WorldWideScience

Sample records for analytical atomic spectrometry

  1. Theory of analytical curves in atomic fluorescence flame spectrometry

    NARCIS (Netherlands)

    Hooymayers, H.P.

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

  2. Development of gas-phase sample-introduction techniques for analytical atomic spectrometry.

    Science.gov (United States)

    Nakahara, Taketoshi

    2005-05-01

    For the last 30 years, several types of gas-phase sample-introduction methods in analytical atomic spectrometry, i.e., atomic absorption spectrometry (AAS), atomic emission spectrometry (AES) and atomic fluorescence spectrometry (AFS), have been investigated and developed in the author's laboratory. Their fundamental results are summarized in this review article. The gas-phase sample-introduction techniques developed in the author's laboratory can be roughly divided into four groups: i) hydride generation, ii) cold-vapor generation of mercury, iii) analyte volatilization reactions and iv) miscellaneous. The analytical figures of merit of the gas-phase sample-introduction methods have been described in detail. Hydride generation has been coupled with the AAS of As, Bi, Ge, Pb, Sb, Se, Sn and Te, with the inductively coupled plasma (ICP) AES of As, Bi, Sn, Se and Sb, with the high-power nitrogen microwave-induced plasma (N2-MIP) AES of As, Bi, Pb, Sb, Se, Sn and Te by their single- and multi-element determinations, with the AFS of As, Bi, Pb, Sb, Se, Sn and Te, and with the ICP mass spectrometry (MS) of As and Se. The cold-vapor generation method for Hg has been combined with atmospheric-pressure helium microwave-induced plasma (He- or Ar-MIP)-AES and AFS. Furthermore, analyte volatilization reactions have been employed in the ICP-AES of iodine, in the He-MIP-AES of iodine bromine, chlorine, sulfur and carbon, and in the ICP-MS of sulfur. As a result, when compared with conventional solution nebulization, a great improvement in the sensitivity has been attained in each instance. In addition, the developed techniques coupled with analytical atomic spectrometry have been successfully applied to the determination of trace elements in a variety of practical samples.

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

    International Nuclear Information System (INIS)

    Montaser, A.

    1993-01-01

    In this research, new high-temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. During the period January 1993--December 1993, emphasis was placed on (a) analytical investigations of atmospheric-pressure helium inductively coupled plasma (He ICP) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies; (b) simulation and computer modeling of plasma sources to predict their structure and fundamental and analytical properties without incurring the enormous cost of experimental studies; (c) spectrosopic imaging and diagnostic studies of high-temperature plasmas; (d) fundamental studies of He ICP discharges and argon-nitrogen plasma by high-resolution Fourier transform spectrometry; and (e) fundamental and analytical investigation of new, low-cost devices as sample introduction systems for atomic spectrometry and examination of new diagnostic techniques for probing aerosols. Only the most important achievements are included in this report to illustrate progress and obstacles. Detailed descriptions of the authors' investigations are outlined in the reprints and preprints that accompany this report. The technical progress expected next year is briefly described at the end of this report

  4. Atomic mass spectrometry

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1997-01-01

    The elemental inorganic analysis seems to be dominated today by techniques based on atomic spectrometry. After an evaluation of advantages and limitations of using mass analysers (ion detectors) versus conventional photomultipliers (photon detector) a brief review of the more popular techniques of the emerging Atomic Mass spectrometry is carried out. Their huge potential for inorganic trace analysis is such that in the future we could well witness how this end of the century and millennium marked the fall of the photons empire in Analytical Atomic Spectrometry. (Author)

  5. Comparison of 4 analytical techniques based on atomic spectrometry for the determination of total tin in canned foodstuffs

    OpenAIRE

    2011-01-01

    Abstract Different techniques for the determination of total tin in beverage and canned food by atomic spectrometry were compared. The performance characteristics of Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry (HG-ICP-AES), Electrothermal Atomization Atomic Absorption Spectrometry (ETA-AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) were determined in term of linearity, ...

  6. Flame emission, atomic absorption and fluorescence spectrometry

    International Nuclear Information System (INIS)

    Horlick, G.

    1980-01-01

    Six hundred and thirty references are cited in this review. The information in the review is divided into 12 major areas: books, reviews, and bibliographies; fundamental studies in flames; developments in instrumentation; measurement techniques and procedure; flame emission spectrometry; flame atomic absorption spectrometry; flame molecular absorption spectrometry; electrothermal atomization atomic absorption spectroscopy; hydride generation techniques; graphite furnace atomic emission spectrometry; atomic fluorescence spectrometry; and analytical comparisons

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Nielsen, Steffen

    1998-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-11-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  10. Trace determination of antimony by hydride generation atomic absorption spectrometry with analyte preconcentration/atomization in a dielectric barrier discharge atomizer

    Czech Academy of Sciences Publication Activity Database

    Zurynková, Pavla; Dědina, Jiří; Kratzer, Jan

    2018-01-01

    Roč. 1010, JUN (2018), s. 11-19 ISSN 0003-2670 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * Stibane * atomization and preconcentration Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 4.950, year: 2016

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

    Science.gov (United States)

    Horlick, Gary

    1984-01-01

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

  12. 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

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Nielsen, Steffen

    1998-01-01

    One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atomic...... for reproducible sample presentation to the AAS instrument, as a means for facilitating conversion techniques for determination of anions, for allowing on-line preconcentration procedures via incorporated column reactors or via (co)precipitation, for exploiting kinetic discrimination schemes in hydride generation...

  14. Trace determination of antimony by hydride generation atomic absorption spectrometry with analyte preconcentration/atomization in a dielectric barrier discharge atomizer.

    Science.gov (United States)

    Zurynková, Pavla; Dědina, Jiří; Kratzer, Jan

    2018-06-20

    Atomization conditions for antimony hydride in the plasma atomizer based on a dielectric barrier discharge (DBD) with atomic absorption spectrometric detection were optimized. Argon was found as the best discharge gas under a flow rate of 50 mL min - 1 while the DBD power was optimum at 30 W. Analytical figures of merit including interference study of As, Se and Bi have been subsequently investigated and the results compared to those found in an externally heated quartz tube atomizer (QTA). The limit of detection (LOD) reached in DBD (0.15 ng mL -1  Sb) is comparable to that observed in QTA (0.14 ng mL -1  Sb). Finally, possibility of Sb preconcentration by stibane in situ trapping in a DBD atomizer was studied. For trapping time of 300 s, the preconcentration efficiency and LOD, respectively, were 103 ± 2% and 0.02 ng mL -1 . Copyright © 2018 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2012-01-01

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

  16. 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

  17. 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.

  18. Analyte enrichment and matrix removal in flow injection analysis-inductively coupled plasma-atomic emission spectrometry: determination of phosphorus in steels

    Science.gov (United States)

    McLeod, C. W.; Cook, I. G.; Worsfold, P. J.; Davies, J. E.; Queay, J.

    A flow injection analysis (FIA) system incorporating a microcolumn of activated alumina has been devised for performing rapid analyte enrichment/matrix removal in inductively coupled plasma-atomic emission spectrometry (ICP-AES). The activated alumina has a high affinity for phosphate ions and the FIA system was tested for the determination of trace P in synthetic aqueous solutions utilizing the PI 213.62 nm line. Phosphate deposition and elution were dependent on sample acidity, column length and the nature and concentration of eluent. Linear calibration was established over the range 0-50 μgP ml -1 and the relative standard deviation was 1.6% at 20 μgP ml -1. The limit of detection was 0.6 μgP ml -1 without analyte enrichment. Application to the analysis of a standard steel (BCS 408) was demonstrated.

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

    Science.gov (United States)

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

    1984-01-01

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

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

    Science.gov (United States)

    Axner, Ove; Ehlers, Patrick; Hausmaninger, Thomas; Silander, Isak; Ma, Weiguang

    2014-10-01

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

  1. Development of an analytical model for the determination of 60Co in aqueous samples by atomic absorption and gamma spectrometry techniques

    International Nuclear Information System (INIS)

    Solis A, N. A.

    2015-01-01

    The applications of the nuclear energy in industry and medicine generate radioactive wastes that must be isolated and confined in order to limit its spread in the biosphere. These types of wastes are generated in hospitals, industry, research centers and nuclear power plants (during de fuel cycle). The radioactive elements (radionuclides) cannot be destroyed by any known method, either chemical or mechanical. Its final destruction is produced by radioactive decay, which makes them stable isotopes, or nuclear transmutation being bombarded with atomic particles. Consequently, the radioactive waste management is to control the radioactive discharges and reduce to tolerable limits, eliminating of effluents and wastes the radionuclides of interest, concentrating them so they can be stored or evacuated so that later not appear in dangerous concentration in the biosphere. In Mexico, the main generators of radioactive wastes are the nuclear power plant of Laguna Verde in Veracruz, Hospitals of the public and private sector, in addition Instituto Nacional de Investigaciones Nucleares (ININ) some institutes and facilities of the UNAM and Instituto Politecnico Nacional (IPN) and industries among others. The aqueous radioactive wastes, particularly those from the nuclear power plants contain traces of cobalt-60. Currently there is no model or analytical technique for the separation of this radionuclide, so it became necessary to develop an analytical model for separation and facilitate their disposal. In this paper was shown that atomic absorption and gamma spectrometry techniques can separate the active concentration of the inactive, which is important because the total concentration can be associated through direct relationships with the wear of metal parts of the nuclear reactor, since the metal alloys of the same reactor containing a fraction of cobalt. Also this analytical and mathematical model that can be reproducible and applicable to full sets of samples and that this

  2. Automatic gamma spectrometry analytical apparatus

    International Nuclear Information System (INIS)

    Lamargot, J.-P.; Wanin, Maurice.

    1980-01-01

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

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

    International Nuclear Information System (INIS)

    Nam, Sang-Ho; Kim, Jae-Jin; Chung, Yong-Sam; Kim, Sun-Ha

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-05-15

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

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

    Science.gov (United States)

    Frentiu, Tiberiu; Ponta, Michaela; Hategan, Raluca

    2013-03-01

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

  6. Economical Alternatives for High Sensitivity in Atomic Spectrometry Laboratory

    Directory of Open Access Journals (Sweden)

    O. Yavuz Ataman

    2007-12-01

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

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

    Czech Academy of Sciences Publication Activity Database

    Dočekal, Bohumil; Vojtková, B.

    2007-01-01

    Roč. 62, č. 3 (2007), s. 304-308 ISSN 0584-8547. [European Furnace Symposium on Atomic Absorption Spectrometry, Electrothermal Vaporization and Atomization /7./ and Solid Sampling Colloquium with Atomic Spectrometry /12./. St. Petersburg, 02.07.2006-07.07.2006] Institutional research plan: CEZ:AV0Z40310501 Keywords : direct solid sampling * electrothermal atomic absorption spectrometry * trace element analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.957, year: 2007

  8. Analytical aspects of hydrogen exchange mass spectrometry

    Science.gov (United States)

    Engen, John R.; Wales, Thomas E.

    2016-01-01

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

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

    International Nuclear Information System (INIS)

    Gaskell, S.J.

    1990-01-01

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

  10. A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    M. Carmen Yebra

    2012-01-01

    Full Text Available A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6% and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee and pharmaceutical preparations (multivitamin tablets. The ranges of concentrations found were 21.4–25.61 μg g-1 for iron, 5.74–18.30 μg g-1 for manganese, and 33.27–57.90 μg g-1 for zinc in soluble solid food samples and 3.75–9.90 μg g-1 for iron, 0.47–5.05 μg g-1 for manganese, and 1.55–15.12 μg g-1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors.

  11. A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Yebra, M. Carmen

    2012-01-01

    A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6%) and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4–25.61 μg g−1 for iron, 5.74–18.30 μg g−1 for manganese, and 33.27–57.90 μg g−1 for zinc in soluble solid food samples and 3.75–9.90 μg g−1 for iron, 0.47–5.05 μg g−1 for manganese, and 1.55–15.12 μg g−1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors. PMID:22567553

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Despite their excellent analytical chemical capacities, Electrothermal Atomic Absorption Spectrometry (ETAAS) and Inductively Coupled Plasma Mass Spectrometry (ICPMS), nevertheless, often require suitable pretreatment of the sample material in order to obtain the necessary sensitivity...

  13. 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

  14. 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

  15. In-situ trapping of bismuthine in externally heated quartz tube atomizers for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Kratzer, Jan; Dědina, Jiří

    2006-01-01

    Roč. 21, č. 2 (2006), s. 208-210 ISSN 0267-9477 R&D Projects: GA AV ČR IAA400310507 Institutional research plan: CEZ:AV0Z40310501 Keywords : bismuth ine preconcentration * quartz surface * hydride generation atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.630, year: 2006

  16. 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

  17. Some advances in inorganic analytical mass spectrometry

    International Nuclear Information System (INIS)

    Svec, H.J.

    1984-01-01

    Three recent developments in mass spectrometry are applicable to analytical problems. High powered laser excitation of metals, semi-conductors, and insulators combined with mass analysis provides an absolute analytical probe. Combining an inductively coupled argon plasma with mass analysis provides facile and sensitive analysis of aqueous solutions. A cryogenic hollow cathode containing ice is a proven ion source for 20 to 50 μL of aqueous samples with prior treatment. 21 refs., 12 figs., 3 tabs

  18. 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

  19. New developments in thermospray sample introduction for atomic spectrometry

    Science.gov (United States)

    Conver, Timothy Shawn; Yang, Jinfu; Koropchak, John A.

    1997-07-01

    The status of thermospray sample introduction for analytical atomic spectrometry was last reviewed in 1992. In this review, we summarize developments in this field since that time, including investigations of aerosol generation processes, noise diagnosis and control with inductively coupled plasma-atomic emission or mass spectrometry (ICP-AES/MS), high flow thermospray, the use of dual-stage desolvation systems based on membrane dryers, and the utilization of thermospray with axially viewed ICP-AES. Since a major advantage of methods based on thermospray is improved limits of detection, the emphasis for applications of thermospray with ICP spectrometries remains focused on environmental sample types, particularly with ICP-MS. Relatedly, the use of thermospray as a means for the direct speciation of Se is also under development.

  20. Optimization of Flame Atomic Absorption Spectrometry for ...

    African Journals Online (AJOL)

    Optimization of Flame Atomic Absorption Spectrometry for Measurement of High Concentrations of Arsenic and Selenium. ... This procedure allowed a rapid determination of As from minimum 4.462 mg/L to higher concentrations without sample pretreatment. Besides As, this method successfully measured Se concentrations ...

  1. Atomic mass spectrometry of materials

    Science.gov (United States)

    Anthony, J. M.; Matteson, S.; Duggan, J. L.; Elliott, P.; Marble, D.; McDaniel, F. D.; Weathers, D.

    1990-12-01

    Texas Instruments and the University of North Texas (UNT) are collaborating on the design of an accelerator mass spectrometry (AMS) system dedicated primarily to the analysis of impurities in electronic materials and metals. An AMS beamline consisting of high-resolution magnetic ( {M}/{dM } > 350) and electrostatic ( {E}/{dE } > 700) analysis followed by a surface barrier detector has been installed on the NEC 9SDH pelletron at UNT, and a "clean" ion source is under development. An existing ion source (NEC Cs sputter source) has been used in conjunction with the AMS beamline to generate computer controlled molecule-free mass analyses of solid samples. Through a careful choice of isotopes and charge states a robust algorithm can be developed for removing molecular interferences from the mass analysis for essentially all materials. Examples using graphite, Si and CdZnTe are discussed.

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

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2001-07-01

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

  3. 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

  4. The relation of double peaks, observed in quartz hydride atomizers, to the fate of free atoms in the determination of arsenic and selenium by atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    D'Ulivo, A.; Dědina, Jiří

    2002-01-01

    Roč. 57, č. 12 (2002), s. 2069-2079 ISSN 0584-8547 R&D Projects: GA ČR GA203/01/0453 Institutional research plan: CEZ:AV0Z4031919 Keywords : hydride atomization * hydride generation * atomic absortion spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.695, year: 2002

  5. Determination of cadmium in aluminium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

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

    1978-12-01

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

  6. Atomic spectrometry update : a review of advances in environmental analysis

    OpenAIRE

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

    2016-01-01

    This is the 31st annual review of the application of atomic spectrometry to the chemical analysis of environmental samples. This update refers to papers published approximately between August 2014 and July 2015 and continues the series of Atomic Spectrometry Updates (ASUs) in Environmental Analysis that should be read in conjunction with other related ASUs in the series, namely: clinical and biological materials, foods and beverages; advances in atomic spectrometry and related techniques; ele...

  7. Direct Determination of Nonmetals in Solution with Atomic Spectrometry.

    Science.gov (United States)

    McGregor, David A.; And Others

    1988-01-01

    Addresses solution nonmetal determinations on a fundamental level. Characterizes research in this area of chemical instrumentation. Discusses the fundamental limitations of nonmetal atomic spectrometry, the status of nonmetals and atomic spectroscopic techniques, and current directions in solution nonmetal determinations. (CW)

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

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2015-01-01

    Roč. 109, JUL (2015), s. 16-23 ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant - others:GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : hydride generation * arsenic * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.289, year: 2015

  9. 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.

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

    African Journals Online (AJOL)

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

  11. 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)

  12. Atomic spectrometry based on metallic tube atomizers heated by flame: Innovative strategies from fundamentals to analysis

    International Nuclear Information System (INIS)

    Arruda, Marco Aurelio Zezzi; Figueiredo, Eduardo Costa

    2009-01-01

    This review describes recent developments in atomic absorption spectrometry using metallic tube atomizers heated by flames. Sample introduction in spray or gaseous form is emphasized, describing some proposed systems for this task and the fundamentals involved in each context. The latest challenges and future possibilities for use of metallic tubes in atomic/mass spectrometry are also considered.

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

    Czech Academy of Sciences Publication Activity Database

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

    2012-01-01

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

  14. 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.)

  15. 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

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

    International Nuclear Information System (INIS)

    Heitmann, U.; Hese, A.; Schoknecht, G.; Gries, W.

    1995-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-15

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

  18. 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)

  19. 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.

  20. Electrochemical hydride generation atomic absorption spectrometry for determination of cadmium

    Energy Technology Data Exchange (ETDEWEB)

    Arbab-Zavar, M.H. [Department of Chemistry, Faculty of Science, Ferdowsi University, Mashhad (Iran, Islamic Republic of)]. E-mail: arbab@um.ac.ir; Chamsaz, M. [Department of Chemistry, Faculty of Science, Ferdowsi University, Mashhad (Iran, Islamic Republic of); Youssefi, A. [Pare-Taavous Research Institute, Mashhad (Iran, Islamic Republic of); Aliakbari, M. [Department of Chemistry, Faculty of Science, Ferdowsi University, Mashhad (Iran, Islamic Republic of)

    2005-08-01

    An electrolytic hydride generation system for determination of another hydride forming element, cadmium, by catholyte variation electrochemical hydride generation (EcHG) atomic absorption spectrometry is described. A laboratory-made electrolytic cell with lead-tin alloy as cathode material is designed as electrolytic generator of molecular hydride. The influences of several parameters on the analytical signal have been evaluated using a Plackett-Burman experimental design. The significant parameters such as cathode surface area, electrolytic current, carrier gas flow rate and catholyte concentration have been optimized using univariate method. The analytical figures of merit of procedure developed were determined. The calibration curve was linear up to 20 ng ml{sup -1}of cadmium. The concentration detection limit (3{sigma}, n = 8) of 0.2 ng ml{sup -1} and repeatability (relative standard deviation, n = 7) of 3.1% were achieved at 10.0 ng ml{sup -1}. It was shown that interferences from major constituents at high concentrations were significant. The accuracy of method was verified using a real sample (spiked tap water) by standard addition calibration technique. Recovery of 104% was achieved for Cd in the spiked tap water sample.

  1. Feasibility of filter atomization in high-resolution continuum source atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Heitmann, Uwe; Becker-Ross, Helmut; Katskov, Dmitri

    2006-01-01

    A prototype spectrometer for high-resolution continuum source atomic absorption spectrometry (HR-CS AAS), built at ISAS Berlin, Germany, was combined with a graphite filter atomizer (GFA), earlier developed at TUT, Pretoria, South Africa. The furnace and auto-sampler units from a commercial AA spectrometer, model AAS vario 6 (Analytik Jena AG, Jena, Germany), were employed in the instrument. Instead of conventional platform tube, the GFA was used to provide low measurement susceptibility to interferences and short determination cycle. The GFA was modified according to the design of the furnace unit and optimal physical parameters of its components (filter and collector) found. Afterwards, optimal GFA was replicated and tested to outline analytical performances of the HR-CS GFA AA spectrometer in view of prospects of multi-element analysis. In particular, reproducibility of performances, repeatability of analytical signals, lifetime, temperature limit and duration of the measurement cycle were examined, and elements available for determination justified. The results show that the peak area of the atomic absorption signal is reproduced in various GFA copies within ± 4% deviation range. The GFA can stand temperatures of 2800 deg. C with 6 s hold time for 55 temperature cycles, and 2700 deg. C (8 s) for about 200 cycles. Only the external tube is prone to destruction while the filter and collector do not show any sign of erosion caused by temperature or aggressive matrix. Analytical signals are affected insignificantly by tube aging. Repeatability of the peak area remains within 1.1-1.7% RSD over more than hundred determination cycles. Peak areas are proportional to the sample volume of injected organic and inorganic liquids up to at least 50 μL. The drying stage is combined with hot sampling and cut down to 15-20 s. The list of metals available for determination with full vapor release includes Al, Co, Cr, Ni, Pt as well as more volatile metals. Characteristic

  2. 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

  3. 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

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

    International Nuclear Information System (INIS)

    Barthelat, J.C.; Pelissier, M.; Durand, P.

    1980-01-01

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

  5. Auger spectrometry of atoms and molecules

    International Nuclear Information System (INIS)

    Krause, M.O.

    1994-01-01

    The author discusses the importance of Auger spectrometry at synchrotron radiation centers. First, he explains how a high energy photon source such as the APS (Advanced Photon Source) could be used to help provide missing spectral information about the shell structure of some elements. The missing data occurs mainly at higher energies in the 1--10 keV ranges as for the K-shells of Z = 30 to 60 elements and the L-shells for Z = 30 to 100 elements. He explains how even though Auger electron spectrometry does not depend on synchrotron radiation it can greatly benefit from this variable photon source as it allows one to select the Auger line group that is most suitable for a specific purpose. Most significantly, a continuous photon source becomes indispensable when one is interested in threshold effects. Lastly, he discusses coherence effects between different inner-shell vacancy states by way of some recent work done at Daresbury

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-04-08

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

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

    International Nuclear Information System (INIS)

    Grindlay, Guillermo; Mora, Juan; Gras, Luis; Loos-Vollebregt, Margaretha T.C. de

    2011-01-01

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

  8. Fast atom bombardment mass spectrometry of condensed tannin sulfonate derivatives

    Science.gov (United States)

    J.J. Karchesy; L.Y. Foo; Richard W. Hemingway; E. Barofsky; D.F. Barofsky

    1989-01-01

    Condensed tannin sulfonate derivatives were studied by fast atom bombardment mass spectrometry (FAB-MS) to assess the feasibility of using this technique for determining molecular weight and structural information about these compounds. Both positive- and negative-ion spectra provided useful data with regard to molecular weight, cation species present, and presence of...

  9. Determination of boron in natural waters using atomic-absorption spectrometry with electrothermal atomization

    International Nuclear Information System (INIS)

    Usenko, S.I.; Prorok, M.M.

    1992-01-01

    A method of direct determination of boron in natural waters using atomic-absorption spectrometry with electrothermal atomization was developed. Concomitant elements Si, K, Mg, Na, present in natural waters in the concentration of 0.05-100 mg/cv 3 , do not produce effect on the value of boron atomic absorption. Boron determination limit constituted 0.02 mg/cm 3 for 25 ml of solution introduced

  10. 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...

  11. Four-parameter analytical local model potential for atoms

    International Nuclear Information System (INIS)

    Fei, Yu; Jiu-Xun, Sun; Rong-Gang, Tian; Wei, Yang

    2009-01-01

    Analytical local model potential for modeling the interaction in an atom reduces the computational effort in electronic structure calculations significantly. A new four-parameter analytical local model potential is proposed for atoms Li through Lr, and the values of four parameters are shell-independent and obtained by fitting the results of X a method. At the same time, the energy eigenvalues, the radial wave functions and the total energies of electrons are obtained by solving the radial Schrödinger equation with a new form of potential function by Numerov's numerical method. The results show that our new form of potential function is suitable for high, medium and low Z atoms. A comparison among the new potential function and other analytical potential functions shows the greater flexibility and greater accuracy of the present new potential function. (atomic and molecular physics)

  12. Laser-excited atomic fluorescence spectrometry in a pressure-controlled electrothermal atomizer.

    Science.gov (United States)

    Lonardo, R F; Yuzefovsky, A I; Irwin, R L; Michel, R G

    1996-02-01

    A theoretical model was developed to describe the loss of analyte atoms in graphite furnaces during atomization. The model was based on two functions, one that described the supply of analyte by vaporization, and another that described the removal of the analyte by diffusion. Variation in working pressure was shown to affect the competition between these two processes. Optimal atomization efficiency was predicted to occur at a pressure where the supply of the analyte was maximized, and gas phase interactions between the analyte and matrix were minimized. Experiments to test the model included the direct determination of phosphorus and tellurium in nickel alloys and of cobalt in glass. In all cases, reduction in working pressure from atmospheric pressure to 7 Pa decreased sensitivity by 2 orders of magnitude, but improved temporal peak shape. For the atomization of tellurium directly from a solid nickel alloy, and the atomization of cobalt from an aqueous solution, no change in sensitivity was observed as the working pressure was reduced from atmospheric pressure to approximately 70 kPa. If a reduction in working pressure affected only the diffusion of the analyte, poorer sensitivity should have been obtained. Only a commensurate increase in analyte vaporization could account for maintained sensitivity at lower working pressures. Overall, analyte vaporization was not dramatically improved at reduced working pressures, and maximum atomization efficiency was found to occur near atmospheric pressure.

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

    Czech Academy of Sciences Publication Activity Database

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

    2014-01-01

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

  14. Determination of strontium in rocks by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Tamari, Yuzo; Tsuji, Haruo; Kusaka, Yuzuru

    1984-01-01

    Strontium in silicate rocks was determined by the following procedure. A rock powder sample prepared to pass through a 100-mesh size sieve (0.1--0.5g) was taken in a Teflon beaker, and 6ml of 46% hydrofluoric acid and 1 ml of 70% perchloric acid were added. After being allowed to stand for over one day, the mixture in the beaker was concentrated by heating on a hot plate until white fumes of the perchloric acid appeared. The content in the beaker was transferred to a glass beaker with 2ml of 61% nitric acid and 0.5ml of the perchloric acid, and concentrated until white fumes appeared. Further, 2ml of 20% hydrochloric acid was added and warmed. After cooling, the rock solution was made up to 100ml with water. To a 50-ml stoppered centrifugal tube, a 10-ml portion of the rock solution was transferred, and 1ml of 2% 8-quinolinol solution was added. Then the solution was adjusted to pH 5 with both saturated sodium acetate solution and hydrochloric acid, and made up to 15ml. The decomposed rock sample solution with 20ml of chloroform was shaken for 5min. The decomposed rock sample solution was shaken with 20ml of chloroform for 5min, and then centrifuged at 2500rpm for 5min to separate an aqueous phase from an organic one. After adding 1ml of 2% lanthanum solution into a 10ml portion of the aqueous phase, strontium was determined by atomic absorption spectrometry at 460.7nm. This method was applied to the rock reference materials, JB-1 and JG-1, issued from the Geological Survey of Japan. Analytical values of strontium in the rocks were almost consistent with their certified and recommended values. (author)

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

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    with an aqueous solution of 6 mmol L-1 of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass......An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination...... spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 sigma) achieved by the HPLC-FAAS system was 1 mg L-1 of selenium (100 mu L injections) for each of the four...

  16. Limit of quantitation in atomic spectrometry: An unambiguous concept?

    International Nuclear Information System (INIS)

    Mermet, Jean-Michel

    2008-01-01

    This document presents a tutorial description of several concepts and definitions of limits of quantitation, such as the so-called 10 s, the RSD net , the method limit, the lower limit of the calibration graph and the uncertainty approaches. Use, advantages, limitations and complexity of the various approaches are illustrated with some examples taken from atomic spectrometry, using ICP-AES, ICP-MS and LIBS. Information that can be deduced from the calibration graph is emphasized

  17. Development of an analytical model for the determination of {sup 60}Co in aqueous samples by atomic absorption and gamma spectrometry techniques; Elaboracion de un modelo analitico para la determinacion de {sup 60}Co en muestras acuosas mediante tecnicas de absorcion atomica y espectrometria gamma

    Energy Technology Data Exchange (ETDEWEB)

    Solis A, N. A.

    2015-07-01

    The applications of the nuclear energy in industry and medicine generate radioactive wastes that must be isolated and confined in order to limit its spread in the biosphere. These types of wastes are generated in hospitals, industry, research centers and nuclear power plants (during de fuel cycle). The radioactive elements (radionuclides) cannot be destroyed by any known method, either chemical or mechanical. Its final destruction is produced by radioactive decay, which makes them stable isotopes, or nuclear transmutation being bombarded with atomic particles. Consequently, the radioactive waste management is to control the radioactive discharges and reduce to tolerable limits, eliminating of effluents and wastes the radionuclides of interest, concentrating them so they can be stored or evacuated so that later not appear in dangerous concentration in the biosphere. In Mexico, the main generators of radioactive wastes are the nuclear power plant of Laguna Verde in Veracruz, Hospitals of the public and private sector, in addition Instituto Nacional de Investigaciones Nucleares (ININ) some institutes and facilities of the UNAM and Instituto Politecnico Nacional (IPN) and industries among others. The aqueous radioactive wastes, particularly those from the nuclear power plants contain traces of cobalt-60. Currently there is no model or analytical technique for the separation of this radionuclide, so it became necessary to develop an analytical model for separation and facilitate their disposal. In this paper was shown that atomic absorption and gamma spectrometry techniques can separate the active concentration of the inactive, which is important because the total concentration can be associated through direct relationships with the wear of metal parts of the nuclear reactor, since the metal alloys of the same reactor containing a fraction of cobalt. Also this analytical and mathematical model that can be reproducible and applicable to full sets of samples and that this

  18. 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

  19. Analytical applications of resonance ionization mass spectrometry (RIMS)

    International Nuclear Information System (INIS)

    Fassett, J.D.; Travis, J.C.

    1988-01-01

    A perspective on the role of resonance ionization mass spectrometry (RIMS) in the field of analytical chemistry is presented. RIMS provides new, powerful, and complementary capabilities relative to traditional methods of inorganic mass spectrometry. Much of the initial work in RIMS has been to illustrate these capabilities and define the potential of RIMS in the generalized field of chemical analysis. Three areas of application are reviewed here: (1) noble gas measurements; (2) materials analysis using isotope dilution (IDMS); and, (3) solids analysis using direct sampling. The role of RIMS is discussed relative to the more traditional mass spectrometric methods of analysis in these areas. The applications are meant to illustrate the present state-of-the-art as well as point to the future state-of-the-art of RIMS in chemical analysis. (author)

  20. Determination of mercury in microwave-digested soil by laser-excited atomic fluorescence spectrometry with electrothermal atomization.

    Science.gov (United States)

    Pagano, S T; Smith, B W; Winefordner, J D

    1994-12-01

    A sample digestion procedure was developed which employs microwave heating of soil and sediment in concentrated nitric acid in a high-pressure closed vessel. Complete dissolution of mercury into the sample solution occurs within 5 min at 59 W/vessel without loss of analyte through overpressurization. Laser-excited atomic fluorescence spectrometry with electrothermal atomization (LEAFS-ETA) was used as the detection method. The scheme uses a two-step excitation, with lambda(1) = 253.7 nm and lambda(2) = 435.8 nm. Direct line fluorescence was measured at 546.2 nm. The absolute instrumental limit of detection was 14 fg; 1.4 pg/ml with a 10 mul sample injection. The recoveries of mercury in two spiked samples were 94 and 98%. The SRM 8406 (Mercury in River Sediment) was digested and analyzed for mercury, and the results (58.4 +/- 1.8 ng/g) agreed well with the reference value of 60 ng/g. The results obtained by LEAFS-ETA with microwave sample digestion are in good agreement with those found by cold vapor atomic absorption spectrometry with EPA Series Method 245.5 sample digestion, which is one of the most commonly used methods for the determination of mercury in soil.

  1. 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.

  2. 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.

  3. 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.

  4. 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

  5. Determination of lead in high-purity silver. Comparison between photon activation and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Loos-Neskovic, C.; Fedoroff, M.; Revel, G.

    1978-01-01

    A chemical separation based on the fixation of silver on nickel ferrocyanide was studied. It was applied to the determination of lead in silver by photon-activation or atomic absorption spectrometry. The first method gave a detection limit of 0.1 μg. The second one could not be applied for concentration less than 50 μg/g, owing to loss by adsorption. Analytical results showed that lead is one of the major metallic impurity in high purity silver. (author)

  6. Investigation of interference mechanism of cobalt chloride on the determination of bismuth by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tokman, Nilgun [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, Maslak, Istanbul 34469 (Turkey); Akman, Suleyman [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, Maslak, Istanbul 34469 (Turkey)]. E-mail: akmans@itu.edu.tr

    2005-03-31

    The interferences of cobalt chloride on the determination of bismuth by electrothermal atomic absorption spectrometry (ETAAS) were examined using a dual cavity platform (DCP), which allows the gas-phase and condensed phase interferences to be distinguished. Effects of pyrolysis temperature, pyrolysis time, atomization temperature, heating rate in the atomization step, gas-flow rate in the pyrolysis and atomization steps, interferent mass and atomization from wall on sensitivity as well as atomization signals were studied to explain the interference mechanisms. The mechanism proposed for each experiment was verified with other subsequent sets of experiments. Finally, modifiers pipetted on the thermally treated sample+interferent mixture and pyrolyzed at different temperatures provided very useful information for the existence of volatilization losses of analyte before the atomization step. All experiments confirmed that when low pyrolysis temperatures are applied, the main interference mechanisms are the gas-phase reaction between bismuth and decomposition products of cobalt chloride in the atomization step. On the other hand, at elevated temperatures, the removal of a volatile compound formed between analyte and matrix constituents is responsible for some temperature-dependent interferences, although gas-phase interferences still continue. The experiments performed with colloidal palladium and nickel nitrate showed that the modifier behaves as both a matrix modifier and analyte modifier, possibly delaying the vaporization of either analyte or modifier or both of them.

  7. 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)

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    1996-01-01

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

  9. Laser-induced plasma spectrometry: truly a surface analytical tool

    International Nuclear Information System (INIS)

    Vadillo, Jose M.; Laserna, J.

    2004-01-01

    For a long period, analytical applications of laser induced plasma spectrometry (LIPS) have been mainly restricted to overall and quantitative determination of elemental composition in bulk, solid samples. However, introduction of new compact and reliable solid state lasers and technological development in multidimensional intensified detectors have made possible the seeking of new analytical niches for LIPS where its analytical advantages (direct sampling from any material irrespective of its conductive status without sample preparation and with sensitivity adequate for many elements in different matrices) could be fully exploited. In this sense, the field of surface analysis could take advantage from the cited advantages taking into account in addition, the capability of LIPS for spot analysis, line scan, depth-profiling, area analysis and compositional mapping with a single instrument in air at atmospheric pressure. This review paper outlines the fundamental principles of laser-induced plasma emission relevant to sample surface studies, discusses the experimental parameters governing the spatial (lateral and in-depth) resolution in LIPS analysis and presents the applications concerning surface examination

  10. 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…

  11. 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.

  12. 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.

  13. 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

  14. Calibration in atomic spectrometry: A tutorial review dealing with quality criteria, weighting procedures and possible curvatures

    International Nuclear Information System (INIS)

    Mermet, Jean-Michel

    2010-01-01

    Calibration is required to obtain analyte concentrations in atomic spectrometry. To take full benefit of it, the adequacy of the coefficient of determination r 2 is discussed, and its use is compared with the uncertainty due to the prediction bands of the regression. Also discussed from a tutorial point of view are the influence of the weighting procedure and of different weighting factors, and the comparison between linear and quadratic regression to cope with curvatures. They are illustrated with examples based on the use of ICP-AES with nebulization and laser ablation, and of LIBS. Use of a calibration graph over several orders of magnitude may be problematic as well as the use of a quadratic regression to cope with possible curvatures. Instrument softwares that allow reprocessing of the calibration by selecting standards around the expected analyte concentration are convenient for optimizing the calibration procedure.

