitted by a polonium-lithium source is given; the results obtained are in excellent agreement with theoretical predictions. (authors) [fr

Dispersive liquid-liquid microextraction (DLLME combined with graphite furnace atomic absorption spectrometry (GFAAS for determination of trace Cu and Zn in water Samples

Directory of Open Access Journals (Sweden)

Ghorbani A.

2014-07-01

Full Text Available Dispersive liquid-liquid microextraction (DLLME combined with graphite furnace atomic absorption spectrometry (GFAAS was proposed for the determination of trace amounts of Copper and Zinc ions using 8-hydroxyquinoline (8-HQ as chelating agent. Several factors influencing the microextraction efficiency of Cu and Zn and their subsequent determinations, such as pH, extraction and disperser solvent type and their volume, concentration of the chelating agent and extraction time were studied, and the optimized experimental conditions were established. After extraction, the enrichment factors were 25 and 26 for Cu and Zn, respectively. The detection limits of the method were 0.025 and 0.0033 μg/L for Cu and Zn, and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Cu and Zn were 8.51% and 7.41%, respectively.

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.

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

International Nuclear Information System (INIS)

Katskov, Dmitri

2015-01-01

The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D 2 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

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

Energy Technology Data Exchange (ETDEWEB)

Katskov, Dmitri, E-mail: katskovda@tut.ac.za

2015-03-01

The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D{sub 2} 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

Modular L-design of hydride atomizers for atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Rezacova, Olga [Institute of Analytical Chemistry of the ASCR, v.v.i., Laboratory of Trace Element Analysis, Videnska 1083, CZ-142 20 Prague (Czech Republic); Charles University in Prague, Faculty of Science, Department of Analytical Chemistry, Albertov 8, Prague 2, CZ 128 43 (Czech Republic); Dedina, Jiri [Institute of Analytical Chemistry of the ASCR, v.v.i., Laboratory of Trace Element Analysis, Videnska 1083, CZ-142 20 Prague (Czech Republic)], E-mail: dedina@biomed.cas.cz

2009-07-15

A novel modular L-shaped design of hydride atomizer for atomic absorption spectrometry is described. It makes it possible to replace the optical tube of the atomizer and, mainly, to employ optical tubes made also from other materials than fused quartz. The design is useful mainly for further improvement of hydride atomizers based on the multiatomizer concept. Employing selenium hydride as the analyte and arsine as the interferent, a preliminary evaluation of performance of three types of L-shaped multiatomizers based on various optical tubes in terms of sensitivity, linearity of calibration graph and resistance to atomization interferences is made. The 'classical' T-shaped multiatomizer was employed as a reference. The L-shaped multiatomizer with the optical tube analogous to that employed in the 'classical' T-shaped multiatomizer offers virtually the same performance as the reference multiatomizer. Optical tube made of fused quartz with holes with smaller diameters does not offer significantly better performance compared to the reference T-shaped multiatomizer. However, the L-shaped multiatomizer with optical tube fabricated from porous quartz glass overpowers all the other multiatomizers substantially in terms of the resistance against interferences: even the maximum As interferent concentration of 5 {mu}g ml{sup - 1} does not significantly influence the observed signal. This should be compared with multiatomizers based on plain fused quartz tubes with holes: tolerance limit around 0.5 {mu}g ml{sup - 1}; interferent concentration of 1 {mu}g ml{sup - 1} causing 20% signal depression.

Extraction method based on emulsion breaking for the determination of Cu, Fe and Pb in Brazilian automotive gasoline samples by high-resolution continuum source flame atomic absorption spectrometry

Science.gov (United States)

Leite, Clarice C.; de Jesus, Alexandre; Kolling, Leandro; Ferrão, Marco F.; Samios, Dimitrios; Silva, Márcia M.

2018-04-01

This work reports a new method for extraction of Cu, Fe and Pb from Brazilian automotive gasoline and their determination by high-resolution continuous source flame atomic absorption spectrometry (HR-CS FAAS). The method was based on the formation of water-in-oil emulsion by mixing 2.0 mL of extraction solution constituted by 12% (w/v) Triton X-100 and 5% (v/v) HNO3 with 10 mL of sample. After heating at 90 °C for 10 min, two well-defined phases were formed. The bottom phase (approximately 3.5 mL), composed of acidified water and part of the ethanol originally present in the gasoline sample, containing the extracted analytes was analyzed. The surfactant and HNO3 concentrations and the heating temperature employed in the process were optimized by Doehlert design, using a Brazilian gasoline sample spiked with Cu, Fe and Pb (organometallic compounds). The efficiency of extraction was investigated and it ranged from 80 to 89%. The calibration was accomplished by using matrix matching method. For this, the standards were obtained performing the same extraction procedure used for the sample, using emulsions obtained with a gasoline sample free of analytes and the addition of inorganic standards. Limits of detection obtained were 3.0, 5.0 and 14.0 μg L-1 for Cu, Fe and Pb, respectively. These limits were estimated for the original sample taking into account the preconcentration factor obtained. The accuracy of the proposed method was assured by recovery tests spiking the samples with organometallic standards and the obtained values ranged from 98 to 105%. Ten gasoline samples were analyzed and Fe was found in four samples (0.04-0.35 mg L-1) while Cu (0.28 mg L-1) and Pb (0.60 mg L-1) was found in just one sample.

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)

Gil, Sandra; Lavilla, Isela; Bendicho, Carlos

2007-01-01

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, CO 2 , H 2 and H 2 O, 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

Species selective preconcentration and quantification of gold nanoparticles using cloud point extraction and electrothermal atomic absorption spectrometry.

Science.gov (United States)

Hartmann, Georg; Schuster, Michael

2013-01-25

The determination of metallic nanoparticles in environmental samples requires sample pretreatment that ideally combines pre-concentration and species selectivity. With cloud point extraction (CPE) using the surfactant Triton X-114 we present a simple and cost effective separation technique that meets both criteria. Effective separation of ionic gold species and Au nanoparticles (Au-NPs) is achieved by using sodium thiosulphate as a complexing agent. The extraction efficiency for Au-NP ranged from 1.01 ± 0.06 (particle size 2 nm) to 0.52 ± 0.16 (particle size 150 nm). An enrichment factor of 80 and a low limit of detection of 5 ng L(-1) is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L(-1). The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L(-1) is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Rapid determination of main components by means of flame-atomic-absorption spectrometry for chromium, silicon and tungsten in CrSiW materials

International Nuclear Information System (INIS)

Mueller, E.; Stahlberg, R.

1985-01-01

The application of Flame-Atomic-Absorption Spectrometry (FAAS) for determining chromium, silicon and tungsten in CrSiW materials is described. The FAAS determinations of the main components are shown under optimum conditions. Sufficient precision and reliability have been achieved for routine analysis. The application of a mixture of acids for preparing CrSiW solutions is proposed. The preparation of samples is discussed in detail. Optimum conditions are recommended for determining chromium, silicon and tungsten using one solution only. (orig.) [de

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Modified mesoporous silica materials for on-line separation and preconcentration of hexavalent chromium using a microcolumn coupled with flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Wang Zheng, E-mail: wangzheng@mail.sic.ac.cn [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Fang Dongmei; Li Qing [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); East China University of Science and Technology, Shanghai 200237 (China); Zhang Lingxia; Qian Rong; Zhu Yan; Qu Haiyun [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Du Yiping [East China University of Science and Technology, Shanghai 200237 (China)

2012-05-06

Highlights: Black-Right-Pointing-Pointer A modified SBA-15 mesoporous silica material (NH{sub 2}-SBA-15) was synthesized as sorbent. Black-Right-Pointing-Pointer The material was used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Black-Right-Pointing-Pointer The NH{sub 2}-SBA-15 enables retain Cr (VI) with an enrichment factor of 44. Black-Right-Pointing-Pointer The micro-column of NH{sub 2}-SBA-15 underwent more than 100 adsorption/desorption cycles. - Abstract: A modified SBA-15 mesoporous silica material NH{sub 2}-SBA-15 was synthesized successfully by grafting {gamma}-aminopropyl-triethoxysilane. The material was characterized using transmission electron microscopy (TEM) and Fourier transform infrared/Raman (FT-IR/Raman) spectroscopy, and used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Effective sorption of Cr (VI) was achieved at pH 2.0 with no interference from Cr (III) and other ions and 0.5 mol L{sup -1} NH{sub 3}{center_dot}H{sub 2}O solution was found optimal for the complete elution of Cr (VI). An enrichment factor of 44 and was achieved under optimized experimental conditions at a sample loading of 2.0 mL min{sup -1} sample loading (300 s) and an elution flow rate of 2.0 mL min{sup -1} (24 s). The precision of the 11 replicate Cr (VI) measurements was 2.1% at the 100 {mu}g L{sup -1} level with a detection limit of 0.2 {mu}g L{sup -1} (3 s, n = 10) using the FAAS. The developed method was successfully applied to trace chromium determination in waste water. The accuracy was validated using a certified reference material of riverine water (GBW08607).

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

International Nuclear Information System (INIS)

Heinemann, G.; Vogt, W.; Jacob, K.

1999-01-01

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.)

RAPID AND SENSITIVE DETERMINATION OF PALLADIUM USING HOMOGENEOUS LIQUID-LIQUID MICROEXTRACTION VIA FLOTATION ASSISTANCE FOLLOWED BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

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Mohammad Rezaee

2015-05-01

Full Text Available A method for the determination of trace amounts of palladium was developed using homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA followed by graphite furnace atomic absorption spectrometry (GFAAS. Ammonium pyrrolidine dithiocarbamate (APDC was used as a complexing agent. This was applied to determine palladium in three types of water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added to the extraction cell which contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Parameters affecting extraction efficiency were investigated and optimized. Under the optimum conditions, the calibration graph was linear in the range of 1.0-200 µg L-1 with a limit of detection of 0.3 µg L-1. The performance of the method was evaluated for the extraction and determination of palladium in water samples and satisfactory results were obtained. In order to verify the accuracy of the approach, the standard addition method was applied for the determination of palladium in spiked synthetic samples and satisfactory results were obtained.

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

Science.gov (United States)

Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

2016-03-04

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

Cloud point extraction combined with electrothermal atomic absorption spectrometry for the speciation of antimony(III) and antimony(V) in food packaging materials

International Nuclear Information System (INIS)

Jiang Xiuming; Wen Shengping; Xiang Guoqiang

2010-01-01

A simple, sensitive method for the speciation of inorganic antimony by cloud point extraction combined with electrothermal atomic absorption spectrometry (ETAAS) is presented and evaluated. The method based on the fact that formation of a hydrophobic complex of antimony(III) with ammonium pyrrolidine dithiocarbamate (APDC) at pH 5.0 and subsequently the hydrophobic complex enter into surfactant-rich phase, whereas antimony(V) remained in aqueous solutions. Antimony(III) in surfactant-rich phase was analyzed by ETAAS after dilution by 0.2 mL nitric acid in methanol (0.1 M), and antimony(V) was calculated by subtracting antimony(III) from the total antimony after reducing antimony(V) to antimony(III) by L-cysteine. The main factors affecting the cloud point extraction, such as pH, concentration of APDC and Triton X-114, equilibrium temperature and incubation time, sample volume were investigated in detail. Under the optimum conditions, the detection limit (3σ) of the proposed method was 0.02 ng mL -1 for antimony(III), and the relative standard deviation was 7.8% (c = 1.0 ng mL -1 , n = 7). The proposed method was successfully applied to speciation of inorganic antimony in the leaching solutions of different food packaging materials with satisfactory results.

A novel separation/preconcentration technique based on ultrasonic dispersion liquid-liquid microextraction for determination of trace cobalt by flame atomic absorption spectrometry

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Jingci Li

2012-12-01

Full Text Available An improved method for the determination of trace cobalt in water samples has been developed using ultrasonic dispersion liquid-liquid microextraction (US-DLLME prior to flame atomic absorption spectrometry (FAAS analysis. In this method, cobalt was extracted into the fine droplets of carbon tetrachloride after chelate formation with the water soluble ligand, ammonium pyrrolidine dithiocarbamate (APDC. The fine droplets of carbon tetrachloride were formed and dispersed in the aqueous sample with the help of ultrasonic waves which accelerated the formation of the fine cloudy solution without using disperser solvents. Under optimum conditions, the calibration curve was linear in the range of 2.5-500 μg L-1, with a detection limit of 0.8 μg L-1. The relative standard deviation (RSD for ten replicate measurements of 20 and 500 μg L-1 of cobalt were 3.3 and 2.2%. This proposed method was successfully applied to tap water, river water, and sea water, and accuracy was assessed through the analysis of certified reference water or recovery experiments. Operation simplicity, low cost, high enrichment factor, and low consumption of the extraction solvent are the main advantages of the proposed method.DOI: http://dx.doi.org/10.4314/bcse.v26i1.2

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. Copyright © 2016. Published by Elsevier B.V.

Application of gamma ray spectrometry and atomic absorption spectrometry for monitoring some radionuclides and heavy metals in sediments from the sudanese red sea coast

International Nuclear Information System (INIS)

Idris, A. M.; Eltayeb, M. A.

2004-01-01

A total of 31 surface sediment samples were collected from port-sudan harbour, sawakin harbour and the fringing reefs area that are located along the Sudanese coast of the red sea. The sampling was performed to provide good spatial coverage taking into account man's activity in port-sudan harbour and the fringing reefs area. the bulk samples were analyzed for some natural and anthropogenic radionuclides ( 226 Ra, 228 Ra, 40 K, 137 Cs) using direct gamma-ray spectrometry. Concentration of some heavy metals were determined in five fractions with grain-size of 1.000-0.500 m lm, 0.500-0.250 m lm, 0.250-0.125 m lm, 0.125-0.063 m lm and less than 0.063 m lm. The fractionation process was performed using dry sieving method. A total of 155 sub-samples (fractions) were digested by wet digestion method and analyzed for Mn, Fe, Ni, Cu, Zn, and Pb using flame atomic absorption spectrometry. Quality assurance of the obtained data was achieved through the analysis of certified reference materials. the radioactivity concentration ranges of ( 226 Ra, 228 Ra, and 40 K,) are 2.5-25.1b/kg, 2.1-13.1b q/kg,21.6- 429 Bq/kg, respectively. For ( 137 Cs)measurements, the highest value is 8.3 Bq/kg while most of samples were below the detection limits of the system. The concentration ranges of Mn, Fe, Cu, Zn, and Pb are 53.3-819 mg/kg, 1.4-51 mg/g, 8-131 mg/kg 9.5-113 mg/kg, 18.4-142 mg/kg, and 4.0-26.6 mg/kg, respectively. The granulometric normalization shows that some samples were subjected to anthropogenic activities. This finding was reinforced by results that were obtained from enrichment factor calculations and statistical multivariate analysis that is principal component analysis (Pca), also the Pca indicates that silt/clay fraction (>0.063 m lm ) is the dominant source for the emission of anthropogenic activities. From viewpoint of mineralogical composition the cluster analysis has distributed the samples into tow clusters. Dominant elements in sediments (Mn and Fe ) recorded

Análise direta de sólidos por espectrometria de absorção atômica com atomização em forno de grafite: uma revisão Solid sampling graphite furnace atomic absorption spectrometry: a review

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Cassiana Seimi Nomura

2008-01-01

Full Text Available This is a review of direct analysis using solid sampling graphite furnace atomic absorption spectrometry. Greater emphasis is dedicated to sample preparation, sample homogeneity, calibration and its application to microanalysis and micro-homogeneity studies. The main advantages and some difficulties related to the applicability of this technique are discussed. A literature search on the application of solid sampling graphite furnace atomic absorption spectrometry in trace element determination in many kinds of samples, including biological, clinical, technological and environmental ones, is also presented.

