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Sample records for atomic absorption spectrom

  1. Hot tube atomic absorption spectrochemistry.

    PubMed

    Woodriff, R; Stone, R W

    1968-07-01

    A small, commercially available atomic absorption instrument is used with a heated graphite tube for the atomic absorption analysis of liquid and solid silver samples. Operating conditions of the furnace are described and a sensitivity of about 5 ng of silver is reported. PMID:20068797

  2. Absorption properties of identical atoms

    SciTech Connect

    Sancho, Pedro

    2013-09-15

    Emission rates and other optical properties of multi-particle systems in collective and entangled states differ from those in product ones. We show the existence of similar effects in the absorption probabilities for (anti)symmetrized states of two identical atoms. The effects strongly depend on the overlapping between the atoms and differ for bosons and fermions. We propose a viable experimental verification of these ideas. -- Highlights: •The absorption rates of a pair of identical atoms in product and (anti)symmetrized states are different. •The modifications of the optical properties are essentially determined by the overlapping between the atoms. •The absorption properties differ, in some cases, for bosons and fermions.

  3. Graphite filter atomizer in atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Katskov, Dmitri A.

    2007-09-01

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

  4. Absorption properties of identical atoms

    NASA Astrophysics Data System (ADS)

    Sancho, Pedro

    2013-09-01

    Emission rates and other optical properties of multi-particle systems in collective and entangled states differ from those in product ones. We show the existence of similar effects in the absorption probabilities for (anti)symmetrized states of two identical atoms. The effects strongly depend on the overlapping between the atoms and differ for bosons and fermions. We propose a viable experimental verification of these ideas.

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

    ERIC Educational Resources Information Center

    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)…

  6. Do Atoms Really "Emit" Absorption Lines?

    ERIC Educational Resources Information Center

    Brecher, Kenneth

    1991-01-01

    Presents three absorption line sources that enhance student understanding of the phenomena associated with the interaction of light with matter and help dispel the misconception that atoms "emit" absorption lines. Sources include neodymium, food coloring and other common household liquids, and fluorescent materials. (MDH)

  7. Detection of palladium by cold atom solution atomic absorption.

    PubMed

    Molloy, John L; Holcombe, James A

    2006-09-15

    One of the largest obstacles in miniaturizing traditional atomic spectroscopic sources is the need for a thermal/electrical source for free atom production. A single article in the literature has demonstrated atomic absorption detection of Ag, Cu, and Pd in solution at room temperature for atoms in the gas phase, which may ultimately permit miniaturization. Unfortunately, several laboratories have found that reproducing the phenomenon has been difficult. Without a sound fundamental explanation of the processes leading to the signal, one must conclude that it can be done, but some unsuspected and unknown design/methodological nuances are responsible for only a single reported success. Gas phase atoms could exist at room temperature "in solution" if the atoms were trapped in very small bubbles. In the current study, submicrometer-sized bubbles were created in a flow-through cell during the mixing of an alcohol-water solution containing a reducing agent with water containing the analyte. A repeatable atomic absorption signal was produced. Replacement of ethanol with 1-propanol and use of a surfactant increased the signal. Limits of detection of approximately 100 ppb in Pd were achieved, and it is estimated that approximately 0.4% of the Pd initially added is contained within the bubbles as gaseous atoms. The paper discusses the fundamental processes needed to achieve a repeatable signal. PMID:16970344

  8. Simultaneous multielement atomic absorption spectrometry with graphite furnace atomization

    NASA Astrophysics Data System (ADS)

    Harnly, James M.; Miller-Ihli, Nancy J.; O'Haver, Thomas C.

    The extended analytical range capability of a simultaneous multielement atomic absorption continuum source spectrometer (SIMAAC) was tested for furnace atomization with respect to the signal measurement mode (peak height and area), the atomization mode (from the wall or from a platform), and the temperature program mode (stepped or ramped atomization). These parameters were evaluated with respect to the shapes of the analytical curves, the detection limits, carry-over contamination and accuracy. Peak area measurements gave more linear calibration curves. Methods for slowing the atomization step heating rate, the use of a ramped temperature program or a platform, produced similar calibration curves and longer linear ranges than atomization with a stepped temperature program. Peak height detection limits were best using stepped atomization from the wall. Peak area detection limits for all atomization modes were similar. Carry-over contamination was worse for peak area than peak height, worse for ramped atomization than stepped atomization, and worse for atomization from a platform than from the wall. Accurate determinations (100 ± 12% for Ca, Cu, Fe, Mn, and Zn in National Bureau of Standards' Standard Reference Materials Bovine Liver 1577 and Rice Flour 1568 were obtained using peak area measurements with ramped atomization from the wall and stepped atomization from a platform. Only stepped atomization from a platform gave accurate recoveries for K. Accurate recoveries, 100 ± 10%, with precisions ranging from 1 to 36 % (standard deviation), were obtained for the determination of Al, Co, Cr, Fe, Mn, Mo, Ni. Pb, V and Zn in Acidified Waters (NBS SRM 1643 and 1643a) using stepped atomization from a platform.

  9. Atomic absorption spectroscopy with high temperature flames.

    PubMed

    Willis, J B

    1968-07-01

    An account is given of the history of the development of high temperature flames for the atomic absorption measurement of metals forming refractory oxides. The principles governing the design of premix burners for such flames, and the relative merits of different types of nebulizer burner systems are described. After a brief account of the structure and emission characteristics of the premixed oxygen-acetylene and nitrous oxide-acetylene flames, the scope and limitations of the latter flame in chemical analysis are discussed. PMID:20068790

  10. Continuum Absorption Coefficient of Atoms and Ions

    NASA Technical Reports Server (NTRS)

    Armaly, B. F.

    1979-01-01

    The rate of heat transfer to the heat shield of a Jupiter probe has been estimated to be one order of magnitude higher than any previously experienced in an outer space exploration program. More than one-third of this heat load is due to an emission of continuum radiation from atoms and ions. The existing computer code for calculating the continuum contribution to the total load utilizes a modified version of Biberman's approximate method. The continuum radiation absorption cross sections of a C - H - O - N ablation system were examined in detail. The present computer code was evaluated and updated by being compared with available exact and approximate calculations and correlations of experimental data. A detailed calculation procedure, which can be applied to other atomic species, is presented. The approximate correlations can be made to agree with the available exact and experimental data.

  11. Les possibilités et limitations de l'atomisation électrothermique en spectrométrie d'absorption atomique lors de l'analyse directe des metaux lourds dans l'eau de mer

    NASA Astrophysics Data System (ADS)

    Hoenig, M.; Wollast, R.

    This work shows the analytical possibilities of an electrothermal atomizer for the direct determination of trace metals in sea-water. The high background signals generated by the matrix perturb in particular volatile elements because of the low decomposition temperature allowed. In the case of cadmium, addition of ascorbic acid to the sample permits the modification of the atomization mechanism and the reduction of the optimum temperature. Under these conditions, absorption peak of the cadmium precedes the background absorption and consequently the analysis is no longer limited by the magnitude of the matrix signal: the determination of cadmium concentrations far below the μg -1 level is easily possible. Although the direct determination of the other elements should be in principle less disturbed by the background, the analytical performance is poorer than for cadmium. Limits of determination of the order from 0.1 to 1 μg -1 can be reached for chromium, copper and manganese. Lead and nickel appeared to be the most difficult elements; their direct determination is only possible in polluted coastal or estuarine waters. The injection of the sample as an aerosol into hot graphite tube showed to be well adapted to this kind of investigations. The simultaneous visualization of specific and background signals allows interpretations which until now were impossible with commercially available apparatus.

  12. 2. VIEW IN ROOM 111, ATOMIC ABSORPTION BERYLLIUM ANALYSIS LABORATORY. ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    2. VIEW IN ROOM 111, ATOMIC ABSORPTION BERYLLIUM ANALYSIS LABORATORY. AIR FILTERS AND SWIPES ARE DISSOLVED WITH ACIDS AND THE REMAINING RESIDUES ARE SUSPENDED IN NITRIC ACID SOLUTION. THE SOLUTION IS PROCESSED THROUGH THE ATOMIC ABSORPTION SPECTROPHOTOMETER TO DETECT THE PRESENCE AND LEVELS OF BERYLLIUM. - Rocky Flats Plant, Health Physics Laboratory, On Central Avenue between Third & Fourth Streets, Golden, Jefferson County, CO

  13. Flameless atomic-absorption determination of gold in geological materials

    USGS Publications Warehouse

    Meier, A.L.

    1980-01-01

    Gold in geologic material is dissolved using a solution of hydrobromic acid and bromine, extracted with methyl isobutyl ketone, and determined using an atomic-absorption spectrophotometer equipped with a graphite furnace atomizer. A comparison of results obtained by this flameless atomic-absorption method on U.S. Geological Survey reference rocks and geochemical samples with reported values and with results obtained by flame atomic-absorption shows that reasonable accuracy is achieved with improved precision. The sensitivity, accuracy, and precision of the method allows acquisition of data on the distribution of gold at or below its crustal abundance. ?? 1980.

  14. Determination of iridium in mafic rocks by atomic absorption

    USGS Publications Warehouse

    Grimaldi, F.S.; Schnepfe, M.M.

    1970-01-01

    Iridium is determined in mineralized mafic rocks by atomic absorption after fire-assay concentration into a gold bead. Interelement interferences in the atomic-absorption determination are removed and Ir sensitivity is increased by buffering the solutions with a mixture of copper and sodium sulphates. Substantial amounts of Ag, Al, Au, Bi, Ca, Cd, Co, Cr, Fe, Ho, Hg, K, La, Mg, Mn, Mo, Ni, Pb, Te, Ti, V, Y, Zn and platinum metals can be tolerated in the atomic-absorption determination. The sensitivity and detection limits are 3.2 and 0.25 ppm of Ir, respectively. ?? 1970.

  15. Visualizing the Solute Vaporization Interference in Flame Atomic Absorption Spectroscopy

    ERIC Educational Resources Information Center

    Dockery, Christopher R.; Blew, Michael J.; Goode, Scott R.

    2008-01-01

    Every day, tens of thousands of chemists use analytical atomic spectroscopy in their work, often without knowledge of possible interferences. We present a unique approach to study these interferences by using modern response surface methods to visualize an interference in which aluminum depresses the calcium atomic absorption signal. Calcium…

  16. Perfect electromagnetic absorption at one-atom-thick scale

    SciTech Connect

    Li, Sucheng; Duan, Qian; Li, Shuo; Yin, Qiang; Lu, Weixin; Li, Liang; Hou, Bo; Gu, Bangming; Wen, Weijia

    2015-11-02

    We experimentally demonstrate that perfect electromagnetic absorption can be realized in the one-atom thick graphene. Employing coherent illumination in the waveguide system, the absorbance of the unpatterned graphene monolayer is observed to be greater than 94% over the microwave X-band, 7–13 GHz, and to achieve a full absorption, >99% in experiment, at ∼8.3 GHz. In addition, the absorption characteristic manifests equivalently a wide range of incident angle. The experimental results agree very well with the theoretical calculations. Our work accomplishes the broadband, wide-angle, high-performance absorption in the thinnest material with simple configuration.

  17. Atomic-absorption determination of rhodium in chromite concentrates

    USGS Publications Warehouse

    Schnepfe, M.M.; Grimaldi, F.S.

    1969-01-01

    Rhodium is determined in chromite concentrates by atomic absorption after concentration either by co-precipitation with tellurium formed by the reduction of tellurite with tin(II) chloride or by fire assay into a gold bead. Interelement interferences in the atomic-absorption determination are removed by buffering the solutions with lanthanum sulphate (lanthanum concentration 1%). Substantial amounts of Ag, Al, Au, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ho, Hg, K, La, Mg, Mn, Mo, Na, Ni, Pb, Te, Ti, V, Y, Zn and platinum metals can be tolerated. A lower limit of approximately 0.07 ppm Rh can be determined in a 3-g sample. ?? 1969.

  18. Determination of palladium and platinum by atomic absorption

    USGS Publications Warehouse

    Schnepfe, M.M.; Grimaldi, F.S.

    1969-01-01

    Palladium and platinum are determined by atomic absorption after fire-assay concentration into a gold bead. The limit of determination is ~0??06 ppm in a 20-g sample. Serious depressive interelement interferences are removed by buffering the solutions with a mixture of cadmium and copper sulphates with cadmium and copper concentrations each at 0??5%. Substantial amounts of Ag, Al, Au, Bi, Ca, Co, Cr, Fe, Hg, K, La, Mg, Mn, Mo, Na, Ni, Pb, Te, Ti, V, Y, Zn, and the platinum metals do not interfere in the atomic-absorption determination. ?? 1969.

  19. Speciation of mercury compounds by differential atomization - atomic absorption spectroscopy

    SciTech Connect

    Robinson, J.W.; Skelly, E.M.

    1982-01-01

    This paper describes the dual stage atomization technique which allows speciation of several mercury-containing compounds in aqueous solution and in biological fluids. The technique holds great promise for further speciation studies. Accurate temperature control, expecially at temperatures less than 200/sup 0/C, is needed to separate the extremely volatile mercury halides and simple organomercurials from each other. Studies with mercury salts and EDTA, L-cysteine and dithioxamide demonstrate that this technique may be used to study the extent of complex formation. Investigations of biological fluids indicate that there is a single predominant form of mercury in sweat and a single predominant form of mercury in urine. The mercury compound in urine is more volatile than that in sweat. Both quantitative and qualitative analyses are possible with this technique.

  20. COMPUTER-ASSISTED FURNACE ATOMIC ABSORPTION SPECTROMETRIC ANALYSIS

    EPA Science Inventory

    The use of furnace atomic absorption instrumentation with a turnkey chromatography data system is described. A simple addition of relays to the furnace power supply allows for automatic start-up of A/D conversion and spectrophotometer zeroing at the proper time. Manipulations inv...

  1. Atomic Absorption Spectroscopy. The Present and the Future.

    ERIC Educational Resources Information Center

    Slavin, Walter

    1982-01-01

    The status of current techniques and methods of atomic absorption (AA) spectroscopy (flame, hybrid, and furnace AA) is discussed, including limitations. Technological opportunities and how they may be used in AA are also discussed, focusing on automation, microprocessors, continuum AA, hybrid analyses, and others. (Author/JN)

  2. A COMPUTER CONTROL AND ACQUISITION SYSTEM FOR ATOMIC ABSORPTION DATA

    EPA Science Inventory

    A system is presented that controls and acquires data from a Perkin-Elmer 603 or similar atomic absorption spectrophotometer operating in the flame mode and equipped with a 200 place auto-sampler. The hardware consists of a PDP11 computer with minimum peripheral equipment and a s...

  3. Developing a Transdisciplinary Teaching Implement for Atomic Absorption Spectroscopy

    ERIC Educational Resources Information Center

    Drew, John

    2008-01-01

    In this article I explain why I wrote the set of teaching notes on Atomic Absorption Spectroscopy (AAS) and why they look the way they do. The notes were intended as a student reference to question, highlight and write over as much as they wish during an initial practical demonstration of the threshold concept being introduced, in this case…

  4. Induced absorption and annihilation in hadronic hydrogen atoms

    NASA Astrophysics Data System (ADS)

    Pomerantsev, Vladimir N.; Popov, Vladimir P.

    The induced absorption or annihilation in the collisions of the hydrogen hadronic atoms in the excited states with ordinary hydrogen have been described in a unified manner with the elastic scattering, Stark transitions, and Coulomb de-excitation in the framework of a close-coupling approach including both the open and closed channels corresponding to both the stationary and non-stationary states of hadronic atom. The general features of the induced absorption cross sections have been studied in a wide range of the complex energy-shift values. The total and differential cross sections of all processes have been calculated for π - p, K - p, and bar p p atoms with the principal quantum numbers n = 2 - 8 and kinetic energy from 0.001 eV up to 100 eV.

  5. Induced absorption and annihilation in hadronic hydrogen atoms

    NASA Astrophysics Data System (ADS)

    Pomerantsev, Vladimir N.; Popov, Vladimir P.

    2012-05-01

    The induced absorption or annihilation in the collisions of the hydrogen hadronic atoms in the excited states with ordinary hydrogen have been described in a unified manner with the elastic scattering, Stark transitions, and Coulomb de-excitation in the framework of a close-coupling approach including both the open and closed channels corresponding to both the stationary and non-stationary states of hadronic atom. The general features of the induced absorption cross sections have been studied in a wide range of the complex energy-shift values. The total and differential cross sections of all processes have been calculated for π - p, K - p, and bar p p atoms with the principal quantum numbers n = 2 - 8 and kinetic energy from 0.001 eV up to 100 eV.

  6. Coherent Enhanced Absorption in an Intracavity Atomic Medium

    NASA Astrophysics Data System (ADS)

    Smith, David D.; Myneni, Krishna; Chang, Hongrok; Odutola, Jamiu A.

    2011-05-01

    The conditions for coherent enhanced absorption of an intracavity atomic medium are discussed. For a symmetric cavity, a specific amplitude and phase relationship between two oppositely oriented input beams results in coherent perfect absorption by the medium. In contrast, for a single input beam, perfect absorption requires a perfectly asymmetric, i.e., single port, cavity. Even when the cavity is not perfectly asymmetric or lossless, we find that enhanced absorption can occur. For a single input to an asymmetric cavity, as the input intensity is increased and the medium saturates, the cavity passes from the over-coupled to the under-coupled regime. We find the counterintuitive result that the cavity absorptance can increase with increasing input intensity in the over-coupled regime, i.e., the atom-cavity system behaves as a reverse saturable absorber. These results were compared with measurements performed using a tunable laser incident on a Fabry-Perot cavity containing an Rb87 cell, taking into account the effects of saturation and beam divergence.

  7. [Application of atomic absorption spectrometry in the engine knock detection].

    PubMed

    Chen, Li-Dan

    2013-02-01

    Because existing human experience diagnosis method and apparatus for auxiliary diagnosis method are difficult to diagnose quickly engine knock. Atomic absorption spectrometry was used to detect the automobile engine knock in in innovative way. After having determined Fe, Al, Cu, Cr and Pb content in the 35 groups of Audi A6 engine oil whose travel course is 2 000 -70 000 kilometers and whose sampling interval is 2 000 kilometers by atomic absorption spectrometry, the database of primary metal content in the same automobile engine at different mileage was established. The research shows that the main metal content fluctuates within a certain range. In practical engineering applications, after the determination of engine oil main metal content and comparison with its database value, it can not only help to diagnose the type and location of engine knock without the disintegration and reduce vehicle maintenance costs and improve the accuracy of engine knock fault diagnosis. PMID:23697150

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

    USGS Publications Warehouse

    Kane, J.S.

    1979-01-01

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

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

    USGS Publications Warehouse

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

    1984-01-01

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

  10. A thin-walled metallic hollow cathode as an atomizer for Zeeman atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Ganeyev, A. A.; Sholupov, S. E.

    1998-03-01

    A new kind of glow discharge atomizer, a thin-walled metallic hollow cathode (TMHC) combined with Zeeman atomic absorption spectrometry using high frequency modulated light polarization (ZAAS-HFM), is studied. A theoretically suggested, and experimentally confirmed, model of the atom confinement in the TMHC yields the appearance of the diffusion traps for atoms at both ends of the cathode, which increases the residence time of the analyte atoms in the analysis volume. The high atomization efficiency in the glow discharge atomizer (caused by the ionic-thermal mechanism of sputtering) and the high selectivity of ZAAS-HFM are demonstrated in the analysis of complex matrix samples such as whole blood and urine. The analytical system TMHC + ZAAS-HFM is characterized by low detection limits, which are comparable to those of graphite furnace atomic absorption spectrometry (GFAAS). Owing to its rather low average power consumption (30-50 W) the TMHC can be used in a portable and mobile spectrometer, and is therefore suitable for the in situ analysis of various sample materials.

  11. 21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and...

  12. 21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and...

  13. 21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and...

  14. 21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and...

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

    PubMed

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

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC. PMID:15910814

  16. A Comprehensive X-Ray Absorption Model for Atomic Oxygen

    NASA Technical Reports Server (NTRS)

    Gorczyca, T. W.; Bautista, M. A.; Hasoglu, M. F.; Garcia, J.; Gatuzz, E.; Kaastra, J. S.; Kallman, T. R.; Manson, S. T.; Mendoza, C.; Raassen, A. J. J.; de Vries, C. P.; Zatsarinny, O.

    2013-01-01

    An analytical formula is developed to accurately represent the photoabsorption cross section of atomic Oxygen for all energies of interest in X-ray spectral modeling. In the vicinity of the K edge, a Rydberg series expression is used to fit R-matrix results, including important orbital relaxation effects, that accurately predict the absorption oscillator strengths below threshold and merge consistently and continuously to the above-threshold cross section. Further, minor adjustments are made to the threshold energies in order to reliably align the atomic Rydberg resonances after consideration of both experimental and observed line positions. At energies far below or above the K-edge region, the formulation is based on both outer- and inner-shell direct photoionization, including significant shake-up and shake-off processes that result in photoionization-excitation and double-photoionization contributions to the total cross section. The ultimate purpose for developing a definitive model for oxygen absorption is to resolve standing discrepancies between the astronomically observed and laboratory-measured line positions, and between the inferred atomic and molecular oxygen abundances in the interstellar medium from XSTAR and SPEX spectral models.

  17. The determination of vanadium in brines by atomic absorption spectroscopy

    USGS Publications Warehouse

    Crump-Wiesner, Hans J.; Feltz, H.R.; Purdy, W.C.

    1971-01-01

    A standard addition method is described for the determination of vanadium in brines by atomic absorption spectroscopy with a nitrous oxide-acetylene flame. Sample pH is adjusted to 1.0 with concentrated hydrochloric acid and the vanadium is directly extracted with 5% cupferron in methyl isobutyl ketone (MIBK). The ketone layer is then aspirated into the flame and the recorded absorption values are plotted as a function of the concentration of the added metal. As little as 2.5 ??g l-1 of vanadium can be detected under the conditions of the procedure. Tungsten and tin interfere when present in excess of 5 and 10 ??g ml-1, respectively. The concentrations of the two interfering ions normally found in brines are well below interference levels. ?? 1971.

  18. Performance characteristics of an S-600 portable atomic absorption spectrophotometer

    SciTech Connect

    Pelieva, L.A.; Dyndar, Zh.I.

    1995-12-01

    Performance characteristics of an S-600 portable atomic absorption spectrophotometer are discussed. The optimum analysis conditions, characteristic mass, and detection limit for determining Be, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, and Zn in solutions and in powders are specified. Direct analysis of solid-state samples (standard soil samples) is described. The relative error of measurement by the calibration graph method lies, with few exceptions, within 7-30%, and by the addition method, within 4-20%. The time needed for a single element determination is 10-20 min.

  19. A heated chamber burner for atomic absorption spectroscopy.

    PubMed

    Venghiattis, A A

    1968-07-01

    A new heated chamber burner is described. The burner is of the premixed type, and burner heads of the types conventionally used in atomic absorption may be readily adapted to it. This new sampling system has been tested for Ag, Al, Ca, Cu, Fe, Mg, Mn, Ni, Pb, Si, Ti, and Zn in aqueous solutions. An improvement of the order of ten times has been obtained in sensitivity, and in detection limits as well, for the elements determined. Interferences controllable are somewhat more severe than in conventional burners but are controllable. PMID:20068792

  20. Measuring Microwaves via Absorption and Dispersion in Rydberg Atoms

    NASA Astrophysics Data System (ADS)

    Stack, Daniel; Kunz, Paul; Meyer, David; Solmeyer, Neal

    2016-05-01

    Weak microwave frequency electromagnetic fields can be difficult to detect and fully characterize with traditional methods. However it is possible to transduce the measurement of these fields from the microwave domain to the optical domain via resonant transitions between Rydberg levels in atomic vapors using electromagnetically-induced transparency and the Autler-Townes effect. This technique allows for sensitive measurements of the microwave field amplitude, polarization, and spatial waveform (via the position of the probe and coupling laser beams) as compared to measurements performed with dipole antennas. We are able to obtain these quantities by monitoring the properties of a probe laser beam as it passes through a rubidium vapor cell. Previous experiments using Rydberg spectroscopy have typically relied on measuring the absorption of the probe laser as it passed through the atomic system. We report on progress to use the polarization rotation of the probe as it passes through the atoms in a static magnetic field, which corresponds to the real part of the susceptibility of the atomic medium, for measuring the characteristics of a microwave frequency signal. This effect is known as Nonlinear Magneto Optical Rotation (NMOR) and has been used for sensitive magnetometry.

  1. Oscillator strength measurements of atomic absorption lines from stellar spectra

    NASA Astrophysics Data System (ADS)

    Lobel, Alex

    2011-05-01

    Herein we develop a new method to determine oscillator strength values of atomic absorption lines with state-of-the-art detailed spectral synthesis calculations of the optical spectrum of the Sun and of standard spectral reference stars. We update the log(gf) values of 911 neutral lines observed in the KPNO-FTS flux spectrum of the Sun and high-resolution echelle spectra (R = 80 000) of Procyon (F5 IV-V) and Eps Eri (K2 V) observed with large signal-to-noise (S/N) ratios of 2000 using the new Mercator-Hermes spectrograph at La Palma Observatory (Spain). We find for 483 Fe I, 85 Ni I, and 51 Si I absorption lines in the sample a systematic overestimation of the literature log(gf) values with central line depths below 15%. We employ a curve-of-growth analysis technique to test the accuracy of the new oscillator strength values and compare calculated equivalent line widths to the Moore, Minnaert, and Houtgast atlas of the Sun. The online SpectroWeb database at http://spectra.freeshell.org interactively displays the observed and synthetic spectra and provides the new log(gf) values together with important atomic line data. The graphical database is under development for stellar reference spectra of every spectral sub-class observed with large spectral resolution and S/N ratios.

  2. A comprehensive X-ray absorption model for atomic oxygen

    SciTech Connect

    Gorczyca, T. W.; Bautista, M. A.; Mendoza, C.; Hasoglu, M. F.; García, J.; Gatuzz, E.; Kaastra, J. S.; Raassen, A. J. J.; De Vries, C. P.; Kallman, T. R.; Manson, S. T.; Zatsarinny, O.

    2013-12-10

    An analytical formula is developed to accurately represent the photoabsorption cross section of O I for all energies of interest in X-ray spectral modeling. In the vicinity of the K edge, a Rydberg series expression is used to fit R-matrix results, including important orbital relaxation effects, that accurately predict the absorption oscillator strengths below threshold and merge consistently and continuously to the above-threshold cross section. Further, minor adjustments are made to the threshold energies in order to reliably align the atomic Rydberg resonances after consideration of both experimental and observed line positions. At energies far below or above the K-edge region, the formulation is based on both outer- and inner-shell direct photoionization, including significant shake-up and shake-off processes that result in photoionization-excitation and double-photoionization contributions to the total cross section. The ultimate purpose for developing a definitive model for oxygen absorption is to resolve standing discrepancies between the astronomically observed and laboratory-measured line positions, and between the inferred atomic and molecular oxygen abundances in the interstellar medium from XSTAR and SPEX spectral models.

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

    NASA Astrophysics Data System (ADS)

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

    2006-05-01

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

  4. Transient absorption spectra of the laser-dressed hydrogen atom

    NASA Astrophysics Data System (ADS)

    Murakami, Mitsuko; Chu, Shih-I.

    2013-10-01

    We present a theoretical study of transient absorption spectra of laser-dressed hydrogen atoms, based on numerical solutions of the time-dependent Schrödinger equation. The timing of absorption is controlled by the delay between an extreme ultra violet (XUV) pulse and an infrared (IR) laser field. The XUV pulse is isolated and several hundred attoseconds in duration, which acts as a pump to drive the ground-state electron to excited p states. The subsequent interaction with the IR field produces dressed states, which manifest as sidebands between the 1s-np absorption spectra separated by one IR-photon energy. We demonstrate that the population of dressed states is maximized when the timing of the XUV pulse coincides with the zero crossing of the IR field, and that their energies can be manipulated in a subcycle time scale by adding a chirp to the IR field. An alternative perspective to the problem is to think of the XUV pulse as a probe to detect the dynamical ac Stark shifts. Our results indicate that the accidental degeneracy of the hydrogen excited states is removed while they are dressed by the IR field, leading to large ac Stark shifts. Furthermore, we observe the Autler-Townes doublets for the n=2 and 3 levels using the 656 nm dressing field, but their separation does not agree with the prediction by the conventional three-level model that neglects the dynamical ac Stark shifts.

  5. Direct analysis of solids by graphite furnace atomic absorption spectrometry using a second surface atomizer

    SciTech Connect

    Rettberg, T.M.; Holcombe, J.A.

    1986-06-01

    The direct graphite furnace atomic absorption spectrometric analysis of solids using the second surface atomizer has been investigated. The atomizer features a gas-cooled Ta insert within the graphite furnace onto which the analyte can be condensed, after which atomization is performed by raising the furnace to a higher temperature and shutting off the coolant gas. The analyses were conducted on standard reference material fly ash, river sediment, and citrus leaves, in addition to filter paper samples. All analyses were conducted without sample pretreatment or use of matrix modifiers. Quantitation was done by using simple aqueous standards. By use of peak heights, the recoveries varied from 81% to 127%, although several determinations were within the certified concentration range. The procedures typically gave low background absorbances and peak shapes that were relatively independent of the original sample matrix.

  6. WIPP Benchmark calculations with the large strain SPECTROM codes

    SciTech Connect

    Callahan, G.D.; DeVries, K.L.

    1995-08-01

    This report provides calculational results from the updated Lagrangian structural finite-element programs SPECTROM-32 and SPECTROM-333 for the purpose of qualifying these codes to perform analyses of structural situations in the Waste Isolation Pilot Plant (WIPP). Results are presented for the Second WIPP Benchmark (Benchmark II) Problems and for a simplified heated room problem used in a parallel design calculation study. The Benchmark II problems consist of an isothermal room problem and a heated room problem. The stratigraphy involves 27 distinct geologic layers including ten clay seams of which four are modeled as frictionless sliding interfaces. The analyses of the Benchmark II problems consider a 10-year simulation period. The evaluation of nine structural codes used in the Benchmark II problems shows that inclusion of finite-strain effects is not as significant as observed for the simplified heated room problem, and a variety of finite-strain and small-strain formulations produced similar results. The simplified heated room problem provides stratigraphic complexity equivalent to the Benchmark II problems but neglects sliding along the clay seams. The simplified heated problem does, however, provide a calculational check case where the small strain-formulation produced room closures about 20 percent greater than those obtained using finite-strain formulations. A discussion is given of each of the solved problems, and the computational results are compared with available published results. In general, the results of the two SPECTROM large strain codes compare favorably with results from other codes used to solve the problems.

  7. The role of atomic absorption spectrometry in geochemical exploration

    USGS Publications Warehouse

    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.

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

    PubMed

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-06-01

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

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

    ERIC Educational Resources Information Center

    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…

  10. Electrothermal atomic absorption spectrometry determination of molybdenum in whole blood

    NASA Astrophysics Data System (ADS)

    Burguera, J. L.; Rondón, C.; Burguera, M.; Roa, M. E.; Petit de Peña, Y.

    2002-03-01

    A method for the determination of molybdenum in whole blood by atomic absorption spectrometry with electrothermal atomization was developed and evaluated. Erbium (25 μg) was chosen from several potential chemical modifiers (Sm, Lu, Ho, Eu and Pd+Mg) as the most appropriate for the sensitive and reliable determination of molybdenum in such sample. The process used was direct dilution of the sample in a ratio 1:2 with a 0.1% (v/v) Triton X-100 solution. The injection of 20 μl of a solution of 15% (w/v) hydrogen peroxide and running the temperature program after 5 firings greatly reduced the effect of build-up of carbonaceous residues within the atomizer. The limit of detection and working ranges, respectively, were 0.6 and 2.0-100.0 μg l -1, and the characteristic mass was 7.2 pg. The relative standard deviation varied from 0.8 to 1.5% for within and between batch determinations, respectively. The determination of molybdenum in Seronorm™ Trace Elements in Whole Blood with known added amounts of the analyte was performed to asses the accuracy. The optimized procedure has been applied to the determination of molybdenum in whole blood specimens of 20 subjects taken before and 10-12 h after receiving an over-supply of 1 mg of molybdenum. The molybdenum concentrations (±S.D.) were 10.9±0.4 μg Mo l -1 (range 9.9-11.6 μg Mo l -1) and 15.4±0.4 μg Mo l -1 (range 13.1-16.9 μg Mo l -1) for the individuals before and after the administration of molybdenum.

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

    NASA Astrophysics Data System (ADS)

    Řezáčová, Olga; Dědina, Jiří

    2009-07-01

    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. Etalon-induced baseline drift and correction in atom flux sensors based on atomic absorption spectroscopy

    SciTech Connect

    Du, Yingge; Chambers, Scott A.

    2014-10-20

    Atom flux sensors based on atomic absorption (AA) spectroscopy are of significant interest in thin film growth as they can provide unobtrusive, element specific real-time flux sensing and control. The ultimate sensitivity and performance of these sensors are strongly affected by baseline drift. Here we demonstrate that an etalon effect resulting from temperature changes in optical viewport housings is a major source of signal instability, which has not been previously considered, and cannot be corrected using existing methods. We show that small temperature variations in the fused silica viewports can introduce intensity modulations of up to 1.5% which in turn significantly deteriorate AA sensor performance. This undesirable effect can be at least partially eliminated by reducing the size of the beam and tilting the incident light beam off the viewport normal.

  13. Etalon-induced Baseline Drift And Correction In Atom Flux Sensors Based On Atomic Absorption Spectroscopy

    SciTech Connect

    Du, Yingge; Chambers, Scott A.

    2014-10-20

    Atom flux sensors based on atomic absorption (AA) spectroscopy are of significant interest in thin film growth as they can provide unobtrusive, element specific, real-time flux sensing and control. The ultimate sensitivity and performance of the sensors are strongly affected by the long-term and short term baseline drift. Here we demonstrate that an etalon effect resulting from temperature changes in optical viewport housings is a major source of signal instability which has not been previously considered or corrected by existing methods. We show that small temperature variations in the fused silica viewports can introduce intensity modulations of up to 1.5%, which in turn significantly deteriorate AA sensor performance. This undesirable effect can be at least partially eliminated by reducing the size of the beam and tilting the incident light beam off the viewport normal.

  14. Light absorption during alkali atom-noble gas atom interactions at thermal energies: a quantum dynamics treatment.

    PubMed

    Pacheco, Alexander B; Reyes, Andrés; Micha, David A

    2006-10-21

    The absorption of light during atomic collisions is treated by coupling electronic excitations, treated quantum mechanically, to the motion of the nuclei described within a short de Broglie wavelength approximation, using a density matrix approach. The time-dependent electric dipole of the system provides the intensity of light absorption in a treatment valid for transient phenomena, and the Fourier transform of time-dependent intensities gives absorption spectra that are very sensitive to details of the interaction potentials of excited diatomic states. We consider several sets of atomic expansion functions and atomic pseudopotentials, and introduce new parametrizations to provide light absorption spectra in good agreement with experimentally measured and ab initio calculated spectra. To this end, we describe the electronic excitation of the valence electron of excited alkali atoms in collisions with noble gas atoms with a procedure that combines l-dependent atomic pseudopotentials, including two- and three-body polarization terms, and a treatment of the dynamics based on the eikonal approximation of atomic motions and time-dependent molecular orbitals. We present results for the collision induced absorption spectra in the Li-He system at 720 K, which display both atomic and molecular transition intensities. PMID:17059261

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

    USGS Publications Warehouse

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

    1967-01-01

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

  16. Absorption-free Bragg reflector using Zeeman sublevels in atomic vapor.

    PubMed

    Chen, Zhongjie; Luo, Bin; Guo, Hong

    2014-06-30

    Absorption-free Bragg reflector has been studied in ions doped in crystals. We propose a new scheme using Zeeman sublevels of atoms to construct an absorption-free Bragg reflector with practical laser power. Its spatial period of refractive index equals half of the wavelength of the incident standing-wave coupling light. The proposal is simulated in a helium atom scheme, and can be extended to alkali earth atoms. PMID:24977814

  17. Electrothermal atomic absorption spectrophotometry of nickel in tissue homogenates.

    PubMed

    Sunderman, F W; Marzouk, A; Crisostomo, M C; Weatherby, D R

    1985-01-01

    A method for analysis of Ni concentrations in tissues is described, which involves (a) tissue dissection with metal-free obsidian knives, (b) tissue homogenization in polyethylene bags by use of a "Stomacher" blender, (c) oxidative digestion with mixed nitric, sulfuric, and perchloric acids, and (d) quantitation of Ni by electrothermal atomic absorption spectrophotometry with Zeeman background correction. The detection limit for Ni in tissues is 10 ng per g, dry weight; the coefficient of variation ranges from 7 to 15 percent, depending on the tissue Ni concentration; the recovery of Ni added in concentration of 20 ng per g, dry weight, to kidney homogenates averages 101 +/- 8 percent (mean +/- SD). In control rats, Ni concentrations are highest in lung (102 +/- 39 ng per g, dry weight) and lowest in spleen (35 +/- 16 ng per g, dry wt.). In descending order of Ni concentrations, the tissues of control rats rank as follows: lung greater than heart greater than bone greater than kidney greater than brain greater than testis greater than fat greater than liver greater than spleen. In rats killed 24 h after sc injection of NiCl2 (0.125 mmol per kg, body weight) Ni concentrations are highest in kidney (17.7 +/- 2.5 micrograms per g, dry weight) and lowest in brain (0.38 +/- 0.14 micrograms per g, dry weight). In descending order of Ni concentrations, the tissues of NiCl2-treated rats rank as follows: kidney much greater than lung greater than spleen greater than testis greater than heart greater than fat greater than liver greater than bone greater than brain.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:4037701

  18. Electrothermal atomic absorption spectrophotometry of nickel in tissue homogenates

    SciTech Connect

    Sunderman, F.W. Jr.; Marzouk, A.; Crisostomo, M.C.; Weatherby, D.R.

    1985-01-01

    A method for analysis of Ni concentrations in tissues is described, which involves (a) tissue dissection with metal-free obsidian knives, (b) tissue homogenization in polyethylene bags by use by a Stomacher blender, (c) oxidative digestion with mixed nitric, sulfuric, and perchloric acids, and (d) quantitation of Ni by electrothermal atomic absorption spectrophotometry with Zeeman background correction. The detection limit for Ni in tissues is 10 ng per g, dry weight; the coefficient of variation ranges from 7 to 15%, depending on the tissue Ni concentration; the recovery of Ni added in concentration of 20 ng per g, dry weight, to kidney homogenates averages 101 +/- 8% (mean +/-SD). In control rats, Ni concentrations are highest in lung (102 +/- 39 ng per g, dry weight) and lowest in spleen (35 +/- 16 ng per g, dry wt.). In descending order of Ni concentrations, the tissues of control rats rank as follows: lung > heart > bone > kidney > brain > testis > fat > liver > spleen. In rats killed 24 h after sc injection of NiCl/sub 2/ (0.125 mmol per kg, body weight) Ni concentrations are highest in kidney (17.7 +/- 2.5 ..mu..g per g, dry weight) and lowest in brain (0.38 +/- 0.14 ..mu..g per g, dry weight). In descending order of Ni concentrations, the tissues of NiCl/sub 2/-treated rats rank as follows: kidney >> lung > spleen > testis > heart > fat > liver > bone > brain. The present method fills the need for an accurate, sensitive, and practical technique to determine tissue Ni concentrations, with stringent precautions to minimize Ni contamination during tissue sampling and processing. 35 references, 5 figures, 1 table.

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

    PubMed

    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. PMID:15561625

  20. Uranium isotopes quantitatively determined by modified method of atomic absorption spectrophotometry

    NASA Technical Reports Server (NTRS)

    Lee, G. H.

    1967-01-01

    Hollow-cathode discharge tubes determine the quantities of uranium isotopes in a sample by using atomic absorption spectrophotometry. Dissociation of the uranium atoms allows a large number of ground state atoms to be produced, absorbing the incident radiation that is different for the two major isotopes.

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

    PubMed

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

    2012-01-01

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

  2. Atomic-absorption determination of beryllium in geological materials by use of electrothermal atomization

    USGS Publications Warehouse

    Campbell, E.Y.; Simon, F.O.

    1978-01-01

    A method is described for the atomic-absorption determination of beryllium in geological materials, that utilizes electrothermal atomization after a separation by solvent extraction. Samples are decomposed with hydrofluoric acid and nitric acid in Teflon-lined pressure decomposition vessels. Beryllium is isolated by its extraction as beryllium acetylacetonate at pH 8 into xylene and back-extraction in 3M hydrochloric acid. The method has been successfully applied to the determination of beryllium in 14 U.S. Geological Survey standard rocks. Four subsamples from four bottles of each standard sample were analysed in random order. The mean beryllium contents (ppm) are: AGV-1, 1.98; PCC-1, 0.024; MAG-1, 2.84; BHVO-1, 0.90; DTS-1, 0.026; SCo-1, 1.74; SDC-1, 2.52; BCR-1, 1.44; GSP-1, 1.22; SGR-1, 0.86; QLO-1, 1.83; RGM-1, 2.21; STM-1, 8.75; G-2, 2.29. An analysis of variance shows that all the samples may be considered homogeneous at F0.95 except AGV-1 and DTS-1 which may be considered homogeneous at F0.99. ?? 1978.

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

    EPA Science Inventory

    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...

  4. THE STANDARD CALIBRATION INSTRUMENT AUTOMATION SYSTEM FOR THE ATOMIC ABSORPTION SPECTROPHOTOMETER. PART III: PROGRAM DOCUMENTATION

    EPA Science Inventory

    This report contains complete documentation for the 15 programs and 11 data files of the EPA Atomic Absorption Instrument Automation System. The system incorporates the following major features: (1) multipoint calibration using first, second, or third degree regression or linear ...

  5. Vacuum Ultraviolet Absorption Measurements of Atomic Oxygen in a Shock Tube

    NASA Technical Reports Server (NTRS)

    Meyer, Scott Andrew

    1995-01-01

    The absorption of vacuum ultraviolet light by atomic oxygen has been measured in the Electric Arc-driven Shock Tube (EAST) Facility at NASA-Ames Research Center. This investigation demonstrates the instrumentation required to determine atomic oxygen concentrations from absorption measurements in impulse facilities. A shock wave dissociates molecular oxygen, producing a high temperature sample of atomic oxygen in the shock tube. A probe beam is generated with a Raman-shifted ArF excimer laser. By suitable tuning of the laser, absorption is measured over a range of wavelengths in the region of the atomic line at 130.49 nm. The line shape function is determined from measurements at atomic oxygen densities of 3x10(exp 17) and 9x10(exp 17) cm(exp -3). The broadening coefficient for resonance interactions is deduced from this data, and this value is in accord with available theoretical models.

  6. Vacuum Ultraviolet Absorption Measurements of Atomic Oxygen in a Shock Tube

    NASA Technical Reports Server (NTRS)

    Meyer, Scott Andrew

    1995-01-01

    The absorption of vacuum ultraviolet light by atomic oxygen has been measured in the Electric Arc-driven Shock Tube (EAST) Facility at NASA-Ames Research Center. This investigation demonstrates the instrumentation required to determine atomic oxygen concentrations from absorption measurements in impulse facilities. A shock wave dissociates molecular oxygen, producing a high temperature sample of atomic oxygen in the shock tube. A probe beam is generated with a Raman-shifted ArF excimer laser. By suitable tuning of the laser, absorption is measured over a range of wavelengths in the region of the atomic line at 130.49 nm. The line shape function is determined from measurements at atomic oxygen densities of 3 x 10(exp 17) and 9 x 10(exp 17) cm(exp -3). The broadening coefficient for resonance interactions is deduced from this data, and this value is in accord with available theoretical models.

  7. Vacuum Ultraviolet Absorption Measurements of Atomic Oxygen in a Shock Tube.

    NASA Astrophysics Data System (ADS)

    Meyer, Scott Andrew

    The absorption of vacuum ultraviolet light by atomic oxygen has been measured in the Electric Arc-driven Shock Tube (EAST) Facility at NASA-Ames Research Center. This investigation demonstrates the instrumentation required to determine atomic oxygen concentrations from absorption measurements in impulse facilities. A shock wave dissociates molecular oxygen, producing a high temperature sample of atomic oxygen in the shock tube. A probe beam is generated with a Raman-shifted ArF excimer laser. By suitable tuning of the laser, absorption is measured over a range of wavelengths in the region of the atomic line at 130.49 nm. The line shape function is determined from measurements at atomic oxygen densities of 3 times 10 ^{17} and 9 times 10^{17} cm ^{-3}. The broadening coefficient for resonance interactions is deduced from this data, and this value is in accord with available theoretical models.

  8. Vacuum Ultraviolet Absorption Measurements of Atomic Oxygen in a Shock Tube

    NASA Technical Reports Server (NTRS)

    Meyer, Scott Andrew

    1995-01-01

    The absorption of vacuum ultraviolet light by atomic oxygen has been measured in the Electric Arc-driven Shock Tube (EAST) Facility at NASA-Ames Research Center. This investigation demonstrates the instrumentation required to determine atomic oxygen concentrations from absorption measurements in impulse facilities. A shock wave dissociates molecular oxygen, producing a high temperature sample of atomic oxygen in the shock tube. A probe beam is generated with a Raman-shifted ArF excimer laser. By suitable tuning of the laser, absorption is measured over a range of wavelengths in the region of the atomic line at 130.49 nm. The line shape function is determined from measurements at atomic oxygen densities of 3 x 10(exp 17) and 9 x 10(exp 17)/cu cm. The broadening coefficient for resonance interactions is deduced from this data, and this value is in accord with available theoretical models.

  9. Some interferences in atomic-absorption spectrometry and extraction of iron and copper.

    PubMed

    Yanagisawa, M; Kihara, H; Suzuki, M; Takeuchi, T

    1970-09-01

    The effect of complexing agents on the atomic-absorption spectrometry of iron and copper extracts was investigated Thiocyanate complexes gave a marked depression of absorption by iron and copper, especially in fuel-rich flames. Chloride, diethyldithiocarbamate and hydroxyquinoline complexes of iron behaved alike, but differently from the thiocyanate complex. PMID:18960816

  10. Measurement of aluminum in neuronal tissues using electrothermal atomization atomic absorption spectrophotometry

    SciTech Connect

    Pierson, K.B.; Evenson, M.A.

    1986-07-01

    Studies characterizing aluminum complexes isolated from neuronal tissues require accurate and precise techniques for aluminum measurement. A solution of 0.01 M nitric acid containing 0.2% Triton X-100 was the optimal diluent for aluminum measurement under the experimental conditions used. Three National Bureau of Standards Standard Reference Materials (SRM) were digested, and the aluminum concentration of each was measured with a Perkin-Elmer 503 atomic absorption spectrophotometer equipped with a Perkin-Elmer HGA 2100 controller. The calculated detection limit of aluminum was 120 pg using 15-..mu..L sample injections (8 ..mu..g/L). Aluminum concentrations present in citrus leaves (SRM 1572), pine needles (SRM 1575), and tomato leaves (SRM 1573) were 100 +- 12 (certified value, 92 +- 15), 522 +- 45 (certified value, 454 +- 30), and 1273 +- 112 (provisional value, 1200) ..mu..g/g, respectively. The within- and between-day precision had coefficients of variation for citrus leaves, pine needles, and tomato leaves of 18 and 12%, 6.3 and 8.6%, and 3.7 and 8.7%, respectively. Aluminum absorbance was enhanced at high pH values and by zinc.

  11. DIRECT DETERMINATION OF PHOSPHORUS IN GASOLINE BY FLAMELESS ATOMIC ABSORPTION SPECTROMETRY

    EPA Science Inventory

    A new method is presented for the determination of phosphorus in gasoline using flameless atomic absorption. Lanthanum nitrate solution is inserted in a graphite furnace prior to direct addition of gasoline. The organic matrix is charred prior to atomization of the phosphorus. Th...

  12. Absorption of twisted light by a mesoscopic atomic target

    NASA Astrophysics Data System (ADS)

    Peshkov, A. A.; Serbo, V. G.; Fritzsche, S.; Surzhykov, A.

    2016-06-01

    The excitation of a hydrogen-atom target by a twisted Bessel light beam is investigated. The atoms are assumed to have a Gaussian spatial distribution in the target. Theoretical analysis is performed within a nonrelativistic framework using a first-order perturbation approach and density matrix formalism. By using this theory, we derive the expressions for excitation cross sections and for alignment parameters of the excited atomic state. In particular, we make calculations for the 1s\\to 2p transition caused by the interaction of Bessel beams with the atomic target. For this transition, we analyze the population of magnetic sublevels for the excited 2p state and study how it is affected by the projection of the total angular momentum of incident light. The calculations indicate that the projection of the total angular momentum of the incident Bessel beam affects the alignment of atoms for sufficiently small targets with size less than 200 nm. This can be observed experimentally by measuring the linear polarization of the subsequent fluorescent light.

  13. Atomic structure of machined semiconducting chips: An x-ray absorption spectroscopy study

    SciTech Connect

    Paesler, M.; Sayers, D.

    1988-12-01

    X-ray absorption spectroscopy (XAS) has been used to examine the atomic structure of chips of germanium that were produced by single point diamond machining. It is demonstrated that although the local (nearest neighbor) atomic structure is experimentally quite similar to that of single crystal specimens information from more distant atoms indicates the presence of considerable stress. An outline of the technique is given and the strength of XAS in studying the machining process is demonstrated.

  14. Targeting Inaccurate Atomic Data in the Eta Car Ejecta Absorption

    NASA Technical Reports Server (NTRS)

    Nielsen, K. E.; Kober, G. Vieira; Gull, T. R.; Blackwell-Whitehead, R.; Nilsson, H.

    2006-01-01

    The input from the laboratory spectroscopist community has on many occasions helped the analysis of the eta Car spectrum. Our analysis has targeted spectra where improved wavelengths and oscillator strengths are needed. We will demonstrate how experimentally derived atomic data have improved our spectral analysis, and illuminate where more work still is needed.

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

    PubMed

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

    2015-01-01

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

  16. Absorption of infrared radiation by electrons in the field of a neutral hydrogen atom

    NASA Technical Reports Server (NTRS)

    Stallcop, J. R.

    1974-01-01

    An analytical expression for the absorption coefficient is developed from a relationship between the cross-section for inverse bremsstrahlung absorption and the cross-section for electron-atom momentum transfer; it is accurate for those photon frequencies v and temperatures such that hv/kT is small. The determination of the absorption of infrared radiation by free-free transitions of the negative hydrogen ion has been extended to higher temperatures. A simple analytical expression for the absorption coefficient has been derived.

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

    NASA Astrophysics Data System (ADS)

    Arslan, Yasin; Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan; Dědina, Jiří

    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- 1. Six and eleven times higher sensitivity, respectively, was provided by atomizers with longer light paths in the observation volume, i.e. externally heated T-tube and externally heated flame-in-T-tube. The latter one, offering limit of detection below 0.01 μg ml- 1, appeared as the most prospective for on-line atomization. Insight into the mechanism of atomization of gold volatile species, into the fate of free atoms and into subsequent analyte transfer allowed to assess possibilities of in-atomizer preconcentration of gold volatile species: it is unfeasible with quartz atomizers but a sapphire tube atomizer could be useful in this respect.