  15. Derivative flame atomic absorption spectrometry and its application in trace analysis

    International Nuclear Information System (INIS)

    Sun, H. W.; Li, L. Q.

    2005-01-01

    Flame atomic absorption spectrometry is an accepted and widely used method for the determination of trace elements in a great variety of samples. But its sensitivity doesn't meet the demands of trace and ultra-trace analysis for some samples. The derivative signal processing technique, with a very high capability for enhancing sensitivity, was developed for flame atomic absorption spectrometry. The signal models of conventional flame atomic absorption spectrometry are described. The equations of derivative signals are established for flame atomic absorption spectrometry, flow injection atomic absorption spectrometry (FI-FAAS) and atom trapping flame atomic absorption spectrometry (AT-FAAS). The principle and performance of the derivative atomic absorption spectrometry are evaluated. The derivative technique based on determination of variation rate of signal intensity with time (dl/dt) is different from the derivative spectrophotometry based on determination of variation rate of signal intensity with wavelength (dl/dhλ). Derivative flame atomic absorption spectrometry has higher sensitivity, lower detection limits and better accuracy. It has been applied to the direct determination of trace elements without preconcentration. If the derivative technique was combined with several preconcentration techniques, the sensitivity would be enhanced further for ultra-trace analysis with good linearity. The applications of derivative flame atomic absorption spectroscopy are reviewed for trace element analysis in biological, pharmaceutical, environmental and food samples

  16. 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

  17. Laser-excited atomic-fluorescence spectrometry with electrothermal tube atomization.

    Science.gov (United States)

    Vera, J A; Leong, M B; Stevenson, C L; Petrucci, G; Winefordner, J D

    1989-12-01

    The performance of graphite-tube electrothermal atomizers is evaluated for laser-excited atomic-fluorescence spectrometry for several elements. Three pulsed laser systems are used to pump tunable dye lasers which subsequently are used to excite Pb, Ga, In, Fe, Ir, and Tl atoms in the hot graphite tube. The dye laser systems used are pumped by nitrogen, copper vapour and Nd:YAG lasers. Detection limits in the femtogram and subfemtogram range are typically obtained for all elements. A commercial graphite-tube furnace is important for the successful utilization of the laser-based method when the determination of trace elements is intended, especially when complicated matrices may be present.

  18. 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

  19. Speciation of protein-bound trace elements by gel electrophoresis and atomic spectrometry.

    Science.gov (United States)

    Ma, Renli; McLeod, Cameron W; Tomlinson, Kerry; Poole, Robert K

    2004-08-01

    The metabolism of trace elements, in particular their binding to proteins in biological systems is of great importance in biochemical, toxicological, and pharmacological studies. As a result there has been a sustained interest over the last two decades in the speciation of protein-bound metals. Various analytical approaches have been employed, combining efficient separation of metalloproteins by liquid chromatography or electrophoresis with high-sensitivity elemental detection. Slab-gel electrophoresis (GE) is a key platform for high-resolution protein separation, and has been combined with autoradiography and various atomic spectrometric techniques for in-gel determination of protein-bound metals. Recently, the combination of GE with state-of-the-art inductively coupled plasma-mass spectrometry (ICP-MS), particularly when linked to laser ablation (LA) for direct gel interrogation, has opened up new opportunities for rapid characterization of metalloproteins. The use of GE and atomic spectrometry for the speciation of protein-bound trace elements is reviewed in this paper. Technical requirements for gel electrophoresis/atomic spectrometric measurement are considered in terms of method compatibilities, detection capability and potential usefulness. The literature is also surveyed to illustrate current status and future trends. Copyright 2004 Wiley-VCH Verlag GmbH and Co.

  20. Ultratrace determination of lead in whole blood using electrothermal atomization laser-excited atomic fluorescence spectrometry.

    Science.gov (United States)

    Wagner, E P; Smith, B W; Winefordner, J D

    1996-09-15

    Laser-excited atomic fluorescence has been used to detect lead that was electrothermally atomized from whole blood in a graphite furnace. A 9 kHz repetition rate copper vapor laser pumped dye laser was used to excite the lead at 283.3 nm, and the resulting atomic fluorescence was detected at 405.8 nm. No matrix modification was used other than a 1:21 dilution of the whole blood with high-purity water. Using the atomic fluorescence peak area as the analytical measure and a background correction technique based upon a simultaneous measurement of the transmitted laser intensity, excellent agreement for NIST and CDC certified whole blood reference samples was obtained with aqueous standards. A limit of detection in blood of 10 fg/mL (100 ag absolute) was achieved.

  1. A sapphire tube atomizer for on-line atomization and in situ collection of bismuthine for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Dědina, Jiří

    2013-01-01

    Roč. 28, č. 4 (2013), s. 593-600 ISSN 0267-9477 Institutional support: RVO:68081715 Keywords : hydride generation * sapphire tube atomizer * in situ collection Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.396, year: 2013

  2. 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.

  3. Analytical local electron-electron interaction model potentials for atoms

    International Nuclear Information System (INIS)

    Neugebauer, Johannes; Reiher, Markus; Hinze, Juergen

    2002-01-01

    Analytical local potentials for modeling the electron-electron interaction in an atom reduce significantly the computational effort in electronic structure calculations. The development of such potentials has a long history, but some promising ideas have not yet been taken into account for further improvements. We determine a local electron-electron interaction potential akin to those suggested by Green et al. [Phys. Rev. 184, 1 (1969)], which are widely used in atom-ion scattering calculations, electron-capture processes, and electronic structure calculations. Generalized Yukawa-type model potentials are introduced. This leads, however, to shell-dependent local potentials, because the origin behavior of such potentials is different for different shells as has been explicated analytically [J. Neugebauer, M. Reiher, and J. Hinze, Phys. Rev. A 65, 032518 (2002)]. It is found that the parameters that characterize these local potentials can be interpolated and extrapolated reliably for different nuclear charges and different numbers of electrons. The analytical behavior of the corresponding localized Hartree-Fock potentials at the origin and at long distances is utilized in order to reduce the number of fit parameters. It turns out that the shell-dependent form of Green's potential, which we also derive, yields results of comparable accuracy using only one shell-dependent parameter

  4. Lithium determination in whole blood by flame atomic emission spectrometry

    International Nuclear Information System (INIS)

    Rahman, S.; Khalid, N.; Nasimullah; Iqbal, M.Z.

    2003-01-01

    A simple and rapid method for the determination of lithium in whole blood using Flame atomic emission spectrometry is described. No sample preparation was required apart from dilution with 0.02 N HNO/sub 3/. The reliability of the method was determined by analyzing Standard Reference Material (SRM) under identical experimental conditions and comparing the determined lithium concentration with the reported value. These were in good agreement with each other. The determined range of lithium in the whole blood of fifty-six healthy adult volunteers (28 males and 28 females) were 13.1 - 47.8 mg L-1. The determined average concentration of lithium in whole blood was compared with the reported values of other countries. The data was statistically analyzed with respect to sex and different age groups. (author)

  5. Analytic approximations for integrated electron-atom excitations

    International Nuclear Information System (INIS)

    McCarthy, I.E.; Saha, B.C.; Stelbovics, A.T.

    1980-09-01

    Accurate calculations of atomic excitations require estimates of the effect of higher excitations on the effective (optical) potential coupling various reaction channels. The total cross section for a particular excitation is proportional to the maximum contribution of that excitation to the imaginary part of the elastic momentum-space optical potential, and is typical of the contribution to the potential in general. Analytic expressions relevant to the calculation of optical potentials are given. Their validity is estimated by comparison with more-accurate calculations and with experimental excitation cross sections

  6. The Validation of Atomic Absorption Spectrometry (AAS) Method for the Determination of Cr, Cu and Pb

    International Nuclear Information System (INIS)

    Purwanto, A.; Supriyanto, C.; Samin P

    2007-01-01

    The validation of analytical method of atomic absorption spectrometry for the determination of Cr, Cu and Pb by using certified reference materials (CRM) have been carried out. The validation of analytical method was done by measurement of precision, accuracy, bias, % D and % RSD by analysis of chromium (Cr), Copper (Cu), and Lead (Pb) elements in CRM samples. Soil-7 is weighted and dissolved 0.3337 gram to use the bomb digester with concentrated nitric acid, perchloric acid, fluoric acid, and than solution to vinal volume is 10 mL with aquabidest. The validity of instrument atomic absorption spectrometer still valid with obtained of accuracy is 95.85 % and precision is 2.86 for Cr.; 103.32 % and 0.45 for Cu., 114.14 % and 9.89 for Pb. The validation of analytical method showed that with obtained of the content of Cr, Cu and Pb elements is 57.51, 11.37 and 68.49 μg/g., this result is still in the range concentration of certificate. (author)

  7. 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

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

    International Nuclear Information System (INIS)

    Jat, J.R.; Nayak, A.K.; Balaji Rao, Y.; Ravindra, H.R.

    2013-01-01

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

  9. Atomic absorption spectrometry and other instrumental methods for quantitative measurements of arsenic

    International Nuclear Information System (INIS)

    Brooks, R.R.; Ryan, D.E.; Zhang, H.

    1981-01-01

    Progress in instrumental methods for quantification of arsenic during the past decade is reviewed. Particular emphasis is placed on atomic absorption spectrometry, where major progress has been made in flame methods in conjunction with hydride generation procedures and in electrothermal methods with the graphite furnace. Specific materials in which arsenic is quantified by atomic absorption techniques are also listed. Progress in the application of neutron activation-γ-spectrometry, emission spectrometry, electrometric methods, X-ray procedures and atomic fluorescence spectrometry is also reviewed. The limits of detection and time requirements of all the techniques are compared. (Auth.)

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

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

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

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

    International Nuclear Information System (INIS)

    Gayone, J.E.; Sanchez, E.A.; Grizzi, O.; Universidad Nacional de Cuyo, Mendoza

    1998-01-01

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

  12. 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

  13. Slurry analysis after lead collection on a sorbent and its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Baysal, Asli; Tokman, Nilgun [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak-Istanbul (Turkey); Akman, Suleyman [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak-Istanbul (Turkey)], E-mail: akmans@itu.edu.tr; Ozeroglu, Cemal [Istanbul University, Department of Chemistry, Faculty of Engineering, 34320 Avcilar-Istanbul (Turkey)

    2008-02-11

    In this study, in order to eliminate the drawbacks of elution step and to reach higher enrichment factors, a novel preconcentration/separation technique for the slurry analysis of sorbent loaded with lead prior to its determination by electrothermal atomic absorption spectrometry was described. For this purpose, at first, lead was collected on ethylene glycol dimethacrylate methacrylic acid copolymer (EGDMA-MA) treated with ammonium pyrolidine dithiocarbamate (APDC) by conventional batch technique. After separation of liquid phase, slurry of the sorbent was prepared and directly pipetted into graphite furnace of atomic absorption spectrophotometer. Optimum conditions for quantitative sorption and preparation of the slurry were investigated. A 100-fold enrichment factor could be easily reached. The analyte element in certified sea-water and Bovine-liver samples was determined in the range of 95% confidence level. The proposed technique was fast and simple and the risks of contamination and analyte loss were low. Detection limit (3{delta}) for Pb was 1.67 {mu}g l{sup -1}.

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

    International Nuclear Information System (INIS)

    Boaventura, G.R.; Rocha Hirson, J. da; Santelli, R.E.

    1989-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Hernandez, A; Mateos, R.; Garcia-Mesa, J.A.; Beltran, G.; Fernandez-Escobar, R.

    2010-07-01

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

  16. Fast atom bombardment tandem mass spectrometry of carotenoids

    Energy Technology Data Exchange (ETDEWEB)

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

    1995-02-01

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

  17. 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.

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

    Science.gov (United States)

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

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

    Science.gov (United States)

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

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

  20. Measuring deuterium enrichment of glucose hydrogen atoms by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Antoniewicz, Maciek R; Kelleher, Joanne K; Stephanopoulos, Gregory

    2011-04-15

    We developed a simple and accurate method for determining deuterium enrichment of glucose hydrogen atoms by electron impact gas chromatography mass spectrometry (GC/MS). First, we prepared 18 derivatives of glucose and screened over 200 glucose fragments to evaluate the accuracy and precision of mass isotopomer data for each fragment. We identified three glucose derivatives that gave six analytically useful ions: (1) glucose aldonitrile pentapropionate (m/z 173 derived from C4-C5 bond cleavage; m/z 259 from C3-C4 cleavage; m/z 284 from C4-C5 cleavage; and m/z 370 from C5-C6 cleavage); (2) glucose 1,2,5,6-di-isopropylidene propionate (m/z 301, no cleavage of glucose carbon atoms); and (3) glucose methyloxime pentapropionate (m/z 145 from C2-C3 cleavage). Deuterium enrichment at each carbon position of glucose was determined by least-squares regression of mass isotopomer distributions. The validity of the approach was tested using labeled glucose standards and carefully prepared mixtures of standards. Our method determines deuterium enrichment of glucose hydrogen atoms with an accuracy of 0.3 mol %, or better, without the use of any calibration curves or correction factors. The analysis requires only 20 μL of plasma, which makes the method applicable for studying gluconeogenesis using deuterated water in cell culture and animal experiments. © 2011 American Chemical Society

  1. Symposium on fast atom and ion induced mass spectrometry of nonvolatile organic solids

    International Nuclear Information System (INIS)

    McNeal, C.J.

    1982-01-01

    The mechanisms of molecular and fragment ion production and the various parameters affecting ion yields were discussed by 6 invited speakers from Europe, Canada, and the US at this symposium. The work reported was almost equally divided between that using low-energy (keV) primary ion (or atom) beams, e.g. fast atom bombardment mass spectrometry (FABMS) and secondary ion mass spectrometry (SIMS) and that using high energy (MeV) particles, e.g. heavy ion induced mass spectrometry (HIIDMS) and 252 Cf-plasma desorption mass spectrometry ( 252 Cf-PDMS). Both theoretical foundations and observed experimental results for both techniques are included

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

    Science.gov (United States)

    Chan, George C. Y. [Bloomington, IN; Hieftje, Gary M [Bloomington, IN

    2010-08-03

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

  3. Recycling nebulization-sample introduction system for inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Kato, Kaneharu; Takashima, Kyoichiro

    1989-01-01

    A recycling nebulization-sample introduction system which exhibits the long-term stability of analyte emission signals while consuming small sample volumes was constructed for inductively coupled plasma atomic emission spectrometry. The present system is composed of five main parts: i.e., a spherical cyclone spray chamber, two commercial concentric nebulizers, two 3-way stopcocks, an aerosol transport tube with heater, and a commercial concentric three-tube plasma torch. It is based on the spray chamber where the two nebulizers are mounted (twin-nebulizer configuration): one is for introduction of a sample or a rinse solution into the spray chamber, and the other one is for recycling nebulization of the solution introduced. The nebulizers are easily demountable symmetrically and horizontally outside the spray chamber. Analytical performance and nebulization characteristics are described in comparison with a conventional sample introduction system. A stable signal of analyte emission intensity was extended to 20 min for 1 ml of sample under the ordinary condition of 0.6l/min carrier gas flow rate. (author)

  4. Bibliometric mapping: eight decades of analytical chemistry, with special focus on the use of mass spectrometry.

    Science.gov (United States)

    Waaijer, Cathelijn J F; Palmblad, Magnus

    2015-01-01

    In this Feature we use automatic bibliometric mapping tools to visualize the history of analytical chemistry from the 1920s until the present. In particular, we have focused on the application of mass spectrometry in different fields. The analysis shows major shifts in research focus and use of mass spectrometry. We conclude by discussing the application of bibliometric mapping and visualization tools in analytical chemists' research.

  5. Direct determination of Hg in polymers by solid sampling-graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Resano, M.; Briceno, J.; Belarra, M.A.

    2009-01-01

    This work explores the potential of solid sampling-graphite furnace atomic absorption spectrometry (SS-GFAAS) for the fast and direct determination of Hg in polymers. Eight certified reference materials with different composition (polyethylene-PE-, polystyrene-PS-, poly vinyl chloride-PVC- and acrylonitrile butadiene styrene-ABS-) were selected for the study, covering a wide Hg content range (from 20 to 1100 μg g - 1 ). The difficulties found in achieving a selective atomization of the analyte from these samples were partially mitigated by the maintenance of the Ar flow during the atomization step, leading to an improved signal-to-background ratio. Even then, when a line source (LS) GFAAS instrument was employed for analysis, it was only possible to develop truly accurate procedures relying on the use of aqueous standards for calibration for PE and PVC samples, and different atomization conditions (1200 deg. C and 1300 deg. C, respectively) were needed for the two types of samples. The use of high-resolution continuum source (HR-CS) GFAAS instrumentation permitted to improve this situation significantly thanks to its higher potential for the correction of high and fast changing background. With such an instrument, satisfactory results could be obtained for all the samples under study using the same atomization conditions (1200 deg. C) and aqueous standard solutions for calibration. Additionally, the HR-CS GFAAS technique presented a lower limit of detection (0.6 μg g - 1 for CS and 2.2 μg g - 1 for LS), a broader linear range (10 to 320 Hg ng for CS, and 20 to 200 ng for LS), and a somewhat improved sensitivity (approximately 0.0030 s ng - 1 for CS using the three central pixels for quantification, and approximately 0.0025 s ng - 1 for LS). Overall, the use of HR-CS GFAAS permits obtaining significant advantages for the determination of this complex analyte in plastics, such as straightforward calibration with aqueous standards, a high sample throughput (15 min

  6. 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

  7. 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.

  8. 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...

  9. Monitoring of Pd in airborne particulates by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Atilgan, Semin [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469, Maslak, Istanbul (Turkey); Akman, Suleyman, E-mail: akmans@itu.edu.tr [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469, Maslak, Istanbul (Turkey); Baysal, Asli [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469, Maslak, Istanbul (Turkey); Bakircioglu, Yasemin [Trakya University, Faculty of Science and Letters, Department of Chemistry, 22030, Edirne (Turkey); Szigeti, Tamas; Ovari, Mihaly; Zaray, Gyula [Eoetvoes Lorand University, Institute of Chemistry, Department of Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary)

    2012-04-15

    An analytical method has been developed for determination of palladium in PM2.5 fractions of urban airborne particulate matter by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry. For the optimization of the experimental conditions, a road dust certified reference material (BCR-723) was used. The influence of pyrolysis and atomization temperatures, the amount of sample introduced into the graphite furnace and the addition of acids, surfactants and modifiers on the analytical signal of Pd were investigated. The limit of detection, calculated based on three times the standard deviations of analytical signals obtained during the atomization of 10 blank filter pieces, was 0.07 pg/m{sup 3}. Since the amount of solid certified reference material introduced into the graphite furnace was about 50-2000 times lower than those required in order to obtain the certified value, the precision was relatively poor. This analytical method was applied for investigation of urban airborne particulate matter collected onto quartz fiber filters by high-volume aerosol samplers in the city center of Istanbul (Turkey) and Budapest (Hungary). The measured Pd concentrations changed in the range of 0.22-0.64 and 0.25-0.86 pg/m{sup 3} in Istanbul and Budapest, respectively. - Highlights: Black-Right-Pointing-Pointer Method development for palladium determination in air samples using solid sampling technique. Black-Right-Pointing-Pointer Analysis by solid sampling electrothermal atomic absorption spectrometry (HR CS ETAAS). Black-Right-Pointing-Pointer Monitoring of Pd in Istanbul and Budapest PM2.5 urban aerosols during one year. Black-Right-Pointing-Pointer Statistical analysis of results.

  10. Matrix digestion of soil and sediment samples for extraction of lead, cadmium and antimony and their direct determination by inductively coupled plasma-mass spectrometry and atomic emission spectrometry

    International Nuclear Information System (INIS)

    Chattopadhyay, P.; Fisher, A.S.; Henon, D.N.; Hill, S.J.

    2004-01-01

    An environmentally friendly and simple method has been developed for complete digestion of lead, cadmium and antimony from soil samples using a magnesium nitrate assisted dry ashing procedure. Statistical data for a series of experiments with standard reference materials are presented, and precision values are found to be comparable for inductively coupled plasma-mass spectrometry and for inductively coupled plasma-atomic emission spectrometry. From a single digest solution all analytes are quantified without involving any preconcentration routes. Inter-method comparison of inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) shows that the probability of the results being different is less than 99 %. (author)

  11. 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.

  12. 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)

  13. 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

  14. 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

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

    International Nuclear Information System (INIS)

    Leon, G.C. de; Shiraishi, K.; Kawamura, H.; Igaraishi, Y.; Palattao, M.V.; Azanon, E.M.

    1990-10-01

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

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

    International Nuclear Information System (INIS)

    Lopes Nunes, Dayana; Pereira dos Santos, Eliane Pereira; Barin, Juliano Smanioto; Mortari, Sergio Roberto; Dressler, Valderi Luiz; Moraes Flores, Erico Marlon de

    2005-01-01

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

  17. Ultrasound assisted pseudo-digestion of street dust samples prior to determination by atomic absorption spectrometry.

    Science.gov (United States)

    Elik, Adil

    2005-05-15

    A sample preparation method based on ultrasound assisted pseudo-digestion of Pb, Cu, Zn and Ni from street dust samples under ultrasonic effect has been described. Parameters influencing pseudo-digestion, such as sonication time, sample mass, particle size and solvent system were fully optimized. Final solutions obtained upon sonication were analyzed by atomic absorption spectrometry. The best conditions for metal pseudo-digestion were as follows: a 25min sonication time, a 0.3g sample mass (in 25ml solvent), a particle size <63mum and a mixture of concentrated HNO(3)-HClO(4)-HF (2:1:1, v/v/v). Analytical results for the four metals by ultrasound assisted pseudo-digestion, acid bomb and conventional wet digestion methods showed a good agreement, thus indicating the possibility of using mild conditions for sample preparation instead of intensive treatments inherent with the digestion methods. In addition, this method reduces the time required for all treatments (pseudo-digestion or digestion, heating to dryness, cooling and separation) with acid bomb and conventional wet digestion methods approximately from 9 to 1h. The accuracy of the method was tested either by comparing obtained results with those of acid bomb and conventional wet digestion methods or by application on two standard reference materials. The average relative standard deviation of ultrasound assisted pseudo-digestion method varied between 0.9 and 1.8% for N=12, depending on the analyte.

  18. Element selective detection of molecular species applying chromatographic techniques and diode laser atomic absorption spectrometry.

    Science.gov (United States)

    Kunze, K; Zybin, A; Koch, J; Franzke, J; Miclea, M; Niemax, K

    2004-12-01

    Tunable diode laser atomic absorption spectroscopy (DLAAS) combined with separation techniques and atomization in plasmas and flames is presented as a powerful method for analysis of molecular species. The analytical figures of merit of the technique are demonstrated by the measurement of Cr(VI) and Mn compounds, as well as molecular species including halogen atoms, hydrogen, carbon and sulfur.

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

    International Nuclear Information System (INIS)

    Lobo, K.K.

    1991-01-01

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

  20. Determination of antimony by using a quartz atom trap and electrochemical hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-01-15

    The analytical performance of a miniature quartz trap coupled with electrochemical hydride generator for antimony determination is described. A portion of the inlet arm of the conventional quartz tube atomizer was used as an integrated trap medium for on-line preconcentration of electrochemically generated hydrides. This configuration minimizes transfer lines and connections. A thin-layer of electrochemical flow through cell was constructed. Lead and platinum foils were employed as cathode and anode materials, respectively. Experimental operation conditions for hydride generation as well as the collection and revolatilization conditions for the generated hydrides in the inlet arm of the quartz tube atomizer were optimized. Interferences of copper, nickel, iron, cobalt, arsenic, selenium, lead and tin were examined both with and without the trap. 3{sigma} limit of detection was estimated as 0.053 {mu}g l{sup -1} for a sample size of 6.0 ml collected in 120 s. The trap has provided 18 fold sensitivity improvement as compared to electrochemical hydride generation alone. The accuracy of the proposed technique was evaluated with two standard reference materials; Trace Metals in Drinking Water, Cat CRM-TMDW and Metals on Soil/Sediment 4, IRM-008.

  1. Determination of antimony by using a quartz atom trap and electrochemical hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Menemenlioglu, Ipek; Korkmaz, Deniz; Ataman, O. Yavuz

    2007-01-01

    The analytical performance of a miniature quartz trap coupled with electrochemical hydride generator for antimony determination is described. A portion of the inlet arm of the conventional quartz tube atomizer was used as an integrated trap medium for on-line preconcentration of electrochemically generated hydrides. This configuration minimizes transfer lines and connections. A thin-layer of electrochemical flow through cell was constructed. Lead and platinum foils were employed as cathode and anode materials, respectively. Experimental operation conditions for hydride generation as well as the collection and revolatilization conditions for the generated hydrides in the inlet arm of the quartz tube atomizer were optimized. Interferences of copper, nickel, iron, cobalt, arsenic, selenium, lead and tin were examined both with and without the trap. 3σ limit of detection was estimated as 0.053 μg l -1 for a sample size of 6.0 ml collected in 120 s. The trap has provided 18 fold sensitivity improvement as compared to electrochemical hydride generation alone. The accuracy of the proposed technique was evaluated with two standard reference materials; Trace Metals in Drinking Water, Cat CRM-TMDW and Metals on Soil/Sediment 4, IRM-008

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

    CERN Document Server

    Verma, H R

    2007-01-01

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

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

    International Nuclear Information System (INIS)

    Khater, Antoine; Szczesniak, Dominik

    2011-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-04-01

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

  5. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Smith, D.H. (ed.)

    1978-11-01

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

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

    International Nuclear Information System (INIS)

    Smith, D.H.

    1978-11-01

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

  8. Lead determination at ng/mL level by flame atomic absorption spectrometry using a tantalum coated slotted quartz tube atom trap.

    Science.gov (United States)

    Demirtaş, İlknur; Bakırdere, Sezgin; Ataman, O Yavuz

    2015-06-01

    Flame atomic absorption spectrometry (FAAS) still keeps its importance despite the relatively low sensitivity; because it is a simple and economical technique for determination of metals. In recent years, atom traps have been developed to increase the sensitivity of FAAS. Although the detection limit of FAAS is only at the level of µg/mL, with the use of atom traps it can reach to ng/mL. Slotted quartz tube (SQT) is one of the atom traps used to improve sensitivity. In atom trapping mode of SQT, analyte is trapped on-line in SQT for few minutes using ordinary sample aspiration, followed by the introduction of a small volume of organic solvent to effect the revolatilization and atomization of analyte species resulting in a transient signal. This system is economical, commercially available and easy to use. In this study, a sensitive analytical method was developed for the determination of lead with the help of SQT atom trapping flame atomization (SQT-AT-FAAS). 574 Fold sensitivity enhancement was obtained at a sample suction rate of 3.9 mL/min for 5.0 min trapping period with respect to FAAS. Organic solvent was selected as 40 µL of methyl isobutyl ketone (MIBK). To obtain a further sensitivity enhancement inner surface of SQT was coated with several transition metals. The best sensitivity enhancement, 1650 fold enhancement, was obtained by the Ta-coated SQT-AT-FAAS. In addition, chemical nature of Pb species trapped on quartz and Ta surface, and the chemical nature of Ta on quartz surface were investigated by X-ray photoelectron spectroscopy (XPS) and Raman Spectroscopy. Raman spectrometric results indicate that tantalum is coated on SQT surface in the form of Ta2O5. XPS studies revealed that the oxidation state of Pb in species trapped on both bare and Ta coated SQT surfaces is +2. For the accuracy check, the analyses of standard reference material were performed by use of SCP SCIENCE EnviroMAT Low (EU-L-2) and results for Pb were to be in good agreement with

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

    Energy Technology Data Exchange (ETDEWEB)

    Bings, N.H., E-mail: bings@uni-mainz.de; Orlandini von Niessen, J.O.; Schaper, J.N.

    2014-10-01

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

  10. New analytical tools combining gel electrophoresis and mass spectrometry

    OpenAIRE

    Tobolkina, Elena

    2014-01-01

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

  11. Accuracy and Precision in Elemental Analysis of Environmental Samples using Inductively Coupled Plasma-Atomic Emission Spectrometry

    International Nuclear Information System (INIS)

    Quraishi, Shamsad Begum; Chung, Yong-Sam; Choi, Kwang Soon

    2005-01-01

    Inductively Coupled Plasma-Atomic Emission Spectrometry followed by micro-wave digestion have been performed on different environmental Certified Reference Materials (CRMs). Analytical results show that accuracy and precision in ICP-AES analysis were acceptable and satisfactory in case of soil and hair CRM samples. The relative error of most of the elements in these two CRMs is within 10% with few exceptions and coefficient of variation is also less than 10%. Z-score as an analytical performance was also within the acceptable range (±2). ICP-AES was found as an inadequate method for Air Filter CRM due to incomplete dissolution, low concentration of elements and very low mass of the sample. However, real air filter sample could have been analyzed with high accuracy and precision by increasing sample mass during collection. (author)

  12. 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)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-12-04

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

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

    Science.gov (United States)

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

    2009-04-15

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

  15. Determination of some metal ions in various meat and baby food samples by atomic spectrometry.

    Science.gov (United States)

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

    2016-04-15

    In this paper, we report a simple and rapid solid phase extraction system for the separation/preconcentration and determination of Cd(II), Co(II), Cu(II), Fe(III), Cr(III), Pb(II), and Zn(II) ions by flame atomic absorption spectrometry (FAAS). This method is based upon the retention of metal ions on a column packed with poly[N-(3-methyl-1H-indole-1-yl)]-2-methacrylamide-co-2-acrylamido-2-methyl-1-propane sulphonic acid-co divinylbenzene] (MMAD) resin as a solid-phase extraction (SPE) sorbent at pH 8. At the optimized conditions, the limits of detection (3 s/b) between 0.12 and 1.6 μg L(-1), preconcentration factor of 100, and the relative standard deviation of ⩽1.8% were achieved (n=10). The accuracy of the method was verified by analyzing certified reference materials (CRMs) and performing recovery experiments. The developed method was successfully applied to the various natural water, meat products and baby food samples. The recoveries of analyte ions were found in added real samples and CRMs from 95% to 102%. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-05-10

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

  17. [Research on optimization of mathematical model of flow injection-hydride generation-atomic fluorescence spectrometry].

    Science.gov (United States)

    Cui, Jian; Zhao, Xue-Hong; Wang, Yan; Xiao, Ya-Bing; Jiang, Xue-Hui; Dai, Li

    2014-01-01

    Flow injection-hydride generation-atomic fluorescence spectrometry was a widely used method in the industries of health, environmental, geological and metallurgical fields for the merit of high sensitivity, wide measurement range and fast analytical speed. However, optimization of this method was too difficult as there exist so many parameters affecting the sensitivity and broadening. Generally, the optimal conditions were sought through several experiments. The present paper proposed a mathematical model between the parameters and sensitivity/broadening coefficients using the law of conservation of mass according to the characteristics of hydride chemical reaction and the composition of the system, which was proved to be accurate as comparing the theoretical simulation and experimental results through the test of arsanilic acid standard solution. Finally, this paper has put a relation map between the parameters and sensitivity/broadening coefficients, and summarized that GLS volume, carrier solution flow rate and sample loop volume were the most factors affecting sensitivity and broadening coefficients. Optimizing these three factors with this relation map, the relative sensitivity was advanced by 2.9 times and relative broadening was reduced by 0.76 times. This model can provide a theoretical guidance for the optimization of the experimental conditions.

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

    Science.gov (United States)

    Kusch, Peter

    2014-01-01

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

  19. Methods of calibration in the direct analysis of solid samples by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Berglund, M.; Baxter, D. C.

    1992-12-01

    One of the major problems involved in the direct analysis of solid samples by electrothermal atomic absorption spectrometry (ETAAS) lies in the calibration step because non-spectral interference effects are often pronounced. Three standardization techniques have been described and used in solid sampling-ETAAS: (i) standard additions method; (ii) calibration relative to a certified reference material; and (iii) calibration curve technique. However, an adequate statistical evaluation of the uncertainty in the analyte concentration in the solid sample is most frequently neglected, and reported errors may be seriously underestimated. This can be attributed directly to the complexity of the statistical expressions required to accurately account for errors in each of the calibration techniques mentioned above, and the general lack of relevant reference literature. The object of this work has been to develop a computer package which will perform the necessary statistical analyses of solid sampling-ETAAS data; the result is the program "SOLIDS" described here in the form of an electronic publication in Spectrochimica Acta Electronica, the electronic section of Spectrochimica Acta Part B. The program could also be useful in other analytical fields where similar calibration methods are used. The hard copy text, outlining the calibration models and their associated errors, is accompanied by a diskette containing the program, some data files, and a manual. Use of the program is exemplified in the text, with some of the data files discussed included on the diskette which, together with the manual, should enable the reader to become familiarized with the operation of the program, and the results generated.

  20. determination of vanadium in foods by atomic absorption spectrometry

    African Journals Online (AJOL)

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

  1. Analytical signal normalization in laser-enhanced ionization spectrometry with laser ablation of solid samples into a flame

    International Nuclear Information System (INIS)

    Labutin, T.A.; Popov, A.M.; Gorbatenko, A.A.; Zorov, N.B.

    2005-01-01

    The characteristics of analytical and reference signals (RS) were studied in laser-enhanced ionization (LEI) spectrometry combined with laser ablation of solid samples into a flame. Optoacoustic (OA) and atomic emission (AE) signals have been considered as possible RS. An algorithm of RS selection has been developed. Correlations between LEI signals and RS, which carry information on sample evaporation processes, have been explored. OA (the 1st minimum) and AE (AlI, λ = 396.1 nm) signals were found to be useful as RS (the correlation coefficients were 0.992 and 0.993, respectively). Both RS did not depend on the analyte (Li) content in the sample. It has been shown that the slope of the correlation plots (LEI vs. RS) depends on the Li content in the solid sample. This slope may be used as a novel type of normalized analytical signal, which does not depend on the ablation pulse energy. The influence of both ablating laser radiation characteristics and sample matrix composition on the analytical signal is eliminated (or at least diminished) when using this normalization

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

    International Nuclear Information System (INIS)

    Garcia, M.; Sardinas, O.; Castaneda, I.; Sanchez, R.

    1990-01-01

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

  3. 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

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

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Dědina, Jiří

    2015-01-01

    Roč. 108, JUN (2015), s. 61-67 ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant - others:GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : silver * volatile species generation * sapphire tube atomizer Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.289, year: 2015

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

    DEFF Research Database (Denmark)

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

    1996-01-01

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

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

    International Nuclear Information System (INIS)

    Ferrua, N.; Cerutti, S.; Salonia, J.A.; Olsina, R.A.; Martinez, L.D.

    2007-01-01

    An on-line procedure for the determination of traces of total mercury in environmental and biological samples is described. The present methodology combines cold vapor generation associated to atomic absorption spectrometry (CV-AAS) with preconcentration of the analyte on a minicolumn packed with activated carbon. The retained analyte was quantitatively eluted from the minicolumn with nitric acid. After that, volatile specie of mercury was generated by merging the acidified sample and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the atomizer device. Optimizations of both, preconcentration and mercury volatile specie generation variables were carried out using two level full factorial design (2 3 ) with 3 replicates of the central point. Considering a sample consumption of 25 mL, an enrichment factor of 13-fold was obtained. The detection limit (3σ) was 10 ng L -1 and the precision (relative standard deviation) was 3.1% (n = 10) at the 5 μg L -1 level. The calibration curve using the preconcentration system for mercury was linear with a correlation coefficient of 0.9995 at levels near the detection limit up to at least 1000 μg L -1 . Satisfactory results were obtained for the analysis of mercury in tap water and hair samples

  7. Analytical model for relativistic corrections to the nuclear magnetic shielding constant in atoms

    International Nuclear Information System (INIS)

    Romero, Rodolfo H.; Gomez, Sergio S.