A new concept of efficient therapeutic drug monitoring using the high-resolution continuum source absorption spectrometry and the surface enhanced Raman spectroscopy

Science.gov (United States)

Xing, Yanlong; Fuss, Harald; Lademann, Jürgen; Huang, Mao Dong; Becker-Ross, Helmut; Florek, Stefan; Patzelt, Alexa; Meinke, Martina C.; Jung, Sora; Esser, Norbert

2018-04-01

In this study, a new therapeutic drug monitoring approach has been tested based on the combination of CaF molecular absorption using high-resolution continuum source absorption spectrometry (HR-CSAS) and surface enhanced Raman spectroscopy (SERS). HR-CSAS with mini graphite tube was successfully tested for clinical therapeutic drug monitoring of the fluorine-containing drug capecitabine in sweat samples of cancer patients: It showed advantageous features of high selectivity (no interference from Cl), high sensitivity (characteristic mass of 0.1 ng at CaF 583.069 nm), low sample consumption (down to 30 nL) and fast measurement (no sample pretreatment and less than 1 min of responding time) in tracing the fluorine signal out of capecitabine. However, this technique has the disadvantage of the total loss of the drug's structure information after burning the sample at very high temperature. Therefore, a new concept of combining HR-CSAS with a non-destructive spectroscopic method (SERS) was proposed for the sensitive sensing and specific identification of capecitabine. We tested and succeed in obtaining the molecular characteristics of the metabolite of capecitabine (named 5-fluorouracil) by the non-destructive SERS technique. With the results shown in this work, it is demonstrated that the combined spectroscopic technique of HR-CSAS and SERS will be very useful in efficient therapeutic drug monitoring in the future.

The use of slurry sampling for the determination of manganese and copper in various samples by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Tokman, Nilgun

2007-01-01

Manganese and copper in multivitamin-mineral supplements and standard reference materials were determined by slurry sampling electrothermal atomic absorption spectrometry. Slurries were prepared in an aqueous solution containing Triton X-100. The effects of different parameters such as ratio of solid to liquid phase volume, total slurry volume and addition of Triton X-100 as a dispersant on the analytical results were investigated. The graphite furnace programs were optimized for slurry sampling depending on the analytes and their concentrations in the samples. The linear calibration method with aqueous standard solutions was used for the quantification. At optimum experimental conditions, R.S.D. values were below 5%. The analytes were determined in the limits of 95% confidence level with respect to certified values in coal and soil standard reference materials and to those found by wet-digestion in multivitamin-mineral supplements. Detection limits (3δ) for Mn and Cu were 0.10 μg L -1 and 1.82 μg L -1 for 10 μL coal standard reference material slurry, respectively

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

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Alves Flávia L.

2000-01-01

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

The comparison of benzene and CO2 absorption methods for radioisotope 14C dating

International Nuclear Information System (INIS)

Satrio and Zainal Abidin

2007-01-01

It had been conducted to research of age determination of carbon samples using CO 2 absorption method. This method as alternative to benzene synthesis method for radioisotope 14 C dating.The aim of the method is to support some hydrology research's especially groundwater dating using environmental radioisotope 14 C.The results which obtain by CO 2 absorption method then compared with the results of benzene synthesis method consists of background counter, standard counter, activity and age limit, age, and material cost or component. The research show that compared with benzene synthesis method, sample preparation using CO 2 absorption method is more simple and relatively low cost. The use of CO 2 absorption method can save the cost about 75 %. The different of both methods is age limit detection. The results of age limit detection when using CO 2 absorption and synthesis benzene methods are 33,310 years and 47,533 years respectively. Whereas, based on t test, the age results of both methods for the same sample are obtained relatively equal. (author)

On-line preconcentration of ultra-trace thallium(I in water samples with titanium dioxide nanoparticles and determination by graphite furnace atomic absorption spectrometry

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Saeid Asadpour

2016-11-01

Full Text Available A new method has been developed for the determination of Tl(I based on simultaneous sorption and preconcentration with a microcolumn packed with TiO2 nanoparticle with a high specific surface area prepared by Sonochemical synthesis prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS. The optimum experimental parameters for preconcentration of thallium, such as elution condition, pH, and sample volume and flow rate have been investigated. Tl(I can be quantitatively retained by TiO2 nanoparticles at pH 9.0, then eluted completely with 1.0 mol L−1 HCl. The adsorption capacity of TiO2 nanoparticles for Tl(I was found to be 25 mg g−1. Also detection limit, precision (RSD, n = 8 and enrichment factor for Tl(I were 87 ng L−1, 6.4% and 100, respectively. The method has been applied for the determination of trace amounts of Tl(I in some environmental water samples with satisfactory results.

[Determination of trace lead and cadmium in transgenic rice by crosslinked carboxymethyl konjac glucomannan microcolumn preconcentration combined with graphite furnace atomic absorption spectrometry].

Science.gov (United States)

Liu, Hua-qing; Li, Sheng-qing; Qu, Yang; Chen, Hao

2012-02-01

A novel method was developed for the determination of trace lead and cadmium in transgenic brown rice based on separation and preconcentration with a micro column packed with crosslinked carboxymethyl konjac glucomannan (CCMKGM) prior to its determination by graphite furnace atomic absorption spectrometry. Variables affecting the separation and preconcentration of lead and cadmium, such as the acidity of the aqueous solution, sample flow rate and volume, and eluent concentration and volume, were optimized. Under optimized condition, detection limits of the method for the determination of trace lead and cadmium in transgenic brown rice were 0.11 and 0.002 microg x L(-1), respectively. The obtained results of lead and cadmium in the certified reference material (GBW10010, GBS1-1) were in good agreement with the certified values. The recoveries were in the range of 90%-103% and 93%-105% for detection of Pb and Cd in transgenic brown rice and the wild-type brown rice samples respectively. This study could provide technical support for determination of trace Pb and Cd in transgenic rice.

Preconcentration, speciation and determination of ultra trace amounts of mercury by modified octadecyl silica membrane disk/electron beam irradiation and cold vapor atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ashkenani, Hamid [Department of Chemistry, Yazd University, Yazd (Iran, Islamic Republic of); Dadfarnia, Shayessteh [Department of Chemistry, Yazd University, Yazd (Iran, Islamic Republic of)], E-mail: sdadfarnia@yazduni.ac.ir; Shabani, Ali Mohammad Haji; Jaffari, Abbas Ali [Department of Chemistry, Yazd University, Yazd (Iran, Islamic Republic of); Behjat, Abbas [Department of physics, Yazd University, Yazd (Iran, Islamic Republic of)

2009-01-15

Mercury (II) and methyl mercury cations at the Sub-ppb level were adsorbed quantitatively from aqueous solution onto an octadecyl-bonded silica membrane disk modified by 2-[(2-mercaptophyenylimino)methyl] phenol (MPMP). The trapped mercury was then eluted with 3 ml ethanol and Hg{sup 2+} ion was directly measured by cold vapor atomic absorption spectrometry, utilizing tin (II) chloride. Total mercury (Hgt) was determined after conversion of MeHg{sup +} into Hg{sup 2+} ion by electron beam irradiation. A sample volume of 1500 ml resulted in a preconcentration factor of 500 and the precision for a sampling volume of 500 ml at a concentration of 2.5 {mu}g l{sup -1} (n = 7) was 3.1%. The limit of detection of the proposed method is 3.8 ng l{sup -1}. The method was successfully applied to analysis of water samples, and the accuracy was assessed via recovery experiment.

Design of a tritium gas cell for beta-ray induced X-ray spectrometry using Monte Carlo simulation

Energy Technology Data Exchange (ETDEWEB)

Hara, Masanori, E-mail: masahara@ctg.u-toyama.ac.jp [Hydrogen Isotope Research Center, Organization for Promotion of Research, University of Toyama, 3190 Gofuku, Toyama City, Toyama 930-8555 (Japan); Abe, Shinsuke; Matsuyama, Masao [Hydrogen Isotope Research Center, Organization for Promotion of Research, University of Toyama, 3190 Gofuku, Toyama City, Toyama 930-8555 (Japan); Aso, Tsukasa [Electronics and Computer Engineering, National Institute of Technology, Toyama College, 1-2 Ebie-neriya, Imizu City, Toyama 933-0293 (Japan); Tatenuma, Katsuyoshi; Kawakami, Tomohiko; Ito, Takeshi [KAKEN Company Limited, 1044 Horimachi, Mito City, Ibaraki 310-0903 (Japan)

2017-06-15

Highlights: • Beta-ray induced X-ray spectrometry (BIXS) is a method for tritium gas analysis. • Gas cell for BIXS was designed by Monte Carlo simulations. • The optimum thickness of the gold layer on a beryllium window was around 150 nm. • This simulation model considered the self-absorption with increasing the cell length. - Abstract: One of the methods used for tritium gas analysis is beta-ray induced X-ray spectrometry (BIXS). Gas cell design is important in this method. The structure of the gas cell for BIXS was optimized by Monte Carlo simulation of beta-ray induced X-ray spectra in various window geometries using the Geant4 tool kit (version 10.01.p02). The simulated spectrum from tritium decay fitted the observed one, and the simulation model was used to obtain the cell parameters for BIXS. The optimum thickness of the gold layer on a beryllium window was around 150 nm. This simulation model also considered the relationship between self-absorption by hydrogen gas and the cell length. Self-absorption increased with increasing cell length and the relationship between the sample pressure and cell length was formulated.

Optimization of microwave assisted digestion procedure for the determination of zinc, copper and nickel in tea samples employing flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Soylak, Mustafa; Tuzen, Mustafa; Souza, Anderson Santos; Korn, Maria das Gracas Andrade; Ferreira, Sergio Luis Costa

2007-01-01

The present paper describes the development of a microwave assisted digestion procedure for the determination of zinc, copper and nickel in tea samples employing flame atomic absorption spectrometry (FAAS). The optimization step was performed using a full factorial design (2 3 ) involving the factors: composition of the acid mixture (CMA), microwave power (MP) and radiation time (RT). The experiments of this factorial were carried out using a certified reference material of tea GBW 07605 furnished by National Research Centre for Certified Reference Materials, China, being the metal recoveries considered as response. The relative standard deviations of the method were found below 8% for the three elements. The procedure proposed was used for the determination of copper, zinc and nickel in several samples of tea from Turkey. For 10 tea samples analyzed, the concentration achieved for copper, zinc and nickel varied at 6.4-13.1, 7.0-16.5 and 3.1-5.7 (μg g -1 ), respectively

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

International Nuclear Information System (INIS)

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

2009-01-01

A recent survey indicated that high-dose vitamin A supplements (HD-VAS) had no apparent effect on vitamin A (VA) status of Zambian children 14 C 2 )-labeled VA was co-administered with the HD-VAS or SI-labeled VA, and 24-hr stool and urine samples were collected for 3 and 7 consecutive days, respectively, and 24-hr urine samples at 4 later time points. Accelerator Mass Spectrometry (AMS) was used to measure the cumulative excretion of 14 C in stool and urine 3d after dosing to estimate, respectively, absorption and retention of the VAS and SI-labeled VA. The urinary elimination rate (UER) was estimated by plotting 14 C in urine vs. time, and fitting an exponential equation to the data. Estimates of mean absorption, retention and the UER were 83.8 ± 7.1%, 76.3 ± 6.7%, and 1.9 ± 0.6%/d, respectively, for the HD-VAS and 76.5 ± 9.5%, 71.1 ± 9.4%, and 1.8 ± 1.2%/d, respectively for the smaller dose of SI-labeled VA. Estimates of absorption, retention and the UER did not differ by size of the VA dose administered (P=0.26, 0.40, 0.88, respectively). Estimated absorption and retention were negatively associated with reported fever (P=0.011) and malaria (P =0.010). HD-VAS and SI-labeled VA were adequately absorbed, retained and utilized in apparently healthy Zambian preschool-age boys, although absorption and retention may be affected by recent infections.

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

International Nuclear Information System (INIS)

Shokri, Masood; Beiraghi, Asadollah; Seidi, Shahram

2015-01-01

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

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)

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

2015-01-01

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

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.

Nickel and strontium nitrates as modifiers for the determination of selenium in wine by Zeeman electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Cvetkovic, J. [Inst. of Agriculture, Skopje (Yugoslavia); Stafilov, T. [Inst. of Chemistry, Faculty of Science Sts. Cyril and Methodius Univ., Skopje (Yugoslavia); Mihajlovic, D. [RZ Tehnicka Kontrola, Skopje (Yugoslavia)

2001-08-01

A mixed matrix modifier of nickel and strontium nitrates was used as a chemical modifier for the determination of selenium in wines by Zeeman electrothermal atomic absorption spectrometry. Wine samples were heated on a boiling water bath with small amounts of nitric acid and hydrogen peroxide. For complete elimination of interference, especially from sulfates and phosphates, selenium is complexed with ammonium pyrolidinedithiocarbamate (APDTC), extracted into methyl isobutyl ketone (MIBK), and measured by ETAAS. The graphite furnace temperature program was optimized for both aqueous and organic solutions. Pyrolysis temperatures of 1300 C and 800 C were chosen for aqueous and organic solutions, respectively; 2700 C and 2100 C were used as optimum atomization temperatures for aqueous and organic solutions, respectively. The optimum modifier mass established is markedly lower than those presented in the literature. The platform atomization ensures pretreatment stabilization up to 1100 C and 1600 C, respectively, for organic and aqueous selenium solutions. The procedure was verified by the method of standard addition. The investigated wine samples originated from the different regions of the Republic of Macedonia. The selenium concentration varied from not detectable to 0.93 {mu}g L{sup -1}. (orig.)