  18. Real-time atomic absorption mercury continuous emission monitor

    NASA Astrophysics Data System (ADS)

    Zamzow, Daniel S.; Bajic, Stanley J.; Eckels, David E.; Baldwin, David P.; Winterrowd, Chris; Keeney, Robert

    2003-08-01

    A continuous emission monitor (CEM) for mercury (Hg) in combustor flue gas streams has been designed and tested for the detection of Hg by optical absorption. A sampling system that allows continuous introduction of stack gas is incorporated into the CEM, for the sequential analysis of elemental and total Hg. A heated pyrolysis tube is used in the system to convert oxidized Hg compounds to elemental Hg for analysis of total Hg; the pyrolysis tube is bypassed to determine the elemental Hg concentration in the gas stream. A key component of the CEM is a laboratory-designed and -assembled echelle spectrometer that provides simultaneous detection of all of the emission lines from a Hg pen lamp, which is used as the light source for the optical absorption measurement. This feature allows for on-line spectroscopic correction for interferent gases such as sulfur dioxide and nitrogen dioxide, typically present in combustion stack gas streams, that also absorb at the Hg detection wavelength (253.65 nm). This article provides a detailed description of the CEM system, the characteristics and performance of the CEM, and the results of field tests performed at the Environmental Protection Agency-Rotary Kiln at Research Triangle Park, NC.

  19. Chlorine analysis by diode laser atomic absorption spectrometry.

    PubMed

    Koch, J; Zybin, A; Niemax, K

    2000-04-01

    The general characteristics of Diode Laser Absorption Spectrometry (DLAAS) in low pressure plasmas particularly with respect to the detection of non-metals are comprehensively recapitulated and discussed. Furthermore, a detector, which is based on DLAAS in a microwave-induced low pressure plasma as an alternative technique for halogene-specific analysis of volatile compounds and polymeric matrices is described. The analytical capability of the technique is demonstrated on the chlorine-specific analysis of ablated polymer fragments as well as gas chromatographically separated hydrocarbons. Since the measurements were carried out by means of a balanced-heterodyne detection scheme, different technical noise contributions, such as laser excess and RAM noise could efficiently be suppressed and the registered absorption was limited only by the principal shot noise. Thus, in the case of the polymer analysis a chlorine-specific absolute detection limit of 10 pg could be achieved. Furthermore, fundamental investigations concerning the influence of hydrocarbons on the dissociation capability of the microwave induced plasma were performed. For this purpose, the carbon-, chlorine- and hydrogen-specific stoichiometry of the compounds were empirically determined. Deviations from the expected proportions were found to be insignificant, implying the possibility of internal standardization relative to the response of a reference sample. PMID:12953476

  20. Double tungsten coil atomic absorption spectrometer based on an acousto-optic tunable filter

    NASA Astrophysics Data System (ADS)

    Jora, M. Z.; Nóbrega, J. A.; Rohwedder, J. J. R.; Pasquini, C.

    2015-01-01

    An atomic absorption spectrometer based on a quartz acousto-optic tunable filter (AOTF) monochromator operating in the 271-453 nm range, is described. The instrument was tailored to study the formation and evolution of electrothermal atomic cloud induced either by one or two tungsten coils. The spectrometer also includes a fast response programmable photomultiplier module for data acquisition, and a power supply capable of driving two parallel tungsten coils independently. The atomization cell herein described was manufactured in PTFE and presents a new design with reduced size. Synchronization between the instant of power delivering to start the atomization process and the detection was achieved, allowing for monitoring the atomization and thermal events synchronously and in real time. Absorption signals can be sampled at a rate of a few milliseconds, compatible with the fast phenomena that occur with electrothermal metallic atomizers. The instrument performance was preliminarily evaluated by monitoring the absorption of radiation of atomic clouds produced by standard solutions containing chromium or lead. Its quantitative performance was evaluated by using Cr aqueous solutions, resulting in detection limits as low as 0.24 μg L- 1, and a relative standard deviation of 3%.

  1. Transient dispersion and absorption in a V-shaped atomic system

    NASA Astrophysics Data System (ADS)

    Sahrai, M.; Maleki, A.; Hemmati, R.; Mahmoudi, M.

    2010-01-01

    We investigate the dynamical behavior of the dispersion and the absorption in a V-type three level atomic system. It is shown that in the presence of decay-induced interference the probe dispersion and absorption are phase dependent. We find that an incoherent pumping field provides an additional control parameter for switching the group velocity of a light pulse. The required switching times for switching the group velocity of a probe field from subluminal to superluminal pulse propagation is then discussed.

  2. Laboratory atomic transition data for precise optical quasar absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Murphy, Michael T.; Berengut, Julian C.

    2014-02-01

    Quasar spectra reveal a rich array of important astrophysical information about galaxies which intersect the quasar line of sight. They also enable tests of the variability of fundamental constants over cosmological time- and distance-scales. Key to these endeavours are the laboratory frequencies, isotopic and hyperfine structures of various metal-ion transitions. Here, we review and synthesize the existing information about these quantities for 43 transitions which are important for measuring possible changes in the fine-structure constant, α, using optical quasar spectra, i.e. those of Na, Mg, Al, Si, Ca, Cr, Mn, Fe, Ni and Zn. We also summarize the information currently missing that precludes more transitions being used. We present an up-to-date set of coefficients, q, which define the sensitivity of these transitions to variations in α. New calculations of isotopic structures and q-coefficients are performed for Si II and Ti II, including Si II λ1808 and Ti IIλλ1910.6/1910.9 for the first time. Finally, simulated absorption-line spectra are used to illustrate the systematic errors expected if the isotopic/hyperfine structures are omitted from profile fitting analyses. To ensure transparency, repeatability and currency of the data and calculations, we supply a comprehensive data base as Supporting Information. This will be updated as new measurements and calculations are performed.

  3. Determination of cadmium in the livers and kidneys of puffins by carbon furnace atomic absorption spectrometry.

    PubMed

    Ottaway, J M; Campbell, W C

    1976-01-01

    A carbon furnace atomic absorption procedure is described for the determination of cadmium in the livers and kidneys of puffins, fratercula arctica. Samples are dried and weighed and 2 to 100 mg are dissolved in sulphuric and nitric acids. These solutions are analysed directly in the carbon furnace against aqueous standards and provide accurate results in the range 0-1 to 100 micrograms/g dry weight. The method is simple and rapid and requires much less of the small total sample than would be required for flame atomic absorption. PMID:1030692

  4. Comparison of liposome entrapment parameters by optical and atomic absorption spectrophotometry.

    PubMed

    Yoss, N L; Popescu, O; Pop, V I; Porutiu, D; Kummerow, F A; Benga, G

    1985-01-01

    Methods for the complete characterization of liposomes prepared by ether-injection are described in detail. The validity of atomic absorption spectrophotometry for measuring markers of trapped volume was checked by comparative determinations of markers with established optical spectrophotometrical methods. The favorable results using atomic absorption spectrophotometry to quantitate the marker Mn2+ are of particular relevance as manganese ion is also the paramagnetic probe in n.m.r. measurements of water permeability of liposomes; our results indicate that in such measurements no other marker need be incorporated. PMID:3986305

  5. Effective Atomic Numbers of Lanthanides with Gamma Radiation for Photon Energy Absorption

    NASA Astrophysics Data System (ADS)

    Shantappa, Anil; Hanagodimath, S. M.

    Effective atomic numbers for photon energy absorption, ZPEA,eff have been calculated for photon from 1 keV to 20 MeV for selected oxides of lanthanides, such as Lanthanum oxide, Cerium oxide, Samarium oxide, Europium oxide, Dysprosium oxide, Thulium oxide, Ytterbium oxide. The ZPEA,eff values then compared with ZPI,eff for photon interaction. The ZPEA,eff values have been found to change with energy and composition of selected lanthanides. Oxides of lanthanides are considered as better shielding materials to the exposure of gamma radiation. The values of effective atomic number for photon energy absorption help in the calculation of absorbed dose.

  6. Methods for analysis of selected metals in water by atomic absorption

    USGS Publications Warehouse

    Fishman, Marvin J.; Downs, Sanford C.

    1966-01-01

    This manual describes atomic-absorption-spectroscopy methods for determining calcium, copper, lithium, magnesium, manganese, potassium, sodium, strontium and zinc in atmospheric precipitation, fresh waters, and brines. The procedures are intended to be used by water quality laboratories of the Water Resources Division of the U.S. Geological Survey. Detailed procedures, calculations, and methods for the preparation of reagents are given for each element along with data on accuracy, precision, and sensitivity. Other topics discussed briefly are the principle of atomic absorption, instrumentation used, and special analytical techniques.

  7. Observing random walks of atoms in buffer gas through resonant light absorption

    NASA Astrophysics Data System (ADS)

    Aoki, Kenichiro; Mitsui, Takahisa

    2016-07-01

    Using resonant light absorption, random-walk motions of rubidium atoms in nitrogen buffer gas are observed directly. The transmitted light intensity through atomic vapor is measured, and its spectrum is obtained, down to orders of magnitude below the shot-noise level to detect fluctuations caused by atomic motions. To understand the measured spectra, the spectrum for atoms performing random walks in a Gaussian light beam is computed, and its analytical form is obtained. The spectrum has 1 /f2 (f is frequency) behavior at higher frequencies, crossing over to a different, but well-defined, behavior at lower frequencies. The properties of this theoretical spectrum agree excellently with the measured spectrum. This understanding also enables us to obtain the diffusion constant, the photon cross section of atoms in buffer gas, and the atomic number density from a single spectral measurement. We further discuss other possible applications of our experimental method and analysis.

  8. Microwave absorption properties of carbon nanocoils coated with highly controlled magnetic materials by atomic layer deposition.

    PubMed

    Wang, Guizhen; Gao, Zhe; Tang, Shiwei; Chen, Chaoqiu; Duan, Feifei; Zhao, Shichao; Lin, Shiwei; Feng, Yuhong; Zhou, Lei; Qin, Yong

    2012-12-21

    In this work, atomic layer deposition is applied to coat carbon nanocoils with magnetic Fe(3)O(4) or Ni. The coatings have a uniform and highly controlled thickness. The coated nanocoils with coaxial multilayer nanostructures exhibit remarkably improved microwave absorption properties compared to the pristine carbon nanocoils. The enhanced absorption ability arises from the efficient complementarity between complex permittivity and permeability, chiral morphology, and multilayer structure of the products. This method can be extended to exploit other composite materials benefiting from its convenient control of the impedance matching and combination of dielectric-magnetic multiple loss mechanisms for microwave absorption applications. PMID:23171130

  9. Atomic absorption spectrophotometric determination of microgram quantities of copper in tea after solvent extraction.

    PubMed

    Aziz-Alrahman, A M

    1985-01-01

    An atomic absorption spectrophotometric method is described for determining trace amounts of copper in tea. The method is based on the solvent extraction of the metal as tetraiodocuprate (I), from 2 M HCl solutions of tea samples which contain 12% (w/v) KI, into methylisobutyl ketone. The organic extracts, containing the ion-association complex of copper are atomized into an air-acetylene flame. The limit of detection is 1.14 micrograms g-1 Cu. PMID:4077371

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

    NASA Astrophysics Data System (ADS)

    Heinrich, Hans-Joachim; Matschat, Ralf

    2007-08-01

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

  11. A COMPUTER INTERFACE FOR A PERKIN-ELMER 5000 ATOMIC ABSORPTION INSTRUMENT

    EPA Science Inventory

    This document contains a detailed description of an ASCII Character Buffer Interface designed to store and forward serial ASCII data received from an EIA RS-232C Interface. The particular application described herein concerns a Perkin-Elmer Model 5000 Atomic Absorption instrument...

  12. [Determination of lead in beard hair by atomic absorption spectrometry (author's transl)].

    PubMed

    Graef, V

    1976-04-01

    The lead content of hair from the electric razor can be determined by atomic absorption spectrometry, using the micro-sampling technique of Delves. 1--5 mg of the washed and dried hair are partially oxidized with hydrogen peroxide prior to analysis. The method is simple and quick and therefore suited for the serial investigation of persons exposed to lead. PMID:1271019

  13. Determination of arsenic and selenium in environmental and agricultural samples by hydride generation atomic absorption spectrometry

    SciTech Connect

    Hershey, J.W.; Oostdyk, T.S.; Keliher, P.N.

    1988-11-01

    Agricultural and environmental samples are digested with acid, and arsenic and selenium are determined using hydride generation atomic absorption spectrometry. Interelement interferences are eliminated by high acid concentrations or cation-exchange resins. Agreement with standard reference material is excellent. The technique is also applied to actual samples.

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

    EPA Science Inventory


    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...

  15. Circuit Board Analysis for Lead by Atomic Absorption Spectroscopy in a Course for Nonscience Majors

    ERIC Educational Resources Information Center

    Weidenhammer, Jeffrey D.

    2007-01-01

    A circuit board analysis of the atomic absorption spectroscopy, which is used to measure lead content in a course for nonscience majors, is being presented. The experiment can also be used to explain the potential environmental hazards of unsafe disposal of various used electronic equipments.

  16. THE STANDARD CALIBRATION INSTRUMENT AUTOMATION SYSTEM FOR THE ATOMIC ABSORPTION SPECTROPHOTOMETER. PART I: FUNCTIONAL SPECIFICATIONS

    EPA Science Inventory

    This document contains a project definition, a set of functional requirements, and a functional design for the automation of flameless atomic absorption (AA) spectrophotometers. The system is a real-time data acquisition system with 'on line' data reduction, quality control and r...

  17. The Use of an Air-Natural Gas Flame in Atomic Absorption.

    ERIC Educational Resources Information Center

    Melucci, Robert C.

    1983-01-01

    Points out that excellent results are obtained using an air-natural gas flame in atomic absorption experiments rather than using an air-acetylene flame. Good results are obtained for alkali metals, copper, cadmium, and zinc but not for the alkaline earths since they form refractory oxides. (Author/JN)

  18. DETERMINING BERYLLIUM IN DRINKING WATER BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROSCOPY

    EPA Science Inventory

    A direct graphite furnace atomic absorption spectroscopy method for the analysis of beryllium in drinking water has been derived from a method for determining beryllium in urine. Ammonium phosphomolybdate and ascorbic acid were employed as matrix modifiers. The matrix modifiers s...

  19. [Determination of sulfur in plant using a high-resolution continuum source atomic absorption spectrometer].

    PubMed

    Wang, Yu; Li, Jia-xi

    2009-05-01

    A method for the analysis of sulfur (S) in plant by molecular absorption of carbon monosulfide (CS) using a high-resolution continuum source atomic absorption spectrometer (CS AAS) with a fuel-rich air/acetylene flame has been devised. The strong CS absorption band was found around 258 nm. The half-widths of some absorption bands were of the order of picometers, the same as the common atomic absorption lines. The experimental procedure in this study provided optimized instrumental conditions (the ratio of acetylene to air, the burner height) and parameters, and researched the spectral interferences and chemical interferences. The influence of the organic solvents on the CS absorption signals and the different digestion procedures for the determination of sulfur were also investigated. The limit of detection achieved for sulfur was 14 mg x L(-1), using the CS wavelength of 257. 961 nm and a measurement time of 3 s. The accuracy and precision were verified by analysis of two plant standard reference materials. The major applications of this method have been used for the determination of sulfur in plant materials, such as leaves. Compared to the others, this method for the analysis of sulfur is rapid, easy and simple for sulfur determination in plant. PMID:19650504

  20. Multielement continuum-source atomic-absorption spectrometry with an echelle-spectrometer/image-dissector system.

    PubMed

    Masters, R; Hsiech, C; Pardue, H L

    1989-01-01

    The continued development of the echelle-spectrometer/image-dissector system for multielement determination by continuum-source atomic-absorption spectrometry is presented. Modifications of the instruments include the use of a 20-groove/mm echelle grating blazed at 76 degrees , and the removal of the magnetic shield from the image dissector. The spectral range is from 300 to 430 nm and the observed resolution is better than 0.005 nm at 400 nm. Calibration curves are linear up to an absorbance of 0.2, and absorption sensitivities are up to 4-fold better than with the previous design. Fundamental characteristics of the detector limit the application of the instrument to sequential single-element quantifications with the electrothermal atomizer, and to sequential multielement quantification with the flame atomizer. The further development of the instrument for simultaneous multielement qualification is discussed. PMID:18964682

  1. Enhanced Reverse Saturable Absorption and Optical Limiting in Heavy-Atom Substituted Phthalocyanines

    NASA Technical Reports Server (NTRS)

    Perry, J. W.; Mansour, K.; Marder, S. R.; Alvarez, D., Jr.; Perry, K. J.; Choong, I.

    1994-01-01

    The reverse saturable absorption and optical limiting response of metal phthalocyaninies can be enhanced by using the heavy-atom effect. Phthalocyanines containing heavy metal atoms, such as In, Sn, and Pb show nearly a factor of two enhancement in the ratio of effective excited-state to ground-state absorption cross sections compared to those containing lighter atoms, such as Al and Si. In an f/8 optical geometry, homogeneous solutions of heavy metal phthalocyanines, at 30% linear transmission, limit 8-ns, 532-nm laser pulses to less than or equal to 3 (micro)J (the energy for 50% probability of eye damage) for incident pulses up to 800 (micro)J.

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

  3. Determination of Calcium in Cereal with Flame Atomic Absorption Spectroscopy: An Experiment for a Quantitative Methods of Analysis Course

    ERIC Educational Resources Information Center

    Bazzi, Ali; Kreuz, Bette; Fischer, Jeffrey

    2004-01-01

    An experiment for determination of calcium in cereal using two-increment standard addition method in conjunction with flame atomic absorption spectroscopy (FAAS) is demonstrated. The experiment is intended to introduce students to the principles of atomic absorption spectroscopy giving them hands on experience using quantitative methods of…

  4. Tunable Diode Laser Atomic Absorption Spectroscopy for Detection of Potassium under Optically Thick Conditions.

    PubMed

    Qu, Zhechao; Steinvall, Erik; Ghorbani, Ramin; Schmidt, Florian M

    2016-04-01

    Potassium (K) is an important element related to ash and fine-particle formation in biomass combustion processes. In situ measurements of gaseous atomic potassium, K(g), using robust optical absorption techniques can provide valuable insight into the K chemistry. However, for typical parts per billion K(g) concentrations in biomass flames and reactor gases, the product of atomic line strength and absorption path length can give rise to such high absorbance that the sample becomes opaque around the transition line center. We present a tunable diode laser atomic absorption spectroscopy (TDLAAS) methodology that enables accurate, calibration-free species quantification even under optically thick conditions, given that Beer-Lambert's law is valid. Analyte concentration and collisional line shape broadening are simultaneously determined by a least-squares fit of simulated to measured absorption profiles. Method validation measurements of K(g) concentrations in saturated potassium hydroxide vapor in the temperature range 950-1200 K showed excellent agreement with equilibrium calculations, and a dynamic range from 40 pptv cm to 40 ppmv cm. The applicability of the compact TDLAAS sensor is demonstrated by real-time detection of K(g) concentrations close to biomass pellets during atmospheric combustion in a laboratory reactor. PMID:26938713

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

    PubMed

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

    1998-04-01

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

  6. Self-corrected Sensors Based On Atomic Absorption Spectroscopy For Atom Flux Measurements In Molecular Beam Epitaxy

    SciTech Connect

    Du, Yingge; Droubay, Timothy C.; Liyu, Andrey V.; Li, Guosheng; Chambers, Scott A.

    2014-04-24

    A high sensitivity atom flux sensor based on atomic absorption spectroscopy has been designed and implemented to control electron beam evaporators and effusion cells in a molecular beam epitaxy system. Using a high-resolution spectrometer and a two-dimensional charge coupled device (CCD) detector in a double-beam configuration, we employ a non-resonant line or a resonant line with lower absorbance from the same hollow cathode lamp as the reference for nearly perfect background correction and baseline drift removal. This setup also significantly shortens the warm-up time needed compared to other sensor technologies and drastically reduces the noise coming from the surrounding environment. In addition, the high-resolution spectrometer allows the most sensitive resonant line to be isolated and used to provide excellent signal-to-noise ratio.

  7. Self-corrected sensors based on atomic absorption spectroscopy for atom flux measurements in molecular beam epitaxy

    SciTech Connect

    Du, Y. E-mail: scott.chambers@pnnl.gov; Liyu, A. V.; Droubay, T. C.; Chambers, S. A. E-mail: scott.chambers@pnnl.gov; Li, G.

    2014-04-21

    A high sensitivity atom flux sensor based on atomic absorption spectroscopy has been designed and implemented to control electron beam evaporators and effusion cells in a molecular beam epitaxy system. Using a high-resolution spectrometer and a two-dimensional charge coupled device detector in a double-beam configuration, we employ either a non-resonant line or a resonant line with low cross section from the same hollow cathode lamp as the reference for nearly perfect background correction and baseline drift removal. This setup also significantly shortens the warm-up time needed compared to other sensor technologies and drastically reduces the noise coming from the surrounding environment. In addition, the high-resolution spectrometer allows the most sensitive resonant line to be isolated and used to provide excellent signal-to-noise ratio.

  8. Three-photon-absorption resonance for all-optical atomic clocks

    SciTech Connect

    Zibrov, Sergei; Novikova, Irina; Phillips, David F.; Taichenachev, Aleksei V.; Yudin, Valeriy I.; Walsworth, Ronald L.; Zibrov, Alexander S.

    2005-07-15

    We report an experimental study of an all-optical three-photon-absorption resonance (known as an 'N resonance') and discuss its potential application as an alternative to atomic clocks based on coherent population trapping. We present measurements of the N-resonance contrast, width and light shift for the D{sub 1} line of {sup 87}Rb with varying buffer gases, and find good agreement with an analytical model of this resonance. The results suggest that N resonances are promising for atomic clock applications.

  9. Tunable Diode Laser Absorption Spectroscopy of Metastable Atoms in Dusty Plasmas

    SciTech Connect

    Hoang Tung Do; Hippler, Rainer

    2008-09-07

    Spatial density profile of neon metastable produced in dusty plasma was investigated by means of tunable diode laser absorption spectroscopy. The line averaged measured density drops about 30% with the presence of dust particles. The observations provide evidence for a significant interaction between atoms and powder particles which are important for energy transfer from plasma to particles. The power per unit area absorbed by dust particles due to the collision of metastable atoms with dust particle surface is about some tens of mW/m{sup 2}.

  10. Atomic calculations and search for variation of the fine-structure constant in quasar absorption spectra

    NASA Astrophysics Data System (ADS)

    Dzuba, V. A.; Flambaum, V. V.

    A brief review of the search for variation of the fine structure constant in quasar absorption spectra is presented. Special consideration is given to the role of atomic calculations in the analysis of the observed data. A range of methods which allow to perform calculations for atoms or ions with different electron structure and which cover practically all periodic table of elements is discussed. Critical compilation of the results of the calculations as well as a review of the most recent results of the analysis are presented.

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

    NASA Astrophysics Data System (ADS)

    Morzan, Ezequiel; Piano, Ornela; Stripeikis, Jorge; Tudino, Mabel

    2012-11-01

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

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

    NASA Astrophysics Data System (ADS)

    Parsons, Patrick J.; Slavin, Walter

    1999-05-01

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

  13. Determination of iodine in seaweed and table salt by an indirect atomic-absorption method.

    PubMed

    Wifladt, A M; Lund, W; Bye, R

    1989-03-01

    Decomposition methods based on fusion with alkali are discussed, with respect to the determination of iodine in biological material. It is shown that sodium hydroxide can be used for the decomposition of seaweed without loss of iodine. In spite of the oxidizing conditions, the iodine will be present as iodide in the final ash. The iodide can be determined by an indirect atomic-absorption method, based on the reaction between iodide and mercury(II), with determination of mercury by cold vapour atomic-absorption spectrometry. The basis of the method is discussed, and it is shown that the use of tin(II) as reductant is essential. The effect of the oxidation state of the iodine on the sensitivity of the method is pointed out. High concentrations of chloride interfere, but it is still possible to determine iodide in iodinated table salt. PMID:18964724

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

    USGS Publications Warehouse

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

    1981-01-01

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

  15. Studies on mass energy-absorption coefficients and effective atomic energy-absorption cross sections for carbohydrates

    NASA Astrophysics Data System (ADS)

    Ladhaf, Bibifatima M.; Pawar, Pravina P.

    2015-04-01

    We measured here the mass attenuation coefficients (μ/ρ) of carbohydrates, Esculine (C15H16O9), Sucrose (C12H22O11), Sorbitol (C6H14O6), D-Galactose (C6H12O6), Inositol (C6H12O6), D-Xylose (C5H10O5) covering the energy range from 122 keV up to 1330 keV photon energies by using gamma ray transmission method in a narrow beam good geometry set-up. The gamma-rays were detected using NaI(Tl) scintillation detection system with a resolution of 8.2% at 662 keV. The attenuation coefficient data were then used to obtain the total attenuation cross-section (σtot), molar extinction coefficients (ε), mass-energy absorption coefficients (μen/ρ) and effective (average) atomic energy-absorption cross section (σa,en) of the compounds. These values are found to be in good agreement with the theoretical values calculated based on XCOM data.

  16. Observation of an electromagnetically induced change of absorption in multilevel rubidium atoms

    NASA Astrophysics Data System (ADS)

    Li, Yong-Qing; Jin, Shao-Zheng; Xiao, Min

    1995-03-01

    A 64.4% reduction in absorption at the rubidium D2 line is observed when a pumping field at 775.8 nm is tuned on resonance to the transition between the excited states 5P3/2 and 5D5/2. As the pumping field is tuned off resonance, an absorption peak appears at the side of the Doppler-broadened D2 line. This modification in absorption is related to pumping-induced atomic coherence in this three-level ladder-type system. This experiment is done in a Rb vapor cell at room temperature and with cw diode lasers for both pumping and probe beams in a Doppler-free configuration.

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

    EPA Science Inventory

    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...

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

    USGS Publications Warehouse

    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.

  19. Proposal for efficient two-dimensional atom localization using probe absorption in a microwave-driven four-level atomic system

    SciTech Connect

    Ding Chunling; Li Jiahua; Yang Xiaoxue; Xiong Hao; Zhang Duo

    2011-10-15

    The behavior of two-dimensional (2D) atom localization is explored by monitoring the probe absorption in a microwave-driven four-level atomic medium under the action of two orthogonal standing-wave fields. Because of the position-dependent atom-field interaction, the information about the position of the atom can be obtained via the absorption measurement of the weak probe field. It is found that the localization behavior is significantly improved due to the joint quantum interference induced by the standing-wave and microwave-driven fields. Most importantly, the atom can be localized at a particular position and the maximal probability of finding the atom in one period of the standing-wave fields reaches unity by properly adjusting the system parameters. The proposed scheme may provide a promising way to achieve high-precision and high-resolution 2D atom localization.

  20. Determination of ytterbium in animal faeces by tungsten coil electrothermal atomic absorption spectrometry.

    PubMed

    Lima, E C; Krug, F J; Nóbrega, J A; Nogueira, A R

    1998-11-01

    A method for ytterbium determination in animal faeces by tungsten coil electrothermal atomic absorption spectrometry (TCAAS) was developed. Faeces were dry-ashed in a muffle furnace, the ashes were treated with hydrochloric acid, and 10 mul of sample solution were delivered into 150-W tungsten coil atomizer. A matrix-matching procedure employing a 66-s heating program proved to be efficient for obtaining accurate results. Characteristic mass and detection limit were 7.1 pg and 0.35 mug g(-1) Yb, respectively. The tungsten coil atomizer lifetime exceeded 300 firings with digested solutions and R.S.D. of measurements was 1.9% after ten consecutive injections of 10.0 mug l(-1) Yb. Accuracy of the proposed method was assessed by employing a graphite furnace atomic absorption spectrometric procedure. Application of the paired t-test did not reveal any significant difference for ytterbium contents determined by both methods at 95% confidence level. It was demonstrated that the proposed procedure can successfully be used for evaluation of kinetic passage rate of feed through digestive tract of animals. PMID:18967363

  1. A metallic furnace atomizer in hydride generation atomic absorption spectrometry: Determination of bismuth and selenium

    NASA Astrophysics Data System (ADS)

    Klassen, Aline; Kim, Manuela Leticia; Tudino, Mabel Beatriz; Baccan, Nivaldo; Arruda, Marco Aurélio Zezzi

    2008-08-01

    A flow injection hydride generation system with a metal furnace atomizer (Inconel 600® alloy) was employed for Bi and Se determination. The presented methods have linear ranges up to 200 and 500 μg L - 1 for Bi and Se, respectively, with good linearities ( r2 = 0.9997 and 0.9974, respectively). The limits of quantification obtained according to IUPAC recommendations were 2.3 μg L - 1 for Bi and 6 μg L - 1 for Se, and the relative standard deviations ( N = 6) based on Bi and Se analytical responses from real samples were 2.7% and 10%, respectively. Accuracy evaluations were based on certified materials such as SRM 361, SRM 363, and SRM 364 (steel alloys) for Bi, Mess-3 (marine sediment), SRM 397 (human hair), and Bio-Rad2 — 69042 (urine) for Se. Good agreements between the results were obtained at the 95% confidence level, according to the t-test.

  2. Determination of selenium using atomically imprinted polymer (AIP) and hydride generation atomic absorption spectrometry.

    PubMed

    de Lima, Grazielle Cabral; do Lago, Ayla Campos; Chaves, Arley Alves; Fadini, Pedro Sergio; Luccas, Pedro Orival

    2013-03-20

    This paper describes selenium determination based on Se(0) preconcentration in the imprinted polymer (synthesized with 2.25mmol SeO2, 4-vinylpyridine and 1-vinylimidazole) with subsequent detection on-line in HG-FAAS. During the synthesis, SeO2 is reduced to Se (0). Therefore, there are no MIP neither IIP in the present work, thus we denominated: AIP, i.e., atomically imprinted polymers. For the optimization of analytical parameters Doehlert design was used. The method presented limit of detection and limit of quantification of 53 and 177ngL(-1), respectively, and linear range from 0.17 up to 6μgL(-1) (r=0.9936). The preconcentration factor (PF), consumptive index (CI) and concentration efficiency (CE) were 232; 0.06mL and 58min(-1) respectively. The proposed method was successfully applied to determine Se in Brazil nuts (0.33±0.03mgkg(-1)), apricot (0.46±0.02mgkg(-1)), white bean (0.47±0.03mgkg(-1)), rice flour (0.47±0.02mgkg(-1)) and milk powder (0.22±0.01mgkg(-1)) samples. It was possible to do 12 analyzes per hour. Accuracy was checked and confirmed by analyzing certified reference material (DORM-2, dogfish muscle), and samples precision was satisfactory with RSD lower than 10%. PMID:23473247

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

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Krawczyk, Magdalena

    2007-03-01

    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 2Te 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 arrangements (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 σ), was 0.9 ng mL - 1 for Te. For a 2 min in situ pre-concentration 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 designs studied include slotted tube, single silica tube and integrated atom trap-cooled atom traps. 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.

  4. Determination of trace and minor elements in alloys by atomic-absorption spectroscopy using an induction-heated graphite-well furnace as atom source-II.

    PubMed

    Ashy, M A; Headridge, J B; Sowerbutts, A

    1974-06-01

    Results are presented for the atomic-absorption spectrophotometric determination of zinc in aluminium and aluminium-silicon alloys, and aluminium, antimony and tin in steels, by means of solid samples dropped into an induction-heated graphite-well furnace to produce the atomic vapour. PMID:18961510

  5. Microplasmas as vacuum ultraviolet source for Cl-atom density measurements by resonance absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Martin, Virginie; Bauville, Gérard; Sadeghi, Nader; Puech, Vincent

    2011-11-01

    A micro-hollow cathode discharge was used to generate radiation on the chlorine atom resonance lines. Such radiation could be used to measure, by resonance absorption spectroscopy, the density of chlorine atoms in either ground state (3p5 2P3/2) or in the fine structure metastable state (3p5 2P1/2), which is located at 882.35 cm-1. Among the nine analysed lines in the 132-142 nm spectral region, only those at 137.953 and 139.653 nm, which are strong enough and are not affected by the self-absorption, can be used for the resonance absorption diagnostic of the ground state and the metastable state, respectively. The best operating conditions of the lamp source are 0.5% of Cl2 in argon at 150 mbar and 4 mA discharge current. The measured 800 ± 30 K gas temperature of the microplasma, indicates that under these specific conditions, these two lines are dominantly Doppler broadened. So their profile is Gaussian shaped with full widths at half maximum of (4.7 ± 0.1) × 10-4 nm.

  6. Method 200.12 - Determination of Trace Elements in Marine Waters by StabilizedTemperature Graphite Furnace Atomic Absorption

    EPA Science Inventory

    This method provides procedures for the determination of total recoverable elements by graphite furnace atomic absorption (GFAA) in marine waters, including estuarine, ocean and brines with salinities of up to 35 ppt.

  7. Spectro web: oscillator strength measurements of atomic absorption lines in the sun and procyon

    NASA Astrophysics Data System (ADS)

    Lobel, A.

    2008-10-01

    We update the online SpectroWeb database of spectral standard reference stars with 1178 oscillator strength values of atomic absorption lines observed in the optical spectrum of the Sun and Procyon (α CMi A). The updated line oscillator strengths are measured with best fits to the disk-integrated KPNO-FTS spectrum of the Sun observed between 4000 Å and 6800 Å using state-of-the-art detailed spectral synthesis calculations. A subset of 660 line oscillator strengths is validated with synthetic spectrum calculations of Procyon observed with ESO-UVES between 4700 Å and 6800 Å. The new log(gf)-values in SpectroWeb are improvements upon the values offered in the online Vienna Atomic Line Database (VALD). We find for neutral iron-group elements, such as Fe I, Ni I, Cr I, and Ti I, a statistically significant over-estimation of the VALD log((gf)-values for weak absorption lines with normalized central line depths below 15 %. For abundant lighter elements (e.g. Mg I and Ca I) this trend is statistically not significantly detectable, with the exception of Si I for which the log(gf)-values of 60 weak and medium-strong lines are substantially decreased to best fit the observed spectra. The newly measured log(gf)-values are available in the SpectroWeb database at http://spectra.freeshell.org, which interactively displays the observed and computed stellar spectra, together with corresponding atomic line data.

  8. Possible atomic structures responsible for the sub-bandgap absorption of chalcogen-hyperdoped silicon

    SciTech Connect

    Wang, Ke-Fan; Shao, Hezhu; Liu, Kong; Qu, Shengchun E-mail: wangyx@henu.edu.cn; Wang, Zhanguo; Wang, Yuanxu E-mail: wangyx@henu.edu.cn

    2015-09-14

    Single-crystal silicon was hyperdoped with sulfur, selenium, and tellurium using ion implantation and nanosecond laser melting. The hyperdoping of such chalcogen elements led to strong and wide sub-bandgap light absorption. Annealing the hyperdoped silicon, even at low temperatures (such as 200–400 °C), led to attenuation of the sub-bandgap absorption. To explain the attenuation process, we modeled it as chemical decomposition reaction from an optically absorbing structure to a non-absorbing structure. Attenuation of the experimental absorption coefficient was fit using the Arrhenius equation. From the fitted data, we extracted the reaction activation energies of S-, Se-, and T-hyperdoped silicon as 0.338 ± 0.029 eV, 0.471 ± 0.040 eV, and 0.357 ± 0.028 eV, respectively. We discuss these activation energies in terms of the bond energies of chalcogen–Si metastable bonds, and suggest that several high-energy interstitial sites, rather than substitutional sites, are candidates for the atomic structures that are responsible for the strong sub-bandgap absorption of chalcogen hyperdoped silicon.

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

    NASA Astrophysics Data System (ADS)

    Pasias, I. N.; Pappa, Ch.; Katsarou, V.; Τhomaidis, N. S.; 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 D2 background correction system, equipped with an end-heated graphite atomizer was undertaken to investigate the different behavior of boron in both techniques. Different chemical modifiers for the determination of boron were tested with both techniques. Ni-citric acid and Ca were the optimal chemical modifiers when simultaneous multi-element atomic absorption spectrometry and single-element atomic absorption spectrometry were used, respectively. By using the single-element atomic absorption spectrometry, the calculated characteristic mass was 220 pg and the calculated limit of detection was 370 μg/kg. On the contrary, with simultaneous multi-element atomic absorption spectrometry, the characteristic mass was 2200 pg and the limit of detection was 5.5 mg/kg.

  10. Coherent population trapping on 87Rb atoms in small-size absorption cells with buffer gas

    NASA Astrophysics Data System (ADS)

    Ermak, S. V.; Petrenko, M. V.; Semenov, V. V.

    2016-02-01

    Coherent population trapping (CPT) on 87Rb atoms in neon atmosphere has been studied in small-size glass absorption cells under conditions of pumping with narrow-band laser radiation at the D2 line of the main doublet. Parameters of the absorption signal have been measured in 3-mm-diameter cells at buffer gas (Ne) pressures varied within 200-400 Torr, cell temperatures within 65-120°C, and pumping radiation power densities within 30-400 μW/cm2. Optimum values of the buffer gas pressures, cell temperature, and pumping power are determined at which the short-term instability of the resonance line is at minimum. Orientational shifts of the CPT resonance signal in gas-filled cells and small-size cells with antirelaxation coating have been compared.

  11. The physical basis for absorption of light. [effects on wave functions of gas molecules and atoms

    NASA Technical Reports Server (NTRS)

    Pickett, H. M.

    1979-01-01

    The effects of light absorption on the wave functions of gas-phase molecules and atoms are investigated by high resolution spectral measurements of radiation emerging from a sample. A Stark-modulated sample of methyl fluoride was irradiated at the 102 GHz rotational transition and the emergent radiation was resolved by means of a spectrum analyzer. For signal oscillator frequencies below or above the molecular resonance by one modulation frequency, the amplitudes of the upper and lower modulation sidebands are found to be of nonuniform intensity, which is inconsistent with amplitude modulation. Emission due to polarization is, however, calculated to be consistent with the results observed, indicating that light absorption should be considered as a subtractive stimulated emission.

  12. Ablation-initiated Isotope-selective Atomic Absorption Spectroscopy of Lanthanide Elements

    SciTech Connect

    Miyabe, M.; Oba, M.; Iimura, H.; Akaoka, K.; Maruyama, Y.; Wakaida, I.; Watanabe, K.

    2009-03-17

    For remote isotope analysis of low-decontaminated trans-uranium (TRU) fuel, absorption spectroscopy has been applied to a laser-ablated plume of lanthanide elements. To improve isotopic selectivity and detection sensitivity of the ablated species, various experimental conditions were optimized. Isotope-selective absorption spectra were measured by observing the slow component of the plume produced under low-pressure rare-gas ambient. The measured minimum line width of about 0.9 GHz was close to the Doppler width of the Gd atomic transition at room temperature. The relaxation rate of high-lying metastable state was found to be higher than that of the ground state, which suggests that higher analytical sensitivity can be obtained using low-lying state transition. Under helium gas environment, Doppler splitting was caused from particle motion. This effect was considered for optimization for isotope selection and analysis. Some analytical performances of this method were determined under optimum conditions and were discussed.

  13. Absorption spectroscopy characterization measurements of a laser-produced Na atomic beam

    SciTech Connect

    Ching, C.H.; Bailey, J.E.; Lake, P.W.; Filuk, A.B.; Adams, R.G.; McKenney, J.

    1996-06-01

    This work describes a pulsed Na atomic beam source developed for spectroscopic diagnosis of a high-power ion diode on the Particle Beam Fusion Accelerator II. The goal is to produce a {approximately} 10{sup 12}-cm{sup {minus}3}-density Na atomic beam that can be injected into the diode acceleration gap to measure electric and magnetic fields from the Stark and Zeeman effects through laser-induced-fluorescence or absorption spectroscopy. A {approximately} 10 ns fwhm, 1.06 {micro}m, 0.6 J/cm{sup 2} laser incident through a glass slide heats a Na-bearing thin film, creating a plasma that generates a sodium vapor plume. A {approximately} 1 {micro}sec fwhm dye laser beam tuned to 5,890 {angstrom} is used for absorption measurement of the Na I resonant doublet by viewing parallel to the film surface. The dye laser light is coupled through a fiber to a spectrograph with a time-integrated CCD camera. A two-dimensional mapping of the Na vapor density is obtained through absorption measurements at different spatial locations. Time-of-flight and Doppler broadening of the absorption with {approximately} 0.1 {angstrom} spectral resolution indicate that the Na neutral vapor temperature is about 0.5 to 2 eV. Laser-induced-fluorescence from {approximately} 1 {times} 10{sup 12}-cm{sup {minus}3} Na I 3s-3p lines observed with a streaked spectrograph provides a signal level sufficient for {approximately} 0.06 {angstrom} wavelength shift measurements in a mock-up of an ion diode experiment.

  14. Neutral atomic absorption lines and far-UV extinction: Possible implications for depletions and grain parameters

    NASA Astrophysics Data System (ADS)

    Welty, Daniel E.

    1990-07-01

    Researchers examine nine lines of sight within the Galaxy and one in the Large Magellanic Cloud (LMC) for which data on both neutral atomic absorption lines (Snow 1984; White 1986; Welty, Hobbs, and York 1989) and far UV extinction (Bless and Savage 1972; Jenkins, Savage, and Spitzer 1986) are available, in order to test the assumption that variations in gamma/alpha will cancel in taking ratios of the ionization balance equation, and to try to determine to what extent that assumption has affected the aforementioned studies of depletions and grain properties.

  15. Determination of heavy metals in solid emission and immission samples using atomic absorption spectroscopy

    SciTech Connect

    Fara, M.; Novak, F.

    1995-12-01

    Both flame and electrothermal methods of atomic absorption spectroscopy (AAS) have been applied to the determination of Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, TI, Se, V and Zn in emission and emission (deposition) samples decomposed in open PTFE test-tubes by individual fuming-off hydrofluoric, perchloroic and nitric acid. An alternative hydride technique was also used for As and Se determination and Hg was determined using a self-contained AAS analyzer. A graphite platform proved good to overcome non-spectral interferences in AAS-ETA. Methods developed were verified by reference materials (inc. NBS 1633a).

  16. Refraction and absorption of x rays by laser-dressed atoms.

    SciTech Connect

    Buth, C.; Santra, R.; Young, L.

    2010-06-01

    X-ray refraction and absorption by neon atoms under the influence of an 800 nm laser with an intensity of 10{sup 13} W/cm{sup 2} is investigated. For this purpose, we use an ab initio theory suitable for optical strong-field problems. Its results are interpreted in terms of a three-level model. On the Ne 1s {yields} 3p resonance, we find electromagnetically induced transparency (EIT) for x rays. Our work opens novel perspectives for ultrafast x-ray pulse shaping.

  17. [Electrothermal atomic absorption determination of arsenic in plants and plant products].

    PubMed

    Karpova, E A; Malysheva, A G; Ermakov, A A; Sidorenkova, N K

    2012-01-01

    The authors have developed the optimal temperature-time parameters of electrothermal atomic absorption determination of arsenic in plants after their acid predigestion. The matrix modifier is 1% nickel nitrate or palladium nitrate solution. Cuvettes (ovens) are simple, made of porous or pyrolytic graphite. The analytical program is suitable for both spectrometers with Zeeman and deuterium background correction. The correctness of the procedure has been estimated from the results of analysis of state reference samples certified for their arsenic content. The coefficient of variation was 20-35% for the concentration range of 0.02-0.2 mg/kg. PMID:22712335

  18. The determination of aluminum, copper, iron, and lead in glycol formulations by atomic absorption spectroscopy

    NASA Technical Reports Server (NTRS)

    1977-01-01

    Initial screening tests and the results obtained in developing procedures to determine Al, Cu, Fe, and Pb in glycol formulations are described. Atomic absorption completion was selected for Cu, Fe and Pb, and after comparison with emission spectroscopy, was selected for Al also. Before completion, carbon, iron, and lead are extracted with diethyl dithio carbamate (DDC) into methyl isobutyl ketone (MIBK). Aluminum was also extracted into MIBK using 8-hydroxyquinoline as a chelating agent. As little as 0.02 mg/l carbon and 0.06 mg/l lead or iron may be determined in glycol formulations. As little as 0.3 mg/l aluminum may be determined.

  19. Telecom-heralded single-photon absorption by a single atom

    NASA Astrophysics Data System (ADS)

    Lenhard, Andreas; Bock, Matthias; Becher, Christoph; Kucera, Stephan; Brito, José; Eich, Pascal; Müller, Philipp; Eschner, Jürgen

    2015-12-01

    We present, characterize, and apply the architecture of a photonic quantum interface between the near infrared and telecom spectral regions. A singly resonant optical parametric oscillator (OPO) operated below threshold, in combination with external filters, generates high-rate (>2.5 ×106s-1 ) narrowband photon pairs (˜7 MHz bandwidth); the signal photons are tuned to resonance with an atomic transition in Ca+, while the idler photons are at telecom wavelength. Interface operation is demonstrated through high-rate absorption of single photons by a single trapped ion (˜670 s-1 ), heralded by coincident telecom photons.

  20. Automated atomic absorption spectrometric determination of total arsenic in water and streambed materials

    USGS Publications Warehouse

    Fishman, M.

    1977-01-01

    An automated method to determine both inorganic and organic forms of arsenic In water, water-suspended mixtures, and streambed materials Is described. Organic arsenic-containing compounds are decomposed by either ultraviolet radiation or by suHurlc acid-potassium persulfate digestion. The arsenic liberated, with Inorganic arsenic originally present, is reduced to arsine with sodium borohydrlde. The arable Is stripped from the solution with the aid of nitrogen and Is then decomposed In a tube furnace heated to 800 ??C which Is placed in the optical path of an atomic absorption spectrometer. Thirty samples per hour can be analyzed to levels of 1 ??g arsenic per liter.

  1. Determination of traces of silver in waters by anion exchange and atomic absorption spectrophotometry

    USGS Publications Warehouse

    Chao, T.T.; Fishman, M. J.; Ball, J.W.

    1969-01-01

    A method has been developed for the accurate determination of 0.1-1 ??g of silver per liter of water. The method permits stabilization of silver in water without loss to container walls. Optimum conditions have been established for the complete recovery of silver from water with an anion-exchange column, for quantitative elution of silver from the resin, and for measurement of silver by atomic absorption spectrophotometry after chelation with ammonium pyrrolidine dithiocarbamate and extraction of the chelate with MIBK. Silver in the 1-10 ??g 1 range can be determined by extraction without pre-concentration on an ion-exchange resin. ?? 1969.

  2. Determination of mercury in soils and sediments by graphite furnace atomic absorption spectrometry with slurry sampling

    NASA Astrophysics Data System (ADS)

    López-García, Ignacio; Sánchez-Merlos, Mateo; Hernández-Córdoba, Manuel

    1997-12-01

    A graphite furnace atomic absorption spectrometric procedure for the determination of mercury is presented, in which the samples are suspended in a solution containing hydrofluoric and nitric acids. Silver nitrate (4% m/v) and potassium permanganate (3%) are incorporated, in the order specified, and aliquots are directly introduced into the graphite furnace. A fast heating programme with no conventional pyrolysis step is used. The detection limit for mercury in a 125 mg ml -1 suspension is 0.1 μg g -1. Calibration is performed by using aqueous standards. The reliability of the procedure is proved by analysing certified reference materials.

  3. Neutral atomic absorption lines and far-UV extinction: Possible implications for depletions and grain parameters

    NASA Technical Reports Server (NTRS)

    Welty, Daniel E.

    1990-01-01

    Researchers examine nine lines of sight within the Galaxy and one in the Large Magellanic Cloud (LMC) for which data on both neutral atomic absorption lines (Snow 1984; White 1986; Welty, Hobbs, and York 1989) and far UV extinction (Bless and Savage 1972; Jenkins, Savage, and Spitzer 1986) are available, in order to test the assumption that variations in gamma/alpha will cancel in taking ratios of the ionization balance equation, and to try to determine to what extent that assumption has affected the aforementioned studies of depletions and grain properties.

  4. Analysis of lithium in deep basalt groundwaters using graphite furnace atomic absorption spectrophotometry

    SciTech Connect

    Dill, J.A.; Marcy, A.D.

    1986-05-01

    Lithium is under consideration for use as a reactive (sorptive) tracer in experiments designed to provide information regarding natural attenuation processes in a basalt-groundwater environment. In support of these activities, background lithium concentrations in samples obtained from a variety of test horizons have been determined using graphite furnace atomic absorption spectrophotometry. Significant interference was observed in these determinations and was found to be due to the presence of silicate in the samples. It was found that these problems could be circumvented through the use of alkaline silicate or synthetic groundwater matrix modifiers. This matrix effect was examined in some detail. Results obtained using the graphite furnace were compared to results obtained using inductively coupled plasma atomic emission spectroscopy.

  5. Atomic absorption determination of traces of cadmium in urine after electrodeposition onto a tungsten wire.

    PubMed

    Zhang, G; Li, J; Fu, D; Hao, D; Xiang, P

    1993-03-01

    A three-coil tungsten wire is used as electrode for the preconcentration of cadmium, which is then placed in a graphite tube for atomization and atomic absorption measurement. The heating parameters of the graphite furnace are optimized using the Modified and Weighted Centroid Simplex Method (MWCS), and computer program for automatic calculation. Sulphuric acid is selected as the supporting electrolyte for electrodeposition. The linear range of the calibration graph is 0.00-0.55 ng/ml. The detection limit is 0.01 ng/ml. For 0.1 ng/ml cadmium the coefficient of variation is 3.35% for ten parallel determinations. No interference occurs in the presence of more than 20 coexisting ions. Traces of cadmium in urine of normal people and in river water and the recoveries for cadmium are determined. The results are satisfactory. PMID:18965645

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

    PubMed

    Saavedra, Y; Fernández, P; González, A

    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 degrees C and 2600 degrees 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(-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(-1) (wet weight). PMID:14745471

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

    NASA Astrophysics Data System (ADS)

    Kántor, Tibor; Bartha, András

    2015-11-01

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

  8. Determination of ruthenium in pharmaceutical compounds by graphite furnace atomic absorption spectroscopy.

    PubMed

    Jia, Xiujuan; Wang, Tiebang; Bu, Xiaodong; Tu, Qiang; Spencer, Sandra

    2006-04-11

    A graphite furnace atomic absorption (GFAA) spectrometric method for the determination of ruthenium (Rh) in solid and liquid pharmaceutical compounds has been developed. Samples are dissolved or diluted in dimethyl sulfoxide (DMSO) without any other treatment before they were analyzed by GFAA with a carefully designed heating program to avoid pre-atomization signal loss and to achieve suitable sensitivity. Various inorganic and organic solvents were tested and compared and DMSO was found to be the most suitable. In addition, ruthenium was found to be stable in DMSO for at least 5 days. Spike recoveries ranged from 81 to 100% and the limit of quantitation (LOQ) was determined to be 0.5 microg g(-1) for solid samples or 0.005 microg ml(-1) for liquid samples based a 100-fold dilution. The same set of samples was also analyzed by ICP-MS with a different sample preparation method, and excellent agreement was achieved. PMID:16314066

  9. Determination of Copper by Graphite Furnace Atomic Absorption Spectrophotometry: A Student Exercise in Instrumental Methods of Analysis.

    ERIC Educational Resources Information Center

    Williamson, Mark A.

    1989-01-01

    Discusses a student exercise which requires the optimizing of the charring and atomization temperatures by producing a plot of absorbance versus temperature for each temperature parameter. Notes that although the graphite furnace atomic absorption spectroscopy technique has widespread industrial use, there are no published, structured experiments…

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

    NASA Astrophysics Data System (ADS)

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

    2008-02-01

    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.