    2006-01-01

    We present a simple analytical model for calculating and rationalizing the main relativistic corrections to the nuclear magnetic shielding constant in atoms. It provides good estimates for those corrections and their trends, in reasonable agreement with accurate four-component calculations and perturbation methods. The origin of the effects in deep core atomic orbitals is manifestly shown

  8. Analytical model for relativistic corrections to the nuclear magnetic shielding constant in atoms

    Energy Technology Data Exchange (ETDEWEB)

    Romero, Rodolfo H. [Facultad de Ciencias Exactas, Universidad Nacional del Nordeste, Avenida Libertad 5500 (3400), Corrientes (Argentina)]. E-mail: rhromero@exa.unne.edu.ar; Gomez, Sergio S. [Facultad de Ciencias Exactas, Universidad Nacional del Nordeste, Avenida Libertad 5500 (3400), Corrientes (Argentina)

    2006-04-24

    We present a simple analytical model for calculating and rationalizing the main relativistic corrections to the nuclear magnetic shielding constant in atoms. It provides good estimates for those corrections and their trends, in reasonable agreement with accurate four-component calculations and perturbation methods. The origin of the effects in deep core atomic orbitals is manifestly shown.

  9. Determination of heavy metals in polar snow and ice by laser-excited atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Bolshov, M.A.; Boutron, C.F.

    1994-01-01

    The new laser-excited atomic fluorescence spectrometry technique offers unrivalled sensitivity for the determination of trace metals in a wide variety of samples. This has allowed the direct determination of Pb, Cd and Bi in Antarctic and Greenland snow and ice down to the sub pg/g level. (authors). 11 refs., 2 figs

  10. [Determination of chloride ion in additives of concrete by flame atomic absorption spectrometry].

    Science.gov (United States)

    Xiong, Min; Shan, Yun

    2003-06-01

    Flame atomic absorption spectrometry due to its high sensitivity and selectivity has been widely used for the determination of micro levels of metal elements in various materials. But this method can not be used for the determination of Cl- directly. In this paper the determination of Cl- in additives of concrete by flame atomic absorption spectrometry was studied. Adding superfluous standard solution of Ag+ to the sample solution, the results were obtained by determining the remanent content of Ag+ having reacted with Cl- quantitatively. The acidity of the sample solution and the precision were studied. The standard rate of recovery obtained was in the range of 96%-104%. By the determination of actual samples it was proved that the method features simple sample preparation, fast determination, and little interference, especially for those samples which contain micro levels of Cl-. The procedure is as follows: weight 0.05-2 g of sample, dissolve it in water and adjust the acidity with nitric acid, add proper standard solution of Ag+, and after 2 h, measure the remanent Ag+ content by atomic absorption spectrometry. A GBC902 atomic absorption spectrometry was employed.

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

    NARCIS (Netherlands)

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

    1979-01-01

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

  12. 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...

  13. 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...

  14. Redox speciation analysis of antimony in soil extracts by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Fuentes, Edwar; Pinochet, Hugo; Gregori, Ida de E-mail: idegrego@ucv.cl; Potin-Gautier, Martine

    2003-07-18

    A sensitive atomic spectrometric method for the redox speciation analysis of antimony in soils is described. The method is based on the selective generation of stibine from Sb(III) in a continuous flow system using atomic fluorescence spectrometry for detection. Sb(V) is masked by citric or oxalic acid in HCl medium. The procedure was optimized with synthetic solutions of Sb(III) and Sb(V). The effect of carboxylic acid and HCl concentration on the recovery of Sb(III) and Sb(V) species from standard solutions, and on the fluorescence signal were studied. Both species were extracted from soil with H{sub 2}O, 0.05 mol l{sup -1} EDTA and 0.25 mol l{sup -1} H{sub 2}SO{sub 4}. Since the soil samples were collected from sites impacted by copper mining activities, the effect of Cu{sup 2+} on the determination of antimony in synthetic solutions and soil extracts was studied. Cu{sup 2+} decreased the Sb(III) signal, but had no effect on the total antimony determination. Therefore, the selective determination of Sb(III) was carried out in citric acid-HCl medium, using the analyte addition technique. Total antimony in soil extracts was determined using the standard calibration technique after reducing Sb(V) to Sb(III) at room temperature with KI-ascorbic acid. The Sb(V) concentration was calculated from the difference between total antimony and Sb(III). The limits of detection (PS Analytical, Excalibur Millennium model) were 17 and 10 ng l{sup -1} for Sb(III) and total antimony, respectively, and the R.S.D. at the 0.5-{mu}g l{sup -1} level were 2.5 and 2.4%, respectively. The total antimony concentration of soils is in the mg kg{sup -1} range; the Sb recovery from the different soils by the extracting solutions was between less than 0.02% and approximately 10%. Similar recoveries were obtained using EDTA and sulfuric acid solutions. Sb(V) was found to be the main antimony species extracted from soils.

  15. New experiments in organic, fast-atom-bomdardment, and secondary-ion mass spectrometry

    International Nuclear Information System (INIS)

    DiDonato, G.C.

    1987-01-01

    The goal of research presented in this dissertation is the creative use of new ionization and instrumental techniques in mass spectrometry. This goal manifests itself in three areas of mass spectrometry. In the first portion, modern, state-of-the-art instrumentation and new experiments were used to re-examine the mass spectra of transition-metal acetates and acetylacetonates. High resolution, chemical ionization, negative chemical ionization, and extended-mass-range mass spectrometry uncovered a wealth of new gas-phase ionic species. Energy-resolved mass spectrometry/mass spectrometry was applied to the characterization of molecular and fragment ion first-row transition-metal acetylacetonates, and comprises the second portion of the thesis. Studies in fast-atom-bombardment mass spectrometry are the subject of the third portion of the dissertation. Since fast-atom bombardment samples a liquid matrix, absolute and relative abundances of sputtered secondary ions are influenced by solution chemistry. The design and construction of an imaging secondary-ion mass spectrometer is the subject of the final portion of the thesis. This instrument provides for direct mass-spectrometric analysis of thin-layer and paper chromatograms and electrophoretograms

  16. 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

  17. Determination of mercury and selenium in herbal medicines and hair by using a nanometer TiO2-coated quartz tube atomizer and hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Li, Shun-Xing; Zheng, Feng-Ying; Cai, Shu-Jie; Cai, Tian-Shou

    2011-01-01

    The nanometer TiO 2 particle was coated onto the inner wall of a T-shaped quartz tube atomizer (QTA) and then was used as a new atomizer (NT-QTA) for the determination of Hg and Se by hydride generation atomic absorption spectrometry (HGAAS). After coating 67.4 mg TiO 2 on a quartz tube, the analytical performance of NT-QTA-HGAAS was compared to conventional QTA-HGAAS and it was improved as follows: (a) the linear range of the calibration curves was expanded from 10.0-80.0 ng mL -1 to 5.0-150.0 ng mL -1 for Hg, and from 10.0-70.0 ng mL -1 to 5.0-100.0 ng mL -1 for Se; (b) the characteristic concentration of was decreased from 2.8 ng mL -1 /1% to 1.1 ng mL -1 /1% for Hg and from 1.2 ng mL -1 /1% to 0.8 ng mL -1 /1% for Se; and (c) the interference from the coexistence of As on the determination of Hg and Se could be eliminated. The achieved technique was applied for the determination of Hg and Se in herbal medicines and hair.

  18. Atomic spectrometry and trends in clinical laboratory medicine

    International Nuclear Information System (INIS)

    Parsons, Patrick J.; Barbosa, Fernando

    2007-01-01

    Increasing numbers of clinical laboratories are transitioning away from flame and electrothermal AAS methods to those based on ICP-MS. Still, for many laboratories, the choice of instrumentation is based upon (a) the element(s) to be determined, (b) the matrix/matrices to be analyzed, and (c) the expected concentration(s) of the analytes in the matrix. Most clinical laboratories specialize in measuring Se, Zn, Cu, and Al in serum, and/or Pb, Cd, Hg, As, and Cr in blood and/or urine, while other trace elements (e.g., Pt, Au etc.) are measured for therapeutic purposes. Quantitative measurement of elemental species is becoming more widely accepted for nutritional and/or toxicological screening purposes, and ICP-MS interfaced with separation techniques, such as liquid chromatography or capillary electrophoresis, offers the advantage of on-line species determination coupled with very low detection limits. Polyatomic interferences for some key elements such as Se, As, and Cr require instrumentation equipped with dynamic reaction cell or collision cell technologies, or might even necessitate the use of sector field ICP-MS, to assure accurate results. Nonetheless, whatever analytical method is selected for the task, careful consideration must be given both to specimen collection procedures and to the control of pre-analytical variables. Finally, all methods benefit from access to reliable certified reference materials (CRMs). While a variety of reference materials (RMs) are available for trace element measurements in clinical matrices, not all can be classified as CRMs. The major metrological organizations (e.g., NIST, IRMM, NIES) provide a limited number of clinical CRMs, however, secondary reference materials are readily available from commercial organizations and organizers of external quality assessment schemes

  19. Investigation of interference mechanisms of nickel chloride on copper determination and of colloidal palladium as modifier in electrothermal atomic absorption spectrometry using a dual cavity platform

    Energy Technology Data Exchange (ETDEWEB)

    Akman, Suleyman [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, Maslak-Istanbul (Turkey); Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis-SC (Brazil)]. E-mail: welz@qmc.ufsc.br; Tokman, Nilgun [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, Maslak-Istanbul (Turkey)

    2005-10-01

    The interference of nickel chloride on the determination of copper by electrothermal atomic absorption spectrometry was investigated using a specially designed dual cavity platform (DCP), which allows the analyte and interferent to vaporize from separate cavities, so that gas and condensed phase interferences can be distinguished to some extent. It was found that, when low pyrolysis temperatures were used, the interference of nickel chloride on copper originated from the formation of copper chloride in the condensed phase, which is not efficiently dissociated in the atomization stage. Alternately, when analyte and interferent were in separate cavities of the DCP, a gas-phase reaction between copper and chlorine in the atomization stage resulted in a similar signal depression. When higher pyrolysis temperatures were used, interference could be attributed to losses of volatile copper chloride in the pyrolysis stage. These losses were more pronounced when analyte and interferent were in separate cavities of the DCP, indicating again a gas-phase reaction between copper and chlorine, as well as a protective action of nickel oxide, when analyte and interferent were mixed. Colloidal palladium used as modifier removed the chloride interference independent of the pyrolysis temperature applied, when copper and nickel chloride were mixed. Colloidal palladium also increased the integrated absorbance for copper by 40-50%, even when analyte and modifier were in separate cavities of the DCP, indicating a strong gas-phase interaction between copper atoms and the modifier through adsorption/desorption processes.

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

    Directory of Open Access Journals (Sweden)

    Liliane Catone Soares

    2015-08-01

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

  1. Spatially resolved measurements to improve analytical performance of solution-cathode glow discharge optical-emission spectrometry

    Science.gov (United States)

    Schwartz, Andrew J.; Ray, Steven J.; Chan, George C.-Y.; Hieftje, Gary M.

    2016-11-01

    Past studies of the solution-cathode glow discharge (SCGD) revealed that elemental and molecular emission are not spatially homogenous throughout the source, but rather conform to specific zones within the discharge. Exploiting this inhomogeneity can lead to improved analytical performance if emission is collected only from regions of the discharge where analyte species emit strongly and background emission (from continuum, elemental and/or molecular sources) is lower. Effects of this form of spatial discrimination on the analytical performance of SCGD optical emission spectrometry (OES) have been investigated with an imaging spectrograph for fourteen atomic lines, with emphasis on detection limits and precision. Vertical profiles of the emission intensity, signal-to-background ratio, and signal-to-noise ratio were collected and used to determine the optimal region to view the SCGD on a per-element basis. With optimized spatial filtering, detection limits ranged from 0.09-360 ppb, a 1.4-13.6 fold improvement over those obtained when emission is collected from the full vertical profile (1.1-840 ppb), with a 4.2-fold average improvement. Precision was found to be unaffected by spatial filtering, ranging from 0.5-2.6% relative standard deviation (RSD) for all elements investigated, closely comparable to the 0.4-2.4% RSD observed when no spatial filtering is used. Spatial profiles also appear useful for identifying optimal line pairs for internal standardization and for flagging the presence of matrix interferences in SCGD-OES.

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

    Directory of Open Access Journals (Sweden)

    Iracema Takase

    2002-12-01

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

  3. Evaluation of the analytic performance of laboratories: inter-laboratorial study of the spectroscopy of atomic absorption

    International Nuclear Information System (INIS)

    Wong Wong, S. M.

    1996-01-01

    The author made an inter-laboratorial study, with the participation of 18 national laboratories, that have spectrophotometer of atomic absorption. To evaluate the methods of analysis of lead, sodium, potasium, calcium, magnesium, zinc, copper, manganese, and iron, in the ambit of mg/l. The samples, distributed in four rounds to the laboratories, were prepared from primary patterns, deionized and distilled water. The study evaluated the homogeneity and stability, and verified its concentration, using as a reference method, the spectrometry method of Inductively Coupled Plasma emission (1CP). To obtain the characteristics of analytic performance, it applied the norm ASTM E 691. To evaluated the analytic performance, it used harmonized protocol of the International Union of Pure and applied chemistry (IUPAC). The study obtained the 29% of the laboratories had a satisfactory analytic performance, 9% had a questionable performance and 62% made an unsatisfactory analytic performance, according to the IUPAC norm. The results of the values of the characteristic performance method, show that there is no intercomparability between the laboratories, which is attributed to the different methodologies of analysis. (S. Grainger)

  4. Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging

    Science.gov (United States)

    Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

    2017-08-01

    Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed.

  5. Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging.

    Science.gov (United States)

    Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

    2017-08-01

    Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed. Graphical Abstract ᅟ.

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

    Science.gov (United States)

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

    2008-09-15

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

  7. 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)

  8. 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)

  9. 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...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-12-01

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

  11. Hydride generation - in-atomizer collection of Pb in quartz tube atomizers for atomic absorption spectrometry – a 212Pb radiotracer study

    Czech Academy of Sciences Publication Activity Database

    Kratzer, Jan; Musil, Stanislav; Vobecký, Miloslav; Dědina, Jiří

    2013-01-01

    Roč. 28, č. 3 (2013), s. 344-353 ISSN 0267-9477 R&D Projects: GA ČR(CZ) GPP206/11/P002 Institutional support: RVO:68081715 Keywords : trap-and-atomizer device * lead determination * radiotracer study Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.396, year: 2013

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

    Energy Technology Data Exchange (ETDEWEB)

    Ho, Koon-Sing; Lui, Kwok-On; Lee, Kin-Ho; Chan, Wing-Tat, E-mail: wtchan@hku.hk

    2013-11-01

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

  13. 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...

  14. Selective Flow-Injection Quantification of Ultra-trace Amounts of Cr(VI) via On-line Complexation and Preconcentration with APDC Followed by Determination by Electrothermal Atomic Absorption Spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Hansen, Elo Harald

    1998-01-01

    is effected by adsorption on the inner wall of a knotted reactor made from PTFE tubing. The complex is subsequently eluted with a monosegmented discrete zone of ethanol (55 mu l), and the analyte is quantified by electrothermal atomic absorption spectrometry (ETAAS). The operations of the FI...

  15. Analytic cross sections for collisions of H, H2, He and Li Atoms and ions with atoms and molecules. 2

    International Nuclear Information System (INIS)

    Ito, Rinsuke; Tabata, Tatsuo; Shirai, Toshizo; Phaneuf, R.A.

    1994-07-01

    Analytic expressions fitted to Barnett's recommended data are given for the cross sections of excitation and spectral line emission by H, H + , He + , He, and He 2+ colliding with atoms and molecules. The expressions use the semiempirical functional forms proposed by Green and McNeal and some modified forms to make it possible not only to interpolate but also to extrapolate the recommended data. (author)

  16. Optimized determination of calcium in grape juice, wines, and other alcoholic beverages by atomic absorption spectrometry.

    Science.gov (United States)

    Olalla, Manuel; González, Maria Cruz; Cabrera, Carmen; Gimenez, Rafael; López, Maria Carmen

    2002-01-01

    This paper describes a study of the different methods of sample preparation for the determination of calcium in grape juice, wines, and other alcoholic beverages by flame atomic absorption spectrometry; results are also reported for the practical application of these methods to the analysis of commercial samples produced in Spain. The methods tested included dealcoholization, dry mineralization, and wet mineralization with heating by using different acids and/or mixtures of acids. The sensitivity, detection limit, accuracy, precision, and selectiviy of each method were established. Such research is necessary because of the better analytical indexes obtained after acid digestion of the sample, as recommended by the European Union, which advocates the direct method. In addition, although high-temperature mineralization with an HNO3-HCIO4 mixture gave the best analytical results, mineralization with nitric acid at 80 degrees C for 15 min gave the most satisfactory results in all cases, including those for wines with high levels of sugar and beverages with high alcoholic content. The results for table wines subjected to the latter treatment had an accuracy of 98.70-99.90%, a relative standard deviation of 2.46%, a detection limit of 19.0 microg/L, and a determination limit of 31.7 microg/L. The method was found to be sufficiently sensitive and selective. It was applied to the determination of Ca in grape juice, different types of wines, and beverages with high alcoholic content, all of which are produced and widely consumed in Spain. The values obtained for Ca were 90.00 +/- 20.40 mg/L in the grape juices, 82.30 +/- 23.80 mg/L in the white wines, 85.00 +/- 30.25 mg/L in the sweet wines, 84.92 +/- 23.11 mg/L in the red wines, 85.75 +/- 27.65 mg/L in the rosé wines, 9.51 +/- 6.65 mg/L in the brandies, 11.53 +/- 6.55 mg/L in the gin, 7.3 +/- 6.32 mg/L in the pacharán, and 8.41 +/- 4.85 mg/L in the anisettes. The method is therefore useful for routine analysis in the

  17. Comprehension of complex biological processes by analytical methods: how far can we go using mass spectrometry?

    International Nuclear Information System (INIS)

    Gerner, C.

    2013-01-01

    Comprehensive understanding of complex biological processes is the basis for many biomedical issues of great relevance for modern society including risk assessment, drug development, quality control of industrial products and many more. Screening methods provide means for investigating biological samples without research hypothesis. However, the first boom of analytical screening efforts has passed and we again need to ask whether and how to apply screening methods. Mass spectrometry is a modern tool with unrivalled analytical capacities. This applies to all relevant characteristics of analytical methods such as specificity, sensitivity, accuracy, multiplicity and diversity of applications. Indeed, mass spectrometry qualifies to deal with complexity. Chronic inflammation is a common feature of almost all relevant diseases challenging our modern society; these diseases are apparently highly diverse and include arteriosclerosis, cancer, back pain, neurodegenerative diseases, depression and other. The complexity of mechanisms regulating chronic inflammation is the reason for the practical challenge to deal with it. The presentation shall give an overview of capabilities and limitations of the application of this analytical tool to solve critical questions with great relevance for our society. (author)

  18. Measurements of sulfur compounds in CO 2 by diode laser atomic absorption spectrometry

    Science.gov (United States)

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

    2003-07-01

    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.

  19. An indirect method for determining phosphorus in aluminium alloys by atomic-absorption spectrometry.

    Science.gov (United States)

    Bernal, J L; Del Nozal, M A; Deban, L; Aller, A J

    1981-07-01

    An indirect method is described for the determination of phosphorus in aluminium alloys. Ammonium molybdate is added to a solution of the aluminium alloy and the molybdophosphoric acid formed is selectively extracted into n-butyl acetate. The twelve molybdenum atoms associated with each phosphate ion are determined by direct atomic-absorption spectrometry with the n-butyl acetate phase in a nitrous oxide-acetylene flame, with measurement at 313.2 nm. The most suitable conditions have been established and the effect of other ions has been studied.

  20. 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...

  1. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-04-15

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

  3. 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)

  4. Determination of diethyllead in the urine by flameless atomic absorption spectrometry.

    OpenAIRE

    Turlakiewicz, Z; Jakubowski, M; Chmielnicka, J

    1985-01-01

    A method for the determination of diethyllead in urine by flameless atomic absorption spectrometry after chelation with glyoxal-bis (2-hydroxyanil) and extraction of the formed complex with methyl isobutyl ketone is described. The method is specific in relation to both triethyllead and inorganic lead. The limit of detection was 3.2 micrograms Pb/l and the relative standard deviation in the concentration range 20-100 micrograms Pb/l was 0.076.

  5. Effect of chemical modification on behavior of various organic vanadium forms during analysis by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Kowalewska, Zofia

    2007-01-01

    The behavior of various organic V forms dissolved in xylene during analysis by electrothermal atomic absorption spectrometry (ETAAS) was compared. The investigated analyte forms included compounds with vanadium at the oxidation state III, IV or V, as well as N, O or S atoms in molecules. Another group consisted of petroleum products containing naturally-occurring V species. Although the characteristic mass determined under different analytical conditions was in the very wide range from 11 up to 55 pg, some rules of V behavior were found. In the case of porphyrins and petroleum products, the application of Pd as a chemical modifier (xylene solution of Pd(II) acetylacetonate) seemed to be crucial. It was shown that Pd must be introduced to a furnace together with a sample. Pd injected and thermally pretreated before the sample injection was less effective for porphyrins and the petroleum products, but it increased signals of V compounds containing O as donor atom. The iodine pretreatment followed by the methyltrioctylammonium chloride (MTOACl) pretreatment was advantageous for these V forms. The air ashing in a graphite tube appeared to be important to improve decomposition of the petroleum products. No significant influence of the V oxidation state on the analytical signal was observed. The behavior of V contained in two Conostan oil standards, the single-element and the S21 multielement standard, was different in many situations. Probably, the joint action of other elements is responsible for this effect. In general, chemical modification was applied in the work for two reasons: to reduce the V volatility (in some cases losses at about 300 deg. C were observed) and to enhance the atomization efficiency. For routine analysis air ashing, modification by Pd introduced into the furnace together with the sample solution and petroleum products with known V content as standard is recommended. Using this procedure the characteristic mass varied from 16 to 19 pg for

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

    Czech Academy of Sciences Publication Activity Database

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-01-01

    Roč. 88, č. 11 (2016), s. 6064-6070 ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation * arsenic preconcentration Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 6.320, year: 2016

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

    Czech Academy of Sciences Publication Activity Database

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-01-01

    Roč. 88, č. 11 (2016), s. 6064-6070 ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation * arsenic preconcentration Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 6.320, year: 2016

  8. Using matrix effects as a probe for the study of the charge-transfer mechanism in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

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

    2004-01-01

    A novel method is presented for using matrix effects as a probe for the charge-transfer reaction between analyte atoms and argon ions in inductively coupled plasma-atomic emission spectrometry (ICP-AES). The method is based on the fact that the matrix effect caused by Ca or Ba depends on whether the studied analyte spectral line is from an ion or a neutral atom. Because the charge transfer reaction directly links atomic and high-energy ionic levels of the analyte, ionic spectral lines excited by charge transfer behave more like neutral-atom emission. As a result, quasi-resonant ionic emission lines exhibit a unique matrix effect character and can be easily identified. A commercial simultaneous full UV-Vis wavelength-coverage ICP spectrometer was used to study the responses of a large pool of spectral lines from a total of 22 elements in the presence of Na, Ca and Ba matrices. Candidate elements with charge-transfer character were thereby identified. The results match closely with those reported in the literature. The technique was further used to study charge-transfer reactions exhibited by the fourth-row metals from Sr to Sb. With the exception of Cd, Sr and Mo, all the other studied fourth-row metals showed positive evidence of excitation and ionization by charge-transfer from argon ion. While Sr showed negative results, the charge transfer-character of Cd and Mo could not be confirmed. It was also found that charge transfer can originate from other low-lying atomic analyte levels, in addition to the atomic ground state, and that charge-transfer reactions can occur at an appreciable rate even with a negative energy defect (i.e. negative ΔE) up to -1.6 eV

  9. 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)

  10. 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.

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

    International Nuclear Information System (INIS)

    Dancsak, Stacia E.; Silva, Sidnei G.; Nóbrega, Joaquim A.; Jones, Bradley T.; Donati, George L.

    2014-01-01

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

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

    DEFF Research Database (Denmark)

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

    1996-01-01

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

  13. Mechanism of yttrium atom formation in electrothermal atomization from metallic and metal-carbide surfaces of a heated graphite atomizer in atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Wahab, H.S.; Chakrabarti, C.L.

    1981-01-01

    Mechanism of Y atom formation from pyrocoated graphite, tantalum and tungsten metal surfaces of a graphite tube atomizer has been studied and a mechanism for the formation for Y atoms is proposed for the first time. (author)

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

    Directory of Open Access Journals (Sweden)

    Heung-Ryoul Noh

    2016-03-01

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

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

    Directory of Open Access Journals (Sweden)

    Yan-Zi Yu

    2015-01-01

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

  16. The behavior of various chemical forms of nickel in graphite furnace atomic absorption spectrometry under different chemical modification approaches

    International Nuclear Information System (INIS)

    Kowalewska, Zofia

    2012-01-01

    Various organic and inorganic Ni forms were investigated using graphite furnace atomic absorption spectrometry. Experiments without chemical modification showed a wide range of characteristic mass values for Ni (from 6.7 to 29 pg) and the importance of interaction with graphite. With the aim of achieving signal unification of organic Ni forms, different ways of chemical modification were tested. Some rules that govern the behavior of Ni were found and confirmed a significant role of the organic component of the analyte molecule in the analytical process. The application of air as an internal furnace gas in the pyrolysis phase and the Pd modifier injected with the sample solution improved the signal of porphyrins, while the application of iodine and methyltrioctylammonium chloride was required for organic compounds containing oxygen-bound Ni atoms. The Ni signal was strongly diminished when an aqueous solution containing hydrochloric acid was measured with the Pd modifier injected over the sample. Using the developed analytical methods, the range of characteristic mass values for various Ni forms totally dissolved in organic or aqueous solution was 6.5–7.9 pg. - Highlights: ► Some rules that govern behavior of organic Ni forms during GFAAS analysis were found. ► Interaction with graphite can significantly influence evaporation of porphyrins. ► Determination of Ni in form of porphyrins needs Pd organic modifier and air ashing. ► Determination of Ni in O-bound organic compounds needs pretreatment with I2+MTOACl. ► Chemical modification for GFAAS determination of Ni in HCl-containing solution.

  17. New analytical treatment for a kind of two dimensional integrals in ion-atom collisions

    International Nuclear Information System (INIS)

    Yang Qifeng; Kuang Yurang

    1994-01-01

    A kind of two-dimensional integrals, separated from two-center matrix elements in ion-atom collisions, is analytically integrated by introducing the Laplace transform into the integrals and expressed by the modified Bessel functions. The traditional Feynman transform is very complicated for this kind of more general integrals related to the excited state capture

  18. 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.

  19. Imaging time-resolved electrothermal atomization laser-excited atomic fluorescence spectrometry for determination of mercury in seawater.

    Science.gov (United States)

    Le Bihan, Alain; Cabon, Jean-Yves; Deschamps, Laure; Giamarchi, Philippe

    2011-06-15

    In this study, direct determination of mercury at the nanogram per liter level in the complex seawater matrix by imaging time-resolved electrothermal atomization laser-excited atomic fluorescence spectrometry (ITR-ETA-LEAFS) is described. In the case of mercury, the use of a nonresonant line for fluorescence detection with only one laser excitation is not possible. For measurements at the 253.652 nm resonant line, scattering phenomena have been minimized by eliminating the simultaneous vaporization of salts and by using temporal resolution and the imaging mode of the camera. Electrothermal conditions (0.1 M oxalic acid as matrix modifier, low atomization temperature) have been optimized in order to suppress chemical interferences and to obtain a good separation of specific signal and seawater background signal. For ETA-LEAFS, a specific response has been obtained for Hg with the use of time resolution. Moreover, an important improvement of the detection limit has been obtained by selecting, from the furnace image, pixels collecting the lowest number of scattered photons. Using optimal experimental conditions, a detection limit of 10 ng L(-1) for 10 μL of sample, close to the lowest concentration level of total Hg in the open ocean, has been obtained.

  20. Systematics of multielement determination with resonance ionization mass spectrometry and thermal atomization

    International Nuclear Information System (INIS)

    Moore, L.J.; Fassett, J.D.; Travis, J.C.

    1984-01-01

    The systematics for multielement determination using resonance ionization mass spectrometry and thermal atomization is developed. The aspects of atomization, ionization, and detection are discussed and resonance ionization is demonstrated for 19 elements. The selective, sequential ionization of seven elements from a single sample is also demonstrated. A one-wavelength, two-photon ionization scheme generally is used in which the first photon excites a bound transition in the near-ultraviolet region and second photon promotes the electron into theionization continuum. The wavelength-dependence ion formation from the thermally produced atom reservoirs is demonstrated for these elements by scanning a Nd:YAG-pumped dye laser across its tunable wavelength range. The observed wavelengths where ionization occurs have been correlated where possible with allowed transitions between known electronic energy levels. The elements accessible by using four common dyes are tabulated. More than 20 elements are accessible within the wavelength range of each dye

  1. Determination of cadmium in coal by metal furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Fudagawa, Noriko; Kawase, Akira

    1985-01-01

    Conditions for determination of cadmium in coal were investigated by atomic absorption spectrometry using a boat-shape tungsten furnace. For concentrating and separating cadmium from the coexisting components cadmium dithizonate-m-xylene solution and the 0.05 mol/l perchloric acid solution were examined. Ashing and atomizing temperatures, sheath gas composition, distribution of the cadmium atoms in the furnace were examined. Similar characteristics were obtained for the determination of cadmium in perchloric acid solution and the chelate m-xylene solution, except that a reduction of the peak time and FWHM (full width at half maximum) was observed for the latter solution. When the atomization temperature is near 2300 deg C, the change in the magnitude of absorbance is small in terms of the temperature. The influence of hydrogen contained in the sheath gas was complicated: Change in the thermal conductivity with increasing hydrogen content, resulted decrease of the atomization temperature but the integrated absorbance did not change so much. The concentration of cadmium atoms decreased linearily in the vertical direction of the furnace, while absorbance in the horizontal direction was almost constant. Cadmium in coal was determined by the methods (1) solvent extraction, (2) back-extraction with perchloric acid, (3) on-boat standard addition method. (author)

  2. Semi-analytical wave functions in relativistic average atom model for high-temperature plasmas

    International Nuclear Information System (INIS)

    Guo Yonghui; Duan Yaoyong; Kuai Bin

    2007-01-01

    The semi-analytical method is utilized for solving a relativistic average atom model for high-temperature plasmas. Semi-analytical wave function and the corresponding energy eigenvalue, containing only a numerical factor, are obtained by fitting the potential function in the average atom into hydrogen-like one. The full equations for the model are enumerated, and more attentions are paid upon the detailed procedures including the numerical techniques and computer code design. When the temperature of plasmas is comparatively high, the semi-analytical results agree quite well with those obtained by using a full numerical method for the same model and with those calculated by just a little different physical models, and the result's accuracy and computation efficiency are worthy of note. The drawbacks for this model are also analyzed. (authors)

  3. Lead concentrations and isotope ratios in street dust determined by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Nageotte, S M; Day, J P

    1998-01-01

    A major source of environmental lead, particularly in urban areas, has been from the combustion of leaded petrol. Street dust has previously been used to assess urban lead contamination, and the dust itself can also be a potential source of lead ingestion, particularly to children. The progressive reduction of lead in petrol, in recent years, would be expected to have been reflected in a reduction of lead in urban dust. We have tested this hypothesis by repeating an earlier survey of Manchester street dust and carrying out a comparable survey in Paris. Samples were collected from streets and parks, lead was extracted by digestion with concentrated nitric acid and determined by electrothermal atomic absorption spectrometry. Lead isotope ratios were measured by inductively coupled plasma mass spectrometry. Results for Manchester show that lead concentrations have fallen by about 40% (street dust averages, 941 micrograms g-1 (ppm) in 1975 down to 569 ppm in 1997). In Paris, the lead levels in street dust are much higher and significant differences were observed between types of street (not seen in Manchester). Additionally, lead levels in parks were much lower than in Manchester. Samples collected under the Eiffel Tower had very high concentrations and lead isotope ratios showed that this was unlikely to be fallout from motor vehicles but could be due to the paint used on the tower. Isotope ratios measurements also revealed that lead additives used in France and the UK come from different sources.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-03-15

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

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

    Science.gov (United States)

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

    2007-03-01

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

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

    Science.gov (United States)

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

    2016-01-15

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

  7. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina por espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method’s performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 ± 11,70)μg.L{sup -1} with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10μg.L{sup −1}. The obtained

  8. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina para espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method's performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 +- 11,70)mug.L{sup -1} with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10{mu}g.L{sup -1}. The

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

    International Nuclear Information System (INIS)

    Oliveira, Silvana R.; Gomes Neto, Jose A.; Nobrega, Joaquim A.; Jones, Bradley T.

    2010-01-01

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

  10. Determination of lead in flour samples directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Tinas, Hande; Ozbek, Nil; Akman, Suleyman

    2018-02-01

    In this study, lead concentrations in various flour samples were determined by high-resolution continuum source graphite furnace atomic absorption spectrometry with solid sampling. Since samples were analyzed directly, the risks and disadvantages of sample digestion were eliminated. Solid flour samples were dried, weighed on the platforms, Pd was added as a modifier and introduced directly into a graphite tube using a manual solid sampler. Platforms and tubes were coated with Zr. The optimized pyrolysis and atomization temperatures were 800 °C and 2200 °C, respectively. The sensitivities of lead in various flour certified reference materials (CRMs) and aqueous standards were not significantly different. Therefore, aqueous standards were safely used for calibration. The absolute limit of detection and characteristic mass were 7.2 pg and 9.0 pg of lead, respectively. The lead concentrations in different types of flour samples were found in the range of 25-52 μg kg- 1. Finally, homogeneity factors representing the heterogeneity of analyte distribution for lead in flour samples were determined.

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

    Science.gov (United States)

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

    2016-08-01

    Monitoring total bromine and bromide concentrations in soils is significant in many environmental studies. Thus fast analytical methodologies that entail simple sample preparation and low-cost analyses are desired. In the present work, the possibilities and drawbacks of low-power total reflection X-ray fluorescence spectrometry (TXRF) for the determination of total bromine and bromide contents in soils were evaluated. The direct analysis of a solid suspension using 20 mg of fine ground soil (TXRF analysis can be directly performed by depositing 10 μL of the internal standardized soil extract sample on a quartz glass reflector in a measuring time of 1500 s. The bromide limit of detection by this approach was 10 μg L(-1). Good agreement was obtained between the TXRF results for the total bromine and bromide determinations in soils and those obtained by other popular analytical techniques, e.g. energy dispersive X-ray fluorescence spectrometry (total bromine) and ionic chromatography (bromide). As a study case, the TXRF method was applied to study bromine accumulation in two agricultural soils fumigated with a methyl bromide pesticide and irrigated with regenerated waste water. Copyright © 2016 Elsevier Ltd. All rights reserved.

  12. Development of an electrothermal atomization laser-excited atomic fluorescence spectrometry procedure for direct measurements of arsenic in diluted serum.

    Science.gov (United States)

    Swart, D J; Simeonsson, J B

    1999-11-01

    A procedure for the direct determination of arsenic in diluted serum by electrothermal atomization laser-excited atomic fluorescence spectrometry (ETA-LEAFS) is reported. Laser radiation needed to excite As at 193.696 and 197.197 nm is generated as the second anti-Stokes stimulated Raman scattering output of a frequency-doubled dye laser operating near 230.5 and 235.5 nm, respectively. Two different LEAFS schemes have been utilized and provide limits of detection of 200-300 fg for As in aqueous standards. When measurements of serum samples diluted 1:10 with deionized water are performed, a stable background signal is observed that can be accounted for by taking measurements with the laser tuned off-wavelength. No As is detected in any of the bovine or human serum samples analyzed. Measurements of 100 pg/mL standard additions of As to a diluted bovine serum sample utilizing either inorganic or organic As species demonstrate a linear relationship of the fluorescence signal to As spike concentration, but exhibit a sensitivity of approximately half that observed in pure aqueous standards. The limit of detection for As in 1:10 diluted serum samples is 65 pg/mL or 650 fg absolute mass, which corresponds to 0.65 ng/mL As in undiluted serum. To our knowledge, the ETA-LEAFS procedure is currently the only one capable of directly measuring As in diluted serum at these levels.

