WorldWideScience

Sample records for analytical atomic spectrometry

  1. 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)

  2. 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)…

  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. 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

  5. Atomic fluorescence spectrometry with the inductively coupled plasma

    International Nuclear Information System (INIS)

    Omenetto, N.; Winefordner, J.D.

    1987-01-01

    Atomic fluorescence spectrometry (AFS) is based on the radiational activation of atoms and ions produced in a suitable atomizer (ionizer) and the subsequent measurement of the resulting radiational deactivation, called fluorescence. Atomic fluorescence spectrometry has been of considerable interest to researchers in atomic spectrometry because of its use for both analytical and diagnostic purposes. Unfortunately, the analytical applications of AFS have suffered from the lack of commercial instrumentation until the recent marketing of the Baird multiple-element, hollow cathode lamp-excited inductively coupled plasma system. This chapter is concerned strictly with the use of the inductively coupled plasma (ICP) as a cell and as a source for AFS. Many of the major references concerning the ICP in analytical AFS are categorized in Table 9.1, along with several reviews and diagnostical studies. For more detailed discussions of the fundamental aspects of AFS, the reader is referred to previous reviews

  6. Toward improved understanding and control in analytical atomic spectrometry

    Science.gov (United States)

    Hieftje, Gary M.

    1989-01-01

    As with most papers which attempt to predict the future, this treatment will begin with a coverage of past events. It will be shown that progress in the field of analytical atomic spectrometry has occurred through a series of steps which involve the addition of new techniques and the occasional displacement of established ones. Because it is difficult or impossible to presage true breakthroughs, this manuscript will focus on how such existing methods can be modified or improved to greatest advantage. The thesis will be that rational improvement can be accomplished most effectively by understanding fundamentally the nature of an instrumental system, a measurement process, and a spectrometric technique. In turn, this enhanced understanding can lead to closer control, from which can spring improved performance. Areas where understanding is now lacking and where control is most greatly needed will be identified and a possible scheme for implementing control procedures will be outlined. As we draw toward the new millennium, these novel procedures seem particularly appealing; new high-speed computers, the availability of expert systems, and our enhanced understanding of atomic spectrometric events combine to make future prospects extremely bright.

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

    International Nuclear Information System (INIS)

    Krata, A.; Bulska, E.

    2005-01-01

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

  8. Trends in tungsten coil atomic spectrometry

    Science.gov (United States)

    Donati, George L.

    Renewed interest in electrothermal atomic spectrometric methods based on tungsten coil atomizers is a consequence of a world wide increasing demand for fast, inexpensive, sensitive, and portable analytical methods for trace analysis. In this work, tungsten coil atomic absorption spectrometry (WCAAS) and tungsten coil atomic emission spectrometry (WCAES) are used to determine several different metals and even a non-metal at low levels in different samples. Improvements in instrumentation and new strategies to reduce matrix effects and background signals are presented. Investigation of the main factors affecting both WCAAS and WCAES analytical signals points to the importance of a reducing, high temperature gas phase in the processes leading to atomic cloud generation. Some more refractory elements such as V and Ti were determined for the first time by double tungsten coil atomic emission spectrometry (DWCAES). The higher temperatures provided by two atomizers in DWCAES also allowed the detection of Ag, Cu and Sn emission signals for the first time. Simultaneous determination of several elements by WCAES in relatively complex sample matrices was possible after a simple acid extraction. The results show the potential of this method as an alternative to more traditional, expensive methods for fast, more effective analyses and applications in the field. The development of a new metallic atomization cell is also presented. Lower limits of detection in both WCAAS and WCAES determinations were obtained due to factors such as better control of background signal, smaller, more isothermal system, with atomic cloud concentration at the optical path for a longer period of time. Tungsten coil-based methods are especially well suited to applications requiring low sample volume, low cost, sensitivity and portability. Both WCAAS and WCAES have great commercial potential in fields as diverse as archeology and industrial quality control. They are simple, inexpensive, effective

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

    International Nuclear Information System (INIS)

    D'Ulivo, Alessandro; Dedina, Jiri

    2002-01-01

    The mechanism at the origin of double peaks formation in quartz hydride atomizers were investigated by continuous flow hydride generation atomic absorption spectrometry. Arsenic and selenium were used as model analytes. The effect of atomization mode (flame-in-gas-shield (FIGS), miniature diffusion flame and double flame (DF)) and some experimental parameters as oxygen supply rate for microflame and the distance from atomization to free atoms detection point, were investigated on the shape of both analytical signals and calibration graphs. Rollover of calibration graphs and double peak formation are strictly related each to the other and could be observed only in FIGS atomizer mode under some particular conditions. A mechanism based on incomplete atomization of hydrides cannot explain the collected experimental evidences because the microflame of FIGS is able to produce quantitative atomization of large amount of hydrides even at supply rate of oxygen close to extinction threshold of microflame. The heterogeneous gas-solid reactions between finely dispersed particles, formed by free atom recombination, and the free atoms in the gaseous phase are at the origin of double peak formation

  10. Inductively coupled plasma as atomization, excitation and ionization sources in analytical atomic spectrometry

    International Nuclear Information System (INIS)

    Kawaguchi, Hiroshi

    1996-01-01

    Studies on inductively coupled plasma (ICP) for atomic emission and mass spectrometry accomplished in our laboratory since 1978 are reviewed. In emission spectrometry, the characteristics of the plasma are studied concerning the spatial profiles of spectral line intensity, axial profiles of gas and excitation temperatures, spectral line widths and matrix effect. The studies are particularly emphasized on the instrumentation such as developments of plasma generator, emission spectrometers, water-cooled torches and sample introduction methods. A slew-scan type spectrometer developed in these works represents a predecessor of the current commercial spectrometers. An ICP mass spectrometer was first developed in Japan in this laboratory in 1984. Non-spectroscopic interference of this method was found to have the correlation with the atomic weight of the matrix element. Plasma gases other than argon such as nitrogen and oxygen were used for the ICP to evaluate their performance in mass spectrometry as for the sensitivity and interferences. (author). 63 refs

  11. 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

  12. 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

  13. 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, ...

  14. 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

  15. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-06-15

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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/cm 3 (10 fg/m 3 or 10 −5 ng/m 3 ), which corresponds to 25 atoms/cm 3 , and Na down to 0.5 zg (zg = zeptogram = 10 −21 g), representing 50 zg/mL (parts-per-sextillion, pps, 1:10 21 ) 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

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

    International Nuclear Information System (INIS)

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2015-01-01

    A detailed optimization of relevant experimental parameters of two hydride atomizers for atomic fluorescence spectrometry: flame-in-gas-shield atomizer with a two-channel shielding unit and a standard atomizer for atomic fluorescence spectrometry, miniature diffusion flame, was performed. Arsine, generated by the reaction with NaBH 4 in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were compared. Under optimum conditions sensitivity obtained with flame-in-gas-shield atomizer was approximately twice higher than with miniature diffusion flame. The additional advantage of flame-in-gas-shield atomizer is significantly lower flame emission resulting in a better signal to noise ratio. The resulting arsenic limits of detection for miniature diffusion flame and flame-in-gas-shield atomizer were 3.8 ng l −1 and 1.0 ng l −1 , respectively. - Highlights: • We optimized and compared two hydride atomizers for atomic fluorescence spectrometry. • Miniature diffusion flame and flame-in-gas-shield atomizer were optimized. • The limit of detection for arsenic was 1.0 ng l −1

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

    Energy Technology Data Exchange (ETDEWEB)

    Marschner, Karel, E-mail: karel.marschner@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Charles University in Prague, Faculty of Science, Department of Analytical Chemistry, Albertov 8, 128 43 Prague (Czech Republic); Musil, Stanislav; Dědina, Jiří [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2015-07-01

    A detailed optimization of relevant experimental parameters of two hydride atomizers for atomic fluorescence spectrometry: flame-in-gas-shield atomizer with a two-channel shielding unit and a standard atomizer for atomic fluorescence spectrometry, miniature diffusion flame, was performed. Arsine, generated by the reaction with NaBH{sub 4} in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were compared. Under optimum conditions sensitivity obtained with flame-in-gas-shield atomizer was approximately twice higher than with miniature diffusion flame. The additional advantage of flame-in-gas-shield atomizer is significantly lower flame emission resulting in a better signal to noise ratio. The resulting arsenic limits of detection for miniature diffusion flame and flame-in-gas-shield atomizer were 3.8 ng l{sup −1} and 1.0 ng l{sup −1}, respectively. - Highlights: • We optimized and compared two hydride atomizers for atomic fluorescence spectrometry. • Miniature diffusion flame and flame-in-gas-shield atomizer were optimized. • The limit of detection for arsenic was 1.0 ng l{sup −1}.

  20. Recent trends in atomic spectrometry with microwave-induced plasmas

    International Nuclear Information System (INIS)

    Broekaert, Jose A.C.; Siemens, Volker

    2004-01-01

    The state-of-the-art and trends of development in atomic spectrometry with microwave-induced plasmas (MIPs) since the 1998s are presented and discussed. This includes developments in devices for producing microwave plasma discharges, with reference also to miniaturized systems as well as to progress in sample introduction for microwave-induced plasmas, such as pneumatic and ultrasonic nebulization using membrane desolvation, to the further development of gaseous analyte species generation systems and to both spark and laser ablation (LA). The features of microwave-induced plasma mass spectrometry (MIP-MS) as an alternative to inductively coupled plasma (ICP)-MS are discussed. Recent work on the use of microwave-induced plasma atomic spectrometry for trace element determinations and monitoring, their use as tandem sources and for particle sizing are discussed. Recent applications of the coupling of gas chromatography and MIP atomic spectrometry for the determination of organometallic compounds of heavy metals such as Pb, Hg, Se and Sn are reviewed and the possibilities of trapping for sensitivity enhancement, as required for many applications especially in environmental work, are showed at the hand of citations from the recent literature

  1. 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

  2. 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.

  3. 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

  4. A low-cost vaporization-atomization system for atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Bruhn F, C.G.; Ambiado V, F.; Woerner V, R.

    1990-01-01

    A low-cost vaporization-atomization system for atomic absorption spectrometry is developed as an alternative to the use of a graphite furnace in electrothermal atomic absorption spectrometry. (Author)

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

    Czech Academy of Sciences Publication Activity Database

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

    2006-01-01

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

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

    International Nuclear Information System (INIS)

    Ataman, O. Yavuz

    2008-01-01

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

  7. 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.

  8. 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.

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

    Science.gov (United States)

    Kowalewska, Zofia; Ruszczyńska, Anna; Bulska, Ewa

    2005-03-01

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

  10. 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

  11. 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

  12. 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

  13. 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.

  14. Inductively coupled plasma-atomic emission spectrometry: analytical assessment of the technique at the beginning of the 90's

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1991-01-01

    The main application of the inductively coupled plasma (ICP) today is in atomic emission spectroscopy (AES), as an excitation spectrochemical source, although uses of an ICP for fluorescence as just an atomizer, and specially for mass spectrometry, as an ionization source, are rocketing in the last few years. Since its inception, only a quarter of a century ago, ICP-AES has rapidly evolved to one of the preferred routine analytical techniques for convenient determination of many elements with high speed, at low levels and in the most varied samples. Perhaps its comparatively high kinetic temperature (capable of atomizing virtually every compound of any sample), its high excitation and ionization temperatures, and its favourable spatial structure at the core of the ICP success. By now, the ICP-AES can be considered as having achieved maturity in that a huge amount of analytical problems can be tackled with this technique, while no major or fundamental changes have been adopted for several years. Despite this fact, important driving forces are still in operation to further improve the ICP-AES sensitivity, selectivity, precision, sample throughput, etc. Moreover, proposals to extend the scope of the technique to traditionally elusive fields (e.g. non-metals and organic compound analysis) are also appearing in the recent literature. In this paper the 'state of the art', the last developments and the expectations in trying to circumvent the limitations of the ICP-AES (on the light of literature data and personal experience) are reviewed. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-08-15

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

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

    Science.gov (United States)

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

    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. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Analytical mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    1990-01-01

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

  18. 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

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

    International Nuclear Information System (INIS)

    Kowalewska, Zofia; Ruszczynska, Anna; Bulska, Ewa

    2005-01-01

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

  20. SOME SPECIATION STUDIES IN FOODSTUFF BY ATOMIC ABSORPTION SPECTROMETRY

    OpenAIRE

    Gücer, S

    2000-01-01

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

  1. 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.

  2. Some analytical aspects of the Moessbauer spectrometry

    International Nuclear Information System (INIS)

    Meisel, W.

    1975-01-01

    Analytical applications of Moessbauer spectrometry are reviewed. Various methods of analysis (qualitative, semiquantitative and quantitative) using the Moessbauer effect are dealt with. Sensitivity and accuracy of Moessbauer spectrometry in analytical applications are discussed. (Z.S.)

  3. Mechanism of selenium hydride atomization, fate of free atoms and temperature distribution in an argon shielded, highly fuel-rich, hydrogen-oxygen diffusion micro-flame studied by atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    D'Ulivo, A.; Dědina, Jiří; Lampugnani, L.; Matoušek, Tomáš

    2002-01-01

    Roč. 17, č. 3 (2002), s. 253-257 ISSN 0267-9477 R&D Projects: GA ČR GA203/01/0453; GA ČR GA203/98/0754 Institutional research plan: CEZ:AV0Z4031919 Keywords : hydride atomization * hydride generation * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.250, year: 2002

  4. Analytical mass spectrometry. Abstracts

    Energy Technology Data Exchange (ETDEWEB)

    1990-12-31

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

  5. 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)

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

    Science.gov (United States)

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

    2016-02-01

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

  7. Atomization mechanisms for barium in furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Styris, D.L.

    1984-01-01

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

  8. 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.

  9. Atomic electron spectrometry with synchrotron radiation

    International Nuclear Information System (INIS)

    Sorensen, S.L.

    1989-01-01

    Techniques of atomic electron spectrometry were applied to atoms in the gaseous and solid states to derive information about fundamental atomic properties. A new method was developed to measure Coster-Kronig yields in metals by photoionization with synchrotron radiation. Photon-energy sensitive Si L-VV Auger satellites were investigated via electron spectrometry. The krypton 1s photoionization spectrum was measured in an experiment which was motivated by the need to understand the krypton 1s satellite spectrum for calibration of an experiment to measure the mass of the electron antineutrino

  10. 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

  11. Modular L-design of hydride atomizers for atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Rezacova, Olga; Dedina, Jiri

    2009-01-01

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

  12. 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.

  13. Modular L-design of hydride atomizers for atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-15

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

  14. 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 ...

  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. 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.

  17. 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

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

    African Journals Online (AJOL)

    spectrometry as alternative method for trace analysis of ... Purpose: To evaluate the comparative efficiency of graphite furnace atomic absorption spectrometry .... Methods comparison and validation .... plasma-optical emission spectrometry.

  19. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-11-15

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  2. 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)

  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. 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

  5. Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  6. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-02-28

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

  8. 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

  9. 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.

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

    Science.gov (United States)

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

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-01-01

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

  12. 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.

  13. 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

  14. Multiple microflame quartz tube atomizer: Study and minimization of interferences in quartz tube atomizers in hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Moraes Flores, Erico Marlon de [Departamento de Quimica, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS (Brazil)], E-mail: flores@quimica.ufsm.br; Medeiros Nunes, Adriane; Luiz Dressler, Valderi [Departamento de Quimica, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS (Brazil); Dedina, Jiri [Institute of Analytical Chemistry of the ASCR, v.v.i., Videnska 1083, CZ-142 20 Prague (Czech Republic)

    2009-02-15

    A systematic study was performed to evaluate the performance of a multiple microflame (MM) quartz tube atomizer (QTA) for minimizing interferences and to improve the extent of the calibration range using a batch system for hydride generation atomic absorption spectrometry (HG AAS). A comparison of the results with conventional QTA on the determination of antimony, arsenic, bismuth and selenium was performed. The interference of As, Bi, Se, Pb, Sn and Sb was investigated using QTA and MMQTA atomizers. Better performance was found for MMQTA, and no loss of linearity was observed up to 160 ng for Se and Sb and 80 ng for As, corresponding to an enhancement of two times for both analytes when compared to QTA (analyte mass refers to a volume of 200 {mu}l). For Bi, the linear range was the same for QTA and MMQTA (140 ng). With the exception of Bi, the tolerance limits for hydride-forming elements were improved more than 50% in comparison to the conventional QTA system, especially for the interferences of As, Sb and Se. However, for Sn as an interferent, no difference was observed in the determination of Se and Sb using the MMQTA system. The use of MMQTA-HG AAS complied with the relatively high sensitivity of conventional QTA and also provided better performance for interferences and the linear range of calibration.

  15. 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.

  16. Fast Atom Bombardment Spectrometry - a novel analytical method for biologically interesting, non-volatile substances

    International Nuclear Information System (INIS)

    Schmid, E.

    1987-03-01

    Today important chemical substances like proteins can be produced easily and in large amounts. The primary structure of proteins can be analysed automatically, however the procedure can take some months of time. A novel method, fast atom bombardment mass spectrometry (FAB-MS) in combination with enzymatic degradation not only decreases the analysis time, but gives also additional information about the primary structure. Especially for the verification of protein structures - which is important for recombinant proteins - FAB-MS is a very useful method. 40 refs., 56 figs. (P.W.)

  17. 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.

  18. Determination of trace heavy metals in soil and sediments by atomic spectrometry following preconcentration with Schiff bases on Amberlite XAD-4

    Energy Technology Data Exchange (ETDEWEB)

    Kara, Derya, E-mail: dkara@balikesir.edu.tr [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100 Balikesir (Turkey); Fisher, Andrew; Hill, Steve J. [School of Earth, Ocean and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth, Devon PL4 8AA (United Kingdom)

    2009-06-15

    A matrix separation and analyte preconcentration system using Amberlite XAD copolymer resins functionalized by Schiff base reactions coupled with atomic spectrometry has been developed. Three different functionalized Amberlite XAD resins were synthesized using 4-phenylthiosemicarbazide, 2,3-dihydroxybenzaldehyde and 2-thiophenecarboxaldehyde as reagents. These resins could be used to preconcentrate transition and other trace heavy metal analytes from nitric acid digests of soil and sediment samples. Analyte retention was shown to work well at pH 6.0. After treatment of the digests with sodium fluoride and buffering to pH 6, samples that contain extremely large concentrations of iron were analysed for trace analytes without the excess iron overloading the capacity of the resin. The analytes Cd, Co, Cu, Ni and Pb were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with 0.1 M HNO{sub 3} directly to the detection system. Flame atomic absorption spectrometry was used as a means of detection during the studies. The efficiency of the chelating resin and the accuracy of the proposed method were evaluated by the analysis of soil (SO-2) and sediment (LGC 6157 and MESS-3) certified reference materials.

  19. Sampling and analyte enrichment strategies for ambient mass spectrometry.

    Science.gov (United States)

    Li, Xianjiang; Ma, Wen; Li, Hongmei; Ai, Wanpeng; Bai, Yu; Liu, Huwei

    2018-01-01

    Ambient mass spectrometry provides great convenience for fast screening, and has showed promising potential in analytical chemistry. However, its relatively low sensitivity seriously restricts its practical utility in trace compound analysis. In this review, we summarize the sampling and analyte enrichment strategies coupled with nine modes of representative ambient mass spectrometry (desorption electrospray ionization, paper vhspray ionization, wooden-tip spray ionization, probe electrospray ionization, coated blade spray ionization, direct analysis in real time, desorption corona beam ionization, dielectric barrier discharge ionization, and atmospheric-pressure solids analysis probe) that have dramatically increased the detection sensitivity. We believe that these advances will promote routine use of ambient mass spectrometry. Graphical abstract Scheme of sampling stretagies for ambient mass spectrometry.

  20. 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.

  1. 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...

  2. 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.

  3. Atom counting with accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Kutschera, Walter

    1995-01-01

    A brief review of the current status and some recent applications of accelerator mass spectrometry (AMS) are presented. Some connections to resonance ionization mass spectroscopy (RIS) as the alternate atom counting method are discussed

  4. 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)

  5. 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)

  6. 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.

  7. 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

  8. 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.

  9. 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

    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...

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

    International Nuclear Information System (INIS)

    Sardans, Jordi; Montes, Fernando; Penuelas, Josep

    2010-01-01

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

  11. 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

  12. 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

  13. 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

  14. 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.

  15. Ultratrace determination of tin by hydride generation in-atomizer trapping atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Průša, Libor [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Charles University in Prague, Faculty of Science, Department of Analytical Chemistry, Hlavova 8, Prague 2, CZ 128 43 Czech Republic (Czech Republic); Dědina, Jiří [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2013-12-04

    Graphical abstract: -- Highlights: •In-atomizer trapping HG-AAS was optimized for Sn. •A compact quartz trap-and-atomizer device was employed. •Generation, preconcentration and atomization steps were investigated in detail. •Hundred percent preconcentration efficiency for tin was reached. •Routine analytical method was developed for Sn determination (LOD of 0.03 ng mL{sup −1} Sn). -- Abstract: A quartz multiatomizer with its inlet arm modified to serve as a trap (trap-and-atomizer device) was employed to trap tin hydride and subsequently to volatilize collected analyte species with atomic absorption spectrometric detection. Generation, atomization and preconcentration conditions were optimized and analytical figures of merit of both on-line atomization as well as preconcentration modes were quantified. Preconcentration efficiency of 95 ± 5% was found. The detection limits reached were 0.029 and 0.14 ng mL{sup −1} Sn, respectively, for 120 s preconcentration period and on-line atomization mode without any preconcentration. The interference extent of other hydride forming elements (As, Se, Sb and Bi) on tin determination was found negligible in both modes of operation. The applicability of the developed preconcentration method was verified by Sn determination in a certified reference material as well as by analysis of real samples.

  16. 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.

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

    International Nuclear Information System (INIS)

    Dedina, Jiri

    2007-01-01

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

  18. 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

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

    OpenAIRE

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

    2005-01-01

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

  20. 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)

  1. 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.

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

    International Nuclear Information System (INIS)

    Kantor, Tibor

    2008-01-01

    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. Atomic and nuclear analytical methods. XRF, Moessbauer, XPS, NAA and ion-beam spectroscopic techniques

    International Nuclear Information System (INIS)

    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), Moessbauer 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. (orig.)

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

    Science.gov (United States)

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

    2015-06-01

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

  5. Analytic of elements for the determination of soil->plant transfer factors

    International Nuclear Information System (INIS)

    Liese, T.

    1985-02-01

    This article describes a part of the conventional analytical work, which was done to determine soil to plant transfer factors. The analytical methods, the experiments to find out the best way of sample digestion and the resulting analytical procedures are described. Analytical methods are graphite furnace atomic absorption spectrometry (GFAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). In case of ICP-AES the necessity of right background correction and correction of the spectral interferences is shown. The reliability of the analytical procedure is demonstrated by measuring different kinds of standard reference materials and by comparison of AAS and AES. (orig./HP) [de

  6. 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…

  7. 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 ...

  8. 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.

  9. Analytical capabilities of laser-probe mass spectrometry

    International Nuclear Information System (INIS)

    Kovalev, I.D.; Madsimov, G.A.; Suchkov, A.I.; Larin, N.V.