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

    PubMed

    Küçükbay, F Zehra; Kuyumcu, Ebru

    2014-09-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of common cold have been studied for their mineral contents. Eleven minor and major elements (essential, non-essential and toxic) were identified in the Asplenium adiantum-nigrum L. , Althaea officinalis L. , Verbascum phlomoides L., Euphorbia chamaesyce L., Zizyphus jujube Miller, Peganum harmala L., Arum dioscoridis Sm., Sambucus nigra L., Piperlongum L., Tussilago farfara L. and Elettaria cardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrometry. Microwave digestion procedure for total concentration was applied under optimized conditions for dissolution of medicinal plants. Plant based biological certified reference materials (CRMs) served as standards for quantification. These elements are found to be present in varying concentrations in the studied plants. The baseline data presented in this work can be used in understanding the role of essential, non-essential and toxic elements in nutritive, preventive and therapeutic properties of medicinal plants. PMID:25532362

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

    PubMed

    Chen, Li-dan; Chen, Kai-kao

    2012-01-01

    The authors studied the innovative applications of atomic absorption spectrometry in the automatic transmission fault detection. After the authors have determined Fe, Cu and Cr contents in the five groups of Audi A6 main metal in automatic transmission fluid whose travel course is respectively 10-15 thousand kilometers, 20-26 thousand kilometers, 32-38 thousand kilometers, 43-49 thousand kilometers, and 52-58 thousand kilometers by atomic absorption spectrometry, the authors founded the database of primary metal content in the Audi A6 different mileage automatic transmission fluid (ATF). The research discovered that the main metal content in the automatic transmission fluid increased with the vehicles mileage and its normal metal content level in the automatic transmission fluid is between the two trend lines. The authors determined the main metal content of automatic transmission fluid which had faulty symptoms and compared it with its database value. Those can not only judge the wear condition of the automatic transmission which had faulty symptoms but also help the automobile detection and maintenance personnel to diagnose automatic transmission failure reasons without disintegration. This reduced automobile maintenance costs, and improved the quality of automobile maintenance. PMID:22497168

  13. Polarisation response of delay dependent absorption modulation in strong field dressed helium atoms probed near threshold

    NASA Astrophysics Data System (ADS)

    Simpson, E. R.; Sanchez-Gonzalez, A.; Austin, D. R.; Diveki, Z.; Hutchinson, S. E. E.; Siegel, T.; Ruberti, M.; Averbukh, V.; Miseikis, L.; Strüber, C. S.; Chipperfield, L.; Marangos, J. P.

    2016-08-01

    We present the first measurement of the vectorial response of strongly dressed helium atoms probed by an attosecond pulse train (APT) polarised either parallel or perpendicular to the dressing field polarisation. The transient absorption is probed as a function of delay between the APT and the linearly polarised 800 nm field of peak intensity 1.3× {10}14 {{W}} {{cm}}-2. The APT spans the photon energy range 16–42 eV, covering the first ionisation energy of helium (24.59 eV). With parallel polarised dressing and probing fields, we observe modulations with periods of one half and one quarter of the dressing field period. When the polarisation of the dressing field is altered from parallel to perpendicular with respect to the APT polarisation we observe a large suppression in the modulation depth of the above ionisation threshold absorption. In addition to this we present the intensity dependence of the harmonic modulation depth as a function of delay between the dressing and probe fields, with dressing field peak intensities ranging from 2 × 1012 to 2 × 1014 {{W}} {{cm}}-2. We compare our experimental results with a full-dimensional solution of the single-atom time-dependent (TD) Schrödinger equation obtained using the recently developed abinitio TD B-spline ADC method and find good qualitative agreement for the above threshold harmonics.

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

    USGS Publications Warehouse

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

    1982-01-01

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

  15. Determination of maduramicin by liquid chromatography with atomic absorption spectrometric detection.

    PubMed

    Johnson, N A

    1989-01-01

    A liquid chromatograph was interfaced to an atomic absorption spectrometer for the detection and quantitation of maduramicin in feed matrixes at the 1-8 ppm level. Ionophores in general form strong 1:1 products with various metal cations, yielding complexes that are insoluble in water but very soluble in organic solvents. Maduramicin, a carboxylic, polyalcohol, polyether antibiotic, is labeled with the sodium cation and analyzed by atomic absorption spectroscopy (AAS). The lower limit of detection is approximately 100-200 ng maduramicin sodium salt. Feeds containing 1-8 ppm maduramicin are extracted with acetone, the extract is passed through an alumina column, the column is eluted with acetonitrile-water (90 + 10), and the eluate is analyzed for maduramicin by liquid chromatography-AAS after concentration and conversion of maduramicin to the sodium salt. Recoveries of maduramicin averaged 89.5%. Liquid chromatography with AAS detection has been shown to be a sensitive and highly specific technique for the determination of ionophores in general and maduramicin in particular. PMID:2708270

  16. Atomic absorption spectroscopic, conductometric and colorimetric methods for determination of some fluoroquinolone antibacterials using ammonium reineckate

    NASA Astrophysics Data System (ADS)

    Al-Ghannam, Sheikha M.

    2008-04-01

    Three accurate, rapid and simple atomic absorption spectrometric (AAS), conductometric and colorimetric methods were developed for the determination of gatifloxacin (GTF), moxifloxacin (MXF) and sparfloxacin (SPF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at λmax 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone. The optimizations of various experimental conditions were described. Optimum concentration ranges for the determination of GTF, MXF and SPF were 5.0-150, 40-440 μg mL -1 and 0.10-1.5 mg mL -1 using atomic absorption (AAS), conductometric and colorimetric methods, respectively. Detection and quantification limits are ranges from 1.5 to 2.3 μg mL -1 using AAS method or 30-45 μg mL -1 using colorimetric method. The proposed procedures have been applied successfully to the analysis of these drugs in pharmaceutical formulations and the results are favourably comparable to the reference methods.

  17. Local atomic structure around Ni, Nb, and Zr atoms in Ni-Nb-Zr-H glassy alloys studied by x-ray absorption fine structure method

    NASA Astrophysics Data System (ADS)

    Oji, H.; Handa, K.; Ide, J.; Honma, T.; Yamaura, S.; Inoue, A.; Umesaki, N.; Emura, S.; Fukuhara, M.

    2009-06-01

    To elucidate hydrogen effects on the atomic configuration of Ni-Nb-Zr-H glassy alloys exhibiting proton-tunneling-induced Coulomb oscillation, we investigated the local atomic configuration around the Ni, Nb, and Zr atoms by x-ray absorption fine structure (XAFS) method. The analysis of the XAFS spectra indicates that there is the significant difference in structural response between the Zr 30 and the Zr 40 at. % alloys when hydrogen atoms are charged; charging the hydrogen atoms basically does not alter the local structures around the three atoms for the Zr 30 at. % alloy but induces the elongation of the Zr-Zr, Zr-Nb, and Nb-Ni distances for the Zr 40 at. % alloy. The distorted icosahedral Zr5Ni5Nb3 clusters assembled in randomly packed manners for the possible models in the Ni-Nb-Zr glassy alloy are proposed. The sites where hydrogen atoms occupy are also inferred.

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

    NASA Astrophysics Data System (ADS)

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

    1998-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2002-04-01

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

  20. Slurry sampling graphite furnace atomic absorption spectrometry: determination of trace metals in mineral coal.

    PubMed

    Silva, M M; Goreti, M; Vale, R; Caramão, E B

    1999-12-01

    A procedure for lead, cadmium and copper determination in coal samples based on slurry sampling using an atomic absorption spectrometer equipped with a transversely heated graphite tube atomizer is proposed. The slurries were prepared by weighing the samples directly into autosampler cups (5-30 mg) and adding a 1.5 ml aliquot of a diluent mixture of 5% v/v HNO(3), 0.05% Triton X-100 and 10% ethanol. The slurry was homogenized by manual stirring before measurement. Slurry homogenization using ultrasonic agitation was also investigated for comparison. The effect of particle size and the use of different diluent compositions on the slurry preparation were investigated. The temperature programmes were optimized on the basis of pyrolysis and atomization curves. Absorbance characteristics with and without the addition of a palladium-magnesium modifier were compared. The use of 0.05% m/v Pd and 0.03% m/v Mg was found satisfactory for stabilizing Cd and Pb. The calibration was performed with aqueous standards. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling. Better recoveries of the analytes were obtained when the particle size was reduced to <37 mum. Several certified coal reference materials (BCR Nos. 40, 180, and 181) were analyzed, and good agreement was obtained between the results from the proposed slurry sampling method and the certificate values. PMID:18967798

  1. Reduction of matrix interferences in furnace atomic absorption with the L'vov Platform

    USGS Publications Warehouse

    Kaiser, M.L.; Koirtyohann, S.R.; Hinderberger, E.J.; Taylor, H.E.

    1981-01-01

    Use of a modified L'vov Platform and ammonium phosphate as a matrix modifier greatly reduced matrix interferences in a commercial Massmann-type atomic absorption furnace. Platforms were readily fabricated from furnace tubes and, once positioned in the furnace, caused no inconvenience in operation. Two volatile elements (Pb, Cd), two of intermediate volatility (Co, Cr) and two which form stable oxides (Al, Sn) were tested in natural water and selected synthetic matrices. In every case for which there was a significant matrix effect during atomization from the tube wall, the platform and platform plus modifier gave improved performance. With lead, for example, an average ratio of 0.48 ?? 0.11 was found when the slope of the standard additions plot for six different natural water samples was compared to the slope of the standard working curve in dilute acid. The average slope ratio between the natural water matrices and the dilute acid matrix was 0.94 ?? 0.03 with the L'vov Platform and 0.96 ?? 0.03 with the platform and matrix modifier. In none of the cases studied did the use of the platform or platform plus modifier cause an interference problem where none existed while atomizing from the tube wall. An additional benefit of the platform was a factor of about two improvement in peak height precision. ?? 1981.

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

    NASA Astrophysics Data System (ADS)

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

    2000-05-01

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

  3. Direct determination of lead in wine materials by atomic absorption spectrometry using an electrothermal atomizer with a graphite filter-insert

    NASA Astrophysics Data System (ADS)

    Zacharia, A. N.; Zhuravlev, A. S.; Chebotarev, A. N.; Arabadgi, M. V.

    2013-01-01

    The operational parameters of an atomizer with a graphite filter-insert and a Pd-Mg matrix modifier are optimized for direct electrothermal atomic absorption determination of lead in some wines and associated materials. A method is proposed for eliminating interferences from mineral and organic components, as well as from nonatomic absorption, and for increasing the detection sensitivity for the element by up to a factor of two. The lower limit for determining the amount of lead in wines is 0.0025 mg/dm3. The relative standard deviation ( S r) does not exceed 10%.

  4. Development and Validation of Spectrophotometric, Atomic Absorption and Kinetic Methods for Determination of Moxifloxacin Hydrochloride

    PubMed Central

    Abdellaziz, Lobna M.; Hosny, Mervat M.

    2011-01-01

    Three simple spectrophotometric and atomic absorption spectrometric methods are developed and validated for the determination of moxifloxacin HCl in pure form and in pharmaceutical formulations. Method (A) is a kinetic method based on the oxidation of moxifloxacin HCl by Fe3+ ion in the presence of 1,10 o-phenanthroline (o-phen). Method (B) describes spectrophotometric procedures for determination of moxifloxacin HCl based on its ability to reduce Fe (III) to Fe (II), which was rapidly converted to the corresponding stable coloured complex after reacting with 2,2′ bipyridyl (bipy). The formation of the tris-complex formed in both methods (A) and (B) were carefully studied and their absorbance were measured at 510 and 520 nm respectively. Method (C) is based on the formation of ion- pair associated between the drug and bismuth (III) tetraiodide in acidic medium to form orange—red ion-pair associates. This associate can be quantitatively determined by three different procedures. The formed precipitate is either filtered off, dissolved in acetone and quantified spectrophotometrically at 462 nm (Procedure 1), or decomposed by hydrochloric acid, and the bismuth content is determined by direct atomic absorption spectrometric (Procedure 2). Also the residual unreacted metal complex in the filtrate is determined through its metal content using indirect atomic absorption spectrometric technique (procedure 3). All the proposed methods were validated according to the International Conference on Harmonization (ICH) guidelines, the three proposed methods permit the determination of moxifloxacin HCl in the range of (0.8–6, 0.8–4) for methods A and B, (16–96, 16–96 and 16–72) for procedures 1–3 in method C. The limits of detection and quantitation were calculated, the precision of the methods were satisfactory; the values of relative standard deviations did not exceed 2%. The proposed methods were successfully applied to determine the drug in its pharmaceutical

  5. Thermomechanical room and canister region benchmark analyses between STEALTH-WI and SPECTROM-32: Draft final report

    SciTech Connect

    Dial, B.W.; Maxwell, D.E.; Yee, G.

    1987-12-01

    This report documents the benchmarking of the two-dimensional waste isolation version of STEALTH (designated STEALTH-WI) against the thermomechanical performance assessment calculations performed by RE/SPEC using SPECTROM-32. An axisymmetric, canister-scale (very-near-field) analysis was performed to compute the peak stress exerted by the salt on the waste package. A plane strain, room-scale (near-field) analysis was also performed to predict disposal room roof-to-floor closure and the temperatures at key locations in the vicinity of the disposal room. Comparisons between the STEALTH and SPECTROM-32 results showed that the temperature predictions agreed to within 5/degree/C, peak canister stresses better than 10%, and the average roof-to-floor closures within 30%. The stress and displacement differences were attributed to differences in the treatment of plasticity in the constitutive laws for salt employed in STEALTH and SPECTROM-32. The temperature differences were due to minor differences in the thermal models employed in STEALTH and SPECTROM- 41, the thermal analysis code which supplies temperatures for SPECTROM-32. 9 refs., 21 figs., 6 tabs.

  6. Atomic Oxygen Abundance in Molecular Clouds: Absorption Toward Sagittarius B2

    NASA Technical Reports Server (NTRS)

    Lis, D. C.; Keene, Jocelyn; Phillips, T. G.; Schilke, P.; Werner, M. W.; Zmuidzinas, J.

    2001-01-01

    We have obtained high-resolution (approximately 35 km/s) spectra toward the molecular cloud Sgr B2 at 63 micrometers, the wavelength of the ground-state fine-structure line of atomic oxygen (O(I)), using the ISO-LWS instrument. Four separate velocity components are seen in the deconvolved spectrum, in absorption against the dust continuum emission of Sgr B2. Three of these components, corresponding to foreground clouds, are used to study the O(I) content of the cool molecular gas along the line of sight. In principle, the atomic oxygen that produces a particular velocity component could exist in any, or all, of three physically distinct regions: inside a dense molecular cloud, in the UV illuminated surface layer (PDR) of a cloud, and in an atomic (H(I)) gas halo. For each of the three foreground clouds, we estimate, and subtract from the observed O(I) column density, the oxygen content of the H(I) halo gas, by scaling from a published high-resolution 21 cm spectrum. We find that the remaining O(I) column density is correlated with the observed (13)CO column density. From the slope of this correlation, an average [O(I)]/[(13)CO] ratio of 270 +/- 120 (3-sigma) is derived, which corresponds to [O(I)]/[(13)CO] = 9 for a CO to (13)CO abundance ratio of 30. Assuming a (13)CO abundance of 1x10(exp -6) with respect to H nuclei, we derive an atomic oxygen abundance of 2.7x10(exp -4) in the dense gas phase, corresponding to a 15% oxygen depletion compared to the diffuse ISM in our Galactic neighborhood. The presence of multiple, spectrally resolved velocity components in the Sgr B2 absorption spectrum allows, for the first time, a direct determination of the PDR contribution to the O(I) column density. The PDR regions should contain O(I) but not (13)CO, and would thus be expected to produce an offset in the O(I)-(13)CO correlation. Our data do not show such an offset, suggesting that within our beam O(I) is spatially coexistent with the molecular gas, as traced by (13)CO

  7. An atomic-absorption method for the determination of gold in large samples of geologic materials

    USGS Publications Warehouse

    VanSickle, Gordon H.; Lakin, Hubert William

    1968-01-01

    A laboratory method for the determination of gold in large (100-gram) samples has been developed for use in the study of the gold content of placer deposits and of trace amounts of gold in other geologic materials. In this method the sample is digested with bromine and ethyl ether, the gold is extracted into methyl isobutyl ketone, and the determination is made by atomicabsorption spectrophotometry. The lower limit of detection is 0.005 part per million in the sample. The few data obtained so far by this method agree favorably with those obtained by assay and by other atomic-absorption methods. About 25 determinations can be made per man-day.

  8. Automation of preparation of nonmetallic samples for analysis by atomic absorption and inductively coupled plasma spectrometry

    NASA Technical Reports Server (NTRS)

    Wittmann, A.; Willay, G.

    1986-01-01

    For a rapid preparation of solutions intended for analysis by inductively coupled plasma emission spectrometry or atomic absorption spectrometry, an automatic device called Plasmasol was developed. This apparatus used the property of nonwettability of glassy C to fuse the sample in an appropriate flux. The sample-flux mixture is placed in a composite crucible, then heated at high temperature, swirled until full dissolution is achieved, and then poured into a water-filled beaker. After acid addition, dissolution of the melt, and filling to the mark, the solution is ready for analysis. The analytical results obtained, either for oxide samples or for prereduced iron ores show that the solutions prepared with this device are undistinguished from those obtained by manual dissolutions done by acid digestion or by high temperature fusion. Preparation reproducibility and analytical tests illustrate the performance of Plasmasol.

  9. Determination of total mercury in human hair and animal fur by combustion atomic absorption spectrometry.

    PubMed

    Cizdziel, J V; Gerstenberger, Shawn

    2004-11-15

    A commercially available mercury (Hg) analyzer based on sample combustion, gold amalgamation, and atomic absorption spectrometry (AAS) was evaluated for the direct determination of Hg in composites of human hair and individual samples of horse fur. Results for human hair reference material (NIES No. 13) were within the certified range. Analyses of "blind" samples from an international interlaboratory (n>16) comparison study produced results within 1S.D. of the consensus means. Precision (%R.S.D.) was found to be <5% and total analyses time per sample was <10min. This study demonstrated that analyzers based on combustion-AAS are suitable for wide-scale monitoring of Hg in human hair and animal fur. PMID:18969690

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

    PubMed

    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. PMID:27566338

  11. Removal of iron interferences by solvent extraction for geochemical analysis by atomic-absorption spectrophotometry

    USGS Publications Warehouse

    Zhou, L.; Chao, T.T.; Sanzolone, R.F.

    1985-01-01

    Iron is a common interferent in the determination of many elements in geochemical samples. Two approaches for its removal have been taken. The first involves removal of iron by extraction with methyl isobutyl ketone (MIBK) from hydrochloric acid medium, leaving the analytes in the aqueous phase. The second consists of reduction of iron(III) to iron(II) by ascorbic acid to minimize its extraction into MIBK, so that the analytes may be isolated by extraction. Elements of interest can then be determined using the aqueous solution or the organic extract, as appropriate. Operating factors such as the concentration of hydrochloric acid, amounts of iron present, number of extractions, the presence or absence of a salting-out agent, and the optimum ratio of ascorbic acid to iron have been determined. These factors have general applications in geochemical analysis by atomic-absorption spectrophotometry. ?? 1985.

  12. [Preliminary study on using acousto-optic tunable filter as wavelength selector for atomic absorption spectrometry].

    PubMed

    Zhao, Li-wei; Zhang, Yi-hua; Wang, Mei-jia; Song, Da-qian; Zhang, Han-qi; Jin, Qin-han

    2002-06-01

    An acousto-optic tunable filter (AOTF) is an all-solid-state, electronic monochromator that is based on the diffraction of light by an acoustic wave in an anisotropic crystal. It is a new kind of tunable small filter with narrow band compared with traditional unicolor filter. The filter can diffract incident white light at a specific wavelength when a specific radio frequency is applied into it. An AAS experimental setup using a microwave plasma torch (MPT) as the atomizer, and a visible AOTF as the wavelength selector was developed and the analytical performance was evaluated by determination of Na. The effect on the absorption signal of some operating conditions, including the observation height, the microwave forward power and the carrier and support gas flow rates for MPT, were investigated. The detection limit for Na was shown to be 0.23 microgram.mL-1 and the relative standard deviation was 2.6% (n = 6). PMID:12938338

  13. Indirect determination of trace phenol in water by atomic-absorption spectrophotometry.

    PubMed

    Bo-Xing, X; Tong-Ming, X; Ming-Neng, S; Yu-Zhi, F

    1985-03-01

    An indirect method for determination of trace phenol in water by atomic-absorption spectrophotometry (AAS) is described. The phenol is brominated in acidic solution with KBrO(3)-KBr solution at room temperature. The excess of bromine is reacted with KI and the I(2) produced is extracted into cyclohexane and then reduced back to I(-) with ascorbic acid. The I(-) is then complexed with Cd(2+) in sulphuric acid medium and the complex extracted into MIBK. The extract is analysed by flame AAS for Cd (and hence indirectly for phenol). The linear concentration range for determination of phenol is 6 x 10(-7)-0.9 x 10(-5)M in aqueous solution. Several foreign ions and organic substances do not interfere. PMID:18963829

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

    NASA Astrophysics Data System (ADS)

    Coufalík, Pavel; Zvěřina, Ondřej; Komárek, Josef

    2016-04-01

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

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

    PubMed

    Çiftçi, Tülin Deniz; Henden, Emur

    2016-08-01

    Arsenic in drinking water is a serious problem for human health. Since the toxicity of arsenic species As(III) and As(V) is different, it is important to determine the concentrations separately. Therefore, it is necessary to develop an accurate and sensitive method for the speciation of arsenic. It was intended with this work to determine the concentrations of arsenic species in water samples collected from Izmir, Manisa and nearby areas. A batch type hydride generation atomic absorption spectrometer was used. As(V) gave no signal under the optimal measurement conditions of As(III). A certified reference drinking water was analyzed by the method and the results showed excellent agreement with the reported values. The procedure was applied to 34 water samples. Eleven tap water, two spring water, 19 artesian well water and two thermal water samples were analyzed under the optimal conditions. PMID:27236436

  16. Determination of butyltin metabolites in the mouse liver by flameless atomic absorption spectrophotometry.

    PubMed

    Uneo, S; Susa, N; Furukawa, Y

    1995-08-01

    A new analytical method for observation of the metabolic status of butyltin compounds in the mouse liver was devised by a combination of extraction, purification and separation followed by quantitative analysis of each butyltin compound. After the extraction of all tin compounds from liver homogenate with ethyl acetate, these compounds were purified by combination of the fractional extract with organic solvents and column chromatography. The purified fraction was also analyzed by thin-layer chromatography, identifying each tin compound from differences in mobility on a silica gel plate. The tin content in the each separated spot on the plates was measured by flameless atomic absorption spectrophotometry after extraction by acid treatment. About 90% of tin was recovered by this method from the liver of mice which had been administered tri- or dibutyltin compound orally. This method will be useful for quantification of each metabolic product formed from butyltin compounds in vivo. PMID:8519922

  17. A summary of transition probabilities for atomic absorption lines formed in low-density clouds

    NASA Technical Reports Server (NTRS)

    Morton, D. C.; Smith, W. H.

    1973-01-01

    A table of wavelengths, statistical weights, and excitation energies is given for 944 atomic spectral lines in 221 multiplets whose lower energy levels lie below 0.275 eV. Oscillator strengths were adopted for 635 lines in 155 multiplets from the available experimental and theoretical determinations. Radiation damping constants also were derived for most of these lines. This table contains the lines most likely to be observed in absorption in interstellar clouds, circumstellar shells, and the clouds in the direction of quasars where neither the particle density nor the radiation density is high enough to populate the higher levels. All ions of all elements from hydrogen to zinc are included which have resonance lines longward of 912 A, although a number of weaker lines of neutrals and first ions have been omitted.

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

    USGS Publications Warehouse

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

    1976-01-01

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

  19. Laser absorption spectroscopy diagnostics of helium metastable atoms generated in dielectric barrier discharge cryoplasmas

    NASA Astrophysics Data System (ADS)

    Urabe, Keiichiro; Muneoka, Hitoshi; Stauss, Sven; Sakai, Osamu; Terashima, Kazuo

    2015-10-01

    Cryoplasmas, which are plasmas whose gas temperatures are below room temperature (RT), have shown dynamic changes in their physical and chemical characteristics when the gas temperature in the plasmas (Tgp) was decreased from RT. In this study, we measured the temporal behavior of helium metastable (Hem) atoms generated in a parallel-plate dielectric barrier discharge at ambient gas temperatures (Tga) of 300, 100, and 14 K and with a gas density similar to atmospheric conditions by laser absorption spectroscopy. The increments of Tgp to Tga were less than 20 K. We found from the results that the Hem lifetime and maximum density become longer and larger over one order of magnitude for lower Tga. The reasons for the long Hem lifetime at low Tga are decreases in the rate coefficients of three-body Hem quenching reactions and in the amounts of molecular impurities with boiling points higher than that of He.

  20. Development of mixed-waste analysis capability for graphite furnace atomic absorption spectrophotometry

    SciTech Connect

    Bass, D.A.; TenKate, L.B.; Wroblewski, A.

    1995-03-01

    Graphite furnace atomic absorption spectrophotometer (GFAAS) are typically configured with ventilation to capture potentially toxic and corrosive gases emitted from the vaporization of sample aliquots. When radioactive elements are present, additional concerns (such as meeting safety guidelines and ALARA principles) must be addressed. This report describes a modification to a GFAAS that provides additional containment of vaporized sample aliquots. The modification was found to increase containment by a factor of 80, given expected operating conditions. The use of the modification allows more mixed-waste samples to be analyzed, permits higher levels of radioactive samples to be analyzed, or exposes the analyst to less airborne radioactivity. The containment apparatus was attached to a Perkin-Elmer Zeeman 5000 spectrophotometer for analysis of mixed-waste samples; however, it could also be used on other systems and in other applications where greater containment of vaporized material is desired.

  1. Near resonant absorption by atoms in intense fluctuating laser fields. Final report

    SciTech Connect

    Smith, S.J.

    1994-01-01

    The objective of this program was to make quantitative measurements of the effects of higher-order phase/frequency correlations in a laser beam on nonlinear optical absorption processes in atoms. The success of this program was due in large part to a unique experimental capability for modulating the extracavity beam of a stabilized ({approx_lt}200 kHz) continuous-wave laser with statistically-well-characterized stochastic phase (or frequency) fluctuations, in order to synthesize laser bandwidths to {approximately}20 MHz (depending on noise amplitude), with profiles variable between Gaussian and Lorentzian (depending on noise bandwidth). Laser driven processes investigated included the following: (1) the optical Autler-Towns effect in the 3S{sub 1/2} (F = 2, M{sub F} = 2) {yields} 3P{sub 3/2} (F = 3, M{sub F} = 3) two- level Na resonance, using a weak probe to the 4D{sub 5/2} level; (2) the variance and spectra of fluorescence intensity fluctuations in the two-level Na resonance; (3) the Hanle effect in the {sup 1}S{sub 0} {minus} {sup 3}P{sub 1}, transition at {lambda} = 555.6 nm in {sup 174} Yb; (4) absorption (and gain) of a weak probe, when the probe is a time-delayed replica of the resonant (with the two-level Na transition) pump laser; and (5) four-wave-mixing in a phase-conjugate geometry, in a sodium cell, and, finally, in a diffuse atomic sodium beam. The experimental results from these several studies have provided important confirmation of advanced theoretical methods.

  2. Determination of Hg, Cd, Mn, Pb and Sn in seafood by solid sampling Zeeman atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Detcheva, A.; Grobecker, K. H.

    2006-04-01

    Direct solid sampling Zeeman atomic absorption spectrometric methods were developed and applied to the determination of mercury, cadmium, manganese, lead and tin in seafood. All elements but mercury were measured by a third generation Zeeman atomic absorption spectrometry combined with an automatic solid sampler. In 3-field- and dynamic mode the calibrations concentration range was substantially extended and high amounts of analyte were detectable without laborious dilution of solid samples. The measurements were based on calibrations using certified reference materials of organic matrices. In case solid certified reference materials were not available calibration by aqueous standard solutions was proved to be an alternative. No matrix effects were observed under the optimized conditions. Results obtained were in good agreement with the certified values. Solid sampling Zeeman atomic absorption spectrometry proved to be a reliable, rapid and low-cost method for the control of trace elements in seafood.

  3. Free-free absorption of infrared radiation in collisions of electrons with neutral rare-gas atoms

    NASA Technical Reports Server (NTRS)

    Stallcop, J. R.

    1974-01-01

    A relationship between the inverse bremsstrahlung absorption cross section and the electron neutral momentum transfer cross section has been utilized to determine the infrared free-free continuum absorption coefficient for the negative ions of helium, neon, argon, krypton, and xenon. The values of the momentum transfer cross section for this calculation have been obtained from experimental measurements. Analytical expressions for the absorption coefficient have also been developed. From the results of this calculation, it is possible to determine the absorption coefficient per unit electron density per neutral atom for temperatures in the range from 2500 to 25,000 K. The results are compared with those from tabulations of previous calculations and those computed from theoretical values of the phase shifts for the elastic scattering of electrons by neutral atoms.

  4. Graphite furnace-atomic absorption spectrophotometric determination of palladium in soil.

    PubMed

    Patel, K S; Sharma, P C; Hoffmann, P

    2000-08-01

    A new and sensitive procedure for the graphite furnace-atomic absorption spectrophotometric (GF-AAS) determination of Pd in soil at nanogram level is described. The method is based on prior separation and enrichment of the metal as Pd(II)-SnCl3- -N-butylacetamide (BAA) complex into 1-pentanol (PN) by solvent extraction method. The value of the molar absorptivity of the complex in three solvents, i.e. ethyl acetate, 1-pentanol, chloroform, lie in the range of (0.70-2.75) x 10(4) L mol(-1) cm(-1) at lambda(max) 360-440 nm. The metal could be enriched into organic solvent, i.e. PN, up to 10-folds. The sensitivity (A = 0.0044) of the method in the term of the peak height was 0.5 ng Pd/mL of the aqueous solution at an enrichment factor (EF) of 5. Optimization of analytical variables during enrichment and GF-AAS determination of the metal are discussed. The method has been applied for the analysis of Pd to soil samples derived from roads and highways in Germany. PMID:11220609

  5. ARECIBO MULTI-EPOCH H I ABSORPTION MEASUREMENTS AGAINST PULSARS: TINY-SCALE ATOMIC STRUCTURE

    SciTech Connect

    Stanimirovic, S.; Weisberg, J. M.; Pei, Z.; Tuttle, K.; Green, J. T.

    2010-09-01

    We present results from multi-epoch neutral hydrogen (H I) absorption observations of six bright pulsars with the Arecibo telescope. Moving through the interstellar medium (ISM) with transverse velocities of 10-150 AU yr{sup -1}, these pulsars have swept across 1-200 AU over the course of our experiment, allowing us to probe the existence and properties of the tiny-scale atomic structure (TSAS) in the cold neutral medium (CNM). While most of the observed pulsars show no significant change in their H I absorption spectra, we have identified at least two clear TSAS-induced opacity variations in the direction of B1929+10. These observations require strong spatial inhomogeneities in either the TSAS clouds' physical properties themselves or else in the clouds' galactic distribution. While TSAS is occasionally detected on spatial scales down to 10 AU, it is too rare to be characterized by a spectrum of turbulent CNM fluctuations on scales of 10{sup 1}-10{sup 3} AU, as previously suggested by some work. In the direction of B1929+10, an apparent correlation between TSAS and interstellar clouds inside the warm Local Bubble (LB) indicates that TSAS may be tracing the fragmentation of the LB wall via hydrodynamic instabilities. While similar fragmentation events occur frequently throughout the ISM, the warm medium surrounding these cold cloudlets induces a natural selection effect wherein small TSAS clouds evaporate quickly and are rare, while large clouds survive longer and become a general property of the ISM.

  6. DETERMINATION OF LEAD AND CADMIUM IN FISH AND CLAM TISSUE BY ATOMIC ABSORPTION SPECTROMETRY WITH A MOLYBDENUM AND LANTHANUM TREATED PYROLYTIC GRAPHITE ATOMIZER

    EPA Science Inventory

    A molybdenum and lanthanum treated pyrolytically coated graphite tube is employed for the furnace atomic absorption spectrometric determination of lead and cadmium directly in nitric-perchloric acid tissue digests. Lanthanum tends to promote the formation of a smooth lead atomiza...

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

    NASA Astrophysics Data System (ADS)

    Huang, Zhuo-er

    1995-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2012-05-01

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

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

    PubMed

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

    2001-08-01

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

  10. Preconcentration and determination of tellurium in garlic samples by hydride generation atomic absorption spectrometry.

    PubMed

    Kaplan, Marcos M; Cerutti, Soledad; Salonia, José A; Gásquez, José A; Martinez, Luis D

    2005-01-01

    A procedure for the determination of traces of total tellurium (Te) in garlic (Allium sativa) is described that combines hydride generation atomic absorption spectrometry with preconcentration of the analyte by coprecipitation. The samples, each spiked with lanthanum nitrate (20 mg/L), are introduced into an Amberlite XAD-4 resin and mixed with ammonium buffer (pH 9.1). Te is preconcentrated by coprecipitation with the generated lanthanum hydroxide precipitate. The precipitate is quantitatively collected in the resin, eluted with hydrochloric acid, and then transferred into the atomizer device. Considering a sample consumption of 25 mL, an enrichment factor of 10 was obtained. The detection limit (3sigma) was 0.03 microg/L, and the precision (relative standard deviation) was 3.5% (n = 10) at the 10 microg/L level. The calibration graph using the preconcentration system for Te was linear with a correlation coefficient of 0.9993. Satisfactory results were obtained for the analysis of Te in garlic samples. PMID:16152948

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

    PubMed

    Saber-Tehrani, Mohammad; Hashemi-Moghaddam, Hamid; Givianrad, Mohammad Hadi; Abroomand-Azar, Parviz

    2006-11-01

    An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 mug g(-1) and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%. PMID:16896613

  12. Determination of trace elements in automotive fuels by filter furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Anselmi, Anna; Tittarelli, Paolo; Katskov, Dmitri A.

    2002-03-01

    The determination of Cd, Cr, Cu, Pb and Ni was performed in gasoline and diesel fuel samples by electrothermal atomic absorption spectrometry using the Transverse Heated Filter Atomizer (THFA). Thermal conditions were experimentally defined for the investigated elements. The elements were analyzed without addition of chemical modifiers, using organometallic standards for the calibration. Forty-microliter samples were injected into the THFA. Gasoline samples were analyzed directly, while diesel fuel samples were diluted 1:4 with n-heptane. The following characteristic masses were obtained: 0.8 pg Cd, 6.4 pg Cr, 12 pg Cu, 17 pg Pb and 27 pg Ni. The limits of determination for gasoline samples were 0.13 μg/kg Cd, 0.4 μg/kg Cr, 0.9 μg/kg Cu, 1.5 μg/kg Pb and 2.5 μg/kg Ni. The corresponding limit of determination for diesel fuel samples was approximately four times higher for all elements. The element recovery was performed using the addition of organometallic compounds to gasoline and diesel fuel samples and was between 85 and 105% for all elements investigated.

  13. Direct determination and speciation of mercury compounds in environmental and biological samples by carbon bed atomic absorption spectroscopy

    SciTech Connect

    Skelly, E.M.

    1982-01-01

    A method was developed for the direct determination of mercury in water and biological samples using a unique carbon bed atomizer for atomic absorption spectroscopy. The method avoided sources of error such as loss of volatile mercury during sample digestion and contamination of samples through added reagents by eliminating sample pretreatment steps. The design of the atomizer allowed use of the 184.9 nm mercury resonance line in the vacuum ultraviolet region, which increased sensitivity over the commonly used spin-forbidden 253.7 nm line. The carbon bed atomizer method was applied to a study of mercury concentrations in water, hair, sweat, urine, blood, breath and saliva samples from a non-occupationally exposed population. Data were collected on the average concentration, the range and distribution of mercury in the samples. Data were also collected illustrating individual variations in mercury concentrations with time. Concentrations of mercury found were significantly higher than values reported in the literature for a ''normal'' population. This is attributed to the increased accuracy gained by eliminating pretreatment steps and increasing atomization efficiency. Absorption traces were obtained for various solutions of pure and complexed mercury compounds. Absorption traces of biological fluids were also obtained. Differences were observed in the absorption-temperatures traces of various compounds. The utility of this technique for studying complexation was demonstrated.

  14. Electrothermal atomic absorption spectrometric determination of arsenic in essential lavender and rose oils.

    PubMed

    Karadjova, Irina B; Lampugnani, Leonardo; Tsalev, Dimiter L

    2005-02-28

    Analytical procedures for electrothermal atomic absorption spectrometric (ETAAS) determination of arsenic in essential oils from lavender (Lavendula angustifolia) and rose (Rosa damascena) are described. For direct ETAAS analysis, oil samples are diluted with ethanol or i-propanol for lavender and rose oil, respectively. Leveling off responses of four different arsenic species (arsenite, arsenate, monomethylarsonate and dimethylarsinate) is achieved by using a composite chemical modifier: l-cysteine (0.05gl(-1)) in combination with palladium (2.5mug) and citric acid (100mug). Transverse-heated graphite atomizer (THGA) with longitudinal Zeeman-effect background correction and 'end-capped' graphite tubes with integrated pyrolytic graphite platforms, pre-treated with Zr-Ir for permanent modification are employed as most appropriate atomizer. Calibration with solvent-matched standard solutions of As(III) is used for four- and five-fold diluted samples of lavender and rose oil, respectively. Lower dilution factors required standard addition calibration by using aqueous (for lavender oil) or i-propanol (for rose oil) solutions of As(III). The limits of detection (LOD) for the whole analytical procedure are 4.4 and 4.7ngg(-1) As in levender and rose oil, respectively. The relative standard deviation (R.S.D.) for As at 6-30ngg(-1) levels is between 8 and 17% for both oils. As an alternative, procedure based on low temperature plasma ashing in oxygen with ETAAS, providing LODs of 2.5 and 2.7ngg(-1) As in levender and rose oil, respectively, and R.S.D. within 8-12% for both oils has been elaborated. Results obtained by both procedures are in good agreement. PMID:18969904

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

    PubMed

    Salih, Bekir; Celikbiçak, Omür; Döker, Serhat; Doğan, Mehmet

    2007-03-28

    Poly(N-(hydroxymethyl)methacrylamide)-1-allyl-2-thiourea) hydrogels, poly(NHMMA-ATU), were synthesized by gamma radiation using (60)Co gamma source in the ternary mixture of NHMMA-ATU-H(2)O. These hydrogels were used for the specific gold, silver, platinum and palladium recovery, pre-concentration and matrix elimination from the solutions containing trace amounts of precious metal ions. Elimination of inorganic matrices such as different transition and heavy metal ions, and anions was performed by adjusting the solution pH to 0.5 that was the selective adsorption pH of the precious metal ions. Desorption of the precious metal ions was performed by using 0.8 M thiourea in 3M HCl as the most efficient desorbing agent with recovery values more than 95%. In the desorption medium, thiourea effect on the atomic signal was eliminated by selecting proper pyrolysis and atomization temperatures for all precious metal ions. Precision and the accuracy of the results were improved in the graphite furnace-atomic absorption spectrometer (GFAAS) measurements by applying the developed matrix elimination method performing the adsorption at pH 0.5. Pre-concentration factors of the studied precious metal ions were found to be at least 1000-fold. Detection limits of the precious metal ions were found to be less than 10 ng L(-1) of the all studied precious metal ions by using the proposed pre-concentration method. Determination of trace levels of the precious metals in the sea-water, anode slime, geological samples and photographic fixer solutions were performed using GFAAS clearly after applying the adsorption-desorption cycle onto the poly(NHMMA-UTU) hydrogels. PMID:17386783

  16. Tributyl phosphate as a sensitivity-enhancing solvent for organotin in carbon furnace atomic absorption spectrometry.

    PubMed

    Li, H; Gong, B; Matsumoto, K

    1996-07-01

    Tributyl phosphate (TBP) has been found to be a sensitivity-enhancing solvent for organotin compounds in graphite furnace atomic absorption spectrometry; (C(4)H(9))(2)Sn(O(2)CCH(3))(2), (C(4)H(9))(2)Sn(O(2)CC(11)H(23))(2), (C(4)H(9))(3)SnCl, and (C(4)H(9))(4)Sn all give 1 order of magnitude higher sensitivities in TBP than in toluene or ethyl acetate. The sensitivities are enhanced further 1-2 orders of magnitude in TBP, when PdCl(2)(CH(3)CN)(2) is added as a matrix modifier in the organic solvent. Among the four organotin compounds, (C(4)H(9))(2)Sn(O(2)CCH(3))(2) and (C(4)H(9))(2)Sn(O(2)CC(11)H(23))(2) give better sensitivities than (C(4)H(9))(3)SnCl and (C(4)H(9))(4)Sn in the absence of palladium in any organic solvent, which suggests that the oxygen atom in the tin compound might form tin oxides that are resistant to volatilization loss during ashing. Scanning electron microscopic, electrothermal vaporization ICPMS, and powder X-ray diffraction studies show that the final products before atomization include phosphorus-containing compounds Sn(2)P(2)O(7), SnP(2)O(7), and Pd(9)P(2), besides tin-palladium alloys, PdSn, Pd(3)Sn, Pd(2)Sn, Pd(3)Sn(2), and PdSn(3). These phosphorus-containing compounds would more efficiently stabilize tin and suppress tin vaporization loss during ashing, to give higher sensitivity. PMID:21619315

  17. Spectroscopy of 1S0- 3P1 transition of magnesium atom in an external absorption cell

    NASA Astrophysics Data System (ADS)

    Bagayev, S. N.; Baraulya, V. I.; Bonert, A. E.; Goncharov, A. N.; Seydaliev, M. R.

    2001-09-01

    The results of saturated absorption spectroscopy of the intercombination 1S0- 3P1 transition of magnesium atoms at 457 nm in an external absorption cell are presented. A laser system based on a Ti:Sa laser with frequency doubling in a LBO nonlinear crystal was used in these experiments. Saturated absorption resonances of magnesium in an external cell at the 1S0- 3P1 transition have been obtained for the first time. Pressure broadening of resonances equal to 12.5±1.5 kHz/mTorr has been measured.

  18. Atomic Transition Frequencies, Isotope Shifts, and Sensitivity to Variation of the Fine Structure Constant for Studies of Quasar Absorption Spectra

    NASA Astrophysics Data System (ADS)

    Berengut, J. C.; Dzuba, V. A.; Flambaum, V. V.; King, J. A.; Kozlov, M. G.; Murphy, M. T.; Webb, J. K.

    Theories unifying gravity with other interactions suggest spatial and temporal variation of fundamental "constants" in the Universe. A change in the fine structure constant, α = {e}2/hslash c , could be detected via shifts in the frequencies of atomic transitions in quasar absorption systems. Recent studies using 140 absorption systems from the Keck telescope and 153 from the Very Large Telescope, suggest that α varies spatially (61). That is, in one direction on the sky α seems to have been smaller at the time of absorption, while in the opposite direction it seems to have been larger.

  19. Mini-Column Ion-Exchange Separation and Atomic Absorption Quantitation of Nickel, Cobalt, and Iron: An Undergraduate Quantitative Analysis Experiment.

    ERIC Educational Resources Information Center

    Anderson, James L.; And Others

    1980-01-01

    Presents an undergraduate quantitative analysis experiment, describing an atomic absorption quantitation scheme that is fast, sensitive and comparatively simple relative to other titration experiments. (CS)

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

    NASA Astrophysics Data System (ADS)

    Katskov, Dmitri; Hlongwane, Miranda; Heitmann, Uwe; Florek, Stefan

    2012-05-01

    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 μg·L- 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.

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

    NASA Astrophysics Data System (ADS)

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

    2001-10-01

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

  2. A Simplified Digestion Protocol for the Analysis of Hg in Fish by Cold Vapor Atomic Absorption Spectroscopy

    ERIC Educational Resources Information Center

    Kristian, Kathleen E.; Friedbauer, Scott; Kabashi, Donika; Ferencz, Kristen M.; Barajas, Jennifer C.; O'Brien, Kelly

    2015-01-01

    Analysis of mercury in fish is an interesting problem with the potential to motivate students in chemistry laboratory courses. The recommended method for mercury analysis in fish is cold vapor atomic absorption spectroscopy (CVAAS), which requires homogeneous analyte solutions, typically prepared by acid digestion. Previously published digestion…

  3. Overcoming Matrix Effects in a Complex Sample: Analysis of Multiple Elements in Multivitamins by Atomic Absorption Spectroscopy

    ERIC Educational Resources Information Center

    Arnold, Randy J.; Arndt, Brett; Blaser, Emilia; Blosser, Chris; Caulton, Dana; Chung, Won Sog; Fiorenza, Garrett; Heath, Wyatt; Jacobs, Alex; Kahng, Eunice; Koh, Eun; Le, Thao; Mandla, Kyle; McCory, Chelsey; Newman, Laura; Pithadia, Amit; Reckelhoff, Anna; Rheinhardt, Joseph; Skljarevski, Sonja; Stuart, Jordyn; Taylor, Cassie; Thomas, Scott; Tse, Kyle; Wall, Rachel; Warkentien, Chad

    2011-01-01

    A multivitamin tablet and liquid are analyzed for the elements calcium, magnesium, iron, zinc, copper, and manganese using atomic absorption spectrometry. Linear calibration and standard addition are used for all elements except calcium, allowing for an estimate of the matrix effects encountered for this complex sample. Sample preparation using…

  4. VUV absorption spectroscopy measurements of the role of fast neutral atoms in high-power gap breakdown

    SciTech Connect

    FILUK,A.B.; BAILEY,JAMES E.; CUNEO,MICHAEL E.; LAKE,PATRICK WAYNE; NASH,THOMAS J.; NOACK,DONALD D.; MARON,Y.

    2000-03-20

    The maximum power achieved in a wide variety of high-power devices, including electron and ion diodes, z pinches, and microwave generators, is presently limited by anode-cathode gap breakdown. A frequently-discussed hypothesis for this effect is ionization of fast neutral atoms injected throughout the anode-cathode gap during the power pulse. The authors describe a newly-developed diagnostic tool that provides the first direct test of this hypothesis. Time-resolved vacuum-ultraviolet absorption spectroscopy is used to directly probe fast neutral atoms with 1 mm spatial resolution in the 10 mm anode-cathode gap of the SABRE 5 MV, 1 TW applied-B ion diode. Absorption spectra collected during Ar RF glow discharges and with CO{sub 2} gas fills confirm the reliability of the diagnostic technique. Throughout the 50--100 ns ion diode pulses no measurable neutral absorption is seen, setting upper limits of 0.12--1.5 x 10{sup 14} cm{sup {minus}3} for ground state fast neutral atom densities of H, C, N, O, F. The absence of molecular absorption bands also sets upper limits of 0.16--1.2 x 10{sup 15} cm{sup {minus}3} for common simple molecules. These limits are low enough to rule out ionization throughout the gap as a breakdown mechanism. This technique can now be applied to quantify the role of neutral atoms in other high-power devices.

  5. Identifying Student and Teacher Difficulties in Interpreting Atomic Spectra Using a Quantum Model of Emission and Absorption of Radiation

    ERIC Educational Resources Information Center

    Savall-Alemany, Francisco; Domènech-Blanco, Josep Lluís; Guisasola, Jenaro; Martínez-Torregrosa, Joaquín

    2016-01-01

    Our study sets out to identify the difficulties that high school students, teachers, and university students encounter when trying to explain atomic spectra. To do so, we identify the key concepts that any quantum model for the emission and absorption of electromagnetic radiation must include to account for the gas spectra and we then design two…

  6. Manganese dioxide causes spurious gold values in flame atomic-absorption readings from HBr-Br2 digestions

    USGS Publications Warehouse

    Campbell, W.L.

    1981-01-01

    False readings, apparently caused by the presence of high concentrations of manganese dioxide, have been observed in our current flame atomic-absorption procedure for the determination of gold. After a hydrobromic acid (HBr)-bromine (Br2) leach, simply heating the sample to boiling to remove excess Br2 prior to extraction with methyl-isobutyl-ketone (MIBK) eliminates these false readings. ?? 1981.

  7. Assessing the Engagement, Learning, and Overall Experience of Students Operating an Atomic Absorption Spectrophotometer with Remote Access Technology

    ERIC Educational Resources Information Center

    Erasmus, Daniel J.; Brewer, Sharon E.; Cinel, Bruno

    2015-01-01

    The use of internet-based technologies in the teaching of laboratories has emerged as a promising education tool. This study evaluated the effectiveness of using remote access technology to operate an atomic absorption spectrophotometer in analyzing the iron content in a crude myoglobin extract. Sixty-two students were surveyed on their level of…

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  9. Atomic Absorption Spectrometry Analysis of Trace Elements in Degenerated Intervertebral Disc Tissue

    PubMed Central

    Kubaszewski, Łukasz; Zioła-Frankowska, Anetta; Frankowski, Marcin; Nowakowski, Andrzej; Czabak-Garbacz, Róża; Kaczmarczyk, Jacek; Gasik, Robert

    2014-01-01

    Background Few studies have investigated trace elements (TE) in human intervertebral disc (IVD) tissue. Trace element presence can have diverse meanings: essential TE show the metabolic modalities of the tissue, while environmentally-related TE indicate pollution and tissue-specific absorption and accumulation. IVD is a highly specific compartment with impaired communication with adjacent bone. Analysis of TE in IVD provides new insights regarding tissue metabolism and IVD communication with other tissues. Material/Methods Thirty intervertebral discs were acquired from 22 patients during surgical treatment for degenerative disease. Atomic absorption spectrometry was used to evaluate the concentrations of Al, Cd, Pb, Cu, Ni, Mo, Mg, and Zn. Results Al, Pb, Cu, Mg, and Zn were detected in all samples. Pb was significantly positively correlated with age, and Ni concentration was weakly correlated with population count in the patient’s place of residence. Only Cu was observed in higher concentrations in IVD compared to in other tissues. Significant positive correlations were observed between the following pairs: Mg/Zn, Mg/Al, Mg/Pb, Zn/Al, Zn/Pb, and Al/Pb. Negative correlations were observed between Mg/Cd, Zn/Cd, Mg/Mo, and Mo/Pb. Conclusions This study is one of few to profile the elements in intervertebral discs in patients with degenerative changes. We report significant differences between trace element concentrations in intervertebral discs compared to in other tissues. Knowledge of the TE accumulation pattern is vital for better understanding intervertebral disc nutrition and metabolism. PMID:25366266

  10. [Determination of nine mineral elements in hulless barley by ultraviolet spectrophotometry and flame atomic absorption spectrometry].

    PubMed

    Liu, Jin; Zhang, Huai-Gang

    2010-04-01

    The contents of nine mineral elements, including sulphur, zinc, calcium, magnesium, potassium, sodium, iron, copper and manganese in five hulless barley (Hordeum vulgare L. var. nudum Hook. f.) lines were determined by ultraviolet spectrophotometry and flames atomic absorption spectrometry (FAAS). For the determination of sulphur, the samples were dissolved by magnesia and anhydrous sodium carbonate at 250 degrees C for 0. 5 h and at 550 degrees C for 3 h in the muffle furnace, and then a certain amount of barium chloride was put into the sample solution for colorimetry of the UV-Vs spectrophotometer. For the determination of other eight mineral elements, all of the samples were dissolved by a kind of incinerating method: first, the sample was put into the muffle furnace at 250 degrees C for 0. 5 h and at 550 degrees C for 2.5 h, then two droplets of 50%HNO3 were distributed into each sample, and the last step was putting the sample into the muffle furnace at 550 degrees C for 0.5 h. And then all of the ash was dissolved by 50%HNO3 to 50 milliliter and determined by flames atomic absorption spectrometry. The precision, accuracy, repeatability and stability of the method were discussed too. The results showed that the relative standard deviations (RSD) were between 1.2% and 3.7%; The average recoveries were 97.44%-101.52% and the relative standard deviations (RSD) of sample determination were 1.3%-3.8%. The repeatability experiment showed that the relative standard deviations (RSD) were 2.6%-6.1%. And the content of each mineral element was the same after 24 hours; All these showed that the method has a good precision, accuracy, repeatability and stability. In all the hulless barley samples, the average contents were in the order of K > S > Mg > Ca > Fe > Na > Zn > Mn > Cu, and the contents of zinc, iron and manganese closely related to people's health were relatively higher than other crops. The data of the experiment could provide an accurate and credible evidence

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

    NASA Astrophysics Data System (ADS)

    de Jesus, Alexandre; Zmozinski, Ariane Vanessa; Damin, Isabel Cristina Ferreira; Silva, Márcia Messias; Vale, Maria Goreti Rodrigues

    2012-05-01

    In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 μg kg- 1 for arsenic and 0.2 μg kg- 1 for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a "cold finger" was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis.