  13. In Situ Analytical Characterization of Contaminated Sites Using Nuclear Spectrometry Techniques. Review of Methodologies and Measurements

    International Nuclear Information System (INIS)

    2017-01-01

    Past and current human activities can result in the contamination of sites by radionuclides and heavy metals. The sources of contamination are various. The most important sources for radionuclide release include global fallout from nuclear testing, nuclear and radiological accidents, waste production from nuclear facilities, and activities involving naturally occurring radioactive material (NORM). Contamination of the environment by heavy metals mainly originates from industrial applications and mineralogical background concentration. Contamination of sites by radionuclides and heavy metals can present a risk to people and the environment. Therefore, the estimation of the contamination level and the identification of the source constitute important information for the national authorities with the responsibility to protect people and the environment from adverse health effects. In situ analytical techniques based on nuclear spectrometry are important tools for the characterization of contaminated sites. Much progress has been made in the design and implementation of portable systems for efficient and effective monitoring of radioactivity and heavy metals in the environment directly on-site. Accordingly, the IAEA organized a Technical Meeting to review the current status and trends of various applications of in situ nuclear spectrometry techniques for analytical characterization of contaminated sites and to support Member States in their national environmental monitoring programmes applying portable instrumentation. This publication represents a comprehensive review of the in situ gamma ray spectrometry and field portable X ray fluorescence analysis techniques for the characterization of contaminated sites. It includes papers on the use of these techniques, which provide useful background information for conducting similar studies, in the following Member States: Argentina, Australia, Brazil, Czech Republic, Egypt, France, Greece, Hungary, Italy, Lithuania

  14. Determination of mercury in sewage sludge by direct slurry sampling graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Baralkiewicz, Danuta; Gramowska, Hanka; Kozka, MaIgorzata; Kanecka, Anetta

    2005-01-01

    Ultrasonic slurry sampling electrothermal atomic absorption spectrometry (ETAAS) method was elaborated to the determination of Hg in sewage sludge samples with the use of KMnO 4 +Pd modifier. The minimum sample amount required for slurry preparation with respect to sample homogeneity was evaluated by weighting masses between 3 and 30 mg directly into the autosampler cups. Validation of the proposed method was performed with the use of Certified Reference Materials of sewage sludge, CRM 007-040 and CRM 144R. Two sewage sludge samples from Poznan (Poland) city were analysed using the present direct method and a method with sample digestion, resulting in no difference within statistical error

  15. Electrochemical hydride generation as a sample-introduction technique in atomic spectrometry: fundamentals, interferences, and applications.

    Science.gov (United States)

    Laborda, Francisco; Bolea, Eduardo; Castillo, Juan R

    2007-06-01

    Electrochemical hydride generation (EC-HG) has been proposed as a valid alternative to chemical generation as a sample-introduction technique in atomic spectrometry. In this review fundamental aspects of the technique are revised, including designs of electrolytic cells, mechanisms of the generation process, and interferences caused by the presence of different species. Special attention is paid to the role of the configuration of the cathodes and their materials on the efficiency of hydride generation and on interferences from concomitant species. An overview of the application of EC-HG to the analysis of real samples is also given.

  16. [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.

  17. Determination of trace amounts of cerium in paint by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Wong, K.L.

    1981-01-01

    The determination of Ce in paint by inductively coupled plasma atomic emission spectrometry (ICP-OES) is described, and the detection limit of ICP-OES of 0.0004 ppM is compared with that of other methods. The effects of the major elemental components of paint, Si, Pb, Cr, and Na on the ICP-OES determination of Ce were studied. The interference of 400 ppM of the other ions on the determination of 10 ppM Ce was small (0 to 3% error). The method is applicable to the range of 0.2 to 700 ppM Ce

  18. Small sample analysis using sputter atomization/resonance ionization mass spectrometry

    International Nuclear Information System (INIS)

    Christie, W.H.; Goeringer, D.E.

    1986-01-01

    We have used secondary ion mass spectrometry (SIMS) to investigate the emission of ions via argon sputtering from U metal, UO 2 , and U 3 O 8 samples. We have also used laser resonance ionization techniques to study argon-sputtered neutral atoms and molecules emitted from these same samples. For the case of U metal, a significant enhancement in detection sensitivity for U is obtained via SA/RIMS. For U in the fully oxidized form (U 3 O 8 ), SA/RIMS offers no improvement in U detection sensitivity over conventional SIMS when sputtering with argon. 9 refs., 1 fig., 2 tabs

  19. 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...

  20. Development and application of acousto-optic background correction for inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    Miller, Heather M; Spudich, Thomas M; Carnahan, Jon W

    2003-06-01

    In two configurations, a solid-state acousto-optic (AO) deflector or modulator is mounted in a 0.5 m monochromator for background correction with inductively coupled plasma atomic emission spectrometry (ICP-AES). A fused silica acousto-optic modulator (AOM) is used in the ultraviolet (UV) spectral region applications while a glass AO deflector (AOD) is used for the visible (VIS) region. The system provides rapid sequential observation of adjacent on- and off-line wavelengths for background correction. Seventeen elements are examined using pneumatic nebulization (PN) and electrothermal vaporization (ETV) sample introduction. Calibration plots were obtained with each sample introduction technique. Potable water and vitamin tablets were analyzed. Flame atomic absorption (FAA) was used to verify the accuracy of the AO background correction system.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-05-01

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

  2. 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...... introduction of membrane pieces into the graphite furnace. The proteins were separated by sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) and subsequently transferred to a polyvinylidene difluoride (PVDF) membrane by semi-dry electroblotting. After staining the membrane, the protein bands...... 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...

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

    International Nuclear Information System (INIS)

    Young, J.P.; Donohue, D.L.; Smith, D.H.

    1984-01-01

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

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

    Science.gov (United States)

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

    2017-07-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-01-01

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

  7. Fast screening of analytes for chemical reactions by reactive low-temperature plasma ionization mass spectrometry.

    Science.gov (United States)

    Zhang, Wei; Huang, Guangming

    2015-11-15

    Approaches for analyte screening have been used to aid in the fine-tuning of chemical reactions. Herein, we present a simple and straightforward analyte screening method for chemical reactions via reactive low-temperature plasma ionization mass spectrometry (reactive LTP-MS). Solution-phase reagents deposited on sample substrates were desorbed into the vapor phase by action of the LTP and by thermal desorption. Treated with LTP, both reagents reacted through a vapor phase ion/molecule reaction to generate the product. Finally, protonated reagents and products were identified by LTP-MS. Reaction products from imine formation reaction, Eschweiler-Clarke methylation and the Eberlin reaction were detected via reactive LTP-MS. Products from the imine formation reaction with reagents substituted with different functional groups (26 out of 28 trials) were successfully screened in a time of 30 s each. Besides, two short-lived reactive intermediates of Eschweiler-Clarke methylation were also detected. LTP in this study serves both as an ambient ionization source for analyte identification (including reagents, intermediates and products) and as a means to produce reagent ions to assist gas-phase ion/molecule reactions. The present reactive LTP-MS method enables fast screening for several analytes from several chemical reactions, which possesses good reagent compatibility and the potential to perform high-throughput analyte screening. In addition, with the detection of various reactive intermediates (intermediates I and II of Eschweiler-Clarke methylation), the present method would also contribute to revealing and elucidating reaction mechanisms. Copyright © 2015 John Wiley & Sons, Ltd.

  8. Analytical approach to the helium-atom ground state using correlated wavefunctions

    Energy Technology Data Exchange (ETDEWEB)

    Bhattacharyya, S.; Bhattacharyya, A.; Talukdar, B. [Visvabharati Univ., Santiniketan (India). Dept. of Physics; Deb, N.C. [Indian Association for the Cultivation of Science, Calcutta (India). Dept. of Theoretical Physics

    1996-03-14

    A realistic three-parameter correlated wavefunction is used to construct an exact analytical expression for the expectation value of the helium-atom Hamiltonian expressed in the interparticle coordinates. The parameters determined variationally are found to satisfy the orbital and correlation cusp conditions to a fair degree of accuracy and yield a value for the ground-state energy which is in good agreement with the exact result. (author).

  9. 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.

  10. Solid sampling-graphite furnace atomic absorption spectrometry for the direct determination of boron in plant tissues

    International Nuclear Information System (INIS)

    Resano, M.; Briceno, J.; Aramendia, M.; Belarra, M.A.

    2007-01-01

    In this work, the potential of graphite furnace atomic absorption spectrometry for the direct determination of B in plant tissues has been investigated. Three certified reference materials (NIST SRM 1570a spinach leaves, NIST SRM 1573a tomato leaves and BCR CRM 679 white cabbage) were selected for this study, the goal always being to develop a fast procedure that could be robust enough to provide a satisfactory performance for all of them, without any modifications in the conditions applied. The use of a suitable chemical modifier was found to be essential for obtaining a reproducible and sufficiently sensitive signal for boron solutions. In this regard, the performance of the combination of citric acid plus W (added as a permanent modifier) was noteworthy, resulting in well-defined signal profiles, a remarkable analyte stabilization during the pyrolysis step (up to 2100 deg. C) and minimal memory effects. This mixture of modifiers provided a good performance for the direct analysis of solid samples as well, but only if a suitable temperature program, favoring the interaction between the analyte and the modifiers, was used. Thus, such a temperature program, with two pyrolysis steps and the addition of NH 4 NO 3 in order to carry out the in situ sample microdigestion, was optimized. Under these conditions, the peak areas obtained for both solid samples and aqueous standards were comparable. Finally, the analysis of the samples was carried out. In all cases, a good agreement with the certified values was obtained, while R.S.D. values ranged between 6 and 10%. It can be concluded that the method proposed shows significant advantages for the determination of this complicated element in solid samples such as the use of aqueous standards for calibration, a high sample throughput (20 min per sample), a suitable limit of detection (0.3 μg g -1 ) and reduced risk of analyte losses and contamination

  11. 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.

  12. Analytical transition-matrix treatment of electric multipole polarizabilities of hydrogen-like atoms

    International Nuclear Information System (INIS)

    Kharchenko, V.F.

    2015-01-01

    The direct transition-matrix approach to the description of the electric polarization of the quantum bound system of particles is used to determine the electric multipole polarizabilities of the hydrogen-like atoms. It is shown that in the case of the bound system formed by the Coulomb interaction the corresponding inhomogeneous integral equation determining an off-shell scattering function, which consistently describes virtual multiple scattering, can be solved exactly analytically for all electric multipole polarizabilities. Our method allows to reproduce the known Dalgarno–Lewis formula for electric multipole polarizabilities of the hydrogen atom in the ground state and can also be applied to determine the polarizability of the atom in excited bound states. - Highlights: • A new description for electric polarization of hydrogen-like atoms. • Expression for multipole polarizabilities in terms of off-shell scattering functions. • Derivation of integral equation determining the off-shell scattering function. • Rigorous analytic solving the integral equations both for ground and excited states. • Study of contributions of virtual multiple scattering to electric polarizabilities

  13. Determination of radium isotopes in environmental samples by gamma spectrometry, liquid scintillation counting and alpha spectrometry: a review of analytical methodology

    International Nuclear Information System (INIS)

    Jia, Guogang; Jia, Jing

    2012-01-01

    Radium (Ra) isotopes are important from the viewpoints of radiation protection and environmental protection. Their high toxicity has stimulated the continuing interest in methodology research for determination of Ra isotopes in various media. In this paper, the three most routinely used analytical techniques for Ra isotope determination in biological and environmental samples, i.e. low-background γ-spectrometry, liquid scintillation counting and α-spectrometry, were reviewed, with emphasis on new methodological developments in sample preparation, preconcentration, separation, purification, source preparation and measurement techniques. The accuracy, selectivity, traceability, applicability and minimum detectable activity (MDA) of the three techniques were discussed. It was concluded that the MDA (0.1 mBq L −1 ) of the α-spectrometry technique coupled with chemical separation is about two orders of magnitude lower than that of low-background HPGe γ-spectrometry and LSC techniques. Therefore, when maximum sensitivity is required, the α-spectrometry technique remains the first choice. - Highlights: ► A review is made for determination of Ra isotopes in environmental samples. ► Gamma spectrometry, LSC and a-spectrometry are the main concerned radiometric approach. ► Sample preparation, preconcentration, separation and source preparation are discussed. ► The methods can analyse air, water, seawater, soil, sediment and foodstuffs samples. ► Some new data obtained recently from our laboratory for Ra method study are included.

  14. [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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-03-01

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

  16. 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.

  17. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-02-05

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

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

    Science.gov (United States)

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

    2015-01-01

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

  1. Analytic description of elastic electron-atom scattering in an elliptically polarized laser field

    Science.gov (United States)

    Flegel, A. V.; Frolov, M. V.; Manakov, N. L.; Starace, Anthony F.; Zheltukhin, A. N.

    2013-01-01

    An analytic description of laser-assisted electron-atom scattering (LAES) in an elliptically polarized field is presented using time-dependent effective range (TDER) theory to treat both electron-laser and electron-atom interactions nonperturbatively. Closed-form formulas describing plateau features in LAES spectra are derived quantum mechanically in the low-frequency limit. These formulas provide an analytic explanation for key features of the LAES differential cross section. For the low-energy region of the LAES spectrum, our result generalizes the Kroll-Watson formula to the case of elliptic polarization. For the high-energy (rescattering) plateau in the LAES spectrum, our result generalizes prior results for a linearly polarized field valid for the high-energy end of the rescattering plateau [Flegel , J. Phys. BJPAPEH0953-407510.1088/0953-4075/42/24/241002 42, 241002 (2009)] and confirms the factorization of the LAES cross section into three factors: two field-free elastic electron-atom scattering cross sections (with laser-modified momenta) and a laser field-dependent factor (insensitive to the scattering potential) describing the laser-driven motion of the electron in the elliptically polarized field. We present also approximate analytic expressions for the exact TDER LAES amplitude that are valid over the entire rescattering plateau and reduce to the three-factor form in the plateau cutoff region. The theory is illustrated for the cases of e-H scattering in a CO2-laser field and e-F scattering in a midinfrared laser field of wavelength λ=3.5μm, for which the analytic results are shown to be in good agreement with exact numerical TDER results.

  2. Analytical chemistry

    International Nuclear Information System (INIS)

    Choi, Jae Seong

    1993-02-01

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

  3. Atomic Force Microscope Controlled Topographical Imaging and Proximal Probe Thermal Desorption/Ionization Mass Spectrometry Imaging

    Energy Technology Data Exchange (ETDEWEB)

    Ovchinnikova, Olga S [ORNL; Kjoller, Kevin [Anasys Instruments Corporation; Hurst, Gregory {Greg} B [ORNL; Pelletier, Dale A [ORNL; Van Berkel, Gary J [ORNL

    2014-01-01

    This paper reports on the development of a hybrid atmospheric pressure atomic force microscopy/mass spectrometry imaging system utilizing nano-thermal analysis probes for thermal desorption surface sampling with subsequent atmospheric pressure chemical ionization and mass analysis. The basic instrumental setup and the general operation of the system were discussed and optimized performance metrics were presented. The ability to correlate topographic images of a surface with atomic force microscopy and a mass spectral chemical image of the same surface, utilizing the same probe without moving the sample from the system, was demonstrated. Co-registered mass spectral chemical images and atomic force microscopy topographical images were obtained from inked patterns on paper as well as from a living bacterial colony on an agar gel. Spatial resolution of the topography images based on pixel size (0.2 m x 0.8 m) was better than the resolution of the mass spectral images (2.5 m x 2.0 m), which were limited by current mass spectral data acquisition rate and system detection levels.

  4. 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)

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

    Science.gov (United States)

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

    1993-08-01

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

  6. [Indirect determination of rare earth elements in Chinese herbal medicines by hydride generation-atomic fluorescence spectrometry].

    Science.gov (United States)

    Zeng, Chao; Lu, Jian-Ping; Xue, Min-Hua; Tan, Fang-Wei; Wu, Xiao-Yan

    2014-07-01

    Based on their similarity in chemical properties, rare earth elements were able to form stable coordinated compounds with arsenazo III which were extractable into butanol in the presence of diphenylguanidine. The butanol was removed under reduced pressure distillation; the residue was dissolved with diluted hydrochloric acid. As was released with the assistance of KMnO4 and determined by hydrogen generation-atomic fluorescence spectrometry in terms of rare earth elements. When cesium sulfate worked as standard solution, extraction conditions, KMnO4 amount, distillation temperature, arsenazo III amount, interfering ions, etc were optimized. The accuracy and precision of the method were validated using national standard certified materials, showing a good agreement. Under optimum condition, the linear relationship located in 0.2-25 microg x mL(-1) and detection limit was 0.44 microg x mL(-1). After the herbal samples were digested with nitric acid and hydrogen peroxide, the rare earth elements were determined by this method, showing satisfactory results with relative standard deviation of 1.3%-2.5%, and recoveries of 94.4%-106.0%. The method showed the merits of convenience and rapidness, simple instrumentation and high accuracy. With the rare earths enriched into organic phase, the separation of analytes from matrix was accomplished, which eliminated the interference. With the residue dissolved by diluted hydrochloric acid after the solvent was removed, aqueous sample introduction eliminated the impact of organic phase on the tubing connected to pneumatic pump.

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

    Science.gov (United States)

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

    2013-03-30

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

  8. Hydrodemetallation and Hydrodesulfurization Spent Catalysts Elemental Analysis: Comparison of Wavelength Dispersive X-ray Fluorescence and Atomic Emission Spectrometries.

    Science.gov (United States)

    Garoux, Laetitia; Gourhand, Sébastien; Hébrant, Marc; Schneider, Michel; Diliberto, Sébastien; Meux, Eric

    2017-08-01

    Petroleum industries continuously consume catalysts on very large scales. The recycling of spent catalysts is thus of major economic and environmental importance and its first step consists of the characterization of the valuable metal content. Wavelength dispersive X-ray fluorescence (WDXRF) analysis is compared with inductively coupled plasma atomic emission spectrometry (ICP-AES) for the analysis of five samples of spent hydrodesulphurization (HDS) and hydrodemetallization (HDM) catalysts. The elements are considered for their economic interest (Co, Ni, Mo, and V) or for the problems that can arise when they are present in the sample in significant quantities (Al, As, P, Fe). First, the systematic comparison of the analysis of known synthetic samples was performed. The originality here is that the samples were first beaded with lithium tetraborate (Li 2 B 4 O 7 ) for WDXRF analysis and then dissolved in hot HCl 6M for ICP-AES measurements. With this processing, we were able to clearly identify the origin of analytical problems when they arose. Second, the semi-quantitative protocol of WDXRF is compared with the quantitative procedure. Finally, the analysis of the spent catalysts is presented and the information gained by the systematic comparison of ICP-AES and WDXRF is shared. The interest of the simultaneous determination by the two techniques when such complicated heterogeneous matrices are involved is clearly demonstrated.

  9. NEW METHOD FOR REMOVAL OF SPECTRAL INTERFERENCES FOR BERYLLIUM ASSAY USING INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S; Matthew Nelson, M; Linda Youmans, L; Maureen Bernard, M

    2008-01-14

    Beryllium has been used widely in specific areas of nuclear technology. Frequent monitoring of air and possible contaminated surfaces in U.S Department of Energy (DOE) facilities is required to identify potential health risks and to protect DOE workers from beryllium-contaminated dust. A new method has been developed to rapidly remove spectral interferences prior to beryllium (Be) measurement by inductively-coupled plasma atomic emission spectrometry (ICP-AES). The ion exchange separation removes uranium (U), thorium (Th), niobium (Nb), vanadium (V), molybdenum (Mo), zirconium (Zr), tungsten (W), iron (Fe), chromium (Cr), cerium (Ce), erbium (Er) and titanium (Ti). A stacked column consisting of Diphonix Resin{reg_sign} and TEVA Resin{reg_sign} reduces the levels of the spectral interferences so that low level Be measurements can be performed accurately. If necessary, an additional anion exchange separation can be used for further removal of interferences, particularly chromium. The method has been tested using spiked filters, spiked wipe samples and certified reference material standards with high levels of interferences added. The method provides very efficient removal of spectral interferences with very good accuracy and precision for beryllium on filters or wipes. A vacuum box system is employed to reduce analytical time and reduce labor costs.

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

    Science.gov (United States)

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

    2016-05-01

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

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

    Science.gov (United States)

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

    2013-12-01

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

  12. Analysis of low molecular weight metabolites in tea using mass spectrometry-based analytical methods.

    Science.gov (United States)

    Fraser, Karl; Harrison, Scott J; Lane, Geoff A; Otter, Don E; Hemar, Yacine; Quek, Siew-Young; Rasmussen, Susanne

    2014-01-01

    Tea is the second most consumed beverage in the world after water and there are numerous reported health benefits as a result of consuming tea, such as reducing the risk of cardiovascular disease and many types of cancer. Thus, there is much interest in the chemical composition of teas, for example; defining components responsible for contributing to reported health benefits; defining quality characteristics such as product flavor; and monitoring for pesticide residues to comply with food safety import/export requirements. Covered in this review are some of the latest developments in mass spectrometry-based analytical techniques for measuring and characterizing low molecular weight components of tea, in particular primary and secondary metabolites. The methodology; more specifically the chromatography and detection mechanisms used in both targeted and non-targeted studies, and their main advantages and disadvantages are discussed. Finally, we comment on the latest techniques that are likely to have significant benefit to analysts in the future, not merely in the area of tea research, but in the analytical chemistry of low molecular weight compounds in general.

  13. Analytical possibilities of total reflection X-ray spectrometry (TXRF) for trace selenium determination in soils.

    Science.gov (United States)

    Marguí, E; Floor, G H; Hidalgo, M; Kregsamer, P; Román-Ross, G; Streli, C; Queralt, I

    2010-09-15

    Selenium content of soils is an important issue due to the narrow range between the nutritious requirement and toxic effects upon Se exposure. However, its determination is challenging due to low concentrations within complex matrices that hamper the analysis in most spectroscopic techniques. In this study, we explored the possibilities of several analytical approaches combined with total reflection X-ray (TXRF) spectrometry for soil Se determinations. The direct analysis of a solid suspension using 20 mg of fine ground material (TXRF analysis of soil extracts due to the high Fe concentrations (∼700 mg/L). On the other hand, a dispersive liquid-liquid microextraction procedure (DLLME) before the TXRF analysis of the soil digest was also developed. The effects of various experimental parameters such as sample volume, effect of major elements present in the soil matrix (Fe), and Se concentration in the sample were investigated. The LOD using this analytical methodology (0.05 mg/kg of Se) was comparable to or lower than those obtained in previous works using other popular spectrometric techniques such as GFAAS, ICPMS, and AFS. The calculated Se concentration for JSAC-0411 ([Se] = 1.32 ± 0.27 mg/kg) using the combination of DLLME and TXRF ([Se] = 1.40 ± 0.23 mg/kg) was in agreement with the certified value.

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

    Science.gov (United States)

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

    2011-01-01

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

  15. Applicability of multisyringe chromatography coupled to cold-vapor atomic fluorescence spectrometry for mercury speciation analysis

    International Nuclear Information System (INIS)

    Guzmán-Mar, J.L.; Hinojosa-Reyes, L.; Serra, A.M.; Hernández-Ramírez, A.; Cerdà, V.

    2011-01-01

    Graphical abstract: An automatic system, based on the applicability of multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) detection is developed for mercury speciation. Highlights: ► The on-line coupling of MSC to CV/AFS was developed for mercury speciation analysis. ► The speciation of MeHg + , Hg 2+ and EtHg + was achieved on a RP C18 monolithic column. ► The hyphenated system provided higher sample throughput compared to HPLC–CV/AFS. ► The limits of detection for mercury species were comparable or better than those reported by HPLC–CV/AFS. ► The developed method also provided low instrumental and operational costs. - Abstract: In this paper, a novel automatic approach for the speciation of inorganic mercury (Hg 2+ ), methylmercury (MeHg + ) and ethylmercury (EtHg + ) using multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) was developed. For the first time, the separation of mercury species was accomplished on a RP C18 monolithic column using a multi-isocratic elution program. The elution protocol involved the use of 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)–acetonitrile (99:1, v/v), followed by 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)–acetonitrile (90:10, v/v). The eluted mercury species were then oxidized under post-column UV radiation and reduced using tin(II) chloride in an acidic medium. Subsequently, the generated mercury metal were separated from the reaction mixture and further atomized in the flame atomizer and detected by AFS. Under the optimized experimental conditions, the limits of detection (3σ) were found to be 0.03, 0.11 and 0.09 μg L −1 for MeHg + , Hg 2+ and EtHg + , respectively. The relative standard deviation (RSD, n = 6) of the peak height for 3, 6 and 3 μg L −1 of MeHg + , Hg 2+ and EtHg + (as Hg) ranged from 2.4 to 4.0%. Compared with the conventional HPLC–CV/AFS hyphenated systems

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

    International Nuclear Information System (INIS)

    Matsushige, I.

    1990-01-01

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

  17. [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.

  18. 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

  19. 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.

  20. 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.

  1. An analytical model accounting for tip shape evolution during atom probe analysis of heterogeneous materials.

    Science.gov (United States)

    Rolland, N; Larson, D J; Geiser, B P; Duguay, S; Vurpillot, F; Blavette, D

    2015-12-01

    An analytical model describing the field evaporation dynamics of a tip made of a thin layer deposited on a substrate is presented in this paper. The difference in evaporation field between the materials is taken into account in this approach in which the tip shape is modeled at a mesoscopic scale. It was found that the non-existence of sharp edge on the surface is a sufficient condition to derive the morphological evolution during successive evaporation of the layers. This modeling gives an instantaneous and smooth analytical representation of the surface that shows good agreement with finite difference simulations results, and a specific regime of evaporation was highlighted when the substrate is a low evaporation field phase. In addition, the model makes it possible to calculate theoretically the tip analyzed volume, potentially opening up new horizons for atom probe tomographic reconstruction. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Seshavatharam, U.V.S.; Lakshminarayana, S.

    2015-01-01

    If N A represents the Avogadro's number, gravitational constant associated with atomic electromagnetic interaction can be expressed as G E ≅ N 2 A G. With G E and with the assumed two new pseudo numbers x ≈ 38.725 and y ≈ 47.415, value of G can be fixed for 10 digits in a verifiable approach. (x, y) can be called as the back ground analytical numbers using by which micro-macro physical constants can be interlinked qualitatively and quantitatively

  3. Analytically approximate screened calculations of atomic-field pair production cross sections

    International Nuclear Information System (INIS)

    Dugne, J.J.

    1976-01-01

    A new method is described to obtain analytically approximate screened cross sections of atomic-field pair production. The Thomas-Fermi-Csavinszky potential model is expanded at the first order and put in the place of the point Coulomb potential in the Dirac equation. That method can be very useful to calculate approximate screened cross sections for the intermediate photon energy range (5m 0 c 2 to about 50m 0 c 2 ) where numerically exact screened cross sections are needing a prohibitive computer time and when the form factor approach based on Born approximation is not always valid. (Auth.)

  4. 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,…

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

    Science.gov (United States)

    Resano, M.; Mozas, E.; Crespo, C.; Pérez, J.; García-Ruiz, E.; Belarra, M. A.

    2012-05-01

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

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

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Ekelund, J.

    1989-01-01

    -effect background corrected graphite furnace atomic absorption spectrometry. A furnace ashing step at 1100 °C was necessary in order to obtain a total recovery of selenium when present in the organic form. Palladium nitrate-magnesium nitrate was used as a matrix modifier. Independent methods were used to determine...

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

    Science.gov (United States)

    Pfennig, Brian W.; Schaefer, Amy K.

    2011-01-01

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

  8. 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

  9. 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.

  10. Complementary Characterization of Cu(In,Ga)Se₂ Thin-Film Photovoltaic Cells Using Secondary Ion Mass Spectrometry, Auger Electron Spectroscopy, and Atom Probe Tomography.

    Science.gov (United States)

    Jang, Yun Jung; Lee, Jihye; Jeong, Jeung-Hyun; Lee, Kang-Bong; Kim, Donghwan; Lee, Yeonhee

    2018-05-01

    To enhance the conversion performance of solar cells, a quantitative and depth-resolved elemental analysis of photovoltaic thin films is required. In this study, we determined the average concentration of the major elements (Cu, In, Ga, and Se) in fabricated Cu(In,Ga)Se2 (CIGS) thin films, using inductively coupled plasma atomic emission spectroscopy, X-ray fluorescence, and wavelengthdispersive electron probe microanalysis. Depth profiling results for CIGS thin films with different cell efficiencies were obtained using secondary ion mass spectrometry and Auger electron spectroscopy to compare the atomic concentrations. Atom probe tomography, a characterization technique with sub-nanometer resolution, was used to obtain three-dimensional elemental mapping and the compositional distribution at the grain boundaries (GBs). GBs are identified by Na increment accompanied by Cu depletion and In enrichment. Segregation of Na atoms along the GB had a beneficial effect on cell performance. Comparative analyses of different CIGS absorber layers using various analytical techniques provide us with understanding of the compositional distributions and structures of high efficiency CIGS thin films in solar cells.

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

    Science.gov (United States)

    Gunduz, S; Akman, S; Kahraman, M

    2011-02-15

    Separation/preconcentration of copper and cadmium using TiO(2) core-Au shell nanoparticles modified with 11-mercaptoundecanoic acid and their slurry analysis by flame atomic absorption spectrometry were described. For this purpose, at first, titanium dioxide nanoparticles were coated with gold shell by reducing the chloroauric acid with sodium borohydride and then modified with 11-mercaptoundecanoic acid. The characterization of modified nanoparticles was performed using ultra-violet spectroscopy and dynamic light scattering. Copper and cadmium were then collected on the prepared sorbent by batch method. The solid phase loaded with the analytes was separated by centrifugation and the supernatant was removed. Finally, the precipitate was slurried and directly aspirated into the flame for the determination of analytes. Thus, elution step and its all drawbacks were eliminated. The effects of pH, amount of sorbent, slurry volume, sample volume and diverse ions on the recovery were investigated. After optimization of experimental parameters, the analytes in different certified reference materials and spiked water samples were quantitatively recovered with 5% RSD. The analytes were enriched up to 20-fold. Limits of detection (N=10, 3σ) for copper and cadmium were 0.28 and 0.15 ng mL(-1), respectively. Copyright © 2010 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-02-15

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

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

    Directory of Open Access Journals (Sweden)

    Dadfarnia Shayessteh

    2006-01-01

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

  14. A novel slurry sampling analysis of lead in different water samples by electrothermal atomic absorption spectrometry after coprecipitated with cobalt/pyrrolidine dithiocarbamate complex

    Energy Technology Data Exchange (ETDEWEB)

    Baysal, A. [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak, Istanbul (Turkey); Akman, S. [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak, Istanbul (Turkey)], E-mail: akmans@itu.edu.tr; Calisir, F. [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak, Istanbul (Turkey)

    2008-10-30

    A preconcentration/separation technique based on the coprecipitation of lead with cobalt/pyrrolidine dithiocarbamate complex (Co(PDC){sub 2}) and subsequently its direct slurry sampling determination by electrothermal atomic absorption spectrometry (AAS) was described. For this purpose, at first, lead was coprecipitated with cobalt/pyrrolidine dithiocarbamate complex formed using ammonium pyrrolidine dithiocarbamate (APDC) as a chelating agent and cobalt as a carrier element. The supernatant was then separated and the slurry of the precipitate prepared in Triton X-100 was directly analyzed by electrothermal atomic absorption spectrometry with respect to lead concentration. The effects of experimental conditions on coprecipitation of lead with gathering precipitate as well as homogeneity and stability of the slurry were investigated. After the optimization of experimental parameters, a 100-fold enrichment of the analyte with quantitative recovery (>90%) and high precision (<10% R.S.D.) were obtained. By using the proposed technique, the lead concentrations in heavy matrices of Certified Sea-water and wastewater samples could be practically and rapidly determined in the range of 95% confidence level. The detection limit of the described method for lead using sample-matching blanks was 1.5 ng/L (3{sigma}, N = 10)

  15. 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.

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

    Science.gov (United States)

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

    2015-03-01

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

  17. Biomedical applications of accelerator mass spectrometry-isotope measurements at the level of the atom.

    Science.gov (United States)

    Barker, J; Garner, R C

    1999-01-01

    Accelerator mass spectrometry (AMS) is a nuclear physics technique developed about twenty years ago, that uses the high energy (several MeV) of a tandem Van de Graaff accelerator to measure very small quantities of rare and long-lived isotopes. Elements that are of interest in biomedicine and environmental sciences can be measured, often to parts per quadrillion sensitivity, i.e. zeptomole to attomole levels (10(-21)-10(-18) mole) from milligram samples. This is several orders of magnitude lower than that achievable by conventional decay counting techniques, such as liquid scintillation counting (LSC). AMS was first applied to geochemical, climatological and archaeological areas, such as for radiocarbon dating (Shroud of Turin), but more recently this technology has been used for bioanalytical applications. In this sphere, most work has been conducted using aluminium, calcium and carbon isotopes. The latter is of special interest in drug metabolism studies, where a Phase 1 adsorption, distribution, metabolism and excretion (ADME) study can be conducted using only 10 nanoCurie (37 Bq or ca. 0.9 microSv) amounts or less of 14C-labelled drugs. In the UK, these amounts of radioactivity are below those necessary to request specific regulatory approval from the Department of Health's Administration of Radioactive Substances Advisory Committee (ARSAC), thus saving on valuable development time and resources. In addition, the disposal of these amounts is much less an environmental issue than that associated with microCurie quantities, which are currently used. Also, AMS should bring an opportunity to conduct "first into man" studies without the need for widespread use of animals. Centre for Biomedical Accelerator Mass Spectrometry (CBAMS) Ltd. is the first fully commercial company in the world to offer analytical services using AMS. With its high throughput and relatively low costs per sample analysis, AMS should be of great benefit to the pharmaceutical and biotechnology

  18. Applicability of multisyringe chromatography coupled to cold-vapor atomic fluorescence spectrometry for mercury speciation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Guzman-Mar, J.L.; Hinojosa-Reyes, L. [Department of Chemistry Sciences, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, Pedro de Alba s/n, C.P. 66451 San Nicolas de los Garza, Nuevo Leon (Mexico); Serra, A.M. [Department of Chemistry, University of the Balearic Islands, E-07122 Palma de Mallorca (Spain); Hernandez-Ramirez, A. [Department of Chemistry Sciences, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, Pedro de Alba s/n, C.P. 66451 San Nicolas de los Garza, Nuevo Leon (Mexico); Cerda, V., E-mail: victor.cerda@uib.es [Department of Chemistry, University of the Balearic Islands, E-07122 Palma de Mallorca (Spain)

    2011-12-05

    Graphical abstract: An automatic system, based on the applicability of multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) detection is developed for mercury speciation. Highlights: Black-Right-Pointing-Pointer The on-line coupling of MSC to CV/AFS was developed for mercury speciation analysis. Black-Right-Pointing-Pointer The speciation of MeHg{sup +}, Hg{sup 2+} and EtHg{sup +} was achieved on a RP C18 monolithic column. Black-Right-Pointing-Pointer The hyphenated system provided higher sample throughput compared to HPLC-CV/AFS. Black-Right-Pointing-Pointer The limits of detection for mercury species were comparable or better than those reported by HPLC-CV/AFS. Black-Right-Pointing-Pointer The developed method also provided low instrumental and operational costs. - Abstract: In this paper, a novel automatic approach for the speciation of inorganic mercury (Hg{sup 2+}), methylmercury (MeHg{sup +}) and ethylmercury (EtHg{sup +}) using multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) was developed. For the first time, the separation of mercury species was accomplished on a RP C18 monolithic column using a multi-isocratic elution program. The elution protocol involved the use of 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)-acetonitrile (99:1, v/v), followed by 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)-acetonitrile (90:10, v/v). The eluted mercury species were then oxidized under post-column UV radiation and reduced using tin(II) chloride in an acidic medium. Subsequently, the generated mercury metal were separated from the reaction mixture and further atomized in the flame atomizer and detected by AFS. Under the optimized experimental conditions, the limits of detection (3{sigma}) were found to be 0.03, 0.11 and 0.09 {mu}g L{sup -1} for MeHg{sup +}, Hg{sup 2+} and EtHg{sup +}, respectively. The relative standard deviation (RSD, n = 6) of the

  19. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-06-30

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

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

    Directory of Open Access Journals (Sweden)

    DAGMAR GALUSKOVÁ

    2014-03-01

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

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

    International Nuclear Information System (INIS)

    Resano, M.; Mozas, E.; Crespo, C.; Pérez, J.; García-Ruiz, E.; Belarra, M.A.

