WorldWideScience

Sample records for atomic emission spectrometry

  1. Flame emission, atomic absorption and fluorescence spectrometry

    International Nuclear Information System (INIS)

    Horlick, G.

    1980-01-01

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

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

    Science.gov (United States)

    Horlick, Gary

    1984-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

    Tanaka, Satoko; Chayama, Kenji

    2009-01-01

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

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

    Science.gov (United States)

    Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

    1987-01-01

    Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

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

    International Nuclear Information System (INIS)

    Montaser, A.

    1993-01-01

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

    LI Jianqiang; LU Yiqiang; JIANG Wei

    2005-01-01

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

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

    International Nuclear Information System (INIS)

    Wong, K.L.

    1981-01-01

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

  10. Sample Preprocessing For Atomic Spectrometry

    International Nuclear Information System (INIS)

    Kim, Sun Tae

    2004-08-01

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

  11. Multielement determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Sawatari, Hideyuki; Asano, Takaaki; Hu, Xincheng; Saizuka, Tomoo; Itoh, Akihide; Hirose, Akio; Haraguchi, Hiroki

    1995-01-01

    The rapid determination of rare earth elements (REEs) has been investigated by an on-line system of high performance liquid chromatography/multichannel inductively coupled plasma atomic emission spectrometry. In the present system, all REEs could be detected simultaneously in a single chromatographic measurement without spectral interferences. Utilizing a cation exchange column and 2-hydroxy-2-methylpropanoic acid aqueous solution as the mobile phase, the detection limits of 0.4-30 ng ml -1 for all REEs were obtained. The system was applied to the determination of REEs in geological standard rock samples and rare earth impurities in high purity rare earth oxides. The REEs in standard rocks could be determined by the present HPLC/ICP-AES system without pretreatment after acid digestion, although the detection limits were not sufficient for the analysis of rare earth oxides. (author)

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

    International Nuclear Information System (INIS)

    Matsushige, I.

    1990-01-01

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

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

    International Nuclear Information System (INIS)

    Yoshida, K.; Haraguchi, H.

    1984-01-01

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

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

    International Nuclear Information System (INIS)

    Mermet, J.M.

    1991-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1977-12-01

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

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

    Science.gov (United States)

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

    2010-08-03

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

  17. Atomic mass spectrometry

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1997-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-10-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    1976-01-01

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

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

    International Nuclear Information System (INIS)

    Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-06-15

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

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

    Science.gov (United States)

    Ombaba, Jackson M.

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

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

    African Journals Online (AJOL)

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

  6. Study of uranium matrix interference on ten analytes using inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ghazi, A.A.; Qamar, S.; Atta, M.A. (A.Q. Khan Research Labs., Rawalpindi (Pakistan))

    1993-08-01

    Maximum allowable concentrations of 12 elements in uranium hexafluoride feed for enrichment to reactor grade material (about 3%), vary from 1 to 100 ppm ([mu]g/g). Using an inductively coupled plasma atomic emission spectrometer, 51 lines of tine of these elements (B, Cr, Mo, P, Sb, Si, Ta, Ti, V and W) has been studied with a uranium matrix to investigate the matrix interference on the basis of signal to background (SBR), and background to background ratios (BBR). Detection limits and limits of quantitative determination (LQDs) were calculated for these elements in a uranium matrix using SBR and relative standard deviation of the background signal (RSD[sub B]) approach. In almost all cases, the uranium matrix interference reduces the SBRs to the extent that direct trace analysis is impossible. A uranium sample having known concentrations of impurities (around LQDs) was directly analysed with results that showed reasonable accuracy and precision. (Author).

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-01-02

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    1990-10-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

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

    1997-01-01

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

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

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1991-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-05-30

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-07-15

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-12-01

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-08-01

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

  2. Determination of the mineral compositions of in six beans by microwave digestion with inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Yan, Q.; Yang, L.; Chen, S.; Liu, X.; Ma, X.

    2012-01-01

    In the study, microwave digestion procedure optimized was applied for digesting beans. Nineteen mineral element concentrations were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The result indicated detection limits for the 19 elements were less than 0.0998, and relative standard deviations were 1.01% - 5.02% for all the elements, and recoveries were 90.89% - 104.55% by adding standard recovery experiment. The study showed the beans selected were abundant in mineral element contents in human nutrition, determination mineral element contents by ICP-AES with microwave digestion technology were a lot of merits of small environmental pollution, fast and accurate determination result, which could satisfy the examination request of bean samples. The results provided evidence that the six beans were a good source of K, P, Mg and Ca. This study is to give important reference value to people due to individual differences by adjusting the dietary to complement the different mineral elements. (author)

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Science.gov (United States)

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

    2011-10-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-10-15

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  7. Determination of boron in waters by using methyl borate generation and flame atomic-emission spectrometry

    International Nuclear Information System (INIS)

    Castillo, J.R.; Mir, J.M.; Martinez, C.; Bendicho, C.

    1985-01-01

    An improved method is proposed for the determination of boron in waters. The esterification reaction between boric acid and methanol in a concentrated sulphuric acid medium and the vaporisation of the methyl borate formed (boiling-point, 68 C) are used in the determination by boron by measuring the emission of the BO 2 radical at 548 nm. This reaction is carried out in a simple and inexpensive generator, designed for this purpose, and the heat developed in it causes the rapid volatilisation of the methyl borate. Thus no collection systems or carrier gas are required. The proposed method gives an improved detection limit and it can be applied to the determination of boron in water samples. It is both rapid and highly selective. (author)

  8. Internal standardization in atomic-emission spectrometry using inductively coupled plasma

    International Nuclear Information System (INIS)

    Moore, G.L.

    1985-01-01

    The principle of internal standardization has been used in quantitative analytical emission spectroscopy since 1925 to minimize the errors arising from fluctuations in sample preparation, excitation-source conditions, and detection parameters. Although modern spectroscopic excitation sources are far more stable and electronic detection methods are more precise than before, the system for the introduction of the sample in spectrometric analysis using inductively coupled plasma (ICP) introduces significant errors, and internal standardization can still play a useful role in improving the overall precision of the analytical results. The criteria for the selection of the elements to be used as internal standards in arc and spark spectrographic analysis apply to a much lesser extent in ICP-spectrometric analysis. Internal standardization is recommended for use in routine ICP-simultaneous spectrometric analysis to improve its accuracy and precision and to provide a monitor for the reassurance of the analyst. However, the selection of an unsuitable reference element can result in misuse of the principle of internal standardization and, although internal standardization can be applied when a sequential monochromator is used, the main sources of error will not be minimized

  9. Trends in tungsten coil atomic spectrometry

    Science.gov (United States)

    Donati, George L.

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

  10. Zeeman atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Hadeishi, T.; McLaughlin, R.

    1978-08-01

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

  11. Atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Haswell, S.J.

    1991-01-01

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

  12. Development of inductively coupled plasma atomic emission spectrometry for palladium and Rhodium determination in platinum-based alloy

    International Nuclear Information System (INIS)

    Kovacevic, R.; Todorovic, M.; Manojlovic, D.; Mutic, J.

    2008-01-01

    Inductively coupled plasma atomic emission spectroscopy with internal standardization was applied for the analysis of an in-house reference platinum alloy containing palladium and rhodium (approximately 5% by weight). In order to compensate for variations in signal recovery due to matrix interferences, and therefore to improve the precision, platinum. the major component, was chosen as an internal standard. Quantitative analysis was based on calibration using a set of matrix-matched calibration standards with and without employing the internal standard. These results were compared with those obtained by X-ray fluorescence spectroscopy. The results for both techniques were in a good agreement, although the precision was slightly better in the inductively coupled plasma atomic emission spectroscopy technique, with or without the internal standard

  13. Semi-automated technique for the separation and determination of barium and strontium in surface waters by ion exchange chromatography and atomic emission spectrometry

    International Nuclear Information System (INIS)

    Pierce, F.D.; Brown, H.R.

    1977-01-01

    A semi-automated method for the separation and the analysis of barium and strontium in surface waters by atomic emission spectrometry is described. The method employs a semi-automated separation technique using ion exchange and an automated aspiration-analysis procedure. Forty specimens can be prepared in approximately 90 min and can be analyzed for barium and strontium content in 20 min. The detection limits and sensitivities provided by the described technique are 0.003 mg/l and 0.01 mg/l respectively for barium and 0.00045 mg/l and 0.003 mg/l respectively for strontium

  14. Use of oxidative and reducing vapor generation for reducing the detection limits of iodine in biological samples by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Vtorushina, Eh.A.; Saprykin, A.I.; Knapp, G.

    2009-01-01

    Procedures of microwave combustion in an oxygen flow and microwave acid decomposition of biological samples were optimized for the subsequent determination of iodine. A new method was proposed for the generation of molecular iodine from periodate iona using hydrogen peroxide as a reductant. Procedures were developed for determining iodine in biological samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) using oxidative and reducing vapor generation; these allowed the detection limit for iodine to be lowered by 3-4 orders of magnitude. The developed procedures were used to analyze certified reference materials of milk (Skim Milk Powder BCR 150) and seaweed (Sea Lettuce BCR 279) and a Supradyn vitamin complex

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    Science.gov (United States)

    Wagatsuma, Kazuaki

    2009-04-01

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

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

    OpenAIRE

    2011-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  19. Determination of Cu, Zn, Pb and Cd by atomic emission spectrometry with inductively coupled plasma in waters and sediments from San Juan Ecosystem, Santiago de Cuba

    International Nuclear Information System (INIS)

    Argota Perez, George; Argota Coello, Humberto; Fernandez-Heredia, Angel

    2014-01-01

    In this paper the levels of concentration of copper, zinc, lead and cadmium in waters and sediments from the ecosystem San Juan in the Santiago of Cuba province were evaluated. Two sampling of the ecosystem in two stations belonging to the high and middle part of the river, in rainy and little rainy periods were carried out. The conservation and treatment of the samples were developed according to established standards and the determinations of the elements were realized using atomic emission spectrometry with inductively coupled plasma. The concentrations intervals of the studied elements were established so much in the superficial waters like in the sediments and it was demonstrated that exists statistical significant differences for the factors station, period and type of sample, being the middle part of the river, the little rainy period and the sediments, where the grater concentrations of the pollutants appear

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

    International Nuclear Information System (INIS)

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

    1989-01-01

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

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

    International Nuclear Information System (INIS)

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

    1987-01-01

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

  2. Standard practice for analysis of aqueous leachates from nuclear waste materials using inductively coupled plasma-atomic emission spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This practice is applicable to the determination of low concentration and trace elements in aqueous leachate solutions produced by the leaching of nuclear waste materials, using inductively coupled plasma-atomic emission spectroscopy (ICP-AES). 1.2 The nuclear waste material may be a simulated (non-radioactive) solid waste form or an actual solid radioactive waste material. 1.3 The leachate may be deionized water or any natural or simulated leachate solution containing less than 1 % total dissolved solids. 1.4 This practice should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral interferences, and procedures for their correction. 1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices...

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  4. Spectral interferences in atomic absorption spectrometry, (5)

    International Nuclear Information System (INIS)

    Daidoji, Hidehiro

    1979-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  6. Volatile organo-selenium speciation in biological matter by solid phase microextraction-moderate temperature multicapillary gas chromatography with microwave induced plasma atomic emission spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Dietz, C.; Sanz Landaluze, J.; Ximenez-Embun, P.; Madrid-Albarran, Y.; Camara, C

    2004-01-16

    Microwave induced plasma atomic emission spectrometry (MIP-AES) in combination with multicapillary (MC) gas chromatography could be proven to be useful for element specific detection of volatile species. Solid phase microextraction (SPME) was used for preconcentration and sample-matrix separation. The fiber desorption unit as well as the heating control for the MC column were in-house developed and multicapillary column was operated at moderate temperatures (30-100 deg. C). The method was optimized for organo-selenium species (dimethylselenide (DMSe), diethylselenide (DEtSe) and dimethyldiselenide (DMDSe)), using a chemometric approach. Stationary phases for the separation column were optimized using a conventional GC and contrasted with the results obtained with the MC. Application was focussed on selenium accumulating biological matter, such as lupine, yeast, Indian mustard and garlic. These samples were grown in hydroponic solution containing inorganic selenium (Na{sub 2}SeO{sub 3} and Na{sub 2}SeO{sub 4}). SPME sampling was carried out in fixed volume flow boxes in headspace above the living plants and in vials using treated samples. Results demonstrate inorganic selenium transformation into volatile organic species during metabolism. Separation is fast, a chromatogram can be obtained in less than 3 min and detection limits were at sub-ppb level for all investigated species. The system is independent from the use of a conventional gas chromatographic oven and can be used as a versatile alternative to highly cost intensive methods such as GC-ICP-MS.

  7. Simultaneous Pre-Concentration of Cadmium and Lead in Environmental Water Samples with Dispersive Liquid-Liquid Microextraction and Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    M. Salahinejad

    2013-06-01

    Full Text Available The dispersive liquid–liquid microextraction (DLLME method for determination of Pb+2 and Cd+2 ions in the environmental water samples was combined with inductively coupled plasma-atomic emission spectrometry (ICP-AES. Ammonium pyrrolidine dithiocarbamate (APDC, chloroform and ethanol were used as chelating agent, extraction solvent and disperser solvent, respectively. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters included extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH, sample volume and amount of the chelating agent.   Under the optimum conditions, the enrichment factor of 75 and 105 for Cd+2 and Pb+2 ions respectively was obtained from only 5.00mL of water sample. The detection limit (S/N=3 was 12 and 0.8ngmL−1 for Pb and Cd respectively. The relative standard deviation (RSDs for five replicate measurements of 0.50 mgL−1 of lead and cadmium was 6.5 and 4.4 % respectively. Mineral, tap, river, sea, dam and spiked water samples were analyzed for Cd and Pb amount.

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

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

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

  9. Investigation into spatial distribution of macroelements in dried drops of albumins and proteins by the methods of atomic-emission multichannel spectrometry

    International Nuclear Information System (INIS)

    Chin', N.Kh.; Zazhogin, A.P.; Bulojchik, Zh.I.; Tanin, A.L.; Pashkovskaya, I.D.; Nechipurenko, N.I.