  12. Mapping atomic and diffuse interstellar band absorption across the Magellanic Clouds and the Milky Way

    NASA Astrophysics Data System (ADS)

    Bailey, Mandy; van Loon, Jacco Th.; Sarre, Peter J.; Beckman, John E.

    2015-12-01

    Diffuse interstellar bands (DIBs) trace warm neutral and weakly ionized diffuse interstellar medium (ISM). Here we present a dedicated, high signal-to-noise spectroscopic survey of two of the strongest DIBs, at 5780 and 5797 Å, in optical spectra of 666 early-type stars in the Small and Large Magellanic Clouds, along with measurements of the atomic Na I D and Ca II K lines. The resulting maps show for the first time the distribution of DIB carriers across large swathes of galaxies, as well as the foreground Milky Way ISM. We confirm the association of the 5797 Å DIB with neutral gas, and the 5780 Å DIB with more translucent gas, generally tracing the star-forming regions within the Magellanic Clouds. Likewise, the Na I D line traces the denser ISM whereas the Ca II K line traces the more diffuse, warmer gas. The Ca II K line has an additional component at ˜200-220 km s-1 seen towards both Magellanic Clouds; this may be associated with a pan-Magellanic halo. Both the atomic lines and DIBs show sub-pc-scale structure in the Galactic foreground absorption; the 5780 and 5797 Å DIBs show very little correlation on these small scales, as do the Ca II K and Na I D lines. This suggests that good correlations between the 5780 and 5797 Å DIBs, or between Ca II K and Na I D, arise from the superposition of multiple interstellar structures. Similarity in behaviour between DIBs and Na I in the Small Magellanic Cloud (SMC), Large Magellanic Cloud (LMC) and Milky Way suggests the abundance of DIB carriers scales in proportion to metallicity.

  13. Hydrogen atom temperature measured with wavelength-modulated laser absorption spectroscopy in large scale filament arc negative hydrogen ion source

    SciTech Connect

    Nakano, H. Goto, M.; Tsumori, K.; Kisaki, M.; Ikeda, K.; Nagaoka, K.; Osakabe, M.; Takeiri, Y.; Kaneko, O.; Nishiyama, S.; Sasaki, K.

    2015-04-08

    The velocity distribution function of hydrogen atoms is one of the useful parameters to understand particle dynamics from negative hydrogen production to extraction in a negative hydrogen ion source. Hydrogen atom temperature is one of the indicators of the velocity distribution function. To find a feasibility of hydrogen atom temperature measurement in large scale filament arc negative hydrogen ion source for fusion, a model calculation of wavelength-modulated laser absorption spectroscopy of the hydrogen Balmer alpha line was performed. By utilizing a wide range tunable diode laser, we successfully obtained the hydrogen atom temperature of ∼3000 K in the vicinity of the plasma grid electrode. The hydrogen atom temperature increases as well as the arc power, and becomes constant after decreasing with the filling of hydrogen gas pressure.

  14. Germanium determination by flame atomic absorption spectrometry: an increased vapor pressure-chloride generation system.

    PubMed

    Kaya, Murat; Volkan, Mürvet

    2011-03-15

    A new chloride generation system was designed for the direct, sensitive, rapid and accurate determination of the total germanium in complex matrices. It was aimed to improve the detection limit of chloride generation technique by increasing the vapor pressure of germanium tetrachloride (GeCl(4)). In order to do so, a novel joint vapor production and gas-liquid separation unit equipped with a home-made oven was incorporated to an ordinary nitrous oxide-acetylene flame atomic absorption spectrometer. Several variables such as reaction time, temperature and acid concentration have been investigated. The linear range for germanium determination was 0.1-10 ng mL(-1) for 1 mL sampling volume with a detection limit (3s) of 0.01 ng mL(-1). The relative standard deviation (RSD) was 2.4% for nine replicates of a 1 ng mL(-1) germanium solution. The method was validated by the analysis of one non-certified and two certified geochemical reference materials, respectively, CRM GSJ-JR-2 (Rhyolite), and GSJ-JR-1 (Rhyolite), and GBW 07107 (Chinese Rock). Selectivity of the method was investigated for Cd(2+), Co(2+), Cu(2+), Fe(3+), Ga(3+), Hg(2+), Ni(2+), Pb(2+), Sn(2+), and Zn(2+) ions and ionic species of As(III), Sb(III), Te(IV), and Se(IV). PMID:21315908

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

    USGS Publications Warehouse

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

    1990-01-01

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

  16. Determination of arsenic in a nickel alloy by flow injection hydride generation atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hanna, C. P.; Tyson, J. F.; Offley, S. G.

    1992-08-01

    The development of a method for the direct determination of trace arsenic quantities in nickel alloy digests, by flow injection hydride generation atomic absorption spectrometry, is described. An optimization study of the manifold and chemical parameters produced system performance, in terms of tolerance of the nickel matrix and sensitivity, such that matrix removal and pre-reduction of As(V) to As (III) prior to arsine generation were eliminated. Full recovery of the As(V) signal from a solution containing 5 ng ml -1 in the presence of 60 μg ml -1 nickel was obtained. Validation of the method was achieved by analyzing a British Chemical Standard (BCS) Certified Reference Material (CRM) #346 IN nickel alloy containing arsenic at a concentration of 50 μg g -1. Following dissolution in nitric and hydrofluoric acids by a microwave assisted procedure, the only subsequent preparation required was dilution by the appropriate factor. Up to 60 injections h -1 may be made, with a detection limit of 0.5 ng ml -1 arsenic (250 pg absolute) as As(V) in a 500 μl sample. The peak height characteristic concentration is 0.46 ng ml -1, with a relative standard deviation of 3.5% for a 10 ng ml -1 As(V) standard ( n = 6).

  17. Cadmium accumulation in the crayfish, Procambarus clarkii, using graphite furnace atomic absorption spectroscopy

    SciTech Connect

    Diaz-Mayans, J.; Hernandez, F.; Medina, J.; Del Ramo, J.; Torreblanca, A.

    1986-11-01

    Lake Albufera and the surrounding rice-field waters are being subject to very heavy loads of sewage and toxic industrial residues (including heavy metals and pesticides) from the many urban and wastewaters in this area. The American red crayfish Procambarus clarkii is native to the Louisiana marshes (USA). In 1978, the crayfish appeared in Lake Albufera near Valencia (Spain), and presently, without adequate sanitary controls, the crayfish is being fished commercially for human consumption. In view of this interest, it is important to have accurate information on concentrations of cadmium in natural waters and cadmium levels of tissues of freshwaters animals used as human food, as well as the accumulation rates of this metal in this animal. In the present study, the authors investigated the accumulation of cadmium in several tissues of the red crayfish, P clarkii (Girard) from Lake Albufera following cadmium exposure. Determinations of cadmium were made by flameless atomic absorption spectroscopy and the standard additions method. Digestion of samples was made by wet ashing in open flasks with concentrated HNO/sub 3/ at 80-90/sup 0/C.

  18. Analysis of the Release Characteristics of Cu-Treated Antimicrobial Implant Surfaces Using Atomic Absorption Spectrometry

    PubMed Central

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

    2012-01-01

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

  19. Slurry sampling for hydride generation atomic absorption spectrometric determination of arsenic in cigarette tobaccos.

    PubMed

    Mierzwa, J; Adeloju, S B; Dhindsa, H S

    1997-06-01

    The development of a slurry sampling hydride generation atomic absorption spectrometric (HGAAS) method for the determination of arsenic in cigarette tobacco samples is described. The method is relatively simple and has been shown to give values of total arsenic close to those obtained using methods requiring total dissolution and decomposition of all vegetable matter before analysis. Pre-treatment of samples slurried in nitric acid by ultrasonication permitted the extraction of about 90% of the total arsenic from tobacco samples. Further improvement in the recovery efficiency (up to 93-94%) was accomplished by the use of an additional step of short microwave-accelerated treatment. L-Cysteine was used as a pre-reduction agent. The accuracy and precision of the slurry sampling HGAAS method were studied using the certified reference material (CRM) CTA-OTL-1 Oriental Tobacco Leaves. Under the optimum conditions, as little as 2.6 ng of arsenic can be detected. The relative standard deviation of the overall procedure was calculated to be below 7.6% at arsenic concentration levels of 0.5-0.9 mg kg-1 and the analytical results obtained for the CRM agreed with the certified value. The main factors that influenced the reliability of the method were sample homogeneity, particle size and slurry concentration. PMID:9282401

  20. Speciation of methylmercury in market seafood by thermal degradation, amalgamation and atomic absorption spectroscopy.

    PubMed

    Ruiz-de-Cenzano, Manuela; Rochina-Marco, Arancha; Cervera, M Luisa; de la Guardia, Miguel

    2014-09-01

    Sample thermal decomposition followed by mercury amalgamation and atomic absorption has been employed for the determination of methylmercury (MeHg) in fish. The method involves HBr leaching of MeHg, extraction into toluene, and back-extraction into an aqueous l-cysteine solution. Preliminary studies were focused on the extraction efficiency, losses, contaminations, and species interconversion prevention. The limit of detection was 0.018µgg(-1) (dry weight). The intraday precision for three replicate analysis at a concentration of 4.2µgg(-1) (dry weight) was 3.5 percent, similar to the interday precision according to analysis of variance (ANOVA). The accuracy was guaranteed by the use of fortified samples involving 83-105 percent recoveries, and certified reference materials TORT-2 (lobster hepatopancreas) and DORM-3 (dogfish liver), providing 107 and 98 percent recovery of certified values. The greenness of the method was also evaluated with the analytical eco-scale being obtained a final score of 73 points which means an acceptable green analysis. The method was applied to fifty-seven market samples of different fish acquired from local markets in several sampling campaigns. The content of MeHg found varied between 0.0311 and 1.24µgg(-1) (wet weight), with values that involve 33-129 percent of the total mercury content. Some considerations about food safety were also done taking into account data about Spanish fish consume and Tolerable Weekly Intake (TWI) established for MeHg. PMID:24927385

  1. Acid effects on the measurement of mercury by cold vapor atomic absorption spectrometry

    SciTech Connect

    Adeloju, S.B.; Mann, T.F.

    1987-07-01

    The influence of nitric, hydrochloric and sulfuric acids on the measurement of mercury by cold vapor atomic absorption spectrometry has been investigated. Small pre-reduction peaks associated with the instability of mercury were observed in solutions containing less than or equal to 12.5, < 2 and less than or equal to 12.5% v/v of each acid, respectively. Mercury was found to be most stable in greater than or equal to 2% v/v hydrochloric acid and the measured absorbance was not greatly influenced by varying concentration of the acid. The mercury absorbance measurements were more sensitive in solutions containing less than or equal to 6.3% v/v hydrochloric acid than in similar concentrations of nitric and sulfuric acids. The use of the three acids as a digestion mixture result in serious interference from nitrogen oxides. The interference was removed by use of expelling agents such as urea and sulfamic acid or overcome by use of excess stannous chloride, prior to the reduction of mercury(II) ions. The determination of mercury in NBS albacore tuna using both of these approaches to overcome the interference problem proved to be successful.

  2. Determination of gold in geological materials by carbon slurry sampling graphite furnace atomic absorption spectrometry.

    PubMed

    Dobrowolski, Ryszard; Kuryło, Michał; Otto, Magdalena; Mróz, Agnieszka

    2012-09-15

    A simple and cost effective preconcentration method on modified activated carbons is described for the determination of traces of gold (Au) in geological samples by carbon slurry sampling graphite furnace atomic absorption spectrometry (GFAAS). The basic parameters affecting the adsorption capacity of Au(III) ions on modified activated carbons were studied in detail and the effect of activated carbons modification has been determined by studying the initial runs of adsorption isotherms. The influence of chlorides and nitrates on adsorption ability of Au(III) ions onto the modified activated carbons for diluted aqueous solution was also studied in detail in respect to the determination of gold in solid materials after digestion steps in the analytical procedure, which usually involves the application of aqua regia. SEM-EDX and XPS studies confirmed that the surface reduction of Au(III) ions to Au(0) is the main gold adsorption mechanism on the activated carbon. Determination of gold after its preconcentration on the modified activated carbon was validated by applying certified reference materials. The experimental results are in good agreement with the certified values. The proposed method has been successfully applied for the determination of Au in real samples using aqueous standards. PMID:22967620

  3. Determination of cobalt in samples containing cobalt and tungsten carbide by electrothermal atomic absorption spectrometry

    SciTech Connect

    Firriolo, J.M.; Kutzman, R.S.

    1985-09-01

    A method has been developed to determine the amount of cobalt (Co) in atmospheric dust samples which include free and sintered Co. Cobalt and tungsten carbide (WC) mixtures ranging from 0-100% Co were prepared for atomic absorption analysis by dissolving the Co in aqua regia. Using this method, the amount of Co in the samples assayed ranged from 90.9-100.1% of that gravimetrically added to the mixtures. The results of this aqua regia dissolution procedure for Co were compared to a hydrofluoric acid method which solubilized both the Co and the WC. Application of the aqua regia dissolution method to samples of sintered WC and Co dust resulted in complete recovery of the Co from these materials. These results were supported by x-ray analysis of the samples before and after dissolution of the Co with aqua regia. The described procedure is advantageous because it avoids the use of highly-caustic hydrofluoric acid and the results are quickly available.

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

    PubMed Central

    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef

    2012-01-01

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

  5. Atomic absorption spectrometric determination of copper, zinc, and lead in geological materials

    USGS Publications Warehouse

    Sanzolone, R.F.; Chao, T.T.

    1976-01-01

    An atomic absorption spectrometric method is described for the determination of copper, zinc, and lead in geological materials. The sample is digested with HF-HCl-H2O2; the final solution for analysis is in 10 % (v/v) HCl. Copper and zinc are determined directly by aspirating the solution into an air-acetylene flame. A separate aliquot of the solution is used for determination of lead; lead is extracted into TOPO-MIBK from the acidic solution in the presence of iodide and ascorbic acid. For a 0.50-g sample, the limits of determination are 10-2000 p.p.m. for Cu and Zn, and 5-5000 p.p.m. for Pb. As much as 40 % Fe or Ca. and 10 % Al, Mg, or Mn in the sample do not interfere. The proposed method can be applied to the determination of copper, zinc, and lead in a wide range of geological materials including iron- and manganese-rich, calcareous and carbonate samples. ?? 1976.

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

    PubMed

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

    2012-01-01

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

  7. Direct determination of Cd, Pb and Cr in honey by slurry sampling electrothermal atomic absorption spectrometry.

    PubMed

    de Andrade, Camila Kulek; dos Anjos, Vanessa Egéa; Felsner, Maria Lurdes; Torres, Yohandra Reyes; Quináia, Sueli Pércio

    2014-03-01

    Slurry sampling electrothermal atomic absorption spectrometry was used for direct determination of Cr, Pb and Cd in honey without sample pretreatment. The honey slurries were prepared in aqueous solution containing hydrogen peroxide and nitric acid. The slurries were directly introduced in the pyrolytic graphite tubes. Pd-Mg was used as a chemical modifier only for Cd determination. Analytical curves were performed with aqueous standards for Pb and Cr and with addition of fructose for Cd. The quantification limits for Cd, Pb and Cr were 2.0, 5.4 and 9.4ngg(-1), respectively. Acceptable precision of the methodology was obtained through repeatability and intermediate precision. In the accuracy study, recoveries were satisfactory (94-101%) for the three elements. The methodology was applied in honey from Paraná (Brazil). The concentrations of Pb, Cd and Cr ranged from 141 to 228ngg(-1), <2.0 to 8ngg(-1) and 83 to 94ngg(-1), respectively. PMID:24176328

  8. Stabilizing agents for calibration in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry.

    PubMed

    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef

    2012-01-01

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

  9. Determination of rhodium: Since the origins until today Atomic absorption spectrometry.

    PubMed

    Bosch Ojeda, C; Sánchez Rojas, F

    2006-02-28

    Rhodium is present at about 0.001ppm in the earths crust. Rhodium metal is known for its stability in corrosive environments, physical beauty and unique physical and chemical properties. Recent interest in the medical and industrial significance of platinum and to a lesser extent palladium and rhodium has been accompanied by an increasing interest in their determination at low levels. Platinum group elements (PGEs: Pt, Pd, Rh, Ru, Ir and Os) play a decisive role in the performance of catalytic converters, world-wide applied in vehicles and in some household utensils, to reduce the emission of gaseous pollutants, such as carbon monoxide, nitrogen oxides and hydrocarbons. Since then, approximately 73% of the world production of rhodium is consumed in the production of autocatalyst. However, the hot exhaust gases flowing through the converter cause abrasion of these units, leading to the emission of these elements to the environment. The concentration level of rhodium (also platinum and palladium) is still very low in the nature; accordingly, their determination in environmental samples specially appears to be a challenging task for analytical chemists. In recent years, the development of analytical methods for the determination of rhodium has increased. The aim of the present review is to evaluate the utility of atomic absorption spectrometry, applied for the quantification of rhodium in different materials, such as environmental, biological, metallurgical and geological samples. PMID:18970480

  10. Atomic Structure of Pt3Ni Nanoframe Electrocatalysts by in Situ X-ray Absorption Spectroscopy.

    PubMed

    Becknell, Nigel; Kang, Yijin; Chen, Chen; Resasco, Joaquin; Kornienko, Nikolay; Guo, Jinghua; Markovic, Nenad M; Somorjai, Gabor A; Stamenkovic, Vojislav R; Yang, Peidong

    2015-12-23

    Understanding the atomic structure of a catalyst is crucial to exposing the source of its performance characteristics. It is highly unlikely that a catalyst remains the same under reaction conditions when compared to as-synthesized. Hence, the ideal experiment to study the catalyst structure should be performed in situ. Here, we use X-ray absorption spectroscopy (XAS) as an in situ technique to study Pt3Ni nanoframe particles which have been proven to be an excellent electrocatalyst for the oxygen reduction reaction (ORR). The surface characteristics of the nanoframes were probed through electrochemical hydrogen underpotential deposition and carbon monoxide electrooxidation, which showed that nanoframe surfaces with different structure exhibit varying levels of binding strength to adsorbate molecules. It is well-known that Pt-skin formation on Pt-Ni catalysts will enhance ORR activity by weakening the binding energy between the surface and adsorbates. Ex situ and in situ XAS results reveal that nanoframes which bind adsorbates more strongly have a rougher Pt surface caused by insufficient segregation of Pt to the surface and consequent Ni dissolution. In contrast, nanoframes which exhibit extremely high ORR activity simultaneously demonstrate more significant segregation of Pt over Ni-rich subsurface layers, allowing better formation of the critical Pt-skin. This work demonstrates that the high ORR activity of the Pt3Ni hollow nanoframes depends on successful formation of the Pt-skin surface structure. PMID:26652294

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

    PubMed

    Gokce, Kaya; Mehmet, Yaman

    2012-01-01

    Eleven plant species were collected from the vicinity of lead-battery plant in the city of Gaziantep, Turkey. Lead, cadmium and copper concentrations in the soil and leaves of plants were determined by atomic absorption spectrometry. Lead, Cd and Cu concentrations in the soil samples taken from battery area were found to be in the ranges of 304-602, 0.4-0.44 and 31-37 mg x kg(-1), respectively. Significantly increased lead concentration up to 2 750 mg x kg(-1) was found in the leaves of Eleagnus angustifolia L. plant. The lead concentrations in the other plant leaves taken from 50 m around battery factory followed the order Ailanthus altissima > Morus sp. > Juglans regia L. > Ficus carica L. > Cydonia oblonga Miller > Prunus x domestica L. The plants, Populus nigra L. , Eleagnus angustifolia L. and Salix sp. were found useful for Cd, and the plant, Eleagnus angusti folia L. for Pb, to be considered as potential biomonitor. Especially, leaves of trees and plants taken from the distance of 50 m from battery plant have relatively higher Pb concentrations. Therefore, people who and animals which live in this area and benefit from these soil and plants have vital risks. PMID:22497165

  12. Detection of Glucose with Atomic Absorption Spectroscopy by Using Oligonucleotide Functionalized Gold Nanoparticle.

    PubMed

    Zhang, Hong; Yan, Honglian; Ling, Liansheng

    2016-06-01

    A novel method for the detection of glucose was established with atomic absorption spectroscopy by using the label of gold nanoparticle (AuNP). Silver-coated glass assembled with oligonucleotide 5'-SH-T12-AGA CAA GAG AGG-3' (Oligo 1) was acted as separation probe, oligonucleotide 5'-CAA CAG AGA ACG-T12-SH-3' modified gold nanoparticle (AuNP-Oligo 2) was acted as signal-reporting probe. Oligonucleotide 5'-CGT TCT CTG TTG CCT CTC TTG TCT-3' (Oligo 3) could hybridize with Oligo 1 on the surface of silver-coated glass and AuNP-Oligo 2, and free AuNP-Oligo 2 could be removed by rinsing with buffer. Hence the concentration of Oligo 3 was transformed into the concentration of gold element. In addition, Oligo 3 could be cleaved into DNA fragments by glucose, glucose oxidase and Fe(2+)-EDTA through Fenton reaction. Thereby the concentration of glucose could be transformed to the absorbance of gold element. Under the optimum conditions, the integrated absorbance decreased proportionally to the concentration of glucose over the range from 50.0 μM to 1.0 mM with a detection limit of 40.0 μM. Moreover, satisfactory result was obtained when the assay was used to determinate glucose in human serum. PMID:27427698

  13. Evaluation of metal contents of household detergent samples from Turkey by flame atomic absorption spectrometry.

    PubMed

    Soylak, Mustafa; Unsal, Yunus Emre; Tuzen, Mustafa

    2013-11-01

    The concentrations of cadmium, copper, chromium, cobalt, iron, lead, manganese, nickel, and zinc in detergent samples from Kayseri, Turkey were determined by flame atomic absorption spectrometry. HClO₄ (10 mL)/HNO₃ (10 mL) mixture was used for the digestion of household detergent samples. The correctness of the analytical procedures was checked with standard addition-recovery tests in different detergent samples for the investigated metal ions. The concentration ranges of the elements in the detergent samples were found as 17.2-60.1, 11.1-40.1, 2.5-32.3, 8.1-10.5, 7.2-21.6, 9.8-17.9, 1.7-3.8, 12.5-22.5, and 2.0-5.8 μg/g for iron, manganese, zinc, copper, lead, cobalt, cadmium, nickel, and chromium, respectively. The values found in this work were compared with some other studies around the world conducted on detergent samples. PMID:23722641

  14. Stability of low concentration calibration standards for graphite furnace atomic absorption spectrophotometry

    SciTech Connect

    Bass, D A; TenKate, L B

    1993-11-01

    Graphite furnace atomic absorption spectrophotometry (GFAAS) is used for determination of ultra-trace metals in environmentally important samples. In the generation of GFAAS calibration curves for many environmental applications, low concentration calibration standards must be prepared dally, as required by the Statement of Work (SOW) for the US Environmental Protection Agency (EPA) Contract Laboratory Program (CLP). This results in significant time and work for the analyst and significant cost to the Analytical Chemistry Laboratory (ACL) for chemicals and waste management. While EPA SW 846 is less prescriptive than the CLP SOW, ACL has been following the CLP guidelines because in-house criteria regarding the stability of GFAAS standards have not been established. A study was conducted to determine the stability of GFAAS standards for analytes commonly used in the ACL (single and mixed) as a function of time. Data were collected over nine months. The results show that GFAAS standards for Sb, Pb, Se, Ag, and TI are stable for a longer period of time than currently assumed by the CLP SOW. Reducing the frequency of preparing these standards will increase efficiency, decrease the handling of hazardous the quantity of hazardous waste generated, and decrease the quantity of hazardous substances to be ordered and stocked by the laboratory. These benefits will improve GFAAS analysis quality, reduce costs, enhance safety, and lower environmental concerns.

  15. Determination of chromium and molybdenum in medical foods by graphite furnace atomic absorption spectrophotometry.

    PubMed

    Phifer, E C

    1995-01-01

    Graphite furnace atomic absorption spectrophotometry was used to determine chromium and molybdenum in 7 medical foods from 5 manufacturers. Linear standard curves were obtained for both elements for concentrations between 5 and 25 ng/mL. Detection limits were 0.24 ng/mL for Cr and 0.67 ng/mL for Mo. Characteristic masses were 3.1 and 14.7 pg for Cr and Mo, respectively. No difference was detected between wet and dry ashing methods, and dry ashing was used to complete the study. The method was validated by assaying various National Institute of Standards and Technology standard reference materials. Analysis of these products for Cr and Mo were within certified values. One product was evaluated by this method for reproducibility (n = 5). Relative standard deviations were 6.8 and 4.8% for Cr and Mo, respectively. This product contained 0.31 +/= 0.02 micrograms Cr/g and 0.63 +/- 0.03 micrograms Mo/g. The remaining products contained 0.09-1.28 micrograms Cr/g and 0.07-2.3 micrograms Mo/g. Mean recovery values were 98 +/- 14% (n = 14) for Cr at spike levels of 0.20-1.89 micrograms/g and 102 +/- 24% (n = 10) for Mo at spike levels of 0.30-1.89 micrograms/g. PMID:8664588

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

    PubMed

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

    2010-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

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

  18. Selective determination of antimony(III) and antimony(V) with ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and dithizone by atomic-absorption spectrometry with a carbon-tube atomizer.

    PubMed

    Kamada, T; Yamamoto, Y

    1977-05-01

    The extraction behaviour of antimony(III) and antimony(V) with ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and dithizone in organic solvents has been investigated by means of frameless atomic-absorption spectrophotometry with a carbon-tube atomizer. The selective extraction of antimony(III) and differential determination of antimony(III) and antimony(V) have been developed. With ammonium pyrrolidinedithiocarbamate and methyl isobutyl ketone, when the aqueous phase/solvent volume ratio is 50 ml/10 ml and the injection volume in the carbon tube is 20 mul, the sensitivity for antimony is 0.2 ng/ml for 1% absorption. The relative standard deviations are ca. 2%. Interferences by many metal ions can be prevented by masking with EDTA. The proposed methods have been applied satisfactorily to determination of antimony(III) and antimony(V) in various types of water. PMID:18962096

  19. Attosecond transient absorption of argon atoms in the vacuum ultraviolet region: line energy shifts versus coherent population transfer

    NASA Astrophysics Data System (ADS)

    Cao, Wei; Warrick, Erika R.; Neumark, Daniel M.; Leone, Stephen R.

    2016-01-01

    Using attosecond transient absorption, the dipole response of an argon atom in the vacuum ultraviolet (VUV) region is studied when an external electromagnetic field is present. An isolated attosecond VUV pulse populates Rydberg states lying 15 eV above the argon ground state. A synchronized few-cycle near infrared (NIR) pulse modifies the oscillating dipoles of argon impulsively, leading to alterations in the VUV absorption spectra. As the NIR pulse is delayed with respect to the VUV pulse, multiple features in the absorption profile emerge simultaneously including line broadening, sideband structure, sub-cycle fast modulations, and 5-10 fs slow modulations. These features indicate the coexistence of two general processes of the light-matter interaction: the energy shift of individual atomic levels and coherent population transfer between atomic eigenstates, revealing coherent superpositions. An intuitive formula is derived to treat both effects in a unifying framework, allowing one to identify and quantify the two processes in a single absorption spectrogram.

  20. Two-photon absorption laser induced fluorescence measurement of atomic oxygen density in an atmospheric pressure air plasma jet

    NASA Astrophysics Data System (ADS)

    Conway, J.; Gogna, G. S.; Gaman, C.; Turner, M. M.; Daniels, S.

    2016-08-01

    Atomic oxygen number density [O] is measured in an air atmospheric pressure plasma jet (APPJ) using two-photon absorption laser induced fluorescence (TALIF). Gas flow is fixed at 8 slpm, the RF power coupled into the plasma jet varied between 5 W and 20 W, and the resulting changes in atomic oxygen density measured. Photolysis of molecular oxygen is employed to allow in situ calibration of the TALIF system. During calibration, O2 photo-dissociation and two-photon excitation of the resulting oxygen atoms are achieved within the same laser pulse. The atomic oxygen density produced by photolysis is time varying and spatially non-uniform which needs to be corrected for to calibrate the TALIF system for measurement of atomic oxygen density in plasma. Knowledge of the laser pulse intensity I 0(t), wavelength, and focal spot size allows correction factors to be determined using a rate equation model. Atomic oxygen is used for calibration and measurement, so the laser intensity can be increased outside the TALIF quadratic laser power dependence region without affecting the calibration reliability as the laser power dependence will still be the same for both. The atomic O density results obtained are not directly benchmarked against other known density measurement techniques. The results show that the plasma jet atomic oxygen content increases as the RF power coupled into the plasma increases.

  1. Oxygen vacancy mediated enhanced photo-absorption from ZnO(0001) nanostructures fabricated by atom beam sputtering

    NASA Astrophysics Data System (ADS)

    Solanki, Vanaraj; Joshi, Shalik R.; Mishra, Indrani; Kabiraj, D.; Mishra, N. C.; Avasthi, D. K.; Varma, Shikha

    2016-08-01

    The nanoscale patterns created on the ZnO(0001) surfaces during atom beam irradiation have been investigated here for their photo absorption response. Preferential sputtering, during irradiation, promotes Zn-rich zones that serve as the nucleation centers for the spontaneous creation of nanostructures. Nanostructured surfaces with bigger (78 nm) nanodots, displaying hexagonal ordering and long ranged periodic behavior, show higher photo absorption and a ˜0.09 eV reduced bandgap. These nanostructures also demonstrate higher concentration of oxygen vacancies which are crucial for these results. The enhanced photo-response, as observed here, has been achieved in the absence of any dopant elements.

  2. Absolute number densities of helium metastable atoms determined by atomic absorption spectroscopy in helium plasma-based discharges used as ambient desorption/ionization sources for mass spectrometry

    NASA Astrophysics Data System (ADS)

    Reininger, Charlotte; Woodfield, Kellie; Keelor, Joel D.; Kaylor, Adam; Fernández, Facundo M.; Farnsworth, Paul B.

    2014-10-01

    The absolute number densities of helium atoms in the 2s 3S1 metastable state were determined in four plasma-based ambient desorption/ionization sources by atomic absorption spectroscopy. The plasmas included a high-frequency dielectric barrier discharge (HF-DBD), a low temperature plasma (LTP), and two atmospheric-pressure glow discharges, one with AC excitation and the other with DC excitation. Peak densities in the luminous plumes downstream from the discharge capillaries of the HF-DBD and the LTP were 1.39 × 1012 cm- 3 and 0.011 × 1012 cm- 3, respectively. Neither glow discharge produced a visible afterglow, and no metastable atoms were detected downstream from the capillary exits. However, densities of 0.58 × 1012 cm- 3 and 0.97 × 1012 cm- 3 were measured in the interelectrode regions of the AC and DC glow discharges, respectively. Time-resolved measurements of metastable atom densities revealed significant random variations in the timing of pulsed absorption signals with respect to the voltage waveforms applied to the discharges.

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

    NASA Astrophysics Data System (ADS)

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

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

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

    SciTech Connect

    Rey-Raap, Natalia

    2012-05-15

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

  5. Electrothermal atomic absorption spectrometric determination of selenium in foods and diets.

    PubMed

    Kumpulainen, J; Raittila, A M; Lehto, J; Koivistoinen, P

    1983-09-01

    The validity of 2 electrothermal atomic absorption spectrometric methods for determination of selenium in foods and diets was tested. By using 0.5% Ni(II) as a matrix modifier to prevent selenium losses during the ashing step, it was shown that selenium can be determined in samples containing greater than or equal to 1 microgram Se/g dry wt without organic extraction. The mean recovery tested, using NBS Bovine Liver, was 98%; recovery of added inorganic selenium in Bovine Liver matrix was 100%. In addition, this method gave values closest to the median value of all participating laboratories using hydride generation AAS or the spectrofluorometric method in a collaborative study on high selenium wheat, flour, and toast samples. For samples with concentrations less than 1 microgram Se/g dry wt, separation of selenium from interfering Fe and P ions by organic extraction was necessary. Using inorganic 75Se in meat and human milk matrixes, an ammonium pyrrolidine dithiocarbamate-methyl isobutyl ketone-extraction system with added Cu(II) as a matrix modifier yielded the best extraction recoveries, 97 and 98%, respectively. Accuracy and precision of the method were tested using several official and unofficial biological standard materials. The mean accuracy was within 4% of the certified or best values of the standard materials and the day-to-day variation was 9%. The Se/Fe or Se/P interference limits proved to be low enough not to affect selenium determinations in practically all foods or diets. The practical detection limit of the method was 3 ng Se/g dry wt for 1.0 g dry wt samples.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:6630125

  6. Determination of calcium, magnesium and strontium in soils by flow injection flame atomic absorption spectrometry.

    PubMed

    Arslan, Z; Tyson, J F

    1999-12-01

    Several procedures for the determination of Ca, Mg and Sr in soils have been compared on the basis of the accuracy of analysis of two NIST reference materials (Montana Soils SRM 2710 and SRM 2711). Samples were dissolved in a mixture of hydrofluoric and nitric acids in sealed vessels in a microwave oven and in teflon beakers on a hot plate. The digests obtained from both dissolution methods were evaporated to dryness in an attempt to remove silicon. Boric acid was added to prevent the precipitation of the lanthanum releasing agent (as lanthanum fluoride) and potassium was added as an ionization buffer. Determinations were made by flame atomic absorption spectrometry with both the nitrous oxide-acetylene flame and the air-acetylene flame, with calibration either by standard additions or against external standards matrix matched with respect to nitric acid, boric acid, lanthanum and potassium. The silicon remaining in the solution was also determined by external calibration. A single-line flow injection manifold was used to overcome any problems due to the presence of high dissolved solids. A volume of 300 mul was injected into a water carrier stream flowing at 8 ml min(-1). To determine Ca in the air-acetylene flame, it was necessary to remove silicon. Magnesium was determined in either flame without complete removal of the silicon, however, for the determination of Sr, it was necessary to remove the silicon and use the nitrous oxide-acetylene flame. The indicative value for Sr in SRM 2710 was too low: the value determined was 360+/-30 mug g(-1). PMID:18967785

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

    PubMed

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

    2016-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Berglund, M.; Baxter, D. C.

    1992-12-01

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

  9. Determination of mercury in phosphate fertilizers by cold vapor atomic absorption spectrometry.

    PubMed

    de Jesus, Robson M; Silva, Laiana O B; Castro, Jacira T; de Azevedo Neto, Andre D; de Jesus, Raildo M; Ferreira, Sergio L C

    2013-03-15

    In this paper, a method for the determination of mercury in phosphate fertilizers using slurry sampling and cold vapor atomic absorption spectrometry (CV QT AAS) is proposed. Because mercury (II) ions form strong complexes with phosphor compounds, the formation of metallic mercury vapor requires the presence of lanthanum chloride as a release agent. Thiourea increases the amount of mercury that is extracted from the solid sample to the liquid phase of the slurry. The method is established using two steps. First, the slurry is prepared using the sample, lanthanum chloride, hydrochloric acid solution and thiourea solution and is sonicated for 20 min. Afterward, mercury vapor is generated using an aliquot of the slurry in the presence of the hydrochloric acid solution and isoamylic alcohol with sodium tetrahydroborate solution as the reducing agent. The experimental conditions for slurry preparation were optimized using two-level full factorial design involving the factors: thiourea and lanthanum chloride concentrations and the duration of sonication. The method allows the determination of mercury by external calibration using aqueous standards with limits of detection and quantification of 2.4 and 8.2 μg kg(-1), respectively, and precision, expressed as relative standard deviation, of 6.36 and 5.81% for two phosphate fertilizer samples with mercury concentrations of 0.24 and 0.57 mg kg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of phosphate fertilizer that was provided by the National Institute of Standards & Technology (NIST). The method was applied to determine mercury in six commercial samples of phosphate fertilizers. The mercury content varied from 33.97 to 209.28 μg kg(-1). These samples were also analyzed employing inductively coupled plasma mass spectrometry (ICP-MS). The ICP-MS results were consistent with the results from our proposed method. PMID:23598130

  10. Determination of total tin in environmental biological and water samples by atomic absorption spectrometry with graphite furnace.

    PubMed

    Dogan, S; Haerdi, W

    1980-01-01

    Analysis of traces of tin using several analytical techniques (X-ray fluorescence, neutron activation, polarographic techniques and atomic absorption) have been tested. Parameters such as simplicity, rapidity, sensitivity and interferences are compared in order to choose the most useful method for practical purpose. Finally, flameless atomic absorption was chosen for the determination of total tin concentration in different natural samples. Digestion of biological samples (plant, plankton, fish, etc.) was achieved by using Lumatom (a trade organic chemical). Thus, the digested sample is directly injected into the graphite furnace. This digestion technique is suitable and rapid with a minimum of error (contamination and losses). For tin analysis in water samples, a preconcentration of tin is carried out by coprecipitation with 1, 10-phenanthroline and tetraphenyl boron. The precipitate is separated and dissolved in alcohol or in Lumatom. The sensitivity of this method is 0.1 ng absolute tin. PMID:7451013

  11. Matrix effects on the determination of manganese in geological materials by atomic-absorption spectrophotometry under different flame conditions

    USGS Publications Warehouse

    Sanzolone, R.F.; Chao, T.T.

    1978-01-01

    Suppression caused by five of the seven matrix elements studied (Si, Al, Fe, Ca and Mg) was observed in the atomic-absorption determination of manganese in geological materials, when synthetic solutions and the recommended oxidizing air-acetylene flame were used. The magnitude of the suppression effects depends on (1) the kind and concentration of the interfering elements, (2) the type of acid medium, and (3) the concentration of manganese to be determined. All interferences noted are removed or alleviated by using a reducing nitrous oxide-acetylene flame. The atomic-absorption method using this flame can be applied to the determination of total and extractable manganese in a wide range of geological materials without interferences. Analyses of six U.S. Geological Survey rock standards for manganese gave results in agreement with the reported values. ?? 1978.

  12. Chromium speciation by solid phase extraction on Dowex M 4195 chelating resin and determination by atomic absorption spectrometry.

    PubMed

    Saygi, Kadriye Ozlem; Tuzen, Mustafa; Soylak, Mustafa; Elci, Latif

    2008-05-30

    A solid phase extraction procedure has been established for chromium speciation in natural water samples prior to determination by atomic absorption spectrometry. The procedure is based on the solid phase extraction of the Cr(VI)- Dowex M 4195 chelating resin. After oxidation of Cr(III) to Cr(VI) by using H2O2, the presented method was applied to the determination of the total chromium. The level of Cr(III) is calculated by difference of total chromium and Cr(VI) levels. The procedure was optimized for some analytical parameters including pH, eluent type, flow rates of sample and eluent, matrix effects, etc. The presented method was applied for the speciation of chromium in natural water samples with satisfactory results (recoveries >95%, RSDs <10%). In the determinations of chromium species, flame atomic absorption spectrometer was used. The results were checked by using NIST SRM 2711 Montana soil and GBW 07603 Bush branched and leaves. PMID:17951001

  13. Identifying student and teacher difficulties in interpreting atomic spectra using a quantum model of emission and absorption of radiation

    NASA Astrophysics Data System (ADS)

    Savall-Alemany, Francisco; Domènech-Blanco, Josep Lluís; Guisasola, Jenaro; Martínez-Torregrosa, Joaquín

    2016-06-01

    Our study sets out to identify the difficulties that high school students, teachers, and university students encounter when trying to explain atomic spectra. To do so, we identify the key concepts that any quantum model for the emission and absorption of electromagnetic radiation must include to account for the gas spectra and we then design two questionnaires, one for teachers and the other for students. By analyzing the responses, we conclude that (i) teachers lack a quantum model for the emission and absorption of electromagnetic radiation capable of explaining the spectra, (ii) teachers and students share the same difficulties, and (iii) these difficulties concern the model of the atom, the model of radiation, and the model of the interaction between them.

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

    NASA Astrophysics Data System (ADS)

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

    2007-03-01

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

  15. Fluorescence detection of white-beam X-ray absorption anisotropy: towards element-sensitive projections of local atomic structure

    PubMed Central

    Korecki, P.; Tolkiehn, M.; Dąbrowski, K. M.; Novikov, D. V.

    2011-01-01

    Projections of the atomic structure around Nb atoms in a LiNbO3 single crystal were obtained from a white-beam X-ray absorption anisotropy (XAA) pattern detected using Nb K fluorescence. This kind of anisotropy results from the interference of X-rays inside a sample and, owing to the short coherence length of a white beam, is visible only at small angles around interatomic directions. Consequently, the main features of the recorded XAA corresponded to distorted real-space projections of dense-packed atomic planes and atomic rows. A quantitative analysis of XAA was carried out using a wavelet transform and allowed well resolved projections of Nb atoms to be obtained up to distances of 10 Å. The signal of nearest O atoms was detected indirectly by a comparison with model calculations. The measurement of white-beam XAA using characteristic radiation indicates the possibility of obtaining element-sensitive projections of the local atomic structure in more complex samples. PMID:21997909

  16. Atom formation processes in the presence of ammonium thiocyanate in a thin-wall tungsten tube atomizer for atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Ohta, Kiyohisa; Mizuno, Takayuki

    Processes of atom formation of Ag, Al, As, Bi, Cd, Cr, Fe, Mn, Ni, Pb, Sb, Se, Sn, Sr and Te in the presence of ammonium thiocyanate in a thin-wall tungsten tube atomizer are described. It was found from a thermodynamic approach that AI, Bi, Cd, Cr, Fe, Ni and Te formed complexes with ammonium thiocyanate and are atomized through the sulfides in argon-hydrogen atmosphere. Atom formation processess for the other elements are different.

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

    PubMed

    Dessuy, Morgana B; Kratzer, Jan; Vale, Maria Goreti R; Welz, Bernhard; Dědina, Jiří

    2011-12-15

    Antimony is one of the constituents of pewter, an alloy composed of a minimum of 90% tin with the balance being made up with copper, antimony and perhaps some bismuth. A method has been developed to determine Sb in acetic acid leachates from pewter cups. The employed instrumentation, an atomic absorption spectrometer, equipped with a quartz trap-and-atomizer device, is simple and relatively inexpensive with low running costs. Interferences due to the presence of tin and ways to control them were investigated in detail. The applied approach made possible to overcome potentially serious interference of Sn leached from the cup material (which was shown to take place in the atomizer), by a combination of (i) high concentration of HCl, which decreases the efficiency of stannane generation and (ii) in-atomizer collection. The resulting Sn tolerance limit was between 10 and 20 mg L(-1). The advantages of the in-atomizer collection are a lower tin interference in the atomizer, and a much better limit of detection (LOD), which makes possible reducing the atomization interference further by working with more diluted sample solutions. Besides the Sn interference, an interference of an unknown volatile compound transported to the atomizer together with stibine was identified in the measured sample solutions. This interference could be controlled using the analyte addition technique. The applicability of the method was tested on solutions containing a wide range of interferents leached from the pewter cups, obtained at leaching times between 1 and 24h. The LOD in the sample solutions was found to be 0.03 μg L(-1) Sb. PMID:22099676

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

    USGS Publications Warehouse

    Meier, A.L.

    1982-01-01

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

  19. Attosecond XUV absorption spectroscopy of doubly excited states in helium atoms dressed by a time-delayed femtosecond infrared laser

    NASA Astrophysics Data System (ADS)

    Yang, Z. Q.; Ye, D. F.; Ding, Thomas; Pfeifer, Thomas; Fu, L. B.

    2015-01-01

    In the present paper, we investigate the time-resolved transient absorption spectroscopy of doubly excited states of helium atoms by solving the time-dependent two-electron Schrödinger equation numerically based on a one-dimensional model. The helium atoms are subjected to an extreme ultraviolet (XUV) attosecond pulse and a time-delayed infrared (IR) few-cycle laser pulse. A superposition of doubly excited states populated by the XUV pulse is identified, which interferes with the direct ionization pathway leading to Fano resonance profiles in the photoabsorption spectrum. In the presence of an IR laser, however, the Fano line profiles are strongly modified: A shifting, splitting, and broadening of the original absorption lines is observed when the XUV attosecond pulse and infrared few-cycle laser pulse overlap in time, which is in good agreement with recent experimental results. At certain time delays, we observe symmetric Lorentz, inverted Fano profiles, and even negative absorption cross sections indicating that the XUV light can be amplified during the interaction with atoms. We further prove that the above pictures are general for different doubly excited states by suitably varying the frequency of the IR field to coherently couple the corresponding states.

  20. On-line ion-exchange preconcentration and determination of traces of platinum by electrothermal atomic absorption spectrometry.

    PubMed

    González García, M M; Sánchez Rojas, F; Bosch Ojeda, C; García de Torres, A; Cano Pavón, J M

    2003-04-01

    A method to determine trace amounts of platinum in different samples based on electrothermal atomic absorption spectrometry is described. The preconcentration step is performed on a chelating resin microcolumn [1,5-bis(2-pyridyl)-3-sulfophenyl methylene thiocarbonohydrazide (PSTH) immobilized on an anion-exchange resin (Dowex 1x8-200)] placed in the autosampler arm. The combination of a peristaltic pump for sample loading and the atomic absorption spectrometer pumps for elution through a selection valve simplifies the hardware. The peristaltic pump and the selection valve are easily controlled electronically with two switches placed in the autosampler, which are activated when the autosampler arm is down. Thus, the process is fully automated without any modification of the software of the atomic absorption spectrometer. Under the optimum conditions with a 60-s preconcentration time, a sample flow rate of 2.4 mL min(-1), and an injection volume of eluent of 40 microL, a linear calibration graph was obtained in the range 0-100 ng mL(-1). The enrichment factor was 14. The detection limit under these conditions is 1 ng mL(-1), and the relative standard deviation (RSD) is 1.6% for 10 ng mL(-1) of Pt. The method has been applied to the determination of platinum in catalyst, vegetation, soil, and natural water samples. The results showed good agreement with the certified value and the recoveries of Pt added to samples were 98-105%. PMID:12733043

  1. Ultra-violet and resonant laser ablation coupled with microwave induced plasma atomic emission spectrometry and determination of tin in nickel based alloys by electrothermal atomizer atomic absorption and laser excited atomic fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Yang, Xiaodong

    Chapter 1 reviews laser ablation in analytical atomic spectrometry. Laser ablation is categorized into two functions: one is used as a sample introduction method, the other function is used as a microprobe analysis method. Both fundamental and applicational aspects are reviewed with the citations of related papers. This chapter also serves as an introduction to the work which is described in chapter 2 and chapter 3 as laser ablation is a relatively new research area for the research group. In chapter 2, instrumentation for excimer (308nm) laser ablation of samples was coupled with a microwave induced plasma (MLP), and evaluated for its potential as an approach to solid sampling for atomic emission spectrometry. Operating parameters were optimized, and the effects of laser repetition rate and number of laser shots on the emission signal were investigated. The UV excimer laser removed more material than would be expected of an infrared laser of similar energy. The chromium detection limit in the solid steel sample was estimated to be about 500 mug/g. In chapter 3, a wavelength tunable optical parametric oscillator (OPO) laser was used to ablate a steel sample into the same apparatus described in chapter 2. The emission signal for the elements was selectively enhanced when the ablation wavelength was tuned to be in resonance with any atomic transition of that element. This was the first report of the observation of resonant ablation by use of optical detection, as prior reports of resonant ablation have used mass spectrometric detectors. Chapter 4 reviews the publications in laser excited atomic fluorescence spectrometry in recent eight years. The focus of the review is on recent development on new instruments and applications of this technique. Chapter 5 studies the determination of tin in nickel-based alloys with laser excited atomic fluorescence in a graphite furnace. Zeeman electrothermal atomizer atomic absorption spectrometry and inductively coupled plasma mass

  2. A passive measurement of dissociated atom densities in atmospheric pressure air discharge plasmas using vacuum ultraviolet self-absorption spectroscopy

    SciTech Connect

    Laity, George; Fierro, Andrew; Dickens, James; Neuber, Andreas; Frank, Klaus

    2014-03-28

    We demonstrate a method for determining the dissociation degree of atmospheric pressure air discharges by measuring the self-absorption characteristics of vacuum ultraviolet radiation from O and N atoms in the plasma. The atom densities are determined by modeling the amount of radiation trapping present in the discharge, without the use of typical optical absorption diagnostic techniques which require external sources of probing radiation into the experiment. For an 8.0 mm spark discharge between needle electrodes at atmospheric pressure, typical peak O atom densities of 8.5 × 10{sup 17} cm{sup −3} and peak N atom densities of 9.9 × 10{sup 17} cm{sup −3} are observed within the first ∼1.0 mm of plasma near the anode tip by analyzing the OI and NI transitions in the 130.0–132.0 nm band of the vacuum ultraviolet spectrum.

  3. [Study on determination of eight metal elements in Hainan arecanut leaf by flame atomic absorption spectrophotometry].

    PubMed

    Liu, Li-yun; Wang, Ping; Feng, Mei-li; Dong, Zhi-guo; Li, Jie

    2008-12-01

    Arecanut is a sort of palm that is important economic crop for the farmers in Hainan province of China, wherein there are many kinds of metal elements such as K, Ca, Na, Mg, Fe, Mn, Cu, Zn etc. These elements are important nutrition for the growth of arecanut. It is very valuable to study on the content of these metal elements in arecanut leaf in terms of plant nutriology of arecanut. The arecanut leaf in Wangling county, Hainan province of China was sampled by diagonal-field-sampling method. Refering to other plant sample determination by FAAS, the detailed studies are done with different digestion and determination methods. In the present paper the effects of mixed acid of HNO3-HClO4 digestion method on determining the amount of metal elements in the arecanut leaf by FAAS is reported, and another one is incineration digestion method. FAAS method was established for the determination of K, Ca, Mg, Na, Fe, Mn, Cu and Zn The samples were incinerated or heated with HNO3-HClO4 (4:1). In the meantime, the optimum parameters of FAAS and effects of different digestion methods on the results were discussed. The recovery rate of standard addition is 98.36%-102.38% in the first method; RSD is 0.42%-2.328% (n=6); The recovery rate of standard addition is 99.22%-103.72% in the second method; RSD is 0.58%-1.283 (n=6). The metal amount determined by the first method is lower than the second method, the ratio is 0.9703-0.9934. The two methods are satisfied, but the latter is better. It is precise enough to common experiment to use flame atomic absorption spectrophotometry with digestion by incineration If the especially precise experiment is required, the digestion methods with mixed acid of HNO3-HClO4 may be introduced. The paper introduced methods dependable for determination of some metal elements in order to study on some nutrient effects of these metal elements in arecanut. PMID:19248529

  4. Determination of yttrium and rare-earth elements in rocks by graphite-furnace atomic-absorption spectrometry.

    PubMed

    Gupta, J G

    1981-01-01

    With use of synthetic solutions and several international standard reference materials a method has been developed for determining traces of Y, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in rocks by electrothermal atomization in a pyrolytically-coated graphite furnace. Depending on the element, the sensitivity is of the order of 10(-9)-10(-12) g at 2500 degrees . To avoid matrix interferences the lanthanides are separated from the common elements by co-precipitation with calcium and iron as carriers. The data for Canadian reference rock SY-2 (syenite), U.S.G.S. reference rocks W-2 (diabase), DNC-1 (diabase) and BIR-1 (basalt), and South African reference rock NIM-18/69 (carbonatite) obtained by graphite-furnace atomization are compared with the values obtained by flame atomic-absorption. The results are in good agreement with literature values. PMID:18962852

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

    PubMed

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

    2008-01-30

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

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

    PubMed

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

    2015-01-01

    The measurement conditions for determining boron using graphite furnace-atomic absorption spectrometry (GF-AAS) were investigated. Differences in the boron absorbance profiles were found using three different commercially available GF-AAS instruments when the graphite atomizers in them were not tuned. The boron absorbances found with and without adjusting the graphite atomizers suggested that achieving an adequate absorbance for the determination of boron requires a sharp temperature profile that overshoots the target temperature during the atomization process. Chemical modifiers that could improve the boron absorbance without the need for using coating agents were tested. Calcium carbonate improved the boron absorbance but did not suppress variability in the peak height. Improvement of boron absorbance was comparatively less using iron nitrate or copper nitrate than using calcium carbonate, but variability in the peak height was clearly suppressed using iron nitrate or copper nitrate. The limit of detection was 0.0026 mg L(-1) when iron nitrate was used. It appears that iron nitrate is a useful new chemical modifier for the quick and simple determination of boron using GF-AAS. PMID:25958863

  7. A first principle study for the adsorption and absorption of carbon atom and the CO dissociation on Ir(100) surface

    SciTech Connect

    Erikat, I. A.; Hamad, B. A.