    2012-01-01

    This paper reports on the use of solid sampling-graphite furnace atomic absorption spectrometry for the direct analysis of synthetic amorphous silica. In particular, determination of hazardous elements such As, Cd, Cr, Cu, Pb and Sb is investigated, as required by regulations of the food industry. The conclusion of the work is that, after proper optimization of the working conditions, paying particular attention to the atomization temperature and the use of proper modifiers (graphite powder, HNO 3 or Pd), it is possible to develop suitable procedures that rely on the use of aqueous standard solutions to construct the calibration curves for all the elements investigated. The proposed method shows important benefits for the cost-effective analysis of such difficult samples in routine labs, permitting fast screening of those elements that are very rarely present in this type of sample, but also accurate quantification of those often found, while offering low limits of detection (always below 0.1 mg g −1 ) that comply well with legal requirements, and precision levels that are fit for the purpose (approx. 6–9% R.S.D.). - Highlights: ► Solid sampling GFAAS is investigated for the direct analysis of silica samples; ► a fast and simple methodology with aqueous standards for calibration is proposed; ► this method permits accurate determination of As, Cd, Cr, Cu, Pb and Sb in the samples of interest; ► LODs below 100 ng g −1 and precision values in the 6–10% RSD range are achieved.

  3. 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.

  4. Separation and enrichment of Ga and In with ion-exchange resin and their determination by platform graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Tang Senjin; Guan Guisheng

    1999-07-01

    The conditions for separating and enriching Ga and In with 003 x 7 ion-exchange resin and the determination of Ga and In by GFAAS (Graphite Furnace Atomic Absorption Spectrometry) are systematically studied. The Ni and V are used as the matrix modifier for the determination of Ga and In. In the range of pH 0.5-7, the Ga and In are adsorbed selectively, and eluted with a solution of 3 mol/L HNO 3 . the detection limit is down to 1.52 ng/ml for Ga, 0.976 ng/ml for In. Analytical results of national standard reference rock samples by this method conform to the recommended values

  5. Preconcentration of trace elements from high-purity thorium and uranium on Chelex-100 and determination by graphite furnace atomic absorption spectrometry with Zeeman-effect background correction

    International Nuclear Information System (INIS)

    Raje, Naina; Kayasth, Satish; Asari, T.P.S.; Gangadharan, S.

    1994-01-01

    Preconcentration of trace impurities from large-sized samples of uranium metal and thorium oxide using a small column of Chelex-100 followed by their determination using graphite furnace atomic absorption spectrometry (GFAAS) is reported. A 0.5-10-g amount of the sample (uranium metal or thorium oxide) was dissolved, complexed with ammonium carbonate and subjected to the ion-exchange procedure. The retained analytes were eluted with 2-4 M nitric acid and brought to a small volume for a final dilution to 10-25 ml for their determination using GFAAS. The validity of the separation procedure and recoveries at μg kg -1 levels was checked by standard addition; the recoveries were >95%

  6. 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.

  7. Preanalytical and analytical variation of surface-enhanced laser desorption-ionization time-of-flight mass spectrometry of human serum

    DEFF Research Database (Denmark)

    Albrethsen, Jakob; Bøgebo, Rikke; Olsen, Jesper

    2006-01-01

    BACKGROUND: Surface-enhanced laser desorption-ionization time-of-flight (SELDI-TOF) mass spectrometry of human serum is a potential diagnostic tool in human diseases. In the present study, the preanalytical and analytical variation of SELDI-TOF mass spectrometry of serum was assessed in healthy...... was 18% (6%-34%, n=4) for 16 peaks, and inter-individual CV was 38% (16%-56%, n=16) for 20 peaks. CONCLUSIONS: The pre-analytical and analytical conditions of SELDI-TOF mass spectrometry of serum have a significant impact on the protein peaks, with the number of peaks low and the assay variation high...

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

    Directory of Open Access Journals (Sweden)

    Sabine Neusatz Guilhen

    2010-01-01

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

  9. [Measurement of thallium content in human urine by atomic absorption spectrometry after acute poisoning].

    Science.gov (United States)

    Luzanova, I S; Pletneva, T V; Maksimova, T V; Salomatin, E M; Lutskiĭ, Ia M

    2008-01-01

    The problem of poisoning with thallium-containing substances continues to be of current concern. According to the Bureau of Forensic Medical Examination, Moscow, specimens of biological materials from more than 20 victims of such poisoning were delivered for analysis in 2006. The total number of thallium poisoning episodes during the period since 1996 exceeded 50. Materials for thallium determination in biological fluids (human blood and urine) using flame atomic absorption spectrometry were prepared by dry mineralization of accurately weighed samples; acidic solutions of the products of mineralization were used for analysis. Due to peculiar kinetic features of thallium ion absorption in the gastro-intestinal tract, blood could not be used as a biological marker of poisoning. The level of thallium in urine samples was found to vary from 1.00 to 4,600 mcg/l (with the estimation of confidence intervals in each case). Results of chemical analysis correlated with pathological symptoms derived from the patients' discharge summaries and literature reports on dose-effect relationships. Based on these findings, practically all the examined cases were characterized as severe acute poisoning.

  10. 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.

  11. Determination of thallium in potassium chloride and electrolyte replenishers by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Nukatsuka, Isoshi; Horiguchi, Ryo; Seitoh, Hiroyuki; Ohzeki, Kunio; Miyashita, Fumihide

    2004-01-01

    Thallium in potassium chloride and electrolyte replenishers was determined by electrothermal atomic absorption spectrometry (ETAAS) with direct injection of a resin suspension. Thallium(III) was extracted on fine particles of a cellulose nitrate resin (CNR) from dilute HCl (pH 1.6) in the presence of ammonium pyrrolidine-1-carbodithioate. The CNR particles were collected on a membrane filter by filtration under suction, suspended in 1.0 mL 10mM HNO3, and then delivered directly to ETAAS as the suspension. The effects of chloride ions were thoroughly investigated. The results showed that the addition of 0.5mM NaCl to the suspension (10mM HNO3) was recommended, after CNR and a membrane filter holding the CNR were washed thoroughly with 0.025M HCl, to eliminate interference from chloride ions. No chemical modifier was required. Extraction from the solution containing up to 2M chloride ion was allowable. The proposed method gave a concentration factor of 50 for a 50 mL sample volume. The detection limit (3sigma, n = 5) was 1 ng (20 pg/mL). The relative standard deviation was 4.9% (n = 5) at 30 ng level of thallium. The content of thallium in potassium chloride was 15.7-32.8 ng/g, and in electrolyte replenishers was 0.18-4.16 ng/mL.

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

    Science.gov (United States)

    Borges, Aline R.; Becker, Emilene M.; François, Luciane L.; de Jesus, Alexandre; Vale, Maria Goreti R.; Welz, Bernhard; Dessuy, Morgana B.; de Andrade, Jailson B.

    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 NH4H2PO4 at 217.001 nm, and a mixture of H2SO4 + Ca and HNO3 + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material ;Trace Elements in Multi-Nutrient Fertilizer;. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part.

  13. An analytic model for accurate spring constant calibration of rectangular atomic force microscope cantilevers.

    Science.gov (United States)

    Li, Rui; Ye, Hongfei; Zhang, Weisheng; Ma, Guojun; Su, Yewang

    2015-10-29

    Spring constant calibration of the atomic force microscope (AFM) cantilever is of fundamental importance for quantifying the force between the AFM cantilever tip and the sample. The calibration within the framework of thin plate theory undoubtedly has a higher accuracy and broader scope than that within the well-established beam theory. However, thin plate theory-based accurate analytic determination of the constant has been perceived as an extremely difficult issue. In this paper, we implement the thin plate theory-based analytic modeling for the static behavior of rectangular AFM cantilevers, which reveals that the three-dimensional effect and Poisson effect play important roles in accurate determination of the spring constants. A quantitative scaling law is found that the normalized spring constant depends only on the Poisson's ratio, normalized dimension and normalized load coordinate. Both the literature and our refined finite element model validate the present results. The developed model is expected to serve as the benchmark for accurate calibration of rectangular AFM cantilevers.

  14. Determination of mercury and selenium in herbal medicines and hair by using a nanometer TiO{sub 2}-coated quartz tube atomizer and hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shun-Xing, E-mail: lishunxing@fjzs.edu.cn [Department of Chemistry and Environmental Science, Zhangzhou Normal University, Zhangzhou 363000 (China); Fujian Province University Key Laboratory of Analytical Science (Zhangzhou Normal University), Zhangzhou 363000 (China); Zheng, Feng-Ying [Department of Chemistry and Environmental Science, Zhangzhou Normal University, Zhangzhou 363000 (China); Fujian Province University Key Laboratory of Analytical Science (Zhangzhou Normal University), Zhangzhou 363000 (China); Cai, Shu-Jie; Cai, Tian-Shou [Department of Chemistry and Environmental Science, Zhangzhou Normal University, Zhangzhou 363000 (China)

    2011-05-15

    The nanometer TiO{sub 2} particle was coated onto the inner wall of a T-shaped quartz tube atomizer (QTA) and then was used as a new atomizer (NT-QTA) for the determination of Hg and Se by hydride generation atomic absorption spectrometry (HGAAS). After coating 67.4 mg TiO{sub 2} on a quartz tube, the analytical performance of NT-QTA-HGAAS was compared to conventional QTA-HGAAS and it was improved as follows: (a) the linear range of the calibration curves was expanded from 10.0-80.0 ng mL{sup -1} to 5.0-150.0 ng mL{sup -1} for Hg, and from 10.0-70.0 ng mL{sup -1} to 5.0-100.0 ng mL{sup -1} for Se; (b) the characteristic concentration of was decreased from 2.8 ng mL{sup -1}/1% to 1.1 ng mL{sup -1}/1% for Hg and from 1.2 ng mL{sup -1}/1% to 0.8 ng mL{sup -1}/1% for Se; and (c) the interference from the coexistence of As on the determination of Hg and Se could be eliminated. The achieved technique was applied for the determination of Hg and Se in herbal medicines and hair.

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

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

    A novel method was developed for the determination of calcium, magnesium, potassium, iron, copper, zinc, and manganese and phosphorous in various kinds of breads samples sold in Turkey by microwave plasma-atomic emission spectrometry (MIP-AES). Breads were dried at 100 °C for one day, ground thoroughly and then digested using nitric acid/hydrogen per oxide (3:1). The analytes in certified reference wheat flour and maize flour samples were determined in the uncertainty limits of the certified values as well as the analytes added to the mixture of ground bread and acid mixture prior to digestion were recovered quantitatively (>90%). Therefore, all determinations were made by linear calibration technique using aqueous standards. The LOD values for Ca, Cu, Fe, K, Mg, Mn, P and Zn were 13.1, 0.28, 4.47, 118, 1.10, 0.41, 7550 and 3.00 ng mL(-1), respectively. No spectral interference was detected at the working wavelengths of the analytes. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

    Chung, Yong Sam; Choi, Kwang Soon; Moon, Jong Hwa; Kim, Sun Ha; Lim, Jong Myoung; Kim, Young Jin; Quraishi, Shamshad Begum

    2003-05-01

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

  18. 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

  19. 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

  20. Determination of lead in hair and its segmental analysis by solid sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Baysal, Asli, E-mail: baysalas@itu.edu.t [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469, Maslak, Istanbul (Turkey); Akman, Suleyman, E-mail: akmans@itu.edu.t [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469, Maslak, Istanbul (Turkey)

    2010-04-15

    A rapid and practical solid sampling electrothermal atomic absorption spectrometric method was described for the determination of lead in scalp hair. Hair samples were washed once with acetone; thrice with distilled-deionized water and again once with acetone and dried at 75 deg. C. Typically 0.05 to 1.0 mg of dried samples were inserted on the platforms of solid sampling autosampler. The effects of pyrolysis temperature, atomization temperature, the amount of sample as well as addition of a modifier (Pd/Mg) and/or auxiliary digesting agents (hydrogen peroxide and nitric acid) and/or a surfactant (Triton X-100) on the recovery of lead were investigated. Hair samples were washed once with acetone; thrice with distilled-deionized water and again once with acetone and dried at 75 deg. C. Typically 0.05 to 1.0 mg of dried samples were inserted on the platforms of solid sampling autosampler. The limit of detection for lead (3sigma, N = 10) was 0.3 ng/g The addition of modifier, acids, oxidant and surfactant hardly improved the results. Due to the risk of contamination and relatively high blank values, the lead in hair were determined directly without adding any reagent(s). Finally, the method was applied for the segmental determination of lead concentrations in hair of different persons which is important to know when and how much a person was exposed to the analyte. For this purpose, 0.5 cm of pieces were cut along the one or a few close strands and analyzed by solid sampling.

  1. Determination of lead in hair and its segmental analysis by solid sampling electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Baysal, Asli; Akman, Suleyman

    2010-01-01

    A rapid and practical solid sampling electrothermal atomic absorption spectrometric method was described for the determination of lead in scalp hair. Hair samples were washed once with acetone; thrice with distilled-deionized water and again once with acetone and dried at 75 deg. C. Typically 0.05 to 1.0 mg of dried samples were inserted on the platforms of solid sampling autosampler. The effects of pyrolysis temperature, atomization temperature, the amount of sample as well as addition of a modifier (Pd/Mg) and/or auxiliary digesting agents (hydrogen peroxide and nitric acid) and/or a surfactant (Triton X-100) on the recovery of lead were investigated. Hair samples were washed once with acetone; thrice with distilled-deionized water and again once with acetone and dried at 75 deg. C. Typically 0.05 to 1.0 mg of dried samples were inserted on the platforms of solid sampling autosampler. The limit of detection for lead (3σ, N = 10) was 0.3 ng/g The addition of modifier, acids, oxidant and surfactant hardly improved the results. Due to the risk of contamination and relatively high blank values, the lead in hair were determined directly without adding any reagent(s). Finally, the method was applied for the segmental determination of lead concentrations in hair of different persons which is important to know when and how much a person was exposed to the analyte. For this purpose, 0.5 cm of pieces were cut along the one or a few close strands and analyzed by solid sampling.

  2. Speciation analysis of arsenic compounds in seafood by ion chromatography-atomic fluorescence spectrometry

    Science.gov (United States)

    Han, Tingting; Ji, Hongwei; Li, Huixin; Cui, He; Song, Tian; Duan, Xiaojuan; Zhu, Qianlin; Cai, Feng; Zhang, Li

    2017-06-01

    Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine (AsB), arsenite (As(III)), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), and arsenate (As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L-1 CH3COONH4 and 15 mmol L-1 Na2CO3 with 10 mL CH3CH2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%-109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L-1 for AsB, 0.426 μg L-1 for As(III), 0.216 μg L-1 for DMA, 0.211 μg L-1 for MMA, and 0.709 μg L-1 for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.

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

    International Nuclear Information System (INIS)

    Rey-Raap, Natalia; Gallardo, Antonio

    2012-01-01

    Highlights: ► New treatments for CFL are required considering the aim of Directive 202/96/CE. ► It is shown that most of the mercury introduced into a CFL is in the phosphor powder. ► Experimental conditions for microwave-assisted sample digestion followed by AAS measurements are described. ► By washing the glass it is possible to reduce the concentration below legal limits. - Abstract: In this study, spent compact fluorescent lamps were characterized to determine the distribution of mercury. The procedure used in this research allowed mercury to be extracted in the vapor phase, from the phosphor powder, and the glass matrix. Mercury concentration in the three phases was determined by the method known as cold vapor atomic absorption spectrometry. Median values obtained in the study showed that a compact fluorescent lamp contained 24.52 ± 0.4 ppb of mercury in the vapor phase, 204.16 ± 8.9 ppb of mercury in the phosphor powder, and 18.74 ± 0.5 ppb of mercury in the glass matrix. There are differences in mercury concentration between the lamps since the year of manufacture or the hours of operation affect both mercury content and its distribution. The 85.76% of the mercury introduced into a compact fluorescent lamp becomes a component of the phosphor powder, while more than 13.66% is diffused through the glass matrix. By washing and eliminating all phosphor powder attached to the glass surface it is possible to classified the glass as a non-hazardous waste.

  4. Incorporating nuclear vibrational energies into the "atom in molecules" analysis: An analytical study.

    Science.gov (United States)

    Gharabaghi, Masumeh; Shahbazian, Shant

    2017-04-21

    The quantum theory of atoms in molecules (QTAIM) is based on the clamped nucleus paradigm and solely working with the electronic wavefunctions, so does not include nuclear vibrations in the AIM analysis. On the other hand, the recently extended version of the QTAIM, called the multi-component QTAIM (MC-QTAIM), incorporates both electrons and quantum nuclei, i.e., those nuclei treated as quantum waves instead of clamped point charges, into the AIM analysis using non-adiabatic wavefunctions. Thus, the MC-QTAIM is the natural framework to incorporate the role of nuclear vibrations into the AIM analysis. In this study, within the context of the MC-QTAIM, the formalism of including nuclear vibrational energy in the atomic basin energy is developed in detail and its contribution is derived analytically using the recently proposed non-adiabatic Hartree product nuclear wavefunction. It is demonstrated that within the context of this wavefunction, the quantum nuclei may be conceived pseudo-adiabatically as quantum oscillators and both isotropic harmonic and anisotropic anharmonic oscillator models are used to compute the zero-point nuclear vibrational energy contribution to the basin energies explicitly. Inspired by the results gained within the context of the MC-QTAIM analysis, a heuristic approach is proposed within the context of the QTAIM to include nuclear vibrational energy in the basin energy from the vibrational wavefunction derived adiabatically. The explicit calculation of the basin contribution of the zero-point vibrational energy using the uncoupled harmonic oscillator model leads to results consistent with those derived from the MC-QTAIM.

  5. Atomic force bio-analytics of polymerization and aggregation of phycoerythrin-conjugated immunoglobulin G molecules

    Science.gov (United States)

    Chen, Yong; Cai, Jiye; Xu, Qingcai; Chen, Zheng W.

    2010-01-01

    While bio-labeled immunoglobulin (IgG) or antibodies are extensively used in imaging studies and therapeutic modality, there have been no reports describing atomic force microscopy (AFM) micrographs of these labeled IgG molecules. Here, AFM studies of phycoerythrin (PE)-conjugated IgG were undertaken to examine whether PE conjugation induced conformational changes or molecular interaction, and subsequently resulted in an alteration in nano-structures of PE-conjugated IgG complex. Once immobilized on mica, single PE-conjugated IgG molecule exhibited globular shape with approximately 60 microns in diameter and 5 microns in height. PE-conjugated IgG were able to form monomers, spindle-like trimers, and hexamers that developed through an end–end connection of two trimers, after they were continuously immobilized on mica. Interestingly, these multimers could aggregate in different directions to form circular monolayers with a highly dense core of PE-conjugated IgG polymers. The formation of these well-organized polymers and aggregates of PE-conjugated IgG may be attributed to the PE conjugation as well as the air–liquid tension on subtract. These findings may help to understand the nano-structures of bio-labeled IgG or antibodies, and facilitate the potential use of PE-conjugated antibodies as markers or immunosensers for AFM bio-analytics of biomolecules in cells and membranes. PMID:15482861

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

    Science.gov (United States)

    Yamamoto, Yuhei; Shirasaki, Toshihiro; Yonetani, Akira; Imai, Shoji

    2015-01-01

    The measurement conditions for determining boron using graphite furnace-atomic absorption spectrometry (GF-AAS) were investigated. Differences in the boron absorbance profiles were found using three different commercially available GF-AAS instruments when the graphite atomizers in them were not tuned. The boron absorbances found with and without adjusting the graphite atomizers suggested that achieving an adequate absorbance for the determination of boron requires a sharp temperature profile that overshoots the target temperature during the atomization process. Chemical modifiers that could improve the boron absorbance without the need for using coating agents were tested. Calcium carbonate improved the boron absorbance but did not suppress variability in the peak height. Improvement of boron absorbance was comparatively less using iron nitrate or copper nitrate than using calcium carbonate, but variability in the peak height was clearly suppressed using iron nitrate or copper nitrate. The limit of detection was 0.0026 mg L(-1) when iron nitrate was used. It appears that iron nitrate is a useful new chemical modifier for the quick and simple determination of boron using GF-AAS.

  7. Continuous Liquid-Sample Introduction for Bunsen Burner Atomic Emission Spectrometry.

    Science.gov (United States)

    Smith, Gregory D.; And Others

    1995-01-01

    Describes a laboratory-constructed atomic emission spectrometer with modular instrumentation components and a simple Bunsen burner atomizer with continuous sample introduction. A schematic diagram and sample data are provided. (DDR)

  8. A dual platform for selective analyte enrichment and ionization in mass spectrometry using aptamer-conjugated graphene oxide.

    Science.gov (United States)

    Gulbakan, Basri; Yasun, Emir; Shukoor, M Ibrahim; Zhu, Zhi; You, Mingxu; Tan, Xiaohong; Sanchez, Hernan; Powell, David H; Dai, Hongjie; Tan, Weihong

    2010-12-15

    This study demonstrates the use of aptamer-conjugated graphene oxide as an affinity extraction and detection platform for analytes from complex biological media. We have shown that cocaine and adenosine can be selectively enriched from plasma samples and that direct mass spectrometric readouts can be obtained without a matrix and with greatly improved signal-to-noise ratios. Aptamer-conjugated graphene oxide has clear advantages in target enrichment and in generating highly efficient ionization of target molecules for mass spectrometry. These results demonstrate the utility of the approach for analysis of small molecules in real biological samples.

  9. 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

  10. The use of silver nanoparticles as an effective modifier for the determination of arsenic and antimony by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-04-15

    Silver nanoparticles (AgNPs) were proposed as a new chemical modifier for the elimination of interferences when determining arsenic and antimony in aqueous NaCl or Na{sub 2}SO{sub 4} solutions and in sea-water by electrothermal atomic absorption spectrometry. For this purpose, the AgNPs were prepared simply by reducing silver nitrate with sodium citrate. The effects of pyrolysis and atomization temperatures and the amounts of interferents and modifiers on the sensitivities of these elements were investigated. In the presence of the proposed modifier, a pyrolysis temperature of at least 1100 deg. C for arsenic and 900 deg. C for antimony could be applied without the loss of analytes, and the interferences were greatly reduced to allow for interference-free determination. The detection limits (N = 10, 3sigma) for arsenic and antimony were 0.022 ng and 0.046 ng, respectively. AgNPs are cheaper and more available compared to many other modifiers. No background was detected, and the blank values were negligible.

  11. Poly(etheretherketone)-turnings a novel sorbent material for lead determination by flow injection flame atomic absorption spectrometry and factorial design optimization.

    Science.gov (United States)

    Anthemidis, Aristidis N; Adam, Ibrahim S I; Zachariadis, George A

    2010-05-15

    A novel hydrophobic sorbent material for on-line column preconcentration and separation systems coupled with atomic spectrometry was developed. Poly(etheretherketone) (PEEK) in the form of turnings was used as packing material and evaluated for trace lead determination in environmental samples. Sample and ammonium diethyl-dithiophosphate (DDPA) reagent were mixed on-line and the Pb(II)-DDPA complex was retained effectively on PEEK-turnings. Isobutyl methyl ketone (IBMK) was adopted for efficient analyte complex elution and subsequently transportation into the nebulizer-burner system for atomization. The developed sorbent material has shown, excellent chemical and mechanical resistance, fast adsorption kinetics permitting the use of high sample flow rates without significant loss of retention efficiency. For 120s sample preconcentration time the sampling frequency was 20h(-1), the enhancement factor was 110, the detection limit (3s) was c(L)=0.32microgL(-1), and the relative standard deviation (RSD) was s(R)=2.2%, at the 50.0microgL(-1) Pb(II) level. The accuracy of the developed method was evaluated by analyzing certified reference materials.

  12. 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.

  13. Stibine preconcentration in a quartz trap with subsequent atomization in the quartz multiatomizer for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Korkmaz, D.; Dědina, Jiří; Ataman, O. Y.

    2004-01-01

    Roč. 19, č. 2 (2004), s. 255-259 ISSN 0267-9477 R&D Projects: GA ČR GA203/01/0453 Institutional research plan: CEZ:AV0Z4031919 Keywords : stibine preconcentration * quartz multiatomizer * efficiency Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2004

  14. Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

    Science.gov (United States)

    Brombach, Christoph-Cornelius; Chen, Bin; Corns, Warren T.; Feldmann, Jörg; Krupp, Eva M.

    2015-03-01

    Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography-cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation.

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

    International Nuclear Information System (INIS)

    Naveen Kumar, P.; Sanjay Kumar; Vijay Kumar; Nandakishore, S.S.; Bangroo, P.N.

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-08-15

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

  17. Sea sponge as a low cost biosorbent for solid phase extraction of some heavy metal ions and determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Karatepe, Aslihan; Soylak, Mustafa

    2014-01-01

    A new, easy, sensitive, and environmentally friendly separation and preconcentration method was developed to determine Cu(ll), Fe(lll), Pb(ll), and Ni(ll) at trace levels by use of a column filled with sea sponge without any complexing reagent, and atomic absorption spectrometry. The influences of analytical parameters, such as pH of the solutions, type of eluent, volume of sample, solution and eluent flow rates, and diverse ions, were examined for the quantitative recoveries of the analyte ions. The metal ions were eluted from the column by using 2 M HNO3. Accurate results were found for spiked samples after applying the preconcentration method. The LOD values were found to be between 1.5 and 5.6 μg/L based on three times the SD of the blanks. The method has been successfully applied to determine Cu(ll), Fe(lll), Pb(ll), and Ni(ll) ions in tap water samples, mineral water samples, and a certified reference material.

  18. Sulfur-nanoparticle-based method for separation and preconcentration of some heavy metals in marine samples prior to flame atomic absorption spectrometry determination.

    Science.gov (United States)

    Ghanemi, Kamal; Nikpour, Yadollah; Omidvar, Omid; Maryamabadi, Ammar

    2011-07-15

    The application of sulfur-nanoparticle-loaded alumina as an efficient adsorbent for the solid-phase extraction (SPE) and determination of trace amounts of Cd, Cu, Zn, and Pb ions was investigated in marine samples using flame atomic absorption spectrometry (FAAS). The nanometer-sized sulfur particles were synthesized in situ, physically loaded onto alumina microparticles, and the parameters influencing the preconcentration of the analytes, such as the pH, solution flow rate and volume, eluent solution, and interfering ions, were examined. The results showed that the optimal conditions for quantitative recovery of the metal ions by adsorption and elution on the sulfur nanoparticles (SNPs) was achieved by employing a flow rate of 15 mL min(-1), a pH of 8.5 for the sample solutions, and an eluent composed of 3.0 mol L(-1) HNO(3) in methanol. The detection limits of this method for Cd, Zn, Cu, and Pb ions were 0.30, 0.21, 0.24, and 0.63 μg L(-1) (n=10), respectively. Application of the proposed method to the analysis of fish certified reference material (DORM-3) produced results that were in good agreement with the certified values. The proposed method was also successfully applied to the determination of analytes in marine samples, including seawater, fish, and oysters. Copyright © 2011 Elsevier B.V. All rights reserved.

  19. Problems, possibilities and limitations of inductively coupled plasma atomic emission spectrometry in the determination of platinum, palladium and rhodium in samples with different matrix composition

    Science.gov (United States)

    Petrova, P.; Velichkov, S.; Velitchkova, N.; Havezov, I.; Daskalova, N.

    2010-02-01

    The economic and geological importance of platinum group of elements has led to the development of analytical methods to quantify them in different types of samples. In the present paper the quantitative information for spectral interference in radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometry in the determination of Pt, Pd and Rh in the presence of complex matrix, containing Al, Ca, Fe, Mg, Mn, P and Ti as matrix constituents was obtained. The database was used for optimum line selections. By using the selected analysis lines the following detection limits in ng g - 1 were obtained: Pt 1700, Pd-1440, Rh-900. The reached detection limits determine the possibilities and limitation of the direct ICP-AES method in the determination of Pt, Pd and Rh in geological and environmental materials. The database for spectral interferences in the presence of aluminum can be used for the determination of platinum group of elements in car catalysts. The accuracy of the analytical results was experimentally demonstrated by two certified reference materials that were analyzed: SARM 7, Pt ore and recycled auto-catalyst certified reference material SRM 2556.

  20. Problems, possibilities and limitations of inductively coupled plasma atomic emission spectrometry in the determination of platinum, palladium and rhodium in samples with different matrix composition

    International Nuclear Information System (INIS)

    Petrova, P.; Velichkov, S.; Velitchkova, N.; Havezov, I.; Daskalova, N.

    2010-01-01

    The economic and geological importance of platinum group of elements has led to the development of analytical methods to quantify them in different types of samples. In the present paper the quantitative information for spectral interference in radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometry in the determination of Pt, Pd and Rh in the presence of complex matrix, containing Al, Ca, Fe, Mg, Mn, P and Ti as matrix constituents was obtained. The database was used for optimum line selections. By using the selected analysis lines the following detection limits in ng g -1 were obtained: Pt 1700, Pd-1440, Rh-900. The reached detection limits determine the possibilities and limitation of the direct ICP-AES method in the determination of Pt, Pd and Rh in geological and environmental materials. The database for spectral interferences in the presence of aluminum can be used for the determination of platinum group of elements in car catalysts. The accuracy of the analytical results was experimentally demonstrated by two certified reference materials that were analyzed: SARM 7, Pt ore and recycled auto-catalyst certified reference material SRM 2556.

  1. 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.

  2. 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).

  3. 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).

  4. [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.

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

    DEFF Research Database (Denmark)

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

    1996-01-01

    A flow injection procedure for the determination of ultra-trace amounts of selenium(IV) is described, which combines hydride generation atomic absorption spectrometry (HGAAS) with on-line preconcentration of the analyte by co-precipitation-dissolution in a filterless knotted Microline reactor...... with hydrochloric acid, allowing an ensuing determination via hydride generation. At different sample flow rates, i.e., 4.8, 6.4 and 8.8 ml/min, enrichment factors of 30, 40 and 46, respectively, were obtained at a sampling frequency of 33 samples/h. The detection limit (3s) was 0.005 µg/l at a sample flow rate...

  6. An analytical method for determination of mercury by cold vapor atomic absorption spectroscopy; Determinazione di mercurio. Metodo per spettrometria di assorbimento atomico a vapori freddi (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Campanella, L. [Rome Univ. La Sapienza, Rome (Italy); Mastroianni, D.; Capri, S.; Pettine, M. [CNR, Rome (Italy). Ist. di Ricerca sulle Acque; Spezia, S.; Bettinelli, M. [ENEL, Unified Modelling Language, Piacenza (Italy)

    1999-09-01

    An analytical procedure for the determination of total mercury in wastewaters and natural waters is described. Aqueous samples are fast digested with nitric acid by using the microwave-oven technique; the analysis of mercury is then performed by cold vapor atomic absorption spectrometry (CV-AAS) using two possible instrumental apparatus (batch system or flow injection). Sodium borohydride is used as the reducing agent for mercury in solution (Method A). The use of amalgamation traps on gold for the preconcentration of mercury lowers the detection limit of the analyte (Method B). [Italian] Viene descritta una procedura analitica per la determinazione del mercurio totale in acque di scarico e naturali. Il campione acquoso viene sottoposto a mineralizzazione con acido nitrico in forno a microonde e analizzato mediante spettroscopia di assorbimento atomico a vapori freddi (CV-AAS) in due possibili configurazioni strumentali (sistema batch oppure flow injection), utilizzando sodio boro idruro come agente riducente del mercurio (metodo A). L'impiego della trappola di oro per la preconcentrazione del mercurio mediante amalgama consente di determinare l'analita a livelli di pochi ng/L (metodo B).

  7. Flame and graphite furnace atomic absorption spectrometry for trace element determination in vegetable oils, margarine and butter after sample emulsification.

    Science.gov (United States)

    Ieggli, C V S; Bohrer, D; Do Nascimento, P C; De Carvalho, L M

    2011-05-01

    Trace element analysis plays an important role in oil characterisation and in the detection of oil adulteration because the quality of edible oils and fats is affected by their trace metal content. In this study, the quantification of selected metals in various oils and fats (rice oil, canola oil, sunflower oil, corn oil, soy oil, olive oil, light margarine, regular margarine and butter) was carried out using flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after sample emulsification. FAAS was used to determine the Na, K, Ca, Mg, Zn and Fe levels in the samples, while GFAAS was used for quantifying Cr, Ni, As, Pb, Cd, Cu and Mn, as these elements appeared in the samples at much lower concentrations. Tween-80 and Triton X-100 were employed as surfactants, and emulsions were prepared by a conventional method that involved heating and mixing of the constituents. Complete stabilisation was achieved through magnetic stirring for 15 min at room temperature. The evaluated figures of merit were linearity, accuracy and sensitivity, which were determined by the characteristic concentration and mass. Analysis of spiked samples demonstrated accuracy, which ranged from 90% (Na) to 112% (Fe) for FAAS and from 83% (Cd) to 121% (Pb) for GFAAS measurements. Atomic absorption spectrometry proved to be a promising approach for the analysis of metals in emulsified edible oils and fats. Additionally, under appropriate emulsification conditions (formulation, stirring time and temperature), the emulsions were homogeneous, had excellent stability, and had appropriate viscosity. The proposed method has proved to be simple, sensitive, reproducible, and economical.

  8. Total uncertainty budget calculation for the determination of mercury in incineration ash (BCR 176R) by atomic fluorescence spectrometry.

    Science.gov (United States)

    Tirez, Kristof; Beutels, Filip; Brusten, Wilfried; Noten, Bart; De Brucker, Nicole

    2002-11-01

    The mercury mass fraction has been determined by atomic fluorescence spectrometry (AFS) in the framework of the project "Certification of a reference material (trace elements in fly ash) in replacement of BCR CRM 176". Calculation of the uncertainty budget, as described in this manuscript, emphasizes a practical and realistic approach to estimation of uncertainty components on the basis of statistical assumptions. GUM Workbench software was used, and resulted in a mercury mass fraction of 1.58+/-0.11 mg kg(-1) (with coverage factor k=2.2, 95% probability) related to dry mass, submitted in the certification exercise. The calculated total uncertainty budget applies to analogous samples analyzed by this procedure.

  9. 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

  10. 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)

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

    International Nuclear Information System (INIS)

    Lopez-Garcia, Ignacio; Briceno, Marisol; Hernandez-Cordoba, Manuel

    2011-01-01

    Highlights: → Arsenic in fish-based food samples can be determined without the need of a dissolution stage. → Speciation of the main forms of arsenic in fish-based baby foods does not require chromatography. → The behavior of arsenic compounds in ETAAS strongly depends on the chemical modifier used. - Abstract: A procedure for the speciation analysis of arsenic in fish-based baby foods is presented. Inorganic arsenic, methylarsonic acid (MA), dimethylarsinic acid (DMA) and arsenobetaine (AB) were determined by electrothermal atomic absorption spectrometry (ETAAS) using suspensions prepared in a 0.01 mol L -1 tetramethylammonium hydroxide (TMAH) solution. Speciation is based on the use of three different chemically modified ETAAS atomizers to obtain the analytical signals. Using a palladium salt as the chemical modifier, the signal corresponding to the total arsenic concentration is obtained. When palladium is replaced by Ce(IV), the signal is solely due to inorganic arsenic (III and V) + MA. If no signal is obtained in this latter case, it is possible to distinguish between DMA and AB using a zirconium coated atomizer. The signal obtained in this way is due solely to DMA, and the concentration of AB can be obtained by the difference with the total arsenic content. Determinations by ETAAS require the use of the standard additions method. The limits of detection for the determination of AB, DMA and inorganic arsenic (+MA) are 15, 25 and 50 ng g -1 expressed as arsenic, respectively. These detection limits are good enough for the procedure to be appropriate for the rapid determination of these compounds, avoiding extraction processes and/or chromatographic separations. Data for commercial samples, as well as for four standard reference materials, are given.

  12. Investigation of chemical modifiers for the determination of lead in fertilizers and limestone using graphite furnace atomic absorption spectrometry with Zeeman-effect background correction and slurry sampling

    Science.gov (United States)

    Borges, Aline R.; Becker, Emilene M.; Dessuy, Morgana B.; Vale, Maria Goreti R.; Welz, Bernhard

    2014-02-01

    In this work, chemical modifiers in solution (Pd/Mg, NH4H2PO4 and NH4NO3/Pd) were compared with permanent modifiers (Ir and Ru) for the determination of lead in fertilizer and limestone samples using slurry sampling and graphite furnace atomic absorption spectrometry with Zeeman-effect background correction. The analytical line at 283.3 nm was used due to some spectral interference observed at 217.0 nm. The NH4H2PO4 was abandoned due to severe spectral interference even at the 283.3-nm line. For Pd/Mg and NH4NO3/Pd the optimum pyrolysis and atomization temperatures were 900 °C and 1900 °C, respectively. For Ru and Ir, the integrated absorbance signal was stable up to pyrolysis temperatures of 700 °C and 900 °C, respectively, and up to atomization temperature of 1700 °C. The limit of detection (LOD) was 17 ng g- 1 using Pd/Mg and 29 ng g- 1 using NH4NO3/Pd. Among the permanent modifiers investigated, the LOD was 22 ng g- 1 Pb for Ir and 10 ng g- 1 Pb for Ru. The accuracy of the method was evaluated using the certified reference material NIST SRM 695. Although Ru provided lower LOD, which can be attributed to a lower blank signal, only the modifiers in solution showed concordant values of Pb concentration for the NIST SRM 695 and the most of analyzed samples. Moreover, the Pd/Mg modifier provided the highest sensitivity and for this reason it is more suitable for the determination of Pb in fertilizers samples in slurry; besides this it presented a better signal-to-noise ratio than NH4NO3/Pd.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-01

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

  14. Analytic solution of a relativistic two-dimensional hydrogen-like atom in a constant magnetic field

    International Nuclear Information System (INIS)

    Villalba, V.M.