    2011-01-01

    Based on local analysis of the line intensities of Al, Ca, Mg, and Zn in spectra for the samples of dried drops of egg albumin, the possibility for estimation of the spatial elemental distribution by the drop diameter was demonstrated using the atomic-emission multichannel spectrometry method. It was found that with an increase in the concentration of the elements with a high diffusion coefficient (Ca) diffusion counteracts their carry-over to the boundary of evaporating drops, simultaneously displacing the salts of other elements (Al, Fe, Zn) to the drop periphery. This work shows that excitation of the analyzed surface of a dried protein drop by double laser pulses enables a semi-quantitative estimation of the distribution of essential elements by the drop radius. Such investigations look very promising in search for markers of various diseases and in the development of methods revealing the pathological processes at the preclinical stage, making it possible to look for the causes of the elemental unbalance, to realize a targeted selection of preparations and active additives, to correct the treatment course. (authors)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-02-15

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

  11. Microwave-assisted versus conventional decomposition procedures applied to a ceramic potsherd standard reference material by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-03-03

    Inductively coupled plasma atomic emission spectrometry (ICP-AES) is a powerful, sensitive analytical technique with numerous applications in chemical characterization including that of ancient pottery, mainly due to its multi-element character, and the relatively short time required for the analysis. A critical step in characterization studies of ancient pottery is the selection of a suitable decomposition procedure for the ceramic matrix. The current work presents the results of a comparative study of six decomposition procedures applied on a standard ceramic potsherd reference material, SARM 69. The investigated decomposition procedures included three microwave-assisted decomposition procedures, one wet decomposition (WD) procedure by conventional heating, one combined microwave-assisted and conventional heating WD procedure, and one fusion procedure. Chemical analysis was carried out by ICP-AES. Five major (Si, Al, Fe, Ca, Mg), three minor (Mn, Ba, Ti) and two trace (Cu, Co) elements were determined and compared with their certified values. Quantitation was performed at two different spectral lines for each element and multi-element matrix-matched calibration standards were used. The recovery values for the six decomposition procedures ranged between 75 and 110% with a few notable exceptions. Data were processed statistically in order to evaluate the investigated decomposition procedures in terms of recovery, accuracy and precision, and eventually select the most appropriate one for ancient pottery analysis.

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

    International Nuclear Information System (INIS)

    Govindaraju, K.; Mevelle, G.

    1987-01-01

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

  13. Determination of Hg(2+) by on-line separation and pre-concentration with atmospheric-pressure solution-cathode glow discharge atomic emission spectrometry.

    Science.gov (United States)

    Li, Qing; Zhang, Zhen; Wang, Zheng

    2014-10-03

    A simple and sensitive method to determine Hg(2+) was developed by combining solution-cathode glow discharge atomic emission spectrometry (SCGD-AES) with flow injection (FI) based on on-line solid-phase extraction (SPE). We synthesized l-cysteine-modified mesoporous silica and packed it in an SPE microcolumn, which was experimentally determined to possess a good mercury adsorption capacity. An enrichment factor of 42 was achieved under optimized Hg(2+) elution conditions, namely, an FI flow rate of 2.0 mL min(-1) and an eluent comprised of 10% thiourea in 0.2 mol L(-1) HNO3. The detection limit of FI-SCGD-AES was determined to be 0.75 μg L(-1), and the precision of the 11 replicate Hg(2+) measurements was 0.86% at a concentration of 100 μg L(-1). The proposed method was validated by determining Hg(2+) in certified reference materials such as human hair (GBW09101b) and stream sediment (GBW07310). Copyright © 2014. Published by Elsevier B.V.

  14. Atom counting with accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Kutschera, Walter

    1995-01-01

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

  15. Comparison of inductively coupled plasma mass spectrometry with inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis for the determination of rare earth elements in Greek bauxites

    International Nuclear Information System (INIS)

    Ochsenkuehn-Petropoulou, Maria; Luck, Joachim

    1991-01-01

    Fore the determination of rare earth elements (REE) in bauxitic materials the techniques of inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and instrumental neutron activation analysis (INAA) were compared. In the NIST (National Institute of Standards and Technology) bauxites SRM 697 Dominican, and SRM 69 b Arkansas, the concentration of some REEs were determined. With the reference bauxite BX-N of the ARNT (Association Nationale de la Recherche Technique) the precision and accuracy of ICP-AES for the determination of REEs in bauxites was tested. Furthermore, Greek bauxites of the Parnassos-Giona area were investigated. In a comparison of the three methods it was possible to calculate from the data series the precision of each method, which showed that the tendency found in the deviations for the different REEs is in accordance with published values. Also the limits of detection for REEs in bauxites were calculated and found to be in the same range as those in the literature. (author)

  16. Determination of hafnium at the 10−4% level (relative to zirconium content) using neutron activation analysis, inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Smolik, Marek; Polkowska-Motrenko, Halina; Hubicki, Zbigniew; Jakóbik-Kolon, Agata; Danko, Bożena

    2014-01-01

    Graphical abstract: -- Highlights: •We worked out ICP-MS method of Hf determination in Zr and Zr compounds. •We used NAA method as reference one. •We obtained pure zirconium matrix by ion exchange (Diphonix ® resin). •These permit to determine ≥1 × 10 −4 % Hf in Zr sample by ICP MS with good precision and accuracy. -- Abstract: Hafnium at the very low level of 1–8 ppm (in relation to zirconium) was determined in zirconium sulfate solutions (originating from investigations of the separation of ca. 44 ppm Hf from zirconium by means of the ion exchange method) by using three independent methods: inductively coupled plasma mass spectrometry (ICP MS), neutron activation analysis (NAA) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results of NAA and ICP MS determinations were consistent with each other across the entire investigated range (the RSD of both methods did not exceed 38%). The results of ICP-AES determination were more diverse, particularly at less than 5 ppm Hf (RSD was significantly higher: 29–253%). The ion exchange method exploiting Diphonix ® resin proved sufficient efficiency in Zr–Hf separation when the initial concentration ratio of the elements ([Zr] 0 /[Hf] 0 ) ranged from 1200 to ca. 143,000

  17. Atomization mechanisms for barium in furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Styris, D.L.

    1984-01-01

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

  18. Evaluation of a new dielectric barrier discharge excitation source for the determination of arsenic with atomic emission spectrometry.

    Science.gov (United States)

    Zhu, Zhenli; He, Haiyang; He, Dong; Zheng, Hongtao; Zhang, Caixiang; Hu, Shenghong

    2014-05-01

    A low power dielectric barrier discharge excitation source was developed to determine arsenic in a cost-effective manner. Arsenic in water was reduced to AsH₃ by hydride generation (HG), which was transported to the miniature dielectric barrier discharge (DBD) excitation source for excitation and optical detection at As 193.7 nm atomic line. The DBD source consists of a quartz tube, a tungsten rod electrode, and a copper coil electrode. The main operation parameters and the potential interferences affecting the determination were investigated. The detection limit for arsenic with the proposed DBD-AES was 4.8 μg L(-1) when the HG products were dried with concentrated H₂SO₄ before introducing to DBD. Repeatability, expressed as the relative standard deviation of the spectral peak height, was 2.8% (n=11) for 0.1 mg L(-1) arsenic solution. The proposed method was successfully applied to the determinations of certified reference material (GBW08605) and nature water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Atomic electron spectrometry with synchrotron radiation

    International Nuclear Information System (INIS)

    Sorensen, S.L.

    1989-01-01

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

  20. Determination of Hg{sup 2+} by on-line separation and pre-concentration with atmospheric-pressure solution-cathode glow discharge atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Qing [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China); Zhang, Zhen [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China); School of Materials Science and Engineering, Shanghai University, Shanghai 200072 (China); Wang, Zheng, E-mail: wangzheng@mail.sic.ac.cn [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China)

    2014-10-03

    Highlights: • A modified SBA-15 mesoporous silica (SH-SBA-15) was synthesized as a sorbent. • On-line SPE combined with SCGD-AES based on FIA was used to detect Hg{sup 2+} firstly. • A simple, low-cost Hg{sup 2+} analysis in a complex matrix was established. • The sensitive detection of Hg{sup 2+} was achieved with a detection limit of 0.75 μg L{sup −1}. - Abstract: A simple and sensitive method to determine Hg{sup 2+} was developed by combining solution-cathode glow discharge atomic emission spectrometry (SCGD-AES) with flow injection (FI) based on on-line solid-phase extraction (SPE). We synthesized L-cysteine-modified mesoporous silica and packed it in an SPE microcolumn, which was experimentally determined to possess a good mercury adsorption capacity. An enrichment factor of 42 was achieved under optimized Hg{sup 2+} elution conditions, namely, an FI flow rate of 2.0 mL min{sup −1} and an eluent comprised of 10% thiourea in 0.2 mol L{sup −1} HNO{sub 3}. The detection limit of FI–SCGD-AES was determined to be 0.75 μg L{sup −1}, and the precision of the 11 replicate Hg{sup 2+} measurements was 0.86% at a concentration of 100 μg L{sup −1}. The proposed method was validated by determining Hg{sup 2+} in certified reference materials such as human hair (GBW09101b) and stream sediment (GBW07310)

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

    Science.gov (United States)

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

    2017-12-01

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

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

    International Nuclear Information System (INIS)

    Kawaguchi, Hiroshi

    1996-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  4. Spontaneous emission by moving atoms

    International Nuclear Information System (INIS)

    Meystre, P.; Wilkens, M.

    1994-01-01

    It is well known that spontaneous emission is not an intrinsic atomic property, but rather results from the coupling of the atom to the vacuum modes of the electromagnetic field. As such, it can be modified by tailoring the electromagnetic environment into which the atom can radiate. This was already realized by Purcell, who noted that the spontaneous emission rate can be enhanced if the atom placed inside a cavity is resonant with one of the cavity is resonant with one of the cavity modes, and by Kleppner, who discussed the opposite case of inhibited spontaneous emission. It has also been recognized that spontaneous emission need not be an irreversible process. Indeed, a system consisting of a single atom coupled to a single mode of the electromagnetic field undergoes a periodic exchange of excitation between the atom and the field. This periodic exchange remains dominant as long as the strength of the coupling between the atom and a cavity mode is itself dominant. 23 refs., 6 figs

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-02-28

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

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

    African Journals Online (AJOL)

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

  7. Atomic emission spectroscopy

    Science.gov (United States)

    Andrew, K. H.

    1975-01-01

    The relationship between the Slater-Condon theory and the conditions within the atom as revealed by experimental data was investigated. The first spectrum of Si, Rb, Cl, Br, I, Ne, Ar, and Xe-136 and the second spectrum of As, Cu, and P were determined. Methods for assessing the phase stability of fringe counting interferometers and the design of an autoranging scanning system for digitizing the output of an infrared spectrometer and recording it on magnetic tape are described.

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  9. Determination of the mineral compositions of some selected oil-bearing seeds and kernels using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES

    Directory of Open Access Journals (Sweden)

    Musa Özcan, M.

    2006-06-01

    Full Text Available The aim of this paper was to establish the mineral contents of oil-bearing seeds and kernels such as peanut, turpentine, walnut, hazelnut, sesame, corn, poppy, almond, sunflower etc., using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES. Significant differences in mineral composition were observed among crops. All seeds and kernels contained high amounts of Al, Ca, Fe, K, Mg, Na, P and Zn. B, Cr, Cu, Li, Ni, Sr, Ti while V contents of the crops were found to be very low. The levels of K and P of all crops in this study were found to be higher than those of other seeds and kernels. The results obtained from analyses of the crops showed that the mean levels of potassiumcontent ranged from 1701.08 mg/kg (corn to 20895.8 mg/kg (soybean, the average content of phosphorus ranged from 3076.9 mg/kg (turpentine to 12006,5 mg/kg to 2617.4 mg/kg (cotton seed, and Ca from 68.4 mg/kg (corn to 13195.7 mg/kg (poppy seed. The results show that these values may  be useful for the evaluation of dietary information. Particularly the obtained results provide evidence that soybean, pinestone and poppy seed are a good source of K, P and Ca, respectively. Whereas pinestone is a good source of zinc.La finalidad del trabajo es establecer el contenido en elementos minerales de semillas oleaginosas tales como cacahuetes, trementina, avellana, sesamo, maiz, almendras, girasol, utilizando ICP-AES. Se han observado diferencias significativas en la composición de minerales entre cosechas. Todas las semillas contienen cantidades elevadas de Al, Ca, Fe, K, Mg, Na, P y Zn. Los contenidos de B, Cr, Cu, Li, Ni, Sr, Ti y V, sin embargo, fueron bajos. Los contenidos de K y P en todas las semillas estudiadas fueron superiores a las de otras semillas. El contenido medio de K osciló entre 1.701,1 mg/kg (maiz a 20.895,8 mg/kg (soja, el P entre 3.076.9 mg/kg (trementina a 12.006.5 mg/kg o 2.617,4 mg/kg (semilla de algodón, y Ca de 68,4 mg/kg (maiz a 13.195,7 mg

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  11. Flotation separation of Cd, Co, Cr, Cu, Ni and Tl from calcium minerals and their determination by inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Zajkova-Paneva, Vesna; Stafilov, Trajche; Boev, Blazho

    2003-01-01

    The method of inductively coupled plasma-atomic spectrometry (ICP-AES), is developed for determination of Cd, Co, Cr, Cu, Ni and Tl in traces in calcite and gypsum. The interferences of Ca as matrix element on Co, Cr, Cu, Ni and Tl intensities during their ICP-AES determination are investigated. The results reveal that Ca does not interfere on intensities of Cr, but tends to decrease the intensity of the other elements. To eliminate those matrix interferences of Ca on trace elements intensities a flotation separation method is proposed. Lead(II) hexamethylenedithiocarbamate, Pb(HMDTC) 2 , is applied as a collector for flotation of trace elements from acidic solutions of mineral samples. The most suitable concentrations of calcite and gypsum solutions for flotation are ascertained. The detection limits of ICP-AES method following flotation of elements present in calcite and gypsum as impurities are determined: 0.022 and 0.061 μg·g -1 for Cd, 0.071 and 0.042 μg·g -1 for Co, 0.026 and 0.132 μg·g -1 for Cr, 0.164 and 0.149 μg·g -1 for Cu, 0.289 and 0.095 μg·g -1 for Ni and 0.645 and 0.7666 μg·g -1 for Tl, respectively. (Original)

  12. Use of stirred tanks for studying matrix effects caused by inorganic acids, easily ionized elements and organic solvents in inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Paredes, Eduardo [Departamento de Quimica Analitica, Nutricion y Bromatologia, University of Alicante, 03080 Alicante (Spain); Maestre, Salvador E. [Departamento de Quimica Analitica, Nutricion y Bromatologia, University of Alicante, 03080 Alicante (Spain); Todoli, Jose L. [Departamento de Quimica Analitica, Nutricion y Bromatologia, University of Alicante, 03080 Alicante (Spain)]. E-mail: jose.todoli@ua.es

    2006-03-15

    A stirred tank was used for the first time to elucidate the mechanism responsible for inductively coupled plasma atomic emission spectroscopy (ICP-AES) matrix effects caused by inorganic, acids and easily ionized elements (EIEs), as well as organic, ethanol and acetic acid, compounds. In order to gradually increase the matrix concentration, a matrix solution was introduced inside a stirred container (tank) initially filled with an aqueous multielement standard. PolyTetraFluoroEthylene (PTFE) tubing was used to deliver the resulting solution to the liquid sample introduction system. Matrix concentration ranged from 0 to 2 mol l{sup -1} in the case of inorganic acids (i.e., nitric, sulfuric, hydrochloric and a mixture of them), from 0 to about 2500 mg l{sup -1} for EIEs (i.e., sodium, calcium and mixtures of both) and from 0% to 15%, w/w for organic compounds. Up to 40-50 different solutions were prepared and measured in a period of time shorter than 6-7 min. This investigation was carried out in terms of emission intensity and tertiary aerosols characteristics. The experimental setup used in the present work allowed to thoroughly study the effect of matrix concentration on analytical signal. Generally speaking, the experiments concerning tertiary aerosol characterization revealed that, in the case of inorganic acids and EIEs, the mechanism responsible for changes in aerosol characteristics was the droplet fission. In contrast, for organic matrices it was found that the interference was caused by a change in both aerosol transport and plasma thermal characteristics. The extent of the interferences caused by organic as well as inorganic compounds was compared for a set of 14 emission lines through a wide range of matrix concentrations. With a stirred tank, it is possible to choose an efficient internal standard for any given matrix composition. The time required to complete this procedure was shorter than 7 min.