    2013-11-07

    We employ density functional theory to examine the adsorption and absorption of carbon atom as well as the dissociation of carbon monoxide on Ir(100) surface. We find that carbon atoms bind strongly with Ir(100) surface and prefer the high coordination hollow site for all coverages. In the case of 0.75 ML coverage of carbon, we obtain a bridging metal structure due to the balance between Ir–C and Ir–Ir interactions. In the subsurface region, the carbon atom prefers the octahedral site of Ir(100) surface. We find large diffusion barrier for carbon atom into Ir(100) surface (2.70 eV) due to the strong bonding between carbon atom and Ir(100) surface, whereas we find a very small segregation barrier (0.22 eV) from subsurface to the surface. The minimum energy path and energy barrier for the dissociation of CO on Ir(100) surface are obtained by using climbing image nudge elastic band. The energy barrier of CO dissociation on Ir(100) surface is found to be 3.01 eV, which is appreciably larger than the association energy (1.61 eV) of this molecule.

  8. A first principle study for the adsorption and absorption of carbon atom and the CO dissociation on Ir(100) surface.

    PubMed

    Erikat, I A; Hamad, B A

    2013-11-01

    We employ density functional theory to examine the adsorption and absorption of carbon atom as well as the dissociation of carbon monoxide on Ir(100) surface. We find that carbon atoms bind strongly with Ir(100) surface and prefer the high coordination hollow site for all coverages. In the case of 0.75 ML coverage of carbon, we obtain a bridging metal structure due to the balance between Ir-C and Ir-Ir interactions. In the subsurface region, the carbon atom prefers the octahedral site of Ir(100) surface. We find large diffusion barrier for carbon atom into Ir(100) surface (2.70 eV) due to the strong bonding between carbon atom and Ir(100) surface, whereas we find a very small segregation barrier (0.22 eV) from subsurface to the surface. The minimum energy path and energy barrier for the dissociation of CO on Ir(100) surface are obtained by using climbing image nudge elastic band. The energy barrier of CO dissociation on Ir(100) surface is found to be 3.01 eV, which is appreciably larger than the association energy (1.61 eV) of this molecule. PMID:24206318

  9. A first principle study for the adsorption and absorption of carbon atom and the CO dissociation on Ir(100) surface

    NASA Astrophysics Data System (ADS)

    Erikat, I. A.; Hamad, B. A.

    2013-11-01

    We employ density functional theory to examine the adsorption and absorption of carbon atom as well as the dissociation of carbon monoxide on Ir(100) surface. We find that carbon atoms bind strongly with Ir(100) surface and prefer the high coordination hollow site for all coverages. In the case of 0.75 ML coverage of carbon, we obtain a bridging metal structure due to the balance between Ir-C and Ir-Ir interactions. In the subsurface region, the carbon atom prefers the octahedral site of Ir(100) surface. We find large diffusion barrier for carbon atom into Ir(100) surface (2.70 eV) due to the strong bonding between carbon atom and Ir(100) surface, whereas we find a very small segregation barrier (0.22 eV) from subsurface to the surface. The minimum energy path and energy barrier for the dissociation of CO on Ir(100) surface are obtained by using climbing image nudge elastic band. The energy barrier of CO dissociation on Ir(100) surface is found to be 3.01 eV, which is appreciably larger than the association energy (1.61 eV) of this molecule.

  10. DETERMINATION OF TRACE AMOUNTS OF SELENIUM IN CORN, LETTUCE, POTATOES, SOYBEANS, AND WHEAT BY HYDRIDE GENERATION/CONDENSATION AND FLAME ATOMIC ABSORPTION SPECTROMETRY

    EPA Science Inventory

    Because of the nutritional and toxicological significance of low selenium concentrations in agricultural crops, a procedure utilizing wet digestion followed by hydride generation/condensation-flame atomic absorption was developed for the routine analysis of selenium in different ...

  11. AN INTRALABORATORY COMPARATIVE STUDY OF HYDRIDE GENERATION AND GRAPHITE FURNACE ATOMIC ABSORPTION TECHNIQUES FOR DETERMINING ORGANIC AND INORGANIC ARSENIC IN COMPLEX WASTEWATERS

    EPA Science Inventory

    A detailed intralaboratory comparison of the determination of arsenic in complex wastewater samples by hydride generation and graphite furnace atomic absorption techniques has been conducted. Two hydride generation techniques were employed. One consisted of the use of sodium boro...

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

    NASA Astrophysics Data System (ADS)

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

    2007-09-01

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

  13. A highly sensitive method for the determination of mercury using vapor generation gold wire microextraction and electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hashemi, Payman; Rahimi, Akram

    2007-04-01

    The study introduces a new simple and highly sensitive method for headspace solid phase microextraction (HS-SPME) coupled with electrothermal atomic absorption spectrometric determination of mercury. In the proposed method, a gold wire, mounted in the headspace of a sample solution in a sealed bottle, is used for collection of mercury vapor generated by addition of sodium tetrahydroborate. The gold wire is then simply inserted in the sample introduction hole of a graphite furnace of an electrothermal atomic absorption spectrometry instrument. By applying an atomization temperature of 600 °C, mercury is rapidly desorbed from the wire and determined with high sensitivity. Factorial design and response surface analysis methods were used for optimization of the effect of five different variables in order to maximize the mercury signal. By using a 0.75 mm diameter gold wire, a sample volume of about 8 ml and an extraction time of 11 min, the sensitivity of mercury determination was enhanced up to 10 4 times in comparison to its ordinary ETAAS determination with direct injection of 10 μl sample solutions. A detection limit of 0.006 ng ml - 1 and a precision better than 4.6% (relative standard deviation) were obtained. The method was successfully applied to the determination of mercury in industrial wastewaters and tuna fish samples.

  14. New Homogeneous Standards by Atomic Layer Deposition for Synchrotron X-ray Fluorescence and Absorption Spectroscopies.

    SciTech Connect

    Butterworth, A.L.; Becker, N.; Gainsforth, Z.; Lanzirotti, A.; Newville, M.; Proslier, T.; Stodolna, J.; Sutton, S.; Tyliszczak, T.; Westphal, A.J.; Zasadzinski, J.

    2012-03-13

    Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotron techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution

  15. 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

    NASA Astrophysics Data System (ADS)

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

    2005-06-01

    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 °C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 °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.

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

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-07-20

    Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1). PMID:27345208

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

    PubMed

    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

  18. A comparison of simultaneous plasma, atomic absorption, and iron colorimetric determinations of major and trace constituents in acid mine waters

    USGS Publications Warehouse

    Ball, J.W.; Nordstrom, D.K.

    1994-01-01

    Sixty-three water samples collected during June to October 1982 from the Leviathan/Bryant Creek drainage basin were originally analyzed by simultaneous multielement direct-current plasma (DCP) atomic-emission spectrometry, flame atomic-absorption spectrometry, graphite-furnace atomic-absorption spectrometry (GFAAS) (thallium only), ultraviolet-visible spectrometry, and hydride-generation atomic-absorption spectrometry.Determinations were made for the following metallic and semi-metallic constituents: AI, As, B, Ba, Be, Bi, Cd, Ca, Cr, Co, Cu, Fe(11), Fe(total), Li, Pb, Mg, Mn, Mo, Ni, K, Sb, Se, Si, Na, Sr, TI, V, and Zn. These samples were re-analyzed later by simultaneous multielement inductively coupled plasma (ICP) atomic-emission spectrometry and Zeeman-corrected GFAAS to determine the concentrations of many of the same constituents with improved accuracy, precision, and sensitivity. The result of this analysis has been the generation of comparative concentration values for a significant subset of the solute constituents. Many of the more recently determined values replace less-than-detection values for the trace metals; others constitute duplicate analyses for the major constituents. The multiple determinations have yielded a more complete, accurate, and precise set of analytical data. They also have resulted in an opportunity to compare the performance of the plasma-emission instruments operated in their respective simultaneous multielement modes. Flame atomic-absorption spectrometry was judged best for Na and K and hydride-generation atomic-absorption spectrometry was judged best for As because of their lower detection limit and relative freedom from interelement spectral effects. Colorimetric determination using ferrozine as the color agent was judged most accurate, precise, and sensitive for Fe. Cadmium, lead, and vanadium concentrations were too low in this set of samples to enable a determination of whether ICP or DCP is a more suitable technique. Of

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

    NASA Astrophysics Data System (ADS)

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

    2011-05-01

    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.

  20. Speciation of methyl- and butyltin compounds and inorganic tin in oysters by hydride generation atomic absorption spectrometry

    SciTech Connect

    Han, J.S.; Weber, J.H.

    1988-02-15

    Because of the toxicity of tributyltin originating from many antifouling marine paints, there is much concern about its effect on aquatic life and, particularly, on shellfish. This paper describes speciation of inorganic tin, methyltin compounds, and butyltin compounds from oyster samples. The authors validated the hydride generation atomic absorption spectrophotometric technique by demonstrating ca. 100% recovery from spiked samples and by the absence of any organotin decomposition products. Absolute detection limits (3sigma) are 1.1-2.5 ng for 0.1-g oyster samples (wet weight). This method is superior to published techniques because of careful validation, low limits of detection, and minimal sample manipulation.

  1. A photon counting and a squeezing measurement method by the exact absorption and dispersion spectrum of Λ-type Atoms.

    PubMed

    Naeimi, Ghasem; Alipour, Samira; Khademi, Siamak

    2016-01-01

    Recently, the master equations for the interaction of two-mode photons with a three-level Λ-type atom are exactly solved for the coherence terms. In this paper the exact absorption spectrum is applied for the presentation of a non-demolition photon counting method, for a few number of coupling photons, and its benefits are discussed. The exact scheme is also applied where the coupling photons are squeezed and the photon counting method is also developed for the measurement of the squeezing parameter of the coupling photons. PMID:27610321

  2. [Use of solubilization for the preparation of samples for determination of heavy metals in biological materials using atomic absorption spectrophotometry].

    PubMed

    Pfüller, U; Fuchs, V; Golbs, S; Ebert, E; Pfeifer, D

    1980-01-01

    Solubilisation was tested for its suitability to prepare organic samples for metal determination. Flameless atomic-absorption spectrophotometry was used as test method. Copper, manganese, zinc, and chromium levels were determined from various organ systems of Wistar rat, in response to "normal" feeding of pelletised standard feed. A comparison between experimentally established concentrations, on the one hand, and literature data, on the other, suggested that solubilisation was applicable with good success to the preparation of samples from which to determine reliable values, in ppm and ppb, of the above elements. PMID:7436671

  3. Determination of silver in soils, sediments, and rocks by organic-chelate extraction and atomic absorption spectrophotometry

    USGS Publications Warehouse

    Chao, T.T.; Ball, J.W.; Nakagawa, H.M.

    1971-01-01

    A useful method for the determination of silver in soil, sediment, and rock samples in geochemical exploration has been developed. The sample is digested with concentrated nitric acid, and the silver extracted with triisooctyl thiophosphate (TOTP) in methyl isobutyl ketone (MIBK) after dilution of the acid digest to approximately 6 M. The extraction of silver into the organic extractant is quantitative and not affected by the nitric acid concentration from 4 M to 8 M, or by different volumes of TOTP-MIBK. The extracted silver is stable and remains in the organic phase up to several days. The silver concentration is determined by atomic absorption spectrophotometry. ?? 1971.

  4. Optimisation of flame parameters for simultaneous multi-element atomic absorption spectrometric determination of trace elements in rocks

    USGS Publications Warehouse

    Kane, J.S.

    1988-01-01

    A study is described that identifies the optimum operating conditions for the accurate determination of Co, Cu, Mn, Ni, Pb, Zn, Ag, Bi and Cd using simultaneous multi-element atomic absorption spectrometry. Accuracy was measured in terms of the percentage recoveries of the analytes based on certified values in nine standard reference materials. In addition to identifying optimum operating conditions for accurate analysis, conditions resulting in serious matrix interferences and the magnitude of the interferences were determined. The listed elements can be measured with acceptable accuracy in a lean to stoicheiometric flame at measurement heights ???5-10 mm above the burner.

  5. [Determination of trace elements in Spirulina platensis (Notdst.) Geitl. by flame atomic absorption spectrometry combined with microsampling pulse nebulization technique].

    PubMed

    Cheng, Cun-Gui; Hong, Qing-Hong; Li, Dan-Ting; Fan, Meng-Hai; Cai, Xiao-Dan

    2006-09-01

    The contents of trace elements Ni, Zn, Mn, Cu, Mg, Fe, Ca and Pb in Spirulina platensis (Notdst.) Geitl. were determined by flame atomic absorption spectrometry combined with microsampling pulse nebulization technique. The results of the determination show that Spirulina platensis (Notdst.) Geitl. are rich in the inorganic elements such as Mg, Zn, Fe, Ca and Cu. Its recovery ratio obtained by standard addition method ranged between 96.58% and 106.12%, and its RSD was lower than 4.26%. The result will provide scientific data for the study on the trace elements in Spirulina platensis (Notdst.) Geitl. and on their relativity of efficacy of medicine. PMID:17112058

  6. New method for determining relative oscillator strengths of atoms through combined absorption and emission measurements - Application to titanium /Ti I/

    NASA Technical Reports Server (NTRS)

    Cardon, B. L.; Smith, P. L.; Whaling, W.

    1979-01-01

    The paper introduces a procedure that combines measurements of absorption and emission by atoms to obtain relative oscillator strengths that are independent of temperature determination in the sources and of assumptions regarding local thermodynamic equilibrium. The experimental observations are formed into sets of transitions and required to satisfy defined ratios. The procedure is illustrated with the published data of Whaling et al. and Smith and Kuehne for 16 transitions in Ti I. It is shown that the relative oscillator strengths resulting from this procedure have calculated uncertainties between 5 and 17% (about 95% confidence level). Evidence is presented to suggest that these uncertainties have been overestimated.

  7. Nonlinear absorption in ionic liquids with transition metallic atoms in the anion

    NASA Astrophysics Data System (ADS)

    Nóvoa-López, José A.; López Lago, Elena; Seijas, Julio A.; Pilar Vázquez-Tato, M.; Troncoso, Jacobo; de la Fuente, Raúl; Salgueiro, José R.; Michinel, Humberto

    2016-02-01

    Nonlinear absorption has been investigated by open aperture Z-scan in ionic liquids obtained by combination of 1-butyl-3-methyl-imidazolium cations with anions containing a transition metal (Co, Zn, Cu or Ni) and thiocyanate groups. The laser source was a Ti:Sapphire oscillator (80-fs pulses, λ = 810 nm, repetition rate of 80.75 MHz). All liquids present quite low heat capacities that favor the development of strong thermal effects. Thermal effects and nonlinear absorption make them potential materials for optical limiting purposes.

  8. Absorption spectra of two-level atoms interacting with a strong polychromatic pump field and an arbitrarily intense probe field

    NASA Astrophysics Data System (ADS)

    Yoon, Tai Hyun; Chung, Myung Sai; Lee, Hai-Woong

    1999-09-01

    A numerical method is introduced that solves the optical Bloch equations describing a two-level atom interacting with a strong polychromatic pump field with an equidistant spectrum and an arbitrarily intense monochromatic probe field. The method involves a transformation of the optical Bloch equations into a system of equations with time-independent coefficients at steady state via double harmonic expansion of the density-matrix elements, which is then solved by the method of matrix inversion. The solutions so obtained lead immediately to the determination of the polarization of the atomic medium and of the absorption and dispersion spectra. The method is applied to the case when the pump field is bichromatic and trichromatic, and the physical interpretation of the numerically computed spectra is given.

  9. CoxFey@C Composites with Tunable Atomic Ratios for Excellent Electromagnetic Absorption Properties

    PubMed Central

    Lv, Hualiang; Ji, Guangbin; Zhang, Haiqian; Li, Meng; Zuo, Zhongzheng; Zhao, Yue; Zhang, Baoshan; Tang, Dongming; Du, Youwei

    2015-01-01

    The shell on the nano-magnetic absorber can prevent oxidation, which is very important for its practical utilization. Generally, the nonmagnetic shell will decrease the integral magnetic loss and thus weaken the electromagnetic absorption. However, maintaining the original absorption properties of the magnetic core is a major challenge. Here, we designed novel and facile CoxFey@C composites by reducing CoxFe3−xO4@phenolic resin (x = 1, 0.5 and 0.25). High saturation magnetization value (Ms) of CoxFey particle, as a core, shows the interesting magnetic loss ability. Meanwhile, the carbon shell may increase the integral dielectric loss. The resulting composite shows excellent electromagnetic absorption properties. For example, at a coating thickness of 2 mm, the RLmin value can reach to −23 dB with an effective frequency range of 7 GHz (11–18 GHz). The mechanisms of the improved microwave absorption properties are discussed. PMID:26659124

  10. CoxFey@C Composites with Tunable Atomic Ratios for Excellent Electromagnetic Absorption Properties

    NASA Astrophysics Data System (ADS)

    Lv, Hualiang; Ji, Guangbin; Zhang, Haiqian; Li, Meng; Zuo, Zhongzheng; Zhao, Yue; Zhang, Baoshan; Tang, Dongming; Du, Youwei

    2015-12-01

    The shell on the nano-magnetic absorber can prevent oxidation, which is very important for its practical utilization. Generally, the nonmagnetic shell will decrease the integral magnetic loss and thus weaken the electromagnetic absorption. However, maintaining the original absorption properties of the magnetic core is a major challenge. Here, we designed novel and facile CoxFey@C composites by reducing CoxFe3-xO4@phenolic resin (x = 1, 0.5 and 0.25). High saturation magnetization value (Ms) of CoxFey particle, as a core, shows the interesting magnetic loss ability. Meanwhile, the carbon shell may increase the integral dielectric loss. The resulting composite shows excellent electromagnetic absorption properties. For example, at a coating thickness of 2 mm, the RLmin value can reach to -23 dB with an effective frequency range of 7 GHz (11-18 GHz). The mechanisms of the improved microwave absorption properties are discussed.

  11. 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

    ERIC Educational Resources Information Center

    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,…

  12. Theory of x-ray absorption by laser-dressed atoms

    SciTech Connect

    Buth, Christian; Santra, Robin

    2007-03-15

    An ab initio theory is devised for the x-ray photoabsorption cross section of atoms in the field of a moderately intense optical laser (800 nm, 10{sup 13} W/cm{sup 2}). The laser dresses the core-excited atomic states, which introduces a dependence of the cross section on the angle between the polarization vectors of the two linearly polarized radiation sources. We use the Hartree-Fock-Slater approximation to describe the atomic many-particle problem in conjunction with a nonrelativistic quantum-electrodynamic approach to treat the photon-electron interaction. The continuum wave functions of ejected electrons are treated with a complex absorbing potential that is derived from smooth exterior complex scaling. The solution to the two-color (x-ray plus laser) problem is discussed in terms of a direct diagonalization of the complex symmetric matrix representation of the Hamiltonian. Alternative treatments with time-independent and time-dependent non-Hermitian perturbation theories are presented that exploit the weak interaction strength between x rays and atoms. We apply the theory to study the photoabsorption cross section of krypton atoms near the K edge. A pronounced modification of the cross section is found in the presence of the optical laser.

  13. Atomic partial charges in condensed phase from an exact sum rule for infrared absorption

    NASA Astrophysics Data System (ADS)

    Vuilleumier, Rodolphe

    2014-05-01

    A general sum rule for infrared intensities provides a definition of effective partial charges which can be experimentally obtained using isotopic substitutions and is valid in both gas and condensed phases. Of particular interest is the case of molecular liquids. We have, therefore, determined the hydrogen partial charges in liquid methanol and liquid water from the available literature. The resulting charges are 0.63 e and 0.14 e for hydrogen atoms bounded to the methanol oxygen and carbon atoms, respectively, and 0.55 e for hydrogen atoms in liquid water. The effective partial charges in liquid water were also computed from density functional based ab initio molecular dynamics simulations and found in good agreement with experiment.

  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

    SciTech Connect

    Ombaba, J.M.

    1992-01-01

    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 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 (mytilus edullus) and sediment from Boston Harbor, industrial waste water and industrial sludge, and (2) the detection of methylcyclopentadienylmanganesetricarbonyl (MMT) and similar compounds used as gasoline additives. An ultrasonic nebulizer 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 considered. The evaluation of a computer-aided optimization program, Drylab GC, using spearmint oil and Environmental Protection Agency (EPA) standard mixture as probes is discussed. The program is used for separation optimization and prediction of gas chromatographic parameters. The program produces a relative resolution map (RRM) which guides the analyst in selecting the most favorable temperature programming rate for the separation.

  15. Atomic absorption spectrometry for the automatic indirect determination of ascorbic acid based on-the reduction of manganese dioxide.

    PubMed

    Noroozifar, Meissam; Khorasani-Motlagh, Mozhgan; Akhavan, Kambiz

    2005-06-01

    A new and simple flow injection method followed by atomic absorption spectrometry has been developed for the indirect determination of ascorbic acid. The proposed method is based on oxidation of ascorbic acid to dehydroascorbic acid using a solid-phase manganese dioxide (30% m/m suspended on silica gel beads) reactor. The flow of the sample through the column reduces the MnO2 to Mn(II) in an acidic carrier stream of 6.3 mM HNO3 (pH 2.2) with flow rate of 4.0 ml/min at room temperature; Mn(II) is measured by atomic absorption spectrometry. The absorbance of Mn(II) is proportional to the concentration of ascorbic acid in the sample. The calibration curve was linear up to 30 mg/L, with a detection limit of 0.2 mg/L for a 220 microL injected sample volume. The developed procedure was found to be suitable for the determination of AsA in pharmaceuticals and foods with a relative standard deviation better than 1.09% and a sampling rate of about 95 h(-1). The results exhibit no interference from the presence of large amounts of organic compounds. The reliability of the method was established by parallel determination against the 2,6-dichlorophenol-indophenol methods. PMID:15984201

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

    PubMed

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

    2012-01-01

    The determination of trace elements in food and soil samples by atomic absorption spectrometry was investigated. A coprecipitation procedure with holmium hydroxide was used for separation-preconcentration of trace elements. Trace amounts of copper(II), manganese(II), cobalt(II), nickel(ll), chromium(lll), iron(Ill), cadmium(ll), and lead(ll) ions were coprecipitated with holmium hydroxide in 2.0 M NaOH medium. The optimum conditions for the coprecipitation process were investigated for several commonly tested experimental parameters, such as amount of coprecipitant, effect of standing time, centrifugation rate and time, and sample volume. The precision, based on replicate analysis, was lower than 10% for the analytes. In order to verify the accuracy of the method, the certified reference materials BCR 141 R calcareous loam soil and CRM 025-050 soil were analyzed. The procedure was successfully applied for separation and preconcentration of the investigated ions in various food and soil samples. An amount of the solid samples was decomposed with 15 mL concentrated hydrochloric acid-concentrated nitric acid (3 + 1). The preconcentration procedure was then applied to the final solutions. The concentration of trace elements in samples was determined by atomic absorption spectrometry. PMID:22816279

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

    PubMed

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

    2014-01-01

    The total selenium (Se) was determined in herbal and pharmaceutical supplements used for liver diseases. The total Se contents were determined in different pharmaceutical and herbal supplements by hydride generation atomic absorption spectrometry (HGAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after microwave-assisted acid digestion. The accuracy of the techniques was evaluated by using certified reference material and the standard addition method. The recoveries of total Se were 99.4 and 99.0% for HGAAS and GFAAS, respectively. The precision of the techniques expressed as RSD were 2.34 and 4.54% for HGAAS and GFAAS measurements, respectively. The LOD values for HGAAS and GFAAS were 0.025 and 0.052 pglg, respectively. The concentrations of Se in pharmaceutical and herbal supplements were found in the range of 19.2-53.8 and 25.0-42.5 pg/g, respectively, corresponding to 35-76% and 45-76% of the total recommended dose of Se for adults. PMID:25632445

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

  19. Colorimetric and atomic absorption spectrometric determination of mucolytic drug ambroxol through ion-pair formation with iron and thiocyanate.

    PubMed

    Levent, Abdulkadir; Sentürk, Zühre

    2010-09-01

    Colorimetric and atomic absorption spectrometric methods have been developed for the determination of mucolytic drug Ambroxol. These procedures depend upon the reaction of iron(III) metal ion with the drug in the presence of thiocyanate ion to form stable ion-pair complex which extractable chloroform. The red-coloured complex was determined either colorimetrically at 510 nm or by indirect atomic absorption spectrometry (AAS) via the determination of the iron content in the formed complex. The optimum experimental conditions for pH, concentrations of Fe(3+) and SCN(-), shaking time, phase ratio, and the number of extractions were determined. Under the proposed conditions, linearity was obeyed in the concentration ranges 4.1x10(-6) - 5.7x10(-5) M (1.7-23.6 µg mL(-1)) using both methods, with detection limits of 4.6x10(-7) M (0.19 µg mL(-1)) for colorimetry and 1.1x10(-6) M (0.46 µg mL(-1)) for AAS. The proposed methods were applied for the determination of Ambroxol in tablet dosage forms. The results obtained were statistically analyzed and compared with those obtained by applying the high-performance liquid chromatographic method with diode-array detection. PMID:20426742

  20. Comparison of four methods for digesting food samples for determination of trace levels of cadmium by flameless atomic absorption spectrophotometry

    SciTech Connect

    Cabanis, M.T.; Cassanas, G.; Cabanis, J.C.; Brun, S.

    1988-01-01

    The authors compared 4 digestion procedures, namely, sulfuric-nitric acid in an open flask, nitric acid under pressure, sulfuric-nitric acid with refluxing, and nitric-hydrochloric-peroxide with refluxing, for the determination of cadmium by flameless atomic absorption spectrophotometry in 3 foodstuffs: rice, beef, and cream cheese. The foodstuffs were homogenized and divided into several batches for analysis. The results were evaluated using a 2-way cross analysis of variance. The study revealed that the digestion procedure was a highly significant factor (P < 10/sup -4/) in the analysis of the 3 foods; whereas the nature of the foodstuffs was not significant for rice and meat and only slightly significant (P < 10/sup -2/) for cream cheese. When the foodstuffs were spiked with a known amount of cadmium, they observed a loss of the metal when the sulfuric-nitric acid procedure in an open flask and the nitric-hydrochloric-peroxide digestion procedure were used. Taken together, the results of the present study indicate that the choice of the reagents used for digestion of foodstuffs is a crucial factor for cadmium determination by flameless atomic absorption spectrophotometry.

  1. Estimation of boron isotope ratios using high resolution continuum source atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Wiltsche, Helmar; Prattes, Karl; Zischka, Michael; Knapp, Günter

    2009-04-01

    In the production of 10B enriched steels, the production-recycling process needs to be closely monitored for inadvertent mix-up of materials with different B isotope levels. A quick and simple method for the estimation of boron isotope ratios in high alloyed steels using high resolution continuum source flame AAS (HR-CS-FAAS) was developed. On the 208.9 nm B line the wavelength of the peak absorption of 10B and 11B differs by 2.5 pm. The wavelength of the peak absorption of boron was determined by fitting a Gauss function through spectra simultaneously recorded by HR-CS-FAAS. It was shown that a linear correlation between the wavelength of the peak absorption and the isotope ratio exists and that this correlation is independent of the total boron concentration. Internal spectroscopic standards were used to compensate for monochromator drift and monochromator resolution changes. Accuracy and precision of the analyzed samples were thereby increased by a factor of up to 1.3. Three steel reference materials and one boric acid CRM, each certified for the boron isotope ratio were used to validate the procedure.

  2. The fabrication of superlow protein absorption zwitterionic coating by electrochemically mediated atom transfer radical polymerization and its application.

    PubMed

    Hu, Yichuan; Yang, Guang; Liang, Bo; Fang, Lu; Ma, Guanglong; Zhu, Qin; Chen, Shengfu; Ye, Xuesong

    2015-02-01

    A well-controllable electrochemically mediated surface-initiated atom transfer radical polymerization (e-siATRP) method for the fabrication of superlow protein absorption zwitterionic hydrogel coatings based on poly(sulbetaine methacrylate) (pSBMA) was developed in this work. The effects of the electric condition on polymerization as well as its antifouling performances both in vitro and in vivo were also investigated. Different potentials (-0.08 V, -0.15 V and -0.22 V) and polymerization times (from 8 to 48 h) were chosen to study the polymerization procedure. X-ray photoelectron spectroscopy, atomic force microscopy and ellipsometry measurements were used to characterize the properties of the polymer layers. Ellipsometry measurements showed that a higher potential provided faster polymerization and thicker polymer layers; however, the protein absorption experiments showed that the best polymerization condition was under a constant potential of -0.15 V and 32 h, under which the protein absorption was 0.8% in an enzyme-linked immunosorbent assay (compared to a bare gold electrode). The electrodes with a pSBMA coating effectively deduced the current sensitivity decay both in undiluted serum and in vivo. The usage of the commercially available polymerization monomer of SBMA, the simple convenient synthesis process regardless of the presence of oxygen and the excellent controllability of e-siATRP make it a very promising and universal technique in the preparation of zwitterionic polymer coatings, especially in the development of biocompatible material for implantable devices such as neural and biosensor electrodes. PMID:25463508

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

    PubMed

    Vilar Fariñas, M; Barciela García, J; García Martín, S; Peña Crecente, R; Herrero Latorre, C

    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(NO3)2 and (NH4)H2PO4-Mg(NO3)2] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 microg 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

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

    NASA Astrophysics Data System (ADS)

    Atilgan, Semin; Akman, Suleyman; Baysal, Asli; Bakircioglu, Yasemin; Szigeti, Tamás; Óvári, Mihály; Záray, Gyula

    2012-04-01

    An analytical method has been developed for determination of palladium in PM2.5 fractions of urban airborne particulate matter by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry. For the optimization of the experimental conditions, a road dust certified reference material (BCR-723) was used. The influence of pyrolysis and atomization temperatures, the amount of sample introduced into the graphite furnace and the addition of acids, surfactants and modifiers on the analytical signal of Pd were investigated. The limit of detection, calculated based on three times the standard deviations of analytical signals obtained during the atomization of 10 blank filter pieces, was 0.07 pg/m3. Since the amount of solid certified reference material introduced into the graphite furnace was about 50-2000 times lower than those required in order to obtain the certified value, the precision was relatively poor. This analytical method was applied for investigation of urban airborne particulate matter collected onto quartz fiber filters by high-volume aerosol samplers in the city center of Istanbul (Turkey) and Budapest (Hungary). The measured Pd concentrations changed in the range of 0.22-0.64 and 0.25-0.86 pg/m3 in Istanbul and Budapest, respectively.

  5. [Determination of aluminum in wheat flour food by microwave digestion-high resolution continuum source graphite furnace atomic absorption spectrometry].

    PubMed

    Ren, Ting; Zhao, Li-jiao; Zhong, Ru-gang

    2011-12-01

    The contents of aluminum (Al) in four kinds of wheat flour food (noodle, dumpling wrapper, twisted cruller and soda biscuit) were determined by high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) combined with microwave digestion. The samples were completely digested by the mixture of HNO3 and H2O2 in closed polytetrafluoroethylene (PTFE) vessels. The conditions for microwave digestion, pyrolysis temperature and atomization temperature were optimized. The optimum experimental conditions were determined as follows. The microwave digestion was performed with HNO3/H2O2 7:1 (volume ratio), microwave power 1000 W and 190 degrees C for 40 minutes. The optimum pyrolysis temperature was 1350 degrees C and the optimum atomization temperature was 2400 degrees C. Magnesium nitrate solution with the concentration of 1 g x L(-1) was used as the matrix modifier. The correlation coefficient for the standard curve was 0.9999, the relative standard deviation (RSD) was from 1.7% to 2.4%, and the recovery for the samples was from 98.16% to 102.67%. The assay method for the determination of Al in wheat flour food established in this study has referential importance for the constituent of the correlated food standards. PMID:22295801

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

    NASA Astrophysics Data System (ADS)

    Gökmen, A.; Yalcin, S.

    1992-01-01

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

  7. Near resonant absorption by atoms in intense, fluctuating fields: (Progress report)

    SciTech Connect

    Not Available

    1989-01-01

    During the present grant period preparations for photon echo studies of the role of phase fluctuations of an optical driving field resonant with the /sup 1/S/sub 0/ - /sup 3/P/sub 1/ transition in /sup 174/Yb are moving forward. This experimental study emphasizes the role of fluctuations as a decorrelating mechanism on a phased array of excited atoms. Improvements in laser stabilization and in the quality of the fluctuation spectrum have been carried out and the first spectroscopic measurements will be carried out during this grant year. In response to an important recent theoretical study we have also applied the phase fluctuation synthesizing capability to the study of the atomic sodium resonance fluorescence line profile, driven by a phase fluctuating laser. The measured fluctuations in the fluorescence, characterized in terms of the standard deviation of the fluorescence intensity, have an unexpected and strong dependence on detuning of the driving laser.

  8. Determination of arsenic in geological materials by electrothermal atomic-absorption spectrometry after hydride generation

    USGS Publications Warehouse

    Sanzolone, R.F.; Chao, T.T.; Welsch, E.P.

    1979-01-01

    Rock and soil samples are decomposed with HClO4-HNO3; after further treatment, arsine is generated and absorbed in a dilute silver nitrate solution. Aliquots of this solution are injected into a carbon rod atomizer. Down to 1 ppm As in samples can be determined and there are no significant interferences, even from chromium in soils. Good results were obtained for geochemical reference samples. ?? 1979.

  9. Heating rates in furnace atomic absorption using the L'vov platform

    USGS Publications Warehouse

    Koirtyohann, S.R.; Giddings, R.C.; Taylor, H.E.

    1984-01-01

    Heating rate profiles for the furnace tube wall, the furnace atmosphere, and a L'vov platform were established for a range of conditions in a cyclically heated graphite atomizer. The tube wall profile was made by direct observation with a recording optical pyrometer. The sodium line reversal method was used to establish the heating rate of the furnace atmosphere, and appearance temperatures for a series metals of differing volatility was used to establish platform profiles. The tube wall heating rate was nearly linear at 2240??C s- until the desired temperature was reached after which the temperature remained constant. The furnace atmosphere reached a given temperature 0.2-0.4 s later than the tube wall through most of the atomize cycle. The platform lagged the tube wall 0.5-0.8 s. Under typical operating conditions the furnace atmosphere was 100-200??C cooler than the tube wall and at nearly constant temperature when the analyte vaporized from the platform. The L'vov platform causes the cyclically heated commercial furnace to approximate the behavior of a constant temperature furnace during atomization. ?? 1984.

  10. Atomic structure of Mn-rich nanocolumns probed by x-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Rovezzi, M.; Devillers, T.; Arras, E.; d'Acapito, F.; Barski, A.; Jamet, M.; Pochet, P.

    2008-06-01

    In this letter, we have used the extended x-ray-absorption fine-structure (EXAFS) technique to investigate the structure of Mn-rich self-organized nanocolumns grown by low temperature molecular beam epitaxy. The EXAFS analysis has shown that Mn-rich nanocolumns exhibit a complex local structure that cannot be described by a simple substitutional model. Additional interatomic distances had to be considered in the EXAFS model which are in excellent agreement with the structure of a Ge-3Mn building block tetrahedron of Ge3Mn5.

  11. Direct measurement of interstellar extinction toward young stars using atomic hydrogen Lyα absorption

    SciTech Connect

    McJunkin, Matthew; France, Kevin; Brown, Alexander; Schneider, P. C.; Herczeg, Gregory J.; Hillenbrand, Lynne; Schindhelm, Eric; Edwards, Suzan

    2014-01-10

    Interstellar reddening corrections are necessary to reconstruct the intrinsic spectral energy distributions (SEDs) of accreting protostellar systems. The stellar SED determines the heating and chemical processes that can occur in circumstellar disks. Measurement of neutral hydrogen absorption against broad Lyα emission profiles in young stars can be used to obtain the total H I column density (N(H I)) along the line of sight. We measure N(H I) with new and archival ultraviolet observations from the Hubble Space Telescope (HST) of 31 classical T Tauri and Herbig Ae/Be stars. The H I column densities range from log{sub 10}(N(H I)) ≈19.6-21.1, with corresponding visual extinctions of A{sub V} =0.02-0.72 mag, assuming an R{sub V} of 3.1. We find that the majority of the H I absorption along the line of sight likely comes from interstellar rather than circumstellar material. Extinctions derived from new HST blue-optical spectral analyses, previous IR and optical measurements, and new X-ray column densities on average overestimate the interstellar extinction toward young stars compared to the N(H I) values by ∼0.6 mag. We discuss possible explanations for this discrepancy in the context of a protoplanetary disk geometry.

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

    PubMed Central

    Hernández-Zavala, Araceli; Matoušek, Tomáš; Drobná, Zuzana; Paul, David S.; Walton, Felecia; Adair, Blakely M.; Jiří, Dědina; Thomas, David J.

    2008-01-01

    Analyses of arsenic (As) species in tissues and body fluids of individuals chronically exposed to inorganic arsenic (iAs) provide essential information about the exposure level and pattern of iAs metabolism. We have previously described an oxidation state-specific analysis of As species in biological matrices by hydride-generation atomic absorption spectrometry (HG-AAS), using cryotrapping (CT) for preconcentration and separation of arsines. To improve performance and detection limits of the method, HG and CT steps are automated and a conventional flame-in-tube atomizer replaced with a recently developed multiple microflame quartz tube atomizer (multiatomizer). In this system, arsines from AsIII-species are generated in a mixture of Tris-HCl (pH 6) and sodium borohydride. For generation of arsines from both AsIII- and AsV-species, samples are pretreated with L-cysteine. Under these conditions, dimethylthioarsinic acid, a newly described metabolite of iAs, does not interfere significantly with detection and quantification of methylated trivalent arsenicals. Analytical performance of the automated HG-CT-AAS was characterized by analyses of cultured cells and mouse tissues that contained mono- and dimethylated metabolites of iAs. The capacity to detect methylated AsIII- and AsV-species was verified, using an in vitro methylation system containing recombinant rat arsenic (+3 oxidation state) methyltransferase and cultured rat hepatocytes treated with iAs. Compared with the previous HG-CT-AAS design, detection limits for iAs and its metabolites have improved significantly with the current system, ranging from 8 to 20 pg. Recoveries of As were between 78 and 117%. The precision of the method was better than 5% for all biological matrices examined. Thus, the automated HG-CT-AAS system provides an effective and sensitive tool for analysis of all major human metabolites of iAs in complex biological matrices. PMID:18677417

  13. Absorption by ground-state lead atoms of the 283. 3-nm resonant line from a lead hollow cathode lamp. An absolute number density calibration

    SciTech Connect

    Simons, J.W. ); Oldenborg, R.C.; Baughcum, S.L. )

    1989-10-19

    An accurate absolute number density calibration curve for absorption by gaseous lead atoms of the 283.3-nm resonant line from a typical lead hollow cathode lamp is reported. This calibration shows the usual curvature in the Beer-Lambert plot for atomic absorption at moderate to high absorbances that is commonly attributed to self-absorption leading to line reversal in the source and/or preferential absorption at the line center when the absorber temperature is not much greater than the source Doppler temperature. A theoretical calculation utilizing a Doppler-limited Fourier transform spectrum of the 283.3-nm emission from the lamp and a tabulated value of the absorption cross section and accounting for the isotopic and nuclear hyperfine components in both the emission and absorption due to naturally occurring lead quantitatively reproduces the experimental calibration curve without any parameter adjustments. It is found that the curvature in the Beer-Lambert plot has more to do with the fact that the absorbing and emitting atoms are a mixture of isotopes giving several isotopic and nuclear hyperfine transitions at slightly different frequencies than it does with preferential absorption at line centers.

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

    NASA Astrophysics Data System (ADS)

    Bencs, László; Laczai, Nikoletta; Ajtony, Zsolt

    2015-07-01

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

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

    PubMed

    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. PMID:26592606

  16. Cold Atomic Hydrogen, Narrow Self-Absorption, and the Age of Molecular Clouds

    NASA Technical Reports Server (NTRS)

    Goldsmith, Paul F.

    2006-01-01

    This viewgraph presentation reviews the history, and current work on HI and its importance in star formation. Through many observations of HI Narrow Self Absorption (HINSA) the conclusions are drawn and presented. Local molecular clouds have HI well-mixed with molecular constituents This HI is cold, quiescent, and must be well-shielded from the UV radiation field The density and fractional abundance (wrt H2) of the cold HI are close to steady state values The time required to convert these starless clouds from purely HI initial state to observed present composition is a few to ten million years This timescale is a lower limit - if dense clouds being swept up from lower density regions by shocks, the time to accumulate material to get A(sub v) is approximately 1 and provide required shielding may be comparable or longer

  17. Cloud point extraction thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

    NASA Astrophysics Data System (ADS)

    Wu, Peng; Zhang, Yunchang; Lv, Yi; Hou, Xiandeng

    2006-12-01

    A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 μg/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

  18. Impact of the analytical blank in the uncertainty evaluation of the copper content in waters by flame atomic absorption spectrometry.

    PubMed

    de Oliveira, Elcio Cruz; Monteiro, Maria Inês Couto; Pontes, Fernanda Veronesi Marinho; de Almeida, Marcelo Dominguez; Carneiro, Manuel Castro; da Silva, Lílian Irene Dias; Alcover Neto, Arnaldo

    2012-01-01

    Chemical analysts use analytical blanks in their analyses, but seldom is this source of uncertainty evaluated. Generally, there is great confusion. Although the numerical value of the blank, in some situations, can be negligible, its source of uncertainty cannot be. This article discusses the uncertainty contribution of the analytical blank using a numerical example of the copper content in waters by flame atomic absorption spectrometry. The results indicate that the uncertainties of the analytical blank can contribute up to 50% when the blank sample is considered in this analysis, confirming its high impact. This effect can be primarily observed where the analyte concentration approaches the lower range of the analytical curve. Even so, the blank is not always computed. Therefore, the relevance of the analytical blank can be confirmed by uncertainty evaluation. PMID:22649945

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

    PubMed

    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. PMID:25078838

  20. Rate and composition control by atomic absorption spectroscopy for the coevaporation of high T sub c superconducting films

    SciTech Connect

    Lu, C. ); Missert, N.; Mooij, J.E.; Rosenthal, P.; Matijasevic, V.; Beasley, M.R.; Hammond, R.H. )

    1989-02-01

    Atomic absorption spectroscopy has been used to control the deposition rates during coevaporation processes with multiple electron-beam sources. This technique is material specific and thus allows the deposition rate of each component to be controlled independently. Because only a light beam is needed to interact with the vapor stream, the sampling region can be selected to be very close to the substrate for precise control of the film composition. With its high sensitivity and no limitations on operation pressure, this technique offers some unique advantages for the preparation of high Tc superconducting films by coevaporation in a high oxygen partial pressure environment. The performance of a multi-source deposition controller and the resultant film properties are presented.

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

    USGS Publications Warehouse

    Viets, J.G.

    1978-01-01

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

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

    USGS Publications Warehouse

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

    1984-01-01

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

  3. Speciation determination of chromium(III) and (VI) using preconcentration cloud point extraction with flame atomic absorption spectrometry (FAAS).

    PubMed

    Kiran, K; Kumar, K Suresh; Prasad, B; Suvardhan, K; Lekkala, Ramesh Babu; Janardhanam, K

    2008-02-11

    bis-[2-Hydroxy-1-naphthaldehyde] thiourea was synthesized and preconcentration cloud point extraction (CPE) for speciation determination of chromium(III) and (VI) in various environmental samples with flame atomic absorption spectrometry (FAAS) has been developed. Chromium(III) complexes with bis-[2-hydroxynaphthaldehyde] thiourea is subsequently entrapped in the surfactant micelles. After complexation of chromium(III) with reagent, the analyte was quantitatively extracted to the surfactant-rich phase in the non-ionic surfactant Triton X-100 after centrifugation. The effect of pH, concentration of chelating agent, surfactant, equilibration temperature and time on CPE was studied. The relative standard deviation was 2.13% and the limits of detection were around 0.18 microg L(-1). PMID:17583423

  4. Comparison of Adsorbed Mercury Screening Method With Cold-Vapor Atomic Absorption Spectrophotometry for Determination of Mercury in Soil

    NASA Technical Reports Server (NTRS)

    Easterling, Donald F.; Hovanitz, Edward S.; Street, Kenneth W.

    2000-01-01

    A field screening method for the determination of elemental mercury in environmental soil samples involves the thermal desorption of the mercury from the sample onto gold and then the thermal desorption from the gold to a gold-film mercury vapor analyzer. This field screening method contains a large number of conditions that could be optimized for the various types of soils encountered. In this study, the conditions were optimized for the determination of mercury in silty clay materials, and the results were comparable to the cold-vapor atomic absorption spectrophotometric method of determination. This paper discusses the benefits and disadvantages of employing the field screening method and provides the sequence of conditions that must be optimized to employ this method of determination on other soil types.

  5. Determination of trace amount of cobalt in feed grains and forages by solvent extraction and graphite furnace atomic absorption spectrometry.

    PubMed

    Blanchflower, W J; Cannavan, A; Kennedy, D G

    1990-10-01

    A method is described for the determination of trace amounts of cobalt in feed grains and forages with a detection limit of 1 ng g-1. Samples are ashed in a muffle furnace and complexed with 2-nitroso-1-naphthol. Following solvent extraction, cobalt is determined using graphite furnace atomic absorption spectrometry. The assay can be carried out in a normal analytical laboratory without the need for special "clean" rooms. Reagents have been selected to keep reagent blank values at low levels, and heptan-2-one is used as extracting solvent to avoid problems with evaporation. The assay has been used for diagnostic purposes and to formulate special low cobalt diets for sheep for experimental purposes. PMID:2270874

  6. Analysis of the Essential Nutrient Strontium in Marine Aquariums by Atomic Absorption Spectroscopy: An Undergraduate Analytical Chemistry Laboratory Exercise

    NASA Astrophysics Data System (ADS)

    Gilles de Pelichy, Laurent D.; Adam, Carl; Smith, Eugene T.

    1997-10-01

    An undergraduate atomic absorption spectroscopy (AAS) laboratory experiment is presented involving the analysis of the essential nutrient strontium in a real-life sample, sea water. The quantitative analysis of strontium in sea water is a problem well suited for an undergraduate analytical chemistry laboratory. Sea water contains numerous components which prevent the direct quantitative determination of strontium. Students learn first hand about the role of interferences in analytical measurements, and about the method of standard addition which is used to minimize these effects. This laboratory exercise also introduces undergraduate students to practical problems associated with AAS. We encourage students as a part of this experiment to collect and analyze marine water samples from local pet shops.

  7. Determination of total mercury in environmental and biological samples by flow injection cold vapour atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Murphy, James; Jones, Phil; Hill, Steve J.

    1996-12-01

    A simple and accurate method has been developed for the determination of total mercury in environmental and biological samples. The method utilises an off-line microwave digestion stage followed by analysis using a flow injection system with detection by cold vapour atomic absorption spectrometry. The method has been validated using two certified reference materials (DORM-1 dogfish and MESS-2 estuarine sediment) and the results agreed well with the certified values. A detection limit of 0.2 ng g -1 Hg was obtained and no significant interference was observed. The method was finally applied to the determination of mercury in river sediments and canned tuna fish, and gave results in the range 0.1-3.0 mg kg -1.

  8. Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Peng, Jin-feng; Liu, Rui; Liu, Jing-fu; He, Bin; Hu, Xia-lin; Jiang, Gui-bin

    2007-05-01

    A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO 3 that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L - 1 ) and a relative standard deviation (2.5% at 50 ng L - 1 level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L - 1 and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples.

  9. Low-volume, high-sensitivity assay for cadmium in blood and urine using conventional atomic absorption spectrophotometry.

    SciTech Connect

    Cerny, E. A.; Bhattacharyya, M. H.; Biosciences Division

    2003-03-15

    An assay for cadmium in whole blood and urine using deuterium background-correction electrothermal atomic absorption spectroscopy (D2-ETAAS) was developed. Cadmium (in a 1- to 2-ml sample) was bound to 15 mg anion-exchange resin, interfering ions were removed in a 2-ml Bio-Spin column, and cadmium was extracted into 100 {mu}l 1 M nitric acid for analysis. Cadmium in the sample extract was concentrated 7-fold for blood and 10-fold for urine over the starting material. These steps produced cadmium atomic absorption traces with high signal to background ratios and allowed analysis against aqueous standards. At {approx}0.1 ng Cd/ml, mean intra- and interassay coefficients of variation were 11-12%. Cadmium recovery for 0.1 to 0.6 ng added cadmium was 107{+-}4% for blood and 94{+-}4% for urine (mean{+-}SE, n=3). The mean detection limit (mean + 3x SD of blank) was 0.008 ng/ml for blood and 0.003 ng/ml for urine. Samples from 'unexposed' animals including humans ranged from 0.051{+-}0.000 to 0.229{+-}0.035 ng/ml. Values were approximately 10-fold lower than those obtained by the method of Stoeppler and Brandt using Zeeman background-correction ETAAS. This new high-sensitivity, low-volume assay will be useful for epidemiological studies, even those involving children, and will provide a means to help determine the contribution of cadmium to disease incidence in the general population.

  10. Determination of mercury in gasoline by cold vapor atomic absorption spectrometry with direct reduction in microemulsion media

    NASA Astrophysics Data System (ADS)

    Brandão, Geisamanda Pedrini; de Campos, Reinaldo Calixto; Luna, Aderval Severino

    2005-06-01

    The determination of Hg in gasoline by cold vapor atomic absorption spectrometry, after direct aqueous NaBH 4 reduction in a three-component (microemulsion) medium, was investigated. Microemulsions were prepared by mixing gasoline with propan-1-ol and 50% v / v HNO 3 at a 20 : 15 : 1 volume ratio. A long-term homogeneous system was immediately formed this way. After reduction, the Hg vapor generated in a reaction flask was transported to an intermediate K 2Cr 2O 7/H 2SO 4 trap solution in order to avoid poisoning of the Au-Pt trap by the gasoline vapors. A second reduction step was then conducted and the generated Hg vapor transported to the Au-Pt trap, followed by thermal release of Hg 0 and atomic absorption measurement. Purified N 2 was used as purge and transport gas. After multivariate optimization by central composite design calibration graphs showed coefficients of correlation of 0.9999 and a characteristic mass of 2 ng was obtained. Typical coefficients of variation of 5% and 6% were found for ten consecutive measurements at concentration levels of 1 and 8 μg L -1 of Hg 2+, respectively. The limit of detection was 0.10 μg L -1 (0.14 μg kg -1) in the original sample. A total measurement cycle took 11 min, permitting duplicate analysis of 3 samples per hour. The results obtained with the proposed procedure in the analysis of commercial gasoline samples were in agreement with those obtained by a comparative procedure. Gasoline samples of the Rio de Janeiro city have shown Hg concentrations below 0.27 μg L -1.