    1978-01-01

    The physical bases and quantitative analytical procedures of laser-probe mass spectrometry are considered in this review. A comparison is made of the capabilities of static and dynamic mass spectrometers. Techniques are studied for improving the analytical characteristics of laser-probe mass spectrometers. The advantages, for quantitative analysis, of the Q-switched mode over the normal pulse mode for lasers are: (a) the possibility of analysing metals, semiconductors and insulators without the use of standards; and (b) the possibility of layer-by-layer and local analysis. (Auth.)

  10. 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.

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

    International Nuclear Information System (INIS)

    Ho, Koon-Sing; Lui, Kwok-On; Lee, Kin-Ho; Chan, Wing-Tat

    2013-01-01

    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

  12. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-11-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  15. 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

  16. 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.

  17. Ambient-temperature trap/release of arsenic by dielectric barrier discharge and its application to ultratrace arsenic determination in surface water followed by atomic fluorescence spectrometry

    Science.gov (United States)

    A novel dielectric barrier discharge reactor (DBDR) was utilized to trap/release arsenic coupled to hydride generation atomic fluorescence spectrometry (HGAFS). On the DBD principle, the precise and accurate control of trap/release procedures was fulfilled at ambient temperature, and an analytical m...

  18. 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

  19. Analytic approaches to atomic response properties

    International Nuclear Information System (INIS)

    Lamm, E.E.

    1980-01-01

    Many important response properties, e.g., multipole polarizabilites and sum rules, photodetachment cross sections, and closely-related long-range dispersion force coefficients, are insensitive to details of electronic structure. In this investigation, analytic asymptotic theories of atomic response properties are constructed that yield results as accurate as those obtained by more elaborate numerical methods. In the first chapter, a novel and simple method is used to determined the multipole sum rules S/sub l/(-k), for positive and negative values of k, of the hydrogen atom and the hydrogen negative ion in the asymptotic approximation. In the second chapter, an analytically-tractable extended asymptotic model for the response properites of weakly-bound anions is proposed and the multipole polarizability, multipole sum rules, and photodetachment cross section determined by the model are computed analytically. Dipole polarizabilities and photodetachment cross sections determined from the model for Li-, Na-, and K- are compared with the numercal results of Moores and Norcross. Agreement is typically within 15% if the pseudopotential is included. In the third chapter a comprehensive and unified treatment of atomic multipole oscillator strengths, dynamic multipole polarizabilites, and dispersion force constants in a variety of Coulomb-like approximations is presented. A theoretically and computationally superior modification of the original Bates-Damgaard (BD) procedure, referred to here as simply the Coulomb approximation (CA), is introduced. An analytic expression for the dynamic multipole polarizability is found which contains as special cases this quantity within the CA, the extended Coulomb approximation (ECA) of Adelman and Szabo, and the quantum defect orbital (QDO) method of Simons

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-01-30

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

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

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium pyrrolidinedithioc......An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium....../preconcentration process of the ensuing sample. An enrichment factor of 21.4, a detection limit of 2.7 ng/l, along with a sampling frequency of 13s/h were obtained at a sample flow rate of 6.0mlmin/sup -1/. The precision (R.S.D.) at the 0.4 mug/l level was 1.8% as compared to 3.2% when quantifying the organic extractant...

  2. 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

  3. Radio-frequency glow discharge spectrometry: A critical review

    International Nuclear Information System (INIS)

    Winchester, Michael R.; Payling, Richard

    2004-01-01

    This paper presents a critical review of analytical radio frequency glow discharge spectrometry (rf-GDS). The historical foundations of rf-GDS are described, and current knowledge of the fundamental physics of analytical rf glow discharges is discussed. Additionally, instrumentation, methodologies, and applications of rf glow discharge optical emission spectrometry (rf-GDOES) and mass spectrometry (rf-GDMS) are reviewed. Although other rf-GDS techniques have appeared [e.g. rf glow discharge atomic absorption spectrophotometry (rf-GDAAS)], the emphasis is placed upon rf-GDOES and rf-GDMS, because they have received by far the most interest from analytical chemical metrologists. This review also provides explanations of some developments that are needed for further progress in the field of analytical rf-GDS

  4. On the possibilities of high-resolution continuum source graphite furnace atomic absorption spectrometry for the simultaneous or sequential monitoring of multiple atomic lines

    International Nuclear Information System (INIS)

    Resano, M.; Rello, L.; Florez, M.; Belarra, M.A.

    2011-01-01

    This paper explores the potential of commercially available high-resolution continuum source graphite furnace atomic absorption spectrometry instrumentation for the simultaneous or sequential monitoring of various atomic lines, in an attempt to highlight the analytical advantages that can be derived from this strategy. In particular, it is demonstrated how i) the monitoring of multiplets may allow for the simple expansion of the linear range, as shown for the measurement of Ni using the triplet located in the vicinity of 234.6 nm; ii) the use of a suitable internal standard may permit improving the precision and help in correcting for matrix-effects, as proved for the monitoring of Ni in different biological samples; iii) direct and multi-element analysis of solid samples may be feasible on some occasions, either by monitoring various atomic lines that are sufficiently close (truly simultaneous monitoring, as demonstrated in the determination of Co, Fe and Ni in NIST 1566a Oyster tissue) or, alternatively, by opting for a selective and sequential atomization of the elements of interest during every single replicate. Determination of Cd and Ni in BCR 679 White cabbage is attempted using both approaches, which permits confirming that both methods can offer very similar and satisfactory results. However, it is important to stress that the second approach provides more flexibility, since analysis is no longer limited to those elements that show very close atomic lines (closer than 0.3 nm in the ultraviolet region) with a sensitivity ratio similar to the concentration ratio of the analytes in the samples investigated.

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

    Science.gov (United States)

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

    2000-12-01

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

  6. 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

  7. 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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  9. 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

  10. 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)

  11. 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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-15

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

  14. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-01

    The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D{sub 2} and Xe lamps within 200–400 nm wavelengths range with a low resolution spectral instrument and linear charge-coupled device. The setup permits the acquisition of 200 spectra during 1 s atomization pulse. Respective data matrix absorbance vs wavelength/time is employed for the quantification of elements in the sample. The calculation algorithm developed includes broad band and continuum background correction, linearization of function absorbance vs. concentration of atomic vapor and integration of thus modified absorbance at the resonance lines of the elements to be determined. Practical application shows that the method can be employed for the direct simultaneous determination of about 20 elements above microgram per liter level within 3–5 orders of the magnitude concentration range. The investigated sources of measurement errors are mainly associated with the atomization and vapor transportation problems, which are aggravated for the simultaneous release of major and minor sample constituents. Respective corrections concerning the selection of analytical lines, optimal sampling volume, matrix modification and cleaning of the atomizer have been introduced in the SMET AAS analytical technology. Under the optimized experimental conditions the calibration curves in Log-Log coordinates for all the investigated analytes in the single or multi-element reference solutions are approximated by the first order equations. The use of these equations as permanent characteristics of the setup enables instant quantification of Al, Ca, Co, Cr, Cu, Fe, Mg, Mn and Ni in the underground

  16. 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...

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  18. 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)

  19. Atmospheric-pressure solution-cathode glow discharge: A versatile ion source for atomic and molecular mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Schwartz, Andrew J. [Department of Chemistry, Indiana University, Bloomington, IN, 47405 (United States); Williams, Kelsey L. [Department of Chemistry and Biochemistry, Kent State University, Kent, OH, 44242 (United States); Hieftje, Gary M. [Department of Chemistry, Indiana University, Bloomington, IN, 47405 (United States); Shelley, Jacob T., E-mail: shellj@rpi.edu [Department of Chemistry and Biochemistry, Kent State University, Kent, OH, 44242 (United States); Department of Chemistry and Chemical Biology, Rensselaer Polytechnic Institute, Troy, NY, 12180 (United States)

    2017-01-15

    An atmospheric-pressure solution-cathode glow discharge (SCGD) has been evaluated as an ion source for atomic, molecular, and ambient desorption/ionization mass spectrometry. The SCGD consists of a direct-current plasma, supported in the ambient air in the absence of gas flows, and sustained upon the surface of a flowing liquid cathode. Analytes introduced in the flowing liquid, as an ambient gas, or as a solid held near the plasma are vaporized and ionized by interactions within or near the discharge. Introduction of acidic solutions containing metal salts produced bare elemental ions as well as H{sub 2}O, OH{sup −} and NO{sub 3}{sup −} adducts. Detection limits for these elemental species ranged from 0.1 to 4 ppb, working curves spanned more than 4 orders of linear dynamic range, and precision varied between 5 and 16% relative standard deviation. Small organic molecules were also efficiently ionized from solution, and both the intact molecular ion and fragments were observed in the resulting SCGD mass spectra. Fragmentation of molecular species was found to be tunable; high discharge currents led to harder ionization, while low discharge currents produced stronger molecular-ion signals. Ambient gases and solids, desorbed by the plasma from a glass probe, were also readily ionized by the SCGD. Indeed, strong analyte signals were obtained from solid samples placed at least 2 cm from the plasma. These findings indicate that the SCGD might be useful also for ambient desorption/ionization mass spectrometry. Combined with earlier results that showed the SCGD is useful for ionization of labile biomolecules, the results here indicate that the SCGD is a highly versatile ion source capable of providing both elemental and molecular mass-spectral information. - Highlights: • Solution-cathode glow discharge used as an ionization source for mass spectrometry. • SCGD-MS can provide atomic as well as intact molecular mass spectra. • Atomic limits of detection range

  20. [Atomic/ionic fluorescence in microwave plasma torch discharge with excitation of high current and microsecond pulsed hollow cathode lamp: Ca atomic/ionic fluorescence spectrometry].

    Science.gov (United States)

    Gong, Zhen-bin; Liang, Feng; Yang, Peng-yuan; Jin, Qin-han; Huang, Ben-li

    2002-02-01

    A system of atomic and ionic fluorescence spectrometry in microwave plasma torch (MPT) discharge excited by high current microsecond pulsed hollow cathode lamp (HCMP HCL) has been developed. The operation conditions for Ca atomic and ionic fluorescence spectrometry have been optimized. Compared with atomic fluorescence spectrometry (AFS) in argon microwave induced plasma (MIP) and MPT with the excitation of direct current and conventional pulsed HCL, the system with HCMP HCL excitation can improve AFS and ionic fluorescence spectrometry (IFS) detection limits in MPT atomizer and ionizer. Detection limits (3 sigma) with HCMP HCL-MPT-AFS/IFS are 10.1 ng.mL-1 for Ca I 422.7 nm, 14.6 ng.mL-1 for Ca II 393.4 nm, and 37.4 ng.mL-1 for Ca II 396.8 nm, respectively.

  1. 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.

  2. Simultaneous determination of arsenic and antimony by hydride generation atomic fluorescence spectrometry with dielectric barrier discharge atomizer

    Energy Technology Data Exchange (ETDEWEB)

    Xing Zhi [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Kuermaiti, Biekesailike [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Products Quality Inspection Institute, Yili, Xinjiang 835000 (China); Wang Juan; Han Guojun; Zhang Sichun [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Zhang Xinrong, E-mail: xrzhang@mail.tsinghua.edu.cn [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China)

    2010-12-15

    Simultaneous determination of As and Sb by hydride generation atomic fluorescence spectrometry was developed with the dielectric barrier discharge plasma as the hydride atomizer. The low-temperature and atmospheric-pressure micro-plasma was generated in a quartz cylindrical configuration device, which was constructed by an axial internal electrode and an outer electrode surrounding outside of the tube. The optimization of the atomizer construction and parameters for hydride generation and fluorescence detection systems were carried out. Under the optimized conditions, the detection limits for As and Sb were 0.04 and 0.05 {mu}g L{sup -1}, respectively. In addition, the applicability of the present method was confirmed by the detection of As and Sb in reference materials of quartz sandstone (GBW07106) and argillaceous limestone (GBW07108). The present work provided a new approach to exploit the miniaturized hydride generation dielectric barrier discharge atomic fluorescence spectrometry system for simultaneous multi-element determination.

  3. Simultaneous determination of arsenic and antimony by hydride generation atomic fluorescence spectrometry with dielectric barrier discharge atomizer

    International Nuclear Information System (INIS)

    Xing Zhi; Kuermaiti, Biekesailike; Wang Juan; Han Guojun; Zhang Sichun; Zhang Xinrong

    2010-01-01

    Simultaneous determination of As and Sb by hydride generation atomic fluorescence spectrometry was developed with the dielectric barrier discharge plasma as the hydride atomizer. The low-temperature and atmospheric-pressure micro-plasma was generated in a quartz cylindrical configuration device, which was constructed by an axial internal electrode and an outer electrode surrounding outside of the tube. The optimization of the atomizer construction and parameters for hydride generation and fluorescence detection systems were carried out. Under the optimized conditions, the detection limits for As and Sb were 0.04 and 0.05 μg L -1 , respectively. In addition, the applicability of the present method was confirmed by the detection of As and Sb in reference materials of quartz sandstone (GBW07106) and argillaceous limestone (GBW07108). The present work provided a new approach to exploit the miniaturized hydride generation dielectric barrier discharge atomic fluorescence spectrometry system for simultaneous multi-element determination.

  4. 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)

  5. 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

  6. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz

    2012-05-15

    A compact trap-and-atomizer device and a preconcentration procedure based on hydride trapping in excess of oxygen over hydrogen in the collection step, both constructed and developed previously in our laboratory, were employed to optimize plumbane trapping in this device and to develop a routine method for ultratrace lead determination subsequently. The inherent advantage of this preconcentration approach is that 100% preconcentration efficiency for lead is reached in this device which has never been reported before using quartz or metal traps. Plumbane is completely retained in the trap-and-atomizer device at 290 Degree-Sign C in oxygen-rich atmosphere and trapped species are subsequently volatilized at 830 Degree-Sign C in hydrogen-rich atmosphere. Effect of relevant experimental parameters on plumbane trapping and lead volatilization are discussed, and possible trapping mechanisms are hypothesized. Plumbane trapping in the trap-and-atomizer device can be routinely used for lead determination at ultratrace levels reaching a detection limit of 0.21 ng ml{sup -1} Pb (30 s preconcentration, sample volume 2 ml). Further improvement of the detection limit is feasible by reducing the blank signal and increasing the trapping time. - Highlights: Black-Right-Pointing-Pointer In-atomizer trapping HG-AAS was optimized for Pb. Black-Right-Pointing-Pointer A compact quartz trap-and-atomizer device was employed. Black-Right-Pointing-Pointer Generation, preconcentration and atomization steps were investigated in detail. Black-Right-Pointing-Pointer 100% preconcentration efficiency for lead was reached. Black-Right-Pointing-Pointer Routine analytical method was developed for Pb determination (LOD of 0.2 ng ml{sup -1} Pb).

  8. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Dancsak, Stacia E. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Silva, Sidnei G.; Nóbrega, Joaquim A. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, São Carlos, SP (Brazil); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Donati, George L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)

    2014-01-02

    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{sup −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{sup −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{sup −1} for Na and K, and between 0.22 and 0.43 mg kg{sup −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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  11. 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

  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. 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

  14. Inductively coupled plasma--atomic emission spectrometry: trace elements in oil matrices

    Energy Technology Data Exchange (ETDEWEB)

    Peterson, Charlie Albert [Iowa State Univ., Ames, IA (United States)

    1977-12-01

    The simultaneous determination of up to 20 trace elements in various oil matrices by inductively coupled plasma-atomic emission spectrometry is reported. The oil matrices investigated were lubricating oils (for wear metals), fuel oil, centrifuged coal liquefaction product, crude soybean oil, and commercial edible oils. The samples were diluted with appropriate organic solvents and injected into the plasma as an aerosol generated by a pneumatic nebulization technique. Detection limits of the 28 elements studied ranged from 0.0006 to 9 μg/g with the majority falling in the 0.01 to 0.1 μg/g range. Analytical calibration curves were linear over at least two orders of magnitude and for some elements this linearity extended over 4.5 orders of magnitude. Relevant data on precision and accuracy are included. Because metals often occur as particles in lubricating oil and coal liquefaction products, the effect of particles on the analytical results was examined. Wear metal particles in used oil did not appear to affect the analytical results. However, incomplete recovery relative to organometallic reference solutions was obtained for iron particles with a nominal mean diameter of 3.0 μm suspended in oil. It was shown that the following factors contributed to incomplete recovery for the particles: settling of the suspended particles in the flask, a difference in nebulization efficiency between particle suspensions and organometallic solutions, and indications of incomplete vaporization of the larger particles in the plasma.

  15. Graphite furnace atomic absorption spectrometry with a tantalum boat for the determination of yttrium, samarium, and dysprosium in a mish metal

    International Nuclear Information System (INIS)

    Daidoji, Hidehiro; Tamura, Shohei

    1982-01-01

    The determination of yttrium, samarium, and dysprodium by means of graphite-furnace atomic absorption spectrometry (AAS) was studied by a tantalum boat inserted into a graphite tube atomizer. These elements could not be determined by the use of a commercial graphite tube, In the atomization from a tantalum boat, better analytical sensitivities and negligible memory effects for these rare earths are obtained. The analytical sensitivities of yttrium, samarium, and dysprodium with the tantalum boat were 0.60 ng, 0.86 ng, and 0.17 ng respectively. This method was applied for the determination of yttrium, samarium, and dysprosium in a mish metal. The measurements were performed with slightly acidified solutions (0.01 mol dm 3 HCI or HNO 3 ). The sensitivities and the precisions for these elements decreased with increasing acid concentration. An enhancement in the sensitivities of yttrium and dysprosium upon the addition of a large excess of lanthanum, neodymium, and praseodymium salts were observed. The yttrium, samarium, and dysprosium in a mish metal were determined with both analytical curves of standard solutions containing an excess of lanthanum, cerium, and neodymium ions and of the standard addition. The precisions for this work were in the 3 - 9.3% range. (author)

  16. 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.

  17. Formulating analytic expressions for atomic collision cross sections

    International Nuclear Information System (INIS)

    Tabata, Tatsuo; Kubo, Hirotaka; Sataka, Masao

    2003-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Pasias, I.N.; Pappa, Ch.; Katsarou, V.; Thomaidis, N.S., E-mail: ntho@chem.uoa.gr; Piperaki, E.A.

    2014-02-01

    The aim of this study is to propose alternative techniques and methods in combination with the classical chemical modification to correct the major matrix interferences in the determination of boron in shrimps. The performance of an internal standard (Ge) for the determination of boron by the simultaneous multi-element atomic absorption spectrometry was tested. The use of internal standardization increased the recovery from 85.9% to 101% and allowed a simple correction of errors during sampling preparation and heating process. Furthermore, a new preparation procedure based on the use of citric acid during digestion and dilution steps improved the sensitivity of the method and decreased the limit of detection. Finally, a comparative study between the simultaneous multi-element atomic absorption spectrometry with a longitudinal Zeeman-effect background correction system, equipped with a transversely-heated graphite atomizer and the single element atomic absorption spectrometry with a D{sub 2} background correction system, equipped with an end-heated graphite atomizer was undertaken to investigate the different behavior of boron in both techniques. Different chemical modifiers for the determination of boron were tested with both techniques. Ni-citric acid and Ca were the optimal chemical modifiers when simultaneous multi-element atomic absorption spectrometry and single-element atomic absorption spectrometry were used, respectively. By using the single-element atomic absorption spectrometry, the calculated characteristic mass was 220 pg and the calculated limit of detection was 370 μg/kg. On the contrary, with simultaneous multi-element atomic absorption spectrometry, the characteristic mass was 2200 pg and the limit of detection was 5.5 mg/kg. - Highlights: • New approaches were developed to cope with interferences of B determination by ETAAS • Ge was used as internal standard for the determination of B by simultaneous ETAAS • Citric acid was used during

  19. Molecular absorption spectrometry in flames and furnaces: A review

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-12-04

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

  20. 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.

  1. Use of a discharge in an hollow cathode as neutral atom source for resonant ionization mass spectrometry

    International Nuclear Information System (INIS)

    Berthoud, T.; Briand, A.; Khelifa, N.; Mauchien, P.

    1987-01-01

    The resonance ionization mass spectrometry in our laboratory is aimed at simplification of isotope measurements of elements present in mixtures and at measurement of very small isotopes. An atomization source which produces an atomic beam collimated from a discharge in a hollow cathode has been developed. First results of this spectrometry with an uranium atomic jet are presented [fr

  2. Practical aspects and trends in analytical organic mass spectrometry

    International Nuclear Information System (INIS)

    Schlunegger, U.P.

    1981-01-01

    Proceeding from the fundamentals of mass spectrometry (MS), some more recent developments of analytical organic MS are shown in comparison with conventional MS. Sections are headed: the vacuum, production of ions in the mass spectrometer, ions in the analyzer of a mass spectrometer, general considerations, practice of modern MS: selected examples

  3. 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...

  4. Recent Studies on the Speciation and Determination of Mercury in Different Environmental Matrices Using Various Analytical Techniques

    Directory of Open Access Journals (Sweden)

    Lakshmi Narayana Suvarapu

    2017-01-01

    Full Text Available This paper reviews the current research on the speciation and determination of mercury by various analytical techniques, including the atomic absorption spectrometry (AAS, voltammetry, inductively coupled plasma optical emission spectrometry (ICP-OES, ICP-mass spectrometry (MS, atomic fluorescence spectrometry (AFS, spectrophotometry, spectrofluorometry, and high performance liquid chromatography (HPLC. Approximately 96 research papers on the speciation and determination of mercury by various analytical instruments published in international journals since 2015 were reviewed. All analytical parameters, including the limits of detection, linearity range, quality assurance and control, applicability, and interfering ions, evaluated in the reviewed articles were tabulated. In this review, we found a lack of information in speciation studies of mercury in recent years. Another important conclusion from this review was that there were few studies regarding the concentration of mercury in the atmosphere.

  5. 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)

  6. 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.

  7. 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)

  8. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-05-15

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

  10. Nuclear and nuclear related analytical methods applied in environmental research

    International Nuclear Information System (INIS)

    Popescu, Ion V.; Gheboianu, Anca; Bancuta, Iulian; Cimpoca, G. V; Stihi, Claudia; Radulescu, Cristiana; Oros Calin; Frontasyeva, Marina; Petre, Marian; Dulama, Ioana; Vlaicu, G.

    2010-01-01

    Nuclear Analytical Methods can be used for research activities on environmental studies like water quality assessment, pesticide residues, global climatic change (transboundary), pollution and remediation. Heavy metal pollution is a problem associated with areas of intensive industrial activity. In this work the moss bio monitoring technique was employed to study the atmospheric deposition in Dambovita County Romania. Also, there were used complementary nuclear and atomic analytical methods: Neutron Activation Analysis (NAA), Atomic Absorption Spectrometry (AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). These high sensitivity analysis methods were used to determine the chemical composition of some samples of mosses placed in different areas with different pollution industrial sources. The concentrations of Cr, Fe, Mn, Ni and Zn were determined. The concentration of Fe from the same samples was determined using all these methods and we obtained a very good agreement, in statistical limits, which demonstrate the capability of these analytical methods to be applied on a large spectrum of environmental samples with the same results. (authors)

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

    Science.gov (United States)

    Goudarzi, Nasser

    2009-02-11

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

  12. 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.