  13. Use of stirred tanks for studying matrix effects caused by inorganic acids, easily ionized elements and organic solvents in inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Paredes, Eduardo; Maestre, Salvador E.; Todoli, Jose L.

    2006-01-01

    A stirred tank was used for the first time to elucidate the mechanism responsible for inductively coupled plasma atomic emission spectroscopy (ICP-AES) matrix effects caused by inorganic, acids and easily ionized elements (EIEs), as well as organic, ethanol and acetic acid, compounds. In order to gradually increase the matrix concentration, a matrix solution was introduced inside a stirred container (tank) initially filled with an aqueous multielement standard. PolyTetraFluoroEthylene (PTFE) tubing was used to deliver the resulting solution to the liquid sample introduction system. Matrix concentration ranged from 0 to 2 mol l -1 in the case of inorganic acids (i.e., nitric, sulfuric, hydrochloric and a mixture of them), from 0 to about 2500 mg l -1 for EIEs (i.e., sodium, calcium and mixtures of both) and from 0% to 15%, w/w for organic compounds. Up to 40-50 different solutions were prepared and measured in a period of time shorter than 6-7 min. This investigation was carried out in terms of emission intensity and tertiary aerosols characteristics. The experimental setup used in the present work allowed to thoroughly study the effect of matrix concentration on analytical signal. Generally speaking, the experiments concerning tertiary aerosol characterization revealed that, in the case of inorganic acids and EIEs, the mechanism responsible for changes in aerosol characteristics was the droplet fission. In contrast, for organic matrices it was found that the interference was caused by a change in both aerosol transport and plasma thermal characteristics. The extent of the interferences caused by organic as well as inorganic compounds was compared for a set of 14 emission lines through a wide range of matrix concentrations. With a stirred tank, it is possible to choose an efficient internal standard for any given matrix composition. The time required to complete this procedure was shorter than 7 min

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

    International Nuclear Information System (INIS)

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-01

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

  16. Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Hola, Marketa; Otruba, Vitezslav; Kanicky, Viktor

    2006-01-01

    Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP-OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm 3 ) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between ± 3% and ± 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA-ICP-OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed. The

  17. Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hola, Marketa [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic); Otruba, Vitezslav [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic); Kanicky, Viktor [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic)]. E-mail: viktork@chemi.muni.cz

    2006-05-15

    Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP-OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm{sup 3}) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between {+-} 3% and {+-} 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA-ICP-OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed

  18. Flow Injection Photochemical Vapor Generation Coupled with Miniaturized Solution-Cathode Glow Discharge Atomic Emission Spectrometry for Determination and Speciation Analysis of Mercury.

    Science.gov (United States)

    Mo, Jiamei; Li, Qing; Guo, Xiaohong; Zhang, Guoxia; Wang, Zheng

    2017-10-03

    A novel, compact, and green method was developed for the determination and speciation analysis of mercury, based on flow injection photochemical vapor generation (PVG) coupled with miniaturized solution cathode glow discharge-atomic emission spectroscopy (SCGD-AES). The SCGD was generated between a miniature hollow titanium tube and a solution emerging from a glass capillary. Cold mercury vapor (Hg(0)) was generated by PVG and subsequently delivered to the SCGD for excitation, and finally the emission signals were recorded by a miniaturized spectrograph. The detection limits (DLs) of Hg(II) and methylmercury (MeHg) were both determined to be 0.2 μg L -1 . Moreover, mercury speciation analysis could also be performed by using different wavelengths and powers from the UV lamp and irradiation times. Both Hg(II) and MeHg can be converted to Hg(0) for the determination of total mercury (T-Hg) with 8 W/254 nm UV lamp and 60 s irradiation time; while only Hg(II) can be reduced to Hg(0) and determined selectively with 4 W/365 nm UV lamp and 20 s irradiation time. Then, the concentration of MeHg can be calculated by subtracting the Hg(II) from the T-Hg. Because of its similar sensitivity and DL at 8 W/254 nm, the simpler and less toxic Hg(II) was used successfully as a primary standard for the quantification of T-Hg. The novel PVG-SCGD-AES system provides not only a 365-fold improvement in the DL for Hg(II) but also a nonchromatographic method for the speciation analysis of mercury. After validating its accuracy, this method was successfully used for mercury speciation analysis of water and biological samples.

  19. Acquired acid resistance of human enamel treated with laser (Er:YAG laser and Co 2 laser and acidulated phosphate fluoride treatment: An in vitro atomic emission spectrometry analysis

    Directory of Open Access Journals (Sweden)

    Anju Mathew

    2013-01-01

    Full Text Available Background: Dental caries is essentially a process of diffusion and dissolution. If the aspect of dissolution can be curtailed some degree of prevention can be achieved. Aims: The present study was carried out to evaluate and compare the effect of Er:YAG laser and Co 2 laser irradiation combined with acidulated phosphate fluoride treatment on in vitro acid resistance of human enamel. Design: An in vitro study was carried out on 30 human premolars to evaluate the enamel′s acid resistance using an atomic emission spectrometry analysis. Materials and Methods: A total of 60 enamel specimens were prepared from 30 human premolars and were randomly assigned to 6 groups: (1 Untreated (control; (2 1.23% acidulated phosphate fluoride (APF gel application alone for 4 min; (3 Er:YAG laser treatment alone; (4 Co 2 laser treatment alone; (5 Er:YAG laser + APF gel application; (6 Co 2 laser + APF gel application. The specimens were then individually immersed in 5 ml of acetate buffer solution (0.1 mol/L, pH 4.5 and incubated at 37°C for 24 h, and the acid resistance was evaluated by determining the calcium ion concentration using the atomic emission spectrometry. Statistical Analysis: An ANOVA model was constructed (P value of 0.05, followed by Tukey′s test for multiple pair wise comparisons of mean values. Results: Significant differences were found between the control group and the test groups ( P < 0.001. Conclusions: Combining acidulated phosphate fluoride with either Er:YAG or Co 2 laser had a synergistic effect in decreasing the enamel demineralization more than either fluoride treatment or laser treatment alone.

  20. Determination of methylmercury in fish tissue by gas chromatography with microwave-induced plasma atomic emission spectrometry after derivatization with sodium tetraphenylborate

    Energy Technology Data Exchange (ETDEWEB)

    Palmieri, H.E.L.; Leonel, L.V. [Comissao Nacional de Energia Nuclear - Centro de Desenvolvimento da Tecnologia Nuclear, Belo Horizonte (Brazil)

    2000-03-01

    The detection of methylmercury species (MeHg) in fish tissue was investigated. Samples were digested with KOH-methanol and acidified prior to extraction with methylene chloride. MeHg was back-extracted from the organic phase into water. An aliquot of this aqueous solution (buffered to pH 5) was subjected to derivatization with sodium tetraphenylborate (NaBPh{sub 4}) and then extracted with toluene. The organic phase containing MePhHg was injected into a gas chromatograph (GC) which is on-line with a microwave-induced plasma atomic emission spectrometer (MIP-AED). The quantification limit was about 0.6 {mu}g/g and 0.1 {mu}g/g of MeHg (as Hg) for 0.08 g of freeze-dried fish powder and 0.5 g of fresh samples, respectively. Two certified reference materials, CRM 464 (tuna fish) from Community Bureau of Reference-BCR and DORM-2 (dogfish muscle) from National Research Council Canada-NRC were selected for checking the accuracy of the method. This methodology was applied to the determination of MeHg in some kinds of fish from the Carmo river with alluvial gold recovery activities (''garimpos'') in Mariana, Minas Gerais, Brazil. (orig.)

  1. Determination of methylmercury in fish tissue by gas chromatography with microwave-induced plasma atomic emission spectrometry after derivatization with sodium tetraphenylborate.

    Science.gov (United States)

    Palmieri, H E; Leonel, L V

    2000-03-01

    The detection of methylmercury species (MeHg) in fish tissue was investigated. Samples were digested with KOH-methanol and acidified prior to extraction with methylene chloride. MeHg was back-extracted from the organic phase into water. An aliquot of this aqueous solution (buffered to pH 5) was subjected to derivatization with sodium tetraphenylborate (NaBPh4) and then extracted with toluene. The organic phase containing MePhHg was injected into a gas chromatograph (GC) which is on-line with a microwave-induced plasma atomic emission spectrometer (MIP-AED). The quantification limit was about 0.6 microg/g and 0.1 microg/g of MeHg (as Hg) for 0.08 g of freeze-dried fish powder and 0.5 g of fresh samples, respectively. Two certified reference materials, CRM 464 (tuna fish) from Community Bureau of Reference-BCR and DORM-2 (dogfish muscle) from National Research Council Canada-NRC were selected for checking the accuracy of the method. This methodology was applied to the determination of MeHg in some kinds of fish from the Carmo river with alluvial gold recovery activities ("garimpos") in Mariana, Minas Gerais, Brazil.

  2. Multielement detection limits and sample nebulization efficiencies of an improved ultrasonic nebulizer and a conventional pneumatic nebulizer in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Olson, K.W.; Haas, W.J. Jr.; Fassel, V.A.

    1977-01-01

    Two important aspects of the analytical performance of a newly developed ultrasonic nebulizer and a specially designed pneumatic nebulizer have been compared for use in inductively coupled plasma--atomic emission spectroscopy (ICP-AES). The ultrasonic nebulizer, when combined with a conventional aerosol desolvation apparatus, provided an order of magnitude or more improvement in simultaneous multielement detection limits as compared to those obtained when the pneumatic nebulizer was used either with or without desolvation. Application of a novel method for direct measurement of the overall efficiency of nebulization to the two systems showed that an approximately tenfold greater rate of sample delivery to the plasma torch was primarily responsible for the superior detection limits afforded by the ultrasonic nebulizer. A unique feature of the ultrasonic nebulizer described is the protection against chemical attack which is achieved by completely enclosing the transducer in an acoustically coupled borosilicate glass cylinder. Direct sample introduction, convenient sample change, and rapid cleanout are other important characteristics of the system which make it an attractive alternate to pneumatic nebulizer systems

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

    African Journals Online (AJOL)

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

  4. Deviation from Boltzmann distribution in excited energy levels of singly-ionized iron in an argon glow discharge plasma for atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Lei; Kashiwakura, Shunsuke; Wagatsuma, Kazuaki, E-mail: wagatuma@imr.tohoku.ac.jp

    2012-01-15

    A Boltzmann plot for many iron ionic lines having excitation energies of 4.7-9.1 eV was investigated in an argon glow discharge plasma when the discharge parameters, such as the voltage/current and the gas pressure, were varied. A Grimm-style radiation source was employed in a DC voltage range of 400-800 V at argon pressures of 400-930 Pa. The plot did not follow a linear relationship over a wide range of the excitation energy, but it yielded a normal Boltzmann distribution in the range of 4.7-5.8 eV and a large overpopulation in higher-lying excitation levels of iron ion. A probable reason for this phenomenon is that excitations for higher excited energy levels of iron ion would be predominantly caused by non-thermal collisions with argon species, the internal energy of which is received by iron atoms for the ionization. Particular intense ionic lines, which gave a maximum peak of the Boltzmann plot, were observed at an excitation energy of ca. 7.7 eV. They were the Fe II 257.297-nm and the Fe II 258.111-nm lines, derived from the 3d{sup 5}4s4p {sup 6}P excited levels. The 3d{sup 5}4s4p {sup 6}P excited levels can be highly populated through a resonance charge transfer from the ground state of argon ion, because of good matching in the excitation energy as well as the conservation of the total spin before and after the collision. An enhancement factor of the emission intensity for various Fe II lines could be obtained from a deviation from the normal Boltzmann plot, which comprised the emission lines of 4.7-5.8 eV. It would roughly correspond to a contribution of the charge transfer excitation to the excited levels of iron ion, suggesting that the charge-transfer collision could elevate the number density of the corresponding excited levels by a factor of ca.10{sup 4}. The Boltzmann plots give important information on the reason why a variety of iron ionic lines can be emitted from glow discharge plasmas.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    International Nuclear Information System (INIS)

    Arruda, Marco Aurelio Zezzi; Figueiredo, Eduardo Costa

    2009-01-01

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

  7. Deuterium measurement by emission spectrometry

    International Nuclear Information System (INIS)

    Niemann, E.G.; Heilig, K.; Dumke, I.