    1998-01-01

    We obtain exact solutions of the Klein-Gordon and Pauli-Schroedinger equations for a two-dimensional hydrogen-like atom in the presence of a constant magnetic field. Analytic solutions for the energy spectrum are obtained for particular values of the magnetic field strength. The results are compared to those obtained in the non-relativistic and spinless case. We obtain that the relativistic spectrum does not present s states. (orig.)

  15. Analytical approaches for Hg determination in wastewater samples by means of total reflection X-ray fluorescence spectrometry.

    Science.gov (United States)

    Marguí, E; Kregsamer, P; Hidalgo, M; Tapias, J; Queralt, I; Streli, C

    2010-07-15

    At present, there is a considerable interest in Hg monitoring in wastewater samples due to its widespread occurrence and the high toxicity of most of its compounds. Hg determination in water samples by means of total reflection X-ray fluorescence spectrometry (TXRF) entails some difficulties due to the high vapor pressure and low boiling point of this element that produce evaporation and loss of Hg from the surface of the reflector during the drying process, commonly used for sample preparation in TXRF analysis. The main goal of the present research was to develop a fast and simple chemical strategy to avoid Hg volatilization during the analysis of wastewater samples by TXRF spectrometry. Three different analytical procedures were tested for this purpose: (i) increasing the viscosity of the wastewater sample by adding a non-ionic surfactant (Triton X-114), (ii) Hg immobilization on the quartz reflectors using the extractant tri-isobutylphosphine (Cyanex 471X) and (iii) formation of a stable and non-volatile Hg complex into the wastewater sample. The best analytical strategy was found to be the formation of a Hg complex with thiourea (pH=10) before the deposition of 10 microL of sample on the reflector for following TXRF analysis. Analytical figures of merit such as linearity, limits of detection, accuracy and precision were carefully evaluated. Finally, the developed methodology was applied for the determination of Hg in different types of wastewater samples (industrial effluents, municipal effluents from conventional systems and municipal effluents from constructed wetlands). Copyright 2010 Elsevier B.V. All rights reserved.

  16. Open Access UHPSFC/MS - an additional analytical resource for an academic mass spectrometry facility.

    Science.gov (United States)

    Herniman, Julie M; Langley, G John

    2016-08-15

    Many compounds submitted for analysis in Chemistry at the University of Southampton do not retain, elute or ionize using open access reversed-phase ultra-high-performance liquid chromatography/mass spectrometry (RP-UHPLC/MS) and require analysis via infusion. An ultra-high-performance supercritical fluid chromatography mass spectrometry approach was implemented to afford high-throughput analysis of these compounds with chromatographic separation. A UPC(2) -TQD MS system has been incorporated into the open access MS provision within Chemistry at the University of Southampton, using an ESCi source (electrospray and atmospheric pressure chemical ionization) and an atmospheric pressure photoionization (APPI) source. Access to instrumentation is enabled via a web-based interface (RemoteAnalyzer™). Compounds such as fluorosugars, fullerenes, phosphoramidites, porphyrins, and rotaxanes exhibiting properties incompatible with RP-UHPLC/MS have been analyzed using automated chromatography and mass spectrometry methods. The speedy return of data enables research in these areas to progress unhindered by sample type. The provision of an electronic web format enables easy incorporation of chromatograms and mass spectra into electronic files and reports. The implementation of UHPSFC/MS increases access to a wide range of chemistries incompatible with reversed-phase chromatography and polar solvents, enabling more than 90% of submitted samples to be analyzed using an open access approach. Further, chromatographic separation is provided where previously flow injection or infusion analyses were the only options. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  17. Atoms

    International Nuclear Information System (INIS)

    Fuchs, Alain; Villani, Cedric; Guthleben, Denis; Leduc, Michele; Brenner, Anastasios; Pouthas, Joel; Perrin, Jean

    2014-01-01

    Completed by recent contributions on various topics (atoms and the Brownian motion, the career of Jean Perrin, the evolution of atomic physics since Jean Perrin, relationship between scientific atomism and philosophical atomism), this book is a reprint of a book published at the beginning of the twentieth century in which the author addressed the relationship between atomic theory and chemistry (molecules, atoms, the Avogadro hypothesis, molecule structures, solutes, upper limits of molecular quantities), molecular agitation (molecule velocity, molecule rotation or vibration, molecular free range), the Brownian motion and emulsions (history and general features, statistical equilibrium of emulsions), the laws of the Brownian motion (Einstein's theory, experimental control), fluctuations (the theory of Smoluchowski), light and quanta (black body, extension of quantum theory), the electricity atom, the atom genesis and destruction (transmutations, atom counting)

  18. Analytical Absorption Cross-Section for Photon by a Hydrogen 2s Atom

    International Nuclear Information System (INIS)

    Ndinya, Boniface Otieno; Okeyo, Stephen Onyango

    2011-01-01

    We calculate the absorption cross-section for photon by a hydrogen 2s atom using the quantum-classical approximation for the total photo cross-section of many electron atoms. With the application of the first-order term of the Baker-Hausdorf expansion, the absorption cross-section for the hydrogen 2s atom decreases to a minimum, the Cooper pair minimum, at low photon energy. Such a minimum is absent in the exact absorption cross-section for photon by a hydrogen 2s atom. We have extended the calculation for the absorption cross-section of the hydrogen 2s atom using the quantum-classical approximation for the total photo cross-section of many electron to include the second-order term of the Baker-Hausdorf expansion and observed a great reduction in the dip associated with the Cooper pair minimum at the zero crossing. (atomic and molecular physics)

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

    Energy Technology Data Exchange (ETDEWEB)

    Brum, Daniel M.; Lima, Claudio F. [Departamento de Quimica, Universidade Federal de Vicosa, A. Peter Henry Rolfs s/n, Vicosa/MG, 36570-000 (Brazil); Robaina, Nicolle F. [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil); Fonseca, Teresa Cristina O. [Petrobras, Cenpes/PDEDS/QM, Av. Horacio Macedo 950, Ilha do Fundao, Rio de Janeiro/RJ, 21941-915 (Brazil); Cassella, Ricardo J., E-mail: cassella@vm.uff.br [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil)

    2011-05-15

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO{sub 3}, the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO{sub 3} medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  20. 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.

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

    International Nuclear Information System (INIS)

    Brum, Daniel M.; Lima, Claudio F.; Robaina, Nicolle F.; Fonseca, Teresa Cristina O.; Cassella, Ricardo J.

    2011-01-01

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO 3 , the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO 3 medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  2. A fully analytical integration of properties over the 3D volume of the β sphere in topological atoms

    Science.gov (United States)

    2018-01-01

    Atomic multipole moments associated with a spherical volume fully residing within a topological atom (i.e., the β sphere) can be obtained analytically. Such an integration is thus free of quadrature grids. A general formula for an arbitrary rank spherical harmonic multipole moment is derived, for an electron density comprising Gaussian primitives of arbitrary angular momentum. The closed expressions derived here are also sufficient to calculate the electrostatic potential, the two types of kinetic energy, as well as the potential energy between atoms. Some integrals have not been solved explicitly before but through recursion and substitution are broken down to more elementary listed integrals. The proposed method is based on a central formula that shifts Gaussian primitives from one center to another, which can be derived from the well‐known plane‐wave expansion (or Rayleigh equation). © 2018 The Authors. Journal of Computational Chemistry Published by Wiley Periodicals, Inc. PMID:29322516

  3. Analytical Model of the Nonlinear Dynamics of Cantilever Tip-Sample Surface Interactions for Various Acoustic-Atomic Force Microscopies

    Science.gov (United States)

    Cantrell, John H., Jr.; Cantrell, Sean A.

    2008-01-01

    A comprehensive analytical model of the interaction of the cantilever tip of the atomic force microscope (AFM) with the sample surface is developed that accounts for the nonlinearity of the tip-surface interaction force. The interaction is modeled as a nonlinear spring coupled at opposite ends to linear springs representing cantilever and sample surface oscillators. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a standard iteration procedure. Solutions are obtained for the phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) techniques including force modulation microscopy, atomic force acoustic microscopy, ultrasonic force microscopy, heterodyne force microscopy, resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), and the commonly used intermittent contact mode (TappingMode) generally available on AFMs. The solutions are used to obtain a quantitative measure of image contrast resulting from variations in the Young modulus of the sample for the amplitude and phase images generated by the A-AFM techniques. Application of the model to RDF-AFUM and intermittent soft contact phase images of LaRC-cp2 polyimide polymer is discussed. The model predicts variations in the Young modulus of the material of 24 percent from the RDF-AFUM image and 18 percent from the intermittent soft contact image. Both predictions are in good agreement with the literature value of 21 percent obtained from independent, macroscopic measurements of sheet polymer material.

  4. 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

  5. Spectrochemical analysis by atomic absorption and emission

    National Research Council Canada - National Science Library

    Lajunen, Lauri

    1992-01-01

    ... of these techniques. Inductively coupled plasma mass spectrometry (ICP-MS) has become a 'hot' analytical technique during the last few years, and is being used in many branches of science. Since the publication of my previous book 'Atomispektrometria' (in Finnish) in 1986, various techniques in analytical atomic spectroscopy have undergone significant dev...

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

    International Nuclear Information System (INIS)

    Borderie, B.

    1980-01-01

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

  7. Understanding the fate of chlorogenic acids in coffee roasting using mass spectrometry based targeted and non-targeted analytical strategies.

    Science.gov (United States)

    Jaiswal, Rakesh; Matei, Marius F; Golon, Agnieszka; Witt, Matthias; Kuhnert, Nikolai

    2012-09-01

    Coffee is one of mankind's most popular beverages obtained from green coffee beans by roasting. Much effort has been expended towards the chemical characterisation of the components of the roasted coffee bean, frequently termed melanoidines, which are dominated byproducts formed from its most relevant secondary metabolites - chlorogenic acids. However, impeded by a lack of suitable authentic reference standards and analytical techniques sufficiently powerful for providing insight into an extraordinarily complex enigmatic material, unsurprisingly little structural and mechanistic information about the products of coffee roasting is available. Here we report on the characterisation of low molecular weight melanoidine fractions of roasted coffee using a conceptually novel combination of targeted and non-targeted mass spectrometrical techniques. We provide an unprecedented account of the chemical composition of roasted coffee beans. Using a targeted analytical approach we show for the first time, by comparison to authentic reference standards obtained by chemical synthesis, that chlorogenic acids follow four distinct reaction pathways including epimerization, acyl migration, lactonisation and dehydration. The analytical strategy employed in a non-targeted approach uses high resolution mass spectrometry to identify the most abundant molecular formulas present in roasted coffee samples and model roasts followed by van Krevelen and homologous series analysis. We identified the molecular formulas formed from reactions of chlorogenic acids, carbohydrates and proteins, both between classes of compounds and within same classes of compounds. Furthermore, we identified two new classes of compounds formed from chlorogenic acids during roasting, chlorogenic acid acetates and O-phenolic quinoyl and shikimoyl esters of chlorogenic acids.

  8. Metal-binding proteins scanning and determination by combining gel electrophoresis, synchrotron radiation X-ray fluorescence and atomic spectrometry.

    Science.gov (United States)

    Verbi, F M; Arruda, S C C; Rodriguez, A P M; Pérez, C A; Arruda, M A Z

    2005-02-28

    In the present work, protein bands from in vitro embriogenic callus (Citrus sinensis L. Osbeck) were investigated using micro-synchrotron radiation X-ray fluorescence (muSR-XRF) after sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) separation. Metal-binding protein quantification was done after microwave oven decomposition of gel by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF), flame atomic absorption spectrometry (FAAS) and flame atomic emission spectrometry (FAES). According to the analysis of the protein bands, it is possible to observe that both 81 and ca. 14 kDa proteins present different Fe signal intensity at different positions. The analysis of 53 kDa protein, showed even more interesting results. Besides Fe, the muSR-XRF experiments indicate the presence of Ca, Cu, K and Zn. Chemical elements such as Cu, K, Fe and Zn were determined by SR-TXRF, Mg by FAAS and Na by FAES. Ca was determined by SR-TXRF and FAAS only for accuracy check. In the mineralised protein bands of 81 and around 14 kDa band, only Fe was determined (105 and 21.8 microg g(-1)). For those protein bands (86-ca. 14 kDa) were determined, Ca, K, Cu and Zn in a wide concentration range (42.4-283, 2.47-96.8, 0.91-15.9 and 3.39-29.7 microg g(-1), respectively).

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-03-31

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

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

    Science.gov (United States)

    Li, J.; Lipson, R. H.

    2014-03-01

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

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

    NARCIS (Netherlands)

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

    2007-01-01

    BACKGROUND: Discovery of the central role of hepcidin in body iron regulation has shed new light on the pathophysiology of iron disorders. Information is lacking on newer analytical approaches to measure hepcidin in serum and urine. Recent reports on the measurement of urine and serum hepcidin by

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

    Czech Academy of Sciences Publication Activity Database

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

    2006-01-01

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

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

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    A sequential injection (SI) on-line matrix removal and trace metal preconcentration procedure by using a novel microcolumn packed with PTFE beads is described, and demonstrated for trace cadmium analysis with detection by electrothermal atomic absorption spectrometry (ETAAS). The analyte is initi......A sequential injection (SI) on-line matrix removal and trace metal preconcentration procedure by using a novel microcolumn packed with PTFE beads is described, and demonstrated for trace cadmium analysis with detection by electrothermal atomic absorption spectrometry (ETAAS). The analyte...... is initially complexed with diethyldithiophosphate (DDPA) and adsorbed onto the column, which is afterwards eluted with 50 mul of ethanol and subsequently introduced via air segmentation into the graphite tube for quantification. The ETAAS determination is synchronized with sample pre-treatment in the SI....../h, quantitative adsorption of cadmium (99% retention efficiency) and an enrichment factor of 59.4 were obtained, as compared with only 46.7% and 28.0 by using a knotted reactor of similar internal surface area as the packed column. The detection limits and precision (RSD, 0.1 mug/l Cd) are at the same levels, i...

  14. 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.

  15. Role of iron modifier on boron atomization process using graphite furnace-atomic absorption spectrometry based on speciation of iron using X-ray absorption fine structure

    Science.gov (United States)

    Yamamoto, Yuhei; Tagami, Azusa; Shiarasaki, Toshihiro; Yonetani, Akira; Yamamoto, Takashi; Imai, Shoji

    2018-04-01

    The role of an Fe modifier on boron atomization process using graphite furnace-atomic absorbance spectrometry was investigated using a spectroscopic approach. The initial state of the Fe modifier in a pyrolytic graphite (PG) furnace was trivalent. With an increase in pyrolysis temperature, the Fe modifier was reduced in a stepwise manner. Fe2O3 and Fe3O4 were dominant at pyrolysis temperatures below 1300 K. From 1300 to 1500 K, FeO was dominant. At temperatures higher than 1700 K, Fe metal was dominant. After a drying step, 17.7% of the initial B remained in the PG furnace. After the pyrolysis step at 773 K, the residual fraction of B was similar to that after the drying step. After the pyrolysis step at a temperature of 1073 K, the residual fraction was 11.7%. At pyrolysis temperatures > 1738 K, the residual fraction was <3.3% (

  16. Feasibility of internal standardization in the direct and simultaneous determination of As, Cu and Pb in sugar-cane spirits by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Caldas, Naise Mary; Ruella Oliveira, Silvana; Anchieta Gomes Neto, Jose

    2009-01-01

    Bismuth and Sb were evaluated as internal standards (IS) to minimize matrix effects on the direct and simultaneous determination of As, Cu, and Pb in cachaca by graphite furnace atomic absorption spectrometry using W-coated platform plus Pd-Mg(NO 3 ) 2 as modifier. For 20 μL injected sample, calibration within the 0.5-10 μg L -1 As, 100-1000 μg L -1 Cu and 0.5-30 μg L -1 Pb intervals were established using the ratios As absorbance to Sb absorbance, Cu absorbance to Bi absorbance and Pb absorbance to Bi absorbance versus analytes concentration, respectively. Typical linear correlations of 0.998, 0.999 and 0.999 were, respectively, obtained. The proposed method was applied for direct determination of As, Cu and Pb in 10 commercial cachaca samples and results were in agreement with those obtained by inductively coupled plasma mass spectrometry at 95% confidence level. The found characteristic masses were 30 pg As, 274 pg Cu and 39 pg Pb. The useful lifetime of the graphite tube was around 760 firings. Recoveries of As, Cu and Pb added to cachaca samples varied, respectively, from 98% to 109%, 97% to 108% and 98% to 104% with internal standards and from 48% to 54%, 53% to 92% and 62% to 97% without internal standards. The limits of detection were 0.13 μg L -1 As, 22 μg L -1 Cu and 0.05 μg L -1 Pb. The relative standard deviations (n = 12) for a spiked sample containing 20 μg L -1 As, Pb and 500 μg L -1 Cu were 1.6%, 1.0%, and 1.8% with IS and 4.3%, 5.2%, and 5.5% without IS

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

    Czech Academy of Sciences Publication Activity Database

    Coufalík, Pavel; Zvěřina, O.; Komárek, J.

    2016-01-01

    Roč. 118, APR (2016), s. 1-5 ISSN 0584-8547 Institutional support: RVO:68081715 Keywords : mercury * HgS * thermal desorption Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.241, year: 2016

  18. Some recent developments in the surface-analytical application of X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Gries, W.H.

    1987-01-01

    Standard depth profiles of an analyte deposited into (diffusion or ion implantation) or on (thin-film deposition) a plane surface can be analyzed for profile type and centroid depth or film thickness by means of a standardless method in which the matrix-attenuated signals of the fluorescing analyte measured at two different take-off angles are related to the mathematical distribution moments of the profile. For a binary thin film the element ratio can also be established. Results obtained on phosphorus profiles in silicon and on zinc sulphide optical coatings are referred to. The quantity or concentration level can be determined by use of a reference standard which may contain the analyte in an entirely different distribution. This simplifies the calibration of secondary reference standards. A good lateral resolution in the sub-millimeter range can be achieved with synchrotron radiation. A further improvement of lateral resolution is possible by direct excitation with electron microbeams, though at significantly inferior detection limits. (orig.)

  19. 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.)

  20. Open-path laser-induced plasma spectrometry for remote analytical measurements on solid surfaces

    Science.gov (United States)

    Palanco, S.; Baena, J. M.; Laserna, J. J.

    2002-03-01

    Open-path laser-induced plasma spectrometry has been studied for elemental analysis at a distance of 45 m from the target. The 230-mJ pulsed radiation of a Q-switched Nd:YAG laser at 1064 nm has been used to produce a plasma on the sample and light emission has been collected under an off-axis open-path scheme. Under such conditions, the main variables influencing the signal response such as beam focal conditions, laser incidence angle and laser penetration depth have been identified and diagnosed on the basis of spectral signal-to-noise ratio considerations. The incidence angle is critical beyond 60°. Crater morphology and ablation rates have been studied also. A semi-quantitative analysis of several stainless steel grades has been implemented using a pattern recognition algorithm, which allowed to discriminate successfully the samples on the basis of their variable content in alloying elements.

  1. Slurry sampling high-resolution continuum source electrothermal atomic absorption spectrometry for direct beryllium determination in soil and sediment samples after elimination of SiO interference by least-squares background correction.

    Science.gov (United States)

    Husáková, Lenka; Urbanová, Iva; Šafránková, Michaela; Šídová, Tereza

    2017-12-01

    In this work a simple, efficient, and environmentally-friendly method is proposed for determination of Be in soil and sediment samples employing slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral effects originating from SiO species were identified and successfully corrected by means of a mathematical correction algorithm. Fractional factorial design has been employed to assess the parameters affecting the analytical results and especially to help in the development of the slurry preparation and optimization of measuring conditions. The effects of seven analytical variables including particle size, concentration of glycerol and HNO 3 for stabilization and analyte extraction, respectively, the effect of ultrasonic agitation for slurry homogenization, concentration of chemical modifier, pyrolysis and atomization temperature were investigated by a 2 7-3 replicate (n = 3) design. Using the optimized experimental conditions, the proposed method allowed the determination of Be with a detection limit being 0.016mgkg -1 and characteristic mass 1.3pg. Optimum results were obtained after preparing the slurries by weighing 100mg of a sample with particle size < 54µm and adding 25mL of 20% w/w glycerol. The use of 1μg Rh and 50μg citric acid was found satisfactory for the analyte stabilization. Accurate data were obtained with the use of matrix-free calibration. The accuracy of the method was confirmed by analysis of two certified reference materials (NIST SRM 2702 Inorganics in Marine Sediment and IGI BIL-1 Baikal Bottom Silt) and by comparison of the results obtained for ten real samples by slurry sampling with those determined after microwave-assisted extraction by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS). The reported method has a precision better than 7%. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. On-line dynamic two-dimensional admicelles solvent extraction coupled to electrothermal atomic absorption spectrometry for determination of chromium(VI) in drinking water

    International Nuclear Information System (INIS)

    Nan Jing; Yan Xiuping

    2005-01-01

    An on-line dynamic two-dimensional admicelles solvent extraction system was coupled to electrothermal atomic absorption spectrometry (ETAAS) for determination of Cr(VI) in drinking water. As a two-dimensional solvent, admicelles were on-line-prepared by passing cetyltrimethylammonium bromide (CTAB) through a microcolumn packed with silica gel. The analyte Cr(VI) was on-line-complexed with pyrrolidine dithiocarbamate (PDC), and the resulting Cr(VI)-PDC was effectively adsolubilized in the admicelles of the microcolumn, and then quantitatively eluted with 30 μl of acetonitrile for ETAAS determination. All the procedures including the formation and decomposition of admicelles and ETAAS determination were performed on-line, ensuring automatic determination of Cr(VI) in drinking water with a high precision. With a consumption of 2.1 ml sample solution, a detection limit (3σ) of 3.0 ng l -1 , and an enhancement factor of 32 were obtained at a sample throughput of 31 samples h -1 . The precision (R.S.D.) for 11 replicate measurements of 50 ng l -1 Cr(VI) was 2.5%. The developed methodology was demonstrated to be reliable and sensitive for automatic determination of ultratrace Cr(VI) in bottled drinking water samples

  3. Automated magnetic sorbent extraction based on octadecylsilane functionalized maghemite magnetic particles in a sequential injection system coupled with electrothermal atomic absorption spectrometry for metal determination.

    Science.gov (United States)

    Giakisikli, Georgia; Anthemidis, Aristidis N

    2013-06-15

    A new automatic sequential injection (SI) system for on-line magnetic sorbent extraction coupled with electrothermal atomic absorption spectrometry (ETAAS) has been successfully developed for metal determination. In this work, we reported effective on-line immobilization of magnetic silica particles into a microcolumn by the external force of two strong neodymium iron boron (NdFeB) magnets across it, avoiding the use of frits. Octadecylsilane functionalized maghemite magnetic particles were used as sorbent material. The potentials of the system were demonstrated for trace cadmium determination in water samples. The method was based on the on-line complex formation with diethyldithiocarbamate (DDTC), retention of Cd-DDTC on the surface of the MPs and elution with isobutyl methyl ketone (IBMK). The formation mechanism of the magnetic solid phase packed column and all critical parameters (chemical, flow, graphite furnace) influencing the performance of the system were optimized and offered good analytical characteristics. For 5 mL sample volume, a detection limit of 3 ng L(-1), a relative standard deviation of 3.9% at 50 ng L(-1) level (n=11) and a linear range of 9-350 ng L(-1) were obtained. The column remained stable for more than 600 cycles keeping the cost down in routine analysis. The proposed method was evaluated by analyzing certified reference materials and natural waters. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. 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.

  5. Masking Agents Evaluation for Lead Determination by Flow Injection-Hydride Generation-Atomic Fluorescence Spectrometry Technique: Effect of KI, L-Cysteine, and 1,10-Phenanthroline

    Directory of Open Access Journals (Sweden)

    Blanca G. Beltrán

    2016-01-01

    Full Text Available Hydride generation (HG of lead technique presents interferences from foreign ions of complex matrix samples. In order to minimize these interferences, the effect of masking agents such as KI, L-cysteine, and 1,10-phenanthroline was studied in the absence and in the presence of selected interfering species (As, Cr, Cu, and Fe. Different modes of addition of masking agents were accomplished, that is, to either sample or KBH4 reducing solution. The lead determinations were performed using a flow injection analysis (FIA system coupled to HG and atomic fluorescence spectrometry (AFS. The linearity of calibration curves (1–10 μg Pb L−1 was not affected by the addition of the masking agents. The use of KI in the reducing solution diminished interferences from concentrations of As and Cu, while 1,10-phenanthroline showed a positive effect on the interference by As. Moreover, Cr and Cu appeared to be the most serious interfering ions for plumbane (PbH4, because they drastically reduced the analytical signal of lead. Fe did not present any interference under the employed experimental conditions, even at high levels. The accuracy was established through the analysis of certified reference material (i.e., BCR-610, groundwater using KI as masking agent. The detection limit reached by FIA-HG-AFS proposed methodology was 0.03 μg Pb L−1.

  6. Photoassisted vapor generation in the presence of organic acids for ultrasensitive determination of Se by electrothermal-atomic absorption spectrometry following headspace single-drop microextraction

    International Nuclear Information System (INIS)

    Figueroa, Raul; Garcia, Monica; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A method is described for the determination of selenium at the pg/mL level by electrothermal-atomic absorption spectrometry using in situ photogeneration of Se vapors, headspace sequestration onto an aqueous microdrop containing Pd(II) and subsequent injection in a graphite tube. Several organic acids (formic, oxalic, acetic, citric and ethylenediaminetetraacetic) have been tried for photoreduction of Se(IV) into volatile Se compounds under UV irradiation. Experimental variables such as UV irradiation time, organic acid concentration, Pd(II) concentration in the drop, sample and drop volumes, extraction time and pH were fully optimized. Low-molecular weight acids such as formic and acetic provided optimal photogeneration of volatile Se species at a 0.6 mol/L concentration. Citric and ethylenediaminetetraacetic acid allowed to use a concentration as low as 1 mmol/L, but extraction times were longer than for formic and acetic acids. Photogeneration of (CH 3 ) 2 Se from Se(IV) in the presence of acetic acid provided a detection limit of 20 pg/mL, a preconcentration factor of nearly 285 and a precision, expressed as relative standard deviation, of 4%. Analytical performance seemed to depend not only on the photogeneration efficiency obtained with each acid but also on the stability of the vapors in the headspace. The method showed a high freedom from interferences caused by saline matrices, but interferences were observed for transition metals at a relatively low concentration

  7. 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

  8. 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.

  9. Determination of total Sb,Se Te, and Bi and evaluation of their inorganic species in garlic by hydride-generation-atomic-fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matos Reyes, M.N.; Cervera, M.L.; Guardia, M. de la [University of Valencia, Department of Analytical Chemistry, Burjassot, Valencia (Spain)

    2009-07-15

    A sensitive and simple analytical method has been developed for determination of Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), Te(VI), and Bi(III) in garlic samples by using hydride-generation-atomic-fluorescence spectrometry (HG-AFS). The method is based on a single extraction of the inorganic species by sonication at room temperature with 1 mol L{sup -1} H{sub 2}SO{sub 4} and washing of the solid phase with 0.1% (w/v) EDTA, followed by measurement of the corresponding hydrides generated under two different experimental conditions directly and after a pre-reduction step. The limit of detection of the method was 0.7 ng g{sup -1} for Sb(III), 1.0 ng g{sup -1} for Sb(V), 1.3 ng g{sup -1} for Se(IV), 1.0 ng g{sup -1} for Se(VI), 1.1 ng g{sup -1} for Te(IV), 0.5 ng g{sup -1} for Te(VI), and 0.9 ng g{sup -1} for Bi(III), in all cases expressed in terms of sample dry weight. (orig.)

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

    Science.gov (United States)

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

    2012-01-01

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

  11. Fully automated dissolution and separation methods for inductively coupled plasma atomic emission spectrometry rock analysis. Application to the determination of rare earth elements

    International Nuclear Information System (INIS)

    Govindaraju, K.; Mevelle, G.

    1987-01-01

    In rock analysis laboratories, sample preparation is a serious problem, or even an enormous bottleneck. Because this laboratory is production-oriented, this problem was attacked by automating progressively, different steps in rock analysis for major, minor and trace elements. This effort has been considerably eased by the fact that all sample preparation schemes in this laboratory for the past three decades have been based on an initial lithium borate fusion of rock samples and all analytical methods based on multi-element atomic emission spectrometry, with switch-over from solid analysis by arc/spark excitation to solution analysis by plasma excitation in 1974. The sample preparation steps which have been automated are: weighing of samples and fluxes, lithium borate fusion, dissolution and dilution of fusion products and ion-exchange separation of difficult trace elements such as rare earth elements (REE). During 1985 and 1986, these different unit operations have been assembled together as peripheral units in the form of a workstation, called LabRobStation. A travelling robot is the master of LabRobStation, with all peripheral units at its reach in 10 m 2 workspace. As an example of real application, the automated determination of REE, based on more than 8000 samples analysed during 1982 and 1986, is presented. (author)

  12. 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.

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

    Science.gov (United States)

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

    2013-05-01

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

  14. Preconcentration procedure using in situ solvent formation microextraction in the presence of ionic liquid for cadmium determination in saline samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Mahpishanian, Shokouh; Shemirani, Farzaneh

    2010-07-15

    A simple in situ solvent formation microextraction methodology based on the application of ionic liquid (IL) as an extractant solvent and sodium hexafluorophosphate (NaPF(6)) as an ion-pairing agent was proposed for the preconcentration of trace levels of cadmium. In this method cadmium was complexed with O,O-diethyldithiophosphate (DDTP) 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). ISFME is a simple and rapid method for extraction and preconcentration of metal ions from sample solutions containing a high concentration of salt. Some effective factors that influence the microextraction efficiency were investigated and optimized. Under the optimum experimental conditions, the limit of detection (3 s) and the enhancement factor were 0.07 microg L(-1) and 78, respectively. The relative standard deviation (R.S.D.) was obtained 2.42%. The accuracy of the method was confirmed by analyzing certified reference materials for trace elements in seawater (GBW (E) 080040 seawater). The proposed method was successfully applied for the determination of cadmium in water samples and food grade salts. Crown Copyright 2010. Published by Elsevier B.V. All rights reserved.

  15. Effect of surfactant addition on ultrasonic leaching of trace elements from plant samples in inductively coupled plasma-atomic emission spectrometry

    Science.gov (United States)

    Borkowska-Burnecka, Jolanta; Jankowiak, Urszula; Zyrnicki, Wieslaw; Anna Wilk, Kazimiera

    2004-04-01

    The applicability of surfactants in sample preparation of plant materials followed by analysis by inductively coupled plasma atomic emission spectrometry has been examined. Reference materials (INCT-MPH-2-Mixed Polish Herbs, INCT-TL-1 black tea leaves and CTA-VTL-2 -Virginia tobacco leaves) and commercially available tea leaves were analyzed. Effects of addition surfactants (Triton X-100, didodecyldimethylammonium bromide and cetyltrimethylammonium bromide) on efficiency of ultrasonic leaching of elements from the plant samples and on plasma parameters were investigated. Low concentrations of the surfactants in solutions did not affect, in practice, analytical line intensities and the nebulization process. Quantitative recovery of some elements could be obtained by ultrasonic diluted acid leaching with the aid of surfactants. However, the element recovery depended on type of surfactant, as well as element and sample material. Plasma parameters, i.e. the excitation temperatures of Ar I, Fe II and Ca II as well as the electron number density and the Mg II/Mg I intensity ratio did not vary significantly due to the surfactants in solutions.

  16. Evaluation of polychlorotrifluoroethylene as sorbent material for on-line solid phase extraction systems: determination of copper and lead by flame atomic absorption spectrometry in water samples.

    Science.gov (United States)

    Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

    2006-08-04

    Polychlorotrifluoroethylene (PCTFE) in the form of beads was applied, as packing material for flow injection on-line column preconcentration and separation systems coupled with flame atomic absorption spectrometry (FAAS). Its performance characteristics were evaluated for trace copper determination in environmental samples. The on-line formed complex of metal with diethyldithiophosphate (DDPA) was sorbed on the PCTFE surface. Isobutyl methyl ketone (IBMK) at a flow rate of 2.8 mL min(-1) was used to elute the analyte complex directly into the nebulizer-burner system of spectrophotometer. The proposed sorbent material reveal, excellent chemical and mechanical resistance, fast adsorption kinetics permitting the use of high sample flow rates up to 15 mL min(-1) without loss of retention efficiency. For copper determination, with 90 s preconcentration time the sample frequency was 30 h(-1), the enhancement factor was 250, which could be further improved by increasing the loading (preconcentration) time. The detection limit (3s) was c(L)=0.07 microg L(-1), and the precision (R.S.D.) was 1.8%, at the 2.0 microg L(-1) Cu(II) level. For lead determination, the detection limit was c(L)=2.7 microg L(-1), and the precision (R.S.D.) 2.2%, at the 40.0 microg L(-1) Pb(II) level. The accuracy of the developed method was evaluated by analyzing certified reference materials and by recovery measurements on spiked natural water samples.

  17. A novel preconcentration procedure using cloud point extraction for determination of lead, cobalt and copper in water and food samples using flame atomic absorption spectrometry.

    Science.gov (United States)

    Citak, Demirhan; Tuzen, Mustafa

    2010-05-01

    In this work, a new cloud point extraction (CPE) procedure was developed for the separation and preconcentration of lead(II), cobalt(II), and copper(II) in various water and food samples. Complexes of metal ions with 1-Phenylthiosemicarbazide (1-PTSC) were extracted into the surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114) from samples. After phase separation, the enriched analytes were determined by flame atomic absorption spectrometry (FAAS). Factors affecting cloud point extraction, such as pH, reagent and surfactant concentrations, temperature, and incubation time were evaluated and optimized. The interference effect of some cations and anions was also studied. After optimization of the CPE conditions, the preconcentration factor of 25 and the limits of detection (L.O.D.) obtained for lead(II), cobalt(II), and copper(II) based on three sigma (n=20) were 3.42, 1.00, and 0.67 microg L(-1), respectively. The method presented precision (R.S.D.) between 1.7% and 4.8% (n=7). The presented preconcentration procedure was applied to the determination of metal ions in reference standard materials (SRM 1515 Apple leaves and GBW 07605 Tea) and some real samples including tap water, spring water, sea water, canned fish, black tea, green tea, tomato sauce and honey. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

  18. Cloud point extraction for the determination of lead and cadmium in urine by graphite furnace atomic absorption spectrometry with multivariate optimization using Box-Behnken design

    International Nuclear Information System (INIS)

    Maranhao, Tatiane de A; Martendal, Edmar; Borges, Daniel L.G.; Carasek, Eduardo; Welz, Bernhard; Curtius, Adilson J.

    2007-01-01

    Cloud point extraction (CPE) is proposed as a pre-concentration procedure for the determination of Pb and Cd in undigested urine by graphite furnace atomic absorption spectrometry (GF AAS). Aliquots of 0.5 mL urine were acidified with HCl and the chelating agent ammonium O,O-diethyl dithiophosphate (DDTP) was added along with the non-ionic surfactant Triton X-114 at the optimized concentrations. Phase separation was achieved by heating the mixture to 50 deg. C for 15 min. The surfactant-rich phase was analyzed by GF AAS, employing the optimized pyrolysis temperatures of 900 deg. C for Pb and 800 deg. C for Cd, using a graphite tube with a platform treated with 500 μg Ru as permanent modifier. The reagent concentrations for CPE (HCl, DDTP and Triton X-114) were optimized using a Box-Behnken design. The response surfaces and the optimum values were very similar for aqueous solutions and for the urine samples, demonstrating that aqueous standards submitted to CPE could be used for calibration. Detection limits of 40 and 2 ng L -1 for Pb and Cd, respectively, were obtained along with an enhancement factor of 16 for both analytes. Three control urine samples were analyzed using this approach, and good agreement was obtained at a 95% statistical confidence level between the certified and determined values. Five real samples have also been analyzed before and after spiking with Pb and Cd, resulting in recoveries ranging from 97 to 118%

  19. 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.