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

  14. 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...

  15. Electrothermal atomization laser-excited atomic fluorescence spectroscopy for the determination of indium

    International Nuclear Information System (INIS)

    Aucelio, R.Q.; Smith, B.W.; Winefordner, J.D.

    1998-01-01

    A dye laser pumped by a high-repetition-rate copper vapor laser was used as the excitation source to determine indium at parts-per-trillion level by electrothermal atomization laser-excited atomic fluorescence spectrometry (ETA-LEAFS). A comparison was made between wall atomization, in pyrolytic and nonpyrolytic graphite tubes, and platform atomization. The influence of several chemical modifiers either in solution or precoated in the graphite tube was evaluated. The influence of several acids and NaOH in the analyte solution was also studied. Optimization of the analytical conditions was carried out to achieve the best signal-to-background ratio and consequently an absolute limit of detection of 1 fg. Some possible interferents of the method were evaluated. The method was evaluated by determining indium in blood, urine, soil, and urban dust samples. Recoveries between 99.17 and 109.17% are reported. A precision of 4.1% at the 10 ng g -1 level in water standards was achieved. copyright 1998 Society for Applied Spectroscopy

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

    International Nuclear Information System (INIS)

    Papadopoulou, D.N.; Zachariadis, G.A.; Anthemidis, A.N.; Tsirliganis, N.C.; Stratis, J.A.

    2004-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Papadopoulou, D.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Zachariadis, G.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Anthemidis, A.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute, Tsimiski 58, GR-67100, Xanthi (Greece); Stratis, J.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece)]. E-mail: jstratis@chem.auth.gr

    2004-12-01

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

  18. 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

  19. 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

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

    International Nuclear Information System (INIS)

    Dulski, P.; Moeller, P.

    1975-07-01

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

  1. 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)

  2. 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...

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

    Energy Technology Data Exchange (ETDEWEB)

    Arslan, Yasin [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Mehmet Akif Ersoy University, Faculty of Arts & Sciences, Chemistry Department, 15030 Burdur (Turkey); Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Dědina, Jiří, E-mail: dedina@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2015-01-01

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

  4. Direct determination of beryllium, cadmium, lithium, lead and silver in thorium nitrate solution by electrothermal atomization atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Thulasidas, S.K.; Kulkarni, M.J.; Porwal, N.K.; Page, A.G.; Sastry, M.D.

    1988-01-01

    An electrothermal atomization atomic absorption spectrometric (ET-AAS) method is developed for the direct determination of Ag, Be, Cd, Li and Pb in thorium nitrate solution. The method offers detection of sub-nanogram amounts of these analytes in 100-microgram thorium samples with a precision of around 10%. A number of spiked samples and pre-analyzed ThO 2 samples have been analyzed to evaluate the performance of the analytical methods developed here

  5. Semi-automatic determination of tin in marine materials by continuous flow hydride generation inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Feng Yonglai; Narasaki, Hisataki; Chen Hongyuan; Tian Liching

    1997-01-01

    A semi-automated continuous flow hydride generation system with inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for the determination of tin in marine materials. The effects of acids (H 2 SO 4 and HCl) were studied. The analytical parameters were thoroughly investigated. Under optimized conditions, the detection limit is 0.4 ng/ml. Interferences from transition elements were investigated and seven masking reagents were tested. L-cysteine hydrochloride monohydrate (1%) was used to mask the interferences from foreign ions. Finally, the accuracy, checked with a marine standard reference material obtained from the National Research Council (NRC), was within the certified value. (orig.). With 6 figs., 4 tabs

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-01

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

  7. Determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Yoshida, K.; Haraguchi, H.

    1984-01-01

    Inductively coupled plasma atomic emission spectrometry (ICP-AES) interfaced with high-performance liquid chromatography (HPLC) has been applied to the determination of rare earth elements. ICP-AES was used as an element-selective detector for HPLC. The separation of rare earth elements with HPLC helped to avoid erroneous analytical results due to spectral interferences. Fifteen rare earth elements (Y and 14 lanthanides) were determined selectively with the HPLC/ICP-AES system using a concentration gradient method. The detection limits with the present HPLC/ICP-AES system were about 0.001-0.3 μg/mL with a 100-μL sample injection. The calibration curves obtained by the peak height measurements showed linear relationships in the concentration range below 500 μg/mL for all rare earth elements. A USGS rock standard sample, rare earth ores, and high-purity lanthanide reagents (>99.9%) were successfully analyzed without spectral interferences

  8. 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

  9. 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.

  10. Analytical chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Jae Seong

    1993-02-15

    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.

  11. Review and evaluation of spark source mass spectrometry as an analytical method

    International Nuclear Information System (INIS)

    Beske, H.E.

    1981-01-01

    The analytical features and most important fields of application of spark source mass spectrometry are described with respect to the trace analysis of high-purity materials and the multielement analysis of technical alloys, geochemical and cosmochemical, biological and radioactive materials, as well as in environmental analysis. Comparisons are made to other analytical methods. The distribution of the method as well as opportunities for contract analysis are indicated and developmental tendencies discussed. (orig.) [de

  12. 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)

  13. Hydride generation – in-atomizer collection of Pb in a quartz trap-and-atomizer device for atomic absorption spectrometry – an interference study

    Energy Technology Data Exchange (ETDEWEB)

    Novotný, Pavel [Institute of Analytical Chemistry of the ASCR, v.v.i., Veveří 97, 602 00 Brno (Czech Republic); High School in Hořice, Husova 1414, 508 01 Hořice (Czech Republic); Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v.v.i., Veveří 97, 602 00 Brno (Czech Republic)

    2013-01-01

    Interferences of selected hydride forming elements (As, Sb, Bi, Se and Sn) on lead determination by hydride generation atomic absorption spectrometry were extensively studied in both on-line atomization and preconcentration (collection) modes. The commonly used on-line atomization mode was found free of significant interferences, whereas strong interference from Bi was observed when employing the preconcentration mode with plumbane collection in a quartz trap-and-atomizer device. Interference of Bi seems to take place in the preconcentration step. Interference of Bi in the collection mode cannot be reduced by increased hydrogen radical amount in the trap and/or the atomizer. - Highlights: ► Interference study on Pb determination by in-atomizer trapping was performed for the first time. ► Bi was found as a severe interferent in the preconcentration mode (Pb:Bi ratio 1:100). ► No interference was found in the on-line atomization (no preconcentration). ► Bi interference occurs during preconcentration.

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

    Energy Technology Data Exchange (ETDEWEB)

    Musil, Stanislav [Institute of Analytical Chemistry of the ASCR, v.v.i., Videnska 1083, 142 20 Prague 4 (Czech Republic); Charles University in Prague, Faculty of Science, Dept. of Analytical Chemistry, Albertov 8, 128 43 Prague 2 (Czech Republic); Kratzer, Jan; Vobecky, Miloslav [Institute of Analytical Chemistry of the ASCR, v.v.i., Videnska 1083, 142 20 Prague 4 (Czech Republic); Hovorka, Jan [Charles University in Prague, Faculty of Science, Institute for Environmental Studies, Benatska 2, 128 01 Prague 2 (Czech Republic); Benada, Oldrich [Institute of Microbiology of the ASCR, v.v.i., Videnska 1083, 142 20 Prague 4 (Czech Republic); Matousek, Tomas, E-mail: matousek@biomed.cas.c [Institute of Analytical Chemistry of the ASCR, v.v.i., Videnska 1083, 142 20 Prague 4 (Czech Republic)

    2009-11-15

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

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

    Science.gov (United States)

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

    2009-03-15

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  19. 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.

  20. 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.

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

    Science.gov (United States)

    Frentiu, Tiberiu; Mihaltan, Alin I; Ponta, Michaela; Darvasi, Eugen; Frentiu, Maria; Cordos, Emil

    2011-10-15

    A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min(-1) Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl(2) reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO(3)-H(2)SO(4) mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml(-1) or 0.08 μg g(-1) in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg(-1), while recovery in two polyethylene certified reference materials in the range 98.7 ± 4.5% (95% confidence level). Copyright © 2011 Elsevier B.V. All rights reserved.

  2. 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.

  3. 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)

  4. 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)

  5. 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

  6. 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.

  7. Abstracts of the 2. Brazilian Meeting on Analytical Chemistry

    International Nuclear Information System (INIS)

    Curtius, A.J.

    1983-01-01

    Abstracts of theoretical and experimental works on Qualitative and Quantitative Analytical Chemistry are presented. Among the various analytical techniques used, emphasis is given to: neutron activation analysis, crystal doping and annealing, isotopic tracing, fission tracks detection, atomic absorption spectrophotometry, emission spectroscopy with induced coupled plasma, X-ray diffraction, nuclear magnetic resonance, mass spectrometry, polarography, ion exchange and/or thin-layer chromatography, electrodeposition, potentiometric titration and others. (C.L.B) [pt

  8. Development of ultrasensitive spectroscopic analysis technology -Development of atomic spectroscopy technology-

    International Nuclear Information System (INIS)

    Cha, Hyung Ki; Song, Ky Seok; Rhee, Young Joo; Baik, Dae Hyun; Shin, Jang Soo; Kim, Duck Hyun; Yang, Ki Ho; Yi, Jong Hoon

    1994-07-01

    In this project, three principal techniques are developed. The laser photoionization spectrometry (LAPIS) is used for the ultrasensitive detection for heavy metals such as Pb and Cd. The Laser atomic fluorescence spectrometry is applied to the quantitative analysis of the lanthanide and actinide elements. And the DIAL remote sensing system is used for monitoring the ozone concentration and the atmospheric pollution. A time-of-flight mass spectrometer and a high efficient atomic beam generator were designed and manufactured. Various spectroscopic parameters and optimum analytical condition were investigated. By using the laser fluorescence technique, U, Eu and Sm in solution were quantitatively analyzed. The basic researches for the direct analytical method of solid samples were also carried out. The DIAL system for ozone remote sensing was developed and ozone concentration above Taejon were obtained. (Author)

  9. Analytical quality control services of the International Atomic Energy Agency

    International Nuclear Information System (INIS)

    Suschny, O.

    1986-01-01

    The International Atomic Energy Agency provides quality control services to analytical laboratories. These services which include the provision of reference materials and the organisation of intercomparisons are rendered for the purpose of assisting laboratories in determining the accuracy of their analytical work. The following classes of materials are presently available: nuclear materials, environmental materials, animal and plant materials, materials for biomedical studies and materials of marine origin. (orig.) [de

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

    International Nuclear Information System (INIS)

    Frentiu, Tiberiu; Mihaltan, Alin I.; Ponta, Michaela; Darvasi, Eugen; Frentiu, Maria; Cordos, Emil

    2011-01-01

    Highlights: → Use of a miniaturized analytical system with microtorch plasma for Hg determination. → Determination of Hg in non- and biodegradable materials using cold vapor generation. → Figures of merit and advantages of the miniaturized system for Hg determination. - Abstract: A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min -1 Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl 2 reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO 3 -H 2 SO 4 mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml -1 or 0.08 μg g -1 in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg -1 , while recovery in two polyethylene certified reference materials in the range 98.7 ± 4.5% (95% confidence level).

  11. Analytic cross sections for collisions of H, H2, He and Li atoms and ions with atoms and molecules. 3

    International Nuclear Information System (INIS)

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

    1995-07-01

    Analytic expressions fitted to Barnett's recommended data are given for the collision cross sections of H, H 2 , He, and Li atoms and ions colliding with atoms and molecules. The collisions treated are ionization collisions, charge-production collisions, electron-loss collisions, and electron detachment collisions. The analytic 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)

  12. 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.

  13. An analytical method for computing atomic contact areas in biomolecules.

    Science.gov (United States)

    Mach, Paul; Koehl, Patrice

    2013-01-15

    We propose a new analytical method for detecting and computing contacts between atoms in biomolecules. It is based on the alpha shape theory and proceeds in three steps. First, we compute the weighted Delaunay triangulation of the union of spheres representing the molecule. In the second step, the Delaunay complex is filtered to derive the dual complex. Finally, contacts between spheres are collected. In this approach, two atoms i and j are defined to be in contact if their centers are connected by an edge in the dual complex. The contact areas between atom i and its neighbors are computed based on the caps formed by these neighbors on the surface of i; the total area of all these caps is partitioned according to their spherical Laguerre Voronoi diagram on the surface of i. This method is analytical and its implementation in a new program BallContact is fast and robust. We have used BallContact to study contacts in a database of 1551 high resolution protein structures. We show that with this new definition of atomic contacts, we generate realistic representations of the environments of atoms and residues within a protein. In particular, we establish the importance of nonpolar contact areas that complement the information represented by the accessible surface areas. This new method bears similarity to the tessellation methods used to quantify atomic volumes and contacts, with the advantage that it does not require the presence of explicit solvent molecules if the surface of the protein is to be considered. © 2012 Wiley Periodicals, Inc. Copyright © 2012 Wiley Periodicals, Inc.

  14. 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

  15. 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.

  16. Determination of technetium by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

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

    1978-01-01

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

  17. 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

  18. 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

  19. 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.

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

    Science.gov (United States)

    Taylor, Howard E.; Garbarino, John R.

    1988-01-01

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

  1. 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.

  2. 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.

  3. Flow injection analysis in inductively coupled plasma spectrometry

    International Nuclear Information System (INIS)

    Rosias, Maria F.G.G.

    1995-10-01

    The main features of flow injection analysis (FIA) as contribution to the inductively coupled plasma (Icp) spectrometry are described. A systematic review of researches using the combined FIA-Icp and the benefits of this association are presented. Flow systems were proposed to perform on-line Icp solution management for multielemental determination by atomic emission spectrometry (Icp-AES) or mass spectrometry. The inclusion of on-line ion exchangers in flow systems for matrix separation and/or analyte preconcentration are presented. Together with those applications the new advent of instruments with facilities for multielement detection on flow injection signals are described. (author). 75 refs., 19 figs

  4. Evaluation of a hydride generation-atomic fluorescence system for the determination of arsenic using a dielectric barrier discharge atomizer

    International Nuclear Information System (INIS)

    Zhu Zhenli; Liu Jixin; Zhang Sichun; Na Xing; Zhang Xinrong

    2008-01-01

    A new atomizer based on atmospheric pressure dielectric barrier discharge (DBD) plasma was specially designed for atomic fluorescence spectrometry (AFS) in order to be applied to the measurement of arsenic. The characteristics of the DBD atomizer and the effects of different parameters (power, discharge gas, gas flow rate, and KBH 4 concentration) were discussed in the paper. The DBD atomizer shows the following features: (1) low operation temperature (between 44 and 70 deg. C, depending on the operation conditions); (2) low power consumption; (3) operation at atmospheric pressure. The detection limit of As(III) using hydride generation (HG) with the proposed DBD-AFS was 0.04 μg L -1 . The analytical results obtained by the present method for total arsenic in reference materials, orchard leaves (SRM 1571) and water samples GBW(E) 080390, agree well with the certified values. The present HG-DBD-AFS is more sensitive and reliable for the determination of arsenic. It is a very promising technique allowing for field arsenic analysis based on atomic spectrometry

  5. Analysis of organic compounds by secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS)

    International Nuclear Information System (INIS)

    Ewinger, H.P.

    1993-05-01

    This study is about the use of secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS) as analytical techniques with depth resolution in determining organic components in environmental solid microparticles. The first application of plasma SNMS to organic compounds revealed the spectra to be composed mainly of signals from the atoms of all participating elements, such as C, H, O, N, S, P, and Cl. In addition, signals produced by multi-atomic clusters can be detected, such as CH, C 2 , CH 2 , C 2 H, and C 3 , as well as signals indicating the presence of organic compounds with hetero elements, such as OH, NH, and CN. Their intensity decreases very markedly with increasing numbers of atoms. Among the signals from bi-atomic clusters, those coming from elements with large mass differences are most intense. The use of plasma SNMS with organic compounds has shown that, except for spurious chemical reactions induced by ion bombardment and photodesorption by the photons of the plasma, it is possible to analyze with resolution in depth, elements of organic solids. A more detailed molecular characterization of organic compounds is possible by means of SIMS on the basis of multi-atomic fragments and by comparison with suitable signal patterns. (orig./BBR) [de

  6. 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.

  7. Recent Developments in the Speciation and Determination of Mercury Using Various Analytical Techniques

    Directory of Open Access Journals (Sweden)

    Lakshmi Narayana Suvarapu

    2015-01-01

    Full Text Available This paper reviews the speciation and determination of mercury by various analytical techniques such as atomic absorption spectrometry, voltammetry, inductively coupled plasma techniques, spectrophotometry, spectrofluorometry, high performance liquid chromatography, and gas chromatography. Approximately 126 research papers on the speciation and determination of mercury by various analytical techniques published in international journals since 2013 are reviewed.

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    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...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-03-15

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

  10. Development of accelerator mass spectrometry in China Institute of Atomic Energy

    International Nuclear Information System (INIS)

    He Ming; Jiang Shan; Dong Kejun; Qiu Jiuzi; Peng Bo; Guan Yongjing; Yin Xinyi; Wu Shaoyong; Li Shihong; Zhou Duo

    2005-01-01

    The measurement method for some radio isotope such as 99 Tc, 182 Hf, 151 Sm is developing in China Institute of Atomic Energy (CIAE) accelerator mass spectrometry (AMS) system, and applications in the fields of nuclear physics, geosciences, life science and materials science is carried out. The brief introduction of these methods and applications are described in this paper. (authors)

  11. Application of resonance ionization mass spectrometry for trace analysis and in fundamental research

    International Nuclear Information System (INIS)

    Passler, G.

    1997-01-01

    Resonance ionization mass spectrometry (RIMS) has been used for ultra-trace analysis on long-lived radioisotopes like Pu, Tc and 89,90 Sr in various environmental samples. The experimental approaches cover pulsed laser spectroscopy on a thermal atomic beam and subsequent time-of-flight mass analysis, a pulsed laser ion source combined with conventional mass spectrometry, and collinear resonance ionization on a mass-separated fast atomic beam. The high sensitivity of RIMS also enables atomic spectroscopy on rare isotopes. For the first time experimental values for the ionization potential of actinides up to Cf have been determined. The paper reviews the dependency of the different experimental approaches on the analytical problem. copyright 1997 American Institute of Physics

  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...... is presented encompassing protein characterization prior to and after cloning of the corresponding gene....

  13. 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.

  14. 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

  15. Analytic structure of the wave function for a hydrogen atom in an analytic potential

    International Nuclear Information System (INIS)

    Hill, R.N.

    1984-01-01

    The rate of convergence of an approximate method for solving Schroedinger's equation depends on the ability of the approximating sequence to mimic the analytic structure of the unknown exact wave function. Thus a knowledge of the analytic structure of the wave function can be of great value when approximation schemes are designed. Consider the Schroedinger equation [- 1/2 del 2 -r -1 +V(r)]Psi(r) = EPsi(r) for a hydrogen atom in a potential V(r). The general theory of elliptic partial differential equations implies that Psi is analytic at regular points, but no general theory is available at singular points. The present paper investigates the Coulomb singular point at r = 0 and shows that, if V(r) = V 1 (x, y, z)+rV 2 (x, y, z) where V 1 and V 2 are analytic functions of x, y, z at x = y = z = 0, then the wave function has the form Psi(r) = Psi 1 (x, y, z)+rPsi 2 (x, y, z) where Psi 1 and Psi 2 are analytic functions of x, y, z at x = y = z = 0

  16. 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

  17. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Frentiu, Tiberiu, E-mail: ftibi@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Mihaltan, Alin I., E-mail: alinblaj2005@yahoo.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania); Ponta, Michaela, E-mail: mponta@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Darvasi, Eugen, E-mail: edarvasi@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Frentiu, Maria, E-mail: frentiu.maria@yahoo.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania); Cordos, Emil, E-mail: emilcordos@gmail.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania)

    2011-10-15

    Highlights: {yields} Use of a miniaturized analytical system with microtorch plasma for Hg determination. {yields} Determination of Hg in non- and biodegradable materials using cold vapor generation. {yields} Figures of merit and advantages of the miniaturized system for Hg determination. - Abstract: A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min{sup -1} Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl{sub 2} reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO{sub 3}-H{sub 2}SO{sub 4} mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml{sup -1} or 0.08 {mu}g g{sup -1} in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg{sup -1}, while recovery in two polyethylene certified reference materials in the range 98.7 {+-} 4.5% (95% confidence level).

  19. 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...

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  1. 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…

  2. Gas Atomization of Aluminium Melts: Comparison of Analytical Models

    Directory of Open Access Journals (Sweden)

    Georgios Antipas

    2012-06-01

    Full Text Available A number of analytical models predicting the size distribution of particles during atomization of Al-based alloys by N2, He and Ar gases were compared. Simulations of liquid break up in a close coupled atomizer revealed that the finer particles are located near the center of the spray cone. Increasing gas injection pressures led to an overall reduction of particle diameters and caused a migration of the larger powder particles towards the outer boundary of the flow. At sufficiently high gas pressures the spray became monodisperse. The models also indicated that there is a minimum achievable mean diameter for any melt/gas system.

  3. Analytic properties of the relativistic Thomas-Fermi equation and the total energy of atomic ions

    International Nuclear Information System (INIS)

    March, N.H.; Senatore, G.

    1985-06-01

    The analytic properties of solutions of the relativistic Thomas-Fermi equation which tend to zero at infinity are first examined, the neutral atom solution being a member of this class. A new length is shown to enter the theory, proportional to the square root of the fine structure constant. This information is used to develop a perturbation expansion around the neutral atom solution, corresponding to positive atomic ions with finite but large radii. The limiting law relating ionic radius to the degree of ionization is thereby displayed in functional form, and solved explicitly to lowest order in the fine structure constant. To embrace this knowledge of heavy positive ions, as well as results from the one-electron Dirac equation, a proposal is then advanced as to the analytic form of the relativistic total energy E(Z,N) of an atomic ion with nuclear charge Ze and total number of electrons N. The fact that, for N>1, the nucleus is known only to bind Z+n electrons, where n is 1 or 2, indicates non-analyticity in the complex Z plane, represented by a circle of radius Z approx.= N. Such non-analyticity is also a property of the non-relativistic energy derived from the many-electron Schroedinger equation. The relativistic theory, however, must also embody a second type of non-analyticity associated with the known property for N=1 that the Dirac equation predicts electron-positron pair production when the electronic binding energy becomes equal to twice the electron rest mass energy. This corresponds to a second circle of non-analyticity in E(Z,N), and hence to a Taylor-Laurent expansion of this quantity in the atomic number Z. The relation of this expansion to the Layzer-Bahcall series is finally discussed. (author)

  4. 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.

  5. 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...

  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. 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)

  8. AM1 and electron impact mass spectrometry study of the ...

    African Journals Online (AJOL)

    Recently, in electron impact mass spectrometry (EIMS), it has been found a good correlation between the fragmentation processes of coumarins and the electronic charges of the atoms of their skeleton. In this paper, the same analytical method has been applied to 4-acyl isochroman-1,3-diones, whose mass spectra had ...

  9. 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)

  10. 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...