    1978-01-01

    The method makes it possible to determine the relative deuterium content of enriched water samples. For this, the relative intensities of the Hα and Dα lines are measured which are emitted by a high-frequency discharge in water vapour. Although the method is not as exact as mass spectrometry, it has the following advantages: - Easy sample preparation (no reduction necessary); - samples of highly different enrichment can be measured one after the other without the danger of memory effects; - much lower apparatus and cost expenditure. The necessary sample size is about the same in both methods. (orig.) [de

  8. Assessing oral bioaccessibility of trace elements in soils under worst-case scenarios by automated in-line dynamic extraction as a front end to inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rosende, María [FI-TRACE group, Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa, km 7.5, Palma de Mallorca, Illes Balears E-07122 (Spain); Magalhães, Luis M.; Segundo, Marcela A. [REQUIMTE, Department of Chemistry, Faculty of Pharmacy, University of Porto, R. de Jorge Viterbo Ferreira, 228, Porto 4050-313 (Portugal); Miró, Manuel, E-mail: manuel.miro@uib.es [FI-TRACE group, Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa, km 7.5, Palma de Mallorca, Illes Balears E-07122 (Spain)

    2014-09-09

    Highlights: • Automatic oral bioaccessibility tests of trace metals under worst-case scenarios. • Use of intricate and realistic digestive fluids (UBM method). • Analysis of large amounts of soils (≥400 mg) in a flow-based configuration. • Smart interface to inductively coupled plasma atomic emission spectrometry. • Comparison of distinct flow systems mimicking physiological conditions. - Abstract: A novel biomimetic extraction procedure that allows for the in-line handing of ≥400 mg solid substrates is herein proposed for automatic ascertainment of trace element (TE) bioaccessibility in soils under worst-case conditions as per recommendations of ISO norms. A unified bioaccessibility/BARGE method (UBM)-like physiological-based extraction test is evaluated for the first time in a dynamic format for accurate assessment of in-vitro bioaccessibility of Cr, Cu, Ni, Pb and Zn in forest and residential-garden soils by on-line coupling of a hybrid flow set-up to inductively coupled plasma atomic emission spectrometry. Three biologically relevant operational extraction modes mimicking: (i) gastric juice extraction alone; (ii) saliva and gastric juice composite in unidirectional flow extraction format and (iii) saliva and gastric juice composite in a recirculation mode were thoroughly investigated. The extraction profiles of the three configurations using digestive fluids were proven to fit a first order reaction kinetic model for estimating the maximum TE bioaccessibility, that is, the actual worst-case scenario in human risk assessment protocols. A full factorial design, in which the sample amount (400–800 mg), the extractant flow rate (0.5–1.5 mL min{sup −1}) and the extraction temperature (27–37 °C) were selected as variables for the multivariate optimization studies in order to obtain the maximum TE extractability. Two soils of varied physicochemical properties were analysed and no significant differences were found at the 0.05 significance level

  9. Assessing oral bioaccessibility of trace elements in soils under worst-case scenarios by automated in-line dynamic extraction as a front end to inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Rosende, María; Magalhães, Luis M.; Segundo, Marcela A.; Miró, Manuel

    2014-01-01

    Highlights: • Automatic oral bioaccessibility tests of trace metals under worst-case scenarios. • Use of intricate and realistic digestive fluids (UBM method). • Analysis of large amounts of soils (≥400 mg) in a flow-based configuration. • Smart interface to inductively coupled plasma atomic emission spectrometry. • Comparison of distinct flow systems mimicking physiological conditions. - Abstract: A novel biomimetic extraction procedure that allows for the in-line handing of ≥400 mg solid substrates is herein proposed for automatic ascertainment of trace element (TE) bioaccessibility in soils under worst-case conditions as per recommendations of ISO norms. A unified bioaccessibility/BARGE method (UBM)-like physiological-based extraction test is evaluated for the first time in a dynamic format for accurate assessment of in-vitro bioaccessibility of Cr, Cu, Ni, Pb and Zn in forest and residential-garden soils by on-line coupling of a hybrid flow set-up to inductively coupled plasma atomic emission spectrometry. Three biologically relevant operational extraction modes mimicking: (i) gastric juice extraction alone; (ii) saliva and gastric juice composite in unidirectional flow extraction format and (iii) saliva and gastric juice composite in a recirculation mode were thoroughly investigated. The extraction profiles of the three configurations using digestive fluids were proven to fit a first order reaction kinetic model for estimating the maximum TE bioaccessibility, that is, the actual worst-case scenario in human risk assessment protocols. A full factorial design, in which the sample amount (400–800 mg), the extractant flow rate (0.5–1.5 mL min −1 ) and the extraction temperature (27–37 °C) were selected as variables for the multivariate optimization studies in order to obtain the maximum TE extractability. Two soils of varied physicochemical properties were analysed and no significant differences were found at the 0.05 significance level

  10. Atomic fluorescence spectrometry with the inductively coupled plasma

    International Nuclear Information System (INIS)

    Omenetto, N.; Winefordner, J.D.

    1987-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-06-15

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

  14. Atomic absorption spectrometry using tungsten and molybdenum tubes as metal atomizer

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  15. Spectrochemical analysis by atomic absorption and emission

    National Research Council Canada - National Science Library

    Lajunen, Lauri

    1992-01-01

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

  16. Discharge on boiling in a channel: effect of channel geometry on the performance characteristics of determining metals in a liquid flow by atomic emission spectrometry

    International Nuclear Information System (INIS)

    Zuev, B.K.; Yagov, V.V.; Grachev, A.S.

    2006-01-01

    Discharge on boiling in a channel was studied as a new atomization and excitation source for spectrochemical analysis in a flow of electrolyte solutions. The discharge arises between the liquid walls of a vapor lock formed in the channel of a dielectric membrane because of the rapid Joule heating of the liquid in the channel. The effect of channel geometry on the reproducibility of the integrated light intensity was studied. The background radiation spectrum was measured over the range 220-900 nm, and the possibility of determining alkali and alkaline earth metals in a flow was studied. The parameters of linear calibration equations and the detection limits for these metals are given [ru

  17. A new nebulization device with exchangeable aerosol generation mode as a useful tool to investigate sample introduction processes in inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Grotti, Marco; Lagomarsino, Cristina; Frache, Roberto

    2004-01-01

    A new sample introduction device has been designed in order to differentiate between the effects of the aerosol production and its following desolvation on analytical performances of an inductively coupled plasma optical spectrometer. This research tool allows to easily switch between the pneumatic and ultrasonic aerosol generation mode and to use a joint desolvation chamber. In this way, a real comparison between aerosol production systems may be attained and the influence of aerosol generation process on analytical figures clearly distinguished from that of the desolvation process. In this work, the separate effects of the aerosol generation and desolvation processes on analytical sensitivity and tolerance towards matrix effects have been investigated. Concerning sensitivity, it was found that both the processes play an important role in determining emission intensities, being the increase in sensitivity due to desolvation higher than that due to the improved aerosol generation efficiency. Concerning the matrix effects, a predominant role of the desolvation system was found, while the influence of the aerosol generation mode was much less important. For nitric acid, the decreasing effect was mitigated by the presence of a desolvation system, due to partial removal of the acid. On the contrary, the depressive effect of sulfuric acid was enhanced by the presence of a desolvation system, due to degradation of the solvent removal efficiency and to further decrease in the analyte transport rate caused by clustering phenomena. Concerning the interferences due to sodium and calcium, a depressive effect was observed, which is enhanced by desolvation

  18. Simultaneous determination of carbohydrates, carboxylic acids, alcohols, and metals in foods by high-performance liquid chromatography inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    Paredes, Eduardo; Maestre, Salvador E; Prats, Soledad; Todolí, José L

    2006-10-01

    The applicability of the HPLC-ICP-AES coupling for the simultaneous determination of carbohydrates, carboxylic acids, alcohols, and metals in a single chromatographic run has been demonstrated in the present work. Five saccharides, glucose, fructose, sucrose, sorbitol, and lactose; five carboxylic acids, citric, tartaric, malic, lactic, and acetic; and three alcohols, glycerol, ethanol, and methanol, have been determined. A H+ cation exchange column has been used to separate these compounds. The chromatograms have been obtained by monitoring the carbon emission signal at 193.09 nm. The results obtained by HPLC-ICP-AES have been compared against those found with conventional detection systems (i.e., refractive index, UV, and photodyode array detectors). The HPLC-ICP-AES method has shown the following features: (i) organic compounds and metals can be simultaneously determined; (ii) the detection method is universal; (iii) for nonvolatile organic compounds, a complete calibration line can be obtained from a single injection; and (iv) it provides absolute limits of detection similar to or lower than those found with conventional detection systems (i.e., on the order of several tens of nanograms of organic compound). The methodology has been validated through the analysis of food samples such as juices, isotonic beverages, wines, and a certified nonfat milk powder sample.

  19. Auger spectrometry of atoms and molecules

    International Nuclear Information System (INIS)

    Krause, M.O.

    1994-01-01

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

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

    International Nuclear Information System (INIS)

    Gaskell, S.J.

    1990-01-01

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

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

    Science.gov (United States)

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

    1989-01-01

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

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  3. Determination of hafnium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

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

    1977-01-01

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

  4. Micro- and nano-volume samples by electrothermal, near-torch vaporization sample introduction using removable, interchangeable and portable rhenium coiled-filament assemblies and axially-viewed inductively coupled plasma-atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Badiei, Hamid R.; Lai, Bryant; Karanassios, Vassili

    2012-11-15

    An electrothermal, near-torch vaporization (NTV) sample introduction for micro- or nano-volume samples is described. Samples were pipetted onto coiled-filament assemblies that were purposely developed to be removable and interchangeable and were dried and vaporized into a small-volume vaporization chamber that clips onto any ICP torch with a ball joint. Interchangeable assemblies were also constructed to be small-size (e.g., less than 3 cm long with max diameter of 0.65 cm) and light-weight (1.4 g) so that they can be portable. Interchangeable assemblies with volume-capacities in three ranges (i.e., < 1 {mu}L, 1-10 {mu}L and 10-100 {mu}L) were fabricated and used. The horizontally-operated NTV sample introduction was interfaced to an axially-viewed ICP-AES (inductively coupled plasma-atomic emission spectrometry) system and NTV was optimized using ICP-AES and 8 elements (Pb, Cd, Zn, V, Ba, Mg, Be and Ca). Precision was 1.0-2.3% (peak height) and 1.1-2.4% (peak area). Detection limits (obtained using 5 {mu}L volumes) expressed in absolute-amounts ranged between 4 pg for Pb to 0.3 fg ({approx} 5 million atoms) for Ca. Detection limits expressed in concentration units (obtained using 100 {mu}L volumes of diluted, single-element standard solutions) were: 50 pg/mL for Pb; 10 pg/mL for Cd; 9 pg/mL for Zn; 1 pg/mL for V; 0.9 pg/mL for Ba; 0.5 pg/mL for Mg; 50 fg/mL for Be; and 3 fg/mL for Ca. Analytical capability and utility was demonstrated using the determination of Pb in pg/mL levels of diluted natural water Certified Reference Material (CRM) and the determination of Zn in 80 nL volumes of the liquid extracted from an individual vesicle. It is shown that portable and interchangeable assemblies with dried sample residues on them can be transported without analyte loss (for the concentrations tested), thus opening up the possibility for 'taking part of the lab to the sample' applications, such as testing for Cu concentration-compliance with the lead

  5. New developments in glow discharge optical emission and mass spectrometry

    International Nuclear Information System (INIS)

    Hoffmann, Volker; Dorka, Roland; Wilken, Ludger; Wetzig, Klaus

    2000-01-01

    This paper describes new developments in flow discharge optical emission (GD-OES) and mass spectrometry (GD-MS) at IFW and presents corresponding new applications (analysis of microelectronic multi-layer system by radio frequency glow discharge optical emission spectrometry (RF-GD-OES) and analysis of pure iron by a new Grimm-type GD-MS source)

  6. Atomic and molecular gas phase spectrometry

    Science.gov (United States)

    Winefordner, J. D.

    1985-10-01

    The major goals of this research have been to develop diagnostical spectroscopic methods for measuring spatial/temporal temperatures and species of combustion flames and plasmas and to develop sensitive, selective, precise, reliable, rapid spectrometric methods of trace analysis of elements present in jet engine lubricating oils, metallurgical samples, and engine exhausts. The diagnostical approaches have been based upon the measurement of metal probes introduced into the flame or plasmas and the measurement of OH in flames. The measurement approaches have involved the use of laser-excited fluorescence, saturated absorption, polarization, and linear absorption. The spatial resolution in most studies is less than 1 cu mm and the temporal resolution is less than 10 ns with the use of pulsed lasers. Single pulse temperature and species measurements have also been carried out. Other diagnostical studies have involved the measurement of collisional redistribution of radiatively excited levels of Na and Tl in acetylene/02/Ar flames and the measurement of lifetimes and quantum efficiencies of atoms and ions in the inductively coupled plasmas, ICP. The latter studies indicate that the high electron number densities in ICPs are not efficient quenchers of excited atoms/ions. Temperatures of microwave atmospheric plasmas produced capacitatively and cool metastable N2 discharge produced by a dielectric discharge have also been measured.

  7. Gas chromatography of organic microcontaminants using atomic emission and mass spectrometric detection combined in one instrument (GC-AED/MS)

    NARCIS (Netherlands)

    Mol, H.G.J.; Hankemeier, T.; Brinkman, U.A.T.

    1999-01-01

    This study describes the coupling of an atomic-emission detector and mass-spectrometric detector to a single gas chromatograph. Splitting of the column effluent enables simultaneous detection by atomic-emission detection (AED) and mass spectrometry (MS) and yields a powerful system for the target

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

    International Nuclear Information System (INIS)

    Broekaert, Jose A.C.; Siemens, Volker

    2004-01-01

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

  9. Theory of atomic spectral emission intensity

    Science.gov (United States)

    Yngström, Sten

    1994-07-01

    The theoretical derivation of a new spectral line intensity formula for atomic radiative emission is presented. The theory is based on first principles of quantum physics, electrodynamics, and statistical physics. Quantum rules lead to revision of the conventional principle of local thermal equilibrium of matter and radiation. Study of electrodynamics suggests absence of spectral emission from fractions of the numbers of atoms and ions in a plasma due to radiative inhibition caused by electromagnetic force fields. Statistical probability methods are extended by the statement: A macroscopic physical system develops in the most probable of all conceivable ways consistent with the constraining conditions for the system. The crucial role of statistical physics in transforming quantum logic into common sense logic is stressed. The theory is strongly supported by experimental evidence.