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.

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

International Nuclear Information System (INIS)

Tokalioglu, Serife; Oymak, Tuelay; Kartal, Senol

2004-01-01

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

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.

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

International Nuclear Information System (INIS)

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

2013-01-01

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 −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

New advanced in alpha spectrometry by liquid scintillation methods

International Nuclear Information System (INIS)

McDowell, W.J.; Case, G.N.

1979-01-01

Although the ability to count alpha particles by liquid scintillation methods has been long recognized, limited use has been made of the method because of problems of high background and alpha energy identification. In recent years some new developments in methods of introducing the alpha-emitting nuclide to the scintillator, in detector construction, and in electronics for processing the energy analog and time analog signals from the detector have allowed significant alleviation of the problems of alpha spectrometry by liquid scintillation. Energy resolutions of 200 to 300 keV full peak width at half maximum and background counts of 99% of all beta plus gamma interference is now possible. Alpha liquid scintillation spectrometry is now suitable for a wide range of applications, from the accurate quantitative determination of relatively large amounts of known nuclides in laboratory-generated samples to the detection and identification of very small, subpicocurie amounts of alpha emitters in environmental-type samples. Suitable nuclide separation procedures, sample preparation methods, and instrument configurations are available for a variety of analyses

[Determination of inorganic elements in different parts of Sonchus oleraceus L by flame atomic absorption spectrometry].

Science.gov (United States)

Wang, Nai-Xing; Cui, Xue-Gui; Du, Ai-Qin; Mao, Hong-Zhi

2007-06-01

Flame atomic absorption spectrometry with air-acetylene flame was used for the determination of inorganic metal elements in different parts ( flower, leaf, stem and root) of Sonchus oleraceus L. The contents of Ca, Mg, K, Na, Fe, Mn, Cu, Zn, Cr, Co, Ni, Pb and Cd in the flower, leaf, stem and root of Sonchus oleraceus L were compared. The order from high to low of the additive weight (microg x g(-1)) for the 13 kinds of metal elements is as follows: leaf (77 213.72) > flower (47 927.15) > stem(42 280.99) > root (28 131.18). From the experimental results it was found that there were considerable differences in the contents of the metal elements in different parts, and there were richer contents of Fe, Zn, Mn and Cu in root and flower, which are necessary to human health, than in other parts.

Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

International Nuclear Information System (INIS)

Andrada, Daniel; Pinto, Frederico G.; Magalhaes, Cristina Goncalves; Nunes, Berta R.; Silva, Jose Bento Borba da; Franco, Milton B.

2006-01-01

The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ETAAS). Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 μL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO 3 1% v/v and 0.02% v/v of cetyl trimethyl ammonium chloride (CTAC) were prepared directly in the autosampler cups and placed into the graphite furnace. For modifiers in solutions 10 μL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 μg), the best pyrolysis and atomization temperatures were 900 and 1600 deg C, respectively, with a characteristic mass of 12 pg (recommended of 10 pg), with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence) for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh) and between 93.9 and 105.2% (Zr+Rh). In both recovery studies, the relative standard deviation (n=3) was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r 2 higher than 0.99. The limits of detection were 0.7 μg L -1 for serum samples, with Zr+Rh permanent, and 1.0 μg L -1 for urine with iridium permanent. (author)

Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

Directory of Open Access Journals (Sweden)

Andrada Daniel

2006-01-01

Full Text Available The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ET AAS. Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 µL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO3 1% v/v and 0.02% v/v of cetil trimethyl ammonium chloride (CTAC were prepared directly in the autosampler cups and placed into the graphite furnace. For modifiers in solutions 10 µL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 µg, the best pyrolysis and atomization temperatures were 900 and 1600 ºC, respectively, with a characteristic mass of 12 pg (recommended of 10 pg, with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh and between 93.9 and 105.2% (Zr+Rh. In both recovery studies, the relative standard deviation (n=3 was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r² higher than 0.99. The limits of detection were 0.7 µg L-1 for serum samples, with Zr+Rh permanent, and 1.0 µg L-1 for urine with iridium permanent.

Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

International Nuclear Information System (INIS)

Cortez Diaz, Mirella del Carmen

2002-01-01

Heavy metals are a big source of environmental contamination and are also highly toxic to humans. Since shellfish are bio-accumulators of these metals, proper techniques for quantifying them should be available. This work aims to develop an analytical method for the quantitative determination of heavy metals in biological materials (shellfish), specifically arsenic and cadmium at the trace level, using graphite furnace atomic absorption spectrometry, for which nickel and phosphate solutions were used to modify the modifiers. Prior to the analysis, the sample was diluted with nitric acid in a DAB II pressure digestion system order to destroy the organic matter. The instrument conditions were initially set (wavelength, slit, integration peaks, graphite tube, etc.), then the work range was defined for each element and the most appropriate operational parameters were studied, such as: temperature, ramp times, hold times and internal gas flow, in the different stage of the electrothermal treatment (drying, calcination, atomization) for the furnace program. Once the above mentioned conditions were set and since this was a biological sample, a matrix chemical modifier had to be used, in order to make the elements that accompany the element being studied more volatile. In this way the chemical and spectral interferences decrease together with the high background absorption of the matrix. Therefore, different matrix modifiers were studied for the definition of each analyte. The method validation was done using Certified Oyster Tissue Reference Material N o 1566a from the National Institute of Standards and Technology applying different tests in order to eliminate outliers. Repeatability, uncertainty, sensitivity, lineal range, working range, detection limit and quantification limit were evaluated for each element, and the results were compared with the values for the certified material. The Fisher and Student tests were the statistical tools used. The experimental values

Study of absorption spectra for alkali and alkaline earth metal salts in flameless atomic absorption spectrometry using a carbon tube atomizer

International Nuclear Information System (INIS)

Yasuda, Seiji; Kakiyama, Hitoo

1975-01-01

Absorption spectra of various salts such as alkali metal salts, alkaline earth dichlorides, and ammonium halides were investigated and absorptions of some molecular species produced in the carbon tube were identified. The aqueous solution (20 μl) containing 1.0 mg/ml of each salt was placed in the carbon tube atomizer and heated in a similar manner to usual flameless atomic absorption method. D 2 -lamp was used as a continuous light source and argon gas was employed as an inert sheath gas. The spectra were obtained over the range of wavelength 200 to 350 nm. When alkali halides were feeded, the absorption spectra agreed with those of alkali halide vapors. Therefore, in such cases vapors of the alkali halides were probably produced by the sublimation or vaporization in the atomizer. The spectra of alkali perchlorates were considered to be those of alkali chlorides produced by the pyrolysis of the perchlorates in the atomizer. The absorptions of alkaline earth chlorides below 250 nm were probably due to their gaseous states. Sulfur dioxide was found to be produced by the pyrolysis of alkali sulfates, bisulfates and sulfites in the atomizer, Alkali phosphates and pyrophosphates gave almost identical spectra below 300 nm. Gamma band spectrum of nitrogen monoxide was observed from 200 to 240 nm during ashing at bout 330 0 C for alkali nitrates and nitrites. Ammonia vapor was produced from ammonium halides during drying at about 170 0 C. Although the absorptions of alkali carbonates and hydroxides were almost undetectable, the same spectra as those of alkali halides were observed by the addition of ammonium halides to the solutions of alkali compounds. This shows that alkali halides are produced in the atomizer by the addition of halide ions. (auth.)

A new atomization cell for trace metal determinations by tungsten coil atomic spectrometry

Energy Technology Data Exchange (ETDEWEB)

Donati, G.L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Wildman, R.B.; Jones, B.T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)

2011-02-28

A new metallic atomization cell is used for trace metal determinations by tungsten coil atomic absorption spectrometry and tungsten coil atomic emission spectrometry. Different protecting gas mixtures are evaluated to improve atomic emission signals. Ar, N{sub 2}, CO{sub 2} and He are used as solvents, and H{sub 2} and C{sub 2}H{sub 2} as solutes. A H{sub 2}/Ar mixture provided the best results. Parameters such as protecting gas flow rate and atomization current are also optimized. The optimal conditions are used to determine the figures of merit for both methods and the results are compared with values found in the literature. The new cell provides a better control of the radiation reaching the detector and a small, more isothermal environment around the atomizer. A more concentrated atomic cloud and a smaller background signal result in lower limits of detection using both methods. Cu (324.7 nm), Cd (228.8 nm) and Sn (286.3 nm) determined by tungsten coil atomic absorption spectrometry presented limits of detection as low as 0.6, 0.1, and 2.2 {mu}g L{sup -1}, respectively. For Cr (425.4 nm), Eu (459.4 nm) and Sr (460.7 nm) determined by tungsten coil atomic emission spectrometry, limits of detection of 4.5, 2.5, and 0.1 {mu}g L{sup -1} were calculated. The method is used to determine Cu, Cd, Cr and Sr in a water standard reference material. Results for Cu, Cd and Cr presented no significant difference from reported values in a 95% confidence level. For Sr, a 113% recovery was obtained.

Determination of sulfur in bovine serum albumin and L-cysteine using high-resolution continuum source molecular absorption spectrometry of the CS molecule

Science.gov (United States)

Andrade-Carpente, Eva; Peña-Vázquez, Elena; Bermejo-Barrera, Pilar

2016-08-01

In this study, the content of sulfur in bovine serum albumin and L-cysteine was determined using high-resolution continuum source molecular absorption spectrometry of the CS molecule, generated in a reducing air-acetylene flame. Flame conditions (height above the burner, measurement time) were optimized using a 3.0% (v/v) sulfuric acid solution. A microwave lab station (Ethos Plus MW) was used for the digestion of both compounds. During the digestion step, sulfur was converted to sulfate previous to the determination. Good repeatability (4-10%) and analytical recovery (91-106%) was obtained.

The new concept of hyphenated analytical system: Simultaneous determination of inorganic arsenic(III), arsenic(V), selenium(IV) and selenium(VI) by high performance liquid chromatography-hydride generation-(fast sequential) atomic absorption spectrometry during single analysis

International Nuclear Information System (INIS)

Niedzielski, P.

2005-01-01

The paper presents a new conception of determination of inorganic speciation forms of arsenic: As(III) and As(V) as well selenium Se(IV) and Se(VI) by means of the high performance liquid chromatography hyphenated with a detection by the atomic absorption spectrometry with hydride generation (HPLC-HG-AAS). The application of optimization procedure conditions of chromatographic separation of arsenic and selenium speciation forms (using anion-exchange Supelco LC-SAX1 column and phosphate buffer at pH 5.40 as a mobile phase) as well as the use of the atomic absorption spectrometry as a detector, which enables work in fast sequential mode, allowed to develop original detection methodology of simultaneous determination of arsenic As(III), As(V) and selenium Se(IV) and Se(VI) speciation forms within a 220 s single analysis. The obtained detection limits were 7.8 ng mL -1 for As(III); 12.0 ng mL -1 for As(V); 2.4 ng mL -1 for Se(IV) and 18.6 ng mL -1 for Se(VI) and precision 10.5%, 12.1%, 14.2% and 17.3%, respectively, for 100 ng mL -1 . The described method was used for ground water analysis

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

Science.gov (United States)

Liang, Pei; Kang, Caiyan; Mo, Yajun

2016-01-01

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

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

Science.gov (United States)

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

2016-04-01

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

Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

Energy Technology Data Exchange (ETDEWEB)

Gil, Sandra [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Fragueiro, Sandra [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain)]. E-mail: bendicho@uvigo.es

2005-01-10

A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-{mu}l volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium.

Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

International Nuclear Information System (INIS)

Gil, Sandra; Fragueiro, Sandra; Lavilla, Isela; Bendicho, Carlos

2005-01-01

A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-μl volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium

Atmospheric pressure photo ionization hydrogen/deuterium exchange mass spectrometry--a method to differentiate isomers by mass spectrometry.

Science.gov (United States)

Ahmed, Arif; Kim, Sunghwan

2013-12-01

In this report, a method for in-source hydrogen/deuterium (H/D) exchange at atmospheric pressure is reported. The method was named atmospheric pressure photo ionization hydrogen/deuterium exchange mass spectrometry (APPI HDX MS). H/D exchange was performed by mixing samples dissolved in toluene with CH3OD solvent and analyzing the mixture using atmospheric pressure photo ionization mass spectrometry (APPI-MS). The APPI HDX spectra obtained with contact times between the analyte solution and methanol-OD (CH3OD) of atmospheric pressure. H/D exchange can be performed in any laboratory with a mass spectrometer and a commercial APPI source. Using this method, multiple H/D exchanges of aromatic hydrogen and/or H/D exchange of active hydrogen were observed. These results demonstrated that H/D exchange can be used to distinguish between isomers containing primary, secondary, and tertiary amines, as well as pyridine and pyrrole functional groups.

Determination of total arsenic and arsenic(III) in phosphate fertilizers by hydride generation atomic absorption spectrometry after ultrasound-assisted extraction based on a control acid media.

Science.gov (United States)

Rezende, Helen Cristine; Coelho, Nivia Maria Melo

2014-01-01

An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample flow rate, and concentrations of the acid and reducer. The determination of As(lll) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 23 factorial design and central composite design. LODs for As(lll) and total As were 0.029 and 0.022 microg/L, respectively. The accuracy of the method was confirmed with certified reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples.

Elimination of ionic interference effects in the atomic absorption spectrometric determination of ruthenium

International Nuclear Information System (INIS)

El-Defrawy, M.M.M.; Posta, J.; Beck, M.T.

1978-01-01

In connection with work on the catalytic effect of ruthenium complexes, new compounds were prepared. Atomic absorption spectrometry (a.a.s.) was to be used for their analysis. The standard methods could not be applied to the complexes studied, therefore the effect of cyanide ions for elimination of interfering effects has been studied, because of the great stability of cyanide complexes. (Auth.)