  11. High-resolution continuum source atomic absorption spectrometry for the simultaneous or sequential monitoring of multiple lines. A critical review of current possibilities

    International Nuclear Information System (INIS)

    Resano, M.; Flórez, M.R.; García-Ruiz, E.

    2013-01-01

    This work examines the capabilities and limitations of commercially available high-resolution continuum source atomic absorption spectrometry instrumentation for multi-line monitoring, discussing in detail the possible strategies to develop multi-element methodologies that are truly simultaneous, or else sequential, but from the same sample aliquot. Moreover, the simultaneous monitoring of various atomic or molecular lines may bring other important analytical advantages, such as: i) expansion of the linear range by monitoring multiplets; ii) improvements in the limit of detection and in precision by summing the signals from different lines of the same element or molecule; iii) simple correction for matrix-effects by selecting a suitable internal standard; or iv) accurate mathematical correction of spectral overlaps by simultaneous monitoring of free lines of the interfering molecule or element. This work discusses how authors have made use of these strategies to develop analytical methodologies that permit the straightforward analysis of complex samples. - Highlights: • HR CS AAS potential for simultaneous multi-line monitoring is critically examined. • Strategies to develop simultaneous multi-element methods are discussed. • Other benefits of multi-line monitoring (e.g., use of an IS or LSBC) are highlighted. • Selected examples from the literature are discussed in detail

  12. Atom-number squeezing and bipartite entanglement of two-component Bose-Einstein condensates: analytical results

    Energy Technology Data Exchange (ETDEWEB)

    Jin, G R; Wang, X W; Li, D; Lu, Y W, E-mail: grjin@bjtu.edu.c [Department of Physics, Beijing Jiaotong University, Beijing 100044 (China)

    2010-02-28

    We investigate spin dynamics of a two-component Bose-Einstein condensate with weak Josephson coupling. Analytical expressions of atom-number squeezing and bipartite entanglement are presented for atom-atom repulsive interactions. For attractive interactions, there is no number squeezing; however, the squeezing parameter is still useful to recognize the appearance of Schroedinger's cat state.

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

    International Nuclear Information System (INIS)

    Pereira Junior, Sergio Matias

    2014-01-01

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

  14. 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.

  15. Curve resolution and figures of merit estimation for determination of trace elements in geological materials by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Lorber, A.; Harel, A.; Goldbart, Z.; Brenner, I.B.

    1987-01-01

    In geochemical analysis using inductively coupled plasma atomic emission spectrometry (ICP-AES), spectral interferences and background enhancement in response to sample concomitants are the main cause of deterioration of the limit of detection (LOD) and inaccuracy of the determination at the trace and minor element levels. In this account, the authors describe the chemometric procedure of curve resolution for compensating for these sources of error. A newly developed method for calculating figures of merit is used to evaluate the correction procedure, test the statistical significance of the determined concentration, and determine LODs for each sample. The technique involves scanning the vicinity of the spectral line of the analyte. With prior knowledge of potential spectral interferences, deconvolution of the overlapped response is possible. Analytical data for a wide range of geological standard reference materials demonstrate the effectiveness of the chemometric techniques. Separation of 0.002 nm spectral coincidence, employing a 0.02 nm resolution spectrometer, is demonstrated

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

    International Nuclear Information System (INIS)

    Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

    2010-01-01

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

  17. 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.

  18. 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...

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

    Energy Technology Data Exchange (ETDEWEB)

    Titretir, Serap [Department of Chemistry, Inoenue University, 44065 Malatya (Turkey); Kenduezler, Erdal [Department of Primary Education, Faculty of Education, Ahi Evran University, 40100 Kirsehir (Turkey); Arslan, Yasin [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Atatuerk University, 25240 Erzurum (Turkey); Kula, Ibrahim [Department of Chemistry, Mugla University, 48000 Mugla (Turkey); Bakirdere, Sezgin [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Zonguldak Karaelmas University, 67100 Zonguldak (Turkey); Ataman, O. Yavuz. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey)], E-mail: ataman@metu.edu.tr

    2008-08-15

    An electrically heated tungsten coil was used as a trap in the determination of antimony. The technique consists of three steps. Initially, SbH{sub 3} is formed by hydride generation procedure; then the analyte species in vapor form are transported to W-coil trap heated at 370 deg. C. Following the preconcentration step, the trap is heated to 895 deg. C; analyte species are revolatilized and transported to the flame-heated quartz atom cell where atomization and the formation of signal take place. The experimental parameters were optimized both for trap and no-trap studies. The most important experimental parameters are concentrations of HCl and NaBH{sub 4} solutions, H{sub 2} and Ar gas flow rates, and collection and revolatilization temperatures of W-coil. Accuracy was tested using a certified reference material, waste water EU-L-1. Limit of detection for the system is 16 ng l{sup -1} using a sample of 36 ml collected in 4.0 min. Enhancement factor in sensitivity was 17.

  20. 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.

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

    International Nuclear Information System (INIS)

    Fuentes, Edwar; Pinochet, Hugo; Gregori, Ida de; Potin-Gautier, Martine

    2003-01-01

    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 2 O, 0.05 mol l -1 EDTA and 0.25 mol l -1 H 2 SO 4 . Since the soil samples were collected from sites impacted by copper mining activities, the effect of Cu 2+ on the determination of antimony in synthetic solutions and soil extracts was studied. Cu 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 -1 for Sb(III) and total antimony, respectively, and the R.S.D. at the 0.5-μg l -1 level were 2.5 and 2.4%, respectively. The total antimony concentration of soils is in the mg kg -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

  2. Feasibility study of the single particle analysis of uranium by laser ionization time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Ha, Yeong Keong; Han, Sun Ho; Pyo, Hyung Yeol; Park, Yong Joon; Song, Kyu Seok

    2004-01-01

    The control of activities in nuclear facilities worldwide is one of the most important tasks of nuclear safeguard. To meet the needs for nuclear safeguard, International Atomic Energy Agency (IAEA) strengthened the control of nuclear activities to detect these activities earlier. Thus, it is very important to develop analytical techniques to determine the isotopic composition of hot particles from swipe samples. The precise measurement of the 234 U/ 238 U, 235 U/ 238 U and 236 U/ 238 U ratios is important because it provides information about the initial enrichment of reactor uranium, core history, and post accident story. Because conventional α-spectrometry is not sufficiently sensitive for the determination of long-lived radionuclides in environmental samples, several analytical techniques, such as SNMS (Sputtered Neutral Mass Spectrometry), RIMS (Resonance Ionization Mass Spectrometry), AMS (Accelerator Mass Spectrometry) etc., have been proposed for uranium isotope measurements. In case of microparticles, analytical techniques such as SIMS (Secondary Ion Mass Spectrometry) have been applied for the isotopic characterization. The aim of this work was the development of a sensitive analytical technique for determination of isotopic ratio of uranium in swipe samples. In this work, feasibility of LIMS (Laser Ionization Mass Spectrometry) for the determination of such particles has been evaluated using a reference material of natural uranium

  3. 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

  4. 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.

  5. Plasma-cavity ringdown spectroscopy for analytical measurement: Progress and prospectives

    Science.gov (United States)

    Zhang, Sida; Liu, Wei; Zhang, Xiaohe; Duan, Yixiang

    2013-07-01

    Plasma-cavity ringdown spectroscopy is a powerful absorption technique for analytical measurement. It combines the inherent advantages of high sensitivity, absolute measurement, and relative insensitivity to light source intensity fluctuations of the cavity ringdown technique with use of plasma as an atomization/ionization source. In this review, we briefly describe the background and principles of plasma-cavity ringdown spectroscopy(CRDS) technology, the instrumental components, and various applications. The significant developments of the plasma sources, lasers, and cavity optics are illustrated. Analytical applications of plasma-CRDS for elemental detection and isotopic measurement in atomic spectrometry are outlined in this review. Plasma-CRDS is shown to have a promising future for various analytical applications, while some further efforts are still needed in fields such as cavity design, plasma source design, instrumental improvement and integration, as well as potential applications in radical and molecular measurements.

  6. 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

  7. 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

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

    International Nuclear Information System (INIS)

    Li Yan; Yin Xuebo; Yan Xiuping

    2008-01-01

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

  9. 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.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  11. [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.

  12. Simultaneous determination of Cr, Ga, In and V in soil and water samples by tungsten coil atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Donati, George L.; Kron, Benjamin E. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)], E-mail: jonesbt@wfu.edu

    2009-06-15

    Tungsten coil atomic emission spectrometry is employed for the simultaneous determination of Cr, Ga, In, and V. Both V and In are detected by this technique for the first time. The atomizer is a simple, inexpensive tungsten filament extracted from a mass-produced, commercially-available 150 W, 15 V microscope bulb. A 25 {mu}l sample aliquot is placed directly on the coil and a small constant-current power source is used to carefully dry, ash and atomize the sample. Analytical signals are detected with a Czerny-Turner spectrograph and a charge coupled device detector. Multiple emission lines from all 4 elements are monitored simultaneously in a 54 nm spectral window. Concentration limits of detection are in the {mu}g l{sup - 1} range for all elements, and the absolute limits of detection are 0.2, 2, 0.5, and 10 ng for Cr, Ga, In, and V, respectively. Even lower values may be obtained by combining the signals for the multiple emission lines of a single element. The method precision is typically better than 5.0% relative standard deviation, and sometimes as good as 0.95% (Ga). Standard reference materials of soil and water are used to check the method accuracy. After a simple acid extraction, the values determined by the method presented no significant difference from the reported values at the 95% confidence level.

  13. Pre-analytical and analytical variation of drug determination in segmented hair using ultra-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Nielsen, Marie Katrine Klose; Johansen, Sys Stybe; Linnet, Kristian

    2014-01-01

    Assessment of total uncertainty of analytical methods for the measurements of drugs in human hair has mainly been derived from the analytical variation. However, in hair analysis several other sources of uncertainty will contribute to the total uncertainty. Particularly, in segmental hair analysis pre-analytical variations associated with the sampling and segmentation may be significant factors in the assessment of the total uncertainty budget. The aim of this study was to develop and validate a method for the analysis of 31 common drugs in hair using ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) with focus on the assessment of both the analytical and pre-analytical sampling variations. The validated method was specific, accurate (80-120%), and precise (CV≤20%) across a wide linear concentration range from 0.025-25 ng/mg for most compounds. The analytical variation was estimated to be less than 15% for almost all compounds. The method was successfully applied to 25 segmented hair specimens from deceased drug addicts showing a broad pattern of poly-drug use. The pre-analytical sampling variation was estimated from the genuine duplicate measurements of two bundles of hair collected from each subject after subtraction of the analytical component. For the most frequently detected analytes, the pre-analytical variation was estimated to be 26-69%. Thus, the pre-analytical variation was 3-7 folds larger than the analytical variation (7-13%) and hence the dominant component in the total variation (29-70%). The present study demonstrated the importance of including the pre-analytical variation in the assessment of the total uncertainty budget and in the setting of the 95%-uncertainty interval (±2CVT). Excluding the pre-analytical sampling variation could significantly affect the interpretation of results from segmental hair analysis. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

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

    Science.gov (United States)

    Ombaba, Jackson M.

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

  15. 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,…

  16. Nanoscience, nanotechnology and spectrometry

    International Nuclear Information System (INIS)

    Adams, Freddy C.; Barbante, Carlo

    2013-01-01

    Nanoscience has outgrown its infancy, and nanotechnology has found important applications in our daily life — with many more to come. Although the central concepts of the nano world, namely the changes of particular physical properties on the length scale of individual atoms and molecules, have been known and developed for quite some time already, experimental advances since the 1980s and recognition of the potential of nanomaterials led to a genuine breakthrough of the inherently multidisciplinary nanoscience field. Analytical nanoscience and nanotechnology and especially the use of micro and nano electro mechanical systems, of the quantum dots and of mass spectrometry, currently provide one of the most promising avenues for developments in analytical science, derived from their two main fields of action, namely (a) the analysis of nano-structured materials and (b) their use as new tools for analysis. An overview is given of recent developments and trends in the field, highlighting the importance and point out future directions, while also touching drawbacks, such as emerging concerns about health and environmental issues. - Highlights: • We review the analysis of nano-structured materials. • Nano-structured materials can be used as new tools for analysis. • Use of nano electro mechanical systems, of quantum dots and of mass spectrometry • Nanotechnologies are among the most promising tools in analytical science

  17. Nanoscience, nanotechnology and spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Adams, Freddy C. [Department of Chemistry, University of Antwerp, B-2610 Wilrijk (Belgium); Barbante, Carlo, E-mail: barbante@unive.it [Institute for the Dynamics of Environmental Processes — CNR, Venice (Italy); Department of Environmental Sciences, Informatics and Statistics, Ca' Foscari University, Venice (Italy)

    2013-08-01

    Nanoscience has outgrown its infancy, and nanotechnology has found important applications in our daily life — with many more to come. Although the central concepts of the nano world, namely the changes of particular physical properties on the length scale of individual atoms and molecules, have been known and developed for quite some time already, experimental advances since the 1980s and recognition of the potential of nanomaterials led to a genuine breakthrough of the inherently multidisciplinary nanoscience field. Analytical nanoscience and nanotechnology and especially the use of micro and nano electro mechanical systems, of the quantum dots and of mass spectrometry, currently provide one of the most promising avenues for developments in analytical science, derived from their two main fields of action, namely (a) the analysis of nano-structured materials and (b) their use as new tools for analysis. An overview is given of recent developments and trends in the field, highlighting the importance and point out future directions, while also touching drawbacks, such as emerging concerns about health and environmental issues. - Highlights: • We review the analysis of nano-structured materials. • Nano-structured materials can be used as new tools for analysis. • Use of nano electro mechanical systems, of quantum dots and of mass spectrometry • Nanotechnologies are among the most promising tools in analytical science.

  18. Sample diagnosis using indicator elements and non-analyte signals for inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Antler, Margaret; Ying Hai; Burns, David H.; Salin, Eric D.

    2003-01-01

    A sample diagnosis procedure that uses both non-analyte and analyte signals to estimate matrix effects in inductively coupled plasma-mass spectrometry is presented. Non-analyte signals are those of background species in the plasma (e.g. N + , ArO + ), and changes in these signals can indicate changes in plasma conditions. Matrix effects of Al, Ba, Cs, K and Na on 19 non-analyte signals and 15 element signals were monitored. Multiple linear regression was used to build the prediction models, using a genetic algorithm for objective feature selection. Non-analyte elemental signals and non-analyte signals were compared for diagnosing matrix effects, and both were found to be suitable for estimating matrix effects. Individual analyte matrix effect estimation was compared with the overall matrix effect prediction, and models used to diagnose overall matrix effects were more accurate than individual analyte models. In previous work [Spectrochim. Acta Part B 57 (2002) 277], we tested models for analytical decision making. The current models were tested in the same way, and were able to successfully diagnose matrix effects with at least an 80% success rate

  19. 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.

  20. 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 atom...

  1. 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)

  2. 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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  4. 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.

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

    International Nuclear Information System (INIS)

    Grinberg, Patricia; Campos, Reinaldo C.; Mester, Zoltan; Sturgeon, Ralph E.

    2003-01-01

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

  6. 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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-04-15

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

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

    Science.gov (United States)

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

    2005-01-01

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

  10. 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.)

  11. Multipumping flow system for improving hydride generation atomic fluorescence spectrometric determinations

    International Nuclear Information System (INIS)

    Lopez-Garcia, Ignacio; Ruiz-Alcaraz, Irene; Hernandez-Cordoba, Manuel

    2006-01-01

    The advantages of using membrane micropumps rather than peristaltic pumps to introduce both sample and reagent solutions for hydride generation atomic fluorescence spectrometry are discussed. Arsenic was used as a test analyte to check the performance of the proposed manifold. Sample and reagent consumption was reduced 8-9 fold compared with continuous mode measurements made with peristaltic pumps, with no deterioration in sensitivity. The calibration graph was linear in the 0.05 to 2.5 μg l -1 As range using peak area as the analytical signal and maximum gain in the detector setting. A limit of detection (3σ) of 0.02 μg l -1 and relative standard deviation values close to 2% for 10 independent measurements of a 1 μg l -1 As solution were obtained. The sampling frequency increased from 45 to 102 h -1 with the subsequent saving in carrier gas used and reduction in wastes generated. The instrumental modification, which could be used for other elements currently determined by atomic fluorescence spectrometry, will permit hydride generators of more reduced dimensions to be constructed

  12. 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.

  13. Critical comparison of performances of inductively coupled plasma atomic emission spectrometry and neutron activation analysis for the determination of elements in human lungs

    International Nuclear Information System (INIS)

    Alimonti, A.; Coni, E.; Caroli, S.; Sabbioni, E.; Nicolaou, G.E.; Pietra, R.

    1989-01-01

    A study was carried out to assess the performance of inductively coupled plasma atomic emission spectrometry (ICP-AES) and neutron activation analysis (NAA) techniques for determining reference values for Al, Cd, Cr, Cu, Mg, Mn, V and Zn in human lungs of urban non-smoking subjects. Experimental data were subjected to the usual basic statistical tests to evaluate the respective merits of the two basically different analytical techniques. Both approaches, if used under carefully optimised experimental conditions, can yield reliable results affected only minimally by systematic and random errors. On the other hand, on a more routine basis, particular attention should be paid to elements such as Al, Cd and V which may pose some problems with both techniques. (author)

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    CERN Document Server

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

    2002-01-01

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

  16. 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.

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

    International Nuclear Information System (INIS)

    Zhang Xiao-Jun; Chen Chang-Le

    2016-01-01

    Within the harmonic approximation, the analytic expression of the dynamical matrix is derived based on the modified analytic embedded atom method (MAEAM) and the dynamics theory of surface lattice. The surface phonon dispersions along three major symmetry directions, and XM-bar are calculated for the clean Ag (100) surface by using our derived formulas. We then discuss the polarization and localization of surface modes at points X-bar and M-bar by plotting the squared polarization vectors as a function of the layer index. The phonon frequencies of the surface modes calculated by MAEAM are compared with the available experimental and other theoretical data. It is found that the present results are generally in agreement with the referenced experimental or theoretical results, with a maximum deviation of 10.4%. The agreement shows that the modified analytic embedded atom method is a reasonable many-body potential model to quickly describe the surface lattice vibration. It also lays a significant foundation for studying the surface lattice vibration in other metals. (paper)

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

    Directory of Open Access Journals (Sweden)

    Yuya Koike

    2017-03-01

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

  19. Study of the analytic quality in the determinations of Cr, Fe, Mn, Cu, Zn, Pb and Hg through conventional and nuclear analytical techniques in mosses of the MATV

    International Nuclear Information System (INIS)

    Caballero S, B.

    2013-01-01

    To evaluate the environmental risks of air pollution and to facilitate the decision-making for control, is necessary to have the capacity to generate data with analytical quality. A comparison between nuclear (Neutron activation analysis and total reflection X-ray fluorescence spectrometry) and no nuclear analytical techniques (atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry) for simultaneous determination of metal content (Cr, Cu, Fe, Hg, Mn, Pb and Zn) in mosses from Metropolitan Area of the Toluca Valley (MATV) was performed. Epiphytic mosses (Fabriona ciliaris and Leskea angustata) were sampled in two campaigns, 16 sites (urban, transition and natural) and were prepared for each technique. The biological certified reference materials were used for the quality control and to evaluate accuracy, precision, linearity, detection and quantification limits. Results show that nuclear analytical techniques and no nuclear applied in chemical analysis of Cr, Cu, Fe, Hg, Mn, Pb and Zn in moss from MATV are comparable and therefore all of these can potentially be used for this purpose. However, if its considered both, the performance parameters and economic/operational characteristics is widely recommended inductively coupled plasma optical emission spectrometry, conventional analytical technique, which showed the highest analytical grade quality. Also were observed spatial and temporal variations in the concentrations of Cr, Cu, Fe, Hg, Mn, Pb and Zn in mosses from MATV and was discussed its potential origin. The urban sites had the highest concentration of anthropogenic elements as Cr, Cu, Fe, Hg, Pb and Zn because are strongly impacted by roads with high vehicle traffic. (Author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-08-01

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

  1. Cobalt as chemical modifier to improve chromium sensitivity and minimize matrix effects in tungsten coil atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Sidnei G. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil); Donati, George L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Santos, Luana N. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Nóbrega, Joaquim A. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil)

    2013-05-30

    Graphical abstract: -- Highlights: •Charge transfer reactions increase the population of Cr{sup +}. •Chromium ions and electrons recombine to form excited-state Cr atoms. •A 10-fold improvement in LOD is observed for Cr emission measurements. •The two-step ionization/excitation mechanism improves sensitivity and accuracy. •High concentrations of Co also minimize matrix effects. -- Abstract: Cobalt is used as chemical modifier to improve sensitivity and minimize matrix effects in Cr determinations by tungsten coil atomic emission spectrometry (WCAES). The atomizer is a tungsten filament extracted from microscope light bulbs. A solid-state power supply and a handheld CCD-based spectrometer are also used in the instrumental setup. In the presence of 1000 mg L{sup −1} Co, WCAES limit of detection for Cr (λ = 425.4 nm) is calculated as 0.070 mg L{sup −1}; a 10-fold improvement compared to determinations without Co modifier. The mechanism involved in such signal enhancement is similar to the one observed in ICP OES and ICP-MS determinations of As and Se in the presence of C. Cobalt increases the population of Cr{sup +} by charge transfer reactions. In a second step, Cr{sup +}/e{sup −} recombination takes place, which results in a larger population of excited-state Cr atoms. This alternative excitation route is energetically more efficient than heat transfer from atomizer and gas phase to analyte atoms. A linear dynamic range of 0.25–10 mg L{sup −1} and repeatability of 3.8% (RSD, n = 10) for a 2.0 mg L{sup −1} Cr solution are obtained with this strategy. The modifier high concentration also contributes to improving accuracy due to a matrix-matching effect. The method was applied to a certified reference material of Dogfish Muscle (DORM-2) and no statistically significant difference was observed between determined and certified Cr values at a 95% confidence level. Spike experiments with bottled water samples resulted in recoveries between 93% and

  2. Quantification of elemental mapping of heterogeneous geological sample by laser ablation inductively coupled plasma mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vaculovič, T.; Breiter, Karel; Korbelová, Zuzana; Venclová, Natalie; Tomková, Kateřina; Jonášová, Šárka; Kanický, V.

    2017-01-01

    Roč. 133, JUL 2017 (2017), s. 200-207 ISSN 0026-265X R&D Projects: GA ČR GA14-13600S Institutional support: RVO:67985831 ; RVO:67985912 Keywords : LA-ICP-MS * induced breakdown spectroscopy * atomic emission spectrometry * in-situ analysis * trace-metals Subject RIV: CB - Analytical Chemistry, Separation; AC - Archeology, Anthropology, Ethnology (ARU-G) OBOR OECD: Analytical chemistry; Archaeology (ARU-G) Impact factor: 3.034, year: 2016

  3. Plasma-related matrix effects in inductively coupled plasma--atomic emission spectrometry by group I and group II matrix-elements

    International Nuclear Information System (INIS)

    Chan, George C.-Y.; Chan, W.-T.