  10. Theory of atomic spectral emission intensity

    International Nuclear Information System (INIS)

    Yngstroem, S.

    1989-02-01

    The theoretical derivation of a new spectral line intensity formula for atomic radiative emission is presented. The theory is based on first principles of quantum physics and statistical physics. It is argued that the formulation of the theory provides a very good example of the manner in which quantum logic transforms into common sense logic. The theory is strongly supported by experimental evidence. (author) (16 refs.)

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

    International Nuclear Information System (INIS)

    Dedina, Jiri

    2007-01-01

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

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

    International Nuclear Information System (INIS)

    Kantor, Tibor

    2008-01-01

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

  13. SOME SPECIATION STUDIES IN FOODSTUFF BY ATOMIC ABSORPTION SPECTROMETRY

    OpenAIRE

    Gücer, S

    2000-01-01

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

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

    International Nuclear Information System (INIS)

    Mermet, Jean-Michel

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-17

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2006-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-06-15

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

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Science.gov (United States)

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

    2010-04-07

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    International Nuclear Information System (INIS)

    Alduan, F.A.; Capdevila, C.

    1979-01-01

    Nineteen trace metals in atmospheric samples have been determined by atomic absorption spectrometry, using a graphite furnace for most elements. Paper filters have been used to collect air samples. The sample preparation procedure involves the removal of organic matter and the conversion of the metals to soluble salts by ashing the filters in an oxygen plasma at 125 deg C for 6 h. and by subsequent dissolution in HN0 3 HCl solution. The sensitivities achieved are in the range of 2,5.10 -5 and 6,3.10 -3 μg/m 3 , for an air volume of 2000 m 3 . (author)

  7. Determination of cadmium in aluminium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

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

    1978-12-01

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

  8. Determination of technetium by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

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

    1978-01-01

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

  9. Analysis of iron-base alloys by low-wattage glow discharge emission spectrometry

    International Nuclear Information System (INIS)

    Wagatsuma, K.; Hirokawa, K.

    1984-01-01

    Several iron-base alloys were investigated by low-wattage glow discharge emission spectrometry. The emission intensity principally depended on the sputtering parameters of constituent elements in the alloy. However, in the case of chromium, stable and firm oxides formed on the surface influencing the yield of ejected atoms. This paper discusses the relation between the sputtering parameters in Fe-Ni, Fe-Cr, and Fe-Co alloys and their relative emission intensities. Additionally, quantitative analysis was performed for some ternary iron-base alloys and commercial stainless steels with the calibration factors of binary alloy systems

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

    Science.gov (United States)

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

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-01-01

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

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

    Science.gov (United States)

    Correia, Paulo R. M.; Oliveira, Pedro V.

    2004-01-01

    The simultaneous determination of cadmium and lead by multi-element atomic absorption spectrometry with electrochemical atomization is proposed by employing a problem-based approach. The reports indicate that the students assimilated the principles of the simultaneous atomic absorption spectrometry (SIMAAS), the role of the chemical modifier, the…

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

  14. Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Ganjali

    2004-04-01

    Full Text Available Ultra-trace amounts of Cu(II were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone -2,2-dimethyl-1,3-propanediimine (SBTD followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

  15. New Isotope Analysis Method: Atom Trap Mass Spectrometry

    International Nuclear Information System (INIS)

    Ko, Kwang Hoon; Park, Hyun Min; Han, Jae Min; Kim, Taek Soo; Cha, Yong Ho; Lim, Gwon; Jeong, Do Young

    2011-01-01

    Trace isotope analysis has been an important role in science, archaeological dating, geology, biology and nuclear industry. Some fission products such as Sr-90, Cs-135 and Kr-85 can be released to the environment when nuclear accident occurs and the reprocessing factory operates. Thus, the analysis of artificially produced radioactive isotopes has been of interest in nuclear industry. But it is difficult to detect them due to low natural abundance less then 10 -10 . In general, radio-chemical method has been applied to detect ultra-trace radio isotopes. But this method has disadvantages of long measurement time for long lived radioisotopes and toxic chemical process for the purification. The Accelerator Mass Spectrometer has high isotope selectivity, but the system is huge and its selectivity is affected by isobars. The laser based method, such as RIMS (Resonance Ionization Mass Spectrometry) has the advantage of isobar-effect free characteristics. But the system size is still huge for high isotope selective system. Recently, ATTA (Atom Trap Trace Analysis) has been successfully applied to detect ultra-trace isotope, Kr-81 and Kr-85. ATTA is the isobar-effect free detection with high isotope selectivity and the system size is small. However, it requires steady atomic beam source during detection, and is not allowed simultaneous detection of several isotopes. In this presentation, we introduce new isotope detection method which is a coupled method of Atom Trap Mass Spectrometry (ATMS). We expect that it can overcome the disadvantage of ATTA while it has both advantages of ATTA and mass spectrometer. The basic concept and the system design will be presented. In addition, the experimental status of ATMS will also be presented

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

    International Nuclear Information System (INIS)

    Blecker, Carlo R.; Hermann, Gerd M.

    2009-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  18. The role of atomic absorption spectrometry in geochemical exploration

    Science.gov (United States)

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

    1992-01-01

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

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    Science.gov (United States)

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

    1989-12-01

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

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

    International Nuclear Information System (INIS)

    Rezacova, Olga; Dedina, Jiri

    2009-01-01

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

  3. Directional emission of single photons from small atomic samples

    DEFF Research Database (Denmark)

    Miroshnychenko, Yevhen; V. Poulsen, Uffe; Mølmer, Klaus

    2013-01-01

    We provide a formalism to describe deterministic emission of single photons with tailored spatial and temporal profiles from a regular array of multi-level atoms. We assume that a single collective excitation is initially shared by all the atoms in a metastable atomic state, and that this state i...... is coupled by a classical laser field to an optically excited state which rapidly decays to the ground atomic state. Our model accounts for the different field polarization components via re-absorption and emission of light by the Zeeman manifold of optically excited states.......We provide a formalism to describe deterministic emission of single photons with tailored spatial and temporal profiles from a regular array of multi-level atoms. We assume that a single collective excitation is initially shared by all the atoms in a metastable atomic state, and that this state...

  4. Inductively coupled plasma-atomic emission spectroscopy

    International Nuclear Information System (INIS)

    Winge, R.K.; Fassel, V.A.; Peterson, V.J.; Floyd, M.A.

    1985-01-01

    This atlas of inductively coupled plasma-atomic emission spectroscopy records the spectra of the elements in a way that would reveal the general nature of the spectra, in all their simplicity or complexity; and offers a definitive summary of the most prominent spectral lines of the elements, i.e., those most likely to be useful for the determination of trace and ultratrace concentrations; it provides reliable estimates, based on the recorded experimental spectra, of the powers of detection of the listed prominent lines; and assesses the very important problem of spectral interferences. The atlas is composed of three main sections. Part I is concerned with the historical aspects of compilations of spectral information. Part II is based on 232 wavelength scans of 70 elements. Each of the wavelength scans covers an 80 nm spectral region. These scans allow a rapid comparison of the background and spectral line intensities emitted in the ICP and provide a ready means for identification of the most prominent lines of each element and for estimation of the trace element analytical capabilities of these lines. A listing of 973 prominent lines with associated detection limits is also presented. Part III addresses the problem of spectral interferences. On this topic a detailed collection of coincidence profiles is presented for 281 of the most prominent lines, each with profiles of ten of the most prevalent concomitants superimposed. (Auth.)

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

    International Nuclear Information System (INIS)

    Krause, M.O.

    1984-01-01

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

  6. Toward improved understanding and control in analytical atomic spectrometry

    Science.gov (United States)

    Hieftje, Gary M.

    1989-01-01

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

  7. Sb(III) and Sb(V) separation and analytical speciation by a continuous tandem on-line separation device in connection with inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Menendez Garcia, A. [Oviedo Univ. (Spain). Dept. of Phys. and Anal. Chem.; Perez Rodriguez, M.C. [Oviedo Univ. (Spain). Dept. of Phys. and Anal. Chem.; Sanchez Uria, J.F. [Oviedo Univ. (Spain). Dept. of Phys. and Anal. Chem.; Sanz-Medel, A. [Oviedo Univ. (Spain). Dept. of Phys. and Anal. Chem.

    1995-09-01

    A sensitive, precise and automated non-chromatographic method for Sb(III) and Sb(V) analytical speciation based on a continuous tandem on-line separation device in connection with inductively coupled plasma-atomic emission (ICP-AES) detection is proposed. Two on-line successive separation steps are included into this method: a continuous liquid-liquid extraction of Sb(III) with ammonium pyrrolidine dithiocarbamate (APDC) into methylisobuthylketone (MIBK), followed by direct stibine generation from the organic phase. Both separation steps are carried out in a continuous mode and on-line with the ICP-AES detector. Optimization of experimental conditions for the tandem separation and ICP-AES detection are investigated in detail. Detection limits for Sb(III) were 3 ng.mL{sup -1} and for Sb(V) 8 ng.mL{sup -1}. Precisions observed are in the range {+-} 5%. The proposed methodology has been applied to Sb(III) and Sb(V) speciation in sea-water samples. (orig.)

  8. A Magnetized Nanoparticle Based Solid-Phase Extraction Procedure Followed by Inductively Coupled Plasma Atomic Emission Spectrometry to Determine Arsenic, Lead and Cadmium in Water, Milk, Indian Rice and Red Tea.

    Science.gov (United States)

    Azimi, Salameh; Es'haghi, Zarrin

    2017-06-01

    A sensitive and simple method using magnetic multi-walled carbon nanotube (MWCNTs-Fe 3 O 4 MNP), as the adsorbent, has been successfully developed for extraction and pre-concentration of arsenic, lead and cadmium with detection by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The nanosorbent was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction pattern (XRD), vibrating sample magnetometer (VSM) and transmission electron microscopy (TEM). The key factors affecting the signal intensity such as pH, adsorbent amount, etc. were investigated. Under optimal conditions, the limits of detection (three-time of signal to noise ratio, S/N 3) were 0.3, 0.6, 0.3 ng/mL for arsenic, lead and cadmium, respectively. Application of the adsorbent was investigated by the analysis of water, milk, Indian rice and red tea. The experimental data was analyzed and obeyed Langmuir and Freundlich adsorption models. The kinetic data was fitted to the pseudo-second-order model. Thermodynamic studies revealed the feasibility and exothermic nature of the system.

  9. Chemical analysis of steel by optical emission spectrometry

    International Nuclear Information System (INIS)

    Hayakawa, M.O.; Kajita, T.; Jeszensky, G.

    1981-01-01

    The development of the chemical analysis for special steels by optical emission spectrometry direct reading method with computer, at the Siderurgica N.S. Aparecida S.A. is presented. Results are presented for the low alloy steels and high speed steel. Also, the contribution of this method to the special steel preparation is commented. (Author) [pt

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

    Science.gov (United States)

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

    2017-09-01

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

  11. Atomic emission and atomic fluorescence spectroscopy in the direct current plasma

    International Nuclear Information System (INIS)

    Hendrick, M.S.

    1985-01-01

    The Direct Current Plasma (DCP) was investigated as a source for Atomic Emission (AE) and Atomic Fluorescence Spectrometry (AFS). The DCP was optimized for AE analyses using simplex optimization and Box-Behnken partial factorial experimental design, varying argon flows, and plasma position. Results were compared with a univariate search carried out in the region of the simplex optimum. Canonical analysis demonstrated that no true optimum exists for sensitivity, precision, or drift. A stationary ridge, where combinations of conditions gave comparable instrumental responses, was found. The DCP as an excitation source for AFS in a flame was used for diagnostic studies of the DCP. Moving the aerosol introduction tube behind the DCP with respect to the flame improved the characteristics of the DCP as a narrow line source, although self-absorption was observed at high concentrations of metal salt solutions in the DCP. Detection limits for Cd, Co, Cr, Cu, Fe, Mg, Mn, Zn, and Ni were in the low ng/mL region. Theoretical expressions for scatter correction with a two-line technique were derived, although no correction was necessary to achieve accurate results for standard reference materials

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

    International Nuclear Information System (INIS)

    Ataman, O. Yavuz

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-08-15

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

  15. Photoionization of Endohedral Atoms: Collective, Reflective and Collateral Emissions

    International Nuclear Information System (INIS)

    Chakraborty, Himadri S.; McCune, Matthew A.; Hopper, Dale E.; Madjet, Mohamed E.; Manson, Steven T.

    2009-01-01

    The photoionization properties of a fullerene-confined atom differ dramatically from that of an isolated atom. In the low energy region, where the fullerene plasmons are active, the electrons of the confined atom emerge through a collective channel carrying a significant chunk of plasmon with it. The photoelectron angular distribution of the confined atom however shows far lesser impact of the effect. At higher energies, the interference between two single-electron ionization channels, one directly from the atom and another reflected off the fullerene cage, producuces oscillatory cross sections. But for the outermost atomic level, which transfers some electrons to the cage, oscillations are further modulated by the collateral emission from the part of the atomic charge density transferred to the cage. These various modes of emissions are studied for the photoionization of Ar endohedrally confined in C 60 .

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-15

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

  17. Electrochemically assisted fast-atom-bombardment mass spectrometry

    International Nuclear Information System (INIS)

    Phillips, L.R.

    1988-01-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  19. Fast atom bombardment tandem mass spectrometry of carotenoids

    Energy Technology Data Exchange (ETDEWEB)

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

    1995-02-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

    McNeal, C.J.

    1982-01-01

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

  3. Determination numbers of ionized atoms from emission and absorption lines

    International Nuclear Information System (INIS)

    Alizadeh Azimi, A.; Shokouhi, N.

    2002-01-01

    Saha, M., (1920) estimated that salter chromosphere is not only due to radiation from neutral atoms, but from ionized atoms. The failure to observe these stellar lines in the laboratory was attributed to internal temperature and pressure about 10* E + 6 K 10* E-7 atm. In this research we found that emission lines of ionized atoms (like Cs) could be measured in laboratory condition, (about 10* E-3 atm and 2000 K) by using Graphite France Atomic Absorption with injection 124 u g C sel. We calculated the numbers of ionized atoms from Bottzman law. We also measured these numbers from area under the energy-time curve

  4. Liquid-Arc/Spark-Excitation Atomic-Emission Spectroscopy

    Science.gov (United States)

    Schlagen, Kenneth J.