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

International Nuclear Information System (INIS)

Romero, Vanesa; Costas-Mora, Isabel; Lavilla, Isela; Bendicho, Carlos

2011-01-01

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

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

Directory of Open Access Journals (Sweden)

A. A. Asweisi

2010-01-01

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

In-situ gamma spectrometry method for determination of environmental gamma dose; Metodo de espectrometria gamma in situ para determinacao de dose gama ambiental

Energy Technology Data Exchange (ETDEWEB)

Conti, Claudio de Carvalho

1995-07-15

This work tries to establish a methodology for germanium detectors calibration, normally used for in situ gamma ray spectrometry, for determining the environmental exposure rate in function of the energy of the incident photons. For this purpose a computer code has been developed, based on the stripping method, for the computational spectra analysis to calculate the contribution of the partial absorption of the gamma rays (Compton effect) in the active and nonactive parts of the detector. The resulting total absorption spectrum is then converted to fluence distribution in function of the energy for the photons reaching the detector, which is then used to calculate the exposure rate or kerma in air. The unfolding and fluency convention parameters are determined by detector calibration using point gamma sources. The method is validated by comparison of the results against the calculated exposure rate at a point of interest for the standards. This method is used for the direct measurement of the exposure rate distribution in function of the energy at the site, in situ measurement technic, leading to rapid results during an emergency situation and also used for indoor measurements. (author)

A method for determination mass absorption coefficient of gamma rays by Compton scattering

International Nuclear Information System (INIS)

El Abd, A.

2014-01-01

A method was proposed for determination mass absorption coefficient of gamma rays for compounds, alloys and mixtures. It is based on simulating interaction processes of gamma rays with target elements having atomic numbers from Z=1 to Z=92 using the MCSHAPE software. Intensities of Compton scattered gamma rays at saturation thicknesses and at a scattering angle of 90° were calculated for incident gamma rays of different energies. The obtained results showed that the intensity of Compton scattered gamma rays at saturations and mass absorption coefficients can be described by mathematical formulas. These were used to determine mass absorption coefficients for compound, alloys and mixtures with the knowledge of their Compton scattered intensities. The method was tested by calculating mass absorption coefficients for some compounds, alloys and mixtures. There is a good agreement between obtained results and calculated ones using WinXom software. The advantages and limitations of the method were discussed. - Highlights: • Compton scattering of γ−rays was used for determining mass absorption coefficient. • Scattered intensities were determined by the MCSHAPE software. • Mass absorption coefficients were determined for some compounds, mixtures and alloys. • Mass absorption coefficients were calculated by Winxcom software. • Good agreements were found between determined and calculated results

Different methods for modeling absorption heat transformer powered by solar pond

International Nuclear Information System (INIS)

Sencan, Arzu; Kizilkan, Onder; Bezir, Nalan C.; Kalogirou, Soteris A.

2007-01-01

Solar ponds are a type of solar collector used for storing solar energy at temperature below 90 o C. Absorption heat transformers (AHTs) are devices used to increase the temperature of moderately warm fluid to a more useful temperature level. In this study, a theoretical modelling of an absorption heat transformer for the temperature range obtained from an experimental solar pond with dimensions 3.5 x 3.5 x 2 m is presented. The working fluid pair in the absorption heat transformer is aqueous ternary hydroxide fluid consisting of sodium, potassium and caesium hydroxides in the proportions 40:36:24 (NaOH:KOH:CsOH). Different methods such as linear regression (LR), pace regression (PR), sequential minimal optimization (SMO), M5 model tree, M5' rules, decision table and back propagation neural network (BPNN) are used for modelling the absorption heat transformer. The best results were obtained by the back propagation neural network model. A new formulation based on the BPNN is presented to determine the flow ratio (FR) and the coefficient of performance (COP) of the absorption heat transformer. The BPNN procedure is more accurate and requires significantly less computation time than the other methods

Hooked differential mobility spectrometry apparatus and method therefore

Science.gov (United States)

Shvartsburg, Alexandre A [Richland, WA; Tang, Keqi [Richland, WA; Ibrahim, Yehia M [Richland, WA; Smith, Richard D [Richland, WA

2009-02-17

Disclosed are a device and method for improved interfacing of differential mobility spectrometry (DMS) or field asymmetric waveform ion mobility spectrometry (FAIMS) analyzers of substantially planar geometry to subsequent or preceding instrument stages. Interfacing is achieved using curved DMS elements, where a thick ion beam emitted by planar DMS analyzers or injected into them for ion filtering is compressed to the gap median by DMS ion focusing effect in a spatially inhomogeneous electric field. Resulting thinner beams are more effectively transmitted through necessarily constrained conductance limit apertures to subsequent instrument stages operated at a pressure lower than DMS, and/or more effectively injected into planar DMS analyzers. The technology is synergetic with slit apertures, slit aperture/ion funnels, and high-pressure ion funnel interfaces known in the art which allow for increasing cross-sectional area of MS inlets. The invention may be used in integrated analytical platforms, including, e.g., DMS/MS, LC/DMS/MS, and DMS/IMS/MS that could replace and/or enhance current LC/MS methods, e.g., for proteomics research.

Comparison of neutron activation analysis with other instrumental methods for elemental analysis of airborne particulate matter

International Nuclear Information System (INIS)

Regge, P. de; Lievens, F.; Delespaul, I.; Monsecour, M.

1976-01-01

A comparison of instrumental methods, including neutron activation analysis, X-ray fluorescence spectrometry, atomic absorption spectrometry and emission spectrometry, for the analysis of heavy metals in airborne particulate matter is described. The merits and drawbacks of each method for the routine analysis of a large number of samples are discussed. The sample preparation technique, calibration and statistical data relevant to each method are given. Concordant results are obtained by the different methods for Co, Cu, Ni, Pb and Zn. Less good agreement is obtained for Fe, Mn and V. The results are not in agreement for the elements Cd and Cr. Using data obtained on the dust sample distributed by Euratom-ISPRA within the framework of an interlaboratory comparison, the accuracy of each method for the various elements is estimated. Neutron activation analysis was found to be the most sensitive and accurate of the non-destructive analysis methods. Only atomic absorption spectrometry has a comparable sensitivity, but requires considerable preparation work. X-ray fluorescence spectrometry is less sensitive and shows biases for Cr and V. Automatic emission spectrometry with simultaneous measurement of the beam intensities by photomultipliers is the fastest and most economical technique, though at the expense of some precision and sensitivity. (author)

Absorption mechanism of three curcumin constituents through in situ intestinal perfusion method

Directory of Open Access Journals (Sweden)

Y.-H. Wang

2017-09-01

Full Text Available This study aimed to investigate the absorption mechanism of three curcumin constituents in rat small intestines. Self-emulsification was used to solubilize the three curcumin constituents, and the rat in situ intestinal perfusion method was used to study factors on drug absorption, including drug mass concentration, absorption site, and the different types and concentrations of absorption inhibitors. Within the scope of experimental concentrations, three curcumin constituents were absorbed in rat small intestines through the active transport mechanism.

Alpha particle analysis using PEARLS spectrometry

International Nuclear Information System (INIS)

McKlveen, J.W.; Klingler, G.W.; McDowell, W.J.; Case, G.N.

1984-01-01

Alpha particle assay by conventional plate-counting methods is difficult because chemical separation, tracer techniques, and/or self-absorption losses in the final sample may cause either non-reproducible results or create unacceptable errors. PEARLS (Photon-Electron Rejecting Alpha Liquid Scintillation) Spectrometry is an attractive alternative since radionuclides may be extracted into a scintillator in which there would be no self-absorption or geometry problems and in which up to 100% chemical recovery and counting efficiency is possible. Sample preparation may include extraction of the alpha emitter of interest by a specific organic-phase-soluble compound directly into the liquid scintillator. Detection electronics use energy and pulse-shape discrimination to provide discrete alpha spectra and virtual absence of beta and gamma backgrounds. Backgrounds on the order of 0.01 cpm are readily achievable. Accuracy and reproducibility are typically in the 100 +-1% range. Specific procedures have been developed for gross alpha, uranium, plutonium, thorium, and polonium assay. This paper will review liquid scintillation alpha counting methods and reference some of the specific applications. 8 refs., 1 fig

Determination of gold and cobalt dopants in advanced materials based on tin oxide by slurry sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

Science.gov (United States)

Filatova, Daria G.; Eskina, Vasilina V.; Baranovskaya, Vasilisa B.; Vladimirova, Svetlana A.; Gaskov, Alexander M.; Rumyantseva, Marina N.; Karpov, Yuri A.

2018-02-01

A novel approach is developed for the determination of Co and Au dopants in advanced materials based on tin oxide using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) with direct slurry sampling. Sodium carboxylmethylcellulose (Na-CMC) is an effective stabilizer for diluted suspensions. Use Na-CMC allows to transfer the analytes into graphite furnace completely and reproducibly. The relative standard deviation obtained by HR CS GFAAS was not higher than 4%. Accuracy was proven by means inductively coupled plasma mass spectrometry (ICP-MS) in solutions after decomposition as a comparative technique. To determine Au and Co in the volume of SnO2, the acid decomposition conditions (HCl, HF) of the samples were suggested by means of an autoclave in a microwave oven.

Modified carbon nanotubes as a sorbent for solid-phase extraction of gold, and its determination by graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Moghaddam, Firouzeh Hassani; Behzadi, Mansoureh; Naghizadeh, Matin; Taher, Mohammad Ali

2015-01-01

A simple, sensitive and accurate method was developed for solid-phase extraction and preconcentration of trace levels of gold in various samples. It is based on the adsorption of gold on modified oxidized multi-walled carbon nanotubes prior to its determination by graphite furnace atomic absorption spectrometry. The type and volume of eluent solution, sample pH value, flow rates of sample and eluent, sorption capacity and breakthrough volume were optimized. Under these conditions, the method showed linearity in the range of 0.2–6.0 ng L −1 with coefficients of determination of >0.99 in the sample. The relative standard deviation for seven replicate determinations of gold (at a level of 0.6 ng L −1 ) is ±3.8 %, the detection limit is 31 pg L −1 (in the initial solution and at an S/N ratio of 3; for n = 8), and the enrichment factor is 200. The sorption capacity of the modified MWCNTs for gold(III) is 4.15 mg g −1 . The procedure was successfully applied to the determination of gold in (spiked) water samples, human hair, human urine and standard reference material with recoveries ranging from 97.0 to 104.2 %. (author)

Use of slurry sampling for the direct determination of zinc in yogurt by high resolution-continuum source flame atomic absorption spectrometry.

Science.gov (United States)

Brandao, Geovani C; de Jesus, Raildo M; da Silva, Erik G P; Ferreira, Sergio L C

2010-06-15

This paper presents an analytical procedure for the direct determination of zinc in yogurt employing sampling slurry and high resolution-continuum source flame atomic absorption spectrometry (HR-CS FAAS). The step optimization established the experimental conditions of: 2.0molL(-1) hydrochloric acid, a sonication time of 20min and a sample mass of 1.0g for a slurry volume of 25mL. This method allows the determination of zinc with a limit of quantification of 0.32microgg(-1). The precision expressed as relative standard deviation (RSD) were 0.82 and 2.08% for yogurt samples containing zinc concentrations of 4.85 and 2.49microgg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of non-fat milk powder furnished by the National Institute of Standard and Technology. The proposed method was applied for the determination of zinc in seven yogurt samples. The zinc content was varied from 2.19 to 4.85microgg(-1). These results agreed with those reported in the literature. The samples were also analyzed after acid digestion and zinc determination by FAAS. No statistical difference was observed between the results obtained by both of the procedures performed.

Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

International Nuclear Information System (INIS)

Virgilio, Alex; Nóbrega, Joaquim A.; Rêgo, Jardes F.; Neto, José A. Gomes

2012-01-01

A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 °C and 2400 °C, respectively. Slopes of calibration curves (50–750 pg Cr, R 2 > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3–17.7 μg g −1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g −1 Cr. The limit of detection was 3.3 ng g −1 Cr. - Highlights: ► Direct solid sampling is first time employed for Cr in plant materials. ► Calibration curves with liquids and solids are coincident. ► Microanalysis of plants for Cr is validated by reference materials. ► The proposed HR-CS GF AAS method is environmental friendly.

Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

Energy Technology Data Exchange (ETDEWEB)

Virgilio, Alex; Nobrega, Joaquim A. [Department of Chemistry, Federal University of Sao Carlos, Post Office Box 676, 13560-970, Sao Carlos-SP (Brazil); Rego, Jardes F. [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil); Neto, Jose A. Gomes, E-mail: anchieta@iq.unesp.br [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil)

2012-12-01

A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 Degree-Sign C and 2400 Degree-Sign C, respectively. Slopes of calibration curves (50-750 pg Cr, R{sup 2} > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 {mu}g g{sup -1} Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 {+-} 2.1 {mu}g g{sup -1} Cr. The limit of detection was 3.3 ng g{sup -1} Cr. - Highlights: Black-Right-Pointing-Pointer Direct solid sampling is first time employed for Cr in plant materials. Black-Right-Pointing-Pointer Calibration curves with liquids and solids are coincident. Black-Right-Pointing-Pointer Microanalysis of plants for Cr is validated by reference materials. Black-Right-Pointing-Pointer The proposed HR-CS GF AAS method is environmental friendly.

Speciation and determination of inorganic mercury and methylmercury by headspace single drop microextraction and electrothermal atomic absorption spectrometry in water and fish

Energy Technology Data Exchange (ETDEWEB)

Sarica, Deniz Yurtsever [Scientific and Technological Research Council of Turkey, Ankara Test and Analysis Laboratory, TUeBITAK/ATAL, Besevler, Ankara (Turkey); Tuerker, Ali Rehber [Science Faculty, Department of Chemistry, Gazi University, Ankara (Turkey)

2012-05-15

In this study, headspace single drop microextraction (HS-SDME) method in combination with electrothermal atomic absorption spectrometry (ETAAS) method was developed and validated for the speciation and determination of inorganic mercury (iHg) and methylmercury (MeHg). MeHg and iHg species were reduced to volatile methylmercury hydride (CH{sub 3}HgH) and elemental mercury, respectively, in the presence of NaBH{sub 4} and trapped onto a drop of acceptor phase in the tip of a microsyringe. Thiourea and ammonium pyrrolydinedithiocarbamate (APDC) were tested as the acceptor phase. The experimental parameters of the method such as microextraction time, temperature, NaBH{sub 4} concentration, acceptor phase concentration, and pH of the medium were investigated to obtain distinctive conditions for mercury species. Possible interference effects have also been investigated. In order to validation of the method, analytical figures of merits such as accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), and linear working range have been evaluated. Accuracy of the method has been verified by analyzing certified reference materials (BCR 453 Tuna fish) and spiked samples. The proposed method was applied for the speciation and determination of mercury species in water and fish samples. Mercury species (MeHg and iHg) have been determined in the real samples with a relative error less than 10%. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Nonlinear Absorptions of CdSeTe Quantum Dots under Ultrafast Laser Radiation

Directory of Open Access Journals (Sweden)

Zhijun Chai

2016-01-01

Full Text Available The oil-soluble alloyed CdSeTe quantum dots (QDs are prepared by the electrostatic method. The basic properties of synthesized CdSeTe QDs are characterized by UV-Vis absorption spectroscopy, photoluminescence spectroscopy, inductively coupled plasma mass spectrometry, and transmission electron microscope. The off-resonant nonlinear optical properties of CdSeTe QDs are studied by femtosecond Z-scan at 1 kHz (low-repetition rate and 84 MHz (high-repetition rate. Nonlinear absorption coefficients are calculated under different femtosecond laser excitations. Due to the long luminescent lifetime of CdSeTe QDs, under the conditions of high-repetition rate, for open-aperture curve, heat accumulation and bleaching of ground state are responsible for the decrease of two-photon absorption (TPA coefficient.