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

    PubMed

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

    2015-05-01

    A simple and expeditious analytical method for determination of zinc in human insulin isophane suspension by flame atomic absorption spectrophotometer (FAAS) was validated. The method was carried out on atomic absorption spectrometer with 0.4 nm bandwidth, 1.0 filter factor on deuterium (D2) background correction. The integration time was set at 3.0 second with 5.0 mA lamp current. The parameters of method validation showed adequate linearity, efficiency and relative standard deviation values were between 0.64%-1.69% (n=7), 1.31%-1.58% (n=10) for repeatability and intermediate precision respectively. The limit of detection 0.0032 μg/mL, 0.0173 μg/mL, 0.0231 μg/mL and limit of quantitation 0.0107μg/mL, 0.0578 μg/mL, 0.0694 μg/mL based on signal to noise (SN), calibration curve method (CCM) and fortification of blank (FB) were obtained respectively. The percentages of recovery for low, medium and high spiked concentration levels of zinc in human insulin were 99.38 ± 0.04 to 100.3 ± 0.03, 98.45 ± 0.38 to 100.3 ± 0.07 and 99.42 ± 0.03 to 99.42 ± 0.08 respectively. With the use of this method, five samples from each vial of human insulin isophane suspension were analyzed and the zinc content was determined. The zinc content were 22.1 ± 0.025 μg/mL and 24.3 ± 0.028 μg/mL which compliance the British Pharmacopoeia standard. PMID:26004720

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

    NASA Astrophysics Data System (ADS)

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

    2005-06-01

    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.

  13. Application of wavelet transforms to determine peak shape parameters for interference detection in graphite-furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Sadler, D. A.; Littlejohn, D.; Boulo, P. R.; Soraghan, J. S.

    1998-08-01

    A procedure to quantify the shape of the absorbance-time profile, obtained during graphite furnace atomic absorption spectrometry, has been used to detect interference effects caused by the presence of a concomitant salt. The quantification of the absorption profile is achieved through the use of the Lipschitz regularity, α0, obtained from the wavelet transform of the absorbance-time profile. The temporal position of certain features and their associated values of α0 provide a unique description of the shape of the absorbance-time profile. Changes to the position or values of α0 between standard and sample atomizations may be indicative of uncorrected interference effects. A weak, but linear, dependence was found of the value of α0 upon the analyte concentration for Cr and Cu. The ability of the Lipschitz regularity to detect interference effects was illustrated for Pb, Se and Cu. For Pb, the lowest concentration of NaCl added, 0.005% m/v, changed both the values of α0 and the peak height absorbance. For Se, no change in the peak height and peak area absorbance signals was detected up to a NaCl concentration of 0.25% m/v. The values of the associated Lipschitz regularities were found to be invariant to NaCl concentration up to this value. For Cu, a concentration of 0.05% m/v NaCl reduced the peak height and peak area absorbance signals by approximately 25% and significantly altered the values of α0.

  14. Determination of boron in blood, urine and bone by electrothermal atomic absorption spectrometry using zirconium and citric acid as modifiers

    NASA Astrophysics Data System (ADS)

    Burguera, Marcela; Burguera, José Luis; Rondón, Carlos; Carrero, Pablo

    2001-10-01

    A comparative study of various potential chemical modifiers (Au, Ba, Be, Ca, Cr, Ir, La, Lu, Mg, Ni, Pd, Pt, Rh, Ru, Sr, V, W, and Zr), and different 'coating' treatments (Zr, W, and W+Rh) of the pyrolytic graphite platform of a longitudinally heated graphite tube atomizer for thermal stabilization and determination of boron was undertaken. The use of Au, Ba, Be, Cr, Ir, Pt, Rh, Ru, Sr and V as modifiers, and of W+Rh coating produced erratic, and noisy signals, while the addition of La, Ni and Pd as modifiers, and the W coating had positive effects, but with too high background absorption signals, rendering their use unsuitable for boron determination even in aqueous solutions. The atomic absorption signal for boron was increased and stabilized when the platform was coated with Zr, and by the addition of Ca, Mg, Lu, W or Zr as modifiers. Only the addition of 10 μg of Zr as a modifier onto Zr-treated platforms allowed the use of a higher pyrolysis temperature without analyte losses. The memory effect was minimized by incorporating a cleaning step with 10 μl of 50 g l -1 NH 4F HF after every three boron measurements. The addition of 10 μl of 15 g l -1 citric acid together with Zr onto Zr-treated platforms significantly improved the characteristic mass to m0=282 pg, which is adequate for biological samples such as urine and bone, although the sensitivity was still inadequate for the determination of boron in blood of subjects without supplementary diet. Under optimized conditions, the detection limit (3σ) was 60 μg l -1. The amount of boron found in whole blood, urine and femur head samples from patients with osteoporosis was in agreement with values previously reported in the literature.

  15. Particular problems encountered in trace metal analysis of plant material by atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hoenig, M.; de Borger, R.

    Various mineralization methods for plant material analysis by AAS are presented and their advantages and limits are discussed. Wet digestion by H 2SO 4HNO 3H 2O 2 mixture appears as a very rapid method which gives good recovery of trace elements and is thus suitable for routine analysis. Determination of relatively high concentrations of Cu, Zn, Fe, Mn, Ni, Cr, Co, Cd, Pb, As, Sb and Tl is carried out by flame AAS with a good analytical speed and without noticeable interferences. Pb, Cd, As, Sb and Tl appear generally in very low concentrations in plants so that electrothermal atomization is necessary. Various interferences are observed in this case. They are discussed and methods are presented for their correction.

  16. Flame and flameless atomic-absorption determination of tellurium in geological materials

    USGS Publications Warehouse

    Chao, T.T.; Sanzolone, R.F.; Hubert, A.E.

    1978-01-01

    The sample is digested with a solution of hydrobromic acid and bromine and the excess of bromine is expelled. After dilution of the solution to approximately 3 M in hydrobromic acid, ascorbic acid is added to reduce iron(III) before extraction of tellurium into methyl isobutyl ketone (MIBK). An oxidizing air-acetylene flame is used to determine tellurium in the 0.1-20 ppm range. For samples containing 4-200 ppb of tellurium, a carbon-rod atomizer is used after the MIBK extract has been washed with 0.5 M hydrobromic acid to remove the residual iron. The flame procedure is useful for rapid preliminary monitoring, and the flameless procedure can determine tellurium at very low concentrations. ?? 1978.

  17. Determination of total tin in geological materials by electrothermal atomic-absorption spectrophotometry using a tungsten-impregnated graphite furnace

    USGS Publications Warehouse

    Zhou, L.; Chao, T.T.; Meier, A.L.

    1984-01-01

    An electrothermal atomic-absorption spectrophotometric method is described for the determination of total tin in geological materials, with use of a tungsten-impregnated graphite furnace. The sample is decomposed by fusion with lithium metaborate and the melt is dissolved in 10% hydrochloric acid. Tin is then extracted into trioctylphosphine oxide-methyl isobutyl ketone prior to atomization. Impregnation of the furnace with a sodium tungstate solution increases the sensitivity of the determination and improves the precision of the results. The limits of determination are 0.5-20 ppm of tin in the sample. Higher tin values can be determined by dilution of the extract. Replicate analyses of eighteen geological reference samples with diverse matrices gave relative standard deviations ranging from 2.0 to 10.8% with an average of 4.6%. Average tin values for reference samples were in general agreement with, but more precise than, those reported by others. Apparent recoveries of tin added to various samples ranged from 95 to 111% with an average of 102%. ?? 1984.

  18. Evaluation of ammonia as diluent for serum sample preparation and determination of selenium by graphite furnace atomic absorption spectrometry*1

    NASA Astrophysics Data System (ADS)

    Hernández-Caraballo, Edwin A.; Burguera, Marcela; Burguera, José L.

    2002-12-01

    A method for the determination of total selenium in serum samples by graphite furnace atomic absorption spectrometry was evaluated. The method involved direct introduction of 1:5 diluted serum samples (1% v/v NH 4OH+0.05% w/v Triton X-100 ®) into transversely heated graphite tubes, and the use of 10 μg Pd+3 μg Mg(NO 3) 2 as chemical modifier. Optimization of the modifier mass and the atomization temperature was conducted by simultaneously varying such parameters and evaluating both the integrated absorbance and the peak height/peak area ratio. The latter allowed the selection of compromise conditions rendering good sensitivity and adequate analyte peak profiles. A characteristic mass of 49 pg and a detection limit (3s) of 6 μg 1 -1 Se, corresponding to 30 μg l -1 Se in the serum sample, were obtained. The analyte addition technique was used for calibration. The accuracy was assessed by the determination of total selenium in Seronorm™ Trace Elements Serum Batch 116 (Nycomed Pharma AS). The method was applied for the determination of total selenium in ten serum samples taken from individuals with no known physical affection. The selenium concentration ranged between 79 and 147 μg l -1, with a mean value of 114±22 μg l -1.

  19. Investigation of lead contents in lipsticks by solid sampling high resolution continuum source electrothermal atomic absorption spectrometry.

    PubMed

    Gunduz, Sema; Akman, Suleyman

    2013-02-01

    In this study, the lead contents of different kinds of lipsticks were determined by solid sampling high resolution continuum source electrothermal atomic absorption spectrometry (SS-HR-CS ET AAS) and the results were compared with those obtained after microwave-assisted acid digestion of the samples. The experimental parameters for solid sampling such as the maximum amount of sample on the platforms of solid autosampler, graphite furnace program were optimized. Samples were directly loaded on the platforms of solid autosampler between 0.25 and 2.0mg and lead was determined applying 800 °C for pyrolysis and 2100 °C for atomization. Under optimized conditions, interference-free determination could be performed using aqueous standards. The LOD and the characteristic mass were 21.3 and 12.6 pg, respectively. The lead in the same lipstick samples was determined after microwave-assisted acid digestion and compared with those found by solid sampling. Mostly, there was no significant difference between the lead concentrations found by the two techniques. The lead in 25 lipstick samples with different properties were 0.11-4.48 ng mg(-1) which were not significantly different from those (<0.026-7.19 ng mg(-1)) reported by FDA for around 400 samples. PMID:23099440

  20. The application of atomic absorption spectrometry for the determination of residual active pharmaceutical ingredients in cleaning validation samples.

    PubMed

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

    2011-03-01

    The objective of this work was the development and validation of atomic absorption spectrometric (AAS) methods for the determination of residual active pharmaceutical ingredients (API) in rinse samples for cleaning validation. AAS as an indirect method for the determination of API in rinse samples can be applied when it is in the form of salt with metal ions or when the metal ion is a part of the API's structure. The electrothermal AAS methods (aqueous and ethanol medium) for the determination of magnesium in esomeprazole magnesium and the flame AAS method for the determination of lithium in lithium carbonate in rinse samples were developed. Various combinations of solvents were tested and a combination of 1% aqueous or ethanol solution of nitric acid for esomeprazole magnesium and 0.1% aqueous solution of nitric acid for lithium carbonate were found to be the most suitable. The atomization conditions in the graphite furnace and in the flame were carefully studied to avoid losses of analyte and to achieve suitable sensitivity. The cleaning verification methods were validated with respect to accuracy, precision, linearity, limit of detection, and quantification. In all the cases, the limits of detection were at the microgram level. The methods were successfully applied for the determination of esomeprazole magnesium and lithium carbonate in rinse samples from cleaning procedures. PMID:20923390

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

    PubMed

    Dobrowolski, Ryszard; Adamczyk, Agnieszka; Otto, Magdalena

    2013-09-15

    A new analytical procedure for vanadium (V) determination in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry (slurry sampling GFAAS) using the mixed permanent modifiers is described. Moreover, the comparison of action of the modifiers based on the iridium (Ir) and carbide-forming elements: tungsten (W) and niobium (Nb) deposited on the graphite tubes is studied, especially in terms of their analytical utility and determination sensitivity. The mechanism of their action was investigated using an X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray detector (EDX). Finally, the mixture of 0.3 μg of Ir and 0.04 μg of Nb was used for the graphite tube permanent modification. The analytical procedure was optimized on the basis of the data from pyrolysis and atomization temperature curves studies. The results obtained for the four certified reference materials (marine sediments: PACS-1 and MESS-1, lake sediment: SL-1, soil: San Joaquin Soil SRM 2709), using the slurry sampling GFAAS and the standard calibration method, were in good agreement with the certified values. The detection and quantification limits and characteristic mass calculated for the proposed procedure were 0.04 µg/g, 0.16 µg/g and 11.9 pg, respectively. The precision (RSD% less than 8%) and the accuracy of vanadium determination in the soil and sediment samples were acceptable. PMID:23708618

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

    PubMed

    Dobrowolski, Ryszard; Dobrzyńska, Joanna; Gawrońska, Barbara

    2015-01-01

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

  3. Determination of cadmium, aluminium, and copper in beer and products used in its manufacture by electrothermal atomic absorption spectrometry.

    PubMed

    Viñas, Pilar; Aguinaga, Nerea; López-García, Ignacio; Hernandez-Córdoba, Manuel

    2002-01-01

    Procedures were developed for determining cadmium, aluminium, and copper in beer and the products used in its manufacture by electrothermal atomic absorption spectrometry. Beer samples were injected into the furnace and solid samples were introduced as suspensions after preparation in a medium containing hydrogen peroxide, nitric acid, and ammonium dihydrogen phosphate for cadmium atomization. Calibration was performed with aqueous standards, and characteristic masses and detection limits were, respectively, 1 and 0.3 pg for cadmium, 18 and 5.4 pg for aluminium, and 5.6 and 6.8 pg for copper. Different samples of beer, wort, brewer's yeast, malt, raw grain, and hops were analyzed by the proposed procedures. Cadmium was found in low concentrations (0.001-0.08 microg/g and 0-1.3 ng/mL); copper (3-13 microg/g and 25-137 ng/mL) and aluminium (0.6-9 microg/g and 0.1-2 microg/mL) were found at higher levels. The reliability of the procedure was confirmed by comparing the results obtained with others based on microwave oven sample digestion, and by analyzing several certified reference materials. PMID:12083268

  4. Compartmentalization of trace elements in guinea pig tissues by INAA (instrumental neutron activation analysis) and AAS (atomic absorption spectroscopy)

    SciTech Connect

    Chatt, A.; Holzbecher, J.; Katz, S.A.

    1988-01-01

    Human scalp hair analysis has received considerable attention from a variety of disciplines over the last 20 yr or so. Trace element levels of hair have been used in environmental, epidemiological, forensic, nutritional, predictive, and preventive medicine studies. There still exist confusion, skepticism, and controversy, however, among the experts as well as lay persons in the interpretation of hair trace element data. Much of the criticism stems from the lack of quantitative and reliable data on the ability of hair to accurately reflect dose-response relationships. To better define the significance or hair trace element levels (under the auspices of the International Atomic Energy Agency), the authors have undertaken a controlled set of animal experiments in which trace element levels in hair and other tissues have been measured after a mild state of systemic intoxication by chronic, low-does exposure to cadmium and selenium. Instrumental neutron activation analysis (INAA) and atomic absorption spectroscopy (AAS) methods have been developed for the determination of several elements with a high degree of precision and accuracy.

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

    PubMed

    Matos, Geraldo Domingues; Arruda, Marco Aurélio Zezzi

    2008-07-15

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

  6. Beyond the single-atom response in absorption line shapes: probing a dense, laser-dressed helium gas with attosecond pulse trains.

    PubMed

    Liao, Chen-Ting; Sandhu, Arvinder; Camp, Seth; Schafer, Kenneth J; Gaarde, Mette B

    2015-04-10

    We investigate the absorption line shapes of laser-dressed atoms beyond the single-atom response, by using extreme ultraviolet (XUV) attosecond pulse trains to probe an optically thick helium target under the influence of a strong infrared (IR) field. We study the interplay between the IR-induced phase shift of the microscopic time-dependent dipole moment and the resonant-propagation-induced reshaping of the macroscopic XUV pulse. Our experimental and theoretical results show that as the optical depth increases, this interplay leads initially to a broadening of the IR-modified line shape, and subsequently, to the appearance of new, narrow features in the absorption line. PMID:25910116

  7. Unraveling the Solid-Liquid-Vapor Phase Transition Dynamics at the Atomic Level with Ultrafast X-Ray Absorption Near-Edge Spectroscopy

    NASA Astrophysics Data System (ADS)

    Dorchies, F.; Lévy, A.; Goyon, C.; Combis, P.; Descamps, D.; Fourment, C.; Harmand, M.; Hulin, S.; Leguay, P. M.; Petit, S.; Peyrusse, O.; Santos, J. J.

    2011-12-01

    X-ray absorption near-edge spectroscopy (XANES) is a powerful probe of electronic and atomic structures in various media, ranging from molecules to condensed matter. We show how ultrafast time resolution opens new possibilities to investigate highly nonequilibrium states of matter including phase transitions. Based on a tabletop laser-plasma ultrafast x-ray source, we have performed a time-resolved (˜3ps) XANES experiment that reveals the evolution of an aluminum foil at the atomic level, when undergoing ultrafast laser heating and ablation. X-ray absorption spectra highlight an ultrafast transition from the crystalline solid to the disordered liquid followed by a progressive transition of the delocalized valence electronic structure (metal) down to localized atomic orbitals (nonmetal—vapor), as the average distance between atoms increases.

  8. Determination of trace amounts of gold in acid-attacked environmental samples by atomic absorption spectrometry with electrothermal atomization after preconcentration.

    PubMed

    Medved, Ján; Bujdos, Marek; Matús, Peter; Kubová, Jana

    2004-05-01

    A method for determination of trace amounts of gold in environmental samples (rocks, soils, sediments, and waters) by atomic absorption spectrometry with electrothermal atomization (ETAAS) after preconcentration using a chelating sorbent Spheron Thiol 1000 is described. The method accurately determines gold between 0.001 and several tens of grams per ton in samples having complex variations in mineralogy. Pulverized samples are roasted at 650 degrees C to oxidize any sulfide and/or carbonaceous material. Samples are then subjected to a series of acid treatments to eliminate any silica matrix and to dissolve the sample. The Spheron Thiol 1000 is added to the sample solution, and then with sorbed gold is filtered out, washed, and ignited at 550 degrees C. The residue is dissolved in aqua regia, evaporated, dissolved in distilled water, transferred to a volumetric flask, and analyzed by ETAAS. The limits of detection of gold, based on the 3 sigma definition, were 0.5 ng g(-1) for 10-g samples (rocks, sediments, soils) and 0.05 ng mL(-1) for 1-L water samples. Precision of determination expressed by the relative standard deviation varied from 2.9% to 16.4%. The accuracy of the method is verified by analysis of certified reference materials. The obtained analytical results are in good agreement with attested values. The developed method was applied for gold determination in environmental samples affected by the acidification (acid mine drainage which is mainly a product of pyrite oxidation) from an open quartzite mine in the Sobov region situated NE of the city of Banská Stiavnica (Slovakia). PMID:14997262

  9. Cloud point extraction for the determination of cadmium and lead in biological samples by graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Maranhão, Tatiane De A.; Borges, Daniel L. G.; da Veiga, Márcia A. M. S.; Curtius, Adilson J.

    2005-06-01

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 °C for both elements and atomization temperatures of 1400 and 1600 °C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3σB) of 6 and 40 ng g-1, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H2O2 and HNO3. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated.

  10. Local surrounding of vanadium atoms in CuCr1 - x V x S2: X-ray absorption spectroscopy analysis

    NASA Astrophysics Data System (ADS)

    Smirnova, Yu. O.; Smolentsev, N. Yu.; Guda, A. A.; Soldatov, M. A.; Kvashnina, K. O.; Glatzel, P.; Korotaev, E. V.; Soldatov, A. V.; Mazalov, L. N.

    2013-03-01

    In the present work local surrounding of vanadium atoms in layered copper-chromium disulfides CuCr1 - x V x S2 is investigated using high-resolution X-ray absorption spectroscopy above vanadium K-edge. Based on experimental and theoretically simulated spectra comparison it is shown that vanadium atoms replace chromium ones even at high concentrations of vanadium and that they are in 3+ oxidation state.

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

    NASA Astrophysics Data System (ADS)

    Kruger, Pamela C.; Parsons, Patrick J.

    2007-03-01

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

  12. The Use of a Microprocessor-Controlled, Video Output Atomic Absorption Spectrometer as an Educational Tool in a Two-Year Technical Curriculum.

    ERIC Educational Resources Information Center

    Kerfoot, Henry B.

    Based on instructional experiences at Charles County Community College, Maryland, this report examines the pedagogical advantage of teaching atomic absorption (AA) spectroscopy with an AA spectrophotometer that is equipped with a microprocessor and video output mechanism. The report first discusses the growing importance of AA spectroscopy in…

  13. Determination of Pb in Biological Samples by Graphite Furnace Atomic Absorption Spectrophotometry: An Exercise in Common Interferences and Fundamental Practices in Trace Element Determination

    ERIC Educational Resources Information Center

    Spudich, Thomas M.; Herrmann, Jennifer K.; Fietkau, Ronald; Edwards, Grant A.

    2004-01-01

    An experiment is conducted to ascertain trace-level Pb in samples of bovine liver or muscle by applying graphite furnace atomic absorption spectrophotometry (GFAAS). The primary objective is to display the effects of physical and spectral intrusions in determining trace elements, and project the usual methods employed to minimize accuracy errors…

  14. USEPA METHOD STUDY 38 - SW-846 METHOD 3010, ACID DIGESTION OF AQUEOUS SAMPLES AND EXTRACTS FOR TRACE METALS BY FLAME ATOMIC ABSORPTION SPECTROSCOPY

    EPA Science Inventory

    An interlaboratory collaborative study was conducted on SW-846 Method 3010, "Acid Digestion of Aqueous Samples and Extracts for Total Metals for Analysis by Flame Atomic Absorption Spectroscopy", to determine the mean recovery and precision for analyses of 21 trace metals in surf...

  15. SINGLE-LABORATORY EVALUATION OF SW-846 METHODS 7090/7091 DETERMINATION OF BERYLLIUM BY FLAME AND FURNACE ATOMIC ABSORPTION SPECTROPHOTOMETRY

    EPA Science Inventory

    The results of a single-laboratory study of the 'Determination of Beryllium by Flame and Furnace Atomic Absorption Spectrophotometry', are described. The study examined the application of these two powerful beryllium detection methods to the analysis of selected liquid and solid ...

  16. Picosecond-TALIF and VUV absorption measurements of absolute atomic nitrogen densities from an RF atmospheric pressure plasma jet with He/O2/N2 gas mixtures

    NASA Astrophysics Data System (ADS)

    West, Andrew; Niemi, Kari; Schröter, Sandra; Bredin, Jerome; Gans, Timo; Wagenaars, Erik

    2015-09-01

    Reactive Oxygen and Nitrogen species (RONS) from RF atmospheric pressure plasma jets (APPJs) are important in biomedical applications as well as industrial plasma processing such as surface modification. Atomic oxygen has been well studied, whereas, despite its importance in the plasma chemistry, atomic nitrogen has been somewhat neglected due to its difficulty of measurement. We present absolute densities of atomic nitrogen in APPJs operating with He/O2/N2 gas mixtures in open air, using picosecond Two-photon Absorption Laser Induced Fluorescence (ps-TALIF) and vacuum ultra-violet (VUV) absorption spectroscopy. In order to apply the TALIF technique in complex, He/O2/N2 mixtures, we needed to directly measure the collisional quenching effects using picosecond pulse widths (32ps). Traditional calculated quenching corrections, used in nanosecond TALIF, are inadequate due to a lack of quenching data for complex mixtures. Absolute values for the densities were found by calibrating against a known density of Krypton. The VUV absorption experiments were conducted on the DESIRS synchrotron beamline using a unique VUV Fourier-transform spectrometer. Atomic nitrogen densities were on the order of 1020 m-3 with good agreement between TALIF and VUV absorption. UK EPSRC grant EP/K018388/1.

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  18. Determination of Fe Content of Some Food Items by Flame Atomic Absorption Spectroscopy (FAAS): A Guided-Inquiry Learning Experience in Instrumental Analysis Laboratory

    ERIC Educational Resources Information Center

    Fakayode, Sayo O.; King, Angela G.; Yakubu, Mamudu; Mohammed, Abdul K.; Pollard, David A.

    2012-01-01

    This article presents a guided-inquiry (GI) hands-on determination of Fe in food samples including plantains, spinach, lima beans, oatmeal, Frosted Flakes cereal (generic), tilapia fish, and chicken using flame atomic absorption spectroscopy (FAAS). The utility of the GI experiment, which is part of an instrumental analysis laboratory course,…

  19. Analysis of an Air Conditioning Coolant Solution for Metal Contamination Using Atomic Absorption Spectroscopy: An Undergraduate Instrumental Analysis Exercise Simulating an Industrial Assignment

    ERIC Educational Resources Information Center

    Baird, Michael J.

    2004-01-01

    A real-life analytical assignment is presented to students, who had to examine an air conditioning coolant solution for metal contamination using an atomic absorption spectroscopy (AAS). This hands-on access to a real problem exposed the undergraduate students to the mechanism of AAS, and promoted participation in a simulated industrial activity.

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

    NASA Astrophysics Data System (ADS)

    van Dalen, Gerard; de Galan, Leo

    1994-12-01

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

  1. Determination of inorganic arsenic species by flow injection hydride generation atomic absorption spectrometry with variable sodium tetrahydroborate concentrations*1

    NASA Astrophysics Data System (ADS)

    Sigrist, Mirna E.; Beldoménico, Horacio R.

    2004-07-01

    This work describes a study on the determination of inorganic arsenic species in ground water and synthetic experimental matrices, using a flow injection system with on-line hydride generation device coupled to an atomic absorption spectrometer with flame-heated quartz atomizer (FI HG AAS). Specific trivalent arsenic determination is based on the slow kinetics of As(V) on the hydride generation reaction using sufficiently low concentrations of sodium tetrahydroborate (NaBH 4) as reductant in highly acidic conditions (pH<0). Under these conditions, the efficiency of hydride generation from As(V) is much lower than that from As(III). The pentavalent form is determined by the difference between total inorganic arsenic and As(III). As(V) interferences were studied using As(III) solutions ranging from 0% to 50% of total inorganic As. The optimized NaBH 4 concentration was 0.035% (w/v). The detection limit was 1.4 μg l -1 As(III). As(V) interferences were 6% in the case of water samples with 6 μg l -1 As(III) in the presence of 54 μg l -1 As(V) (i.e. 10% As(III)). Interferences of methylated arsenic species (MMA and DMA) were evaluated. Speciation method was satisfactorily applied to 20 field arsenical water samples from Santa Fe, Argentina, with values ranging from 30 to 308 μg l -1 total As. We found from 0% to 36% As(III) in the 20 field samples. The developed methodology constitutes an economic, simple and reliable way to evaluate inorganic arsenic distribution in underground waters or similar systems with negligible or no content of organoarsenicals.

  2. Absolute atomic oxygen and nitrogen densities in radio-frequency driven atmospheric pressure cold plasmas: Synchrotron vacuum ultra-violet high-resolution Fourier-transform absorption measurements

    SciTech Connect

    Niemi, K.; O'Connell, D.; Gans, T.; Oliveira, N. de; Joyeux, D.; Nahon, L.; Booth, J. P.

    2013-07-15

    Reactive atomic species play a key role in emerging cold atmospheric pressure plasma applications, in particular, in plasma medicine. Absolute densities of atomic oxygen and atomic nitrogen were measured in a radio-frequency driven non-equilibrium plasma operated at atmospheric pressure using vacuum ultra-violet (VUV) absorption spectroscopy. The experiment was conducted on the DESIRS synchrotron beamline using a unique VUV Fourier-transform spectrometer. Measurements were carried out in plasmas operated in helium with air-like N{sub 2}/O{sub 2} (4:1) admixtures. A maximum in the O-atom concentration of (9.1 {+-} 0.7) Multiplication-Sign 10{sup 20} m{sup -3} was found at admixtures of 0.35 vol. %, while the N-atom concentration exhibits a maximum of (5.7 {+-} 0.4) Multiplication-Sign 10{sup 19} m{sup -3} at 0.1 vol. %.

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

    NASA Astrophysics Data System (ADS)

    Mora, Juan; Canals, Antonio; Hernandis, Vicente

    1996-10-01

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

  4. Atomic-absorption spectrometric determination of cobalt, nickel, and copper in geological materials with matrix masking and chelation-extraction

    USGS Publications Warehouse

    Sanzolone, R.F.; Chao, T.T.; Crenshaw, G.L.

    1979-01-01

    An atomic-absorption spectrometric method is reported for the determination of cobalt, nickel, and copper in a variety of geological materials including iron- and manganese-rich, and calcareous samples. The sample is decomposed with HP-HNO3 and the residue is dissolved in hydrochloric acid. Ammonium fluoride is added to mask iron and 'aluminum. After adjustment to pH 6, cobalt, nickel, and copper are chelated with sodium diethyl-dithiocarbamate and extracted into methyl isobutyl ketone. The sample is set aside for 24 h before analysis to remove interferences from manganese. For a 0.200-g sample, the limits of determination are 5-1000 ppm for Co, Ni, and Cu. As much as 50% Fe, 25% Mn or Ca, 20% Al and 10% Na, K, or Mg in the sample either individually or in various combinations do not interfere. Results obtained on five U.S. Geological Survey rock standards are in general agreement with values reported in the literature. ?? 1979.

  5. Electrothermal atomic absorption spectrometric determination of copper in nickel-base alloys with various chemical modifiers*1

    NASA Astrophysics Data System (ADS)

    Tsai, Suh-Jen Jane; Shiue, Chia-Chann; Chang, Shiow-Ing

    1997-07-01

    The analytical characteristics of copper in nickel-base alloys have been investigated with electrothermal atomic absorption spectrometry. Deuterium background correction was employed. The effects of various chemical modifiers on the analysis of copper were investigated. Organic modifiers which included 2-(5-bromo-2-pyridylazo)-5-(diethylamino-phenol) (Br-PADAP), ammonium citrate, 1-(2-pyridylazo)-naphthol, 4-(2-pyridylazo)resorcinol, ethylenediaminetetraacetic acid and Triton X-100 were studied. Inorganic modifiers palladium nitrate, magnesium nitrate, aluminum chloride, ammonium dihydrogen phosphate, hydrogen peroxide and potassium nitrate were also applied in this work. In addition, zirconium hydroxide and ammonium hydroxide precipitation methods have also been studied. Interference effects were effectively reduced with Br-PADAP modifier. Aqueous standards were used to construct the calibration curves. The detection limit was 1.9 pg. Standard reference materials of nickel-base alloys were used to evaluate the accuracy of the proposed method. The copper contents determined with the proposed method agreed closely with the certified values of the reference materials. The recoveries were within the range 90-100% with relative standard deviation of less than 10%. Good precision was obtained.

  6. The determination of wear metals in used lubricating oils by flame atomic absorption spectrometry using sulphanilic acid as ashing agent.

    PubMed

    Ekanem, E J; Lori, J A; Thomas, S A

    1997-11-01

    A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of calcium, magnesium, zinc, iron, chromium and nickel by flame atomic absorption spectrometry. Sulphanilic acid was added to oil samples and the mixture coked and the coke ashed at 550 degrees C. The solutions of the ash were analysed by flame AAS for the metals. The release of calcium, zinc, iron and chromium was improved by the addition of sulphanilic acid to samples. The relative standard deviations of metal concentration results in the initial oil samples were 1.5% for Ca (1500 mg l(-1) level), 0.3% for Mg (100 mg l(-1) level), 3.1% for Zn (1500 mg l(-1) level), 0.7% for Fe (500 mg l(-1) level), 0.02% for Cr (50 mg l(-1) level) and 0.002% for Ni (10 mg l(-1) level). The optimum sample size for efficient metal release was 20 g while the optimum sulphanilic acid to oil ratio was 0.05 g per gram of oil for Zn and Cr and 0.10 g for Ca and Fe. Results obtained by this procedure were highly reproducible and comparable with those obtained for the same samples using standard procedures. PMID:18966959

  7. Evaluation of four sample treatments for determination of platinum in automotive catalytic converters by graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Puig, Ana I.; Alvarado, José I.

    2006-09-01

    Conventional and microwave assisted digestion, both using aqua regia, alkaline fusion with lithium metaborate and aqueous slurries were evaluated as sample treatments for determination of Pt in automotive catalytic converters by Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). Determination of platinum by GF-AAS in samples of the catalytic converter's substrates, prepared by the four methods described, indicates that the highest platinum concentration i.e. maximum Pt extraction in the range of 748 ± 15-998 ± 10 μg mL - 1 , is obtained for samples dissolved by alkaline fusion, closely followed by analysis of aqueous plus Triton X-100 slurries 708 ± 14-958 ± 10 μg mL - 1 , while neither one of the acid digestion procedures achieved total dissolution of the samples. Slurry analysis is thus shown to be a viable alternative and is recommended, based on its speed and ease of implementation. Aqueous standards calibration curves and the standard addition methods were also compared. The results showed that no appreciable matrix effects are present, regardless of the sample preparation procedure used. Precision of the measurements, expressed as percentage relative standard deviation, ranged between 2.5 to 4.9%. Accuracy of the results was assessed by recovery tests which rendered values between 98.9 and 100.9%.

  8. Quantification of minerals and trace elements in raw caprine milk using flame atomic absorption spectrophotometry and flame photometry.

    PubMed

    Singh, Mahavir; Yadav, Poonam; Garg, V K; Sharma, Anshu; Singh, Balvinder; Sharma, Himanshu

    2015-08-01

    This study reports minerals and trace elements quantification in raw caprine milk of Beetal breed, reared in Northern India and their feed, fodder & water using flame atomic absorption spectrophotometry and flame photometry. The mineral and trace elements' concentration in the milk was in the order: K > Ca > Na > Fe > Zn > Cu. The results showed that minerals concentration in caprine milk was lesser than reference values. But trace elements concentration (Fe and Zn) was higher than reference values. Multivariate statistical techniques, viz., Pearsons' correlation, Cluster analysis (CA) and Principal component analysis (PCA) were applied to analyze the interdependences within studied variables in caprine milk. Significantly positive correlations were observed between Fe - Zn, Zn - K, Ca - Na and Ca - pH. The results of correlation matrix were further supported by Cluster analysis and Principal component analysis as primary cluster pairs were found for Ca - pH, Ca - Na and Fe - Zn in the raw milk. No correlation was found between mineral & trace elements content of the milk and feed. PMID:26243956

  9. Extension of working range in Zeeman graphite furnace atomic absorption spectrometry by nonlinear calibration with prior correction for stray light

    NASA Astrophysics Data System (ADS)

    Lonardo, Robert F.; Yuzefovsky, Alexander I.; Zhou, Jack X.; McCaffrey, John T.; Michel, Robert G.

    1996-09-01

    The nonlinear working range of a Perkin-Elmer 4100Zl atomic absorption spectrometer was improved in three steps. Firstly, each absorbance datum within the transient profile was corrected for the presence of stray light by an algorithm originally developed by L'vov and co-workers (Spectrochim. Acta Part B, 47 (1992) 889-895 and 1187-1202), but with the incorporation of the Newton method of successive approximations (Spectrochim. Acta Part B, 49 (1994) 1643-1656. Secondly, a dip correction procedure was performed on temporal signal profiles that exhibited a dip due to rollover. In the final step, an analytically useful working curve was generated by the nonlinear calibration routine of Barnett (Spectrochim. Acta Part B, 39 (1984) 829). Goodness of fit between the resultant calibration curve and the data was measured by the method suggested by Miller-Ihli et al. (Spectrochim. Acta Part B, 39 (1984) 1603) that is based on the sum of squares of the percentage deviation (SSPD) and the root mean square (RMS) percentage deviation. For lead, silver, copper, thallium, and cadmium, the analytical nonlinear working range was increased by as much as one and a half orders of magnitude, without any significant effect on the RMS. For chromium and manganese, no significant improvement in the nonlinear working range was observed, while the RMS improved by 50%. In the case of nickel, neither the working range nor the RMS was improved.

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

    NASA Astrophysics Data System (ADS)

    Woińska, Sylwia; Godlewska-Żyłkiewicz, Beata

    2011-07-01

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

  11. Determination of cadmium and lead in beverages after leaching from pewter cups using graphite furnace atomic absorption spectrometry.

    PubMed

    Dessuy, Morgana B; Vale, Maria Goreti R; Welz, Bernhard; Borges, Aline R; Silva, Márcia M; Martelli, Patrícia B

    2011-07-15

    Two simple methods have been developed to determine cadmium and lead in different kinds of beverages and vinegar leached from pewter cups produced in Brazil. Leaching experiments have been carried out with different solutions: beer, sugar cane spirit, red and white wine, vinegar and a 3% acetic acid solution. The solutions were kept in cups with and without solder for 24h. Lead and cadmium have been determined using graphite furnace atomic absorption spectrometry with deuterium background correction. The limits of detection were 0.05 and 1.4 μg L(-1), and the characteristic mass was 1.0 pg and 19 pg for Cd and Pb, respectively. With the developed methods it was possible to determine accurately cadmium and lead by direct analysis in these liquids and to evaluate the leaching of these metals from pewter cups. The results presented in this work show that pewter cups are not cadmium- and lead-free; this point goes against the manufacturers' declaration that their products are lead-free. PMID:21645758

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

    PubMed

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

    2013-01-01

    A simple method has been developed to determine antimony and lead in pewter alloy cups produced in Brazil, using fast sequential determination by high-resolution continuum source flame atomic absorption spectrometry. The samples were dissolved in HCl and H(2)O(2), employing a cold finger system in order to avoid analyte losses. The main resonance line of lead at 217.001 nm and a secondary line of antimony at 212.739 nm were used. The limits of detection for lead and antimony were 0.02 and 5.7 mg L(-1), respectively. The trueness of the method was established by recovery tests and comparing the results obtained by the proposed method with those obtained by inductively coupled plasma optical emission spectrometry. The results were compared using a student's t-test and there was no significant difference at a 95% confidence interval. With the developed methods, it was possible to determine accurately antimony and lead in pewter samples. The lead concentration found in the analysed samples was around 1 mg g(-1), which means that they are not lead free; however, the content was below the maximum allowed level of 5 mg g(-1). The antimony content, which was found to be between 40 and 46 mg g(-1), is actually of greater concern, as antimony is known to be potentially toxic already at very low concentrations, although there is no legislation yet for this element. PMID:23046152

  13. A study of mechanism of nickel interferences in hydride generation atomic absorption spectrometric determination of arsenic and antimony

    NASA Astrophysics Data System (ADS)

    Henden, Emur; İşlek, Yasemin; Kavas, Miray; Aksuner, Nur; Yayayürük, Onur; Çiftçi, Tülin Deniz; İlktaç, Raif

    2011-11-01

    Studies have been carried out to clarify the mechanism of nickel interferences in the hydride generation atomic absorption spectrometric determination of arsenic and antimony. The most serious nickel interferences are observed when nickel/nickel boride nanoparticles are produced during NaBH 4 reduction. In this study these particles have been observed to have diameters of less than 40 nm and sorb As(III), As(V) and Sb(III) species rather than arsine and stibine generated as so far assumed. Bulk chemical composition and surface structure of these nanoparticles were studied and it was found that if the NaBH 4 reduction is carried out while passing nitrogen through the solution the black nanoparticles were composed of Ni 2B and, if the reduction is carried out under air the black nanoparticles were found to consist of Ni 3B or possibly a mixture of Ni(0) and Ni 2B. Surface analysis studies with scanning electron microscopy, energy dispersive X-ray spectrometry, X-ray photoelectron spectrometry and X-ray diffraction analysis have shown that the particles have amorphous structure consisting of Ni(0), Ni 2B, Ni 3B and Ni(OH) 2. However, sorption studies have shown that Ni(0) and Ni(OH) 2 do not sorb the analyte ions and arsine and stibine significantly.

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

    PubMed

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

    2016-05-01

    This work describes a new method for the extraction and determination of gold nanoparticles in environmental samples by means of in-situ suspended aggregate microextraction and electrothermal atomic absorption spectrometry. The method relies on the in-situ formation of a supramolecular aggregate phase through ion-association between a cationic surfactant and a benzene sulfonic acid derivative. Gold nanoparticles are physically entrapped into the aggregate phase which is separated from the bulk aqueous solution by vacuum filtration on the surface of a cellulose filter in the form of a thin film. The film is removed from the filter surface and is dissociated into an acidified methanolic solution which is used for analysis. Under the optimized experimental conditions, gold nanoparticles can be efficiently extracted from water samples with recovery rates between 81.0-93.3%, precision 5.4-12.0% and detection limits as low as 75femtomolL(-1) using only 20mL of sample volume. The satisfactory analytical features of the method along with the simplicity indicate the efficiency of this new approach to adequately collect and extract gold nanoparticle species from water samples. PMID:26946014

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

    PubMed Central

    Chamsaz, Mahmoud; Akhoundzadeh, Jeiran; Arbab-zavar, Mohammad Hossein

    2012-01-01

    A simple microextraction method based on solidification of a floating organic drop (SFOD) was developed for preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Ammonium pyrolidinedithiocarbamate (APDC) was used as complexing agent, and the formed complex was extracted into a 20 μL of 1-undecanol. The extracted complex was diluted with ethanol and injected into a graphite furnace. An orthogonal array design (OAD) with OA16 (45) matrix was employed to study the effects of different parameters such as pH, APDC concentration, stirring rate, sample solution temperature and the exposure time on the extraction efficiency. Under the optimized experimental conditions the limit of detection (based on 3 s) and the enhancement factor were 0.058 μg L−1 and 113, respectively. The relative standard deviation (RSD) for 8 replicate determinations of 1 μg L−1 of Pb was 8.8%. The developed method was validated by the analysis of certified reference materials and was successfully applied to the determination of lead in water and infant formula base powder samples. PMID:25685441

  16. Fast determination of phosphorus in honey, milk and infant formulas by electrothermal atomic absorption spectrometry using a slurry sampling procedure

    NASA Astrophysics Data System (ADS)

    López-García, I.; Viñas, P.; Romero-Romero, R.; Hernández-Córdoba, M.

    2007-01-01

    A procedure for the electrothermal atomic absorption spectrometric determination of phosphorus in honey, milk and infant formulas using slurried samples is described. Suspensions prepared in a medium containing 50% v/v concentrated hydrogen peroxide, 1% v/v concentrated nitric acid, 10% m/v glucose, 5% m/v sucrose and 100 mg l - 1 of potassium were introduced directly into the furnace. For the honey samples, multiple injection of the sample was necessary. The modifier selected was a mixture of 20 μg palladium and 5 μg magnesium nitrate, which was injected after the sample and before proceeding with the drying and calcination steps. Calibration was performed using aqueous standards prepared in the same suspension medium and the graph was linear between 5 and 80 mg l - 1 of phosphorus. The reliability of the procedure was checked by comparing the results obtained by the new developed method with those found when using a reference spectrophotometric method after a mineralization step, and by analyzing several certified reference materials.

  17. Resonance absorption measurements of atom concentrations in reacting gas mixtures. III. Pyrolysis of CD/sub 4/ behind shock waves

    SciTech Connect

    Chiang, C.C.; Baker, J.A.; Skinner, G.B.

    1980-05-01

    Dilute mixtures (10 to 100 ppM) of CD/sub 4/ in argon were pyrolyzed behind reflected shock waves at temperatures of 1780 to 2440 K and total pressures of 2 to 3 atm. Progress of the reaction was followed by analysis for D atoms by using resonance absorption spectroscopy. Rate constants were determined as follows: CD/sub 4/ ..-->.. CD/sub 3/ + D, k/sub 1/ = 1.4 x 10/sup 11/ exp(-81000/RT) s/sup -1/; CD/sub 4/ + Ar ..-->.. CD/sub 3/ + D + Ar, k/sub 1a/ = 2.1 x 10/sup 16/ exp(-84900/RT) mol/sup -1/ cm/sup 3/ s/sup -1/; D + CD/sub 4/ ..-->.. D/sub 2/ + CD/sub 3/,k/sub 2/ = 2.1 x 10/sup 15/exp(-22300/RT) mol/sup -1/ cm/sup 3/ s/sup -1/, where activation energies are in calories. These data have been correlated with similar data by Roth and Just on pyrolysis of CH/sub 4/, with laser schlieren data by Tabayashi and Bauer on pyrolysis of CH/sub 4/ and CD/sub 4/, and with other data on CH/sub 4/ pyrolysis, via RRKM and activated complex theory calculations.

  18. Determination of nickel in water, food, and biological samples by electrothermal atomic absorption spectrometry after preconcentration on modified carbon nanotubes.

    PubMed

    Taher, Mohammad Ali; Mazaheri, Lida; Ashkenani, Hamid; Mohadesi, Alireza; Afzali, Daryoush

    2014-01-01

    A new and sensitive SPE method using modified carbon nanotubes for extraction and preconcentration, and electrothermal atomic absorption spectrometric determination of nickel (Ni) in real samples at ng/L levels was investigated. First, multiwalled carbon nanotubes were oxidized with concentrated HNO3, then modified with 2-(5-bormo-2-pyridylazo)-5-diethylaminophenol reagent. The adsorption was achieved quantitatively on a modified carbon nanotubes column in a pH range of 6.5 to 8.5; the adsorbed Ni(II) ions were then desorbed by passing 5.0 mL of 1 M HNO3. The effects of analytical parameters, including pH of the solution, eluent type and volume, sample volume, flow rate of the eluent, and matrix ions, were investigated for optimization of the presented procedure. The enrichment factor was 180, and the LOD for Ni was 4.9 ng/L. The method was applied to the determination of Ni in water, food, and biological samples, and reproducible results were obtained. PMID:24672882

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

    PubMed Central

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

    2011-01-01

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

  20. Determination of trace nickel in hydrogenated cottonseed oil by electrothermal atomic absorption spectrometry after microwave-assisted digestion.

    PubMed

    Zhang, Gai

    2012-01-01

    Microwave digestion of hydrogenated cottonseed oil prior to trace nickel determination by electrothermal atomic absorption spectrometry (ETAAS) is proposed here for the first time. Currently, the methods outlined in U.S. Pharmacopeia 28 (USP28) or British Pharmacopeia (BP2003) are recommended as the official methods for analyzing nickel in hydrogenated cottonseed oil. With these methods the samples may be pre-treated by a silica or a platinum crucible. However, the samples were easily tarnished during sample pretreatment when using a silica crucible. In contrast, when using a platinum crucible, hydrogenated cottonseed oil acting as a reducing material may react with the platinum and destroy the crucible. The proposed microwave-assisted digestion avoided tarnishing of sample in the process of sample pretreatment and also reduced the cycle of analysis. The programs of microwave digestion and the parameters of ETAAS were optimized. The accuracy of the proposed method was investigated by analyzing real samples. The results were compared with the ones by pressurized-PTFE-bomb acid digestion and ones obtained by the U.S. Pharmacopeia 28 (USP28) method. The new method involves a relatively rapid matrix destruction technique compared with other present methods for the quantification of metals in oil. PMID:22133102

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

    PubMed

    Hartmann, Georg; Schuster, Michael

    2013-01-25

    The determination of metallic nanoparticles in environmental samples requires sample pretreatment that ideally combines pre-concentration and species selectivity. With cloud point extraction (CPE) using the surfactant Triton X-114 we present a simple and cost effective separation technique that meets both criteria. Effective separation of ionic gold species and Au nanoparticles (Au-NPs) is achieved by using sodium thiosulphate as a complexing agent. The extraction efficiency for Au-NP ranged from 1.01 ± 0.06 (particle size 2 nm) to 0.52 ± 0.16 (particle size 150 nm). An enrichment factor of 80 and a low limit of detection of 5 ng L(-1) is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L(-1). The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L(-1) is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples. PMID:23312311

  2. An automatic countercurrent liquid-liquid micro-extraction system coupled with atomic absorption spectrometry for metal determination.

    PubMed

    Mitani, Constantina; Anthemidis, Aristidis N

    2015-02-01

    A novel and versatile automatic sequential injection countercurrent liquid-liquid microextraction (SI-CC-LLME) system coupled with atomic absorption spectrometry (FAAS) is presented for metal determination. The extraction procedure was based on the countercurrent flow of aqueous and organic phases which takes place into a newly designed lab made microextraction chamber. A noteworthy feature of the extraction chamber is that it can be utilized for organic solvents heavier or lighter than water. The proposed method was successfully demonstrated for on-line lead determination and applied in environmental water samples using an amount of 120 μL of chloroform as extractant and ammonium diethyldithiophosphate as chelating reagent. The effect of the major experimental parameters including the volume of extractant, as well as the flow rate of aqueous and organic phases were studied and optimized. Under the optimum conditions for 6 mL sample consumption an enhancement factor of 130 was obtained. The detection limit was 1.5 μg L(-1) and the precision of the method, expressed as relative standard deviation (RSD) was 2.7% at 40.0 μg L(-1) Pb(II) concentration level. The proposed method was evaluated by analyzing certified reference materials and spiked environmental water samples. PMID:25435230

  3. Speciation of inorganic lead and trialkyllead compounds by flame atomic absorption spectrometry following continuous selective preconcentration from aqueous solutions

    NASA Astrophysics Data System (ADS)

    Baena, Josefa R.; Gallego, Mercedes; Valcárcel, Miguel

    1999-12-01

    A new method for the speciation of inorganic lead and trialkyllead compounds involving the selective separation of the analytes in a continuous system and their subsequent introduction into a flame atomic absorption spectrometer was developed. The proposed flow system consists of two units. In the first unit, total inorganic lead at concentrations from 8 to 200 ng ml -1 is continuously precipitated as lead chromate and the filtrate, containing trialkyllead cations, is collected in a vessel, the precipitate then being dissolved in diluted acid and driven to the instrument. In the second unit, trimethyllead (TML +) and triethyllead (TEL +) cations at ng ml -1 levels are complexed with sodium diethyldithiocarbamate and retained on a C 60 pre-conditioned fullerene column; the mixture of both species was resolved by conditioning the sorbent column with n-hexane or isobutyl methyl ketone solvents. Detection limits of 1-2 ng ml -1 can be achieved by using a sample volume of 50 ml. Special attention was given to the reliability and robustness of the global flow injection method in assessing its applicability to both types of organolead compounds and inorganic lead present in different proportions. Trimethyllead provides the poorest results as consequence of its low adsorption constant on C 60; however, the three different types of species (Pb 2+/TML +/TEL +) can be effectively determined in proportions from 1:1:1 to 30:12:1 with relative errors less than 10%.

  4. Detection of silver nanoparticles in parsley by solid sampling high-resolution-continuum source atomic absorption spectrometry.

    PubMed

    Feichtmeier, Nadine S; Leopold, Kerstin

    2014-06-01

    In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples. PMID:24292434

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

    USGS Publications Warehouse

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

    1981-01-01

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

  6. A new coupling of ionic liquid based-single drop microextraction with tungsten coil electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Wen, Xiaodong; Deng, Qingwen; Wang, Jiwei; Yang, Shengchun; Zhao, Xia

    2013-03-01

    In this work, an improved method of ionic liquid based-single drop microextraction (IL-SDME) preconcentration was firstly coupled with tungsten coil electrothermal atomic absorption spectrometry (W-coil ET-AAS) detection. The new coupling was developed and applied for the determination of ultra-trace cadmium. Experimental parameters influencing the performance of IL-SDME as well as instrumental conditions were studied systematically, including IL-drop volume, chelating agent concentration, pH, stirring rate and time, heating program of W-coil ET-AAS, flow rate of carrier gas. Under the optimal conditions, the limit of detection (LOD) for cadmium was 0.015 μg L-1 (sampling amount on W-coil was 10 μL). The sensitivity enhancement factor was 42, while the improvement factor of LOD was 33. The established method was applied to determine cadmium in standard reference materials of rice and real water samples successfully. The developed IL-SDME-W-coil ET-AAS coupling represents a simple, green and highly sensitive method for cadmium determination.

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

    NASA Astrophysics Data System (ADS)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A.

    2013-08-01

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

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

    PubMed

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

    2016-01-01

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

  9. Determination of Beryllium in Soil and Sediment by Graphite Furnace Atomic Absorption with a Microwave-Acid Digestion Method.