    1992-01-01

    Constituents of solutions identified in situ. Liquid-arc/spark-excitation atomic-emission spectroscopy (LAES) is experimental variant of atomic-emission spectroscopy in which electric arc or spark established in liquid and spectrum of light from arc or spark analyzed to identify chemical elements in liquid. Observations encourage development of LAES equipment for online monitoring of process streams in such industries as metal plating, electronics, and steel, and for online monitoring of streams affecting environment.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-02-15

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

  7. The application of atomic absorption spectrometry to chemical analysis

    International Nuclear Information System (INIS)

    Walsh, A.

    1980-01-01

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

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

    Science.gov (United States)

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

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

    Czech Academy of Sciences Publication Activity Database

    D'Ulivo, A.; Dědina, Jiří

    2002-01-01

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

  10. Atom localization via controlled spontaneous emission in a five-level atomic system

    International Nuclear Information System (INIS)

    Wang Zhiping; Yu Benli; Zhu Jun; Cao Zhigang; Zhen Shenglai; Wu Xuqiang; Xu Feng

    2012-01-01

    We investigate the one- and two-dimensional atom localization behaviors via spontaneous emission in a coherently driven five-level atomic system by means of a radio-frequency field driving a hyperfine transition. It is found that the detecting probability and precision of atom localization behaviors can be significantly improved via adjusting the system parameters. More importantly, the two-dimensional atom localization patterns reveal that the maximal probability of finding an atom within the sub-wavelength domain of the standing waves can reach unity when the corresponding conditions are satisfied. As a result, our scheme may be helpful in laser cooling or the atom nano-lithography via atom localization. - Highlights: ► One- and two-dimensional atom localization behaviors via spontaneous emission in five-level atoms are investigated. ► An assisting radio-frequency field is used to control the atom localization behaviors. ► High-precision and high-resolution two-dimensional atom localization can be realized in this scheme.

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

    Science.gov (United States)

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

    2000-12-01

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

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

    Directory of Open Access Journals (Sweden)

    Welz Bernhard

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-12-15

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2015-01-01

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

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

    International Nuclear Information System (INIS)

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

    1987-01-01

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

  17. High-precision atom localization via controllable spontaneous emission in a cycle-configuration atomic system.

    Science.gov (United States)

    Ding, Chunling; Li, Jiahua; Yu, Rong; Hao, Xiangying; Wu, Ying

    2012-03-26

    A scheme for realizing two-dimensional (2D) atom localization is proposed based on controllable spontaneous emission in a coherently driven cycle-configuration atomic system. As the spatial-position-dependent atom-field interaction, the frequency of the spontaneously emitted photon carries the information about the position of the atom. Therefore, by detecting the emitted photon one could obtain the position information available, and then we demonstrate high-precision and high-resolution 2D atom localization induced by the quantum interference between the multiple spontaneous decay channels. Moreover, we can achieve 100% probability of finding the atom at an expected position by choosing appropriate system parameters under certain conditions.

  18. Theory of analytical curves in atomic fluorescence flame spectrometry

    NARCIS (Netherlands)

    Hooymayers, H.P.

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

  19. Optical emissions from oxygen atom reactions with adsorbates

    Science.gov (United States)

    Oakes, David B.; Fraser, Mark E.; Gauthier-Beals, Mitzi; Holtzclaw, Karl W.; Malonson, Mark; Gelb, Alan H.

    1992-12-01

    Although most optical materials are inert to the ambient low earth orbit environment, high velocity oxygen atoms will react with adsorbates to produce optical emissions from the ultraviolet into the infrared. The adsorbates arise from chemical releases or outgassing from the spacecraft itself. We have been investigating kinetic and spectral aspects of these phenomenon by direct observation of the 0.2 to 13 micrometers chemiluminescence from the interaction of a fast atomic oxygen beam with a continuously dosed surface. The dosing gases include fuels, combustion products and outgassed species such as unsymmetrical dimethylhydrazine (UDMH), NO, H2O and CO. The surface studied include gold and magnesium fluoride. In order to relate the results to actual spacecraft conditions these phenomena have been explored as a function of O atom velocity, dosant flux and substrate temperature. UDMH dosed surfaces exhibit spectra typical (wavelength and intensity) of carbonaceous surfaces. The primary emitters are CO, CO2, and OH. H2O dosed surfaces are dominated by OH and /or H2O emission while CO dosed surfaces are dominated by CO and CO2 emissions. The nitric oxide dosed surface produces a glow from 0.4 to 5.4 micrometers due to NO2* continuum emission. The emission was observed to increase by a factor of two upon cooling the surface from 20 degree(s)C to -35 degree(s)C.

  20. Pyrolysis gas chromatographic atomic emission detection for sediments, coals and other petrochemical precursors

    Energy Technology Data Exchange (ETDEWEB)

    Seeley, J.A.; Zeng, Y.D.; Uden, P.C.; Eglinton, T.I.; Ericson, I. (Massachusetts University, Amherst, MA (USA). Dept. of Chemistry)

    1992-09-01

    On-line flash pyrolysis coupled to a capillary gas chromatograph for the characterization of marine sediments, coals and other heterogeneous solid samples is described. A helium microwave-induced plasma is used for chromatographic detection by atomic emission spectrometry. Simultaneous multi-element detection is achieved with a photodiode array detector. The optical path of the gas chromatographic atomic emission detector is purged with helium, allowing simultaneous, sensitive detection of atomic emission from sulfur 181 nm, phosphorous 186 nm, arsenic 189 nm, selenium 196 nm and carbon 193 nm. Several sediment and coal samples have been analysed for their carbon, nitrogen, sulfur, oxygen, phosphorous, arsenic and selenium content. Qualitative information indicating the occurrence and distribution of these elements in the samples can be used to gauge the relative stage of diagenetic evolution of the samples and provide information on their depositional environment. In some instances the chromatographic behaviour of the compounds produced upon pyrolysis is improved through on-line alkylation. This on-line derivatization is achieved by adding liquid reagents to the pyrolysis probe or by adding liquid reagents to the pyrolysis probe or by adding solid reagents either to the solid sample or by packing the reagent in the injection port of the chromatograph.

  1. Cooling atoms with extraresonant stimulated emission below the Doppler limit

    International Nuclear Information System (INIS)

    Shevy, Y.

    1989-01-01

    The process of cooling atoms with radiation pressure is well understood in terms of absorption and spontaneous emission of fluorescence photons. This process imposes a lower limit on the minimum equilibrium temperature of laser cooled two level atoms of K b T = ℎΓ 21 /2 (the Doppler limit), where Γ 21 is the excited state decay rate to the ground state. At high laser intensity, it has been demonstrated that the stimulated emission process changes the sign of the force to a heating force at the red side of the atomic resonance and to a cooling force at blue detunings. Although this stimulated force is more efficient than the radiation pressure force, it has been generally accepted that this force cannot lead to lower equilibrium temperatures due to the large heating caused by diffusion of momentum at high intensity. These conclusions are valid only when the sole damping mechanism is the excited state decay to the ground state by spontaneous emission. However, when the atomic system is opened, i.e., is allowed to decay to other levels, or the dipole decay rate is altered by dephasing events, the stimulated force is dramatically modified. Under this conditions the stimulated force can occur at lower laser intensity and can even reverse sign to provide damping at the red side of resonance. These phenomena originate from extraresonances in the stimulated emission process between the two counterpropagating waves. These resonances appear as a dispersive feature in pump probe spectra (Two Wave Mixing) and are closely related to the extraresonances in four wave mixing studied originally by Bloembergen and co-workers. This paper establishes this connection and the potential of these phenomena for laser cooling. The implications of these results to the recently observed ultra-cold Na and Cs atoms are also discussed

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  4. Emission Spectrum Property of Modulated Atom-Field Coupling System

    International Nuclear Information System (INIS)

    Gao Yun-Feng; Feng Jian; Li Yue-Ke

    2013-01-01

    The emission spectrum of a two-level atom interacting with a single mode radiation field in the case of periodic oscillation coupling coefficient is investigated. A general expression for the emission spectrum is derived. The numerical results for the initial field in pure number stare are calculated. It is found that the effect of the coupling coefficient modulation on the spectral structure is very obvious in the case of a low modulation frequency and larger amplitude when the initial field is vacuum, which is potentially useful for exploring a modulated light source. (electromagnetism, optics, acoustics, heat transfer, classical mechanics, and fluid dynamics)

  5. Delta-electron emission in fast heavy ion atom collisions

    International Nuclear Information System (INIS)

    Schmidt-Boecking, H.; Ramm, U.; Berg, H.; Kelbch, C.; Feng Jiazhen; Hagmann, S.; Kraft, G.; Ullrich, J.

    1991-01-01

    The δ-electron emission processes occuring in fast heavy ion atom collisons are explained qualitatively. The different spectral structures of electron emission arising from either the target or the projectile are explained in terms of simple models of the kinetics of momentum transfer induced by the COULOMB forces. In collisions of very heavy ions with matter, high nuclear COULOMB forces are created. These forces lead to a strong polarization of the electronic states of the participated electrons. The effects of this polarization are discussed. (orig.)

  6. Utilization of atomic emission spectroscopy methods for determination of rare earth elements

    International Nuclear Information System (INIS)

    Kubova, J.; Polakovicova, J.; Medved, J.; Stresko, V.

    1997-01-01

    The authors elaborated and applied procedures for rare earth elements (REE) determination using optical emission spectrograph with D.C arc excitation and ICP atomic emission spectrometry.Some of these analytical method are described. The proposed procedure was applied for the analysis of different types of geological materials from several Slovak localities. The results the REE determination were used for e.g. investigation of REE distribution in volcanic rocks, rhyolite tuffs with uranium-molybdenum mineralization, sandstones with heavy minerals accumulations, phosphatic sandstones, granites, quartz-carbonate veins and in the meteorite found in the locality Rumanova. The REE contents were determined in 19 mineral water sources and the results obtained by the both mentioned methods compared. The total REE contents in the analysed mineral water samples were between 2 · 10 -7 and 3 · 10 -5 g dm -3

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

    International Nuclear Information System (INIS)

    D'Ulivo, Alessandro; Dedina, Jiri

    2002-01-01

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

  8. Precise atomic mass measurements by deflection mass spectrometry

    CERN Document Server

    Barber, R C

    2003-01-01

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

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

    International Nuclear Information System (INIS)

    Krata, A.; Bulska, E.

    2005-01-01

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

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

    International Nuclear Information System (INIS)

    DiDonato, G.C.

    1987-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

    Vojtková, Blanka; Dočekal, Bohumil

    2005-01-01

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

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

    NARCIS (Netherlands)

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

    1979-01-01

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

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

    Science.gov (United States)

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

  16. Emission spectrum of a harmonically trapped Λ-type three-level atom

    International Nuclear Information System (INIS)

    Guo Hong; Tang Pei

    2013-01-01

    We theoretically investigate the emission spectrum for a Λ-type three-level atom trapped in the node of a standing wave. We show that the atomic center-of-mass motion not only directly affects the peak number, peak position, and peak height in the atomic emission spectrum, but also influences the effects of the cavity field and the atomic initial state on atomic emission spectrum. (electromagnetism, optics, acoustics, heat transfer, classical mechanics, and fluid dynamics)

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    1996-01-01

    One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atomic...... the point of sample injection/introduction to the point of detection. Hence, in FI-fAAS this feature allows not only to obtain improved repeatability but also improved accuracy, and because the wash to sample ratio is high it permits the handling of samples with elevated salt contents - which...

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

    Science.gov (United States)

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

    2006-06-01

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

  19. Urinary nickel: measurement of exposure by inductively coupled plasma argon emission spectrometry.

    Science.gov (United States)

    Koizumi, Chisato; Usuda, Kan; Hayashi, Satsuki; Dote, Tomotaro; Kono, Koichi

    2004-09-01

    Nickel is a rare earth metal and is widely used in modern industry. Its overexposure in human beings can provoke significant effects including lung, cardiovascular and kidney diseases. As an index of occupational exposure, urine is widely used for the monitoring of nickel concentration because it is a minimally invasive method. Recent studies have used atomic absorption spectrometry to measure nickel concentration. In this study, we introduced novel inductively coupled plasma argon emission spectrometry (ICPAES) which enables us to measure multiple elements simultaneously with smaller volume and with lower detection limits compared to conventional atomic absorption emission spectrometry, and we established the new measuring method by determining the appropriate wavelengths for nickel concentration. Furthermore, using the established new measuring method, we investigated the correlation between a single oral administration of nickel and urine elimination in rats. As a result, different concentrations of nickel standard solutions were measured by ICPAES, and among five specific wavelengths of nickel, 221.647 and 231.604 nm were chosen because they had the highest inclines of both signal to background ratio and emission intensity in simple linear regression analysis. Next, by using healthy human urine samples that had not been exposed to nickel, 231.604 nm was determined to be the most appropriate wavelength because it did not present abnormal intensity due to obstacle wavelength. Male Wistar rats received an oral administration of nickel ranging from 0.025 to 250 mg/kg, which is equivalent to 0.0015 - 15% of LD50, and during the following 24 h, urine samples were collected and the nickel concentration was measured by ICPAES. With a single oral administration of nickel, there was an increase in urine nickel concentration in a dose-dependent manner and the appropriate equation was developed. Acute renal failure was not observed in this dosage of oral nickel

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-08-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-12-04

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

  2. Influence of Na, K, Ca and Mg on lead atomization by tungsten coil atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Oliveira Pedro V. de

    2000-01-01

    Full Text Available The atomization of lead in an electrothermal tungsten coil atomizer in the presence and absence of Na+, K+, Ca2+ and Mg2+ was investigated with the objective of understanding the interference processes. The lead atomization was less affected by Ca2+ and Mg2+ than by Na+ and K+. In the absence of concomitants, lead atomization efficiency was improved by the presence of H2 (10% v/v in the purge gas composition, during pyrolysis and atomization steps. The interference caused by Na+ and Ca2+ was negligible when the pyrolysis step was accomplished without H2 in the purge gas composition. The results showed that Na+, K+, Ca2+ and Mg2+ are directly involved in competition reactions for H2 in condensed phase.