Determination of metallic impurities in raw materials for radioisotope production by atomic absorption spectroscopy

International Nuclear Information System (INIS)

Roca, M.; Alvarez, F.; Capdevila, C.

1969-01-01

Atomic absorption spectrometry has been used for the determination of traces of calcium in scandium oxide, copper in zinc, iron in cobalt oxide, manganese In ferric oxide, nickel in copper and zinc in gallium oxide. The influences on the sensitivities arising from the hollow cathode currents, the gas pressures and the acid concentrations have been considered. A study of the interferences from the metallic matrices has also been performed, the interference due to the absorption of the manganese radiation by the atoms of iron being the most outstanding . In order to remove the interfering elements and increase sensitivity, pre-concentration methods have been tested. The addition methods has also been used. (Author) 14 refs

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

International Nuclear Information System (INIS)

Leal, L.O.; Elsholz, O.; Forteza, R.; Cerda, V.

2006-01-01

A new software-controlled time-based multisyringe flow injection system for mercury determination by cold-vapor atomic absorption spectrometry is proposed. Precise known volumes of sample, reducing agent (1.1% SnCl 2 in 3% HCl) and carrier (3% HCl) are dispensed into a gas-liquid separation cell with a multisyringe burette coupled with one three-way solenoid valve. An argon flow delivers the reduced mercury to the spectrometer. The optimization of the system was carried out testing reaction coils and gas-liquid separators of different design as well as changing parameters, such as sample and reagents volumes, reagent concentrations and carrier gas flow rate, among others. The analytical curves were obtained within the range 50-5000 ng L -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

Investigation of an alternating current plasma as an element selective atomic emission detector for high-resolution capillary gas chromatography and as a source for atomic absorption and atomic emission spectrometry

Science.gov (United States)

Ombaba, Jackson M.

This thesis deals with the construction and evaluation of an alternating current plasma (ACP) as an element-selective detector for high resolution capillary gas chromatography (GC) and as an excitation source for atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES). The plasma, constrained in a quartz discharge tube at atmospheric pressure, is generated between two copper electrodes and utilizes helium as the plasma supporting gas. The alternating current plasma power source consists of a step-up transformer with a secondary output voltage of 14,000 V at a current of 23 mA. The device exhibits a stable signal because the plasma is self-seeding and reignites itself every half cycle. A tesla coil is not required to commence generation of the plasma if the ac voltage applied is greater than the breakdown voltage of the plasma-supporting gas. The chromatographic applications studied included the following: (1) the separation and selective detection of the organotin species, tributyltin chloride (TBT) and tetrabutyltin (TEBT), in environmental matrices including mussels (Mvutilus edullus) and sediment from Boston Harbor, industrial waste water and industrial sludge, and (2) the detection of methylcyclopentadienyl manganesetricarbonyl (MMT) and similar compounds used as gasoline additives. An ultrasonic nebulizer (common room humidifier) was utilized as a sample introduction device for aqueous solutions when the ACP was employed as an atomization source for atomic absorption spectrometry and as an excitation source for atomic emission spectrometry. Plasma diagnostic parameters studied include spatial electron number density across the discharge tube, electronic, excitation and ionization temperatures. Interference studies both in absorption and emission modes were also considered. Figures of merits of selected elements both in absorption and emission modes are reported. The evaluation of a computer-aided optimization program, Drylab GC, using

Interferometric measurement of lines shift in flames in connection with interpretation of lined absorption method in atomic absorption spectroscopy

International Nuclear Information System (INIS)

L'vov, B.V.; Polzik, L.K.; Katskov, D.A.; Kruglikova, L.P.

1975-01-01

This paper is concerned with interferometric measuring of the line shift in flames in the view of interpretation of absorption lines in the atomic absorption spectroscopy. The newly measured line shifts were compared to the known data on Lorentz broadening of the same lines obtained by methods free of the systematic errors. The resonant lines of the alkaline earth elements (Sr, Ca, Ba) were investigated. To reduce self-absorption in the flame the solutions with minimum concentrations of the elements were used. The computation scheme includes the spectrometer apparatus width and line broadening due to the self-absorption. Formulae are given for computing the values studied. Good agreement was observed between the computed and experimental results. Error analysis was performed. It was concluded that any line shifts in the hydrocarbons were correctly taken into an account in the absolute computations of absorption

Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero, E-mail: carlos.herrero@usc.es

2014-11-01

The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption–elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L{sup −1}, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64–22.9 μg Pb L{sup −1}). - Highlights: • Lead determination in urine using a solid phase extraction procedure followed by ETAAS • Carbon nanotubes as SPE adsorbent for Pb in urine • Matrix elimination for the Pb determination in urine by using SPE based on carbon nanotubes • The detection limit was 0.08 μg Pb L{sup −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. Copyright © 2014 Elsevier Ltd. All rights reserved.

X-ray spectrometry with synchrotron radiation; Roentgenspektrometrie mit Synchrotronstrahlung

Energy Technology Data Exchange (ETDEWEB)

Mueller, Matthias [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany). Arbeitsgruppe ' Roentgen- und IR-Spektrometrie' ; Gerlach, Martin; Holfelder, Ina; Hoenicke, Philipp; Lubeck, Janin; Nutsch, Andreas; Pollakowski, Beatrix; Streeck, Cornelia; Unterumsberger, Rainer; Weser, Jan; Beckhoff, Burkhard

2014-12-15

The X-ray spectrometry of the PTB at the BESSY II storage ring with radiation in the range from 78 eV to 10.5 keV is described. After a description of the instrumentation development reference-sample free X-ray fluorescence analysis, the determination of fundamental atomic parameters, X-ray fluorescence analysis under glance-angle incidence, highly-resolving absorption spectrometry, and emission spectrometry are considered. Finally liquid cells and in-situ measurement techniques are described. (HSI)

Synthesize of silver-nanoparticles by plant extract and its application for preconcentration of cadmium followed by flame atomic absorption spectrometry.

Science.gov (United States)

Almertaha, Abdul-Hossein; Eftekhari, Mohammad; Chamsaz, Mahmoud; Gheibi, Mohammad

2018-02-02

In this paper, Mentha pulegium leaves extract was used as a green reducing agent for the synthesis of silver-nanoparticles. The synthesized silver-nanoparticles were characterized by UV-VIS spectrophotometry, transmission electron microscopy, X-ray spectroscopy and used as an adsorbent for preconcentration of trace levels of cadmium (ІІ). After the desorption of cadmium (ІІ) in 5 mol L -1 formic acid, the desorbent solution was aspirated into the flame atomic absorption spectrometry for the determination of cadmium. In order to optimize the experimental condition, a response surface methodology based on central composite design was used. The optimum conditions are: pH: 8.6, amounts of adsorbent: 30 mg, 10 min extraction time and desorption time of 2 min. Under the optimum condition, the calibration curve was linear in the range of 5-200 μg L -1 cadmium (ІІ) ion with a correlation coefficient of 0.9995. The limit of detection was 1.1 μg L -1 and the relative standard deviation for 25 μg L -1 cadmium (ІІ) ion was 3.0% (n = 5). In order to check the applicability of the proposed method, different real samples were analyzed. Also, the accuracy of this method was successfully checked by the analysis of certified reference material and spike tests.

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)

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

2012-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

K Latin-Small-Letter-Dotless-I l Latin-Small-Letter-Dotless-I nc, Ersin, E-mail: ekilinc@dicle.edu.tr [Dicle University, Faculty of Science, Department of Chemistry, Laboratory of Chemical Analysis, TR 21280 Diyarbak Latin-Small-Letter-Dotless-I r (Turkey); Bak Latin-Small-Letter-Dotless-I rdere, Sezgin [Y Latin-Small-Letter-Dotless-I ld Latin-Small-Letter-Dotless-I z Technical University, Faculty of Education, Department of Science Education, TR 34210 Esenler-Istanbul (Turkey); Ayd Latin-Small-Letter-Dotless-I n, F Latin-Small-Letter-Dotless-I rat [Dicle University, Faculty of Science, Department of Chemistry, Laboratory of Chemical Analysis, TR 21280 Diyarbak Latin-Small-Letter-Dotless-I r (Turkey); Ataman, O. Yavuz [Middle East Technical University, Faculty of Arts and Sciences, Department of Chemistry, 06800 Ankara (Turkey)

2012-07-15

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{sup -1}. %RSD was calculated as 4.0% for five replicate measurements of 7.5 ng mL{sup -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.

X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Vries, J.L. de.

1976-01-01

The seventh edition of Philips' Review of Literature on x-ray fluorescence spectrometry starts with a list of conference proceedings on the subject, organised by the Philips organisation at regular intervals in various European countries. It is followed by a list of bulletins. The bibliography is subdivided according to spectra, equipment, applications and absorption analysis

Mechanism of selenium hydride atomization, fate of free atoms and temperature distribution in an argon shielded, highly fuel-rich, hydrogen-oxygen diffusion micro-flame studied by atomic absorption spectrometry

Czech Academy of Sciences Publication Activity Database

D'Ulivo, A.; Dědina, Jiří; Lampugnani, L.; Matoušek, Tomáš

2002-01-01

Roč. 17, č. 3 (2002), s. 253-257 ISSN 0267-9477 R&D Projects: GA ČR GA203/01/0453; GA ČR GA203/98/0754 Institutional research plan: CEZ:AV0Z4031919 Keywords : hydride atomization * hydride generation * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.250, year: 2002

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

Science.gov (United States)

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

2010-06-30

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

Selective reduction of arsenic species by hydride generation - atomic absorption spectrometry. Part 2 - sample storage and arsenic determination in natural waters

Directory of Open Access Journals (Sweden)

Quináia Sueli P.

2001-01-01

Full Text Available Total arsenic, arsenite, arsinate and dimethylarsinic acid (DMA were selectively determined in natural waters by hydride generation - atomic absorption spectrometry, using sodium tetrahydroborate(III as reductant but in different reduction media. River water samples from the north region of Paraná State, Brazil, were analysed and showed arsenate as the principal arsenical form. Detection limits found for As(III (citrate buffer, As(III + DMA (acetic acid and As(III + As(V (hydrochloric acid were 0.6, 1.1 and 0.5 mg As L-1, respectively. Sample storage on the proper reaction media revealed to be a useful way to preserve the water sample.

Determination of lead in whole blood: Comparison of the LeadCare blood lead testing system with zeeman longitudinal electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Pineau, A.; Viallefont, A.; Fauconneau, B.; Rafael, M.; Guillard, O.

2002-01-01

This study compares the efficiency of blood lead level analysis by graphite furnace atomic absorption spectrometry (GFAAS) and the portable LeadCare Blood lead testing system (LCS). Recoveries of two added lead concentrations of 22 and 42 μg/dL ranged from 102.4 to 105.5% for LCS and from 96.3 to 97.2% for GFAAS. Measurement of a certified sample (Certified Danish Whole Blood) at a blood lead concentration of 26.2 μg/dL gave within- and between-run coefficients of variation which were both approximately 8% by LCS and 2% by GFAAS. Comparison of the tested method (LCS) versus GFAAS from analysis of 76 samples of blood lead collected from workers in different industrial sectors showed imperfect overall correlation (r = 0.95). The LCS is quite suitable for screening purposes, but requires the use of non-frozen blood collected less than 24 h before. Conservative threshold values should be applied when using the LCS for initial screening in the field. (orig.)

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

Science.gov (United States)

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

2016-01-15

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

MASS SPECTROMETRY PROTEOMICS METHOD AS A RAPID SCREENING TOOL FOR BACTERIAL CONTAMINATION OF FOOD

Science.gov (United States)

2017-06-01

MASS SPECTROMETRY PROTEOMICS METHOD AS A RAPID SCREENING TOOL FOR BACTERIAL CONTAMINATION OF FOOD ECBC-TR...TITLE AND SUBTITLE Mass Spectrometry Proteomics Method as a Rapid Screening Tool for Bacterial Contamination of Food 5a. CONTRACT NUMBER 5b...the MSPM to correctly classify whether or not food samples were contaminated with Salmonella enterica serotype Newport in this blinded pilot study

Modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction followed by atomic absorption spectrometry for trace determination of zinc in water and food samples

International Nuclear Information System (INIS)

Zeeb, M.; Sadeghi, M.