    2003-01-01

    The effects of Na, K, Ca and Ba matrices on the plasma excitation conditions in inductively coupled plasma-atomic emission spectrometry (ICP-AES) were studied. Normalized relative intensity was used to indicate the extent of the plasma-related matrix effects. The group I matrices have no effects on the plasma excitation conditions. In contrast, the group II matrices depress the normalized relative intensities of some spectral lines. Specifically, the Group II matrices have no effects on the normalized relative intensity of atomic lines of low upper energy level (soft lines), but reduce the normalized relative intensity of some ionic lines and atomic lines of high energy level (hard lines). The Group II matrices seem to shift the Saha balance of the analytes only; no shift in the Boltzmann balance was observed experimentally. Moreover, for some ionic lines with sum of ionization and excitation potentials close to the ionization potential of argon (15.75 eV), the matrix effect is smaller than other ionic lines of the same element. The reduced matrix effects may be attributed qualitatively to charge transfer excitation mechanism of these ionic lines. Charge transfer reaction renders ionic emission lines from the quasi-resonant levels similar in characteristics of atomic lines. The contribution of charge transfer relative to excitation by other non-specific excitation mechanisms (via Saha balance and Boltzmann balance) determines the degree of atomic behavior of a quasi-resonant level. A significant conclusion of this study is that plasma-related matrix effect depends strongly on the excitation mechanism of a spectral line. Since, in general, more than one excitation mechanism may contribute to the overall excitation of an emission line, the observed matrix effects reflect the sum of the effects due to individual excitation mechanisms. Excitation mechanisms, in addition to the often-used total excitation energy, should be considered in matrix effect studies

  4. Plasma-cavity ringdown spectroscopy for analytical measurement: Progress and prospectives

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Sida; Liu, Wei [Research Center of Analytical Instrumentation, Analytical and Testing Center, College of Chemistry, Sichuan University, Chengdu (China); Zhang, Xiaohe [College of Water Resources and Hydropower, Sichuan University, Chengdu (China); Duan, Yixiang, E-mail: yduan@scu.edu.cn [Research Center of Analytical Instrumentation, Analytical and Testing Center, College of Chemistry, Sichuan University, Chengdu (China)

    2013-07-01

    Plasma-cavity ringdown spectroscopy is a powerful absorption technique for analytical measurement. It combines the inherent advantages of high sensitivity, absolute measurement, and relative insensitivity to light source intensity fluctuations of the cavity ringdown technique with use of plasma as an atomization/ionization source. In this review, we briefly describe the background and principles of plasma-cavity ringdown spectroscopy(CRDS) technology, the instrumental components, and various applications. The significant developments of the plasma sources, lasers, and cavity optics are illustrated. Analytical applications of plasma-CRDS for elemental detection and isotopic measurement in atomic spectrometry are outlined in this review. Plasma-CRDS is shown to have a promising future for various analytical applications, while some further efforts are still needed in fields such as cavity design, plasma source design, instrumental improvement and integration, as well as potential applications in radical and molecular measurements. - Highlights: • Plasma-based cavity ringdown spectroscopy • High sensitivity and high resolution • Elemental and isotopic measurements.

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

    International Nuclear Information System (INIS)

    Saito, Morimasa

    1994-01-01

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

  6. 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

  7. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    International Nuclear Information System (INIS)

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

    2005-01-01

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 deg. C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 deg. C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g -1

  8. Spring meeting of the scientific associations for atomic physics, high speed physics, mass spectrometry, molecular physics, plasma physics

    International Nuclear Information System (INIS)

    1996-01-01

    The volume contains the abstracts of the contributions to the Spring Meeting in Rostock with aspects of atomic physics, molecular physics, high speed physics, plasma physics and mass spectrometry. (MM)

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

    International Nuclear Information System (INIS)

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

    1975-01-01

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

  10. [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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Matos Reyes, M.N. [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain); Department of Chemistry, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente, 225, 22453-900, Rio de Janeiro, RJ (Brazil); Cervera, M.L. [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain)], E-mail: m.luisa.cervera@uv.es; Campos, R.C. [Department of Chemistry, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente, 225, 22453-900, Rio de Janeiro, RJ (Brazil); Guardia, M. de la [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain)

    2007-09-15

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

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

    Science.gov (United States)

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

    2017-09-01

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

  13. Test of atomic theory by photoelectron spectrometry with synchrotron radiation

    International Nuclear Information System (INIS)

    Krause, M.O.

    1984-01-01

    The successful combination of synchrotron radiation with electron spectrometry, accomplished at Daresbury, England and Orsay, France, made it possible to investigate sigma/sub x/ and β/sub x/ continuously over the very soft x-ray or the uv range of photon energies. The detailed and highly differentiated data resulting from this advanced experimentation put theory to a stringent test. In the interplay between theory and experiment, sophisticated Hartree Fock (HF) based models were developed which included both relativistic and many-electron effects. These theoretical models have provided us with a better insight than previously possible into the physics of the photon-atom interaction and the electronic structure and dynamics of atoms. However, critical experiments continue to be important for further improvements of theory. A number of such experiments are discussed in this presentation. The dynamic properties determined in these studies include in addition to sigma/sub x/ and β/sub x/ the spin polarization parameters. As a result the comparison between theory and experiment becomes rigorous, detailed and comprehensive. 46 references, 6 figures

  14. Determination of total antimony and inorganic antimony species by hydride generation in situ trapping flame atomic absorption spectrometry: a new way to (ultra)trace speciation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Henryk Matusiewicz; Magdalena Krawczyk

    2008-07-01

    The analytical performance of non-chromatographic coupled hydride generation, integrated atom trap (HG-IAT) atomizer flame absorption spectrometry (FAAS) systems were evaluated for the speciation analysis of antimony in environmental samples. Antimony, using formation of stibine (SbH{sub 3}) vapors were atomized in an air-acetylene flame-heated IAT. A new design of HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements was investigated. For the estimation of Sb(III) and Sb(V) concentrations in samples, the difference between the analytical sensitivities of the absorbance signals obtained for antimony hydride without and with previous treatment of samples with L-cysteine can be used. The concentration of Sb(V) was calculated by the difference between total Sb and Sb(III). A dramatic improvement in detection limit was achieved compared with that obtained using either of the atom trapping techniques, presented above, separately. This novel approach decreases the detection limit down to low pg mL{sup -1} levels. The concentration detection limit, defined as 3 times the blank standard deviation was 0.2 ng mL{sup -1}. For a 120 s in situ pre-concentration time , sensitivity enhancement compared to flame AAS, was 550 fold for Sb, using hydride generation-atom trapping technique. The accuracy of the method was verified by the use of certified reference materials (NIST SRM 2704 Buffalo River Sediment, SRM 2710 Montana Soil, SRM 1633a Coal Fly Ash, SRM 1575 Pine Needles, SRM 1643e Trace Elements in Water) and by aqueous standard calibration technique. The measured Sb content, in reference materials, were in satisfactory agreement with the certified values. The hyphenated technique was applied for antimony determinations in soil, sediment, coal fly ash, sewage and river water.

  15. 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

  16. 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.

  17. 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.

  18. 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

  19. Resonance Ionization Mass Spectrometry (RIMS): applications in spectroscopy and chemical dynamics

    International Nuclear Information System (INIS)

    Naik, P.D.; Kumar, Awadhesh; Upadhyaya, Hari; Bajaj, P.N.

    2009-01-01

    Resonance ionization is a photophysical process wherein electromagnetic radiation is used to ionize atoms, molecules, transient species, etc., by exciting them through their quantum states. The number of photons required to ionize depends on the species being investigated and energy of the photon. Once a charged particle is produced, it is easy to detect it with high efficiency. With the advent of narrow band high power pulsed and cw tunable dye lasers, it has blossomed into a powerful spectroscopic and analytical technique, commonly known as resonance ionization spectroscopy (RIS)/resonance enhanced multiphoton ionization (REMPI). The alliance of resonance ionization with mass spectrometry has grown into a still more powerful technique, known as resonance ionization mass spectrometry (RIMS), which has made significant contributions in a variety of frontier areas of research and development, such as spectroscopy, chemical dynamics, analytical chemistry, cluster science, surface science, radiochemistry, nuclear physics, biology, environmental science, material science, etc. In this article, we shall describe the application of resonance ionization mass spectrometry to spectroscopy of uranium and chemical dynamics of polyatomic molecules

  20. 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.)

  1. Electrochemical selenium hydride generation with in situ trapping in graphite tube atomizers

    Czech Academy of Sciences Publication Activity Database

    Šíma, Jan; Rychlovský, P.

    2003-01-01

    Roč. 58, č. 5 (2003), s. 919-930 ISSN 0584-8547 R&D Projects: GA ČR GA203/98/0754; GA ČR GA203/01/0453 Institutional research plan: CEZ:AV0Z4031919 Keywords : hydride generation * electrothermal atomic absorption spectrometry * In situ trapping Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.361, year: 2003

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

    International Nuclear Information System (INIS)

    Bings, N.H.; Orlandini von Niessen, J.O.; Schaper, J.N.

    2014-01-01

    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

  3. 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

  4. 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%

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  6. Performance of a liquid-junction interface for capillary electrophoresis mass spectrometry using continuous-flow fast-atom bombardment

    NARCIS (Netherlands)

    Reinhoud, N.J.; Niessen, W.M.A.; Tjaden, U.R.; Gramberg, L.G.; Verheij, E.R.; Greef, J. van der

    1989-01-01

    The on-line coupling of capillary electrophoresis and mass spectrometry using a continuous-flow fast-atom bombardment system in combination with a liquid-junction interface is described. The influence of the liquid-junction coupling on the efficiency and the resolution is investigated. Qualitative

  7. 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).

  8. 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).

  9. 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.

  10. Determination of caesium in river and sea waters by electrothermal atomic-absorption spectrometry. Interference of cobalt and iron

    International Nuclear Information System (INIS)

    Frigieri, P.; Trucco, R.; Ciaccolini, I.; Pampurini, G.

    1980-01-01

    For the enrichment or the simple recovery of caesium from river and sea waters, selective inorganic exchangers were considered. Ammonium hexacyanocobalt ferrate (NCFC) was chosen because it can be used in strongly acidic solutions (with the exception of concentrated sulphuric acid). Caesium is fully retained by the NCFC chromatographic column and can then be recovered by dissolution in hot sulphuric acid. The solution is then diluted and analysed, either directly or following caesium separation, by atomic-absorption spectrometry. To check the reliability of the analytical procedure, a series of experiments were carried out in which the possible interfering species were added to the aqueous caesium solution prior to analysis. The well known ionic interference in flame atomisation processes caused by magnesium, calcium, strontium and metals was investigated by electrothermal atomisation measurements. The experimental data showed that this effect does not occur even when these elements are present in concentrations of the order of thousands of parts per million. However, strong interferences from iron and cobalt were observed. (author)

  11. 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.

  12. High Precision Seawater Sr/Ca Measurements in the Florida Keys by Inductively Coupled Plasma Atomic Emission Spectrometry: Analytical Method and Implications for Coral Paleothermometry

    Science.gov (United States)

    Khare, A.; Kilbourne, K. H.; Schijf, J.

    2017-12-01

    Standard methods of reconstructing past sea surface temperatures (SSTs) with coral skeletal Sr/Ca ratios assume the seawater Sr/Ca ratio is constant. However, there is little data to support this assumption, in part because analytical techniques capable of determining seawater Sr/Ca with sufficient accuracy and precision are expensive and time consuming. We demonstrate a method to measure seawater Sr/Ca using inductively coupled plasma atomic emission spectrometry where we employ an intensity ratio calibration routine that reduces the self- matrix effects of calcium and cancels out the matrix effects that are common to both calcium and strontium. A seawater standard solution cross-calibrated with multiple instruments is used to correct for long-term instrument drift and any remnant matrix effects. The resulting method produces accurate seawater Sr/Ca determinations rapidly, inexpensively, and with a precision better than 0.2%. This method will make it easier for coral paleoclimatologists to quantify potentially problematic fluctuations in seawater Sr/Ca at their study locations. We apply our method to test for variability in surface seawater Sr/Ca along the Florida Keys Reef Tract. We are collecting winter and summer samples for two years in a grid with eleven nearshore to offshore transects across the reef, as well as continuous samples collected by osmotic pumps at four locations adjacent to our grid. Our initial analysis of the grid samples indicates a trend of decreasing Sr/Ca values offshore potentially due to a decreasing groundwater influence. The values differ by as much as 0.05 mmol/mol which could lead to an error of 1°C in mean SST reconstructions. Future work involves continued sampling in the Florida Keys to test for seasonal and interannual variability in seawater Sr/Ca, as well as collecting data from small reefs in the Virgin Islands to test the stability of seawater Sr/Ca under different geologic, hydrologic and hydrographic environments.

  13. THE STUDY OF HEAVY METAL FROM ENVIRONMENTAL SAMPLES BY ATOMIC TECHNIQUES

    Directory of Open Access Journals (Sweden)

    Ion V. POPESCU

    2011-05-01

    Full Text Available Using the Atomic Absorption Spectrometry (AAS and Energy Dispersive X-ray spectrometry (EDXRF techniques we analyzed the contents of heavy metals ( Cd, Cr, Ni, Pb, Ti, Sr, Co, Bi from eight wild mushrooms and soil substrate samples (48 samples of eight fungal species and 32 underlying soil samples, collected from ten forest sites of Dambovița County Romania. It was determined that the elements, especially heavy metals, in soil were characteristic of the acidic soils of the Romanian forest lands and are influenced by industrial pollution. Analytical possibilities of AAS and EDXRF analytical techniques have been compared and the heavy metal transfer from substrate to mushrooms has been studied. The coefficient of accumulation of essential and heavy metals has been calculated as well. Heavy metal contents of all analyzed mushrooms were generally higher than previously reported in literature.

  14. Study on solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent

    International Nuclear Information System (INIS)

    Yang Guangyu; Fen Weibo; Lei Chun; Xiao Weilie; Sun Handong

    2009-01-01

    A solid phase extraction and graphite furnace atomic absorption spectrometry (GFAAS) for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent was studied. Trace amounts of chromium, nickel, silver, cobalt, copper, cadmium and lead were reacted with 2-(2-quinolinil-azo)-4-methyl-1,3-dihydroxidobenzene (QAMDHB) followed by adsorption onto MCI GEL CHP 20Y solid phase extraction column, and 1.0 mol L -1 HNO 3 was used as eluent. The metal ions in 300 mL solution can be concentrated to 1.0 mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0 g of resin were greater than 95% without interference from alkaline, earth alkaline and some metal ions. When detected with graphite furnace atomic absorption spectrometry, the detection limits in the original samples were 1.4 ng L -1 for Cr(III), 1.0 ng L -1 for Ni(II), 0.85 ng L -1 for Ag(I), 1.2 ng L -1 for Co(II), 1.0 ng L -1 for Cu(II), 1.2 ng L -1 for Cd(II) and 1.3 ng L -1 for Pb(II). The validation of the procedure was performed by the analysis of the certified standard reference materials, and the presented procedure was applied to the determination of analytes in biological, water and soil samples with good results (recoveries range from 89 to 104%, and R.S.D.% lower than 3.2%. The results agreed with the standard value or reference method)

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

    Science.gov (United States)

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

    2006-06-01

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

  16. Comparison of the analytical methods used to determine natural and artificial radionuclides from environmental samples by gamma, alpha and beta spectrometry

    DEFF Research Database (Denmark)

    Pöllänen, Roy; Virtanen, Sinikka; Kämäräinen, Meerit

    In CAMNAR, an extensive interlaboratory exercise on the analytical methods used to determine several radionuclides present in the environmental samples was organized. Activity concentration of different natural radionuclides, such as Rn-222, Pb-210, Po-210, K-40, Ra-226, Ra-228 and isotopes...... of uranium, in addition to artificial Cs-137 and Am-241 were analysed from lake sediment samples and drinking water. The measurement techniques were gamma-ray spectrometry, alpha spectrometry, liquid scintillation counting and inductively coupled plasma mass spectrometry. Twenty six laboratories from nine...

  17. 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)

  18. 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.

  19. Analytic cross sections for collisions of H, H2, He and Li atoms and ions with atoms and molecules, 1

    International Nuclear Information System (INIS)

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

    1993-06-01

    Analytic expressions fitted to Barnett's recommended data are given for the cross sections of the following reactions: (1) electron capture by H, H + , H 2 + , He + , and He 2+ colliding with atoms, molecules, and ions and (2) electron capture into excited states by H + , He + , and He 2+ colliding with atoms and molecules. The latter category includes cross sections for photon emission due to electron capture. 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)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-08-01

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

  1. Mercury speciation in thawed out and refrozen fish samples by gas chromatography coupled to inductively coupled plasma mass spectrometry and atomic fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Krystek, Petra; Ritsema, Rob [National Institute for Public Health and the Environment (RIVM), Laboratory for Analytical Chemistry, Bilthoven (Netherlands)

    2005-01-01

    Different sub-sampling procedures were applied for the determination of mercury species (as total mercury Hg, methylmercury MeHg{sup +} and inorganic mercury Hg{sup 2+}) in frozen fish meat. Analyses were carried out by two different techniques. After the sample material was pre-treated by microwave digestion, atomic fluorescence spectroscopy (AFS) was used for the determination of total Hg. Speciation analysis was performed according to the following procedure: dissolution of sample material in tetramethylammonium hydroxide (TMAH), derivatisation with sodium tetraethylborate (NaBEt{sub 4}), extraction into isooctane and measurement with gas chromatography inductively coupled plasma mass spectrometry (GC-ICPMS) for the identification and quantification of methylmercury (MeHg{sup +}) and inorganic mercury (Hg{sup 2+}). The concentration range of total Hg measured in the shark fillets is between 0.9 and 3.6 {mu}g g{sup -1} thawed out shark fillet. Speciation analysis leads to {>=}94% Hg present as MeHg{sup +}. Homogeneity, storage conditions and stability of analytical species and sample materials have great influence on analytical results. Sub-sampling of half-frozen/partly thawed out fish and analysis lead to significantly different concentrations, which are on average a factor of two lower. (orig.)

  2. 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

  3. 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)

  4. Analytical chemistry instrumentation

    International Nuclear Information System (INIS)

    Laing, W.R.

    1986-01-01

    In nine sections, 48 chapters cover 1) analytical chemistry and the environment 2) environmental radiochemistry 3) automated instrumentation 4) advances in analytical mass spectrometry 5) fourier transform spectroscopy 6) analytical chemistry of plutonium 7) nuclear analytical chemistry 8) chemometrics and 9) nuclear fuel technology

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

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Xianjuan [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Gan Wuer, E-mail: wgan@ustc.edu.cn [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Wan Lingzhong; Deng Yun; Yang Qinghua; He Youzhao [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China)

    2010-12-15

    An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH{sub 4} and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL{sup -1} (3{sigma}) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL{sup -1} Sn(IV) standard solution.

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

    International Nuclear Information System (INIS)

    Naeemullah, A.; Kazi, T.G.

    2011-01-01

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

  7. Determination of trace elements in maifanite by outer cover electrode atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    LI Jianqiang; LU Yiqiang; JIANG Wei

    2005-01-01

    Maifanite is a nature medicinal stone used in many fields for long time. The research on it showed that there are many trace elements in maifanite. In this paper, 36 trace elements in maifanite were determined by outer cover electrode atomic emission spectrometry, and the determination conditions were studied systematically. The results show that the concentrafions of elements, which are beneficial to human health, are higher, and the elements harmful to people health such as As, Cd, Hg, Cr, and Pb are tiny in maifanite. The precision and the accuracy were also discussed.

  8. The determination of long life radionuclides by means of sector field ICP mass spectrometry

    International Nuclear Information System (INIS)

    Kerl, W.; Becker, J.S.; Dietze, H.J.; Dannecker, W.

    1996-01-01

    Different analytical processes for determining long life radionuclides by means of double-focussing sector field ICP mass spectrometry are described. In determining long life radionuclides by means of ICP-MS, on the one hand the analytical problem areas are in the interference of isobaric atom or molecule ions (eg: 151 Eu + - 151 Sm + , 79 Se + - 39 Ar 40 ArH + ) and on the other hand in the high detection limits when using commercial sample introduction systems (eg: For 129 I). An online coupling of HPLC and ICP-MS was built up for the separation of isobaric atom ions and was tested for the separation of isobaric atom ions and was tested for its efficiency in the separation of lanthanides. Special sample introduction systems for ICP-MS were developed for the analysis of 129 I, by which the sensitivity of detection can be appreciably improved compared to commercial sample introduction systems. (orig.) [de

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

    International Nuclear Information System (INIS)

    Capdevila, C.; Alduan, F.A.

    1980-01-01

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

  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. Mass spectrometry at the Pittsburgh conference

    International Nuclear Information System (INIS)

    Borman, S.

    1987-01-01

    Each year analytical chemists flock to the Pittsburgh Conference to learn about the latest trends in analytical instrumentation. In this Focus, a number of prominent mass spectroscopists who attended this year's meeting in Atlantic City, NJ, discuss their perceptions of current developments in the field of mass spectrometry (MS). In the June 1 issue of Analytical Chemistry, the authors coverage of the Pittsburgh Conferences continues with a follow-up article on specific developments in hyphenated mass spectrometry - primarily liquid chromatography - MS (LC/MS) and gas chromatography - infrared spectrometry MS (GC/IR/MS)

  13. 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.

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

    International Nuclear Information System (INIS)

    Bye, R.

    1986-01-01

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

  15. [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.

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

    Science.gov (United States)

    Jiang, Xianjuan; Gan, Wuer; Wan, Lingzhong; Deng, Yun; Yang, Qinghua; He, Youzhao

    2010-12-15

    An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH(4) and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL(-1) (3σ) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL(-1) Sn(IV) standard solution. Copyright © 2010 Elsevier B.V. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Alves Flávia L.

    2000-01-01

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

  18. 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.

  19. Macro elemental analysis of food samples by nuclear analytical technique

    Science.gov (United States)

    Syahfitri, W. Y. N.; Kurniawati, S.; Adventini, N.; Damastuti, E.; Lestiani, D. D.

    2017-06-01

    Energy-dispersive X-ray fluorescence (EDXRF) spectrometry is a non-destructive, rapid, multi elemental, accurate, and environment friendly analysis compared with other detection methods. Thus, EDXRF spectrometry is applicable for food inspection. The macro elements calcium and potassium constitute important nutrients required by the human body for optimal physiological functions. Therefore, the determination of Ca and K content in various foods needs to be done. The aim of this work is to demonstrate the applicability of EDXRF for food analysis. The analytical performance of non-destructive EDXRF was compared with other analytical techniques; neutron activation analysis and atomic absorption spectrometry. Comparison of methods performed as cross checking results of the analysis and to overcome the limitations of the three methods. Analysis results showed that Ca found in food using EDXRF and AAS were not significantly different with p-value 0.9687, whereas p-value of K between EDXRF and NAA is 0.6575. The correlation between those results was also examined. The Pearson correlations for Ca and K were 0.9871 and 0.9558, respectively. Method validation using SRM NIST 1548a Typical Diet was also applied. The results showed good agreement between methods; therefore EDXRF method can be used as an alternative method for the determination of Ca and K in food samples.