  20. 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.

  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.

  2. 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)

  3. Assessment of cadmium and iron adsorption in sediment, employing a flow injection analysis system with on line filtration and detection by flame atomic absorption spectrometry and thermospray flame furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Fagner Moreira de; Marchioni, Camila; Barros, Juan A. V de A. [Universidade Federal de Alfenas (UNIFAL-MG), Instituto de Química, Rua GabrielMonteiro da Silva, 714, CEP 37130-000, Alfenas-MG (Brazil); Lago, Ayla Campos do [Universidade Federal de São Carlos (UFSCar-SP), Departamento de Química, 10Rodovia Washington Luís, Km 235-SP 310, CEP 16565-905, São Carlos-SP (Brazil); Wisniewski, Célio [Universidade Federal de Alfenas (UNIFAL-MG), Instituto de Química, Rua GabrielMonteiro da Silva, 714, CEP 37130-000, Alfenas-MG (Brazil); Luccas, Pedro Orival, E-mail: pedro.luccas@unifal-mg.edu.br [Universidade Federal de Alfenas (UNIFAL-MG), Instituto de Química, Rua GabrielMonteiro da Silva, 714, CEP 37130-000, Alfenas-MG (Brazil)

    2014-01-27

    Graphical abstract: -- Highlights: •A FIA system with on-line filtration for isotherms adsorption studies was proposed. •Isotherms for iron and cadmium elements in bottom lake sediment were done. •Inferences about adsorption/desorption mechanisms were feasible. •The proposed method turns the isotherm studies fast and reliable. -- Abstract: This work presents an evaluation of iron and cadmium adsorption in sediment of the Furnas Hydroelectric Plant Reservatory located in Alfenas, Minas Gerais (Brazil). The metal determination was done employing a flow injection analysis (FIA) with an on-line filtering system. As detection techniques, flame atomic absorption spectrometry (FAAS) for iron and thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) for cadmium determinations were used. The developed methodology presented good limits of detection, being 190 μg L{sup −1} for iron and 1.36 μg L{sup −1} for cadmium, and high sampling frequency for both metals 144 and 60 readings h{sup −1} for iron and cadmium, respectively. Both metals obey the Langmuir model, with maximum adsorptive capacity of 0⋅169 mg g{sup −1} for iron and 7⋅991 mg g{sup −1} for cadmium. For iron, a pseudo-first-order kinetic model was obtained with a theoretical Q{sub e} = 9⋅8355 mg g{sup −1} (experimental Q{sub e} = 9⋅5432 mg g{sup −1}), while for cadmium, a pseudo-second-order kinetic model was obtained, with a theoretical Q{sub e} = 0.3123 mg g{sup −1} (experimental Q{sub e} = 0⋅3052 mg g{sup −1})

  4. Analytical challenges in characterization of high purity materials

    Indian Academy of Sciences (India)

    Unknown

    K L RAMAKUMAR. Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085, India ... 2. Analytical challenges in spark source mass spectrometry (SSMS). 2.1 Determination of hydrogen. Despite some of its limitations, SSMS with conventional .... Inductively coupled plasma mass spectrometry. (ICPMS).

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

    Science.gov (United States)

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

    2006-08-01

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

  6. Influence of citric acid as chemical modifier for lead determination in dietary calcium supplement samples by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Cezar Paz de Mattos, Julio; Medeiros Nunes, Adriane; Figueiredo Martins, Ayrton; Luiz Dressler, Valderi; Marlon de Moraes Flores, Erico

    2005-01-01

    Citric acid was used as a chemical modifier for Pb determination by graphite furnace atomic absorption spectrometry in dietary supplement samples (calcium carbonate, dolomite and oyster shell samples) and its efficiency was compared to the use of palladium. Pyrolysis and atomization curves were established without use of chemical modifier, with the addition of 20, 100 and 200 μg of citric acid, and with 3 μg of palladium. The citric acid modifier made possible the interference-free Pb determination in the presence of high concentrations of Ca and Mg nitrates. Acid sample digestion involving closed vessels (microwave-assisted and conventional heating) and acid attack using polypropylene vessels at room temperature were compared. All digestion procedures presented similar results for calcium carbonate and dolomite samples. However, for oyster shell samples accurate results were obtained only with the use of closed vessel systems. Analyte addition and matrix-matched standards were used for calibration. The characteristic mass for Pb using citric acid and palladium were 16 and 25 pg, respectively. The relative standard deviation (RSD) was always less than 5% when citric acid was used. The relative and absolute limits of detection were 0.02 μg g -1 and 8 pg with citric acid and 0.1 μg g -1 and 44 pg with the Pd modifier, respectively (n = 10, 3σ). The recovery of Pb in spiked calcium supplement samples (10 μg l -1 ) was between 98% and 105%. With the use of 100 μg of citric acid as chemical modifier, problems such as high background absorption and high RSD values were minimized in comparison to the addition of 3 μg of palladium

  7. Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

    Science.gov (United States)

    Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

    2013-11-15

    A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. In situ metathesis ionic liquid formation dispersive liquid-liquid microextraction for copper determination in water samples by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Stanisz, Ewa; Zgoła-Grześkowiak, Agnieszka

    2013-10-15

    In situ synthesis of ionic liquid extractant for dispersive liquid-liquid microextraction (in situ IL DLLME) combined with electrothermal atomic absorption spectrometry (ET AAS) for determination of copper in water samples was developed. Analytical signals were obtained without the back-extraction of copper from the IL phase prior to its determination by AAS. Some essential parameters of the microextraction and detection techniques such as the pH of sample solution, volume of components for in situ synthesis, matrix interferences and main parameters of graphite furnace atomizer have been studied. Under optimal conditions, high extraction efficiency for copper was achieved for the extraction of 0.7 µg L(-1) in 10.0 mL of sample solution employing 8 μL of 1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (HmimNTf2) as the extraction solvent. The detection limit was found as 0.004 µg L(-1) with an enrichment factor of 200. The relative standard deviation (RSD) for seven replicate measurements of 0.7 µg L(-1) in sample solution was 4%. The accuracy of the proposed method was evaluated by analysis of the Certified Reference Materials: NIST SRM 2709 (San Joaquin Soil), NBS SRM 2704 (Buffalo River Sediment), NRCC DOLT-2 (Dogfish Liver) and NIST SRM 1643e (Trace Element in Water). The measured copper contents in the reference materials were in satisfactory agreement with the certified values. The method was successfully applied to analysis of the tap, lake and mineral water samples. © 2013 Elsevier B.V. All rights reserved.

  9. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    Science.gov (United States)

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

  10. In-field determination of trace dissolved manganese in estuarine and coastal waters with automatic on-line preconcentration and flame atomic fluorescence spectrometry.

    Science.gov (United States)

    Feng, Sichao; Yuan, Dongxing; Huang, Yongming; Lin, Kunning; Zhou, Tingjin

    2017-04-22

    An automatic on-line preconcentration and detection system for analysis of trace dissolved manganese (Mn) in estuarine and coastal waters was established, using preconcentration with IDA chelating resin and detection with flame atomic fluorescence spectrometer (FAFS). The rinse (pre-eluent) solution was optimized, for removing the interference ions while retaining the target element. It was found that the interference ions affected the chelating efficiency of Mn, causing variation of the detection blank and sensitivity. This effect varied when sample volume presented as preconcentration time changed. The influence at preconcentration times of 120 s, 30 s and 10 s were carefully investigated and reported. Ten folds of the foreign trace metals Zn, Cu, Ni, Fe, and Al did not show obvious interference on Mn preconcentration and detection. The method detection limit was 0.9 nmol L -1 (n = 7, preconcentration time 120 s). The linear detection range could be adjusted with designed preconcentration time. In addition to high precision and accuracy, the proposed analytical system had the advantages of high integration, and required normal site preparation, low energy supply and simple auxiliary equipment, which was appropriate for in-field operation. Compared with other common in-field applied molecular spectrometry instruments, the inherent high selectivity and multi-element applicability of FAFS highlighted the superiority and potential of the proposed analytical system. It was successfully applied to in-field vehicle-board determination of dissolved Mn in coastal waters around Xiamen, Fujian, China, and it was also used to analyze natural water samples collected from the Jiulongjiang Estuary, Fujian, China. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Brombach, Christoph-Cornelius [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Chen, Bin; Corns, Warren T. [PS Analytical, Arthur House, Crayfields Industrial Estate, Main Road, Orpington, Kent BR5 3HP (United Kingdom); Feldmann, Jörg [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Krupp, Eva M., E-mail: e.krupp@abdn.ac.uk [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom)

    2015-03-01

    Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography–cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation. - Highlights: • We demonstrate that a novel mixture of thiourea-thiolsilica shows an excellent trapping of MeHg between a broad pH range 1–6. • We develop the method so that it can potentially be automated for inorganic and methyl-mercury. • The method is matrix independent with highly accurate results for MeHg in hair CRM extracts and spiked water samples • The limit of detection is around 40 pg/L when just 200 mL sample is used, without any intensive preparation.

  12. Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Carletto, Jeferson Schneider; Luciano, Raquel Medeiros; Bedendo, Gizelle Cristina; Carasek, Eduardo

    2009-01-01

    A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML 2 ). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5 x 10 -2 mol L -1 , extraction temperature 40 deg. C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 μL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 μL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 μg L -1 , relative standard deviation (RSD) 5.5% and the working linear range 2-30 μg L -1 .

  13. Combined use of atomic force microscopy, X-ray photoelectron spectroscopy, and secondary ion mass spectrometry for cell surface analysis.

    Science.gov (United States)

    Dague, Etienne; Delcorte, Arnaud; Latgé, Jean-Paul; Dufrêne, Yves F

    2008-04-01

    Understanding the surface properties of microbial cells is a major challenge of current microbiological research and a key to efficiently exploit them in biotechnology. Here, we used three advanced surface analysis techniques with different sensitivity, probing depth, and lateral resolution, that is, in situ atomic force microscopy, X-ray photoelectron spectroscopy, and secondary ion mass spectrometry, to gain insight into the surface properties of the conidia of the human fungal pathogen Aspergillus fumigatus. We show that the native ultrastructure, surface protein and polysaccharide concentrations, and amino acid composition of three mutants affected in hydrophobin production are markedly different from those of the wild-type, thereby providing novel insight into the cell wall architecture of A. fumigatus. The results demonstrate the power of using multiple complementary techniques for probing microbial cell surfaces.

  14. Determination of boron in the waters of Troia by inductively coupled plasma-atomic emission spectrometry (ICP-AES

    Directory of Open Access Journals (Sweden)

    HASAN OZCAN

    2005-10-01

    Full Text Available The inductively coupled plasma-atomic emission spectrometry method (ICP-EAS is proposed for the determination of boron in Troia water sources. In this study, boron samples were taken from 25 different locations during November 2002 and May 2003. The 249.773 nm boron emmision line was not affected by the samplematrix. The boron content was determined without further pretreatment of samples proposed ICP-AES method. An analysis of a given sample was completed in about 15 min. The determined boron concentrations in surface and ground water sources were between 0.00444–1.11200mgl-1. Inorder to compare the results obtained by the proposed method, selected water samples were also analysed titrimetically. Pearson correlation coefficient analysis showed that there is a close relationship between the ICP-AES and the titrimetric method and the determination coefficient (R2 was calculated to be 91.34 %.

  15. 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)

  16. A solid phase extraction procedure for the determination of Cd(II) and Pb(II) ions in food and water samples by flame atomic absorption spectrometry.

    Science.gov (United States)

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

    2015-05-01

    A relatively rapid, accurate and precise solid phase extraction method is presented for the determination of cadmium(II) and lead(II) in various food and water samples. Quantitation is carried out by flame atomic absorption spectrometry (FAAS). The method is based on the retention of the trace metal ions on Dowex Marathon C, a strong acid cation exchange resin. Some important parameters affecting the analytical performance of the method such as pH, flow rate and volume of the sample solution; type, concentration, volume, flow rate of the eluent; and matrix effects on the retention of the metal ions were investigated. Common coexisting ions did not interfere on the separation and determination of the analytes. The detection limits (3 σb) for Cd(II) and Pb(II) were found as 0.13 and 0.18 μg L(-1), respectively, while the limit of quantification values (10 σb) were computed as 0.43 and 0.60 μg L(-1) for the same sequence of the analytes. The precision (as relative standard deviation was lower than 4% at 5 μg L(-1) Cd(II) and 10 μg L(-1) Pb(II) levels, and the preconcentration factor was found to be 250. The accuracy of the proposed procedure was verified by analysing the certified reference materials, SPS-WW2 Batch 108 wastewater level 2 and INCT-TL-1 tea leaves, with the satisfactory results. In addition, for the accuracy of the method the recovery studies (⩾ 95%) were carried out. The method was applied to the determination of the analytes in the various natural waters (lake water, tap water, waste water with boric acid, waste water with H2SO4) and food samples (pomegranate flower, organic pear, radish leaf, lamb meat, etc.), and good results were obtained. While the food samples almost do not contain cadmium, they have included lead at low levels of 0.13-1.12 μg g(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

  17. Determination of Total Arsenic and Speciation in Apple Juice by Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry: An Experiment for the Analytical Chemistry Laboratory

    Science.gov (United States)

    He, Ping; Colon, Luis A.; Aga, Diana S.

    2016-01-01

    A two-part laboratory experiment was designed for upper-level analytical chemistry students to provide hands-on experience in the use of high performance liquid chromatography (HPLC) for separation and inductively coupled plasma mass spectrometry (ICP-MS) for detection. In the first part of the experiment, the students analyze total arsenic in…

  18. Thorium: one of the analytical techniques in neutronic activation and alpha spectrometry of the CDTN (Brazilian Nuclear Technology Development Center) in the last three decades

    International Nuclear Information System (INIS)

    Menezes, M.A.B.C.; Sabino, C.V.S.

    1994-01-01

    For long years, the CDTN (Brazilian Nuclear Technology Development Center ) has applied several analytical techniques in the thorium determination. This work is about the evolution of the neutronic activation in the thorium 232 analysis from the 1960's to now. The importance of the analysis request and alpha spectrometry for the thorium 228 and thorium 232 determination is emphasized. (J.A.M.M.)

  19. Achieving 100% efficient postcolumn hydride generation for As speciation analysis by atomic fluorescence spectrometry

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2016-01-01

    Roč. 88, č. 7 (2016), s. 4041-4047 ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * HPLC Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 6.320, year: 2016

  20. Achieving 100% efficient postcolumn hydride generation for As speciation analysis by atomic fluorescence spectrometry

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2016-01-01

    Roč. 88, č. 7 (2016), s. 4041-4047 ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * HPLC Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 6.320, year: 2016

  1. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen–argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, E. H.; Pritzl, G.

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting the ...

  2. Internal standardization--atomic spectrometry and geographical pattern recognition techniques for the multielement analysis and classification of Catalonian red wines.

    Science.gov (United States)

    Iglesias, Mònica; Besalú, Emili; Anticó, Enriqueta

    2007-01-24

    Major and minor (K, P, Ca, Mg, Na, Fe, Mn, Zn, and Sr) and trace (Ba, Ni, Pb, V, Co, Cd, and Sb) elements from wine samples from the Denomination of Origin (DO) Empordà-Costa Brava (Catalonia, Spain) were analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES) and mass spectrometry (ICP-MS) respectively. Previously, a comparison of different calibration methodologies and sample digestion treatments had been carried out using ANOVA statistical tool. The obtained results demonstrated that internal standardization provides reliable results with the advantage that no further manipulation of the sample is needed. A principal component analysis of the concentration data was performed to differentiate the samples of DO Empordà-Costa Brava from wine samples from other wine-producing regions in Spain (i.e., Penedès, Somontano, and Rioja). It was found that Sr and Ba contents discriminate the two DO groups. Moreover, a discriminant analysis function involving both variables distinguishes the two groups with a 100% classification rate. At the level of the leave-one-out cross-validation, all of the Empordà-Costa Brava samples were well classified, whereas the other DOs presented two borderline misclassifications.

  3. 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.

  4. Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

    International Nuclear Information System (INIS)

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

    2015-01-01

    Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine sediment samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS AAS) and direct solid sample analysis has been developed. The application of fast programs in combination with direct solid sampling allows to eliminate the drying and pretreatment steps, however makes impossible the use of liquid standards for calibration. Iridium treated platforms were applied throughout the present study. Calibration technique based on the use of solid certified reference materials (marine sediments) similar to the nature of the analyzed sample and statistics of regression analysis were applied to the real sediment samples. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signals. The ISO-17025 requirements and Eurachem guidelines were followed in the validation of the proposed analytical procedure. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability reproducibility, limits of detection and quantification and expanded uncertainty (k = 2) for all investigated elements were assessed. Two different approaches for the estimation of measurement uncertainty were applied and obtained results compared. The major contributors to the combined uncertainty of the analyte mass fraction were found to be the homogeneity of the samples and the microbalance precision. The influence of sample particle sizes on the total combined uncertainty was also evaluated. Traceability to SI system of units of the obtained by the proposed analytical procedure results was demonstrated. Additionally, validation of the methodology developed was effectuated by the comparison of the obtained results with independent method e.g. ICP-MS with external calibration. The use of solid sampling HR CS AAS for the determination of trace elements in marine sediment matrix gives significant advantages

  5. 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)

  6. Sputtering of copper atoms by keV atomic and molecular ions A comparison of experiment with analytical and computer based models

    CERN Document Server

    Gillen, D R; Goelich,

    2002-01-01

    Non-resonant multiphoton ionisation combined with quadrupole and time-of-flight analysis has been used to measure energy distributions of sputtered copper atoms. The sputtering of a polycrystalline copper target by 3.6 keV Ar sup + , N sup + and CF sub 2 sup + and 1.8 keV N sup + and CF sub 2 sup + ion bombardment at 45 deg. has been investigated. The linear collision model in the isotropic limit fails to describe the high energy tail of the energy distributions. However the TRIM.SP computer simulation has been shown to provide a good description. The results indicate that an accurate description of sputtering by low energy, molecular ions requires the use of computer simulation rather than analytical approaches. This is particularly important when considering plasma-surface interactions in plasma etching and deposition systems.

  7. Spatial discrimination against background with different optical systems for collection of fluorescence in laser-excited atomic fluorescence spectrometry with a graphite tube electrothermal atomizer.

    Science.gov (United States)

    Yuzefovsky, A I; Lonardo, R F; Michel, R G

    1995-07-01

    A single 90 degrees off-axis ellipsoidal mirror fragment was used in a dispersive detection system for electrothermal atomization laser-excited atomic fluorescence spectrometry. The performance of the new optical arrangement was compared with those of optical arrangements that employed a plane mirror in combination with biconvex or plano-convex lenses. All the optical arrangements collected fluorescence in a scheme called front surface illustration. BEAM-4, an optical ray tracing program, was used for calculations of spatial ray distributions and optical collection efficiency for the various optical configurations. Experimentally, the best collection efficiency was obtained by use of the ellipsoidal mirror, in qualitative agreement with simulations done by use of the BEAM-4 software. The best detection limit for cobalt with the new optical arrangement was 20 fg, which was a factor of 5 better than that obtained with conventional optical arrangements with otherwise the same instrumentation. The signal-to-background ratio and the fluorescence collection efficiency were also studied as a function of position of the optical components for the various optical arrangements. For both cobalt and phosphorus, the signal-to-background ratio with the new optical arrangement remained stable within 10-20% during +/- 8 mm shifts in the position of the detection system from the focal plane of the optics. Overall, the new optical arrangement offered high collection efficiency, excellent sensitivity, and facile optical alignment due to efficient spatial separation between the fluorescence signal and the background radiation. The advantages of the new optical arrangement were particularly important during measurements in the presence of high levels of blackbody radiation.

  8. Use of atomic absorption spectrometry to determine metallic impurities in coal

    International Nuclear Information System (INIS)

    Silva, M.J.S.F. da.

    1983-01-01

    The Brazilian Energetic Alternative Program expects the reduction of our dependence on foreign energy sources, by replacing fuel oil by mineral coal. Its gasification by means of nuclear energy must be also considered. However, the intensive burning of coal leads to serious environmental problems. During its combustion the release to atmosphere of toxic elements such as As, Hg, Pb, Zn and others is of great concern. Hence, it is important to have reliable analytical methods which can monitor inorganic constituents at various stages of coal production and utilization. The AAS is a suitable analytical technique to determine pollutants in coal because it is sensitive, simple, economic and cover a large range of concentration. The need of a previous treatment of sample is overcome by using an acid attack (HNO 3 + HClO 4 + HF) which has been proved to be rapid and efficient. (Author) [pt

  9. Determination of Mercury in Milk by Cold Vapor Atomic Fluorescence: A Green Analytical Chemistry Laboratory Experiment

    Science.gov (United States)

    Armenta, Sergio; de la Guardia, Miguel

    2011-01-01

    Green analytical chemistry principles were introduced to undergraduate students in a laboratory experiment focused on determining the mercury concentration in cow and goat milk. In addition to traditional goals, such as accuracy, precision, sensitivity, and limits of detection in method selection and development, attention was paid to the…

  10. 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.

  11. 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.

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

    Science.gov (United States)

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

    2002-12-01

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

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

  14. Analytical performance of an inductively coupled plasma optical emission spectrometry with Dual View configuration

    Directory of Open Access Journals (Sweden)

    Silva Júlio C. J.

    2003-01-01

    Full Text Available The analytical performance of axially and radially viewed inductively coupled plasma optical emission spectrometers (AX-ICP OES and RD-ICP OES, respectively were evaluated in terms of the Mg II/Mg I ratio, matrix effects, and detection limits (LOD. All solutions were made in either 1% v v-1 nitric acid or in a 10% v v-1 water-soluble tertiary amine solution (CFA-C adjusted to pH 8. Using a nebulization gas flow-rate of 0.5 L min-1 and applied power of 1.3 kW, Mg II/Mg I ratio was at least 15 in any medium for both configurations. Under robust conditions, plasma processes were practically not affected by the presence of 0.1% m v-1 of Ca, K, or Na in both configurations. However, interference effects were observed with non-robust conditions, mainly with AX-ICP OES in both media. The best detection limits were obtained using AX-ICP OES under robust conditions, with solutions prepared in the amine medium.

  15. Analytical approaches for determination of bromine in sediment core samples by X-ray fluorescence spectrometry.

    Science.gov (United States)

    Pashkova, Galina V; Aisueva, Tatyana S; Finkelshtein, Alexander L; Ivanov, Egor V; Shchetnikov, Alexander A

    2016-11-01

    Bromine has been recognized as a valuable indicator for paleoclimatic studies. Wavelength dispersive X-ray fluorescence (WDXRF) and total reflection X-ray fluorescence (TXRF) methods were applied to study the bromine distributions in lake sediment cores. Conventional WDXRF technique usually requires relatively large mass of a sediment sample and a set of calibration samples. Some analytical approaches were developed to apply WDXRF to small sediment core samples in the absence of adequate calibration samples with a known Br content. The mass of a sample to be analyzed was reduced up to 200-300mg and the internal standard method with correction using fundamental parameters was developed for Br quantification. TXRF technique based on the direct analysis of a solid suspension using 20mg of sediment sample by internal standard method was additionally tested. The accuracy of the WDXRF and TXRF techniques was assessed by the comparative analysis of reference materials of sediments, soil and biological samples. In general, good agreement was achieved between the reference values and the measured values. The detection limits of Br were 1mg/kg and 0.4mg/kg for WDXRF and TXRF respectively. The results of the Br determination obtained with different XRF techniques were comparable to each other and used for paleoclimatic reconstructions. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Surface analytical investigation of diamond coatings and nucleation processes by secondary ion mass spectrometry

    International Nuclear Information System (INIS)

    Steiner, R.

    1993-10-01

    Imaging SIMS for the investigation of substrate surfaces: the influence of the substrate surface on diamond nucleation is a major topic in the investigation of the chemical vapour deposition (CVD) of diamond. It is well known that the nucleation density can be enhanced by scratching the substrate surface with abrasive powders. Diamond can nucleate at scratches or at residues of the polishing material. In the present work the surface of refractory metals (Mo, Nb, Ta, W) polished with silicon carbide and diamond powder is studied by imaging (2- or 3-D) secondary ion mass spectrometry (SIMS). In first experiments the distribution of SiC and/or diamond residues after polishing was determined. The reaction of diamond with the substrate during heating to deposition temperatures was investigated. Investigation of WC/Co hardmetal substrates: it is well known that Co contained in the binder phase of the hard metal inhibits a strong adhesion between the diamond film and the substrate, which is need for an application as cutting tool. Several attempts to improve the adhesion have been reported up to now. In this work a pre-treatment procedure leading to the formation of Co compounds (borides and silicides) which are stable under diamond deposition conditions were investigated. Furthermore, the application of intermediate sputter layers consisting of chromium and titanium were studied. Investigation of P-doped diamond coatings: in the quaternary phase diagram C-P-B-N exist some phases with diamond structure and superhard phases (e.g BP, c-BN). Also a hypothetical superhard phase of the composition C 3 N 4 is predicted. A scientific objective is the synthesis of such phases by chemical vapour deposition. An increase of the phosphorus concentration effects a distinct change in the morphology of the deposited coatings. A major advantage of SIMS is that the concentration profiles can be measured through the whole film, due to the sputter removal of the sample, and the interface

  17. Combination of atomic force microscopy and mass spectrometry for the detection of target protein in the serum samples of children with autism spectrum disorders

    Science.gov (United States)

    Kaysheva, A. L.; Pleshakova, T. O.; Kopylov, A. T.; Shumov, I. D.; Iourov, I. Y.; Vorsanova, S. G.; Yurov, Y. B.; Ziborov, V. S.; Archakov, A. I.; Ivanov, Y. D.

    2017-10-01

    Possibility of detection of target proteins associated with development of autistic disorders in children with use of combined atomic force microscopy and mass spectrometry (AFM/MS) method is demonstrated. The proposed method is based on the combination of affine enrichment of proteins from biological samples and visualization of these proteins by AFM and MS analysis with quantitative detection of target proteins.

  18. Evaluation of an inductively-coupled plasma with an extended-sleeve torch as an atomization cell for laser-excited fluorescence spectrometry.

    Science.gov (United States)

    Kosinski, M A; Uchida, H; Winefordner, J D

    1983-05-01

    An inductively-coupled plasma (ICP) with an extended-sleeve torch has been evaluated as an atomization cell for laser-excited fluorescence spectrometry. Limits of detection for 20 lines are given. The detection power is almost equivalent to that obtained by excitation with a hollow-cathode lamp. Interelement effects and spectral interferences are discussed.

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

    DEFF Research Database (Denmark)

    Fiamegkos, I.; Cordeiro, F.; Robouch, P.

    2016-01-01

    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...

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

    DEFF Research Database (Denmark)

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

    1997-01-01

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

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

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Sturup, Stefan; Spliid, Henrik

    1999-01-01

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

  2. Determination of trace impurities of aluminium, cadmium, chromium, copper and nickel in indium phosphate by flameless atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Chruscinska, T.J.

    1990-01-01

    The sample (0.25 g) was treated with a nitric (0.9 ml) + hydrochloric (0.25 ml) acid mixture, heated to syrup under glass and then dissolved with 5 mol · 1 -1 HNO 3 (1 ml). The traces were determined in 0.2 mol · 1 -1 HNO 3 using Perkin-Elmer Model 430 Atomic Absorption Spectrometer equipped with a HGA 76B Graphite Furnace and an AS-1 Auto Sampling System. Pyrolytically coated and then tantalum treated tubes was employed. Additive errors due to contamination with, and loss of, the analyte element were controlled by estimation of the blank value and recovery. Background was corrected throughout. The background correction system efficiency was checked for the continuum background by two line method and for structured background by decreasing the slit or choosing different analytical lines. No other multiplicative (influencing the slope of the analytical curve) matrix interferences were found except for cadmium. (author). 12 refs, 4 tabs, 3 figs

  3. Direct sampling graphite furnace atomic absorption spectrometry - feasibility of Na and K determination in desalted crude oil

    Science.gov (United States)

    Seeger, Tassia S.; Machado, Eduarda Q.; Flores, Erico M. M.; Mello, Paola A.; Duarte, Fabio A.

    2018-03-01

    In this study, Na and K were determined in desalted crude oil by direct sampling graphite furnace atomic absorption spectrometry (DS-GF AAS), with the use of a Zeeman-effect background correction system with variable magnetic field. The analysis was performed in low and high sensitivity conditions. Sodium determination was performed in two low-sensitivity conditions: 1) main absorption line (589.0 nm), gas stop flow during the atomization step and 3-field dynamic mode (0.6-0.8 T); and 2) secondary absorption line (330.3 nm), gas stop flow during the atomization and 2-field mode (0.8 T). In K determination, some parameters, such as high-sensitivity mode, main absorption line (766.5 nm), gas stop flow during the atomization and 2-field mode (0.8 T), were used. Suitability of chemical modifiers, such as Pd and W-Ir was also evaluated. The heating program for Na and K was based on the pyrolysis and atomization curves. Calibration was performed by aqueous standards. Accuracy was evaluated by the analysis of Green Petroleum Coke (SRM NIST 2718) and Trace Elements in Fuel Oil (SRM NIST 1634c). Recovery tests were also performed and results were compared with those obtained by GF AAS after crude oil digestion by microwave-assisted digestion. The characteristic mass of Na was 17.1 pg and 0.46 ng in conditions 1 and 2, respectively, while the one of K was 1.4 pg. Limits of detection and quantification by DS-GF AAS were 30 and 40 ng g-1 for Na and 3.2 and 4.2 ng g-1 for K, respectively. Sodium and K were determined in three crude oil samples with API density ranging from 20.9 to 28.0. Sodium and K concentration ranged from 1.5 to 73 μg g-1 and from 23 to 522 ng g-1, respectively.

  4. Analytical investigation of one-dimensional Rydberg atoms interacting with half-cycle pulses

    International Nuclear Information System (INIS)

    Bersons, I.; Veilande, R.

    2004-01-01

    Classical, quantum-mechanical, and semiclassical expressions for the transition probability in one-dimensional Rydberg atom irradiated by short half-cycle pulse are derived and compared. The simple formulas obtained for excitation of Rydberg atom by two time delayed weak half-cycle pulses reproduce well the experimental data and the solutions of time-dependent Schroedinger equation. When the transferred momenta are stronger and positive, the transition probabilities exhibit fast oscillations with time delay between the pulses. The classical transition probability is constant in time. For negative transferred momenta a focusing phenomenon is observed, and there is a region in time delay, where the transition probabilities oscillate with the Kepler period

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

    Science.gov (United States)

    Salih, Bekir; Celikbiçak, Omür; Döker, Serhat; Doğan, Mehmet

    2007-03-28

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

  6. 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

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

    International Nuclear Information System (INIS)

    Xiang Guoqiang; Zhang Yingming; Jiang Xiuming; He Lijun; Fan Lu; Zhao Wenjie

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-07-15

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

  9. Thermodynamics of atomic and ionized hydrogen: analytical results versus equation-of-state tables and Monte Carlo data.

    Science.gov (United States)

    Alastuey, A; Ballenegger, V

    2012-12-01

    We compute thermodynamical properties of a low-density hydrogen gas within the physical picture, in which the system is described as a quantum electron-proton plasma interacting via the Coulomb potential. Our calculations are done using the exact scaled low-temperature (SLT) expansion, which provides a rigorous extension of the well-known virial expansion-valid in the fully ionized phase-into the Saha regime where the system is partially or fully recombined into hydrogen atoms. After recalling the SLT expansion of the pressure [A. Alastuey et al., J. Stat. Phys. 130, 1119 (2008)], we obtain the SLT expansions of the chemical potential and of the internal energy, up to order exp(-|E_{H}|/kT) included (E_{H}≃-13.6 eV). Those truncated expansions describe the first five nonideal corrections to the ideal Saha law. They account exactly, up to the considered order, for all effects of interactions and thermal excitations, including the formation of bound states (atom H, ions H^{-} and H_{2}^{+}, molecule H_{2},⋯) and atom-charge and atom-atom interactions. Among the five leading corrections, three are easy to evaluate, while the remaining ones involve well-defined internal partition functions for the molecule H_{2} and ions H^{-} and H_{2}^{+}, for which no closed-form analytical formula exist currently. We provide accurate low-temperature approximations for those partition functions by using known values of rotational and vibrational energies. We compare then the predictions of the SLT expansion, for the pressure and the internal energy, with, on the one hand, the equation-of-state tables obtained within the opacity program at Livermore (OPAL) and, on the other hand, data of path integral quantum Monte Carlo (PIMC) simulations. In general, a good agreement is found. At low densities, the simple analytical SLT formulas reproduce the values of the OPAL tables up to the last digit in a large range of temperatures, while at higher densities (ρ∼10^{-2} g/cm^{3}), some

  10. International Atomic Energy Agency consultants' meeting on Analytical Quality Control Services, Vienna, 17-19 September 1990

    International Nuclear Information System (INIS)

    1990-10-01

    An International Atomic Energy Agency Consultants' Meeting on Analytical Quality Control Services was held at the Vienna International Center 17-19 September 1990. The Consultants generally conclude that the current methods of the preparation of the materials for intercomparison studies and facilities are adequate for the current Agency mission for trace element and radionuclide materials, but it is suggested that freeze-drying facilities for biological materials are needed. This is critically important for many of the collected materials uniquely important to the Agency mission. Also new equipment for automated sieving analysis be acquired for some applications. Homogeneity testing performed by AQCS includes the determination of several trace elements (radionuclides) of different concentrations of several sub-samples taken from one bottle and the results are compared with those obtained for sub-samples taken from various bottles chosen at random using one way analysis of variance. This procedure is found to be appropriate and could be used further. TC and CRP should be promoted in relation to the development of reliable analytical methods for the determination of so called ''difficult elements'' like: Mo, Al, I, F, Li, Co, Cd and Ni as well as 237 Np, 226 Ra, 228 Ra. Intercomparison runs should stay open to the whole international community although it would be desirable to consult ''reference labs'' for the certification of selected (''difficult'') analytes. The presently employed programme for intercomparison studies for data evaluation are valuable and suitable. Refs, figs and tabs

  11. 7th Czechoslovak spectroscopic conference and VIIIth CANAS (Conference on analytical atomic spectroscopy). Abstracts. Vol. 2

    International Nuclear Information System (INIS)

    1984-01-01

    The conference on spectroscopy held in Ceske Budejovice on June 18-22, 1984, proceeded in three sessions: atomic spectroscopy, molecular spectroscopy and special spectroscopic techniques. In the molecular spectroscopy session, 81 papers were read of which 12 were inputted in INIS. The subject of inputted papers was the use of NMR for the analysis of organic compounds and for the study of radiation defects in semiconductors, and the use of infrared spectroscopy for the analysis of nuclear and irradiated materials. (J.P.)

  12. On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yebra, M.C.; Moreno-Cid, A.

    2003-01-01

    Manganese is extracted on-line from solid seafood samples by a simple continuous ultrasound-assisted extraction system (CUES). This system is connected to an on-line manifold, which permits the flow-injection flame atomic absorption spectrometric determination of manganese. Optimisation of the continuous leaching procedure is performed by an experimental design. The proposed method allows the determination of manganese with a relative standard deviation of 0.9% for a sample containing 23.4 μg g -1 manganese (dry mass). The detection limit is 0.4 μg g -1 (dry mass) for 30 mg of sample and the sample throughput is ca. 60 samples per hour. Accurate results are obtained by measuring TORT-1 certified reference material. The procedure is finally applied to mussel, tuna, sardine and clams samples

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

    Science.gov (United States)

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

    1976-01-01

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

  14. Three-dimensional molecular imaging using mass spectrometry and atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Wucher, Andreas [Department of Physics, University of Duisburg-Essen, D-47048 Duisburg (Germany)], E-mail: andreas.wucher@uni-due.de; Cheng Juan; Zheng Leiliang; Willingham, David; Winograd, Nicholas [Department of Chemistry, Pennsylvania State University, University Park, PA 16802 (United States)

    2008-12-15

    We combine imaging ToF-SIMS depth profiling and wide area atomic force microscopy to analyze a test structure consisting of a 300 nm trehalose film deposited on a Si substrate and pre-structured by means of a focused 15-keV Ga{sup +} ion beam. Depth profiling is performed using a 40-keV C{sub 60}{sup +} cluster ion beam for erosion and mass spectral data acquisition. A generic protocol for depth axis calibration is described which takes into account both lateral and in-depth variations of the erosion rate. By extrapolation towards zero analyzed lateral area, an 'intrinsic' depth resolution of about 8 nm is found which appears to be characteristic of the cluster-surface interaction process.