2011-01-01

We report on a new method for the microextraction and determination of zinc (II). The ion is accumulated via ionic-liquid cold-induced aggregation dispersive liquid-liquid microextraction (IL-CIA-DLLME) followed by flame atomic absorption spectrometry (FAAS). The ionic liquid (IL) 1-hexyl-3-methylimidazolium hexafluorophosphate is dispersed into a heated sample solution containing sodium hexafluorophosphate as a common ion source. The solution is then placed in an ice-water bath upon which a cloudy solution forms due to the decrease of the solubility of the IL. Zinc is complexed with 8-hydroxyquinoline and extracted into the IL. The enriched phase is dissolved in a diluting agent and introduced to the FAAS. The method is not influenced by variations in the ionic strength of the sample solution. Factors affecting the performance were evaluated and optimized. At optimum conditions, the limit of detection is 0.18 μg L -1 , and the relative standard deviation is 3.0% (at n=5). The method was validated by recovery experiments and by analyzing a certified reference material and successfully applied to the determination of Zn (II) in water and food samples. (author)

Introduction of Flame Atomic Absorption Spectrometry (FAAS) For River Water Samples Analysis

International Nuclear Information System (INIS)

Shakirah Abd Shukor; Mohd Suhaimi Hamzah; Shamsiah Abdul Rahman

2015-01-01

Metal contamination in water is a major component in the determination of water quality monitoring. In spite of the viability of several other metal ion analysis techniques for river water, atomic absorption spectroscopy (AAS) method is most commonly used due to the reproducibility results, short analysis time, cost effective, lower level detection and robust. Therefore, this article gives an overview on the principles, instrumentation techniques, sample preparations, instrument calibration and data analysis in a simple manner for beginner. (author)

The advantage of using the henry straight line in {gamma} spectrometry (1963); Interet de l'utilisation de la droite de henry en spectrometrie {gamma} (1963)

Energy Technology Data Exchange (ETDEWEB)

Jockey, [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1963-07-01

The Henry construction is a convenient way to interpret the total absorption peaks in gamma spectrometry by exploiting their statistical significance. It is so possible to determine graphically, and accurately, such values as: - position of the peak - resolution, etc. The main practical applications are considered. (author) [French] La construction de la droite de Henry fournit un moyen commode d'interpreter les pics d'absorption totale en spectrometrie gamma en exploitant leur signification statistique, il est ainsi possible de determiner graphiquement, avec precision, des notions telles que: - position du pic - resolution, etc. Les principales applications pratiques sont envisagees. (auteur)

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

Science.gov (United States)

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

2013-09-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-10-12

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

Passive ranging using a filter-based non-imaging method based on oxygen absorption.

Science.gov (United States)

Yu, Hao; Liu, Bingqi; Yan, Zongqun; Zhang, Yu

2017-10-01

To solve the problem of poor real-time measurement caused by a hyperspectral imaging system and to simplify the design in passive ranging technology based on oxygen absorption spectrum, a filter-based non-imaging ranging method is proposed. In this method, three bandpass filters are used to obtain the source radiation intensities that are located in the oxygen absorption band near 762 nm and the band's left and right non-absorption shoulders, and a photomultiplier tube is used as the non-imaging sensor of the passive ranging system. Range is estimated by comparing the calculated values of band-average transmission due to oxygen absorption, τ O 2 , against the predicted curve of τ O 2 versus range. The method is tested under short-range conditions. Accuracy of 6.5% is achieved with the designed experimental ranging system at the range of 400 m.

Preconcentration of trace amounts of lead in water samples with cetyltrimethylammonium bromide coated magnetite nanoparticles and its determination by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Mohammad Faraji

2016-11-01

Full Text Available A sensitive and simple magnetic solid phase extraction procedure was presented for the preconcentration of lead ions in environmental water samples. In the present study, lead ions form complexes with 1-(2-pyridilazo-2-naphthol reagent (PAN in basic medium, and then are quantitatively extracted to the surface of cetyltrimethylammonium bromide (CTAB-coated magnetite nanoparticles (Fe3O4 NPs. After magnetic separation of adsorbent, the adsorbent was eluted with 0.5% (v/v HCl in methanol prior to its analysis by flame atomic absorption spectrometry (FAAS. The pH of sample, concentrations of PAN, amounts of CTAB and Fe3O4 NPs, sample volume and desorption conditions were optimized. Under optimum conditions, the calibration curve was linear in the range of 0.05–100 ng mL−1 with R2 = 0.9996. Detection and quantification limits of the proposed method were 0.005 and 0.05 ng mL−1, respectively. Enhancement factor of 1050 was achieved using this method to extract 1000 mL of different environmental water samples. Compared with conventional solid phase extraction methods, the advantages of this method still include easy preparation of sorbents, short times of sample pre-treatment, high extraction yield, and high breakthrough volume. It shows great analytical potential in preconcentration of lead from large volume water samples.

Trace-element analysis of uranium ores by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Coetzee, P.P.; De Villiers, W.v Z.

1985-01-01

The determination of seventeen trace elements (As, Ba, Co, Cr, Cu, Mo, Nb, Ni, Pb, Sr, Th, U, V, Y, Zn, and Zr) in uranium ores by x-ray fluorescence spectrometry was investigated. For the elements with analyte lines in the vicinity of the U-L lines, large overlap corrections were necessary and only a few completely interference-free background positions were available. Consequently, the Feather and Willis method was used for determining the background intensity at the peak positions as well as mass absorption coefficients. As a result of the presence of the U-L absorption edges, both primary and secondary mass absorption coefficients had to be used for matrix corrections. Furthermore, it was observed that the background intensity in the region of the uranium lines increased with increasing uranium content of the sample, instead of the expected decrease due to the increasing mass absorption coefficient. This was attributed to the scattering of uranium lines in the spectrometer chamber. A method was developed to correct the measured intensities for this effect. The contribution from the scattering of uranium lines to the measured intensity at the various 20 positions was determined on samples with different uranium concentrations and for which the mass absorption coefficients and concentrations of the various elements were known

Research on 3-D terrain correction methods of airborne gamma-ray spectrometry survey

International Nuclear Information System (INIS)

Liu Yanyang; Liu Qingcheng; Zhang Zhiyong

2008-01-01

The general method of height correction is not effectual in complex terrain during the process of explaining airborne gamma-ray spectrometry data, and the 2-D terrain correction method researched in recent years is just available for correction of section measured. A new method of 3-D sector terrain correction is studied. The ground radiator is divided into many small sector radiators by the method, then the irradiation rate is calculated in certain survey distance, and the total value of all small radiate sources is regarded as the irradiation rate of the ground radiator at certain point of aero- survey, and the correction coefficients of every point are calculated which then applied to correct to airborne gamma-ray spectrometry data. The method can achieve the forward calculation, inversion calculation and terrain correction for airborne gamma-ray spectrometry survey in complex topography by dividing the ground radiator into many small sectors. Other factors are considered such as the un- saturated degree of measure scope, uneven-radiator content on ground, and so on. The results of for- ward model and an example analysis show that the 3-D terrain correction method is proper and effectual. (authors)

Determination of concentration of heavy metals (Pb, Cd, Fe) in animal tissues using atomic absorption spectrometry

International Nuclear Information System (INIS)

RAZAFINTSALAMA, V.T.

2009-01-01

Heavy metals are classified among the inorganic compounds. The latter type of metal is found in rocks, fertilizers, urban mud but may also originate from the atmospheric pollution. A particular characteristic of heavy metals is their bioaccumulation in the food chain. Therefore, lead and cadmium, which are classified as heavy metals may be easily found in animal products and can lead to food poisoning if their concentrations are higher than the maximum permissible values as requested by international agencies such as the c odex alimentarius . The values are set down and differ according to types of food for human consuption and the trading companies take action accordingly. Therefore, it is necessary to set up a quality control system through analytical laboratory measurements and testings. This study underlies the method of determination of lead, cadmium and iron in animal tissues by atomic absorption spectrometry. The results showed that the method is sensitive and reliable. For each analyte, the Z-score lies between -2 and 2, indicating that the method is working properly. The analytical results showed that: (i) only beef and chicken meats and beef liver contain lead [0,09μg.g - 1; 0,29μg.g - 1]. The limit value of 0,1μg.g - 1 is almost reached in beef and chicken meats, (ii) as far as cadmium is concerned, the five studied samples contain this analyte [0,02μg.g - 1; 0,9μg.g - 1]. Except the chicken liver of which the concentration (0,15μg.g - 1) exceeds the maximum permissible value (0,1μg.g - 1), the others are in conformity with the standards and appropriate to be consumed,(iii) iron is higher in the liver and kidney samples: beef liver 282mg.g - 1, chicken liver 250 mg.g - 1, pork kidney 247mg.g - 1. The study also showed that the calcium concentration in animal tissues is low and they can be classified as poor-calcium food. [fr

Determination of calcium, magnesium, sodium, and potassium in foodstuffs by using a microsampling flame atomic absorption spectrometric method after closed-vessel microwave digestion: method validation.

Science.gov (United States)

Chekri, Rachida; Noël, Laurent; Vastel, Christelle; Millour, Sandrine; Kadar, Ali; Guérin, Thierry

2010-01-01

This paper describes a validation process in compliance with the NFIEN ISO/IEC 17025 standard for the determination of the macrominerals calcium, magnesium, sodium, and potassium in foodstuffs by microsampling with flame atomic absorption spectrometry after closed-vessel microwave digestion. The French Standards Commission (Agence Francaise de Normalisation) standards NF V03-110, NF EN V03-115, and XP T-90-210 were used to evaluate this method. The method was validated in the context of an analysis of the 1322 food samples of the second French Total Diet Study (TDS). Several performance criteria (linearity, LOQ, specificity, trueness, precision under repeatability conditions, and intermediate precision reproducibility) were evaluated. Furthermore, the method was monitored by several internal quality controls. The LOQ values obtained (25, 5, 8.3, and 8.3 mg/kg for Ca, Mg, Na, and K, respectively) were in compliance with the needs of the TDS. The method provided accurate results as demonstrated by a repeatability CV (CVr) of < 7% and a reproducibility CV (CVR) of < 12% for all the elements. Therefore, the results indicated that this method could be used in the laboratory for the routine determination of these four elements in foodstuffs with acceptable analytical performance.

A simple source preparation method for alpha-ray spectrometry of volcanic rock sample

International Nuclear Information System (INIS)

Takahashi, Masaomi; Kurihara, Yuichi; Sato, Jun

2006-01-01

A simple source preparation method was developed for the alpha-ray spectrometry to determine U and Th in volcanic rockes. Isolation of U and Th from volcanic rocks was made by use of UTEVA-Spec. resin, extraction chromatograph material. U and Th were extracted by TTA-benzene solution and organic phase was evaporated drop by drop on a hot stainless steel planchet to dryness. This method was found to be effective for the preparation of sources for alpha-ray spectrometry. (author)

A method for determination mass absorption coefficient of gamma rays by Compton scattering.

Science.gov (United States)

El Abd, A

2014-12-01

A method was proposed for determination mass absorption coefficient of gamma rays for compounds, alloys and mixtures. It is based on simulating interaction processes of gamma rays with target elements having atomic numbers from Z=1 to Z=92 using the MCSHAPE software. Intensities of Compton scattered gamma rays at saturation thicknesses and at a scattering angle of 90° were calculated for incident gamma rays of different energies. The obtained results showed that the intensity of Compton scattered gamma rays at saturations and mass absorption coefficients can be described by mathematical formulas. These were used to determine mass absorption coefficients for compound, alloys and mixtures with the knowledge of their Compton scattered intensities. The method was tested by calculating mass absorption coefficients for some compounds, alloys and mixtures. There is a good agreement between obtained results and calculated ones using WinXom software. The advantages and limitations of the method were discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

Science.gov (United States)

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

2016-08-15

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

A general method for targeted quantitative cross-linking mass spectrometry

Science.gov (United States)

Chemical cross-linking mass spectrometry (XL-MS) provides protein structural information by identifying covalently linked proximal amino acid residues on protein surfaces. The information gained by this technique is complementary to other structural biology methods such as x-ray crystallography, NM...

Status of determining transuranic nuclides speciation in aqueous solution with laser spectrometry

International Nuclear Information System (INIS)

Wang Bo; Liu Dejun; Yao Jun; Chen Xi; Long Haoqi; Zeng Jishu; Su Xiguang; Fan Xianhua

2007-01-01

The knowledge about speciation of transuranic nuclides in aqueous solution is a basis for understanding the chemical and migration behavior of transuranic nuclides in aqueous solution. The speciation of transuranic nuclides with trace concentration is complicated in near neutral aqueous solutions, including change of oxidation state, complexation and colloid generation, etc. The concentrations of transuranium in near neutral aqueous solution usually below the sensitivity range of method such as conventional absorption spectroscopy. The radioactive analysis method has a very low detection limits for radionuclides, however, it wouldn' t allow the direct measurement of the transuranic species. In contrast with these methods, laser spectroscopy is an ideal method with high sensitivity, and non-contact and non-destructive for determining the speciation of transuranic nuclides. This paper summarizes the status and application of LIPAS (Laser-induced Photoacoustic Spectrometry), LIBD (Laser-induced Breakdown Detection) and TRLFS (Time-resolved Laser Fluorescence Spectrometry) to determine the speciation of transuranic nuclides with trace concentration in aqueous solutions. (authors)

Determination of lead at trace levels in mussel and sea water samples using vortex assisted dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry.

Science.gov (United States)

Erarpat, Sezin; Özzeybek, Gözde; Chormey, Dotse Selali; Bakırdere, Sezgin

2017-12-01

In this study, dispersive liquid-liquid microextraction (DLLME) and slotted quartz tube (SQT) were coupled to flame atomic absorption spectrometry (FAAS) to increase the sensitivity of lead. Conditions such as the formation of the lead-dithizone complex, efficiency of the DLLME method and the output of the SQT were systematically optimized to improve the detection limit for the analyte. The conventional FAAS system was improved upon by about 3.0 times with SQT-FAAS, 32 times with DLLME-FAAS and 142 times with DLLME-SQT-FAAS. The method was applicable over a wide linear range (10-500 μg L -1 ). The limit of detection (LOD) determined by DLLME-SQT-FAAS for seawater and mussel were 2.7 μg L -1 and 270 μg kg -1 , respectively. The percent recoveries obtained for mussel and seawater samples (spiked at 20 and 50 μg L -1 ) were 95-96% and 98-110%, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

An Accurate Method for Computing the Absorption of Solar Radiation by Water Vapor

Science.gov (United States)

Chou, M. D.

1980-01-01

The method is based upon molecular line parameters and makes use of a far wing scaling approximation and k distribution approach previously applied to the computation of the infrared cooling rate due to water vapor. Taking into account the wave number dependence of the incident solar flux, the solar heating rate is computed for the entire water vapor spectrum and for individual absorption bands. The accuracy of the method is tested against line by line calculations. The method introduces a maximum error of 0.06 C/day. The method has the additional advantage over previous methods in that it can be applied to any portion of the spectral region containing the water vapor bands. The integrated absorptances and line intensities computed from the molecular line parameters were compared with laboratory measurements. The comparison reveals that, among the three different sources, absorptance is the largest for the laboratory measurements.

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)

Lavilla, I.; Mosquera, A.; Millos, J.; Cameselle, J.; Bendicho, C.

2006-01-01

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

Self-absorption corrections for well-type germanium detectors

International Nuclear Information System (INIS)

Appleby, P.G.; Richardson, N.; Nolan, P.J.