  20. Time-resolved X-ray scattering by electronic wave packets: analytic solutions to the hydrogen atom

    DEFF Research Database (Denmark)

    Simmermacher, Mats; Henriksen, Niels Engholm; Møller, Klaus Braagaard

    2017-01-01

    Modern pulsed X-ray sources permit time-dependent measurements of dynamical changes in atoms and molecules via non-resonant scattering. The planning, analysis, and interpretation of such experiments, however, require a firm and elaborated theoretical framework. This paper provides a detailed...... description of time-resolved X-ray scattering by non-stationary electronic wave packets in atomic systems. A consistent application of the Waller-Hartree approximation is discussed and different contributions to the total differential scattering signal are identified and interpreted. Moreover......, it is demonstrated how the scattering signal of wave packets in the hydrogen atom can be expressed analytically. This permits simulations without numerical integration and establishes a benchmark for both efficiency and accuracy. Based on that, scattering patterns of an exemplary wave packet in the hydrogen atom...

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

    Energy Technology Data Exchange (ETDEWEB)

    Solis A, N. A.

    2015-07-01

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

  2. New analytical methodology to reach the actinide determination accuracy ({+-} 2%) required by the OSMOSE program

    Energy Technology Data Exchange (ETDEWEB)

    Boyer-Deslys, V.; Combaluzier, T.; Dalier, V.; Martin, J.C.; Viallesoubranne, C. [DRCP/SE2A/LAMM, CEA/VALRHO - Marcoule, BP 17171, 30207 Bagnols-sur-Ceze (France); Crozet, M. [LEHA, CEA/VALRHO - Marcoule, BP 17171, 30207 Bagnols-sur-Ceze (France)

    2008-07-01

    This article describes the analytical procedure optimized by LAMM (Laboratory for Analysis and Materials Methodology) in order to characterize the actinide-doped pellets used in the Osmose (Oscillation in Minerve of isotopes in eupraxis spectra) program (developed for transmutation reactor physics). Osmose aims at providing precise experimental data (absorption cross sections) for heavy nuclides (atomic mass from 232 to 245). This procedure requires the use of the analytical equipment and expertise of the LAMM: TIMS (Thermal Ionization Mass Spectrometer), ICP (Inductively Coupled Plasma) QMS (Quadrupole Mass Spectrometer), SFMS (Sector Field Mass Spectrometer), AES (Atomic Emission Spectrometer), alpha spectrometry and photo-gravimetric analysis. These techniques have met all the specification requirements: extended uncertainties (k=2) below {+-} 2% on the uranium and dopant concentrations, the impurity concentration and the americium-241 concentration.

  3. 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)

  4. Matrix modifiers application during microimpurities determination in complex samples by electrothermal atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Bejzel', N.F.; Daaman, F.I.; Fuks-Pol', G.R.; Yudelevich, I.G.

    1993-01-01

    The review covers publications of primarily last 5 years and is devoted to the use of matrix modifiers (MM) for the determinations of trace impurities in complex samples by electrothermal atomic-absorption analysis. The role of MM in analytical process has been discussed as well as MM influence on all the elements of analytical system; factors, determining the effectiveness of MM action, the basis types of MM have been described. A great body of information is tabulated on the use of different MM for the determination of particular analysis in geological, medicobiological, technological, ecological samples and in pure materials and chemicals

  5. Matrix modification for determination of microimpurities in complex samples by electrothermal atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Bejzel', N.F.; Daaman, F.I.; Fuks-Pol', G.R.; Yudelevich, I.G.

    1993-01-01

    The review covers publications of primarily last 5 years and is devoted to the use of matrix modifiers (MM) for the determinations of trace impurities in complex samples by electrothermal atomic-absorption analysis. The role of MM in analytical process has been discussed as well as MM influence on all the elements of analytical system; factors, determining the effectiveness of MM action, the basis types of MM have been described. A great body of information is tabulated on the use of different MM for the determination of particular analysis in geological, medicobiological, technological, ecological samples and in pure materials and chemicals

  6. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, Ignacio; Briceno, Marisol [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, Manuel, E-mail: hcordoba@um.es [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain)

    2011-08-05

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

  8. Simultaneous determination of cadmium, iron and tin in canned foods using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Leao, Danilo J; Junior, Mario M S; Brandao, Geovani C; Ferreira, Sergio L C

    2016-06-01

    A method was established to simultaneously determine cadmium, iron and tin in canned-food samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). The quantification step has been performed using the primary line (228.802nm) for cadmium and the adjacent secondary lines (228.725nm and 228.668nm) for iron and tin, respectively. The selected chemical modifier was an acid solution that contained a mixture of 0.1% (w/v) Pd and 0.05% (w/v) Mg. The absorbance signals were measured based on the peak area using 3 pixels for cadmium and 5 pixels for iron and tin. Under these conditions, cadmium, iron and tin have been determined in canned-food samples using the external calibration technique based on aqueous standards, where the limits of quantification were 2.10ngg(-1) for cadmium, 1.95mgkg(-1) for iron and 3.00mgkg(-1) for tin, and the characteristic masses were 1.0pg for cadmium, 0.9ng for iron and 1.1ng for tin. The precision was evaluated using two solutions of each metal ion, and the results, which were expressed as the relative standard deviation (RSD%), were 3.4-6.8%. The method accuracy for cadmium and iron was confirmed by analyzing a certified reference material of apple leaves (NIST 1515), which was supplied by NIST. However, for tin, the accuracy was confirmed by comparing the results of the proposed method and another analytical technique (inductively coupled plasma optical emission spectrometry). The proposed procedure was applied to determine cadmium, iron and tin in canned samples of peeled tomato and sardine. Eleven samples were analyzed, and the analyte concentrations were 3.57-62.9ngg(-1), 2.68-31.48mgkg(-1) and 4.06-122.0mgkg(-1) for cadmium, iron and tin, respectively. In all analyzed samples, the cadmium and tin contents were lower than the permissible maximum levels for these metals in canned foods in the Brazilian legislation. Copyright © 2016. Published by Elsevier B.V.

  9. 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.

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

    International Nuclear Information System (INIS)

    Shimizu, Tokuo; Shijo, Yoshio; Sakai, Kaoru

    1981-01-01

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

  11. 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

  12. 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)

  13. 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

    Energy Technology Data Exchange (ETDEWEB)

    Petrova, P.; Velichkov, S. [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria); Velitchkova, N. [Geological Institute, Bulgarian Academy of Sciences, Acad. G. Bontchev Str., bl.24, 1113 Sofia (Bulgaria); Havezov, I. [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria); Daskalova, N., E-mail: das15482@svr.igic.bas.b [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria)

    2010-02-15

    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{sup -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.

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

    OpenAIRE

    NUKATSUKA, Isoshi; OHZEKI, Kunio

    2006-01-01

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

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

    DEFF Research Database (Denmark)

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

    1986-01-01

    A procedure is described for the direct determination of zinc in human serum by fully automated, microcomputer controlled flow injection atomic absorption spectrometry (Fl-AAS). The Fl system is pumpless, using the negative pressure created by the nebuliser. It only consists of a three-way valve......, programmable from the microcomputer, to control the sample volume. No pre-treatment of the samples is necessary. The limit of detection is 0.14 mg l–1, and only small amounts of serum (

  16. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    International Nuclear Information System (INIS)

    Herrero Latorre, C.; Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R.M.

    2012-01-01

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes – due to their high adsorption and desorption capacities – have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  17. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-07-01

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

  19. 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

  20. An appraisal of neutron activation analysis and other analytical techniques for the determination of arsenic, selenium and tin in environmental samples

    International Nuclear Information System (INIS)

    Peterson, P.J.; Girling, C.A.; Klumpp, D.W.; Minski, M.J.

    1979-01-01

    The paper presents an experimental comparison between neutron activation analysis, atomic absorption spectrophotometry and fluorescence spectrophotometry used for the determination of trace amounts of As, Se and Sn and the other two analytical techniques mentioned. Gamma-ray spectrometry has been used to determine 76 As (tsub(1/2)=26.3 h) after 1 day's irradiation at a thermal neutron flux of 1.6x10 12 n.cm -2 .s -1 . High sensitivity was also obtained using an atomic absorption spectrophotometer coupled with covalent hydride generation. Advantages of the latter technique include simplicity of operation, high speed of analysis and negligible background correction. When used in conjuction with selective reduction and a cold-trap this method quantitatively distinguishes between the valence states and some methylated derivatives. Selenium has been analysed by gamma-ray spectrometry using 77 Sesup(m) (tsub(1/2)=17.5 s) after cyclic activation at a thermal neutron flux of 2x10 12 n.cm -2 .s -1 . Atomic absorption spectrophotometry following hydride generation, or fluorescence spectrophotometry of the 2,3 diaminonaphthalene complex constitute additional sensitive analytical methods for the determination of Se. These have the added advantage that valence states can be selectively measured. Low concentrations of Sn have been determined by neutron activation analysis and by spectrophotometric techniques using phenylfluorone as the complexing reagent, but these methods depend on selective extraction of Sn(IV) iodide. Whilst maintaining high sensitivity, these problems were avoided by using the hydride generation technique with an atomic absorption spectrophotometer. Comparative analytical values for Bowen's kale and NBS orchard leaves are presented

  1. 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

  2. Experimental evidence of state-selective charge transfer in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

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

    2004-01-01

    State-selective charge-transfer behavior was observed for Fe, Cr, Mn and Cu in inductively coupled plasma (ICP)-atomic emission spectrometry. Charge transfer from Ar + to Fe, Cr and Mn is state-selective because of inefficient collisional mixing of the quasiresonant charge-transfer energy levels with nearby levels. This low efficiency is the consequence of differences in electronic configuration of the core electrons. The reason for state-selective charge-transfer behavior to Cu is not clear, although a tentative explanation based on efficiency of intramultiplet and intermultiplet mixing for this special case is offered

  3. An Investigation on the Extraction and Quantitation of a Hexavalent Chromium in Acrylonitrile Butadiene Styrene Copolymer (ABS) and Printed Circuit Board (PCB) by Ion Chromatography Coupled with Inductively Coupled Plasma Atomic Emission Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Sang Ho; Kim, Yu Na [Mokpo National University, Muan (Korea, Republic of)

    2012-06-15

    A hexavalent chromium (Cr (VI)) is one of the hazardous substances regulated by the RoHS. The determination of Cr (VI) in various polymers and printed circuit board (PCB) has been very important. In this study, the three different analytical methods were investigated for the determination of a hexavalent chromium in Acrylonitrile Butadiene Styrene copolymer (ABS) and PCB. The results by three analytical methods were obtained and compared. An analytical method by UV-Visible spectrometer has been generally used for the determination of Cr (VI) in a sample, but a hexavalent chromium should complex with diphenylcarbazide for the detection in the method. The complexation did make an adverse effect on the quantitative analysis of Cr (VI) in ABS. The analytical method using diphenylcarbazide was also not applicable to printed circuit board (PCB) because PCB contained lots of irons. The irons interfered with the analysis of hexavalent chromium because those also could complex with diphenylcarbazide. In this study, hexavalent chromiums in PCB have been separated by ion chromatography (IC), then directly and selectively detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantity of Cr (VI) in PCB was 0.1 mg/kg

  4. Improving the analytical performance and versatility of paper spray mass spectrometry via paper microfluidics.

    Science.gov (United States)

    Murray, Ian; Walker, Glenn; Bereman, Michael S

    2016-06-20

    Two paper-based microfluidic techniques, photolithography and wax patterning, were investigated for their potential to improve upon the sensitivity, reproducibility, and versatility of paper spray mass spectrometry. The main limitation of photolithography was the significant signal (approximately three orders of magnitude) above background which was attributed to the chemicals used in the photoresist process. Hydrophobic barriers created via wax patterning were discovered to have approximately 2 orders of magnitude less background signal compared to analogous barriers created using photolithography. A minimum printed wax barrier thickness of approximately 0.3 mm was necessary to consistently retain commonly used paper spray solvents (1 : 1 water : acetonitrile/methanol) and avoid leakage. Constricting capillary flow via wax-printed channels yielded both a significant increase in signal and detection time for detection of model analytes. This signal increase, which was attributed to restricting the radial flow of analyte/solvent on paper (i.e., a concentrating effect), afforded a significant increase in sensitivity (p ≪ 0.05) for the detection of pesticides spiked into residential tap water using a five-point calibration curve. Finally, unique mixing designs using wax patterning can be envisioned to perform on-paper analyte derivatization.

  5. Advances in atomic spectroscopy

    CERN Document Server

    Sneddon, J

    2000-01-01

    This fifth volume of the successful series Advances in Atomic Spectroscopy continues to discuss and investigate the area of atomic spectroscopy.It begins with a description of the use of various atomic spectroscopic methods and applications of speciation studies in atomic spectroscopy. The emphasis is on combining atomic spectroscopy with gas and liquid chromatography. In chapter two the authors describe new developments in tunable lasers and the impact they will have on atomic spectroscopy. The traditional methods of detection, such as photography and the photomultiplier, and how they are being replaced by new detectors is discussed in chapter three. The very active area of glow discharge atomic spectrometry is presented in chapter four where, after a brief introduction and historical review, the use of glow discharge lamps for atomic spectroscopy and mass spectrometry are discussed. Included in this discussion is geometry and radiofrequency power. The future of this source in atomic spectroscopy is also dis...

  6. Utilization of electrodeposition for electrothermal atomic absorption spectrometry determination of gold

    International Nuclear Information System (INIS)

    Konecna, Marie; Komarek, Josef

    2007-01-01

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

  7. Silver nanostructures in laser desorption/ionization mass spectrometry and mass spectrometry imaging.

    Science.gov (United States)

    Sekuła, Justyna; Nizioł, Joanna; Rode, Wojciech; Ruman, Tomasz

    2015-09-21

    Silver nanoparticles have been successfully applied as a matrix replacement for the laser desorption/ionization time-of-flight mass spectrometry (LDI-ToF-MS). Nanoparticles, producing spectra with highly reduced chemical background in the low m/z region, are perfectly suited for low-molecular weight compound analysis and imaging. Silver nanoparticles (AgNPs) can efficiently absorb ultraviolet laser radiation, transfer energy to the analyte and promote analyte desorption, but also constitute a source of silver ions suitable for analyte cationisation. This review provides an overview of the literature on silver nanomaterials as non-conventional desorption and ionization promoters in LDI-MS and mass spectrometry imaging.

  8. Recent advances in analytical determination of cisplatin and its hydrolysis products

    International Nuclear Information System (INIS)

    Ramos Rodriguez, Yalexmiy; Hernandez Castro, Carlos

    2009-01-01

    Cisplatin (cis-diaminedichloroplatinum [II] is a coordination compound, used in the treatment of several solid tumors. Cisplatin and its hydrolysis products exhibit a great pharmacological effect but are very toxic and probably carcinogenic. The present review summarizes the most important advances in the last years in the techniques employed for the detection and quantification of cisplatin and its hydrolysis products and in the different matrixes studied. The new emerging techniques and their modifications recently developed, fundamentally the combined use of detection and separation techniques for the analysis of platinum species and their impact on the speed, sensitivity and specificity of the analytical determination, with regard to the techniques used in the last century are discussed. High-Performance Liquid Chromatography and Capillary Electrophoresis, coupled with detection methods such as Mass Spectrometry, Inductively Coupled Plasma-Mass Spectrometry, Atomic Absorption Spectrometry and more recently, High-Field Asymmetric Waveform Ion Mobility Spectrometry are the methods more employed. The analysis of cisplatin and its hydrolysis products in new and more complex matrixes is also presented

  9. Analytical chemistry of actinides

    International Nuclear Information System (INIS)

    Chollet, H.; Marty, P.

    2001-01-01

    Different characterization methods specifically applied to the actinides are presented in this review such as ICP/OES (inductively coupled plasma-optical emission spectrometry), ICP/MS (inductively coupled plasma spectroscopy-mass spectrometry), TIMS (thermal ionization-mass spectrometry) and GD/OES (flow discharge optical emission). Molecular absorption spectrometry and capillary electrophoresis are also available to complete the excellent range of analytical tools at our disposal. (authors)

  10. Rapid determination of {sup 135}Cs and precise {sup 135}Cs/{sup 137}Cs atomic ratio in environmental samples by single-column chromatography coupled to triple-quadrupole inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Guosheng [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori 036-8564 (Japan); Division of Nuclear Technology and Applications, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Beijing Engineering Research Center of Radiographic Techniques and Equipment, Beijing 100049 (China); Tazoe, Hirofumi [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori 036-8564 (Japan); Yamada, Masatoshi, E-mail: myamada@hirosaki-u.ac.jp [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori 036-8564 (Japan)

    2016-02-18

    For source identification, measurement of {sup 135}Cs/{sup 137}Cs atomic ratio not only provides information apart from the detection of {sup 134}Cs and {sup 137}Cs, but it can also overcome the application limit that measurement of the {sup 134}Cs/{sup 137}Cs ratio has due to the short half-life of {sup 134}Cs (2.06 y). With the recent advancement of ICP-MS, it is necessary to improve the corresponding separation method for rapid and precise {sup 135}Cs/{sup 137}Cs atomic ratio analysis. A novel separation and purification technique was developed for the new generation of triple-quadrupole inductively coupled plasma-mass spectrometry (ICP-MS/MS). The simple chemical separation, incorporating ammonium molybdophosphate selective adsorption of Cs and subsequent single cation-exchange chromatography, removes the majority of isobaric and polyatomic interference elements. Subsequently, the ICP-MS/MS removes residual interference elements and eliminates the peak tailing effect of stable {sup 133}Cs, at m/z 134, 135, and 137. The developed analytical method was successfully applied to measure {sup 135}Cs/{sup 137}Cs atomic ratios and {sup 135}Cs activities in environmental samples (soil and sediment) for radiocesium source identification. - Highlights: • A simple {sup 135}Cs/{sup 137}Cs analytical method was developed. • The separation procedure was based on AMP adsorption and one column chromatography. • {sup 135}Cs/{sup 137}Cs was measured by ICP-MS/MS. • Decontamination factors for Ba, Mo, Sb, and Sn were improved. • {sup 135}Cs/{sup 137}Cs atomic ratios of 0.341–0.351 were found in Japanese soil samples.

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

    International Nuclear Information System (INIS)

    Niedzielski, P.

    2005-01-01

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

  12. 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.

  13. 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.

  14. Zeeman atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Hadeishi, T.; McLaughlin, R.

    1978-08-01

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

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

    OpenAIRE

    Ensafi, Ali A.; Shiraz, Ameneh Zendegi

    2008-01-01

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

  16. [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.

  17. Comparison in the analytical performance between krypton and argon glow discharge plasmas as the excitation source for atomic emission spectrometry.

    Science.gov (United States)

    Wagatsuma, Kazuaki

    2009-04-01

    The emission characteristics of ionic lines of nickel, cobalt, and vanadium were investigated when argon or krypton was employed as the plasma gas in glow discharge optical emission spectrometry. A dc Grimm-style lamp was employed as the excitation source. Detection limits of the ionic lines in each iron-matrix alloy sample were compared between the krypton and the argon plasmas. Particular intense ionic lines were observed in the emission spectra as a function of the discharge gas (krypton or argon), such as the Co II 258.033 nm for krypton and the Co II 231.707 nm for argon. The explanation for this is that collisions with the plasma gases dominantly populate particular excited levels of cobalt ion, which can receive the internal energy from each gas ion selectively, for example, the 3d(7)4p (3)G(5) (6.0201 eV) for krypton and the 3d(7)4p (3)G(4) (8.0779 eV) for argon. In the determination of nickel as well as cobalt in iron-matrix samples, more sensitive ionic lines could be found in the krypton plasma rather than the argon plasma. Detection limits in the krypton plasma were 0.0039 mass% Ni for the Ni II 230.299-nm line and 0.002 mass% Co for the Co II 258.033-nm line. However, in the determination of vanadium, the argon plasma had better analytical performance, giving a detection limit of 0.0023 mass% V for the V II 309.310-nm line.

  18. Cu,Cr and As determination in preserved woods (Eucalyptus ssp.) by X-ray fluorescence spectrometries; Determinacao de cobre, cromo e arsenio em madeira preservada (Eucalyptus sp.) pelas espectrometrias de fluorescencia de raios X

    Energy Technology Data Exchange (ETDEWEB)

    Pereira Junior, Sergio Matias

    2014-07-01

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

  19. Electrochemically assisted fast-atom-bombardment mass spectrometry

    International Nuclear Information System (INIS)

    Phillips, L.R.

    1988-01-01

    The hybridization of electrochemistry and fast atom bombardment (FAB) mass spectrometry (MS) creates a new hyphenated technique, referred to as electrochemically assisted FAB (EFAB) MS, which improves the applicability of FAB MS in selectivity and extends the range of compounds to include low polarity molecules, and also reduces mass spectral complications due to matrix-related artifacts. FAB MS has proven to be indispensable in analysis of samples that are otherwise too intractable for conventional MS, such as peptides, oligosaccharides, and oligonucleotides, due to low volatility and ready thermal degradation. There are limits on its applicability, however, in that it works best with samples that are already ionic, or predisposed to become so by simple proton transfer to or from the matrix. A wide range of chemical substances can be ionized/analyzed by electrochemical methods. Therefore, a possible approach towards improving applicability of FAB MS is through its hybridization with electrochemistry. Samples are activated by electrolysis, carried out directly in the sample matrix through use of a modified FAB sample probe which was constructed containing a small electrolytic cell on the tip. In operation, one electrode is held at normal sample-probe/ion-source voltage, while the other electrode can be continuously varied ±15 volts to create electrochemical potentials. Several chemical substances, known to be unresponsive to FAB MS, have been examined by EFAB MS. Resultant spectra generally show a dramatic increases in signal/chemical noise ratio of structurally significant ions when compared to normal FAB spectra

  20. 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…

  1. 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

  2. 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)

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

    Science.gov (United States)

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

    2015-12-01

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

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

    Directory of Open Access Journals (Sweden)

    SIMONA MURKO

    2010-01-01

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

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

    Science.gov (United States)

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

    2018-06-01

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

  6. 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)

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-01

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

  9. 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.

  10. 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.

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

    International Nuclear Information System (INIS)

    Elhag, A. Y.

    2004-01-01

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

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

    International Nuclear Information System (INIS)

    Cheung, Yan; Schwartz, Andrew J.; Chan, George C.-Y.; Hieftje, Gary M.