    PubMed

    Lin, Hai-lan; Gan, Jie; Yu, Lei; Zhu, Ri-long; Tian, Yun; Luo, Yue-ping

    2015-11-01

    A method for determination of beryllium in soils and sediments by microwave-acid digestion/graphite furnace atomic absorption (GFAA) is described. In this paper, the working conditions of the instrument are optimized, the drawing of calibration curve is expounded, the pretreatment process of soil and sediments (including microwave heating process and the selection of digestion system) is discussed, and the interference of coexisting elements is examined. The sample was pretreated by microwave digestion parameters using HNO₃/ HCl/HF mixed acid system. The method is fast and simple without matrix modifier, and has no interference by coexisting ions, and has high repeatability and reproducibility. Under the optimal experimental conditions, the limit of detection (LOD) is 0.004 9 mg · kg⁻¹ (sample quantity 0.200 0 g, sample volume 25 mL), and the limits of quantitation (LOQ) is 0.20 mg · kg⁻¹. This method is used to measure the standard samples and actual samples, whether in the laboratory, or between laboratories, has good accuracy and precision. PMID:26978948

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

    SciTech Connect

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

    1981-01-01

    The Methyl isobutyl ketone-Amine synerGistic Iodide Complex (MAGIC) extraction system offers the advantage that a large number of trace elements can be rapidly determined with a single sample preparation procedure. However, many of the elements extracted by the MAGIC system form volatile organometallic halide salts when the organic extract is heated in the graphite furnace. High concentrations of some elements such as Cu and Zn extracted by the system from anomalous geological samples produce serious interferences when certain other elements are determined by flameless atomic absorption. Stripping systems have been developed using solutions of HNO/sub 3/, H/sub 2/SO/sub 4/, and CH/sub 3/COOH individually or combined with H/sub 2/O/sub 2/ in order to circumvent these problems. With these systems most of the elements in the organic extract can be sequentially stripped into an aqueous phase. Organometallic volatilization and the most serious interelement interferences, therefore, can be eliminated by stripping with various combinations of reagents in a series of steps.

  11. Ultrasound-promoted cold vapor generation in the presence of formic acid for determination of mercury by atomic absorption spectrometry.

    PubMed

    Gil, Sandra; Lavilla, Isela; Bendicho, Carlos

    2006-09-01

    A new cold vapor technique within the context of green chemistry is described for determination of mercury in liquid samples following high-intensity ultrasonication. Volatile Hg evolved in a sonoreactor without the use of a chemical reducing agent is carried to a quartz cell kept at room temperature for measurement of the atomic absorption. The mechanism involved lies in the reduction of Hg(II) to Hg(0) by reducing gases formed upon sonication and subsequent volatilization of Hg(0) due to the degassing effect caused by the cavitation phenomenon. Addition of a low molecular weight organic acid such as formic acid favors the process, but vapor generation also occurs from Hg solutions in ultrapure water. The detection limit of Hg was 0.1 microg/L, and the repeatability, expressed as relative standard deviation, was 4.4% (peak height). Addition of small amounts of oxidizing substances such as the permanganate or dichromate anions completely suppressed the formation of Hg(0), which confirms the above mechanism. Effect of other factors such as ultrasound irradiation time, ultrasound amplitude, and the presence of concomitants are also investigated. Some complexing anions such as chloride favored the stabilization of Hg(II) in solution, hence causing an interference effect on the ultrasound-assisted reduction/volatilization process. PMID:16944910

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

    NASA Astrophysics Data System (ADS)

    Mierzwa, Jerzy; Dobrowolski, Ryszard

    1998-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2005-01-01

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

  14. Correlation between Soft X-ray Absorption and Emission Spectra of the Nitrogen Atoms within Imidazolium-Based Ionic Liquids.

    PubMed

    Horikawa, Yuka; Tokushima, Takashi; Takahashi, Osamu; Hoke, Hiroshi; Takamuku, Toshiyuki

    2016-08-01

    Soft X-ray absorption spectroscopy (XAS) has been performed on the N K-edge of two imidazolium-based ionic liquids (ILs), 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)amide ([C2mim][TFSA]) and 1-ethyl-3-methylimidazolium bromide ([C2mim][Br]), to clarify the electronic structures of the ILs. Soft X-ray emission spectroscopy (XES) has also been applied to the ILs by excitation at various X-ray energies according to the XAS spectra. It was possible to fully associate the XAS peaks with the XES peaks. Additionally, both XAS and XES spectra of the ILs were well reproduced by the theoretical spectra for a single-molecule model on [C2mim](+) and [TFSA](-) using density functional theory. The assignments for the XAS and XES peaks of the ILs were accomplished from both experimental and theoretical approaches. The theoretical XAS and XES spectra of [C2mim](+) and [TFSA](-) did not significantly depend on the conformations of the ions. The reproducibility of the theoretical spectra for the single-molecule model suggested that the interactions between the cations and anions are very weak in the ILs, thus scarcely influencing the electronic structures of the nitrogen atoms. PMID:27388151

  15. Cloud point extraction and flame atomic absorption spectrometry determination of lead (II) in environmental and food samples.

    PubMed

    Soylak, Mustafa; Yilmaz, Erkan; Ghaedi, Mehrorang; Montazerozohori, Mortaza; Sheibani, Marjan

    2012-01-01

    A cloud point extraction procedure for the preconcentration of Pb2+ in various samples following complexation with 2,2'-(1E,1'E)-1,1'-(2,2'-azanediylbis(ethane-2,1-diyl)bis(azan-1-yl-1-ylidene)) bis(ethan-1-yl-1-ylidene)diphenol in Triton X-114 after centrifugation is reported. A 0.5 mL portion of methanol acidified with 1.0 M HNO3 was added to the surfactant-rich phase prior to analysis by flame atomic absorption spectrometry. The influence of analytical parameters--including pH, concentrations of ligand, Triton X-114, and HNO3, bath temperature, heating time, and centrifugation rate and time--were optimized, and the effect of the matrix ions on the recovery of Pb2+ was investigated. An LOD of 1.9 ng/mL along with a preconcentration factor of 50 with RSD of 1.0% for Pb2+ were achieved. The proposed procedure was applied to the analysis of various real samples. PMID:23451399

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

    PubMed Central

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

    2016-01-01

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

  17. Behaviour of chemical modifiers in the determination of arsenic by electrothermal atomic absorption spectrometry in petroleum products.

    PubMed

    Reboucas, Marcio V; Ferreira, Sergio L C; de Barros Neto, Benicio

    2005-07-15

    Most comparative studies on the efficiency of chemical modifiers have been conducted in aqueous media. In the present work, we proposed a detailed study of the use of different chemical modifiers for direct determination of arsenic in complex organic matrices by electrothermal atomic absorption spectrometry (ETAAS). Palladium, rhodium, tungsten, silver, lanthanum and a mixture of palladium and magnesium were tested. The figures of merit used for evaluation and comparison were acquired in the optimal conditions for each modifier, established by multivariate optimization of the main variables based on Doehlert designs. Singular features were observed for the chemical behaviour of some modifiers in organic matrices compared to aqueous media, such as the worse performance of Pd+Mg modifier and no notice of severe tube corrosion from La application. Lanthanum was chosen as the best chemical modifier for the present application, according to predefined criteria. Lanthanum showed the minimum limit of detection, characteristic concentration and blank signal among all tested species and no effect of the concomitants usually present in petrochemical feedstocks. Using a 200mgL(-1) lanthanum solution as a chemical modifier, the average relative standard deviations of 7 and 16% (at 3-15mugL(-1) level) and characteristic concentrations of 0.47 and 0.77mugL(-1) for naphtha and petroleum condensates, respectively, were observed. PMID:18970155

  18. Atomic absorption spectroscopic, conductometric and colorimetric methods for determination of fluoroquinolone antibiotics using ammonium reineckate ion-pair complex formation

    NASA Astrophysics Data System (ADS)

    Ragab, Gamal H.; Amin, Alaa S.

    2004-03-01

    Three accurate, rapid and simple atomic absorption spectrometric, conductometric and colorimetric methods were developed for the determination of norfloxacin (NRF), ciprofloxacin (CIP), ofloxacin (OFL) and enrofloxacin (ENF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at λmax 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone in the range 5.0-65, 4.0-48, 5.0-56 and 6.0-72 μg ml -1 of NRF, CPF, OFL and ENF, respectively. The optimizations of various experimental conditions were described. The results obtained showed good recoveries of 99.15±1.15, 99.30±1.40, 99.60±1.50, and 99.00±1.25% with relative standard deviations of 0.81, 1.06, 0.97, and 0.69% for NRF, CPF, OFL, and ENF, respectively. Applications of the proposed methods to representative pharmaceutical formulations are successfully presented.

  19. Determination of heavy metal contents by atomic absorption spectroscopy (AAS) in some medicinal plants from Pakistani and Malaysian origin.

    PubMed

    Akram, Sobia; Najam, Rahila; Rizwani, Ghazala H; Abbas, Syed Atif

    2015-09-01

    This study depicts a profile of existence of heavy metals (Cu, Ni, Zn, Cd, Hg, Mn, Fe, Na, Ca, and Mg) in some important herbal plants like (H. Integrifolia, D. regia, R. communis, C. equisetifolia, N. oleander, T. populnea, M. elengi, H. schizopetalus, P. pterocarpum) from Pakistan and an antidiabetic Malaysian herbal drug product containing (Punica granatum L. (Mast) Hook, Momordica charantia L., Tamarindus indica L., Lawsonia inermis L.) using atomic absorption spectrophotometer. Heavy metals in these herbal plants and Malaysian product were in the range of 0.02-0.10 ppm of Cu, 0.00-0.02 ppm of Ni, 0.02-0.29 ppm of Zn, 0.00-0.04 ppm of Cd, 0.00-1.33 ppm of Hg, 0.00-0.54 ppm of Mn, 0.22-3.16 ppm of Fe, 0.00-9.17 ppm of Na, 3.27-15.63 ppm of Ca and 1.85-2.03 ppm of Mg. All the metals under study were within the prescribed limits except mercury. Out of 10 medicinal plants/product under study 07 were beyond the limit of mercury permissible limits. Purpose of this study is to determine heavy metals contents in selected herbal plants and Malaysian product, also to highlight the health concerns related to the presence of toxic levels of heavy metals. PMID:26408897

  20. Fractionation analysis of manganese and zinc in beers by means of two sorbent column system and flame atomic absorption spectrometry.

    PubMed

    Pohl, Pawel; Prusisz, Bartlomiej

    2007-03-15

    In the present article, a method of operational fractionation of Mn and Zn in beer using flame atomic absorption spectrometry was developed. The proposed fractionation scheme was based on use of a hydrophobic adsorbing resin Amberlite XAD7 (first column, 2g resin bed) connected in a series with a strong cation exchanger Dowex 50Wx4 (second column, 1g resin bed). After passing the samples of beers through the columns, distinct groupings of Mn and Zn species retained on the sorbents, i.e., hydrophobic fraction of polyphenols bound metal species and cationic metal species fraction, respectively, were determined in respective eluates obtained after complete recovery of Mn and Zn species with 10ml of 2.0moll(-1) HNO(3) (first column) and 10ml of 4.0moll(-1) HCl (second column). In addition, the effluents collected were analyzed prior to the evaluation of the third, residual fraction, presumably attributed to any hydrophilic anionic and inert metal species. The established fractionation patterns for Mn and Zn were discussed in reference to likely associations of metals with endogenous food bioligands and possible availability of the distinguished metal species classes. The quality of the results was proved by the recovery experiments. PMID:19071499

  1. Determination of Low Levels of Lead in Beer Using Solid-Phase Extraction and Detection by Flame Atomic Absorption Spectrometry

    PubMed Central

    Alves, Vanessa N.; Borges, Simone S. O.; Neto, Waldomiro B.; Coelho, Nívia M. M.

    2011-01-01

    In this study, a method for the determination of low concentrations of lead in beer samples using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry (FAAS) was developed. Moringa oleifera seeds were used as a biosorbent material. Chemical and flow variables of the online preconcentration system, such as sample pH, preconcentration flow rate, eluent flow rate, eluent concentration, particle size, and sorbent mass, were studied. The optimum extraction conditions were obtained using a sample pH of 6.0, sample flow rate of 6.0 mL min−1, 63.0 mg of sorbent mass, and 2.0 mol L−1 HNO3 at a flow rate of 2.0 mL min−1 as the eluent. With the optimized conditions, the preconcentration factor, precision, detection limit, consumption index, and sample throughput were estimated as 93, 0.3% (10.0 μg L−1, n = 7), 7.5 μg L−1, 0.11 mL, and 23 samples per hour, respectively. The method developed was successfully applied to beer samples and recovery tests, with recovery ranging from 80% to 100%. PMID:22013389

  2. Analysis of lead in 55 brands of dietary calcium supplements by graphite furnace atomic absorption spectrometry after microwave digestion.

    PubMed

    Kim, Meehye; Kim, Changmin; Song, Insang

    2003-02-01

    The lead (Pb) contents of calcium (Ca) supplements available in Korea were determined by graphite furnace atomic absorption spectrometry using Zeeman background correction and peak area mode. All samples were microwave-digested in concentrated HNO(3). Ammonium dihydrogen phosphate and magnesium nitrate were used as matrix modifiers. Fifty-five brands of Ca supplements were classified into seven categories based on the major composite: bone, milk, oyster/clam shell, egg shell, algae, shark cartilage and chelated. The mean Pb contents of Ca supplements were 1.1 microg g(-1) (coefficient of variation 5.7%), ranging from n.d. (not detected) to 6.7 microg g(-1). Ca supplements made of bone have the highest Pb contents (2.3 microg g(-1)) with a wide range (0.1-6.7 microg g(-1)). The results were similar to those reported in other countries. The mean daily intakes of Pb from the supplement could be about 5 microg (mean Pb concentration 1.1 microg g(-1) x mean daily intake 4.5 g) taking 2% of provisional tolerable daily intake that the FAO/WHO Joint Food Additive and Contaminants Committee has set to evaluate its safety. However, measures to prevent potentials of Pb toxicity from overtaking some Ca supplements should be considered. PMID:12623663

  3. U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION, AND MAINTENANCE OF THE PERKIN-ELMER ZEEMAN/5000 SYSTEM ATOMIC ABSORPTION SPECTROPHOTOMETER (BCO-L-6.0)

    EPA Science Inventory

    The purpose of this SOP is to outline the start-up, calibration, operation, and maintenance procedures for the Perkin-Elmer 5000 atomic absorption spectrophotometer (PE 5000 AA), and the Perkin Elmer 5000 Zeeman graphite furnace atomic absorption spectrophotometer (PE 5000Z GFAA)...

  4. NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION AND MAINTENANCE OF THE PERKIN-ELMER ZEEMAN/5000 SYSTEM ATOMIC ABSORPTION SPECTROMETER (BCO-L-6.0)

    EPA Science Inventory

    The purpose of this SOP is to outline the start-up, calibration, operation, and maintenance procedures for the Perkin-Elmer 5000 atomic absorption spectrophotometer (PE 5000 AA), and the Perkin Elmer 5000 Zeeman graphite furnace atomic absorption spectrophotometer (PE 5000Z GFAA)...

  5. Absorption spectroscopy measurements of argon metastable and resonant atom density in atmospheric pressure Ar-He surface-wave plasmas using a low pressure lamp

    SciTech Connect

    Munoz, J.; Margot, J.; Calzada, M. D.

    2012-01-15

    The densities of metastable and resonant atom were measured in atmospheric pressure Ar-He surface-wave plasmas. Measurements were performed using an absorption spectroscopy method taking into account the Voigt profiles of the plasma lines. The density values of the argon {sup 3}P{sub 2}, {sup 3}P{sub 0} (metastable atoms) and {sup 3}P{sub 1} (resonant atoms) levels measured in pure argon discharges are in good agreement with those reported in the literature. A drastic decrease of metastable and resonant densities is observed when introducing helium in amounts as low as 2%. The influence of electron density and gas temperature on the population mechanisms (direct electron excitation from the ground state and dissociative recombination) of metastable and resonant atoms is discussed using a simplified theoretical model.

  6. Semi-permanent lutetium modifier for the determination of beryllium in urine by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Burguera, J. L.; Burguera, M.; Rondón, C.; Carrero, P.

    1999-11-01

    The determination of beryllium using electrothermal atomic absorption spectrometry with deuterium background correction in the presence of various isomorphous metals and Mg(NO 3) 2 was studied. While, Eu, Ir and Sm had no effect on the transient signals, the addition of Lu and Mg(NO 3) 2 improved the sensitivity of the beryllium signal with respect to that obtained in the absence of modifier. Although, Mg(NO 3) 2 has improved the signal with respect to its sensitivity, it also increased the tail and the background (BG) signals, specially when urine samples are under study. Whereas, when Lu was used the analytical signal is virtually free of BG interference indicating that the urine matrix interference was almost eliminated. Besides, the addition of 6 μg of Lu ensured that the signals were effectively constant for five firings following the furnace program, which included: three drying, and the pyrolysis, atomization, cleaning and cooling steps. The effect of some components, likely to interfere in the accurate determination of beryllium (such as: Al, Ca, Cl, Co, Cr, Fe, Mg and Mn) were investigated. At the physiological levels, most of these elements had no effect, except in the case of chloride when Mg(NO 3) 2 was used as modifier. In this case, the tolerance limit was of 3000 mg Cl - l -1. The characteristic masses were 1.19, 0.45 and 0.48 pg, when integrated absorbance was measured for beryllium without the addition of any modifier and in the presence of Lu and Mg(NO 3) 2, respectively. The limits of detection (3σ) were 85, 19 and 58 fg, respectively. The accuracy and precision with the use of Lu and Mg(NO 3) 2 was tested for the direct determination of beryllium in urine samples. Quantification was performed with aqueous standards. The results obtained for the determination of beryllium in reference materials (Trace Elements in Urine), together with good recovery of spiked analyte, using either Lu or Mg(NO 3) 2 modification demonstrate the applicability of

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

    NASA Astrophysics Data System (ADS)

    Hagarová, Ingrid; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb-dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l- 1 HNO3. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l- 1, quantification limit of 0.38 μg l- 1, relative standard deviation of 4.2% (for 2 μg l- 1 of Pb; n = 26), linearity of the calibration graph in the range of 0.5-4.0 μg l- 1 (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91-96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters.

  8. Method validation for the determination of total mercury in fish muscle by cold vapour atomic absorption spectrometry.

    PubMed

    Nascimento Neto, A P; Costa, L C S Magalhães; Kikuchi, A N S; Furtado, D M S; Araujo, M Q; Melo, M C C

    2012-01-01

    A method was validated for the determination of total Hg in fish muscle using continuous flow cold vapour atomic absorption (CVAAS) after microwave digestion in closed vessels. The method was validated according to European Union Regulations 333/2007 and 657/2002, considering the maximum level for the metal in fish, established by European Union regulation 1881/2006. The procedure for determining linear range, selectivity, recovery, precision, trueness, decision limit (CCα), detection capability (CCβ), measurement uncertainty and robustness of the method is reported. The results of the validation process demonstrate the method fulfils the provisions of the Commission Regulation. The selectivity study indicated that there was no matrix effect on the calibration curve between the concentration range of 1.0 and 30.0 µg Hg l(-1). The mean recovery calculated at six levels of fortification was in the range of 94-104%. The limit of detection (LOD) and limit of quantification (LOQ) values were 4.90 and 15.7 µg kg(-1), while the CCα and CCβ values were 0.517 and 0.533 mg kg(-1), respectively, for the maximum contaminant level of 0.500 mg kg(-1). The relative expanded measurement uncertainty of the method was 0.055 mg kg(-1). The method was not affected by slight variations of some critical factors (ruggedness minor changes) as sample mass and volume of the HNO(3) and H(2)O(2) used in the digestion step. The method allowed accurate confirmation analyses of the CRM DORM 3. In fact, the Z-scores attained in a proficiency test round were well below the reference value of 2.0, proving the excellent performance of the laboratory. PMID:22250927

  9. Speciation of methylcyclopentadienyl manganese tricarbonyl by high-performance liquid chromatography-diode laser atomic absorption spectrometry.

    PubMed

    Butcher, D J; Zybin, A; Bolshov, M A; Niemax, K

    1999-12-01

    Methylcyclopentadienyl manganese tricarbonyl (MMT) is a fuel additive that has been marketed for use in unleaded gasoline since December 1995. The widespread use of this additive has been suggested to cause health risks, but limitations in data regarding its degradation products and their toxicity prevent an accurate evaluation. To monitor the organomanganese compounds, it is clearly advantageous to employ low-cost, high-sensitivity, manganese-specific instrumentation to perform speciation. In this work, instrumentation fitting these criteria was obtained by the combination of high-performance liquid chromatography (HPLC) with diode laser atomic absorption spectrometry (DLAAS) and was used to determine MMT, its nonmethylated derivative, cyclopentadienyl manganese tricarbonyl (CMT), and inorganic manganese. DLAAS was shown to be a versatile analytical technique for total Mn determination, with a detection limit of 1 ng/mL and a linear dynamic range (LDR) of almost 5 orders of magnitude. Analytical figures of merit for HPLC-DLAAS included a detection limit of 2 ng(as Mn)/mL, a LDR of 3 orders of magnitude, and an analysis time of three minutes. The organometallic compounds are characterized by rapid photolysis in sunlight, and hence, experiments were performed to evaluate whether normal laboratory lighting is suitable for their determination. Our results showed that normal laboratory protocols may be employed except that the organomanganese compounds should be stored away from light except during sample introduction procedures. The ability of the instrumentation to selectively preconcentrate organomanganese compounds while removing inorganic manganese was demonstrated. Sufficient resolution was obtained to determine a 20-fold excess of CMT compared with MMT. The ability of the system to do practical analysis was demonstrated by the accurate determination of MMT in spiked samples of gasoline, human urine, and tap water. These results demonstrate the suitability of

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

    NASA Astrophysics Data System (ADS)

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

    2008-08-01

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

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

    NASA Astrophysics Data System (ADS)

    Kaercher, Luiz Eduardo; Goldschmidt, Fabiane; Paniz, José Neri Gottfried; de Moraes Flores, Érico Marlon; Dressler, Valderi Luiz

    2005-06-01

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

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

    PubMed

    Silva, Edson Luiz; Roldan, Paulo Dos Santos

    2009-01-15

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

  13. Determination of trace elements in dolomite and gypsum by atomic absorption spectrometry: overcoming the matrix interference by flotation separation

    NASA Astrophysics Data System (ADS)

    Stafilov, Trajče; Zendelovska, Dragica; Pavlovska, Gorica; Čundeva, Katarina

    2002-05-01

    The interferences of Ca and Mg as matrix elements in dolomite and gypsum on Ag, Cd, Cr, Mn, Tl and Zn absorbances during their electrothermal atomic absorption spectrometric (ETAAS) determination are investigated. The results reveal that Ca and Mg do not interfere on Zn and Mn, tend to decrease absorbances of Ag, Cd and Cr, while Tl suffers the most significant influence. A flotation separation method is proposed to eliminate matrix interferences. Hydrated iron(III) oxide, Fe 2O 3· xH 2O, and iron(III) hexamethylenedithiocarbamate, Fe(HMDTC) 3, are applied as flotation collectors. The influence of hydrophobic dithiocarbamate anion, HMDTC, on flotation recoveries of each analyte is studied. The most suitable concentrations of dolomite and gypsum solutions for flotation are determined. To avoid flotation suppression due to the reaction of Ca 2+ and Mg 2+ with surfactant ions, a fit foaming agent was selected. The elements present in dolomite and gypsum as traces have been analyzed by ETAAS. Their ETAAS limits of detection following flotation are found to be 0.021 μg·g -1 for Ag, 0.019 μg·g -1 for Cd, 0.014 μg·g -1 for Cr and 0.11 μg·g -1 for Tl. The determination of Mn and Zn can be performed by flame AAS (FAAS). The limit of detection for Mn is 1.5 μg·g -1, while for Zn 0.8 μg·g -1.

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

    PubMed Central

    2011-01-01

    Arsenic is the toxic element, which creates several problems in human being specially when inhaled through air. So the accurate and precise measurement of arsenic in suspended particulate matter (SPM) is of prime importance as it gives information about the level of toxicity in the environment, and preventive measures could be taken in the effective areas. Quality assurance is equally important in the measurement of arsenic in SPM samples before making any decision. The quality and reliability of the data of such volatile elements depends upon the measurement of uncertainty of each step involved from sampling to analysis. The analytical results quantifying uncertainty gives a measure of the confidence level of the concerned laboratory. So the main objective of this study was to determine arsenic content in SPM samples with uncertainty budget and to find out various potential sources of uncertainty, which affects the results. Keeping these facts, we have selected seven diverse sites of Delhi (National Capital of India) for quantification of arsenic content in SPM samples with uncertainty budget following sampling by HVS to analysis by Atomic Absorption Spectrometer-Hydride Generator (AAS-HG). In the measurement of arsenic in SPM samples so many steps are involved from sampling to final result and we have considered various potential sources of uncertainties. The calculation of uncertainty is based on ISO/IEC17025: 2005 document and EURACHEM guideline. It has been found that the final results mostly depend on the uncertainty in measurement mainly due to repeatability, final volume prepared for analysis, weighing balance and sampling by HVS. After the analysis of data of seven diverse sites of Delhi, it has been concluded that during the period from 31st Jan. 2008 to 7th Feb. 2008 the arsenic concentration varies from 1.44 ± 0.25 to 5.58 ± 0.55 ng/m3 with 95% confidence level (k = 2). PMID:21466671

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

    PubMed

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

    2015-01-01

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

  16. Low temperature hydrogen plasma-assisted atomic layer deposition of copper studied using in situ infrared reflection absorption spectroscopy

    SciTech Connect

    Chaukulkar, Rohan P.; Rai, Vikrant R.; Agarwal, Sumit; Thissen, Nick F. W.

    2014-01-15

    Atomic layer deposition (ALD) is an ideal technique to deposit ultrathin, conformal, and continuous metal thin films. However, compared to the ALD of binary materials such as metal oxides and metal nitrides, the surface reaction mechanisms during metal ALD are not well understood. In this study, the authors have designed and implemented an in situ reflection-absorption infrared spectroscopy (IRAS) setup to study the surface reactions during the ALD of Cu on Al{sub 2}O{sub 3} using Cu hexafluoroacetylacetonate [Cu(hfac){sub 2}] and a remote H{sub 2} plasma. Our infrared data show that complete ligand-exchange reactions occur at a substrate temperature of 80 °C in the absence of surface hydroxyl groups. Based on infrared data and previous studies, the authors propose that Cu(hfac){sub 2} dissociatively chemisorbs on the Al{sub 2}O{sub 3} surface, where the Al-O-Al bridge acts as the surface reactive site, leading to surface O-Cu-hfac and O-Al-hfac species. Surface saturation during the Cu(hfac){sub 2} half-cycle occurs through blocking of the available chemisorption sites. In the next half-reaction cycle, H radicals from an H{sub 2} plasma completely remove these surface hfac ligands. Through this study, the authors have demonstrated the capability of in situ IRAS as a tool to study surface reactions during ALD of metals. While transmission and internal reflection infrared spectroscopy are limited to the first few ALD cycles, IRAS can be used to probe all stages of metal ALD starting from initial nucleation to the formation of a continuous film.

  17. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of antimony by automated-hydride atomic absorption spectrophotometry

    USGS Publications Warehouse

    Brown, G.E.; McLain, B.J.

    1994-01-01

    The analysis of natural-water samples for antimony by automated-hydride atomic absorption spectrophotometry is described. Samples are prepared for analysis by addition of potassium and hydrochloric acid followed by an autoclave digestion. After the digestion, potassium iodide and sodium borohydride are added automatically. Antimony hydride (stibine) gas is generated, then swept into a heated quartz cell for determination of antimony by atomic absorption spectrophotometry. Precision and accuracy data are presented. Results obtained on standard reference water samples agree with means established by interlaboratory studies. Spike recoveries for actual samples range from 90 to 114 percent. Replicate analyses of water samples of varying matrices give relative standard deviations from 3 to 10 percent.

  18. Determination of gold, indium, tellurium and thallium in the same sample digest of geological materials by atomic-absorption spectroscopy and two-step solvent extraction

    USGS Publications Warehouse

    Hubert, A.E.; Chao, T.T.

    1985-01-01

    A rock, soil, or stream-sediment sample is decomposed with hydrofluoric acid, aqua regia, and hydrobromic acid-bromine solution. Gold, thallium, indium and tellurium are separated and concentrated from the sample digest by a two-step MIBK extraction at two concentrations of hydrobromic add. Gold and thallium are first extracted from 0.1M hydrobromic acid medium, then indium and tellurium are extracted from 3M hydrobromic acid in the presence of ascorbic acid to eliminate iron interference. The elements are then determined by flame atomic-absorption spectrophotometry. The two-step solvent extraction can also be used in conjunction with electrothermal atomic-absorption methods to lower the detection limits for all four metals in geological materials. ?? 1985.

  19. [Investigations on ashing of animal tissues for the determinations of trace metals by means of polarography or atomic-absorption spectrometry (author's transl)].

    PubMed

    Suzutani, T

    1980-01-01

    A comparison has been made of three ashing methods for animal tissues with subsequent determination of minute quantities of metals by polarography or atomic-absorption spectrometry. Wet oxidation method with many disadvantages and few advantages has been shown not to be useful for the purpose. Both dry ashing in a muffle-furnace at 530 degrees C and low-temperature ashing are equally applicable to atomic-absorption spectrometry, but dry ashing in a furnace is more excellent with polarography. For obtaining ashes with constant compositions it is far more difficult with low-temperature ashing than with dry ashing in a furnace. Hence, dry ashing in a furnace is most widely applicable. PMID:7409725

  20. Flow injection on-line dilution for zinc determination in human saliva with electrothermal atomic absorption spectrometry detection.

    PubMed

    Burguera-Pascu, Margarita; Rodríguez-Archilla, Alberto; Burguera, José Luis; Burguera, Marcela; Rondón, Carlos; Carrero, Pablo

    2007-09-26

    An automated method is described for the determination of zinc in human saliva by electrothermal atomic absorption spectrometry (ET AAS) after on-line dilution of samples with a significant reduction of sample consumption per analysis (<0.4 mL including the dead volume of the system). In order to fulfill this aim without changing the sample transport conduits during the experiments, a flow injection (FI) dilution system was constructed. Its principal parts are: one propulsion device (peristaltic pump, PP) for either samples, standards or washing solution all located in an autosampler tray and for the surfactant solution (Triton X-100) used as diluent, and a two-position time based solenoid injector (TBSI(1)) which allowed the introduction of 10 microL of either solution in the diluent stream. To avoid unnecessary waste of samples, the TBSI(1) also permitted the recirculation of the solutions to their respective autosampler cups. The downstream diluted solution fills a home made sampling arm assembly. The sequential deposition of 20 microL aliquots of samples or standards on the graphite tube platform was carried out by air displacement with a similar time based solenoid injector (TBSI(2)). The dilution procedure and the injection of solutions into the atomizer are computer controlled and synchronized with the operation of the temperature program. Samples or standards solutions were submitted to two drying steps (at 90 and 130 degrees C), followed by pyrolysis and atomization at 700 and 1700 degrees C, respectively. The aqueous calibration was linear up to 120.0 microgL(-1) for diluted standard solutions/samples and its slope was similar (p>0.05) to the standard addition curve, indicating lack of matrix effect. The precision tested by repeated analysis of real saliva samples was less than 3% and the detection limit (3sigma) was of 0.35 microgL(-1). To test the accuracy of the proposed procedure, recovery tests were performed, obtaining mean recovery of added zinc of

  1. Characterization of the physico-chemical properties of polymeric materials for aerospace flight. [differential thermal and atomic absorption spectroscopic analysis of nickel cadmium batteries

    NASA Technical Reports Server (NTRS)

    Rock, M.

    1981-01-01

    Electrodes and electrolytes of nickel cadmium sealed batteries were analyzed. Different thermal analysis of negative and positive battery electrodes was conducted and the temperature ranges of occurrence of endotherms indicating decomposition of cadmium hydroxide and nickel hydroxide are identified. Atomic absorption spectroscopy was used to analyze electrodes and electrolytes for traces of nickel, cadmium, cobalt, and potassium. Calibration curves and data are given for each sample analyzed. Instrumentation and analytical procedures used for each method are described.

  2. Absorption spectroscopy of heavy alkaline earth metals Ba and Sr in rare gas matrices--CCSD(T) calculations and atomic site occupancies.

    PubMed

    Davis, Barry M; McCaffrey, John G

    2016-01-28

    Isolation of the heavier alkaline earth metals Ba and Sr in the solid rare gases (RGs) Ar, Kr, and Xe is analysed with absorption spectroscopy and interpreted partly with the assistance of ab initio calculations of the diatomic M ⋅ RG ground state interaction potentials. The y(1)P ← a(1)S resonance transitions in the visible spectral region are used to compare the isolation conditions of these two metal atom systems and calcium. Complex absorption bands were recorded in all three metal atom systems even after extensive sample annealing. Coupled cluster calculations conducted on the ground states of the nine M ⋅ RG diatomics (M = Ca, Sr, and Ba; RG = Ar, Kr, and Xe) at the coupled cluster single, double, and non-iterative triple level of theory revealed long bond lengths (>5 Å) and shallow bound regions (<130 cm(-1)). All of the M ⋅ RG diatomics have bond lengths considerably longer than those of the rare gas dimers, with the consequence that isolation of these metal atoms in a single substitutional site of the solid rare gas is unlikely, with the possible exception of Ca/Xe. The luminescence of metal dimer bands has been recorded for Ba and Sr revealing very different behaviours. Resonance fluorescence with a lifetime of 15 ns is observed for the lowest energy transition of Sr2 while this transition is quenched in Ba2. This behaviour is consistent with the absence of vibrational structure on the dimer absorption band in Ba2 indicating lifetime broadening arising from efficient relaxation to low-lying molecular states. More extensive 2D excitation-emission data recorded for the complex site structures present on the absorption bands of the atomic Ba and Sr systems will be presented in future publications. PMID:26827218

  3. Absorption spectroscopy of heavy alkaline earth metals Ba and Sr in rare gas matrices—CCSD(T) calculations and atomic site occupancies

    NASA Astrophysics Data System (ADS)

    Davis, Barry M.; McCaffrey, John G.

    2016-01-01

    Isolation of the heavier alkaline earth metals Ba and Sr in the solid rare gases (RGs) Ar, Kr, and Xe is analysed with absorption spectroscopy and interpreted partly with the assistance of ab initio calculations of the diatomic M ṡ RG ground state interaction potentials. The y1P←a1S resonance transitions in the visible spectral region are used to compare the isolation conditions of these two metal atom systems and calcium. Complex absorption bands were recorded in all three metal atom systems even after extensive sample annealing. Coupled cluster calculations conducted on the ground states of the nine M ṡ RG diatomics (M = Ca, Sr, and Ba; RG = Ar, Kr, and Xe) at the coupled cluster single, double, and non-iterative triple level of theory revealed long bond lengths (>5 Å) and shallow bound regions (<130 cm-1). All of the M ṡ RG diatomics have bond lengths considerably longer than those of the rare gas dimers, with the consequence that isolation of these metal atoms in a single substitutional site of the solid rare gas is unlikely, with the possible exception of Ca/Xe. The luminescence of metal dimer bands has been recorded for Ba and Sr revealing very different behaviours. Resonance fluorescence with a lifetime of 15 ns is observed for the lowest energy transition of Sr2 while this transition is quenched in Ba2. This behaviour is consistent with the absence of vibrational structure on the dimer absorption band in Ba2 indicating lifetime broadening arising from efficient relaxation to low-lying molecular states. More extensive 2D excitation-emission data recorded for the complex site structures present on the absorption bands of the atomic Ba and Sr systems will be presented in future publications.

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

    USGS Publications Warehouse

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

    1990-01-01

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

  5. Determination of lead in blood by chelation with ammonium pyrrolidine dithio-carbamate followed by tungsten-coil atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Salido, Arthur; Sanford, Caryn L.; Jones, Bradley T.

    1999-08-01

    An inexpensive, bench-top blood Pb analyzer has been developed. The system is based on tungsten-coil atomic absorption spectrometry. Pb atomization occurs on W-coils extracted from commercially available slide projector bulbs. The system has minimal power requirements: 120 ACV and 15 A. A small, computer-controlled CCD spectrometer is used as the detector. A Pb hollow cathode lamp is used as the source. Blood Pb is chelated with ammonium pyrrolidine dithio-carbamate and extracted into methyl iso-butyl ketone (4-methyl 2-pentanone). Twenty-microliter volumes of the organic phase are deposited on the W-coil, dried at 1.4 A, charred at 2.3 A and atomized at 6.0 A. Graphite furnace atomic absorption spectrometry is used as a comparison for W-coil results. Levels 1-4 of a NIST standard reference material 955b ‘lead in bovine blood’ are used to test accuracy and precision. The analytical figures of merit for the system are: 12-pg instrument detection limit, 24-pg blood detection limit and a characteristic mass of 28 pg.

  6. Effect of magnesium acetylacetonate on the signal of organic forms of vanadium in graphite furnace atomic absorption spectrometry.

    PubMed

    Kowalewska, Zofia; Welz, Bernhard; Castilho, Ivan N B; Carasek, Eduardo

    2013-01-15

    The aim of this work was to investigate the influence of magnesium acetylacetonate (MgA) on the signal of organic forms of vanadium in xylene solution by graphite furnace atomic absorption spectrometry. MgA alone or mixed with palladium acetylacetonate (PdA) was considered as a chemical modifier. It has been found that MgA does not improve, but decreases significantly the integrated absorbance of V in the form of alkyl-aryl sulfonates, acetylacetonates, porphyrins and in lubricating oils, while its effect is negligible in the case of "dark products" from petroleum distillation, i.e., heavy oil fractions and residues. The decrease is also observed in the presence of Pd. The MgA (or MgA+PdA) effect on the integrated absorbance of V has been studied using the following variants: different ways of modifier application, various pyrolysis temperature, additional application of air ashing, preliminary pretreatment with iodine and methyltrioctylammonium chloride, application of various graphite furnace heating systems (longitudinal or transverse) and various optical and background correction systems (medium-resolution line source spectrometer with deuterium background correction or high-resolution continuum source spectrometer). The experiments indicate formation of more refractory compounds as a possible reason for the decrease of the integrated absorbance for some forms of V in the presence of MgA. The application of MgA as a chemical modifier in V determination is not recommended. Results of this work have general importance as, apart from the intentional use of MgA as a modifier, organic Mg compounds, present in petroleum products for other reason (e.g. as an additive), can influence the signal of V compounds and hence the accuracy in V determination. Generally, petroleum products with known amount of V are recommended as standards; however, lubricating oils can be inadequate for "dark products" from petroleum distillation. In the case of unknown samples it is

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

    NASA Astrophysics Data System (ADS)

    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

  8. Determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry.

    PubMed

    Silva, Laiana O B; Leao, Danilo J; dos Santos, Debora C; Matos, Geraldo D; de Andrade, Jailson B; Ferreira, Sergio L C

    2014-09-01

    The present paper describes the development of a method for the determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry (CVG AAS). Chemometric tools were employed to characterize the influence of several factors on the generation of volatile copper species. First, a two-level full factorial design was performed that included the following chemical variables: hydrochloric acid concentration, tetrahydroborate concentration, sulfanilamide concentration and tetrahydroborate volume, using absorbance as the response. Under the established experimental conditions, the hydrochloric acid concentration had the greatest influence on the generation of volatile copper species. Subsequently, a Box-Behnken design was performed to determine the optimum conditions for these parameters. A second chemometric study employing a two-level full factorial design was performed to evaluate the following physical factors: tetrahydroborate flow rate, flame composition, alcohol volume and sample volume. The results of this study demonstrated that the tetrahydroborate flow rate was critical for the process. The chemometric experiments determined the following experimental conditions for the method: hydrochloric acid concentration, 0.208 M; tetrahydroborate concentration, 4.59%; sulfanilamide concentration, 0.79%; tetrahydroborate volume, 2.50 mL; tetrahydroborate flow rate, 6.50 mL min(-1); alcohol volume, 200 µL; and sample volume, 7.0 mL. Thus, this method, using a slurry volume of 500 µL and a final dilution of 7 mL, allowed for the determination of copper with limits of detection and quantification of 0.30 and 0.99 µg L(-1), respectively. Precisions, expressed as RSD%, of 4.6 and 2.8% were obtained using copper solutions at concentrations of 5.0 and 50.0 µg L(-1), respectively. The accuracy was evaluated by the analysis of a certified reference material of urban particulate matter. The copper concentration

  9. Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry: ultra trace determination of cadmium in water samples.

    PubMed

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

    2007-03-01

    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 microL methanol (disperser solvent) containing 34 microL 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 microL). Then a 20 microL 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

  10. Rapid determination of lead in water samples by dispersive liquid-liquid microextraction coupled with electrothermal atomic absorption spectrometry.

    PubMed

    Naseri, Mohammad Taghi; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub; Kiani, Armin

    2008-03-15

    The need for highly reliable methods for the determination of trace and ultratrace elements has been recognized in analytical chemistry and environmental science. A simple and powerful microextraction technique was used for the detection of the lead ultratrace amounts in water samples using the dispersive liquid-liquid microextraction (DLLME), followed by the electrothermal atomic absorption spectrometry (ET AAS). In this microextraction technique, a mixture of 0.50 mL acetone (disperser solvent), containing 35 microL carbon tetrachloride (extraction solvent) and 5 microL diethyldithiophosphoric acid (chelating agent), was rapidly injected by syringe into the 5.00 mL water sample, spiked with lead. In this process, the lead ions reacted with the chelating agent and were extracted into the fine droplets of CCl(4). After centrifugation (2 min at 5000 rpm), the fine CCl4 droplets were sedimented at the bottom of the conical test tube (25+/-1 microL). Then, 20 microL from the sedimented phase, containing the enriched analyte, was determined by ET AAS. The next step was the optimization of various experimental conditions, affecting DLLME, such as the type and the volume of the extraction solvent, the type and the volume of the disperser solvent, the extraction time, the salt effect, pH and the chelating agent amount. Moreover, the effect of the interfering ions on the analytes recovery was also investigated. Under the optimum conditions, the enrichment factor of 150 was obtained from only a 5.00 mL water sample. The calibration graph was linear in the range of 0.05-1 microg L(-1) with the detection limit of 0.02 microg L(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 0.50 microg L(-1) of lead was 2.5%. The relative lead recoveries in mineral, tap, well and sea water samples at the spiking level of 0.20 and 0.40 microg L(-1) varied from 93.5 to 105.0. The characteristics of the proposed method were compared with the cloud point

  11. Mass energy-absorption coefficients and average atomic energy-absorption cross-sections for amino acids in the energy range 0.122-1.330 MeV

    NASA Astrophysics Data System (ADS)

    More, Chaitali V.; Lokhande, Rajkumar M.; Pawar, Pravina. P.

    2016-05-01

    Mass attenuation coefficients of amino acids such as n-acetyl-l-tryptophan, n-acetyl-l-tyrosine and d-tryptophan were measured in the energy range 0.122-1.330 MeV. NaI (Tl) scintillation detection system was used to detect gamma rays with a resolution of 8.2% at 0.662 MeV. The measured attenuation coefficient values were then used to determine the mass energy-absorption coefficients (σa,en) and average atomic energy-absorption cross sections (μen/ρ) of the amino acids. Theoretical values were calculated based on XCOM data. Theoretical and experimental values are found to be in good agreement.

  12. Application of a diode-laser absorption technique with the d(2) transition of atomic rb for hypersonic flow-field measurements.

    PubMed

    Trinks, O; Beck, W H

    1998-10-20

    With a first application of semiconductor lasers to absorption measurements of seeded atomic Rb in high-enthalpy flow fields, a diagnostic technique for time-resolved determination of flow velocity and gas temperature with a line-shape analysis was developed. In our measurements a GaAlAs diode laser was used to scan repetitively at 15 kHz over 1.3 cm(-1) across the D(2) resonance transition (5S(1/2) ? 5P(3/2), 780.2 nm) of seeded atomic Rb to obtain multiple absorption line shapes. The time-dependent signal contains highly resolved spectral line-shape information, which we interpret by fitting the spectrally resolved line shapes to Voigt profiles. Kinetic temperatures in the range 900-1400 K and gas velocities in the range 3900-6200 ms(-1) were obtained from the Doppler-broadened component of the line shape and from the Doppler shift, respectively, of the absorption frequency. PMID:18301526

  13. NHEXAS PHASE I REGION 5 STUDY--STANDARD OPERATING PROCEDURE FOR THE CALIBRATION OF PERKIN ELMER (PE) MODEL 5100 ZL ATOMIC ABSORPTION SPECTROMETER: GRAPHITE FURNACE (NHX/SOP-171-005)

    EPA Science Inventory

    This procedure describes the calibration procedures and performance checks required to ensure the consistent performance of the Perkin Elmer (PE) Model 5100 zl atomic absorption spectrometer with graphite furnace unit as a whole. Separate calibration procedures were not required ...

  14. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chromium in water by graphite furnace atomic absorption spectrophotometry

    USGS Publications Warehouse

    McLain, B.J.

    1993-01-01

    Graphite furnace atomic absorption spectrophotometry is a sensitive, precise, and accurate method for the determination of chromium in natural water samples. The detection limit for this analytical method is 0.4 microg/L with a working linear limit of 25.0 microg/L. The precision at the detection limit ranges from 20 to 57 percent relative standard deviation (RSD) with an improvement to 4.6 percent RSD for concentrations more than 3 microg/L. Accuracy of this method was determined for a variety of reference standards that was representative of the analytical range. The results were within the established standard deviations. Samples were spiked with known concentrations of chromium with recoveries ranging from 84 to 122 percent. In addition, a comparison of data between graphite furnace atomic absorption spectrophotometry and direct-current plasma atomic emission spectrometry resulted in suitable agreement between the two methods, with an average deviation of +/- 2.0 microg/L throughout the analytical range.

  15. Uniform Fe3O4 coating on flower-like ZnO nanostructures by atomic layer deposition for electromagnetic wave absorption.

    PubMed

    Wan, Gengping; Wang, Guizhen; Huang, Xianqin; Zhao, Haonan; Li, Xinyue; Wang, Kan; Yu, Lei; Peng, Xiange; Qin, Yong

    2015-11-21

    An elegant atomic layer deposition (ALD) method has been employed for controllable preparation of a uniform Fe3O4-coated ZnO (ZnO@Fe3O4) core-shell flower-like nanostructure. The Fe3O4 coating thickness of the ZnO@Fe3O4 nanostructure can be tuned by varying the cycle number of ALD Fe2O3. When serving as additives for microwave absorption, the ZnO@Fe3O4-paraffin composites exhibit a higher absorption capacity than the ZnO-paraffin composites. For ZnO@500-Fe3O4, the effective absorption bandwidth below -10 dB can reach 5.2 GHz and the RL values below -20 dB also cover a wide frequency range of 11.6-14.2 GHz when the coating thickness is 2.3 mm, suggesting its potential application in the treatment of the electromagnetic pollution problem. On the basis of experimental observations, a mechanism has been proposed to understand the enhanced microwave absorption properties of the ZnO@Fe3O4 composites. PMID:26458422

  16. Direct determination of total sulfur in wine using a continuum-source atomic-absorption spectrometer and an air-acetylene flame.

    PubMed

    Huang, Mao Dong; Becker-Ross, Helmut; Florek, Stefan; Heitmann, Uwe; Okruss, Michael

    2005-08-01

    Determination of sulfur in wine is an important analytical task, particularly with regard to food safety legislation, wine trade, and oenology. Hitherto existing methods for sulfur determination all have specific drawbacks, for example high cost and time consumption, poor precision or selectivity, or matrix effects. In this paper a new method, with low running costs, is introduced for direct, reliable, rapid, and accurate determination of the total sulfur content of wine samples. The method is based on measurement of the molecular absorption of carbon monosulfide (CS) in an ordinary air-acetylene flame by using a high-resolution continuum-source atomic-absorption spectrometer including a novel high-intensity short-arc xenon lamp. First results for total sulfur concentrations in different wine samples were compared with data from comparative ICP-MS measurements. Very good agreement within a few percent was obtained. PMID:15999269

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

    NASA Astrophysics Data System (ADS)

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

    2010-04-01

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

  18. Automated continuous monitoring of inorganic and total mercury in wastewater and other waters by flow-injection analysis and cold-vapour atomic absorption spectrometry

    PubMed Central

    Birnie, S. E.

    1988-01-01

    An automated continuous monitoring system for the determination of inorganic and total mercury by flow-injection analysis followed by cold-vapour atomic absorption spectrometry is described. The method uses a typical flow-injection manifold where digestion and reduction of the injected sample takes place. Mercury is removed by aeration from the flowing stream in a specially designed air-liquid separator and swept into a silica cell for absorption measurement at a wavelength of 253.7 nm. A calibration curve up to 10 μg Hg ml-1 using three different path length cells is obtained with a detection limit of 0.02 μg Hg ml-1. The sampling rate of an injection every 3 min produces 20 results per hour from a flowing stream. PMID:18925201

  19. Determination of cadmium and lead at low levels by using preconcentration at fullerene coupled to thermospray flame furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Pereira, M. G.; Pereira-Filho, E. R.; Berndt, H.; Arruda, M. A. Z.

    2004-04-01

    A new and sensitive method for Cd and Pb determinations, based on the coupling of thermospray flame furnace atomic absorption spectrometry and a preconcentrator system, was developed. The procedure comprised the chelating of Cd and Pb with ammonium pyrrolidinedithiocarbamate with posterior adsorption of the chelates on a mixture (40 mg) of C 60 and C 70 at a flow rate of 2.0 ml min -1. These chelates were eluted from the adsorbent by passing a continuous flow of ethanol (80% v/v) at 0.9 ml min -1 to a nickel tube placed in an air/acetylene flame. After sample introduction into the tube by using a ceramic capillary (0.5 mm i.d.), the analytical signals were registered as peak height. Under these conditions, improvement factors in detectability of 675 and 200 were obtained for Cd and Pb, respectively, when compared to conventional flame atomic absorption spectrometry. Spiked samples (mineral and tap waters) and drinking water containing natural concentrations of Cd were employed for evaluating accuracy by comparing the results obtained from the proposed methodology with those using electrothermal atomic absorption spectrometry. In addition, certified reference materials (rye grass, CRM 281 and pig kidney, CRM 186) were also adopted for the accuracy tests. Due to the good linearity ranges for Cd (0.5-5.0 μg l -1) and Pb (10-250 μg l -1), samples with different concentrations could be analyzed. Detection limits of 0.1 and 2.4 μg l -1 were obtained for Cd and Pb, respectively, and RSD values <4.5% were observed ( n=10). Finally, a sample throughput of 24 determinations per hour was possible.

  20. Morphological and spectroscopic investigation of the behavior of permanent iridium modifier deposited on pyrolytic graphite coated and zirconium treated platforms in electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Slaveykova, Vera I.; Lampugnani, Leonardo; Tsalev, Dimiter L.; Sabbatini, L.

    1997-12-01

    In order to better characterise a permanent modifier based on iridium deposited on zirconium or tungsten treated platforms of transversely heated graphite atomizer, and to gain additional information about its chemical behavior directed to an eventual further optimization, a series of experiments were carried out, both by surface techniques such as scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS or ESCA) and X-ray fluorescence (XRF) and by electrothermal atomic absorption spectrometry on the iridium release from unmodified and various other modified pyrolytic graphite platforms. Special attention was paid to the influence of the amount of iridium, zirconium carbide coating of the platform surface and the presence of citric acid on the iridium vaporization during pyrolysis and atomization. The processes of iridium losses during pyrolysis and atomization and peak maximum alignment depend on the amount of the iridium deposited on the pyrolytic graphite coated platforms in the presence of nitric acid. A fractional order of release which suggests an atom vaporization from the surface or edges of the iridium islands was estimated. In the presence of citric acid, mass independence and zero order of the atom release were found. The zirconium treatment of the platform results in change of the spatial distribution of iridium and hence its vaporization. Vaporization temperatures as high as 2100°C, and first order of the process of atom generation were obtained. While it was possible to study the iridium atomization from uncoated and zirconium coated surfaces, evidencing a different order for the release process, the same was not possible for the tungsten coated platforms due to an 'overstabilization' that brought the iridium atomization temperature out of the working range of the instrument used. The different chemical behavior of tungsten and zirconium was also confirmed by XPS investigations. With tungsten, evidence of both WC and WO bonding

  1. Determination of traces of Mo in soils and geological materials by solvent extraction of the molybdenum-thiocyanate complex and atomic absorption.