  3. Effect of atomic initial phase difference on spontaneous emission of an atom embedded in photonic crystal

    International Nuclear Information System (INIS)

    Bing, Zhang; Xiu-Dong, Sun; Xiang-Qian, Jiang

    2010-01-01

    We investigate the effect of initial phase difference between the two excited states of a V-type three-level atom on its steady state behaviour of spontaneous emission. A modified density of modes is introduced to calculate the spontaneous emission spectra in photonic crystal. Spectra in free space are also shown to compare with that in photonic crystal with different relative positions of the excited levels from upper band-edge frequency. It is found that the initial phase difference plays an important role in the quantum interference property between the two decay channels. For a zero initial phase, destructive property is presented in the spectra. With the increase of initial phase difference, quantum interference between the two decay channels from upper levels to ground level turns to be constructive. Furthermore, we give an interpretation for the property of these spectra. (atomic and molecular physics)

  4. Spontaneous emission of an atom in the presence of nanobodies

    International Nuclear Information System (INIS)

    Klimov, Vasilii V; Ducloy, M; Letokhov, V S

    2001-01-01

    The effect of nanobodies, i.e., the bodies whose size is small compared to the emission wavelength, on spontaneous emission of an atom located near them is considered. The results of calculations performed within the framework of quantum and classical electrodynamics are presented both in analytic and graphical forms and can be readily used for planning experiments and analysis of experimental data. It is shown that nanobodies can be used to control efficiently the rate of spontaneous transitions. Thus, an excited atom located near a nanocylinder or a nanospheroid pole, whose transition dipole moment is directed normally to the nanobody surface, can decay with the rate that is tens and hundreds times higher than the decay rate in a free space. In the case of some (negative) dielectric constants, the decay rate can increase by a factor of 10 5 -10 6 and more. On the other hand, the decay of an excited atom whose transition dipole moment is directed tangentially to the nanobody surface substantially slows down. The probability of nonradiative decay of the excited state is shown to increase substantially in the presence of na-nobodies possessing losses. (review)

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

    Science.gov (United States)

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

    1994-12-01

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

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

    Science.gov (United States)

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

    2008-09-15

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

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

    Science.gov (United States)

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

    1996-09-15

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

  8. Bringing part of the lab to the field: On-site chromium speciation in seawater by electrodeposition of Cr(III)/Cr(VI) on portable coiled-filament assemblies and measurement in the lab by electrothermal, near-torch vaporization sample introduction and inductively coupled plasma-atomic emission spectrometry

    Science.gov (United States)

    Badiei, Hamid R.; McEnaney, Jennifer; Karanassios, Vassili

    2012-12-01

    A field-deployable electrochemical approach to preconcentration, matrix clean up and selective electrodeposition of Cr(III) and Cr(III) + Cr(VI) in seawater is described. Using portable, battery-operated electrochemical instrumentation, Cr species in seawater were electrodeposited in the field on portable coiled-filament assemblies made from Re. Assemblies with dried residues of Cr(III) or Cr(III) + Cr(VI) on them were transported to the lab for concentration determination by electrothermal, near-torch vaporization (NTV) sample introduction and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Electrodeposition offers selective species deposition, preconcentration and matrix clean up from seawater samples. For selective deposition, free Cr(VI) was electrodeposited at - 0.3 V and Cr(III) + Cr(VI) at - 1.6 V (both vs Ag/AgCl). Interestingly, at 0 V (vs Ag/AgCl) and in the absence of an electrodeposition potential only Cr(VI) was spontaneously and selectively adsorbed on the coil and reasons for this are given. Due to preconcentration afforded by electrodeposition, the detection limits obtained after a 60 s electrodeposition at the voltages stated above using buffered (pH = 4.7) artificial seawater spiked with either Cr(III) or Cr(VI) were 20 pg/mL for Cr(III) and 10 pg/mL for Cr(VI). For comparison, the detection limit for Cr obtained by pipetting directly on the coil 5 μL of diluted standard solution was 500 pg/mL, thus it was concluded that electrodeposition offered 40 to 60 fold improvements. Matrix clean up is required due to the high salt content of seawater and this was addressed by simply rinsing the coil with 18.2 MΩ water without any loss of Cr species. Reasons for this are provided. The method was validated in the lab using buffered artificial seawater and it was used in the field for the first time by sampling seawater, buffering it and immediately electrodepositing Cr species on portable assemblies on-site. Electrodeposition in the

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

    Science.gov (United States)

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

    2002-02-01

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

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

    Science.gov (United States)

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

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

    Science.gov (United States)

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

    1996-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    Science.gov (United States)

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

    1981-07-01

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

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

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

  17. Direct determination of selenoproteins in polyvinylidene difluoride membranes by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Sidenius, U; Gammelgaard, Bente

    2000-01-01

    A method for the direct determination of selenoproteins in plastic membranes after protein separation by gel electrophoresis was developed. Quantification was based on the determination of the selenium content of the proteins by electrothermal atomic absorption spectrometry (ET-AAS) after manual...... were excised and chemical modifier was added on top of the excised membrane prior to atomic absorption measurement. Acceptable linearity was achieved in the range 2-10 ng Se, corresponding to selenium concentrations close to 1 mg/L, when aqueous solutions of selenomethionine standard as well...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-04-08

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

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

    Science.gov (United States)

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

    2011-04-08

    The analysis of wine is of great importance since wine components strongly determine its stability, organoleptic or nutrition characteristics. In addition, wine analysis is also important to prevent fraud and to assess toxicological issues. Among the different analytical techniques described in the literature, atomic spectrometry has been traditionally employed for elemental wine analysis due to its simplicity and good analytical figures of merit. The scope of this review is to summarize the main advantages and drawbacks of various atomic spectrometry techniques for elemental wine analysis. Special attention is paid to interferences (i.e. matrix effects) affecting the analysis as well as the strategies available to mitigate them. Finally, latest studies about wine speciation are briefly discussed. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Smith, D.H. (ed.)

    1978-11-01

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

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

    International Nuclear Information System (INIS)

    Smith, D.H.

    1978-11-01

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

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

    Directory of Open Access Journals (Sweden)

    Yuya Koike

    2017-03-01

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

  4. In-situ optical emission spectrometry during galvanostatic aluminum anodising

    International Nuclear Information System (INIS)

    Mercier, D.; Van Overmeere, Q.; Santoro, R.; Proost, J.

    2011-01-01

    In this study, we report on the use of optical emission spectrometry (OES) for the online detection of changes in the Al concentration ejected in a 1.0 mol dm -3 sulphuric acid electrolyte during galvanostatic anodising of Al thin film substrates. The technique relies on the coupling of an Inductively Coupled Plasma (ICP) spectrometer to a specially designed electrochemical flow cell. This has allowed to correlate, for the first time, the kinetics of Al dissolution to well-established morphological changes related to porous anodic oxide formation and growth. A deconvolution algorithm was first developed in order to decompose the experimental ICP/OES signal into elementary distributions, each one characteristic for a specific kinetic regime. The highest dissolution rate systematically occurred during the first step, associated with barrier oxide formation. This is followed by a systematic decrease in the rate of Al dissolution during pore formation. During steady-state porous oxide growth, the Al dissolution rate increases again, but still remains below the level established during barrier oxide growth. In each of these three kinetic regimes, a linear variation of the Al dissolution rate with current density was observed in the range 0.5-5.0 mA cm -2 , with slope values of, respectively, 35 ± 2, 24 ± 2 and 28 ± 1 μg C -1 . Regarding the temporal transitions between the different regimes, a desynchronisation was observed between the kinetic (dissolution) and morphological transitions, the time offset going in opposite directions for barrier and steady-state porous oxide growth. Finally, using the measured Al dissolution rates, the current density dependence of the film formation efficiency for both porous and barrier oxide growth has been established.

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

    International Nuclear Information System (INIS)

    Li Fangqing

    2006-01-01

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

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

    OpenAIRE

    NUKATSUKA, Isoshi; OHZEKI, Kunio

    2006-01-01

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

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

    International Nuclear Information System (INIS)

    Capdevila, C.; Alduan, F.A.

    1980-01-01

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

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

    DEFF Research Database (Denmark)

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

    1986-01-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2014-06-11

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

  11. Modeling Emission of Heavy Energetic Neutral Atoms from the Heliosphere

    International Nuclear Information System (INIS)

    Swaczyna, Paweł; Bzowski, Maciej

    2017-01-01

    Observations of energetic neutral atoms (ENAs) are a fruitful tool for remote diagnosis of the plasma in the heliosphere and its vicinity. So far, instruments detecting ENAs from the heliosphere were configured for observations of hydrogen atoms. Here, we estimate emissions of ENAs of the heavy chemical elements helium, oxygen, nitrogen, and neon. A large portion of the heliospheric ENAs is created in the inner heliosheath from neutralized interstellar pick-up ions (PUIs). We modeled this process and calculated full-sky intensities of ENAs for energies 0.2–130 keV/nuc. We found that the largest fluxes among considered species are expected for helium, smaller for oxygen and nitrogen, and smallest for neon. The obtained intensities are 50–10 6 times smaller than the hydrogen ENA intensities observed by IBEX . The detection of heavy ENAs will be possible if a future ENA detector is equipped with the capability to measure the masses of observed atoms. Because of different reaction cross-sections among the different species, observations of heavy ENAs can allow for a better understanding of global structure of the heliosphere as well as the transport and energization of PUIs in the heliosphere.

  12. Modeling Emission of Heavy Energetic Neutral Atoms from the Heliosphere

    Energy Technology Data Exchange (ETDEWEB)

    Swaczyna, Paweł; Bzowski, Maciej, E-mail: pswaczyna@cbk.waw.pl [Space Research Centre of the Polish Academy of Sciences (CBK PAN), Bartycka 18A, 00-716 Warsaw (Poland)

    2017-09-10

    Observations of energetic neutral atoms (ENAs) are a fruitful tool for remote diagnosis of the plasma in the heliosphere and its vicinity. So far, instruments detecting ENAs from the heliosphere were configured for observations of hydrogen atoms. Here, we estimate emissions of ENAs of the heavy chemical elements helium, oxygen, nitrogen, and neon. A large portion of the heliospheric ENAs is created in the inner heliosheath from neutralized interstellar pick-up ions (PUIs). We modeled this process and calculated full-sky intensities of ENAs for energies 0.2–130 keV/nuc. We found that the largest fluxes among considered species are expected for helium, smaller for oxygen and nitrogen, and smallest for neon. The obtained intensities are 50–10{sup 6} times smaller than the hydrogen ENA intensities observed by IBEX . The detection of heavy ENAs will be possible if a future ENA detector is equipped with the capability to measure the masses of observed atoms. Because of different reaction cross-sections among the different species, observations of heavy ENAs can allow for a better understanding of global structure of the heliosphere as well as the transport and energization of PUIs in the heliosphere.

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

    International Nuclear Information System (INIS)

    1996-01-01

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

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

    Science.gov (United States)

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

    2017-04-01

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

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

    International Nuclear Information System (INIS)

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

    1981-01-01

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

  16. Measurement of fluorescence emission spectrum of few strongly driven atoms using an optical nanofiber.

    Science.gov (United States)

    Das, Manoj; Shirasaki, A; Nayak, K P; Morinaga, M; Le Kien, Fam; Hakuta, K

    2010-08-02

    We show that the fluorescence emission spectrum of few atoms can be measured by using an optical nanofiber combined with the optical heterodyne and photon correlation spectroscopy. The observed fluorescence spectrum of the atoms near the nanofiber shows negligible effects of the atom-surface interaction and agrees well with the Mollow triplet spectrum of free-space atoms at high excitation intensity.

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

    International Nuclear Information System (INIS)

    Bye, R.

    1986-01-01

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

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

    Science.gov (United States)

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

    2011-06-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, H.; Krawczyk, M. [Politechn Poznanska, Poznan (Poland)

    2007-03-15

    The analytical performance of coupled hydride generation - integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H{sub 2}Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangernents (a water-cooled single silica tube, double-slotted quartz tube or an 'integrated trap') was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3{sigma}), was 0.9 ng mL{sup -1} for Te. For a 2 min in situ preconcentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% (n = 6) for Te. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-01-15

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

  2. Two-dimensional sub-half-wavelength atom localization via controlled spontaneous emission.

    Science.gov (United States)

    Wan, Ren-Gang; Zhang, Tong-Yi

    2011-12-05

    We propose a scheme for two-dimensional (2D) atom localization based on the controlled spontaneous emission, in which the atom interacts with two orthogonal standing-wave fields. Due to the spatially dependent atom-field interaction, the position probability distribution of the atom can be directly determined by measuring the resulting spontaneously emission spectrum. The phase sensitive property of the atomic system leads to quenching of the spontaneous emission in some regions of the standing-waves, which significantly reduces the uncertainty in the position measurement of the atom. We find that the frequency measurement of the emitted light localizes the atom in half-wavelength domain. Especially the probability of finding the atom at a particular position can reach 100% when a photon with certain frequency is detected. By increasing the Rabi frequencies of the driving fields, such 2D sub-half-wavelength atom localization can acquire high spatial resolution.

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

    Directory of Open Access Journals (Sweden)

    Sanda Rončević

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  5. Bringing part of the lab to the field: On-site chromium speciation in seawater by electrodeposition of Cr(III)/Cr(VI) on portable coiled-filament assemblies and measurement in the lab by electrothermal, near-torch vaporization sample introduction and inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Badiei, Hamid R.; McEnaney, Jennifer; Karanassios, Vassili

    2012-01-01

    A field-deployable electrochemical approach to preconcentration, matrix clean up and selective electrodeposition of Cr(III) and Cr(III) + Cr(VI) in seawater is described. Using portable, battery-operated electrochemical instrumentation, Cr species in seawater were electrodeposited in the field on portable coiled-filament assemblies made from Re. Assemblies with dried residues of Cr(III) or Cr(III) + Cr(VI) on them were transported to the lab for concentration determination by electrothermal, near-torch vaporization (NTV) sample introduction and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Electrodeposition offers selective species deposition, preconcentration and matrix clean up from seawater samples. For selective deposition, free Cr(VI) was electrodeposited at − 0.3 V and Cr(III) + Cr(VI) at − 1.6 V (both vs Ag/AgCl). Interestingly, at 0 V (vs Ag/AgCl) and in the absence of an electrodeposition potential only Cr(VI) was spontaneously and selectively adsorbed on the coil and reasons for this are given. Due to preconcentration afforded by electrodeposition, the detection limits obtained after a 60 s electrodeposition at the voltages stated above using buffered (pH = 4.7) artificial seawater spiked with either Cr(III) or Cr(VI) were 20 pg/mL for Cr(III) and 10 pg/mL for Cr(VI). For comparison, the detection limit for Cr obtained by pipetting directly on the coil 5 μL of diluted standard solution was 500 pg/mL, thus it was concluded that electrodeposition offered 40 to 60 fold improvements. Matrix clean up is required due to the high salt content of seawater and this was addressed by simply rinsing the coil with 18.2 MΩ water without any loss of Cr species. Reasons for this are provided. The method was validated in the lab using buffered artificial seawater and it was used in the field for the first time by sampling seawater, buffering it and immediately electrodepositing Cr species on portable assemblies on-site. Electrodeposition in the

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-11-01

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

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

    Science.gov (United States)

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

    2004-08-01

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

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    2002-01-01

    Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS...