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Cheung, Yan; Schwartz, Andrew J.; Chan, George C.-Y.; Hieftje, Gary M., E-mail: hieftje@indiana.edu

    2015-08-01

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

  14. Quenching of the OH and nitrogen molecular emission by methane addition in an Ar capacitively coupled plasma to remove spectral interference in lead determination by atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Frentiu, T., E-mail: ftibi@chem.ubbcluj.r [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Ponta, M., E-mail: mponta@chem.ubbcluj.r [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Mihaltan, A.I., E-mail: alinblaj2005@yahoo.co [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania); Darvasi, E., E-mail: edarvasi@chem.ubbcluj.r [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Frentiu, M., E-mail: frentiu.maria@yahoo.co [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania); Cordos, E., E-mail: emilcordos@gmail.co [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania)

    2010-07-15

    A new method is proposed to remove the spectral interference on elements in atomic fluorescence spectrometry by quenching of the molecular emission of the OH radical (A{sup 2{Sigma}+} {yields} X{sup 2{Pi}}) and N{sub 2} second positive system (C{sup 3{Pi}}{sub u} {yields} B{sup 3{Sigma}}{sub g}) in the background spectrum of medium power Ar plasmas. The experiments were carried out in a radiofrequency capacitively coupled plasma (275 W, 27.12 MHz) by CH{sub 4} addition. The quenching is the result of the high affinity of OH radical for a hydrogen atom from the CH{sub 4} molecule and the collisions of the second kind between nitrogen excited molecules and CH{sub 4}, respectively. The decrease of the emission of N{sub 2} second positive system in the presence of CH{sub 4} is also the result of the deactivation of the metastable argon atoms that could excite the nitrogen molecules. For flow rates of 0.7 l min{sup -1} Ar with addition of 7.5 ml min{sup -1} CH{sub 4}, the molecular emission of OH and N{sub 2} was completely removed from the plasma jet spectrum at viewing heights above 60 mm. The molecular emission associated to CH and CH{sub 2} species was not observed in the emission spectrum of Ar/CH{sub 4} plasma in the ultraviolet range. The method was experimented for the determination of Pb at 283.31 nm by atomic fluorescence spectrometry with electrodeless discharge lamp and a multichannel microspectrometer. The detection limit was 35 ng ml{sup -1}, 2-3 times better than in atomic emission spectrometry using the same plasma source, and similar to that in hollow cathode lamp microwave plasma torch atomic fluorescence spectrometry.

  15. Preconcentration and determination of zinc and lead ions by a combination of cloud point extraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tavallali, H. [Chemistry Department, Payamenore University, Shiraz (Iran); Shokrollahi, A.; Zahedi, M. [Chemistry Department, Yasouj University, Yasouj (Iran); Niknam, K. [Chemistry Department, Persian Gulf University, Bushehr (Iran); Soylak, M. [Chemistry Department, University of Erciyes, Kayseri (Turkey); Ghaedi, M.

    2009-04-15

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of lead(II) and zinc(II). After complexation with 3-[(4-bromophenyl) (1-H-inden-3-yl)methyl]-1 H-indene (BPIMI), the analytes were quantitatively extracted to a phase rich in Triton X-114 after centrifugation. Methanol acidified with 1 mol/L HNO{sub 3} was added to the surfactant rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of bis((1H-benzo [d] imidazol-2yl)ethyl)sulfane, Triton X-114, pH and amount of surfactant were all optimized. Detection limits (3 SDb/m) of 2.5 and 1.6 ng/mL for Pb{sup 2+} and Zn{sup 2+} along with preconcentration factors of 30 and an enrichment factor of 32 and 48 for Pb{sup 2+}and Zn {sup 2+} ions were obtained, respectively. The proposed cloud point extraction was been successfully applied for the determination of these ions in real samples with complicated matrices such as food and soil samples, with high efficiency. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  16. 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.)

  17. 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.

  18. 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…

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-09-15

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

  1. Weak-field asymptotic theory of tunneling ionization: benchmark analytical results for two-electron atoms

    International Nuclear Information System (INIS)

    Trinh, Vinh H; Morishita, Toru; Tolstikhin, Oleg I

    2015-01-01

    The recently developed many-electron weak-field asymptotic theory of tunneling ionization of atoms and molecules in an external static electric field (Tolstikhin et al 2014, Phys. Rev. A 89, 013421) is extended to the first-order terms in the asymptotic expansion in field. To highlight the results, here we present a simple analytical formula giving the rate of tunneling ionization of two-electron atoms H − and He. Comparison with fully-correlated ab initio calculations available for these systems shows that the first-order theory works quantitatively in a wide range of fields up to the onset of over-the-barrier ionization and hence is expected to find numerous applications in strong-field physics. (fast track communication)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  4. Role of Mass Spectrometry in Clinical Endocrinology.

    Science.gov (United States)

    Ketha, Siva S; Singh, Ravinder J; Ketha, Hemamalini

    2017-09-01

    The advent of mass spectrometry into the clinical laboratory has led to an improvement in clinical management of several endocrine diseases. Liquid chromatography tandem mass spectrometry found some of its first clinical applications in the diagnosis of inborn errors of metabolism, in quantitative steroid analysis, and in drug analysis laboratories. Mass spectrometry assays offer analytical sensitivity and specificity that is superior to immunoassays for many analytes. This article highlights several areas of clinical endocrinology that have witnessed the use of liquid chromatography tandem mass spectrometry to improve clinical outcomes. Copyright © 2017 Elsevier Inc. All rights reserved.

  5. Evaluation of V, Ir, Ru, V-Ir, V-Ru, and W-V as permanent chemical modifiers for the determination of cadmium, lead, and zinc in botanic and biological slurries by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Acar, Orhan

    2005-01-01

    Permanent modifiers (V, Ir, Ru, V-Ir, V-Ru, and W-V) thermally coated on to platforms of pyrolytic graphite tubes were employed for the determination of Cd, Pb, and Zn in botanic and biological slurries by electrothermal atomic absorption spectrometry (ETAAS). Conventional Pd + Mg(NO 3 ) 2 modifier mixture was also used for the determination of analytes in slurries and digested samples. Optimum masses and mass ratios of permanent modifiers for Cd, Pb, and Zn in slurry sample solutions were investigated. The 280 μg of V, 280 μg of V + 200 μg of Ir, 280 μg of V + 200 μg of Ru or 240 μg of W + 280 μg of V in 0.2% (v/v) Triton X-100 plus 0.5% (v/v) HNO 3 mixture was found as efficient as 5 μg of Pd + 3 μg of Mg(NO 3 ) 2 modifier mixture for obtaining thermal stabilization, and for obtaining best recoveries. Optimization conditions of analytes, such as pyrolysis and atomization temperature, characteristic masses and detection limits, and atomization and background peak profiles were studied with permanent and 5 μg of Pd + 3 μg of Mg(NO 3 ) 2 conventional modifiers and compared with each other. The permanent V-Ir, V-Ru, and W-V modifiers remained stable for approximately 250-300 firings when 20 μl of slurries and digested samples were delivered into the atomizer. In addition, the mixed permanent modifiers increase the tube lifetime by 50-95% when compared with untreated platforms. The characteristic masses and detection limits of analytes (dilution factor of 125 ml g -1 ) obtained with V-Ir based on integrated absorbance as example for 0.8% (m/v) slurries were 1.0 pg and 3 ng g -1 for Cd, 18 pg and 17 ng g -1 for Pb, and 0.7 pg and 4 ng g -1 for Zn, respectively. The results of analytes obtained by employing V-Ir, V-Ru, and W-V permanent modifier mixtures in botanic and biological certified and standard reference materials were in agreement with the certified values of reference materials

  6. 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

  7. Flame emission spectrometry using atomic absorption apparatus. I. Determination of Sr in sea water

    International Nuclear Information System (INIS)

    Aizawa, S.; Yoshimura, E.; Hamachi, M.; Haraguchi, H.; Dokiya, Y.; Fuwa, K.

    1976-01-01

    Flame emission determination of Sr in seawater was studied using an ordinary atomic absorption apparatus. The analytical line 4607 A was used with a background correction at 4616 A. The ionization was negligible in an air acetylene flame with seawater, and the interference of H 2 SO 4 was eliminated using the higher part of the flame. Sr concentration of seawater of Tokyo Bay and Sagami Bay has been determined

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  9. 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.

  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. Analytical Chemistry Division annual progress report for period ending December 31, 1990

    Energy Technology Data Exchange (ETDEWEB)

    1991-04-01

    The Analytical Chemistry Division has programs in inorganic mass spectrometry, optical spectroscopy, organic mass spectrometry, and secondary ion mass spectrometry. It maintains a transuranium analytical laboratory and an environmental analytical laboratory. It carries out chemical and physical analysis in the fields of inorganic chemistry, organic spectroscopy, separations and synthesis. (WET)

  12. 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.

  13. 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.

  14. 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.

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

    International Nuclear Information System (INIS)

    Sedykh, Eh.M.; Lyabusheva, O.A.; Bannykh, L.N.; Tambiev, A.Kh.

    2005-01-01

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

  16. Quantitation of stable isotopic tracers of calcium by fast atom bombardment mass spectrometry

    International Nuclear Information System (INIS)

    Jiang, X.; Smith, D.L.

    1987-01-01

    Instrumentation and methodology developed for quantitation of stable isotopic traces in urine are described. Calcium is isolated from urine as the insoluble oxalate salt which is subsequently dissolved in hydrochloric acid. The isotopic content of the acid solution is determined by use of a conventional mass spectrometer equipped with a fast atom bombardment ion source. Calcium ions are desorbed from the sample surface by a beam of high-energy xenon atoms and detected with a high-resolution mass spectrometer. A data acquisition system has been developed to control the mass spectrometer and record the ion signals. Detailed analysis of potential sources of error indicates that the precision of the method is presently limited primarily by an isotope effect that occurs during ion desorption. Results presented here demonstrate that the relative abundances of calcium isotopes in urine can be determined with high precision (coefficient of variation < 0.2%) and that the method is a viable alternative to conventional thermal ionization mass spectrometry. The method is especially attractive because it uses a conventional high-resolution mass spectrometer which is routinely used for analysis of organic substances

  17. Determination of gold in geological samples - the present and the future

    International Nuclear Information System (INIS)

    Feriancik, E.

    1997-01-01

    This paper reviews some analytical techniques which have been described for the gold analysis of geological materials: spectrophotometry; flame atomic absorption spectrometry; graphite coupled plasma atomic emission spectrometry; inductively coupled plasma atomic emission spectrometry; inductively coupled plasma-mass spectrometry; neutron activation; electro-analysis methods and fire assay

  18. Use of magnesium as a test element for inductively coupled plasma atomic emission spectrometry diagnosis

    International Nuclear Information System (INIS)

    Mermet, J.M.

    1991-01-01

    To optimize atomization and ionization processes in an inductively coupled plasma used as a source in atomic emission spectrometry, the Mg II 280.270-nm/Mg I 285-213-nm line intensity ratio is used. A theoretic ratio is calculated assuming a local thermodynamic equilibrium.A review of previously published experimental values of the ratio is given as a function of the parameters influencing the energy transfer between the plasma and injected species. In particular, the effects of the power, the carrier gas flow-rate, the i.d. of the torch injector, the use of a sheathing gas and the presence of hydrogen are described. Values of the ratio close to the theoretical values are obtained with a high power (>1.4 kW), a lower carrier gas flow-rate ( -1 ) and a large i.d. of the injector (>2 mm). This optimization can also be applied to the minimization of interference effects due to the presence of sodium. (author). 64 refs.; 9 figs.; 1 tab

  19. Advances in low atomic number element analysis by wavelength dispersive x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Vrebos, B.

    1996-01-01

    Traditionally, the analysis of low atomic number has been a chal1enging task for wavelength dispersive x-ray fluorescence spectrometry. Among the most important factors influencing analysis of the low atomic number elements (from Z=11 downwards) are the fluorescence yield, absorption and the dispersion. The effect of each of these factors on the overall performance will be illustrated. The long wavelengths involved (longer than I nm) used to pose severe problems concerning the monochromator used. Early instruments relied on lead stearate or Blodgett Langmuir soap films for the diffraction of the characteristic radiation. Nowadays, synthetic multilayers are commonly used. The performance of these multilayers is determined by the reflectivity, the resolution and the absorption of the characteristic radiation to be diffracted. These parameters can be optimised by adequately selecting the composition of the materials involved. The sensitivity of the modem instruments is sufficient to allow quantitative analysis. However, this aspect of WDS XRF is still met with considerable scepticism. Examples of quantitative analysis will be given to illustrate the current capability

  20. 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

  1. Accelerator mass spectrometry: ultrasensitive analysis of global science

    International Nuclear Information System (INIS)

    Tuniz, C.; Bird, J.B.; Fink, D.; Herzog, G.F.

    1998-01-01

    Accelerator mass spectrometry (AMS), an innovative analytical technique, measures rare atoms at unprecedented levels of sensitivity, revolutionizing the science of radiocarbon dating and accessing new environmental tracers and chronometers. AMS can study extraterrestrial materials, the earth sciences, the future of the global environment, and the history of mankind. The Shroud of Turin, meteorites from Mars, the crown of Charlemagne, and ancient air trapped in Antarctic ice indicate some of the samples on which AMS has been applied. This book has compiled the diverse set of scientific literature into a single volume, suitable as a text or resource on the major AMS-related outcomes, issues, and methods. It explains how scientists and researchers succeeded in counting Carbon-14 atoms at an extraordinary level, examines the impact of AMS on the branches of scientific technology and historical research, provides an understanding of the chronology and significance of past and present environmental changes, details the advances in AMS equipment, technology, and methods as well as the expansion of AMS research

  2. Analytical spectroscopy. Analytical Chemistry Symposia Series, Volume 19

    International Nuclear Information System (INIS)

    Lyon, W.S.

    1984-01-01

    This book contains papers covering several fields in analytical chemistry including lasers, mass spectrometry, inductively coupled plasma, activation analysis and emission spectroscopy. Separate abstracting and indexing was done for 64 papers in this book

  3. 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

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

    Science.gov (United States)

    Strong, B; Murray-Smith, R

    1974-12-01

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

  5. Electrospray Ionization Mass Spectrometry: A Technique to Access the Information beyond the Molecular Weight of the Analyte

    Science.gov (United States)

    Banerjee, Shibdas; Mazumdar, Shyamalava

    2012-01-01

    The Electrospray Ionization (ESI) is a soft ionization technique extensively used for production of gas phase ions (without fragmentation) of thermally labile large supramolecules. In the present review we have described the development of Electrospray Ionization mass spectrometry (ESI-MS) during the last 25 years in the study of various properties of different types of biological molecules. There have been extensive studies on the mechanism of formation of charged gaseous species by the ESI. Several groups have investigated the origin and implications of the multiple charge states of proteins observed in the ESI-mass spectra of the proteins. The charged analytes produced by ESI can be fragmented by activating them in the gas-phase, and thus tandem mass spectrometry has been developed, which provides very important insights on the structural properties of the molecule. The review will highlight recent developments and emerging directions in this fascinating area of research. PMID:22611397

  6. Electrospray ionization mass spectrometry: a technique to access the information beyond the molecular weight of the analyte.

    Science.gov (United States)

    Banerjee, Shibdas; Mazumdar, Shyamalava

    2012-01-01

    The Electrospray Ionization (ESI) is a soft ionization technique extensively used for production of gas phase ions (without fragmentation) of thermally labile large supramolecules. In the present review we have described the development of Electrospray Ionization mass spectrometry (ESI-MS) during the last 25 years in the study of various properties of different types of biological molecules. There have been extensive studies on the mechanism of formation of charged gaseous species by the ESI. Several groups have investigated the origin and implications of the multiple charge states of proteins observed in the ESI-mass spectra of the proteins. The charged analytes produced by ESI can be fragmented by activating them in the gas-phase, and thus tandem mass spectrometry has been developed, which provides very important insights on the structural properties of the molecule. The review will highlight recent developments and emerging directions in this fascinating area of research.

  7. 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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  9. 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

  10. On-line Incorporation of Cloud Point Extraction in Flame Atomic Absorption Spectrometric Determination of Silver

    OpenAIRE

    DALALI, Nasser; JAVADI, Nasrin; AGRAWAL, Yadvendra KUMAR

    2008-01-01

    A cloud point extraction method was incorporated into a flow injection system, coupled with flame atomic absorption spectrometry, for determination of trace amounts of silver. The analyte in the aqueous solution was acidified with 0.2 mol L-1 sulfuric acid and complexed with dithizone. The cloud point extraction was performed using the non-ionic surfactant Triton X-114. After obtaining the cloud point, the surfactant-rich phase containing the dithizonate complex was collected in a m...

  11. Development of precise analytical methods for strontium and lanthanide isotopic ratios using multiple collector inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Ohno, Takeshi; Takaku, Yuichi; Hisamatsu, Shun'ichi

    2007-01-01

    We have developed precise analytical methods for strontium and lanthanide isotopic ratios using multiple collector-ICP-mass spectrometry (MC-ICP-MS) for experimental and environmental studies of their behavior. In order to obtain precise isotopic data using MC-ICP-MS, the mass discrimination effect was corrected by an exponential law correction method. The resulting isotopic data demonstrated that highly precise isotopic analyses (better than 0.1 per mille as 2SD) could be achieved. We also adopted a de-solvating nebulizer system to improve the sensitivity. This system could minimize the water load into the plasma and provided about five times larger intensity of analyte than a conventional nebulizer system did. (author)

  12. Proceedings of the twenty ninth ISMAS international symposium on mass spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, Suresh K.; Pranaw Kumar; Jaison, P.G.; Sarkar, Arnab; Telmore, Vijay M.

    2015-02-01

    Mass spectrometry is a truly multi-disciplinary science and has emerged as an indispensable analytical tool due to its high sensitivity, specificity and universality. It is playing a key role in variety of scientific disciplines of chemistry, physics, biology, archaeology, material science etc. Progress in the field of mass spectrometry in the last two decades has led to the advent of new ion sources, improvements in existing mass analyzers and introduction of hybrid mass analyzers. As the technique continues to advance, many new applications have emerged particularly in health sciences and for forensic applications. The current world scenario demands determination at single atom and single molecule with high specificity. The vendors in the international mass spectrometric instrumentation market are guided by these requirements as well as the inputs from mass spectrometrists around the world engaged in new developments. Papers relevant to INIS are indexed separately

  13. Atomic absorption spectrophotometry in perspective

    International Nuclear Information System (INIS)

    Soffiantini, V.

    1981-01-01

    Atomic absorption spectrophotometry is essentially an analytical technique used for quantitative trace metal analysis in a variety of materials. The speed and specificity of the technique is its greatest advantage over other analytical techniques. What atomic absorption spectrophotometry can and cannot do and its advantages and disadvantages are discussed, a summary of operating instructions are given, as well as a summary of analytical interferences. The applications of atomic absorption spectrophotometry are also shortly discussed

  14. Ninth ISMAS workshop on mass spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.

    2000-12-01

    Mass spectrometry has wide-ranging applications in such diverse areas as nuclear industry, agriculture, drugs, environment, petroleum and lentils. There is an urgent need to absorb and assimilate state-of-the-art technological developments in the field. Emerging trends in atomic mass spectrometry, advances in organic mass spectrometry, qualitative and quantitative analyses by mass spectrometry and mass spectrometry in oceanography are some of the areas that need to be expeditiously examined and are covered in this volume. Papers relevant to INIS are indexed separately

  15. 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.

  16. [Atomic/ionic fluorescence in microwave plasma torch discharge excited by high current microsecond pulsed hollow cathode lamp-europium atomic/ionic fluorescence spectrometry].

    Science.gov (United States)

    Gong, Z; Liang, F; Yang, P; Jin, Q; Huang, B

    1999-06-01

    Eu atomic and ionic fluorescence spectrometry in microwave plasma torch discharge excited by high current microsecond pulsed hollow cathode lamp (HCMP HCL-MPT AFS/IFS) was studied. Operating conditions were optimized. The best detection limits for AFS and IFS obtained with a desolvated ultrasonic nebulization system were 42.0 ng/mL for Eu I 462.7 nm and 21.8 ng/mL for Eu II 381.97 nm, respectively, both were better than those given by the instruction manual of a Baird ICP AFS-2000 spectrometer using pneumatic concentric nebulizer with desolvation for AFS, but were significantly higher than those obtained by using the Baird spectrometer with a mini-monochromator and a ultrasonic nebulzer system.

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

    Science.gov (United States)

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

    2017-10-01

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

  18. 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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    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

  20. Analytical strategies in mass spectrometry-based phosphoproteomics

    DEFF Research Database (Denmark)

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

    2011-01-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  2. Direct analyte-probed nanoextraction coupled to nanospray ionization-mass spectrometry of drug residues from latent fingerprints.

    Science.gov (United States)

    Clemons, Kristina; Wiley, Rachel; Waverka, Kristin; Fox, James; Dziekonski, Eric; Verbeck, Guido F

    2013-07-01

    Here, we present a method of extracting drug residues from fingerprints via Direct Analyte-Probed Nanoextraction coupled to nanospray ionization-mass spectrometry (DAPNe-NSI-MS). This instrumental technique provides higher selectivity and lower detection limits over current methods, greatly reducing sample preparation, and does not compromise the integrity of latent fingerprints. This coupled to Raman microscopy is an advantageous supplement for location and identification of trace particles. DAPNe uses a nanomanipulator for extraction and differing microscopies for localization of chemicals of interest. A capillary tip with solvent of choice is placed in a nanopositioner. The surface to be analyzed is placed under a microscope, and a particle of interest is located. Using a pressure injector, the solvent is injected onto the surface where it dissolves the analyte, and then extracted back into the capillary tip. The solution is then directly analyzed via NSI-MS. Analyses of caffeine, cocaine, crystal methamphetamine, and ecstasy have been performed successfully. © 2013 American Academy of Forensic Sciences.

  3. Comparison of ultra-violet and inductively coupled plasma-atomic emission spectrometry for the on-line quantification of selenium species after their separation by reversed-phase liquid chromatography

    International Nuclear Information System (INIS)

    Tsopelas, Fotios N.; Ochsenkuehn-Petropoulou, Maria Th.; Mergias, Ioannis G.; Tsakanika, Lambrini V.

    2005-01-01

    An analytical approach for selenium speciation using liquid chromatography (LC) coupled with ultra-violet (UV) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was developed. The separation of the investigated selenium species, selenites, selenates, selenomethionine, selenocystine, selenocystamine and dimethyldiselenide was accomplished in less than 6 min on a BIO Wide Pore RP-18 column using sodium salt of n-octanesulfonic acid as ion-pairing modifier. The on-line detection of the separated selenium species was performed using UV spectrometry at the optimum wavelength of 192 nm, obtained by the UV spectra of the investigated individual selenium species. ICP-AES was also used as element specific on-line detector, after its coupling with the chromatographic system. The UV and ICP-AES detectors were compared for their suitability, including sensitivity and detection limits, for the on-line quantification of the six selenium species. The developed LC-UV as well as LC-ICP-AES techniques were successfully applied to a selenized yeast candidate reference material, after its enzymatic extraction with protease XIV. It was found that the described LC-UV technique is suitable for the determination of selenomethionine, the main selenium compound in the yeast, with an accuracy of 5%, although the UV detector is not element specific and it is rarely used for selenium speciation. This finding can prove valuable for routine laboratories to perform selenium speciation in such materials

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

    OpenAIRE

    Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria das Graças Andrade; Bezerra, Marcos de Almeida

    2009-01-01

    Texto completo: acesso restrito. p. 1041-1045 A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L−1 nitric acid solution, the analytes are determinate employing fla...