1992-01-01

Corrections for self-absorption are of vital importance to accurate determination by gamma spectrometry of radionuclides such as 210 Pb, 241 Am and 234 Th which emit low energy gamma radiation. A simple theoretical model for determining the necessary corrections for well-type germanium detectors is presented. In this model, self-absorption factors are expressed in terms of the mass attenuation coefficient of the sample and a parameter characterising the well geometry. Experimental measurements of self-absorption are used to evaluate the model and to determine a semi-empirical algorithm for improved estimates of the geometrical parameter. (orig.)

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

Directory of Open Access Journals (Sweden)

Harry Budiman

2010-06-01

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

Trace metal analysis of road dust by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Powell, M.J.; Liu, L.; Gnanalingham, N.; Peters, L.

2000-01-01

Dust from roads in an air impingement zone close to anthropogenic sources of air pollutants can be a concern for people living in the immediate vicinity. The Ministry of the Environment (MOE) has conducted a case study to monitor the concentration of uranium, strontium, thorium and arsenic in road dust from one such area. A method for the analysis of road dust by inductively coupled plasma mass spectrometry (ICP-MS) has been developed with detection limits in the ng/1 range. A digestion technique has been developed by conducting experiments using single and combinations of acids in open-vessel wet digestions. Accuracy has been determined by the use of matrix representative certified reference materials (CRMs). Digestion precision was determined by elemental concentration measurements of the most representative CRM through replicates. Spike recovery data were from 95% to 110% for all elements, and inter-method comparison studies between hydride generation atomic absorption spectrometry (AAS) inductively coupled plasma atomic emission spectrometry (ICP-AES) and ICP-MS for arsenic and strontium show good agreement. (author)

New Isotope Analysis Method: Atom Trap Mass Spectrometry

International Nuclear Information System (INIS)

Ko, Kwang Hoon; Park, Hyun Min; Han, Jae Min; Kim, Taek Soo; Cha, Yong Ho; Lim, Gwon; Jeong, Do Young

2011-01-01

Trace isotope analysis has been an important role in science, archaeological dating, geology, biology and nuclear industry. Some fission products such as Sr-90, Cs-135 and Kr-85 can be released to the environment when nuclear accident occurs and the reprocessing factory operates. Thus, the analysis of artificially produced radioactive isotopes has been of interest in nuclear industry. But it is difficult to detect them due to low natural abundance less then 10 -10 . In general, radio-chemical method has been applied to detect ultra-trace radio isotopes. But this method has disadvantages of long measurement time for long lived radioisotopes and toxic chemical process for the purification. The Accelerator Mass Spectrometer has high isotope selectivity, but the system is huge and its selectivity is affected by isobars. The laser based method, such as RIMS (Resonance Ionization Mass Spectrometry) has the advantage of isobar-effect free characteristics. But the system size is still huge for high isotope selective system. Recently, ATTA (Atom Trap Trace Analysis) has been successfully applied to detect ultra-trace isotope, Kr-81 and Kr-85. ATTA is the isobar-effect free detection with high isotope selectivity and the system size is small. However, it requires steady atomic beam source during detection, and is not allowed simultaneous detection of several isotopes. In this presentation, we introduce new isotope detection method which is a coupled method of Atom Trap Mass Spectrometry (ATMS). We expect that it can overcome the disadvantage of ATTA while it has both advantages of ATTA and mass spectrometer. The basic concept and the system design will be presented. In addition, the experimental status of ATMS will also be presented

Direct molecular analysis of whole-body animal tissue sections by MALDI imaging mass spectrometry.

Science.gov (United States)

Reyzer, Michelle L; Chaurand, Pierre; Angel, Peggi M; Caprioli, Richard M

2010-01-01

The determination of the localization of various compounds in a whole animal is valuable for many applications, including pharmaceutical absorption, distribution, metabolism, and excretion (ADME) studies and biomarker discovery. Imaging mass spectrometry is a powerful tool for localizing compounds of biological interest with molecular specificity and relatively high resolution. Utilizing imaging mass spectrometry for whole-body animal sections offers considerable analytical advantages compared to traditional methods, such as whole-body autoradiography, but the experiment is not straightforward. This chapter addresses the advantages and unique challenges that the application of imaging mass spectrometry to whole-body animal sections entails, including discussions of sample preparation, matrix application, signal normalization, and image generation. Lipid and protein images obtained from whole-body tissue sections of mouse pups are presented along with detailed protocols for the experiments.

Study on solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent

International Nuclear Information System (INIS)

Yang Guangyu; Fen Weibo; Lei Chun; Xiao Weilie; Sun Handong

2009-01-01

A solid phase extraction and graphite furnace atomic absorption spectrometry (GFAAS) for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent was studied. Trace amounts of chromium, nickel, silver, cobalt, copper, cadmium and lead were reacted with 2-(2-quinolinil-azo)-4-methyl-1,3-dihydroxidobenzene (QAMDHB) followed by adsorption onto MCI GEL CHP 20Y solid phase extraction column, and 1.0 mol L -1 HNO 3 was used as eluent. The metal ions in 300 mL solution can be concentrated to 1.0 mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0 g of resin were greater than 95% without interference from alkaline, earth alkaline and some metal ions. When detected with graphite furnace atomic absorption spectrometry, the detection limits in the original samples were 1.4 ng L -1 for Cr(III), 1.0 ng L -1 for Ni(II), 0.85 ng L -1 for Ag(I), 1.2 ng L -1 for Co(II), 1.0 ng L -1 for Cu(II), 1.2 ng L -1 for Cd(II) and 1.3 ng L -1 for Pb(II). The validation of the procedure was performed by the analysis of the certified standard reference materials, and the presented procedure was applied to the determination of analytes in biological, water and soil samples with good results (recoveries range from 89 to 104%, and R.S.D.% lower than 3.2%. The results agreed with the standard value or reference method)

Laser absorption spectroscopy - Method for monitoring complex trace gas mixtures

Science.gov (United States)

Green, B. D.; Steinfeld, J. I.

1976-01-01

A frequency stabilized CO2 laser was used for accurate determinations of the absorption coefficients of various gases in the wavelength region from 9 to 11 microns. The gases investigated were representative of the types of contaminants expected to build up in recycled atmospheres. These absorption coefficients were then used in determining the presence and amount of the gases in prepared mixtures. The effect of interferences on the minimum detectable concentration of the gases was measured. The accuracies of various methods of solution were also evaluated.

Mass Spectrometry Coupled Experiments and Protein Structure Modeling Methods

Directory of Open Access Journals (Sweden)

Lee Sael

2013-10-01

Full Text Available With the accumulation of next generation sequencing data, there is increasing interest in the study of intra-species difference in molecular biology, especially in relation to disease analysis. Furthermore, the dynamics of the protein is being identified as a critical factor in its function. Although accuracy of protein structure prediction methods is high, provided there are structural templates, most methods are still insensitive to amino-acid differences at critical points that may change the overall structure. Also, predicted structures are inherently static and do not provide information about structural change over time. It is challenging to address the sensitivity and the dynamics by computational structure predictions alone. However, with the fast development of diverse mass spectrometry coupled experiments, low-resolution but fast and sensitive structural information can be obtained. This information can then be integrated into the structure prediction process to further improve the sensitivity and address the dynamics of the protein structures. For this purpose, this article focuses on reviewing two aspects: the types of mass spectrometry coupled experiments and structural data that are obtainable through those experiments; and the structure prediction methods that can utilize these data as constraints. Also, short review of current efforts in integrating experimental data in the structural modeling is provided.

Direct olive oil analysis by mass spectrometry: A comparison of different ambient ionization methods.

Science.gov (United States)

Lara-Ortega, Felipe J; Beneito-Cambra, Miriam; Robles-Molina, José; García-Reyes, Juan F; Gilbert-López, Bienvenida; Molina-Díaz, Antonio

2018-04-01

Analytical methods based on ambient ionization mass spectrometry (AIMS) combine the classic outstanding performance of mass spectrometry in terms of sensitivity and selectivity along with convenient features related to the lack of sample workup required. In this work, the performance of different mass spectrometry-based methods has been assessed for the direct analyses of virgin olive oil for quality purposes. Two sets of experiments have been setup: (1) direct analysis of untreated olive oil using AIMS methods such as Low-Temperature Plasma Mass Spectrometry (LTP-MS) or paper spray mass spectrometry (PS-MS); or alternatively (2) the use of atmospheric pressure ionization (API) mass spectrometry by direct infusion of a diluted sample through either atmospheric pressure chemical ionization (APCI) or electrospray (ESI) ionization sources. The second strategy involved a minimum sample work-up consisting of a simple olive oil dilution (from 1:10 to 1:1000) with appropriate solvents, which originated critical carry over effects in ESI, making unreliable its use in routine; thus, ESI required the use of a liquid-liquid extraction to shift the measurement towards a specific part of the composition of the edible oil (i.e. polyphenol rich fraction or lipid/fatty acid profile). On the other hand, LTP-MS enabled direct undiluted mass analysis of olive oil. The use of PS-MS provided additional advantages such as an extended ionization coverage/molecular weight range (compared to LTP-MS) and the possibility to increase the ionization efficiency towards nonpolar compounds such as squalene through the formation of Ag + adducts with carbon-carbon double bounds, an attractive feature to discriminate between oils with different degree of unsaturation. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of ultra trace arsenic species in water samples by hydride generation atomic absorption spectrometry after cloud point extraction

Energy Technology Data Exchange (ETDEWEB)

Ulusoy, Halil Ibrahim, E-mail: hiulusoy@yahoo.com [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey); Akcay, Mehmet; Ulusoy, Songuel; Guerkan, Ramazan [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey)

2011-10-10

Graphical abstract: The possible complex formation mechanism for ultra-trace As determination. Highlights: {yields} CPE/HGAAS system for arsenic determination and speciation in real samples has been applied first time until now. {yields} The proposed method has the lowest detection limit when compared with those of similar CPE studies present in literature. {yields} The linear range of the method is highly wide and suitable for its application to real samples. - Abstract: Cloud point extraction (CPE) methodology has successfully been employed for the preconcentration of ultra-trace arsenic species in aqueous samples prior to hydride generation atomic absorption spectrometry (HGAAS). As(III) has formed an ion-pairing complex with Pyronine B in presence of sodium dodecyl sulfate (SDS) at pH 10.0 and extracted into the non-ionic surfactant, polyethylene glycol tert-octylphenyl ether (Triton X-114). After phase separation, the surfactant-rich phase was diluted with 2 mL of 1 M HCl and 0.5 mL of 3.0% (w/v) Antifoam A. Under the optimized conditions, a preconcentration factor of 60 and a detection limit of 0.008 {mu}g L{sup -1} with a correlation coefficient of 0.9918 was obtained with a calibration curve in the range of 0.03-4.00 {mu}g L{sup -1}. The proposed preconcentration procedure was successfully applied to the determination of As(III) ions in certified standard water samples (TMDA-53.3 and NIST 1643e, a low level fortified standard for trace elements) and some real samples including natural drinking water and tap water samples.

Cell-patterned glass spray for direct drug assay using mass spectrometry

International Nuclear Information System (INIS)

Wu, Jing; Wang, Shiqi; Chen, Qiushui; Jiang, Hao; Liang, Shuping; Lin, Jin-Ming

2015-01-01

In this work, the establishment of a glass spray mass spectrometry (GS-MS) platform for direct cell-based drug assay was described. Cell co-culture, drug-induced cell apoptosis, proliferation analysis and intracellular drug absorption measurement were performed simultaneously on this specifically designed platform. Two groups of co-cultured cells (NIH-3T3/HepG2 and HepG2/MCF-7) were cultivated and they showed high viability within 3 days. The biocompatibility of the platform facilitated the subsequent bioassays, in which, cyclophosphamide (CPA) and genistein were used as the model drugs. The distinctions of cell apoptosis and proliferation between the mono-cultured and co-cultured cells were clearly observed and well explained by in situ GS-MS measurements. A satisfactory linearity of the calibration curve between the relative MS intensity and CPA concentrations was obtained using stable isotope labeling method (y = 0.16545 + 0.0985x, R"2 = 0.9937). The variations in the quantity of absorbed drug were detected and the results were consistent with the concentration-dependence of cell apoptosis. All the results demonstrated that direct cell-based drug assay could be performed on the stable isotope labeling assisted GS-MS platform in a facile and quantitative manner. - Highlights: • A versatile glass spray mass spectrometry (GS-MS) platform for direct cell-based drug assay was developed in this paper. • It has characteristics of the atmospheric pressure ionization method. • It is multifunctional for cell co-culture, bioassays, qualitative and quantitative intracellular drug absorption measurement. • GS-MS has the potential to increase the use of mass spectrometry in biological analysis.

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

Science.gov (United States)

Viets, J.G.

1978-01-01

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

Efficient methods for time-absorption (α) eigenvalue calculations

International Nuclear Information System (INIS)

Hill, T.R.

1983-01-01

The time-absorption eigenvalue (α) calculation is one of the options found in most discrete-ordinates transport codes. Several methods have been developed at Los Alamos to improve the efficiency of this calculation. Two procedures, based on coarse-mesh rebalance, to accelerate the α eigenvalue search are derived. A hybrid scheme to automatically choose the more-effective rebalance method is described. The α rebalance scheme permits some simple modifications to the iteration strategy that eliminates many unnecessary calculations required in the standard search procedure. For several fast supercritical test problems, these methods resulted in convergence with one-fifth the number of iterations required for the conventional eigenvalue search procedure

On-line micro-volume introduction system developed for lower density than water extraction solvent and dispersive liquid–liquid microextraction coupled with flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Anthemidis, Aristidis N.; Mitani, Constantina; Balkatzopoulou, Paschalia; Tzanavaras, Paraskevas D.

2012-01-01

Highlights: ► A dispersive liquid–liquid micro extraction method for lead and copper determination. ► A micro-volume transportation system for extractant solvent lighter than water. ► Analysis of natural water samples. - Abstract: A simple and fast preconcentration/separation dispersive liquid–liquid micro extraction (DLLME) method for metal determination based on the use of extraction solvent with lower density than water has been developed. For this purpose a novel micro-volume introduction system was developed enabling the on-line injection of the organic solvent into flame atomic absorption spectrometry (FAAS). The effectiveness and efficiency of the proposed system were demonstrated for lead and copper preconcentration in environmental water samples using di-isobutyl ketone (DBIK) as extraction solvent. Under the optimum conditions the enhancement factor for lead and copper was 187 and 310 respectively. For a sample volume of 10 mL, the detection limit (3 s) and the relative standard deviation were 1.2 μg L −1 and 3.3% for lead and 0.12 μg L −1 and 2.9% for copper respectively. The developed method was evaluated by analyzing certified reference material and it was applied successfully to the analysis of environmental water samples.