    PubMed

    Kim, C H; Owens, C M; Smythe, L E

    1974-06-01

    Comprehensive studies of the extraction of the molybdenum-thiocyanate complex with methyl isobutyl ketone have resulted in an improved method for the determination of traces of molybdenum in soils and geological materials by atomic-absorption spectroscopy. The method is applicable in the range 1-500 ppm Mo, with 1-g samples, giving relative standard deviations not exceeding about 8% at a level of 1 ppm. The limit of detection is 0.1 ppm. There are few interferences, and large quantities of iron are without effect. PMID:18961481

  2. Determination of trace amounts of molybdenum in plant tissue by solvent extraction-atomic-absorption and direct-current plasma emission spectrometry.

    PubMed

    Lajunen, L H; Kubin, A

    1986-03-01

    Methods are presented for determination of molybdenum in plant tissue by flame and graphite-furnace atomic-absorption spectrometry and direct-current argon-plasma emission spectrometry. The samples are digested in HNO(3)-H(2)SO(4)-HC1O(4) mixture, and Mo is separated and concentrated by chelation and extraction. Three organic solvents (methyl isobutyl ketone, di-isobutyl ketone and isoamyl alcohol) and two ligands (8-hydroxyquinoline and toluene-3,4-dithiol) were studied. The procedure were tested on pine needle and birch leaf samples. PMID:18964076

  3. Phase-dependent high refractive index without absorption in a four-level inverted-Y atomic system

    SciTech Connect

    Zhi-Qiang Zeng; Fu-Ti Liu; Yu-Ping Wang; Zeng-Hui Gao

    2015-01-31

    We consider a closed four-level inverted-Y system in the presence and the absence of a microwave field. It is found that due to the quantum coherence between the two lower levels, either induced by the spontaneous decay or by the microwave field, the refraction – absorption properties of the system can be modulated by controlling the relative phase of the applied fields in both driven ways. In particular, by properly setting the values of the relative phase, the desirable high index of refraction without absorption can be achieved. (nonlinear optical phenomena)

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

    NASA Astrophysics Data System (ADS)

    Fan, Zhefeng; Zhou, Wei

    2006-07-01

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

  5. Evaluation of microwave digestion and solvent extraction for the determination of trace amounts of selenium in feeds and plant and animal tissues by electrothermal atomic absorption spectrometry.

    PubMed

    Hocquellet, P; Candillier, M P

    1991-05-01

    A sensitive method for the accurate determination of Se in agricultural products at sub-ppm levels is described. The proposed procedure involves the wet oxidation of samples by using a mixture of nitric, sulphuric and perchloric acids, co-extraction of Se and added Pd with diethylammonium N,N-diethyldithiocarbamate in chloroform, and electrothermal atomic absorption spectrometric determination of Se in the organic extract. Atomization and extraction conditions are discussed. Special attention is given to the wet oxidation step, and its advantages in speed and simplicity over conventional heating have been evaluated using an automated microwave digestion system. The results reported, obtained from several reference materials, confirm the accuracy of the method with which a detection limit of 0.002 micrograms g-1 of Se can be achieved. PMID:1877754

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

  7. Permanent iridium modifier deposited on tungsten and zirconium-treated platforms in electrothermal atomic absorption spectrometry: vaporization of bismuth, silver and tellurium

    NASA Astrophysics Data System (ADS)

    Slaveykova, Vera I.; Lampugnani, Leonardo; Tsalev, Dimiter L.; Sabbatini, L.; De Giglio, Elvira

    1999-04-01

    The stabilizing role of permanent iridium modifier deposited on tungsten-treated (WTP) and zirconium-treated (ZrTP) platforms of transversely heated graphite atomizer (THGA) was studied in detail by electrothermal atomic absorption spectrometry (ETAAS) and different surface techniques in model experiments for Ag, Bi and Te. The comparison of the stabilizing efficiency of permanent Ir modifier on WTP and ZrTP and each of the single components, reveals the better effect of Ir on WTP and Ir itself. The extent of analyte losses during pre-atomization and the strength of analyte association with the modifier were estimated by the plotting of `differential vaporization curves'. The existence of double peaks of Ag, Bi and Te in WTP and Ir on WTP was confirmed and possible reasons for their formation were discussed. The absorbance profiles presented as differential curves reveal an existence of at least two different types of precursors determining processes of atom generation. The observed differences in the behavior of Ir permanent modifier on WTP and ZrTP, respectively, were explained by the different extent of iridium-tungsten and iridium-zirconium interaction and surface distribution. XRF, ESCA and SEM studies reveal non-uniform distribution of the modifier on the graphite substrate and the presence of oxide containing species on the surface.

  8. Sorption of trace metals on human hair and application for cadmium and lead pre-concentration with flame atomic absorption determination.

    PubMed

    Sweileh, Jamal A

    2003-02-01

    Human hair shavings were characterized as a sorbent for trace metals. At pH 7.0 metal sorption follows the order Pb(II)>Cd(II)>Cr(VI)>Fe(III)>Cu(II)>Ni(II)>Mn(VI). Metal recovery is quantitative for Pb and Cd after 30 min of equilibration. Recovery of other metals is less quantitative and varies with pH. For example, while Cu is best recovered at pH 5, Ni and Mn are sorbed optimally in the basic pH region. Sorbed metals can be washed off the sorbent with 0.5 mol L(-1) strong mineral acids or more completely with 0.1 mol L(-1) ethylenediaminetetraacetic acid (EDTA). Typical sorption isotherms were obtained for Cd and Pb with sorption capacities of 39 and 26 micromol g(-1), respectively. Hair sorbent was used for 40-fold pre-concentration of Cd and Pb from treated wastewater samples followed by flame atomic absorption spectroscopic (FAAS) determination. Comparison of the data obtained for lead and cadmium by the proposed pre-concentration method with that by graphite furnace atomic absorption spectroscopy (GFAAS) showed 79 to 86% recovery and comparable analytical precision. Common cations and anions at the levels normally present in natural water do not interfere in the proposed pre-concentration-FAAS method. PMID:12589512

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

    NASA Astrophysics Data System (ADS)

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

    2014-12-01

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

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

    PubMed

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

    2014-09-01

    In this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 μm column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin. Ambient temperature storage was found to be harmful to all model proteins, whereas short-term storage up to 14 days could be done in an ordinary refrigerator. Freezing the protein solutions was always complicated and had to be evaluated for each protein in the corresponding solvent. To keep the proteins in their native state a gentle freezing temperature should be chosen, hence liquid nitrogen should be avoided. Furthermore, a high-resolution continuum source atomic absorption spectrometry method was developed to observe the adsorption of proteins on container material and chromatographic columns. Adsorption to any container led to a sample loss and lowered the recovery rates. During the pretreatment and high-performance size-exclusion chromatography, adsorption caused sample losses of up to 33%. PMID:24964383

  11. Direct atomic absorption determination of cadmium and lead in strongly interfering matrices by double vaporization with a two-step electrothermal atomizer

    NASA Astrophysics Data System (ADS)

    Grinshtein, Ilia L.; Vilpan, Yuri A.; Saraev, Alexei V.; Vasilieva, Lubov A.

    2001-03-01

    Thermal pretreatment of a sample using double vaporization in a two-step atomizer with a purged vaporizer makes possible the direct analysis of samples with strongly interfering matrices including solids. A porous-graphite capsule or a filter inserted into the vaporizer is used for solid sample analysis. The technique was used for the direct determination of Cd and Pb in human urine, potatoes, wheat, bovine liver, milk powder, grass-cereal mixtures, caprolactam, bituminous-shale and polyvinyl chloride plastic without chemical modification or any other sample pretreatment.

  12. Interacting He and Ar atoms: Revised theoretical interaction potential, dipole moment, and collision-induced absorption spectra

    SciTech Connect

    Meyer, Wilfried; Frommhold, Lothar

    2015-09-21

    Coupled cluster quantum chemical calculations of the potential energy surface and the induced dipole surface are reported for the He–Ar van der Waals collisional complex. Spectroscopic parameters are derived from global analytical fits while an accurate value for the long-range dipole coefficient D{sub 7} is obtained by perturbation methods. Collision-induced absorption spectra are computed quantum mechanically and compared with existing measurements.

  13. Spectral aspects of the determination of Si in organic and aqueous solutions using high-resolution continuum source or line source flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Kowalewska, Zofia; Pilarczyk, Janusz; Gościniak, Łukasz

    2016-06-01

    High-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) was applied to reveal and investigate spectral interference in the determination of Si. An intensive structured background was observed in the analysis of both aqueous and xylene solutions containing S compounds. This background was attributed to absorption by the CS molecule formed in the N2O-C2H2 flame. The lines of the CS spectrum at least partially overlap all five of the most sensitive Si lines investigated. The 251.611 nm Si line was demonstrated to be the most advantageous. The intensity of the structured background caused by the CS molecule significantly depends on the chemical form of S in the solution and is the highest for the most-volatile CS2. The presence of O atoms in an initial S molecule can diminish the formation of CS. To overcome this S effect, various modes of baseline fitting and background correction were evaluated, including iterative background correction (IBC) and utilization of correction pixels (WRC). These modes were used either independently or in conjunction with least squares background correction (LSBC). The IBC + LSBC mode can correct the extremely strong interference caused by CS2 at an S concentration of 5% w:w in the investigated solution. However, the efficiency of this mode depends on the similarity of the processed spectra and the correction spectra in terms of intensity and in additional effects, such as a sloping baseline. In the vicinity of the Si line, three lines of V were recorded. These lines are well-separated in the HR-CS FAAS spectrum, but they could be a potential source of overcorrection when using line source flame atomic absorption spectrometry (LS FAAS). The expected signal for the 251.625 nm Fe line was not registered at 200 mg L- 1 Fe concentration in the solution, probably due to the diminished population of Fe atoms in the high-temperature flame used. The observations made using HR-CS FAAS helped to establish a "safe" level

  14. A technique coupling the analyte electrodeposition followed by in-situ stripping with electrothermal atomic absorption spectrometry for analysis of samples with high NaCl contents

    NASA Astrophysics Data System (ADS)

    Čánský, Zdeněk; Rychlovský, Petr; Petrová, Zuzana; Matousek, J. P.

    2007-03-01

    A technique coupling the analyte electrodeposition followed by in-situ stripping with electrothermal atomic absorption spectrometry has been developed for determination of lead and cadmium in samples with high salt contents. To separate the analyte from the sample matrix, the analyte was in-situ quantitatively electrodeposited on a platinum sampling capillary serving as the cathode (sample volume, 20 μL). The spent electrolyte containing the sample matrix was then withdrawn, the capillary with the analyte deposited was washed with deionized water and the analyte was stripped into a chemically simple electrolyte (5 g/L NH 4H 2PO 4) by reversing the polarity of the electrodeposition circuit. Electrothermal atomization using a suitable optimized temperature program followed. A fully automated manifold was designed for this coupled technique and the appropriate control software was developed. The operating conditions for determination of Pb and Cd in samples with high contents of inorganic salts were optimized, the determination was characterized by principal analytical parameters and its applicability was verified on analyses of urine reference samples. The absolute limits of detection for lead and cadmium (3 σ criterion) in a sample containing 30 g/L NaCl were 8.5 pg and 2.3 pg, respectively (peak absorbance) and the RSD values amounted to 1.6% and 1.9% for lead (at the 40 ng mL - 1 level) and cadmium (at the 4.0 ng mL - 1 level), respectively. These values (and also the measuring sensitivity) are superior to the results attained in conventional electrothermal atomic absorption spectrometric determination of Pb and Cd in pure solutions (5 g/L NH 4H 2PO 4). The sensitivity of the Pb and Cd determination is not affected by the NaCl concentration up to a value of 100 g/L, demonstrating an efficient matrix removal during the electrodeposition step.

  15. Determination of cadmium, chromium, copper and lead in sediments and soil samples by electrothermal atomic absorption spectrometry using zirconium containing chemical modifiers.

    PubMed

    Acar, Orhan

    2006-05-01

    A method for direct determination of cadmium, chromium, copper and lead in sediments and soil samples by electrothermal atomic absorption spectrometry using Zr, Ir, etylenediamine acetic acid (EDTA), Zr + EDTA, Ir + EDTA, Zr + Ir and Zr + Ir + EDTA as chemical modifiers in 0.5% (v/v) Triton X-100 plus 0.2% (v/v) nitric acid mixture used as diluent was developed. The effects of mass and mass ratio of modifiers on analytes in sample solutions were studied. The optimum masses and mass ratios of modifiers: 20 microg of Zr, 4 microg of Ir, 100 microg of EDTA and 20 microg of Zr + 4 microg of Ir + 100 microg of EDTA, were used to enhance the analyte signals. Pyrolysis and atomization temperatures, atomization and background absorption profiles, characteristic masses, and detection limits of analytes in samples were compared in the presence or absence of a modifier. The detection limits and characteristic masses of analytes in a 0.5% (m/v) dissolved sample (dilution factor of 200 ml g(-1)) obtained with Zr + Ir + EDTA are 8.0 ng g(-1) and 1.2 pg for Cd, 61 ng g(-1) and 4.3 pg for Cr, 32 ng g(-1) and 23 pg for Cu, and 3.4 ng g(-1) and 19 pg for Pb, respectively. The Zr + Ir + EDTA modifier mixture was found to be preferable for the determination of analytes in sediment and soil-certified and standard reference materials. Depending on the sample type, the percent recoveries of analytes were increased from 81 to 103% by using the proposed modifier mixture; the results obtained are in good agreement with the certified values. PMID:16770053

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

    PubMed

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

    2011-08-01

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

  17. Development of a simple method for the determination of lead in lipstick using alkaline solubilization and graphite furnace atomic absorption spectrometry.

    PubMed

    Soares, Aline Rodrigues; Nascentes, Clésia Cristina

    2013-02-15

    A simple method was developed for determining the total lead content in lipstick samples by graphite furnace atomic absorption spectrometry (GFAAS) after treatment with tetramethylammonium hydroxide (TMAH). Multivariate optimization was used to establish the optimal conditions of sample preparation. The graphite furnace heating program was optimized through pyrolysis and atomization curves. An aliquot containing approximately 50mg of the sample was mixed with TMAH and heated in a water bath at 60°C for 60 min. Using Nb as the permanent modifier and Pd as the chemical modifier, the optimal temperatures were 900°C and 1800°C for pyrolysis and atomization, respectively. Under optimum conditions, the working range was from 1.73 to 50.0 μg L(-1), with detection and quantification limits of 0.20 and 0.34 μg g(-1), respectively. The precision was evaluated under conditions of repeatability and intermediate precision and showed standard deviations of 2.37%-4.61% and 4.93%-9.75%, respectively. The % recovery ranged from 96.2% to 109%, and no significant differences were found between the results obtained using the proposed method and the microwave decomposition method for real samples. Lead was detected in 21 tested lipstick samples; the lead content in these samples ranged from 0.27 to 4.54 μg g(-1). PMID:23598019

  18. The determination of total Se in urine and serum by graphite furnace atomic absorption spectrometry using Ir as permanent modifier and in situ oxidation for complete trimethylselenonium recovery.

    PubMed

    Grinberg, Patricia; Gonçalves, Rodrigo Araújo; de Campos, Reinaldo Calixto

    2005-12-01

    The present work evaluated the use of iridium (Ir) as permanent modifier for the determination of total selenium in urine and serum by graphite furnace atomic absorption spectrometry. Concerning urine, the presence of trimethylselenonium (TMSe(+)) was especially considered. Pyrolysis and atomization temperatures of 1,000 and 2,100 degrees C, respectively, were used. For nondigested urine and serum samples, 0.2% v/v HNO(3) and Triton X-100 were used as diluents, respectively, and the same initial platform Ir treatment was effective for up to 1,100 atomization cycles. Good precision [less than 5% relative standard deviation (RSD)] can be achieved with the proposed method. Low TMSe(+) recovery was observed for nondigested urine samples. Thus, if this species is to be considered in urine analysis, a previous external mineralization step was found to be necessary. Alternatively, an in situ oxidation treatment was developed. Detection limits of 8, 10, and 7 mug l(-1) were obtained after dilution, microwave-assisted digestion, and in situ oxidation procedures, respectively. The accuracy of the method was validated by the analysis of certified reference or commercial quality control materials and spiked samples. PMID:16267645

  19. Local atomic structure of chromium bearing precipitates in chromia doped uranium dioxide investigated by combined micro-beam X-ray diffraction and absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Kuri, G.; Mieszczynski, C.; Martin, M.; Bertsch, J.; Borca, C. N.; Delafoy, Ch.

    2014-06-01

    Experimental studies have evidenced the presence of some chromium oxide precipitates in chromia (Cr2O3) doped UO2 fuels, currently being used in many light water reactors. The main objective of this study was to analyze the atomic scale microstructure of these precipitates in a non-destructive way employing modern synchrotron-based X-ray radiation. To investigate UO2 microstructures and chemical compositions of the precipitates an industrial grade fresh Cr2O3-doped UO2 pellet (produced with an initial amount of 0.16 wt.% Cr2O3 powder) was examined using scanning electron microscopy (SEM) and electron probe micro analysis (EPMA). Average grain diameter of the UO2 matrix was measured by SEM image analysis method. Precipitates were detected by EPMA. For all precipitates of micrometer scale analyzed by EPMA the composition was determined to be very close to Cr2O3. The structural property and the next neighbor Cr atomic environment in these precipitates were studied by a combination of more sensitive tools such as micro-focused X-ray diffraction (μ-XRD) and absorption spectroscopy (μ-XAS). According to the XRD data, the chromia precipitates contain structural disorder and have a somewhat distorted lattice structure as compared to that of standard and crystalline α-Cr2O3 hexagonal crystal unit cell. The μ-XAS results provide insight into the local atomic environment of chromium including the oxidation state assignment.

  20. Dynamic linear response of atoms in plasmas and photo-absorption cross-section in the dipole approximation

    NASA Astrophysics Data System (ADS)

    Caizergues, C.; Blenski, T.; Piron, R.

    2016-03-01

    We report results on the self-consistent linear response theory of quantum average-atoms in plasmas. The approach is based on the two first orders of the cluster expansion of the plasma susceptibility. A change of variable is applied, which allows us to handle the diverging free-free transitions contribution in the self-consistent induced electron density and potential. The method is first tested on the case of rare gas isolated neutral atoms. A test of the Ehrenfest-type sum rule is then performed in a case of an actual average-atom in a plasma. At frequencies much higher than the plasma frequency, the sum rule seems to be fulfilled within the accuracy of the numerical methods. Close to the plasma frequency, the method seems not to account for the cold-plasma dielectric function renormalization in the sum rule, which was correctly reproduced in the case of the Thomas-Fermi-Bloch self-consistent linear response. This suggests the need for a better accounting for the outgoing waves in the asymptotic boundary conditions.

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

    NASA Astrophysics Data System (ADS)

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

    2011-02-01

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

  2. Metal Speciation in the ppt Range by HPLC and Diode Laser Atomic Absorption Spectrometry in a Flame.

    PubMed

    Zybin, A; Schaldach, G; Berndt, H; Niemax, K

    1998-12-01

    A simple, compact, and powerful instrument for metal speciation in the ppt range is described. The instrument includes a HPLC module for separation and a diode laser for element-selective detection by wavelength modulation absorption spectrometry in an analytical flame. The high detection power for metal species is due to a two-beam arrangement with logarithmic amplification of the normalized signal, which compensates the laser residual amplitude modulation noise, the offset, and its fluctuation. The analytical figures of merit are demonstrated by measurements of very low concentrations of Cr(VI) in tap water. PMID:21644686

  3. [Study of adsorption and desorption of behaviors of Pb2+ on thiol-modified bentonite by flame atomic absorption spectrometry].

    PubMed

    Chen, Wen; Xiong, Qiong-Xian; Pang, Xiao-Feng; Zhu, Xia-Ping; Han, Mei; Zhao, Qiu-Xiang; Liu, Wen-Hua

    2013-03-01

    A comparative analysis of the functional groups and surface structure of the Ca-bentonite (RB) and thiol-modified bentonite (TMB) were characterized by means of FTIR and SEM. The absorptive property of Pb2+ on TMB and RB and its influential factors was studied and the conditions for the adsorption were optimized by using FAAS method. Then the conditions for desorption of Pb2+ from the TMB by using simulated acid rain were studied and the contrast analysis of absorptive stability of Pb2+ on TMB and RB was given. The results showed that the adsorption rate of Pb2+ by TMB could reach more than 98%, when the initial Pb2+ concentration was 100 mg.L-1, the liquid-solid ratio was 5 g.L-1, pH was 6. 0, KNO3 ionic strength was 0. 1 mol.L-1 and adsorption period was 60min at 25 C. The saturated adsorption capacity of TMB was 67.27 mg.g-1; it's much more than that of RB (9.667 mg.g-1). The adsorption of Pb2+ on TMB follows Langmuir and Freundlich isotherm models well. Desorption experiments of Pb2+ from TMB with simulated acid rain (pH 3. 50) were done, and the desorption rate was 0. The results showed that TMB has a strong adsorption and fixation capacity for PbZ+; it is adapted to lead contaminated soil for chemical remediation. PMID:23705461

  4. Use of cetyltrimethylammonium bromide as surfactant for the determination of copper and chromium in gasoline emulsions by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    dos Santos, Denilson S. S.; Teixeira, Alete P.; Barbosa, José T. P.; Ferreira, Sérgio L. C.; Korn, Maria das Graças A.; Teixeira, Leonardo S. G.

    2007-09-01

    In this work, the use of cetyltrimethylammonium bromide as surfactant for the preparation of oil-in-water emulsions for the determination of Cu and Cr in gasoline by electrothermal atomic absorption spectrometry (ET AAS) was evaluated. The surfactant amount was tested in the range of 25 to 300 mg, added to 2 ml of gasoline, and completed to 10 mL with 0.1% (v/v) nitric acid solution. 150 mg of surfactant was found optimum, and a sonication time of 10 min sufficient to form an oil-in-water emulsion that was stable for several hours. The ET AAS temperature program was established based on pyrolysis and atomization curves. The pyrolysis temperatures were set at 700 and 1300 °C for Cu and Cr, respectively and the selected atomization temperatures were 2400 and 2500 °C. The time and temperature of the drying stage and the atomization time were experimentally tested to provide optimum conditions. The limits of detection were found to be 5 μg L - 1 and 1.5 μg L - 1 for Cu and Cr, respectively in the original gasoline samples. The relative standard deviation (RSD) ranged from 4 to 9% in oil-in-water emulsions spiked with 5 μg L - 1 and 15 μg L - 1 of each metal, respectively. Recoveries varied from 90 to 98%. The accuracy of the proposed method was tested by an alternate procedure using complete evaporation of the gasoline sample. The method was adequate for the determination of Cu and Cr in gasoline samples collected from different gas stations in Salvador, BA, Brazil.

  5. Slurry sampling graphite furnace atomic absorption spectrometry: a preliminary examination of results from an international collaborative study

    NASA Astrophysics Data System (ADS)

    Miller-Ihli, N. J.

    1995-06-01

    An international collaborative study was initiated to evaluate the current state-of-the-art for solid sampling. Samples were sent to 28 laboratories and data were received from 18 collaborators, 16 of which reported slurry results. A preliminary check of performance using NIST SRM 1643c acidified water, showed that at least 13 laboratories were able to provide accurate results within ±10% of the mean certified Pb and Cr concentrations. The focus of this work was slurry analytical data reported by collaborators. Average performance by collaborators for the determination of Pb in NIST SRM 2704 Buffalo River Sediment was 103% recovery based on the mean certified reference value and was 84% recovery based on the mean certified reference value for NRCC PACS-1, a marine estuarine sediment, which was identified to collaborators as an unknown sediment. Average performance by collaborators for Cr in SRM 2704 was 96% based on the mean certified reference value and was 78% recovery based on the mean certified reference value for PACS-1. The use of secondary wavelengths and the importance of analysis of a representative subsample are highlighted. Possible problems leading to inaccurate results being reported by collaborators are discussed including the use of mini-flows, matrix modifiers, low atomization temperatures, short atomization times, and expulsion losses.

  6. A fast and accurate microwave-assisted digestion method for arsenic determination in complex mining residues by flame atomic absorption spectrometry.

    PubMed

    Pantuzzo, Fernando L; Silva, Julio César J; Ciminelli, Virginia S T

    2009-09-15

    A fast and accurate microwave-assisted digestion method for arsenic determination by flame atomic absorption spectrometry (FAAS) in typical, complex residues from gold mining is presented. Three digestion methods were evaluated: an open vessel digestion using a mixture of HCl:HNO(3):HF acids (Method A) and two microwave digestion methods using a mixture of HCl:H(2)O(2):HNO(3) in high (Method B) and medium-pressure (Method C) vessels. The matrix effect was also investigated. Arsenic concentration from external and standard addition calibration curves (at a 95% confidence level) were statistically equal (p-value=0.122) using microwave digestion in high-pressure vessel. The results from the open vessel digestion were statistically different (p-value=0.007) whereas in the microwave digestion in medium-pressure vessel (Method C) the dissolution of the samples was incomplete. PMID:19345010

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

    PubMed

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

    2015-03-01

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

  8. FINGERPRINTING INORGANIC ARSENIC AND ORGANOARSENIC COMPOUNDS IN IN SITU OIL SHALE RETORT AND PROCESS VOTERS USING A LIQUID CHROMATOGRAPH COUPLED WITH AN ATOMIC ABSORPTION SPECTROMETER AS A DETECTOR

    SciTech Connect

    Fish, Richard H.; Brinckman, Frederick E.; Jewett, Kenneth L.

    1981-07-01

    Inorganic arsenic and organoarsenic compounds were speciated in seven oil shale retort and process waters, including samples from simulated, true and modified in situ processes, using a high performance liquid chromatograph automatically coupled to a graphite furnace atomic absorption detector. The molecular forms of arsenic at ppm levels (({micro}g/mL) in these waters are identified for the first time, and shown to include arsenate, methylarsonic acid and phenylarsonic acid. An arsenic-specific fingerprint chromatogram of each retort or process water studied has significant impliestions regarding those arsenical species found and those marginally detected, such as dimethylarsinic acid and the suspected carcinogen arsenite. The method demonstrated suggests future means for quantifying environmental impacts of bioactive organometal species involved in oil shale retorting technology.

  9. An improved method for the determination of trace levels of arsenic and antimony in geological materials by automated hydride generation-atomic absorption spectroscopy

    USGS Publications Warehouse

    Crock, J.G.; Lichte, F.E.

    1982-01-01

    An improved, automated method for the determination of arsenic and antimony in geological materials is described. After digestion of the material in sulfuric, nitric, hydrofluoric and perchloric acids, a hydrochloric acid solution of the sample is automatically mixed with reducing agents, acidified with additional hydrochloric acid, and treated with a sodium tetrahydroborate solution to form arsine and stibine. The hydrides are decomposed in a heated quartz tube in the optical path of an atomic absorption spectrometer. The absorbance peak height for arsenic or antimony is measured. Interferences that exist are minimized to the point where most geological materials including coals, soils, coal ashes, rocks and sediments can be analyzed directly without use of standard additions. The relative standard deviation of the digestion and the instrumental procedure is less than 2% at the 50 ??g l-1 As or Sb level. The reagent-blank detection limit is 0.2 ??g l-1 As or Sb. ?? 1982.

  10. Trace and Essential Elements Analysis in Cymbopogon citratus (DC.) Stapf Samples by Graphite Furnace-Atomic Absorption Spectroscopy and Its Health Concern.

    PubMed

    Anal, Jasha Momo H

    2014-01-01

    Cymbopogon citratus (DC.) Stapf commonly known as lemon grass is used extensively as green tea and even as herbal tea ingredient across the world. Plants have the ability to uptake metals as nutrient from the soil and its environment which are so essential for their physiological and biochemical growth. Concentrations of these twelve trace elements, namely, Mg, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Mo, As, Cd, and Pb, are analysed by graphite furnace-atomic absorption spectroscopy (GF-AAS) and are compared with the permissible limits of FAO/WHO, ICMR, and NIH, USA, which are found to be within permissible limits. Toxic metals like As, Cd, and Pb, analysed are within the tolerable daily diet limit and at low concentration. PMID:25525430

  11. Solid-phase extraction and atomic absorption spectrometric determination of cobalt using an octadecyl bonded silica membrane disk modified with Cyanex 272.

    PubMed

    Karve, Manjusha; Gholave, Jayram V

    2011-01-01

    A simple SPE method for determination of cobalt(II) using a C18 bonded silica membrane disk impregnated with Cyanex 272 has been developed. Cobalt(II) was quantitatively sorbed at pH 6.0 from a sample solution and eluted using 10.0 mL 1.0 M HNO3 prior to its flame atomic absorption spectrometric determination. The influence of eluting agents, the minimum volume and maximum flow rate of the eluent, and interfering ions on cobalt(II) was studied. The method developed for cobalt(II) had an LOD of 1.4 microg/L, and a preconcentration factor > 200 with an RSD of 0.6%. The reusability of the modified disk was for 40 cycles. The method was applied for the determination of cobalt in certified samples, urine, and industrial sludge samples. PMID:21563699

  12. Octadecyl bonded silica membrane disk modified with Cyanex302 for separation and flame atomic absorption spectrometric determination of nickel from tap water and industrial effluent.

    PubMed

    Karve, Manjusha; Rajgor, Reeta V

    2009-07-15

    A simple and reliable method based upon impregnation of Cyanex302 on octadecyl bonded silica membrane disk has been developed for separation and atomic absorption spectrometric determination of nickel. The influence of various parameters like aqueous phase pH, flow rate and volume of eluent were investigated systematically to optimize the conditions for quantitative sorption and desorption of nickel. The break through volume for nickel was greater than 1.0 dm(3), enrichment factor more than 100 and a detection limit of 2.1 microg dm(-3) was achieved. The method applied for detection of nickel in tap water and effluent sample had a relative standard deviation (R.S.D.) of 0.4%. PMID:19124200

  13. [Determination of total mercury in water samples, sediments and solids in suspension in aquatic systems by cold-vapor atomic absorption spectrophotometry].

    PubMed

    Vieira, J L; Passarelli, M M

    1996-06-01

    The use of metallic mercury in the extraction and concentration of gold causes the discarding of tons of this metal in the environment, leading to a considerable increase in the natural levels of the same and the contamination of the surrounding areas. Thus it is extremely important to monitor the presence of this metal in various sectors of the environment with a view aiming to preventing human exposure to excessive concentrations which can result in serious episodes of mercury poisoning. It is also important to estimate the possibility of river sediments becoming potential sources of contamination of human beings. The determination of total mercury was undertaken by using cold vapor atomic absorption spectrometry. River waters, as well as sediments and suspended solids were used as samples for the standardization of the analytical procedure. Later on, this method was tested on samples originating in gold mining areas for the purpose of assessing its validity. PMID:9110471

  14. Evaluation of cadmium in greenhouse soils and agricultural products of Jiroft (Iran) using microwave digestion prior to atomic absorption spectrometry determination.

    PubMed

    Afzali, Daryoush; Fathirad, Fariba; Afzali, Zahra; Majdzadeh-Kermani, Seyed Mohammad Javad

    2015-03-01

    This study determines total levels of potentially toxic trace element, Cd (II) in Jiroft (Kerman, Iran) greenhouse soil and agricultural products that are grown in these greenhouses (tomatoes and cucumbers), and the comparison with soil outside of greenhouse using microwave digestion prior to flame atomic absorption spectrometry determination. The results show that the cadmium concentration in greenhouse soil is 0.9-1.9 mg kg(-1) and out of greenhouse is 0.4-1.0 mg kg(-1). Also, cadmium concentration range in tomatoes and cucumbers is about 0.07-0.40 mg kg(-1). The obtained results show that the concentration of this metal in greenhouse soil is higher than outside soil samples and is below the safe limit. PMID:25697307

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

    PubMed

    Goudarzi, Nasser

    2009-02-11

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

  16. Trace and Essential Elements Analysis in Cymbopogon citratus (DC.) Stapf Samples by Graphite Furnace-Atomic Absorption Spectroscopy and Its Health Concern

    PubMed Central

    Anal, Jasha Momo H.

    2014-01-01

    Cymbopogon citratus (DC.) Stapf commonly known as lemon grass is used extensively as green tea and even as herbal tea ingredient across the world. Plants have the ability to uptake metals as nutrient from the soil and its environment which are so essential for their physiological and biochemical growth. Concentrations of these twelve trace elements, namely, Mg, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Mo, As, Cd, and Pb, are analysed by graphite furnace-atomic absorption spectroscopy (GF-AAS) and are compared with the permissible limits of FAO/WHO, ICMR, and NIH, USA, which are found to be within permissible limits. Toxic metals like As, Cd, and Pb, analysed are within the tolerable daily diet limit and at low concentration. PMID:25525430

  17. Studies on effective atomic numbers for photon energy absorption and electron density of some narcotic drugs in the energy range 1 keV-20 MeV

    NASA Astrophysics Data System (ADS)

    Gounhalli, Shivraj G.; Shantappa, Anil; Hanagodimath, S. M.

    2013-04-01

    Effective atomic numbers for photon energy absorption ZPEA,eff, photon interaction ZPI,eff and for electron density Nel, have been calculated by a direct method in the photon-energy region from 1 keV to 20 MeV for narcotic drugs, such as Heroin (H), Cocaine (CO), Caffeine (CA), Tetrahydrocannabinol (THC), Cannabinol (CBD), Tetrahydrocannabivarin (THCV). The ZPEA,eff, ZPI,eff and Nel values have been found to change with energy and composition of the narcotic drugs. The energy dependence ZPEA,eff, ZPI,eff and Nel is shown graphically. The maximum difference between the values of ZPEA,eff, and ZPI,eff occurs at 30 keV and the significant difference of 2 to 33% for the energy region 5-100 keV for all drugs. The reason for these differences is discussed.

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

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

    In the present work, spectral interferences on the determination of lead in fertilizer and limestone samples were investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry at the main analytical lines: 217.001 and 283.306 nm. For these investigations, samples were introduced into the furnace as slurry together with a mixture of Pd and Mg as chemical modifier. Spectral interferences were observed for some samples at both analytical lines. In order to verify whether a wet digestion procedure would avoid these interferences, a reference method for wet digestion of fertilizers was employed as an alternative sample preparation procedure. However, the same interferences were also observed in the digested samples. In order to identify and eliminate the fine-structured background using a least-squares background correction, reference spectra were generated using the combination of different species. The use of the latter technique allowed the elimination of spectral interferences for most of the investigated samples, making possible the determination of lead in fertilizer and limestone samples free of interferences. The best results were found using a reference spectrum of NH4H2PO4 at 217.001 nm, and a mixture of H2SO4 + Ca and HNO3 + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material “Trace Elements in Multi-Nutrient Fertilizer”. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part.

  19. Direct solid sample analysis with graphite furnace atomic absorption spectrometry—a fast and reliable screening procedure for the determination of inorganic arsenic in fish and seafood.

    PubMed

    Zmozinski, Ariane V; Llorente-Mirandes, Toni; Damin, Isabel C F; López-Sánchez, José F; Vale, Maria Goreti R; Welz, Bernhard; Silva, Márcia M

    2015-03-01

    Direct solid sample analysis with graphite furnace atomic absorption spectrometry (SS-GF AAS) was investigated initially with the intention of developing a method for the determination of total As in fish and other seafood. A mixture of 0.1% Pd+0.06% Mg+0.06% Triton X-100 was used as the chemical modifier, added in solution over the solid samples, making possible the use of pyrolysis and atomization temperatures of 1200 °C and 2400 °C, respectively. The sample mass had to be limited to 0.25 mg, as the integrated absorbance did not increase further with increasing sample mass. Nevertheless, the recovery of As from several certified reference materials was of the order of 50% lower than the certified value. Strong molecular absorption due to the phosphorus monoxide molecule (PO) was observed with high-resolution continuum source AAS (HR CS AAS), which, however, did not cause any spectral interference. A microwave-assisted digestion with HNO3/H2O2 was also investigated to solve the problem; however, the results obtained for several certified reference materials were statistically not different from those found with direct SS-GF AAS. Accurate values were obtained using inductively coupled plasma mass spectrometry (ICP-MS) to analyze the digested samples, which suggested that organic As compounds are responsible for the low recoveries. HPLC-ICP-MS was used to determine the arsenobetaine (AB) concentration. Accurate results that were not different from the certified values were obtained when the AB concentration was added to the As concentration found by SS-GF AAS for most certified reference materials (CRM) and samples, suggesting that SS-GF AAS could be used as a fast screening procedure for inorganic As determination in fish and seafood. PMID:25618661

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

    NASA Astrophysics Data System (ADS)

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

    2005-06-01

    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.

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

    PubMed

    Gonzáles, A P S; Firmino, M A; Nomura, C S; Rocha, F R P; Oliveira, P V; Gaubeur, I

    2009-03-23

    The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 molL(-1) HNO(3). The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 microgL(-1), with a detection limit estimated as 3 microgL(-1) at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n=20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111% range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level. PMID:19264168

  2. Mineral content of vertebral trabecular bone: accuracy of dual energy quantitative computed tomography evaluated against neutron activation analysis and flame atomic absorption spectrometry.

    PubMed

    Louis, O; Van den Winkel, P; Covens, P; Schoutens, A; Osteaux, M

    1994-01-01

    The goal of this study was to evaluate the accuracy of preprocessing dual energy quantitative computed tomography (QCT) for assessment of trabecular bone mineral content (BMC) in lumbar vertebrae. The BMC of 49 lumbar vertebrae taken from 16 cadavers was measured using dual energy QCT with advanced software and hardware capabilities, including an automated definition of the trabecular region of interest (ROI). The midvertebral part of each vertebral body was embedded in a polyester resin and, subsequently, an experimental ROI was cut out using a scanjet image transmission procedure and a computer-assisted milling machine in order to mimic the ROI defined on QCT. After low temperature ashing, the experimental ROIs reduced to a bone powder were submitted to either nondestructive neutron activation analysis (n = 49) or to flame atomic absorption spectrometry (n = 45). BMC obtained with neutron activation analysis was closely related (r = 0.896) to that derived from atomic absorption spectrometry, taken as the gold standard, with, however, a slight overestimation. BMC values measured by QCT were highly correlated with those assessed using the two reference methods, all correlation coefficients being > 0.841. The standard errors of the estimate ranged 47.4-58.9 mg calcium hydroxyapatite in the regressions of BMC obtained with reference methods against BMC assessed by single energy QCT, 47.1-51.9 in the regressions involving dual energy QCT. We conclude that the trabecular BMC of lumbar vertebrae can be accurately measured by QCT and that the superiority in accuracy of dual energy is moderate, which is possible a characteristic of the preprocessing method. PMID:8024849

  3. An electrochemical flow-cell for permanent modification of graphite tube with palladium for mercury determination by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Moreno, Ruben G. M.; de Oliveira, Elisabeth; Pedrotti, Jairo J.; Oliveira, Pedro V.

    2002-04-01

    An electrochemical procedure for palladium deposition on the inner surface of pyrolytic graphite-coated tubes for permanent chemical modification and a cold vapor generation system for the pre-concentration and determination of mercury trace levels in rain, potable, and non-potable water and lake sediment by electrothermal atomic absorption spectrometry is proposed. A tubular electrochemical flow-cell was assembled on the original geometry of the graphite tube, which operated as the working electrode. A stainless steel tube, positioned downstream from the working electrode, was used as the auxiliary electrode. The applied potential was measured against a micro Ag/AgCl (sat) reference electrode inserted in the auxiliary electrode. Palladium solution in acetate buffer (100 mmol l -1, pH=4.8), flowing at 0.5 ml min -1 for 60 min was used to perform the electrodeposition. A homemade cold vapor generation system composed of a peristaltic pump, an injector-commutator, a flow meter and a disposable polyethylene gas-liquid separator flask (approx. 4.0 ml volume) were used. Volumes of 1.0 ml of reagent (2.0% w/v NaBH 4 in 0.10 mol l -1 of NaOH) and 1.0 ml of reference or sample solution in 0.25 mol l -1 of HNO 3 were carried to the gas-liquid separator using the peristaltic pump. The mercury vapor was carried out to the modified graphite tube by argon flow (200 ml min -1), and pre-concentrated for 120 s. The characteristic mass for 1.0 ml of reference solution was 26 pg (R.S.D.=0.12%, n=5). The detection limit obtained was 93 pg ( n=20, 3δ). The reliability of the entire procedure was confirmed by addition and recovery tests and cold vapor atomic absorption spectrometry.

  4. Silver and lanthanum as effective modifiers in trace determination of cadmium in nickel-base alloys by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Tsai, Suh-Jen Jane; Chang, Li-Lin; Chang, Shiow-Ing

    1997-01-01

    Trace cadmium in nickel-base superalloys was determined by a stabilized temperature platform furnace using atomic absorption spectrometry with a deuterium arc background correction system. The volatility of cadmium limits the pyrolysis temperature. This prevents the removal of the interfering alloy matrix at the thermal pretreatment step. Hence, an enormously high background signal has been observed. Chemical modifiers including ammonium citrate, 1-(2-pyridylazo)-naphthol, 4-(2pyridylazo)resorcinol, 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol, Triton-X 100, EDTA, potassium nitrate, palladium nitrate, magnesium nitrate, aluminum chloride, ammonium dihydrogen phosphate, lanthanum oxide, lanthanum chloride and silver nitrate have been studied. Matrix interferences were effectively reduced by silver and lanthanum. The 100-300°C increase in the pyrolysis temperature effectively reduced the non-specific absorption from the alloy matrix. Interferences from foreign ions were also investigated. The merit of the proposed method was increased by the excellent agreement between the certified and the experimental values of Cd in the standard reference material, IN100, and the recovery obtained (100-104%). The precision of six successive replicate measurements was 4.9% with Ag modifier and 2.5% with La modifier, respectively. The results of analysing Tracealloy B were also satisfactory.

  5. Synthesis of a new molecularly imprinted polymer for sorption of the silver ions from geological and antiseptic samples for determination by flame atomic absorption spectrometry.

    PubMed

    Hashemi-Moghaddam, Hamid; Yahyazadeh, Faegheh; Vardini, Mohammad Taghi

    2014-01-01

    A new molecularly imprinted polymer (MIP) was synthesized using methacrylic acid (functional monomer), ethylene glycol dimethacrylate (crosslinker), 2,2'-azobisisobutironitril (initiator), silver (Ag) dithizone complex (template), and chloroform (porogenic solvent). This process was a noncovalent, bulk, thermal radical-polymerization. To compare the performance of this polymer, control polymer (nonimprinted polymer) was prepared under well-defined conditions without the use of a template. Extraction experiments were performed on the MIP and a nonimprinted polymer. Then, various parameters were optimized, such as pH, time, concentration of sample, and type of eluent for elution of Ag from polymer. In addition, interfering effects were investigated on the absorption of Ag by the MIP. This polymer was used for the rapid extraction and preconcentration of Ag from an antiseptic and geological sample. Finally, the amount of Ag was measured by flame atomic absorption spectrometry after preconcentration by the synthesized MIP, and results were compared with a direct inductively coupled plasma method. The results showed high performance of this method in preconcentration of Ag. PMID:25902996

  6. Estimation of effective atomic numbers of some solutions for photon energy absorption in the energy region 0.2-1.5 MeV: An alternative method

    NASA Astrophysics Data System (ADS)

    Kurudirek, Murat

    2011-12-01

    The effective atomic numbers (ZPEAeff), which are used to describe the composite materials in terms of equivalent elements, have been estimated in some solutions for photon energy absorption in the energy region 0.2-1.5 MeV. Since the mass energy absorption (μen/ρ) and mass attenuation coefficients (μ/ρ) remain more or less the same for any given material in the photon energy region 0.2-1.5 MeV where Compton scattering is the main dominant photon interaction process, semi-empirical relations including both μen/ρ and μ/ρ have been constituted as a function of energy. These parameters were then used to obtain ZPEAeff with the help of a Z-wise interpolation procedure. The results were compared with the experimental as well as other theoretical estimations wherever possible. Consequently, the present method is found to be readily applicable to the given solutions in order to estimate accurate values of ZPEAeff for which it is not possible to directly obtain experimentally using the conventional gamma spectrometry system.

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

    PubMed

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

    2012-05-21

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

  9. Excitonic absorption of million-atom (In,Ga)As/GaAs self-assembled quantum dots

    NASA Astrophysics Data System (ADS)

    Narvaez, Gustavo A.; Zunger, Alex

    2006-03-01

    We calculate the optical absorption spectra of (In,Ga)As/GaAs self-assembled quantum dots by adopting an atomistic pseudopotential approach to calculate the single-particle electron and hole confined states of the dot followed by a calculation of the neutral exciton X^0 states |&(ν)circ;(X^0)> based on the configuration-interaction approach. We predict three types of allowed transitions that would be naively expected to be forbidden. (i) Transitions involving low-lying electron and hole states that are forbidden in simple effective mass models (e.g. 1S-2S, 1S-1P) become allowed by virtue of single-particle band-mixing. (ii) Transitions involving a deep hole state, with a mixture of heavy-hole and light-hole character, and an electron in the lowest state are found to have oscillator strengths that are comparable in magnitude to those of the expected allowed transitions. Thus, simple models based on single-band envelope functions cannot predict these transitions. (iii) Transitions whose intensity is large due to many-body borrowing of oscillator strength from allowed transitions. The transitions in (i) and (ii) appear, respectively, as low-energy and high-energy satellites of the allowed P-P transitions, as observed in PLE.

  10. Using X-ray absorption spectra to monitor specific radiation damage to anomalously scattering atoms in macromolecular crystallography.

    PubMed

    Oliéric, V; Ennifar, E; Meents, A; Fleurant, M; Besnard, C; Pattison, P; Schiltz, M; Schulze-Briese, C; Dumas, P

    2007-07-01

    Radiation damage in macromolecular crystals is not suppressed even at 90 K. This is particularly true for covalent bonds involving an anomalous scatterer (such as bromine) at the 'peak wavelength'. It is shown that a series of absorption spectra recorded on a brominated RNA faithfully monitor the extent of cleavage. The continuous spectral changes during irradiation preserve an 'isosbestic point', each spectrum being a linear combination of 'zero' and 'infinite' dose spectra. This easily yields a good estimate of the partial occupancy of bromine at any intermediate dose. The considerable effect on the near-edge features in the spectra of the crystal orientation versus the beam polarization has also been examined and found to be in good agreement with a previous study. Any significant influence of the (C-Br bond/beam polarization) angle on the cleavage kinetics of bromine was also searched for, but was not detected. These results will be useful for standard SAD/MAD experiments and for the emerging 'radiation-damage-induced phasing' method exploiting both the anomalous signal of an anomalous scatterer and the 'isomorphous' signal resulting from its cleavage. PMID:17582167

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

    PubMed

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

    2016-04-01

    High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. PMID:26838392

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

    NASA Astrophysics Data System (ADS)

    Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero

    2014-11-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

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

  14. Direct determination of phosphorus in different food samples by means of solid sampling electrothermal atomic absorption spectrometry using Pd+Ca chemical modifier

    NASA Astrophysics Data System (ADS)

    Coşkun, Nihat; Akman, Süleyman

    2005-03-01

    In this study, direct determination of phosphorus in different food samples (milk powder, banana, and dried banana) and in various standard reference materials (apple leaves, bovine liver, pine needles) using solid sampling electrothermal atomic absorption spectrometry was investigated. Aqueous standards were used for all determinations. 5 μg Pd+5 μg Ca modifier mixture was used in all experiments. Pyrolysis temperature and atomization temperature were 1100 °C and 2500 °C, respectively. High background was reduced by applying a cool-down step in the furnace program. The accuracy of solid sampling results was checked by determination of the phosphorus content after dissolving samples. There was no significant error between results found by solid sampling and solution techniques. In addition solid certified materials were investigated. There were no significant differences between the phosphorus content of CRM and results obtained. The limit of detection, based on three times the standard deviation was 0.018 μg P.

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

    NASA Astrophysics Data System (ADS)

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

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 °C and 2400 °C, respectively. Slopes of calibration curves (50-750 pg Cr, R2 > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 μg g- 1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g- 1 Cr. The limit of detection was 3.3 ng g- 1 Cr.

  16. Ultra-trace determination of lead in water and food samples by using ionic liquid-based single drop microextraction-electrothermal atomic absorption spectrometry.

    PubMed

    Manzoori, Jamshid L; Amjadi, Mohammad; Abulhassani, Jafar

    2009-06-30

    An improved single drop microextraction procedure was developed for the preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry. Ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6], was used as an alternative to volatile organic solvents for extraction. Lead was complexed with ammonium pyrroldinedithiocarbamate (APDC) and extracted into a 7-microL ionic liquid drop. The extracted complex was directly injected into the graphite furnace. Several variables affecting microextraction efficiency and ETAAS signal, such as pyrolysis and atomization temperature, pH, APDC concentration, extraction time, drop volume and stirring rate were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enhancement factor were 0.015 microg L(-1) and 76, respectively. The relative standard deviation (RSD) for five replicate determinations of 0.2 microg L(-1) Pb was 5.2%. The developed method was validated by the analysis of certified reference materials and applied successfully to the determination of lead in several real samples. PMID:19463561

  17. Ionic liquid-based single drop microextraction combined with electrothermal atomic absorption spectrometry for the determination of manganese in water samples.

    PubMed

    Manzoori, Jamshid L; Amjadi, Mohammad; Abulhassani, Jafar

    2009-02-15

    Room temperature ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C(4)MIM][PF(6)], was used as an alternative to volatile organic solvents in single drop microextraction-electrothermal atomic absorption spectrometry (SDME-ETAAS). Manganese was extracted from aqueous solution into a drop of the ionic liquid after complextaion with 1-(2-thiazolylazo)-2-naphthol (TAN) and the drop was directly injected into the graphite furnace. Several variables affecting microextraction efficiency and ETAAS signal, such as pyrolysis and atomization temperature, pH, TAN concentration, extraction time, drop volume and stirring rate were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enhancement factor were 0.024 microg L(-1) and 30.3, respectively. The relative standard deviation (RSD) for five replicate determinations of 0.5 microg L(-1) Mn(II) was 5.5%. The developed method was validated by the analysis of a certified reference material (NIST SRM 1643e) and applied successfully to the determination of manganese in several natural water samples. PMID:19084676

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

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

    PubMed

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

    2016-08-15

    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. PMID:27260436

  20. An improved impaction-graphite furnace system for the direct and near real-time determination of cadmium, chromium, lead and manganese in aerosols and cigarette smoke by simultaneous multielement atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Lee, Yong-Ill; Smith, Mark V.; Indurthy, Suneetha; Deval, Anupama; Sneddon, Joseph

    1996-01-01

    The design, operating characteristics, and preliminary evaluation of an improved impaction-graphite furnace system, based on a theoretical study of particle size collected, are presented. After direct collection, the graphite furnace from the system is inserted in an atomic absorption spectrometer for analysis by simultaneous multielement atomic absorption spectrometry. This system has the potential for the direct and near real-time (few minutes) determination of metals in aerosols. The system has been preliminarily evaluated using aqueous solutions of chromium, and has then been applied to the determination of cadmium, chromium, lead, and manganese in cigarette smoke. Results show an increase ranging from almost five (lead) to sixteen (cadmium) over background levels.