  5. The recent developments in dispersive liquid–liquid microextraction for preconcentration and determination of inorganic analytes

    Directory of Open Access Journals (Sweden)

    H.M. Al-Saidi

    2014-12-01

    Full Text Available Recently, increasing interest on the use of dispersive liquid–liquid microextraction (DLLME developed in 2006 by Rezaee has been found in the field of separation science. DLLME is miniaturized format of liquid–liquid extraction in which acceptor-to-donor phase ratio is greatly reduced compared with other methods. In the present review, the combination of DLLME with different analytical techniques such as atomic absorption spectrometry (AAS, inductively coupled plasma-optical emission spectrometry (ICP-OES, gas chromatography (GC, and high-performance liquid chromatography (HPLC for preconcentration and determination of inorganic analytes in different types of samples will be discussed. Recent developments in DLLME, e.g., displacement-DLLME, the use of an auxiliary solvent for adjustment of density of extraction mixture, and the application of ionic liquid-based DLLME in determination of inorganic species even in the presence of high content of salts are presented in the present review. Finally, comparison of DLLME with the other liquid-phase microextraction approaches and limitations of this technique are provided.

  6. Study of the analytic quality in the determinations of Cr, Fe, Mn, Cu, Zn, Pb and Hg through conventional and nuclear analytical techniques in mosses of the MATV; Estudio de la calidad analitica en las determinaciones de Cr, Fe, Mn, Cu, Zn, Pb y Hg a traves de tecnicas analiticas nucleares y convencionales en musgos de la ZMVT

    Energy Technology Data Exchange (ETDEWEB)

    Caballero S, B.

    2013-07-01

    To evaluate the environmental risks of air pollution and to facilitate the decision-making for control, is necessary to have the capacity to generate data with analytical quality. A comparison between nuclear (Neutron activation analysis and total reflection X-ray fluorescence spectrometry) and no nuclear analytical techniques (atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry) for simultaneous determination of metal content (Cr, Cu, Fe, Hg, Mn, Pb and Zn) in mosses from Metropolitan Area of the Toluca Valley (MATV) was performed. Epiphytic mosses (Fabriona ciliaris and Leskea angustata) were sampled in two campaigns, 16 sites (urban, transition and natural) and were prepared for each technique. The biological certified reference materials were used for the quality control and to evaluate accuracy, precision, linearity, detection and quantification limits. Results show that nuclear analytical techniques and no nuclear applied in chemical analysis of Cr, Cu, Fe, Hg, Mn, Pb and Zn in moss from MATV are comparable and therefore all of these can potentially be used for this purpose. However, if its considered both, the performance parameters and economic/operational characteristics is widely recommended inductively coupled plasma optical emission spectrometry, conventional analytical technique, which showed the highest analytical grade quality. Also were observed spatial and temporal variations in the concentrations of Cr, Cu, Fe, Hg, Mn, Pb and Zn in mosses from MATV and was discussed its potential origin. The urban sites had the highest concentration of anthropogenic elements as Cr, Cu, Fe, Hg, Pb and Zn because are strongly impacted by roads with high vehicle traffic. (Author)

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

    International Nuclear Information System (INIS)

    Matsumiya, Hiroaki; Kageyama, Tomohiro; Hiraide, Masataka

    2004-01-01

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

  8. Use of gradient dilution to flag and overcome matrix interferences in axial-viewing inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Cheung, Yan; Schwartz, Andrew J.; Hieftje, Gary M.

    2014-01-01

    Despite the undisputed power of inductively coupled plasma-atomic emission spectrometry (ICP-AES), its users still face serious challenges in obtaining accurate analytical results. Matrix interference is perhaps the most important challenge. Dilution of a matrix-containing sample is a common practice to reduce matrix interference. However, determining the optimal dilution factor requires tedious and time-consuming offline sample preparation, since emission lines and the effect of matrix interferences are affected differently by the dilution. The current study exploits this difference by employing a high-performance liquid chromatography gradient pump prior to the nebulizer to perform on-line mixing of a sample solution and diluent. Linear gradient dilution is performed on both the calibration standard and the matrix-containing sample. By ratioing the signals from two emission lines (from the same or different elements) as a function of dilution factor, the analyst can not only identify the presence of a matrix interference, but also determine the optimal dilution factor needed to overcome the interference. A ratio that does not change with dilution signals the absence of a matrix interference, whereas a changing ratio indicates the presence of an interference. The point on the dilution profile where the ratio stabilizes indicates the optimal dilution factor to correct the interference. The current study was performed on axial-viewing ICP-AES with o-xylene as the solvent

  9. 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)

  10. 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.

  11. Exploration of robust operating conditions in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Tromp, John W.; Pomares, Mario; Alvarez-Prieto, Manuel; Cole, Amanda; Ying Hai; Salin, Eric D.

    2003-01-01

    'Robust' conditions, as defined by Mermet and co-workers for inductively coupled plasma (ICP)-atomic emission spectrometry, minimize matrix effects on analyte signals, and are obtained by increasing power and reducing nebulizer gas flow. In ICP-mass spectrometry (MS), it is known that reduced nebulizer gas flow usually leads to more robust conditions such that matrix effects are reduced. In this work, robust conditions for ICP-MS have been determined by optimizing for accuracy in the determination of analytes in a multi-element solution with various interferents (Al, Ba, Cs, K, Na), by varying power, nebulizer gas flow, sample introduction rate and ion lens voltage. The goal of the work was to determine which operating parameters were the most important in reducing matrix effects, and whether different interferents yielded the same robust conditions. Reduction in nebulizer gas flow and in sample input rate led to a significantly decreased interference, while an increase in power seemed to have a lesser effect. Once the other parameters had been adjusted to their robust values, there was no additional improvement in accuracy attainable by adjusting the ion lens voltage. The robust conditions were universal, since, for all the interferents and analytes studied, the optimum was found at the same operating conditions. One drawback to the use of robust conditions was the slightly reduced sensitivity; however, in the context of 'intelligent' instruments, the concept of 'robust conditions' is useful in many cases

  12. Spectroscopy stepping stones

    International Nuclear Information System (INIS)

    Hammer, M.R.; Sturman, B.T.

    2003-01-01

    Determining the elemental composition of samples has long been a basic task of analytical science. Some very powerful and convenient approaches are based on the wavelength-specific absorption or emission of light by gas-phase atoms. Techniques briefly described as examples of analytical atomic spectrometry include atomic emission and absorption spectroscopy, inductively coupled plasma emission and mass spectroscopy and laser induced breakdown spectrometry

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

    Energy Technology Data Exchange (ETDEWEB)

    Baytak, Sitki [Department of Chemistry, Faculty of Science and Arts, Harran University, 63100 Sanliurfa (Turkey); Tuerker, A. Rehber [Department of Chemistry, Faculty of Science and Arts, Gazi University, 06500 Ankara (Turkey)]. E-mail: aturker@gazi.edu.tr

    2006-02-28

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

  14. 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

  15. Alpha and beta detection and spectrometry

    International Nuclear Information System (INIS)

    Saro, S.

    1984-01-01

    The theory of alpha and beta radioactive decay, the interaction of alpha and beta particles with matter, and their detection and spectrometry are dealt with in seven chapters: 1. Alpha transformation of atomic nuclei; 2. Basic properties of detectors and statistics of detection; 3. Alpha detectors and spectrometers; 4. Applications of alpha detection and spectrometry; 5. Beta transformation of atomic nuclei; 6. Beta particle detectors and spectrometers; 7. Detection of low energy beta particles. Chapter 8 is devoted to sampling and preparation of samples for radiometry. (E.F.)

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

    Science.gov (United States)

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

    2010-06-15

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

  17. 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.

  18. Determination of trace amounts of lead, arsenic, nickel and cobalt in high-purity iron oxide pigment by inductively coupled plasma atomic emission spectrometry after iron matrix removal with extractant-contained resin

    International Nuclear Information System (INIS)

    Xu Yuyu; Zhou Jianfeng; Wang Guoxin; Zhou Jinfan; Tao Guanhong

    2007-01-01

    Inductively coupled plasma atomic emission spectrometry (ICP-AES) was applied to the determination of lead, arsenic, nickel and cobalt in high-purity iron oxide pigment. Samples were dissolved with hydrochloric acid and hydrogen peroxide. The digest was passed through a column, which was packed with a polymer resin containing a neutral organophosphorus extractant, tri-n-butylphosphate. Iron was sorbed selectively on the resin and the analytes of interest passed through the column, allowing the effective separation of them from the iron matrix. Conditions of separation were optimized. The detection limits (3σ) in solution were 10, 40, 7 and 5 μg L -1 , and in pigment were 0.2, 0.8, 0.14 and 0.1 mg kg -1 for lead, arsenic, cobalt and nickel, respectively. The recoveries ranged from 95% to 107% when sample digests were spiked with 5 μg of the analytes of interest, and relative standard deviations (n = 6) were 1.5-17.6% for the determination of the spiked samples. The method was successfully applied to the determination of trace amounts of these elements in high-purity iron oxide pigment samples

  19. 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.

  20. X-ray spectrometry for preventive conservation of cultural heritage

    Indian Academy of Sciences (India)

    Analytical chemistry does play a key role in the chemical characterization of the environment and it appears that X-ray spectrometry, in its many forms, is one of the most relevant analytical techniques in preventive conservation, as it is in cultural heritage research in general. X-ray spectrometry has indeed been the method ...

  1. Determination of cadmium in seawater by chelate vapor generation atomic fluorescence spectrometry

    Science.gov (United States)

    Sun, Rui; Ma, Guopeng; Duan, Xuchuan; Sun, Jinsheng

    2018-03-01

    A method for the determination of cadmium in seawater by chelate vapor generation (Che-VG) atomic fluorescence spectrometry is described. Several commercially available chelating agents, including ammonium pyrrolidine dithiocarbamate (APDC), sodium dimethyl dithiocarbamate (DMDTC), ammonium dibutyl dithiophosphate (DBDTP) and sodium O,O-diethyl dithiophosphate (DEDTP), are compared with sodium diethyldithiocarbamate (DDTC) for the Che-VG of cadmium, and results showed that DDTC and DEDTP had very good cadmium signal intensity. The effect of the conditions of Che-VG with DDTC on the intensity of cadmium signal was investigated. Under the optimal conditions, 85 ± 3% Che-VG efficiency is obtained for cadmium. The detection limit (3σ) obtained in the optimal conditions was 0.19 ng ml- 1. The relative standard deviation (RSD, %) for ten replicate determinations at 2 ng ml- 1 Cd was 3.42%. The proposed method was successfully applied to the ultratrace determination of cadmium in seawater samples by the standard addition method.

  2. Surrogate analyte approach for quantitation of endogenous NAD(+) in human acidified blood samples using liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Liu, Liling; Cui, Zhiyi; Deng, Yuzhong; Dean, Brian; Hop, Cornelis E C A; Liang, Xiaorong

    2016-02-01

    A high-performance liquid chromatography tandem mass spectrometry (LC-MS/MS) assay for the quantitative determination of NAD(+) in human whole blood using a surrogate analyte approach was developed and validated. Human whole blood was acidified using 0.5N perchloric acid at a ratio of 1:3 (v:v, blood:perchloric acid) during sample collection. 25μL of acidified blood was extracted using a protein precipitation method and the resulting extracts were analyzed using reverse-phase chromatography and positive electrospray ionization mass spectrometry. (13)C5-NAD(+) was used as the surrogate analyte for authentic analyte, NAD(+). The standard curve ranging from 0.250 to 25.0μg/mL in acidified human blood for (13)C5-NAD(+) was fitted to a 1/x(2) weighted linear regression model. The LC-MS/MS response between surrogate analyte and authentic analyte at the same concentration was obtained before and after the batch run. This response factor was not applied when determining the NAD(+) concentration from the (13)C5-NAD(+) standard curve since the percent difference was less than 5%. The precision and accuracy of the LC-MS/MS assay based on the five analytical QC levels were well within the acceptance criteria from both FDA and EMA guidance for bioanalytical method validation. Average extraction recovery of (13)C5-NAD(+) was 94.6% across the curve range. Matrix factor was 0.99 for both high and low QC indicating minimal ion suppression or enhancement. The validated assay was used to measure the baseline level of NAD(+) in 29 male and 21 female human subjects. This assay was also used to study the circadian effect of endogenous level of NAD(+) in 10 human subjects. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Evaluation of a tungsten coil atomization-laser-induced fluorescence detection approach for trace elemental analysis

    International Nuclear Information System (INIS)

    Ezer, Muhsin; Elwood, Seth A.; Jones, Bradley T.; Simeonsson, Josef B.

    2006-01-01

    The analytical utility of a tungsten (W)-coil atomization-laser-induced fluorescence (LIF) approach has been evaluated for trace level measurements of elemental chromium (Cr), arsenic (As), selenium (Se), antimony (Sb), lead (Pb), tin (Sn), copper (Cu), thallium (Tl), indium (In), cadmium (Cd), zinc (Zn) and mercury (Hg). Measurements of As, Cr, In, Se, Sb, Pb, Tl, and Sn were performed by laser-induced fluorescence using a single dye laser operating near 460 nm whose output was converted by frequency doubling and stimulated Raman scattering to wavelengths ranging from 196 to 286 nm for atomic excitation. Absolute limits of detection (LODs) of 1, 0.3, 0.3, 0.2, 1, 6, 1, 0.2 and 0.8 pg and concentration LODs of 100, 30, 30, 20, 100, 600, 100, 20, and 80 pg/mL were achieved for As, Se, Sb, Sn, In, Cu, Cr, Pb and Tl, respectively. Determinations of Hg, Pb, Zn and Cd were performed using two-color excitation approaches and resulted in absolute LODs of 2, 30, 5 and 0.6 pg, respectively, and concentration LODs of 200, 3000, 500 and 60 pg/mL, respectively. The sensitivities achieved by the W-coil LIF approaches compare well with those reported by W-coil atomic absorption spectrometry, graphite furnace atomic absorption spectrometry, and graphite furnace electrothermal atomization-LIF approaches. The accuracy of the approach was verified through the analysis of a multielement reference solution containing Sb, Pb and Tl which each had certified performance acceptance limits of 19.6-20.4 μg/mL. The determined concentrations were 20.05 ± 2.60, 20.70 ± 2.27 and 20.60 ± 2.46 μg/mL, for Sb, Pb and Tl, respectively. The results demonstrate that W-coil LIF provides good analytical performance for trace analyses due to its high sensitivity, linearity, and capability to measure multiple elements using a single tunable laser and suggest that the development of portable W-coil LIF instrumentation using compact, solid-state lasers is feasible

  4. Evaluation of a tungsten coil atomization-laser-induced fluorescence detection approach for trace elemental analysis.

    Science.gov (United States)

    Ezer, Muhsin; Elwood, Seth A; Jones, Bradley T; Simeonsson, Josef B

    2006-06-30

    The analytical utility of a tungsten (W)-coil atomization-laser-induced fluorescence (LIF) approach has been evaluated for trace level measurements of elemental chromium (Cr), arsenic (As), selenium (Se), antimony (Sb), lead (Pb), tin (Sn), copper (Cu), thallium (Tl), indium (In), cadmium (Cd), zinc (Zn) and mercury (Hg). Measurements of As, Cr, In, Se, Sb, Pb, Tl, and Sn were performed by laser-induced fluorescence using a single dye laser operating near 460 nm whose output was converted by frequency doubling and stimulated Raman scattering to wavelengths ranging from 196 to 286 nm for atomic excitation. Absolute limits of detection (LODs) of 1, 0.3, 0.3, 0.2, 1, 6, 1, 0.2 and 0.8 pg and concentration LODs of 100, 30, 30, 20, 100, 600, 100, 20, and 80 pg/mL were achieved for As, Se, Sb, Sn, In, Cu, Cr, Pb and Tl, respectively. Determinations of Hg, Pb, Zn and Cd were performed using two-color excitation approaches and resulted in absolute LODs of 2, 30, 5 and 0.6 pg, respectively, and concentration LODs of 200, 3000, 500 and 60 pg/mL, respectively. The sensitivities achieved by the W-coil LIF approaches compare well with those reported by W-coil atomic absorption spectrometry, graphite furnace atomic absorption spectrometry, and graphite furnace electrothermal atomization-LIF approaches. The accuracy of the approach was verified through the analysis of a multielement reference solution containing Sb, Pb and Tl which each had certified performance acceptance limits of 19.6-20.4 microg/mL. The determined concentrations were 20.05+/-2.60, 20.70+/-2.27 and 20.60+/-2.46 microg/mL, for Sb, Pb and Tl, respectively. The results demonstrate that W-coil LIF provides good analytical performance for trace analyses due to its high sensitivity, linearity, and capability to measure multiple elements using a single tunable laser and suggest that the development of portable W-coil LIF instrumentation using compact, solid-state lasers is feasible.

  5. Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Acar, O.

    2012-01-01

    The Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive) and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds) were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS) using an Sc + Ir + NH 4 H 2 PO 4 chemical modifier mixture and flame atomic absorption spectrometer (FAAS) after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD) for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 μg L - 1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM) and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH 4 H 2 PO 4 mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compared with international and national food quality guidelines as well as with literature values. (Author) 48 refs.

  6. Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Acar, O.

    2012-07-01

    The Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive) and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds) were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS) using an Sc + Ir + NH{sub 4}H{sub 2}PO{sub 4} chemical modifier mixture and flame atomic absorption spectrometer (FAAS) after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD) for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 {mu}g L{sup -}1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM) and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH{sub 4}H{sub 2}PO{sub 4} mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compared with international and national food quality guidelines as well as with literature values. (Author) 48 refs.

  7. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection

    DEFF Research Database (Denmark)

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-01-01

    The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed...

  8. 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

  9. Determination of fluorine concentrations using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry to analyze fluoride precipitates.

    Science.gov (United States)

    Lee, H. A.; Lee, J.; Kwon, E.; Kim, D.; Yoon, H. O.

    2015-12-01

    In recent times, fluorine has been receiving increasing attention due to the possibility for chemical (HF) leakage accidents and its high toxicity to human and environment. In this respect, a novel approach for the determination of fluorine concentrations in water samples using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry was investigated in this study. The main disadvantage of WDXRF technique for fluorine analysis is low analytical sensitivity for light elements with atomic number (Z) less than 15. To overcome this problem, we employed the precipitation reaction which fluoride is reacted with cation such as Al3+ and/or Ca2+ prior to WDXRF analysis because of their high analytical sensitivity. The cation was added in fluoride solutions to form precipitate (AlF3 and/or CaF2) and then the solution was filtered through Whatman filter. After drying at 60 °C for 5 min, the filter was coated with X-ray film and directly analyzed using WDXRF spectrometry. Consequently, we analyzed the cation on filter and subsequently fluorine concentration was calculated inversely based on chemical form of precipitate. This method can improve the analytical sensitivity of WDXRF technique for fluorine analysis and be applicable to various elements that can make precipitate.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-03-15

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  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. Surface analysis by imaging mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vidová, Veronika; Volný, Michael; Lemr, Karel; Havlíček, Vladimír

    2009-01-01

    Roč. 74, 7-8 (2009), s. 1101-1116 ISSN 0010-0765 Institutional research plan: CEZ:AV0Z50200510 Keywords : secondary ion mass spectrometry * matrix assisted laser desorption ionization * mass spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.856, year: 2009

  14. Tin Content Determination in Canned Fruits and Vegetables by Hydride Generation Inductively Coupled Plasma Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    Sanda Rončević

    2012-01-01

    Full Text Available Tin content in samples of canned fruits and vegetables was determined by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-OES, and it was compared with results obtained by standard method of flame atomic absorption spectrometry (AAS. Selected tin emission lines intensity was measured in prepared samples after addition of tartaric acid and followed by hydride generation with sodium borohydride solution. The most favorable line at 189.991 nm showed the best detection limit (1.9 μg L−1 and limit of quantification (6.4 μg kg−1. Good linearity and sensitivity were established from time resolved analysis and calibration tests. Analytical accuracy of 98–102% was obtained by recovery study of spiked samples. Method of standard addition was applied for tin determination in samples from fully protected tinplate. Tin presence at low-concentration range was successfully determined. It was shown that tenth times less concentrations of Sn were present in protected cans than in nonprotected or partially protected tinplate.

  15. Syntheses of deuterated leu-enkephalins and their use as internal standards for the quantification of leu-enkephalin by fast atom bombardment mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Benfenati, E. (Istituto di Ricerche Farmacologiche Mario Negri, Bergamo (Italy) Istituto di Ricerche Farmacologiche Mario Negri, Milan (Italy)); Icardi, G.; Chen, S. (Istituto di Ricerche Farmacologiche Mario Negri, Bergamo (Italy)); Fanelli, R. (Istituto di Ricerche Farmacologiche Mario Negri, Milan (Italy))

    1990-04-01

    We have developed a synthetic method for the preparation of di- and pentadeuterated leu-enkephalin (LE), Tyr-Gly-Gly-Phe-Leu, by proton-deuterium exchange using CF[sub 3]COOO[sup 2]H. Four to six deuterium atoms are introduced using a reaction temperature of 120[sup o]C and if 5% of [sup 2]H[sub 2]O is added the di-deuterated LE is obtained. These deuterated compounds are used as internal standards to plot calibration curves of LE using fast atom bombardment mass spectrometry. (author).

  16. 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.

  17. The use of selective adsorbents in capillary electrophoresis-mass spectrometry for analyte preconcentration and microreactions: a powerful three-dimensional tool for multiple chemical and biological applications.

    Science.gov (United States)

    Guzman, N A; Stubbs, R J

    2001-10-01

    Much attention has recently been directed to the development and application of online sample preconcentration and microreactions in capillary electrophoresis using selective adsorbents based on chemical or biological specificity. The basic principle involves two interacting chemical or biological systems with high selectivity and affinity for each other. These molecular interactions in nature usually involve noncovalent and reversible chemical processes. Properly bound to a solid support, an "affinity ligand" can selectively adsorb a "target analyte" found in a simple or complex mixture at a wide range of concentrations. As a result, the isolated analyte is enriched and highly purified. When this affinity technique, allowing noncovalent chemical interactions and biochemical reactions to occur, is coupled on-line to high-resolution capillary electrophoresis and mass spectrometry, a powerful tool of chemical and biological information is created. This paper describes the concept of biological recognition and affinity interaction on-line with high-resolution separation, the fabrication of an "analyte concentrator-microreactor", optimization conditions of adsorption and desorption, the coupling to mass spectrometry, and various applications of clinical and pharmaceutical interest.

  18. 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.

  19. 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.

  20. Investigation of plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry caused by matrices with low second ionization potentials-identification of the secondary factor

    International Nuclear Information System (INIS)

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

    2006-01-01

    Plasma-related matrix effects induced by a comprehensive list of matrix elements (a total of fifty-one matrices) in inductively coupled plasma-atomic emission spectrometry were investigated and used to confirm that matrix effects caused by elements with a low second ionization potential are more severe than those from matrix elements having a low first ionization potential. Although the matrix effect is correlated unambiguously with the second ionization potential of a matrix, the correlation is not monotonic, which suggests that at least one other factor is operative. Through study of a large pool of matrix elements, it becomes possible to identify another critical parameter that defines the magnitude of the matrix effect; namely the presence of low-lying energy levels in the doubly charged matrix ion. Penning ionization by Ar excited states is proposed as the dominant mechanism for both analyte ionization/excitation and matrix effects; matrices with a low second ionization potential can effectively quench the population of Ar excited states through successive Penning ionization followed by ion-electron recombination and lead to more severe matrix effects