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

    Science.gov (United States)

    Çiftçi, Tülin Deniz; Henden, Emur

    2016-08-01

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

  16. 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.

  17. 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.

  18. Selective extraction of traffic-related antimony compounds for speciation analysis by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zih-Perenyi, K., E-mail: perkat@freestart.h [L. Eoetvoes University, Institute of Chemistry, H-1518 Budapest 112, P.O. Box 32. (Hungary); Neurohr, K., E-mail: kata.neurohr@gmail.co [L. Eoetvoes University, Institute of Chemistry, H-1518 Budapest 112, P.O. Box 32. (Hungary); Nagy, G. [Semmelweis University, Faculty of Pharmacy, H-1085 Budapest, Ulloi Str. 26. (Hungary); Balla, M., E-mail: balla@reakt.bme.h [Budapest University of Technology and Economics, Institute of Nuclear Techniques, H-1111 Budapest, Muegyetem rakpart 9 (Hungary); Lasztity, A., E-mail: alasztity@gmail.co [L. Eoetvoes University, Institute of Chemistry, H-1518 Budapest 112, P.O. Box 32. (Hungary)

    2010-09-15

    Most traffic-related antimony air pollutants are derived from brake dust. Brake dust contains Sb{sub 2}S{sub 3}, used as a friction material in brake pads, and its high-temperature oxidation products, Sb{sub 2}O{sub 3} or Sb{sub 2}O{sub 4}. Systematic investigations were carried out to find the most selective leaching conditions for these substances. First, solubility experiments of the pure potential compounds mentioned above were carried out. Then, the leaching of these compounds from home-made artificial dusts previously spiked with these compounds at the trace level was investigated. A 0.5 mol L{sup -1} citric acid solution proved to leach the whole Sb{sub 2}O{sub 3} content while extracting less than 10% Sb{sub 2}S{sub 3} and no Sb{sub 2}O{sub 4} at all. It was found that Sb{sub 2}O{sub 3} and Sb{sub 2}S{sub 3} traces were soluble in a 6 mol L{sup -1} HCl solution, quantitatively and selectively. Graphite furnace atomic absorption spectrometry and hydride generation graphite furnace atomic absorption spectrometry methods were developed to determine the Sb content of the extracts. The proposed method proved to be applicable to settled dust containing traffic-related Sb compounds. The detection limits were 1.2 and 0.3 {mu}g g{sup -1} for leaching by citric acid and HCl solution, respectively, which were adequate for Sb content determination in the urban dust studied. The reproducibility of the method expressed as relative standard deviation was about 7%. The results showed that the concentration of leachable Sb was 40 {mu}g g{sup -1} in the settled dust of Budapest, about half of which corresponded to Sb{sub 2}O{sub 3}. The Sb{sub 2}O{sub 4} content calculated as the difference of total and leachable fraction was about 10% with high uncertainty.

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

    Science.gov (United States)

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

    2015-04-01

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

  20. Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Zhang Yanlin; Adeloju, Samuel B.

    2012-01-01

    Highlights: ► Successful speciation of inorganic and organic Hg with Fe 3+ , Cu 2+ and thiourea as catalysts. ► Best sensitivity enhancement and similar sensitivity for MeHg and Hg 2+ with Fe 3+ . ► Successful use of Hg 2+ as the primary standard for quantification of inorganic and total-Hg. ► Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. ► Integration with FIA for rapid analysis with a sample throughput of 180 h −1 . - Abstract: A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH 4 were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe 3+ , Cu 2+ and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu 2+ and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe 3+ gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg 2+ . Due to similarity of resulting sensitivity, Hg 2+ was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury, respectively. The use of flow injection enabled rapid analysis with a sample throughput of 180 h −1 .

  1. Applicability of cloud point extraction for the separation trace amount of lead ion in environmental and biological samples prior to determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Sayed Zia Mohammadi

    2016-09-01

    Full Text Available A sensitive cloud point extraction procedure(CPE for the preconcentration of trace lead prior to its determination by flame atomic absorption spectrometry (FAAS has been developed. The CPE method is based on the complex of Pb(II ion with 1-(2-pyridylazo-2-naphthol (PAN, and then entrapped in the non-ionic surfactant Triton X-114. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PAN and Triton X-114, equilibration temperature and time, were investigated in detail. A preconcentration factor of 30 was obtained for the preconcentration of Pb(II ion with 15.0 mL solution. Under the optimal conditions, the calibration curve was linear in the range of 7.5 ng mL−1–3.5 μg mL−1 of lead with R2 = 0.9998 (n = 10. Detection limit based on three times the standard deviation of the blank (3Sb was 5.27 ng mL−1. Eight replicate determinations of 1.0 μg mL−1 lead gave a mean absorbance of 0.275 with a relative standard deviation of 1.6%. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed method has been applied for determination of trace amounts of lead in biological and water samples with satisfactory results.

  2. Determination of Pb (Lead, Cd (Cadmium, Cr (Chromium, Cu (Copper, and Ni (Nickel in Chinese tea with high-resolution continuum source graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Wen-Si Zhong

    2016-01-01

    Full Text Available The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5% and recoveries (98.91–101.32%. The lead contents in tea leaves were 0.48–10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73–63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea.

  3. Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

    2018-03-01

    A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. L-tyrosine immobilized on multiwalled carbon nanotubes: a new substrate for thallium separation and speciation using stabilized temperature platform furnace-electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Pacheco, Pablo H; Gil, Raúl A; Smichowski, Patricia; Polla, Griselda; Martinez, Luis D

    2009-12-10

    An approach for the separation and determination of inorganic thallium species is described. A new sorbent, L-tyrosine-carbon nanotubes (L-tyr-CNTs), was used and applied to the analysis of tap water samples. At pH 5.0, L-tyr was selective only towards Tl(III), while total thallium was determined directly by stabilized temperature platform furnace-electrothermal atomic absorption spectrometry (STPF-ETAAS). The Tl(III) specie, which was retained by L-tyrosine, was quantitatively eluted from the column with 10% of nitric acid. An on-line breakthrough curve was used to determine the column capacity, which resulted to be 9.00 micromol of Tl(III) g(-1) of L-tyr-CNTs with a molar ratio of 0.14 (moles of Tl bound to moles of L-tyr at pH 5). Transient peak areas revealed that Tl stripping from the column occurred instantaneously. Effects of sample flow rate, concentration and flow rate of the eluent, and interfering ions on the recovery of the analyte were systematically investigated. The detection limit for the determination of total thallium (3sigma) by STPF-ETAAS was 150 ng L(-1). The detection limit (3sigma) for Tl(III) employing the separation system was 3 ng L(-1), with an enrichment factor of 40. The precision of the method expressed as the relative standard deviation (RSD) resulted to be 3.4%. The proposed method was applied to the speciation and determination of inorganic thallium in tap water samples. The found concentrations were in the range of 0.88-0.91 microg L(-1) of Tl(III), and 3.69-3.91 microg L(-1) of total thallium.

  5. Determination of Pb (Lead), Cd (Cadmium), Cr (Chromium), Cu (Copper), and Ni (Nickel) in Chinese tea with high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Zhong, Wen-Si; Ren, Ting; Zhao, Li-Jiao

    2016-01-01

    The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5%) and recoveries (98.91-101.32%). The lead contents in tea leaves were 0.48-10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73-63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea. Copyright © 2015. Published by Elsevier B.V.

  6. L-Tyrosine immobilized on multiwalled carbon nanotubes: A new substrate for thallium separation and speciation using stabilized temperature platform furnace-electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pacheco, Pablo H.; Gil, Raul A. [Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, P.O. Box 375, 5700 San Luis (Argentina); Instituto de Quimica de San Luis (INQUISAL-CONICET), Chacabuco y Pedernera, CP 5700, San Luis (Argentina); Smichowski, Patricia, E-mail: smichows@cnea.gov.ar [Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Rivadavia 1917, CP C1033 AAJ, Ciudad de Buenos Aires (Argentina); Comision Nacional de Energia Atomica, Gerencia Quimica, Av. Gral. Paz 1499, B1650KNA San Martin (Argentina); Polla, Griselda [Comision Nacional de Energia Atomica, Gerencia de Investigacion y Aplicaciones, Av.Gral. Paz 1499, B1650KNA San Martin (Argentina); Martinez, Luis D., E-mail: ldm@unsl.edu.ar [Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, P.O. Box 375, 5700 San Luis (Argentina); Instituto de Quimica de San Luis (INQUISAL-CONICET), Chacabuco y Pedernera, CP 5700, San Luis (Argentina)

    2009-12-10

    An approach for the separation and determination of inorganic thallium species is described. A new sorbent, L-tyrosine-carbon nanotubes (L-tyr-CNTs), was used and applied to the analysis of tap water samples. At pH 5.0, L-tyr was selective only towards Tl(III), while total thallium was determined directly by stabilized temperature platform furnace-electrothermal atomic absorption spectrometry (STPF-ETAAS). The Tl(III) specie, which was retained by L-tyrosine, was quantitatively eluted from the column with 10% of nitric acid. An on-line breakthrough curve was used to determine the column capacity, which resulted to be 9.00 {mu}mol of Tl(III) g{sup -1} of L-tyr-CNTs with a molar ratio of 0.14 (moles of Tl bound to moles of L-tyr at pH 5). Transient peak areas revealed that Tl stripping from the column occurred instantaneously. Effects of sample flow rate, concentration and flow rate of the eluent, and interfering ions on the recovery of the analyte were systematically investigated. The detection limit for the determination of total thallium (3{sigma}) by STPF-ETAAS was 150 ng L{sup -1}. The detection limit (3{sigma}) for Tl(III) employing the separation system was 3 ng L{sup -1}, with an enrichment factor of 40. The precision of the method expressed as the relative standard deviation (RSD) resulted to be 3.4%. The proposed method was applied to the speciation and determination of inorganic thallium in tap water samples. The found concentrations were in the range of 0.88-0.91 {mu}g L{sup -1} of Tl(III), and 3.69-3.91 {mu}g L{sup -1} of total thallium.

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

    Science.gov (United States)

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

    2015-01-07

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

  8. L-Tyrosine immobilized on multiwalled carbon nanotubes: A new substrate for thallium separation and speciation using stabilized temperature platform furnace-electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Pacheco, Pablo H.; Gil, Raul A.; Smichowski, Patricia; Polla, Griselda; Martinez, Luis D.

    2009-01-01

    An approach for the separation and determination of inorganic thallium species is described. A new sorbent, L-tyrosine-carbon nanotubes (L-tyr-CNTs), was used and applied to the analysis of tap water samples. At pH 5.0, L-tyr was selective only towards Tl(III), while total thallium was determined directly by stabilized temperature platform furnace-electrothermal atomic absorption spectrometry (STPF-ETAAS). The Tl(III) specie, which was retained by L-tyrosine, was quantitatively eluted from the column with 10% of nitric acid. An on-line breakthrough curve was used to determine the column capacity, which resulted to be 9.00 μmol of Tl(III) g -1 of L-tyr-CNTs with a molar ratio of 0.14 (moles of Tl bound to moles of L-tyr at pH 5). Transient peak areas revealed that Tl stripping from the column occurred instantaneously. Effects of sample flow rate, concentration and flow rate of the eluent, and interfering ions on the recovery of the analyte were systematically investigated. The detection limit for the determination of total thallium (3σ) by STPF-ETAAS was 150 ng L -1 . The detection limit (3σ) for Tl(III) employing the separation system was 3 ng L -1 , with an enrichment factor of 40. The precision of the method expressed as the relative standard deviation (RSD) resulted to be 3.4%. The proposed method was applied to the speciation and determination of inorganic thallium in tap water samples. The found concentrations were in the range of 0.88-0.91 μg L -1 of Tl(III), and 3.69-3.91 μg L -1 of total thallium.

  9. Determination of trace cadmium in rice by liquid spray dielectric barrier discharge induced plasma - chemical vapor generation coupled with atomic fluorescence spectrometry

    Science.gov (United States)

    Liu, Xing; Zhu, Zhenli; Bao, Zhengyu; Zheng, Hongtao; Hu, Shenghong

    2018-03-01

    Cadmium contamination in rice has become an increasing concern in many countries including China. A simple, cost-effective, and highly sensitive method was developed for the determination of trace cadmium in rice samples based on a new high-efficient liquid spray dielectric barrier discharge induced plasma (LSDBD) vapor generation coupled with atomic fluorescence spectrometry (AFS). The analytical procedure involves the efficient formation of Cd volatile species by LSDBD plasma induced chemical processes without the use of any reducing reagents (Na/KBH4 in conventional hydride generation). The effects of the addition of organic substances, different discharge parameters such as discharge voltage and discharge gap, as well as the foreign ion interferences were investigated. Under optimized conditions, a detection limit of 0.01 μg L- 1 and a precision of 0.8% (RSD, n = 5, 1 μg L- 1 Cd) was readily achieved. The calibration curve was linear in the range between 0.1 and 10 μg L- 1, with a correlation coefficient of R2 = 0.9995. Compared with the conventional acid-BH4- vapor generation, the proposed method not only eliminates the use of unstable and expensive reagents, but also offers high tolerance for coexisting ions, which is well suited to the direct analysis of environmental samples. The validation of the proposed method was demonstrated by the analysis of Cd in reference material of rice (GBW080684). It was also successfully applied to the determination of trace cadmium in locally collected 11 rice samples, and the obtained Cd concentrations are ranged from 7.2 to 517.7 μg kg- 1.

  10. Determination of inorganic arsenic in algae using bromine halogenation and on-line nonpolar solid phase extraction followed by hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Zhang, Weihong; Qi, Yuehan; Qin, Deyuan; Liu, Jixin; Mao, Xuefei; Chen, Guoying; Wei, Chao; Qian, Yongzhong

    2017-08-01

    Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and on-line nonpolar solid phase extraction (SPE) followed by hydride generation atomic fluorescence spectrometry (HG-AFS). The separation of iAs from algae was first performed by nonpolar SPE sorbent using Br - for arsenic halogenation. Algae samples were extracted with 1% perchloric acid. Then, 1.5mL extract was reduced by 1% thiourea, and simultaneously reacted (for 30min) with 50μL of 10% KBr for converting iAs to AsBr 3 after adding 3.5mL of 70% HCl to 5mL. A polystyrene (PS) resin cartridge was employed to retain arsenicals, which were hydrolyzed, eluted from the PS resin with H 2 O, and categorized as iAs. The total iAs was quantified by HG-AFS. Under optimum conditions, the spiked recoveries of iAs in real algae samples were in the 82-96% range, and the method achieved a desirable limit of detection of 3μgkg -1 . The inter-day relative standard deviations were 4.5% and 4.1% for spiked 100 and 500μgkg -1 respectively, which proved acceptable for this method. For real algae samples analysis, the highest presence of iAs was found in sargassum fusiforme, followed by kelp, seaweed and laver. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Supramolecular-Based Ultrasonic-Assisted Dispersion Solidification Liquid-Liquid Microextraction of Copper and Cobalt Prior to Their Flame Atomic Absorption Spectrometry Determination.

    Science.gov (United States)

    Shokrollahi, Ardeshir; Ebrahimi, Foroogh

    2017-11-01

    In the present work, a simple, efficient, and environmentally friendly method was proposed for the simultaneous preconcentration and determination of minute quantities of copper and cobalt in water samples and serum by a supramolecular-based ultrasonic-assisted dispersion solidification liquid-liquid microextraction (DSLLME) procedure coupled with flame atomic absorption spectrometry. The procedure is based on the DSLLME of copper and cobalt with decanoic acid-tetrahydrofuran supramolecular solvent (SUPRAS) in the presence of sodium diethyldithiocarbamate, as the complexing agent. SUPRAS is a nanostructured liquid generated from amphiphiles through a sequential self-assembly process occurring on two scales, molecular and nano. Several variables that affect the extraction efficiency-including pH, concentration of complexing agent, volume of the extraction and dispersive solvents (volume of SUPRAS), sonication time, and ionic strength-were investigated and optimized. The method provided enrichment factors of 23.31 and 22.38 for copper and cobalt, respectively. The preconcentration factor for the two analytes was 20.00. Calibration plots were linear in the range of 5.00-700.00 ng/mL for copper and 5.00-500.00 ng/mL for cobalt, with correlations of determination of 0.9973 and 0.9981. The precision of the method were expressed as RSDs for six replicate measurements and LODs and found to be ±4.10 and ±2.30% for copper and 2.90 and 3.50 ng/mL for cobalt. The proposed method was successfully applied to the simultaneous determination of trace copper and cobalt in real water samples and serum with satisfactory results.

  12. MPTS-silica coated capillary microextraction on line hyphenated with inductively coupled plasma atomic emission spectrometry for the determination of Cu, Hg and Pb in biological samples.

    Science.gov (United States)

    Zheng, Fei; Hu, Bin

    2007-09-15

    A novel sol-gel 3-mercaptopropyltrimethoxysilane (MPTS) modified silica coating was developed for capillary microextraction (CME) of trace Cu, Hg and Pb prior to their on line determination by inductively coupled plasma-atomic emission spectrometry (ICP-AES). This organic-inorganic hybrid coating was in situ created on the inner walls of fused silica capillary using a sol solution containing TMOS (tetramethoxysilane) as a precursor, MPTS as a co-precursor, ethanol as the solvent and hydrochloric acid as a catalyst. The structure of the capillary coating was characterized by FT-IR spectroscopy, Raman spectroscopy, SEM and TEM. The factors affecting on the capillary microextraction of analytes such as pH, sample flow rate and volume, elution solution and interfering ions had been investigated, and the optimized experimental parameters were obtained. Under the optimized conditions, the absorption capacity of MPTS-silica coated capillary was found to be 1.17, 1.96 and 1.19mugm(-1) for Cu, Hg and Pb, and the limits of detection were as low as 0.17 0.22 and 0.52ngmL(-1), respectively. With a sampling frequency of 12h(-1), the relative standard deviations (R.S.D.s) were 4.2, 2.6 and 3.8% (C=4ngmL(-1), n=7, sample volume=1mL) for Cu, Hg and Pb, respectively. The proposed method had been successfully applied to the determination of Cu, Hg and Pb in human urine, human serum and preserved egg. To validate the proposed method, certified reference materials of BCR151 milk powder, GBW07601 (GSH-1) human hair, GSBZ 50016-90 and GSB 07-1183-2000 water samples were analyzed and the determined values were in a good agreement with the certified values.

  13. 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.

  14. Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

    2016-02-05

    An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be <5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L(-1) and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

    Science.gov (United States)

    Sadeghi, Susan; Ashoori, Vahid

    2017-10-01

    The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF 6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF 6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL -1 , respectively, with a detection limit of 6.9 ng mL -1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  16. Preconcentration and determination of vanadium and molybdenum in milk, vegetables and foodstuffs by ultrasonic-thermostatic-assisted cloud point extraction coupled to flame atomic absorption spectrometry.

    Science.gov (United States)

    Gürkan, Ramazan; Korkmaz, Sema; Altunay, Nail

    2016-08-01

    A new ultrasonic-thermostatic-assisted cloud point extraction procedure (UTA-CPE) was developed for preconcentration at the trace levels of vanadium (V) and molybdenum (Mo) in milk, vegetables and foodstuffs prior to determination via flame atomic absorption spectrometry (FAAS). The method is based on the ion-association of stable anionic oxalate complexes of V(V) and Mo(VI) with [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) at pH 4.5, and then extraction of the formed ion-association complexes into micellar phase of polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5). The UTA-CPE is greatly simplified and accelerated compared to traditional cloud point extraction (CPE). The analytical parameters optimized are solution pH, the concentrations of complexing reagents (oxalate and Nile blue A), the PONPE 7.5 concentration, electrolyte concentration, sample volume, temperature and ultrasonic power. Under the optimum conditions, the calibration curves for Mo(VI) and V(V) are obtained in the concentration range of 3-340µgL(-1) and 5-250µgL(-1) with high sensitivity enhancement factors (EFs) of 145 and 115, respectively. The limits of detection (LODs) for Mo(VI) and V(V) are 0.86 and 1.55µgL(-1), respectively. The proposed method demonstrated good performances such as relative standard deviations (as RSD %) (≤3.5%) and spiked recoveries (95.7-102.3%). The accuracy of the method was assessed by analysis of two standard reference materials (SRMs) and recoveries of spiked solutions. The method was successfully applied into the determination of trace amounts of Mo(VI) and V(V) in milk, vegetables and foodstuffs with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. 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.

  18. Determination of trace elements in refined gold samples by inductively coupled plasma atomic emission spectrometry

    Directory of Open Access Journals (Sweden)

    Steharnik Mirjana

    2013-01-01

    Full Text Available This paper presents a method for determination the trace contents of silver, copper, iron, palladium, zinc and platinum in refined gold samples. Simultaneous inductively coupled plasma atomic emission spectrometer with radial torch position and cross flow nebulizer was used for determination. In order to compare the different calibration strategies, two sets of calibration standards were prepared. The first set was based on matrix matched calibration standards and the second was prepared without the addition of matrix material. Detection limits for matrix matching calibrations were higher for some elements than those without matrix matching. In addition, the internal standardization method was applied and experiments indicated that indium was the best option as internal standard. The obtained results for gold sample by matrix matching and matrix free calibrations were compared with the obtained results by standard addition method. The accuracy of the methods was tested performing recovery test. Recoveries for spiked sample were in the range of 90-115 %. The accuracy of the methods was also tested by analysis of certified reference material of high pure goldAuGHP1. The best results were achieved by matrix free calibration and standard addition method using indium as internal standard at wavelength of 230 nm. [Projekat Ministarstva nauke Republike Srbije, br. 34024: Development of Technologies for Recycling of Precious, Rare and Associated Metals from Solid Waste in Serbia to High Purity Products

  19. Hyperfine structure measurements of neutral iodine atom (127I) using Fourier Transform Spectrometry

    Science.gov (United States)

    Ashok, Chilukoti; Vishwakarma, S. R.; Bhatt, Himal; Ankush, B. K.; Deo, M. N.

    2018-01-01

    We report the hyperfine Structure (hfs) splitting observations of neutral iodine atom (II) in the 6000 - 10,000 cm-1 near infrared spectral region. The measurements were carried out using a high-resolution Fourier Transform Spectrometer (FTS), where an electrodeless discharge lamp (EDL), excited using microwaves, was employed as the light source and InGaAs as the light detector. A specially designed setup was used to lower the plasma temperature of the medium so as to reduce the Doppler width and consequently to increase the spectral resolution of hfs components. A total of 183 lines with hfs splitting have been observed, out of which hfs in 53 spectral lines are reported for the first time. On the basis of hfs analysis, we derived the magnetic dipole and electric quadrupole coupling constants, A and B respectively for 30 even and 30 odd energy levels and are compared with the values available in the literature. New hfs values for 5 even and 4 odd levels are also reported here for the first time.

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

    Science.gov (United States)

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

    1990-01-01

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

  1. 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)

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

    International Nuclear Information System (INIS)

    Ruiz, Frine; Benzo, Zully; Quintal, Manuelita; Garaboto, Angel; Albornoz, Alberto; Brito, Joaquin L.

    2006-01-01

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

  3. Effects of coupling efficiency on atomic spectrometry with a microwave-induced plasma

    International Nuclear Information System (INIS)

    Burns, B.A.

    1987-01-01

    The atmospheric-pressure, microwave-induced argon plasma from a TM 010 mode cavity is made nearly 100% efficient by matching the impedance of the generator to the impedance of the load. The impedance match is achieved by increasing the size of the coupling probe and by varying cavity permittivity and microwave probe position to lower the reflected power to nearly zero watts. The efficient microwave plasma is capable of operating with as little as 5 watts of power, producing plasma plumes of 16 cm in length when operated at 100 watts, reflecting almost no measurable power, and generating virtually no cavity heat. With plasma power known for all operating conditions, experiments were performed to help create a model for the efficient operation of the cavity at all input powers. This model was used to correlate the plasma electron density with plasma power for a further fundamental understanding of the microwave-induced plasma. The model for the efficient microwave plasma is related to the changes in cavity E-field intensity with changes in plasma electron production. The model describes the flow of power from the generator to the plasma and allows correlation of observed phenomena, i.e., plasma electron density and analyte emission intensity, with plasma power

  4. Bio-analytical method development and validation of Rasagiline by high performance liquid chromatography tandem mass spectrometry detection and its application to pharmacokinetic study

    OpenAIRE

    Ravi Kumar Konda; Babu Rao Chandu; B.R. Challa; Chandrasekhar B. Kothapalli

    2012-01-01

    The most suitable bio-analytical method based on liquidâliquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mmÃ50 mm, 3.5 μm) column provided chromatographic separation of analyte followed by detection with mass spectrometry. The method involved simple isocratic chromatographic condition and mass spectrometric detection in the positive ion...

  5. 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.

  6. Determination of essential and toxic elements in commercial baby foods by instrumental neutron activation analysis and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Vallinoto, Priscila

    2013-01-01

    The World Health Organization recommends that infants should be breast fed exclusively for at least six months after birth. After this period, it is recommended to start introducing complementary foods, in order to meet the child's nutritional, mineral and energy needs. Commercial food products for infants form an important part of the diet for many babies. Thus, it is very important that such food contains sufficient amounts of minerals. Inadequate complementary feeding is a major cause of high rates of infant malnutrition in developing countries. In this study, essential elements: Ca, Cl, Co, Cr, Fe, K, Mg, Mn, Na, Se and Zn and toxic elements: As, Cd, Hg levels were determined in twenty seven different commercial infant food product samples by Instrumental Neutron Activation Analysis (INAA) and Atomic Absorption Spectrometry (AAS). In order to validate both methodologies the reference material: INCT MPH-2 Mixed Polish Herbs and NIST - SRM 1577b Bovine Liver by INAA and NIST - SRM 1548th Typical Diet and NIST - SRM 1547 Peach Leaves by AAS were analyzed. The twenty seven baby food samples were acquired from Sao Paulo city supermarkets and stores. Essential and toxic elements were determined. Most of the essential element concentrations obtained were lower than the World Health Organization requirements, while concentrations of toxic elements were below the tolerable upper limit. These low essential element concentrations in these samples indicate that infants should not be fed only with commercial complementary foods. (author)

  7. 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

  8. Studies on analysis of gallium and indium in zinc ores by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Hwang, Youn Ok; Sim, Sang Kwon; Sung, Hack Je; Yang, Myung Kwon

    1993-01-01

    The separation of gallium and indium from the matrix elements such as zinc and other ions, especially from Fe(III) ion was studied for the determination of trace level of them in zinc ores and zinc blendes by inductively coupled plasma atomic emission spectrometry(ICP-AES). Gallium and indium were extracted from the sample solution with a solvent of tributyl phosphate(TBP). The type and concentration of acid, interferences of other ions, the ratio of aqueous phase to organic phase, TBP concentration, sripping efficiency were optimized for the effective extraction. Gallium and indium were separated from other ions in the 5N hydrochloric acid solution of the samples by the extraction with 100% TBP. In this time, Fe(III) was reduced to Fe(II) with hydroxylamine hydrochloride to prevent its coextraction prior to the main extraction. After stripped from organic phase by the back-extraction with 0.02N HCl, they were determined in the aqueous phase by ICP-AES. This method was known to be quantitative from the overall extraction of more than 95%. (Author)

  9. Detection of hepatitis C virus core protein in serum by atomic force microscopy combined with mass spectrometry.

    Science.gov (United States)

    Ivanov, Yuri D; Kaysheva, Anna L; Frantsuzov, Pavel A; Pleshakova, Tatyana O; Krohin, Nikolay V; Izotov, Alexander A; Shumov, Ivan D; Uchaikin, Vasiliy F; Konev, Vladimir A; Ziborov, Vadim S; Archakov, Alexander I

    2015-01-01

    A method for detection and identification of core antigen of hepatitis C virus (HCVcoreAg)-containing particles in the serum was proposed, with due account taken of the interactions of proteotypic peptides with Na(+), K(+), and Cl(-) ions. The method is based on a combination of reversible biospecific atomic force microscopy (AFM)-fishing and mass spectrometry (MS). AFM-fishing enables concentration, detection, and counting of protein complexes captured on the AFM chip surface, with their subsequent MS identification. Biospecific AFM-fishing of HCVcoreAg-containing particles from serum samples was carried out using AFM chips with immobilized antibodies against HCVcoreAg (HCVcoreAgim). Formation of complexes between anti-HCVcoreAgim and HCVcoreAg-containing particles on the AFM chip surface during the fishing process was demonstrated. These complexes were registered and counted by AFM. Further MS analysis allowed reliable identification of HCVcoreAg within the complexes formed on the AFM chip surface. It was shown that MS data processing, with account taken of the interactions between HCVcoreAg peptides and Na(+), K(+) cations, and Cl(-) anions, allows an increase in the number of peptides identified.

  10. Microplasma source based on a dielectric barrier discharge for the determination of mercury by atomic emission spectrometry.

    Science.gov (United States)

    Zhu, Zhenli; Chan, George C-Y; Ray, Steven J; Zhang, Xinrong; Hieftje, Gary M

    2008-11-15

    A low-power, atmospheric-pressure microplasma source based on a dielectric barrier discharge (DBD) has been developed for use in atomic emission spectrometry. The small plasma (0.6 mm x 1 mm x 10 mm) is generated within a glass cell by using electrodes that do not contact the plasma. Powered by an inexpensive ozone generator, the discharge ignites spontaneously, can be easily sustained in Ar or He at gas flow rates ranging from 5 to 200 mL min(-1), and requires less than 1 W of power. The effect of operating parameters such as plasma gas identity, plasma gas flow rate, and residual water vapor on the DBD source performance has been investigated. The plasma can be operated without removal of residual water vapor, permitting it to be directly coupled with cold vapor generation sample introduction. The spectral background of the source is quite clean in the range from 200 to 260 nm with low continuum and structured components. The DBD source has been applied to the determination of Hg by continuous-flow, cold vapor generation and offers detection limits from 14 (He-DBD) to 43 pg mL(-1) (Ar-DBD) without removal of the residual moisture. The use of flow injection with the He-DBD permits measurement of Hg with a 7.2 pg limit of detection, and with repetitive injections having an RSD of <2% for a 10 ng mL(-1) standard.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-10-17

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

  12. Ultrasensitive determination of mercury in human saliva by atomic fluorescence spectrometry based on solidified floating organic drop microextraction

    International Nuclear Information System (INIS)

    Yuan, C.-G.; Wang, J.; Jin, Y.

    2012-01-01

    We report on a new, rapid and simple method for the determination of ultra-trace quantities of mercury ion in human saliva. It is based on solidified floating organic drop microextraction and detection by cold vapor atomic fluorescence spectrometry (CV-AFS). Mercury ion was complexed with diethyldithiocarbamate, and the hydrophobic complex was then extracted into fine droplets of 1-undecanol. By cooling in an ice bath after extraction, the droplets in solution solidify to form a single ball floating on the surface of solution. The solidified micro drop containing the mercury complex was then transferred for determination by CV-AFS. The effects of pH value, concentration of chelating reagent, quantity of 1-undecanol, sample volume, equilibration temperature and time were investigated. Under the optimum conditions, the preconcentration of a 25-mL sample is accomplished with an enrichment factor of 182. The limit of detection is 2.5 ng L -1 . The relative standard deviation for seven replicate determinations at 0.1 ng mL -1 level is 4.1%. The method was applied to the determination of mercury in saliva samples collected from four volunteers. Two volunteers having dental amalgam fillings had 0.4 ng mL -1 mercury in their saliva, whereas mercury was not detectable in the saliva of two volunteers who had no dental fillings. (author)

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

    Directory of Open Access Journals (Sweden)

    Andrzej Nowakowski

    2015-05-01

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

  14. Coprecipitation with metal hydroxides for the determination of beryllium in seawater by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Hiraide, M.; Ishikawa, K.; Chen, Z.S.; Kawaguchi, H.

    1994-01-01

    Coprecipitation first with magnesium hydroxide. next with tin(IV) hydroxide is developed for the determination of traces of beryllium in seawater. To a 200-ml sample is added a sodium hydroxide solution to form magnesium hydroxide at pH 11.5, on which beryllium is quantitatively coprecipitated. The precipitate is separated by centrifugation and dissolved in 2 ml of 12 mol/l hydrochloric acid. The resulting solution (ca. 10 ml) is mixed with 2 mg of tin(IV) carrier and the pH is adjusted to 5.0 to collect the beryllium on tin(IV) hydroxide, leaving magnesium ions in the solution. The tin(IV) hydroxide is centrifuged, dissolved in 0.1 ml of 5 mol/l hydrobromic acid, and then diluted to 1 ml with water. Magnesium is so added as to be 500 μg/ml for increasing the sensitivity about four times, and the beryllium in the solution is determined by graphite furnace atomic absorption spectrometry. The experiments with synthetic seawater samples showed that pg-μg amounts of beryllium can be coprecipitated on the metal hydroxides and beryllium at the low ng/l level can be determined with reasonable precision (RSD < 10%). The detection limit of the proposed method is 0.5 ng/l of beryllium in seawater. (author)

  15. Determination of total and inorganic mercury in fish samples with on-line oxidation coupled to atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Shao Lijun; Gan Wuer; Su Qingde

    2006-01-01

    An atomic fluorescence spectrometry system for determination of total and inorganic mercury with electromagnetic induction-assisted heating on-line oxidation has been developed. Potassium peroxodisulphate was used as the oxidizing agent to decompose organomercury compounds. Depending on the temperature selected, inorganic or total mercury could be determined with the same manifold. Special accent was put on the study of the parameters influencing the on-line digestion efficiency. The tolerance to the interference of coexisting ions was carefully examined in this system. Under optimal conditions, the detection limits (3σ) were evaluated to be 2.9 ng l -1 for inorganic mercury and 2.6 ng l -1 for total mercury, respectively. The relative standard deviations for 10 replicate determinations of 1.0 μg l -1 Hg were 2.4 and 3.2% for inorganic mercury and total mercury, respectively. The proposed method was successfully applied to the determination of total and inorganic mercury in fish samples

  16. Antimony speciation analysis in sediment reference materials using high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Potin-Gautier, M.; Pannier, F.; Quiroz, W.; Pinochet, H.; Gregori, I. de

    2005-01-01

    This work presents the development of suitable methodologies for determination of the speciation of antimony in sediment reference samples. Liquid chromatography with a post-column photo-oxidation step and hydride generation atomic fluorescence spectrometry as detection system is applied to the separation and determination of Sb(III), Sb(V) and trimethylantimony species. Post-column decomposition and hydride generation steps were studied for sensitive detection with the AFS detector. This method was applied to investigate the conditions under which speciation analysis of antimony in sediment samples can be carried out. Stability studies of Sb species during the extraction processes of solid matrices, using different reagents solutions, were performed. Results demonstrate that for the extraction yield and the stability of Sb species in different marine sediment extracts, citric acid in ascorbic acid medium was the best extracting solution for antimony speciation analysis in this matrix (between 55% and 65% of total Sb was recovered from CRMs, Sb(III) being the predominant species). The developed method allows the separation of the three compounds within 6 min with detection limits of 30 ng g -1 for Sb(III) and TMSbCl2 and 40 ng g -1 for Sb(V) in sediment samples

  17. Antimony speciation analysis in sediment reference materials using high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Potin-Gautier, M. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Pannier, F. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France)]. E-mail: Florence.pannier@univ-pau.fr; Quiroz, W. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Pinochet, H. [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Gregori, I. de [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile)

    2005-11-30

    This work presents the development of suitable methodologies for determination of the speciation of antimony in sediment reference samples. Liquid chromatography with a post-column photo-oxidation step and hydride generation atomic fluorescence spectrometry as detection system is applied to the separation and determination of Sb(III), Sb(V) and trimethylantimony species. Post-column decomposition and hydride generation steps were studied for sensitive detection with the AFS detector. This method was applied to investigate the conditions under which speciation analysis of antimony in sediment samples can be carried out. Stability studies of Sb species during the extraction processes of solid matrices, using different reagents solutions, were performed.