Demonstration of a collimated in situ method for determining depth distributions using gamma-ray spectrometry

CERN Document Server

Benke, R R

2002-01-01

In situ gamma-ray spectrometry uses a portable detector to quantify radionuclides in materials. The main shortcoming of in situ gamma-ray spectrometry has been its inability to determine radionuclide depth distributions. Novel collimator designs were paired with a commercial in situ gamma-ray spectrometry system to overcome this limitation for large area sources. Positioned with their axes normal to the material surface, the cylindrically symmetric collimators limited the detection of un attenuated gamma-rays from a selected range of polar angles (measured off the detector axis). Although this approach does not alleviate the need for some knowledge of the gamma-ray attenuation characteristics of the materials being measured, the collimation method presented in this paper represents an absolute method that determines the depth distribution as a histogram, while other in situ methods require a priori knowledge of the depth distribution shape. Other advantages over previous in situ methods are that this method d...

Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

International Nuclear Information System (INIS)

Pena, Francisco; Lavilla, Isela; Bendicho, Carlos

2008-01-01

Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Pena, Francisco; Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain)], E-mail: bendicho@uvigo.es

2008-04-15

Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 {mu}g/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters.

The metabolism and gastrointestinal absorption of neptunium and protactinium in adult baboons

International Nuclear Information System (INIS)

Ralston, L.G.; Cohen, N.; Bhattacharyya, H.; Larsen, R.P.; Ayres, L.; Oldham, R.D.; Moretti, E.S.

1985-01-01

The metabolism of neptunium and protactinium was studied in adult female baboons following intravenous injection and intragastric intubation. Neptunium-239, Np-237, and Pa-233 were prepared as either citrate-buffer, nitrate, or bicarbonate solutions with oxidation states of (V) and (VI). Samples of blood, urine, feces and autopsy tissues were measured by gamma spectrometry. Retention of neptunium and protactinium was determined in vivo using whole and partial body gamma-scintillation spectrometry with [NaI-CsI(T1)] detectors. Fed and fasted baboons were administered solutions of Np(VI) bicarbonate (10/sup -8/ to 10/sup -1/ mg/kg) and Pa(V) citrate-buffer (10/sup -9/ mg/kg) by gavage. The gastrointestinal absorption value for neptunium in two fasted baboons, sacrificed at 1 day post administration, was determined to be 0.92 +- 0.04%. Of the total amount of neptunium absorbed, 52 +- 3% was retained in bone, 6 + 2% was in liver, and 42 +- 0.1% was excreted in urine. The metabolism of neptunium followed oral and iv administrations was found to be similar. This observation was also true for baboons which had received oral and iv doses of protactinium. A method was developed to estimate GI absorption values for both nuclides in baboons, which were not sacrificed, by comparison of activities present in bioassay samples after injection and gavage. Absorption values calculated by this method for neptunium and protactinium in fasted baboons were 1.8 +- 0.8% and 0.65 +- 0.01%, respectively. Values for fed animals were 1 to 2 orders of magnitude less than those for fasted animals. Further experiments are currently underway to evaluate this assay technique

A standards-based method for compositional analysis by energy dispersive X-ray spectrometry using multivariate statistical analysis: application to multicomponent alloys.

Science.gov (United States)

Rathi, Monika; Ahrenkiel, S P; Carapella, J J; Wanlass, M W

2013-02-01

Given an unknown multicomponent alloy, and a set of standard compounds or alloys of known composition, can one improve upon popular standards-based methods for energy dispersive X-ray (EDX) spectrometry to quantify the elemental composition of the unknown specimen? A method is presented here for determining elemental composition of alloys using transmission electron microscopy-based EDX with appropriate standards. The method begins with a discrete set of related reference standards of known composition, applies multivariate statistical analysis to those spectra, and evaluates the compositions with a linear matrix algebra method to relate the spectra to elemental composition. By using associated standards, only limited assumptions about the physical origins of the EDX spectra are needed. Spectral absorption corrections can be performed by providing an estimate of the foil thickness of one or more reference standards. The technique was applied to III-V multicomponent alloy thin films: composition and foil thickness were determined for various III-V alloys. The results were then validated by comparing with X-ray diffraction and photoluminescence analysis, demonstrating accuracy of approximately 1% in atomic fraction.

SELF-ABSORPTION CORRECTIONS BASED ON MONTE CARLO SIMULATIONS

Directory of Open Access Journals (Sweden)

Kamila Johnová

2016-12-01

Full Text Available The main aim of this article is to demonstrate how Monte Carlo simulations are implemented in our gamma spectrometry laboratory at the Department of Dosimetry and Application of Ionizing Radiation in order to calculate the self-absorption within the samples. A model of real HPGe detector created for MCNP simulations is presented in this paper. All of the possible parameters, which may influence the self-absorption, are at first discussed theoretically and lately described using the calculated results.

A novel fiber-packed column for on-line preconcentration and speciation analysis of chromium in drinking water with flame atomic absorption spectrometry.

Science.gov (United States)

Monasterio, Romina P; Altamirano, Jorgelina C; Martínez, Luis D; Wuilloud, Rodolfo G

2009-02-15

A novel on-line preconcentration and determination system based on a fiber-packed column was developed for speciation analysis of Cr in drinking water samples prior to its determination by flame atomic absorption spectrometry (FAAS). All variables involved in the development of the preconcentration method including, pH, eluent type, sample and eluent flow rates, interfering effects, etc., were studied in order to achieve the best analytical performance. A preconcentration factor of 32 was obtained for Cr(VI) and Cr(III). The levels of Cr(III) species were calculated by difference of total Cr and Cr(VI) levels. Total Cr was determined after oxidation of Cr(III) to Cr(VI) with hydrogen peroxide. The calibration graph was linear with a correlation coefficient of 0.999 at levels near the detection limit and up to at least 50 microg L(-1). The relative standard deviation (R.S.D.) was 4.3% (C=5 microg L(-1) Cr(VI), n=10, sample volume=25 mL). The limit of detection (LOD) for both Cr(III) and Cr(VI) species was 0.3 microg L(-1). Verification of the accuracy was carried out by the analysis of a standard reference material (NIST SRM 1643e "Trace elements in natural water"). The method was successfully applied to the determination of Cr(III) and Cr(VI) species in drinking water samples.

Thermodynamic analysis of absorption refrigeration cycles using the second law of thermodynamics method

Energy Technology Data Exchange (ETDEWEB)

Aphornratana, S; Eames, I W [Sheffield Univ. (United Kingdom). Dept. of Mechanical and Process Engineering

1995-05-01

The paper provides an easy to follow description of the second law (of thermodynamics) method as applied to a single-effect absorption refrigerator cycle. Results are presented in a novel graphical format, which aids insight and understanding of those factors that most affect the performance of absorption refrigerators, and which in turn provides strong indicators for the direction of future research. A novel method of calculating the entropy of lithium bromide solutions is offered. (author)

Cloud point extraction-flame atomic absorption spectrometry for pre-concentration and determination of trace amounts of silver ions in water samples.

Science.gov (United States)

Yang, Xiupei; Jia, Zhihui; Yang, Xiaocui; Li, Gu; Liao, Xiangjun

2017-03-01

A cloud point extraction (CPE) method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS) The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I)/diethyldithiocarbamate (DDTC) complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I)/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL -1 Ag + in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL -1 for both Zn 2+ and Cu 2+ , 80 μg·mL -1 for Pb 2+ , 1000 μg·mL -1 for Mn 2+ , and 100 μg·mL -1 for both Cd 2+ and Ni 2+ . The calibration curve was linear in the range of 1-500 ng·mL -1 with a limit of detection (LOD) at 0.3 ng·mL -1 . The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.

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

Science.gov (United States)

Martinis, Estefanía M; Bertón, Paula; Olsina, Roberto A; Altamirano, Jorgelina C; Wuilloud, Rodolfo G

2009-08-15

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

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

International Nuclear Information System (INIS)

Martinis, Estefania M.; Berton, Paula; Olsina, Roberto A.; Altamirano, Jorgelina C.; Wuilloud, Rodolfo G.

2009-01-01

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

Methods for recalibration of mass spectrometry data

Science.gov (United States)

Tolmachev, Aleksey V [Richland, WA; Smith, Richard D [Richland, WA

2009-03-03

Disclosed are methods for recalibrating mass spectrometry data that provide improvement in both mass accuracy and precision by adjusting for experimental variance in parameters that have a substantial impact on mass measurement accuracy. Optimal coefficients are determined using correlated pairs of mass values compiled by matching sets of measured and putative mass values that minimize overall effective mass error and mass error spread. Coefficients are subsequently used to correct mass values for peaks detected in the measured dataset, providing recalibration thereof. Sub-ppm mass measurement accuracy has been demonstrated on a complex fungal proteome after recalibration, providing improved confidence for peptide identifications.

Determination of iron absorption and excretion by whole-body counting; Determination de l'absorption et de l'excretion du fer par la methode de comptage global humain

Energy Technology Data Exchange (ETDEWEB)

Hollard, D; Benabid, Y; Berard, M; Bonnin, J; Darnault, J; Millet, M [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

1969-07-01

Using a whole-body counter, the authors have studied {sup 59}Fe absorption and loss in 8 normal subjects and in 30 iron deficient patients. Results showed that whole-body counting provided an excellent and simple method for iron retention measurements, obviating many inaccuracies of previous technic. Normal absorption of radio iron with this procedure has ranged from 9 per cent to 20 per cent of the administered tracer in normal subjects, with a mean of 15 per cent. A significant increase in {sup 59}Fe absorption was noted in 21 iron-deficient patients in whom the retention ranged from 40 to 100 per cent. However, 3 iron-deficient patients were found to have low absorption, and their severe iron deficiency could be correlated with this defect in absorption. This method permits also the determination of the rate of iron excretion during the following months and therefore the study of the mechanism of some pathological loss. (authors) [French] L'utilisation de la methode de comptage humain global a permis aux auteurs d'etudier l'absorption et l'excretion du fer-59 chez 8 sujets temoins et 30 sujets hyposideremiques. Les resultats montrent que cette technique simple et directe offre de nombreux avantages sur les methodes employees jusqu'a maintenant pour cette determination. La valeur normale de l'absorption du fer chez les temoins est d'environ 15 pour cent de la dose ingeree. Ce chiffre est tres fortement augmente chez 21 sujets hyposideremiques, pouvant atteindre 100 pour cent de la dose ingeree. Par contre, pour 3 malades, cette absorption est si faible qu'elle suggere une carence par defaut d'absorption. Cette methode permet egalement de suivre l'excretion du fer au cours des mois qui suivent l'examen et de determiner le mecanisme de fuites anormales. (auteurs)

Computational methods for protein identification from mass spectrometry data.

Directory of Open Access Journals (Sweden)

Leo McHugh

2008-02-01

Full Text Available Protein identification using mass spectrometry is an indispensable computational tool in the life sciences. A dramatic increase in the use of proteomic strategies to understand the biology of living systems generates an ongoing need for more effective, efficient, and accurate computational methods for protein identification. A wide range of computational methods, each with various implementations, are available to complement different proteomic approaches. A solid knowledge of the range of algorithms available and, more critically, the accuracy and effectiveness of these techniques is essential to ensure as many of the proteins as possible, within any particular experiment, are correctly identified. Here, we undertake a systematic review of the currently available methods and algorithms for interpreting, managing, and analyzing biological data associated with protein identification. We summarize the advances in computational solutions as they have responded to corresponding advances in mass spectrometry hardware. The evolution of scoring algorithms and metrics for automated protein identification are also discussed with a focus on the relative performance of different techniques. We also consider the relative advantages and limitations of different techniques in particular biological contexts. Finally, we present our perspective on future developments in the area of computational protein identification by considering the most recent literature on new and promising approaches to the problem as well as identifying areas yet to be explored and the potential application of methods from other areas of computational biology.

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

International Nuclear Information System (INIS)

Mendil, Durali; Uluoezlue, Ozguer Dogan; Tuezen, Mustafa; Soylak, Mustafa

2009-01-01

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

Study on the application of electrothermal atomization atomic absorption spectrometry for the determination of metallic Cu, Pb, Zn, Cd traces in sea water samples

International Nuclear Information System (INIS)

Nguyen Thi Kim Dung; Doan Thanh Son; Tran Thi Ngoc Diep

2004-01-01

The trace amount of some heavy metallic elements (Cu, Zn, Pb, Cd) in sea water samples were determined directly (without separation) and quantitatively by using Electro-Thermal Atomization Atomic Absorption Spectrometry (ETA-AAS). The effect of mainly major constituents such as Na, Mg, Ca, K, and the mutual effect of the trace elements, which were present in the matrix on the absorption intensity of each analyzed element was studied. The adding of a certain chemical modification for each trace element was also investigated in order to eliminate the overall effect of the background during the pyrolysis and atomization. The sea water sample after fitrating through a membrane with 0.45 μm-hole size was injected in to the graphite tube via an autosampler (MPE50). 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 graphite furnace such as dry temperature, pyrolysis temperature, atomization temperature, 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)

A simple optimized microwave digestion method for multielement monitoring in mussel samples

International Nuclear Information System (INIS)

Saavedra, Y.; Gonzalez, A.; Fernandez, P.; Blanco, J.

2004-01-01

With the aim of obtaining a set of common decomposition conditions allowing the determination of several metals in mussel tissue (Hg by cold vapour atomic absorption spectrometry; Cu and Zn by flame atomic absorption spectrometry; and Cd, PbCr, Ni, As and Ag by electrothermal atomic absorption spectrometry), a factorial experiment was carried out using as factors the sample weight, digestion time and acid addition. It was found that the optimal conditions were 0.5 g of freeze-dried and triturated samples with 6 ml of nitric acid and subjected to microwave heating for 20 min at 180 psi. This pre-treatment, using only one step and one oxidative reagent, was suitable to determine the nine metals studied with no subsequent handling of the digest. It was possible to carry out the determination of atomic absorption using calibrations with aqueous standards and matrix modifiers for cadmium, lead, chromium, arsenic and silver. The accuracy of the procedure was checked using oyster tissue (SRM 1566b) and mussel tissue (CRM 278R) certified reference materials. The method is now used routinely to monitor these metals in wild and cultivated mussels, and found to be good

Trends in tungsten coil atomic spectrometry