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

    International Nuclear Information System (INIS)

    Schmid, E.

    1987-03-01

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

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

    Science.gov (United States)

    Li, Tao; Wang, Yuan-Zhong

    2008-04-01

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

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

    OpenAIRE

    Ensafi, Ali A.; Shiraz, Ameneh Zendegi

    2008-01-01

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

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

    CERN Document Server

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

    2002-01-01

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

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

    Science.gov (United States)

    Swart, D J; Simeonsson, J B

    1999-11-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-08-01

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

  16. Sub-microanalysis of solid samples with near-field enhanced atomic emission spectroscopy

    Science.gov (United States)

    Wang, Xiaohua; Liang, Zhisen; Meng, Yifan; Wang, Tongtong; Hang, Wei; Huang, Benli

    2018-03-01

    A novel approach, which we have chosen to name it as near-field enhanced atomic emission spectroscopy (NFE-AES), was proposed by introducing a scanning tunnelling microscope (STM) system into a laser-induced breakdown spectrometry (LIBS). The near-field enhancement of a laser-illuminated tip was utilized to improve the lateral resolution tremendously. Using the hybrid arrangement, pure metal tablets were analyzed to verify the performance of NFE-AES both in atmosphere and in vacuum. Due to localized surface plasmon resonance (LSPR), the incident electromagnetic field is enhanced and confined at the apex of tip, resulting in sub-micron scale ablation and elemental emission signal. We discovered that the signal-to-noise ratio (SNR) and the spectral resolution obtained in vacuum condition are better than those acquired in atmospheric condition. The quantitative capability of NFE-AES was demonstrated by analyzing Al and Pb in Cu matrix, respectively. Submicron-sized ablation craters were achieved by performing NFE-AES on a Si wafer with an Al film, and the spectroscopic information from a crater of 650 nm diameter was successfully obtained. Due to its advantage of high lateral resolution, NFE-AES imaging of micro-patterned Al lines on an integrated circuit of a SIM card was demonstrated with a sub-micron lateral resolution. These results reveal the potential of the NFE-AES technique in sub-microanalysis of solids, opening an opportunity to map chemical composition at sub-micron scale.

  17. Development of the Flame Test Concept Inventory: Measuring Student Thinking about Atomic Emission

    Science.gov (United States)

    Bretz, Stacey Lowery; Murata Mayo, Ana Vasquez

    2018-01-01

    This study reports the development of a 19-item Flame Test Concept Inventory, an assessment tool to measure students' understanding of atomic emission. Fifty-two students enrolled in secondary and postsecondary chemistry courses were interviewed about atomic emission and explicitly asked to explain flame test demonstrations and energy level…

  18. Improved documentation of spectral lines for inductively coupled plasma emission spectrometry

    Science.gov (United States)

    Doidge, Peter S.

    2018-05-01

    An approach to improving the documentation of weak spectral lines falling near the prominent analytical lines used in inductively coupled plasma optical emission spectrometry (ICP-OES) is described. Measurements of ICP emission spectra in the regions around several hundred prominent lines, using concentrated solutions (up to 1% w/v) of some 70 elements, and comparison of the observed spectra with both recent published work and with the output of a computer program that allows calculation of transitions between the known energy levels, show that major improvements can be made in the coverage of spectral atlases for ICP-OES, with respect to "classical" line tables. It is argued that the atomic spectral data (wavelengths, energy levels) required for the reliable identification and documentation of a large majority of the weak interfering lines of the elements detectable by ICP-OES now exist, except for most of the observed lines of the lanthanide elements. In support of this argument, examples are provided from a detailed analysis of a spectral window centered on the prominent Pb II 220.353 nm line, and from a selected line-rich spectrum (W). Shortcomings in existing analyses are illustrated with reference to selected spectral interferences due to Zr. This approach has been used to expand the spectral-line library used in commercial ICP-ES instruments (Agilent 700-ES/5100-ES). The precision of wavelength measurements is evaluated in terms of the shot-noise limit, while the absolute accuracy of wavelength measurement is characterised through comparison with a small set of precise Ritz wavelengths for Sb I, and illustrated through the identification of Zr III lines; it is further shown that fractional-pixel absolute wavelength accuracies can be achieved. Finally, problems with the wavelengths and classifications of certain Au I lines are discussed.

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

    Science.gov (United States)

    Panyabut, Teerawat; Sirirat, Natnicha; Siripinyanond, Atitaya

    2018-02-13

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

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

    International Nuclear Information System (INIS)

    Elhag, A. Y.

    2004-01-01

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

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

    International Nuclear Information System (INIS)

    Dian Anggraini; Rosika Kriswarini; Yusuf N

    2007-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2014-01-01

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

  3. Comparison of 15N analysis by optical emission spectrometry and mass spectrometry for clinical studies during total parenteral nutrition

    International Nuclear Information System (INIS)

    Ragon, A.; Reynier, J.P.; Guiraud, G.

    1985-01-01

    During total and stable parenteral nutrition, a branched chain amino acid enriched solution containing [ 15 N]leucine was infused into a patient to determine the fate of the nitrogen administered through this formulation. Measurements of 15 N isotopic enrichments were performed on the same biological samples (urinary urea, total plasma proteins and albumin) by optical emission spectrometry (OES) and mass spectrometry (MS) to determine if OES with its specific advantages (cost, handling maintenance) constituted even with low enrichments a useful alternative technique to MS considered as the reference method. The results show that OES constituted a very useful analytical technique to obtain reliable information in clinical metabolic studies when low 15 N enrichments must be determined. (Auth.)

  4. Pulsed, atmospheric pressure plasma source for emission spectrometry

    Science.gov (United States)

    Duan, Yixiang; Jin, Zhe; Su, Yongxuan

    2004-05-11

    A low-power, plasma source-based, portable molecular light emission generator/detector employing an atmospheric pressure pulsed-plasma for molecular fragmentation and excitation is described. The average power required for the operation of the plasma is between 0.02 W and 5 W. The features of the optical emission spectra obtained with the pulsed plasma source are significantly different from those obtained with direct current (dc) discharge higher power; for example, strong CH emission at 431.2 nm which is only weakly observed with dc plasma sources was observed, and the intense CN emission observed at 383-388 nm using dc plasma sources was weak in most cases. Strong CN emission was only observed using the present apparatus when compounds containing nitrogen, such as aniline were employed as samples. The present apparatus detects dimethylsulfoxide at 200 ppb using helium as the plasma gas by observing the emission band of the CH radical. When coupled with a gas chromatograph for separating components present in a sample to be analyzed, the present invention provides an apparatus for detecting the arrival of a particular component in the sample at the end of the chromatographic column and the identity thereof.

  5. Determination of lithium and potassium in uranium oxide powders and pellets by Flame Atomic Emission Spectrometric method

    International Nuclear Information System (INIS)

    Jat, J.R.; Balaji Rao, Y.; Prasada Rao, G.; Prahlad, B.

    2012-01-01

    The present paper describes a method developed at Control Laboratory, NFC which includes prior separation of lithium and potassium from uranium matrix before their measurements. Solvent extraction, using Tri-n-Butyl Phosphate (TBP) in CCI 4 followed by Tri-n-Octyl Phosphine Oxide (TOPO) in CCI 4 , is employed for prior separation of Li and K. The resultant aqueous solution was analyzed by Flame-Atomic Emission Spectrometric (AES) method. Solvent extraction conditions are optimized for measurement of Li and K in the same aliquot. Experimental conditions such as instrument calibration, flame condition, fuel flow, sample flow rate through nebulizer, burner height etc. are also optimized. Under the optimal condition the detection limits achieved for lithium is 0.02 ppm and 0.2 ppm for potassium. A RSD of ± 3 % for Li at 0.05 ppm and ± 4% for K at 1 ppm level has been achieved in this method. The results of lithium in the sample are compared with the values obtained by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Similarly, values of potassium are compared with Flame-Atomic Absorption Spectrometry (Flame-AAS) technique. The comparisons are in good agreement. The above method is simple, sensitive, reproducible and can be used for measurement of lithium and potassium in UO 2 powder and pellets on regular basis

  6. Apparatus and method for transient thermal infrared emission spectrometry

    Science.gov (United States)

    McClelland, John F.; Jones, Roger W.

    1991-12-24

    A method and apparatus for enabling analysis of a solid material (16, 42) by applying energy from an energy source (20, 70) top a surface region of the solid material sufficient to cause transient heating in a thin surface layer portion of the solid material (16, 42) so as to enable transient thermal emission of infrared radiation from the thin surface layer portion, and by detecting with a spectrometer/detector (28, 58) substantially only the transient thermal emission of infrared radiation from the thin surface layer portion of the solid material. The detected transient thermal emission of infrared radiation is sufficiently free of self-absorption by the solid material of emitted infrared radiation, so as to be indicative of characteristics relating to molecular composition of the solid material.

  7. 134Cs emission probabilities determination by gamma spectrometry

    Science.gov (United States)

    de Almeida, M. C. M.; Poledna, R.; Delgado, J. U.; Silva, R. L.; Araujo, M. T. F.; da Silva, C. J.

    2018-03-01

    The National Laboratory for Ionizing Radiation Metrology (LNMRI/IRD/CNEN) of Rio de Janeiro performed primary and secondary standardization of different radionuclides reaching satisfactory uncertainties. A solution of 134Cs radionuclide was purchased from commercial supplier to emission probabilities determination of some of its energies. 134Cs is a beta gamma emitter with 754 days of half-life. This radionuclide is used as standard in environmental, water and food control. It is also important to germanium detector calibration. The gamma emission probabilities (Pγ) were determined mainly for some energies of the 134Cs by efficiency curve method and the Pγ absolute uncertainties obtained were below 1% (k=1).

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

    International Nuclear Information System (INIS)

    Shimizu, Tokuo; Shijo, Yoshio; Sakai, Kaoru

    1981-01-01

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

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

    International Nuclear Information System (INIS)

    Gatford, C.; Torrance, K.

    1988-06-01

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

  10. Isotopic Tracing of Fuel Components in Particulate Emissions from Diesel Engines using Accelerator Mass Spectrometry (AMS)

    International Nuclear Information System (INIS)

    Buchholz, B A; Mueller, C J; Garbak, J.

    2001-01-01

    Accelerator mass spectrometry (AMS) is an isotope-ratio measurement technique developed in the late 1970s for tracing long-lived radioisotopes (e.g., 14 C half life = 5760 y). The technique counts individual nuclei rather than waiting for their radioactive decay, allowing measurement of more than 100 low-level 14 C samples per day (Vogel et al, 1995). The LLNL AMS system is shown in Fig.1. The contemporary quantity of 14 C in living things ( 14 C/C = 1.2 x 10 -12 or 110 fmol 14 C/ g C) is highly elevated compared to the quantity of 14 C in petroleum-derived products. This isotopic elevation is sufficient to trace the fate of bio-derived fuel components in the emissions of an engine without the use of radioactive materials. If synthesis of a fuel component from biologically-derived source material is not feasible, another approach is to purchase 14 C-labeled material (e.g., dibutyl maleate (DBM)) and dilute it with petroleum-derived material to yield a contemporary level of 14 C. In each case, the virtual absence of 14 C in petroleum based fuels gives a very low 14 C background that makes this approach to tracing fuel components practical. Regulatory pressure to significantly reduce the particulate emissions from diesel engines is driving research into understanding mechanisms of soot formation. If mechanisms are understood, then combustion modeling can be used to evaluate possible changes in fuel formulation and suggest possible fuel components that can improve combustion and reduce PM emissions. The combustion paradigm assumes that large molecules break down into small components and then build up again during soot formation. AMS allows us to label specific fuel components, including oxygenates, trace the carbon atoms, and test this combustion modeling paradigm. Volatile and non-volatile organic fractions (VOF, NVOF) in the PM can be further separated. The VOF of the PM can be oxidized with catalysts in the exhaust stream to further decrease PM. The effectiveness

  11. {sup 134}Cs emission probabilities determination by gamma spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, M.C.M. de, E-mail: candida@cnen.gov.br [Comissão Nacional de Energia Nuclear (DINOR/CNEN), Riode Janeiro, RJ (Brazil); Poledna, R.; Delgado, J.U.; Silva, R.L.; Araujo, M.T.; Silva, C.J. da [Instituto de Radioproteção e Dosimetria (LNMRI/IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2017-07-01

    The National Laboratory for Ionizing Radiation Metrology (LNMRI/IRD/CNEN) of Rio de Janeiro performed primary and secondary standardization of different radionuclides reaching satisfactory uncertainties. A solution of {sup 134}Cs radionuclide was purchased from commercial supplier to emission probabilities determination of some of its energies. {sup 134}Cs is a beta gamma emitter with 754 days of half-life. This radionuclide is used as standard in environmental, water and food control. It is also important to germanium detector calibration.The gamma emission probabilities (Pγ) were determined mainly for some energies of the {sup 134}Cs by efficiency curve method and the Pγ absolute uncertainties obtained were below 1% (k=1). (author)

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

    Science.gov (United States)

    Frentiu, Tiberiu; Ponta, Michaela; Hategan, Raluca

    2013-03-01

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

  13. Analysis of zirconium alloys using inductively-coupled plasma emission spectrometry

    International Nuclear Information System (INIS)

    White, G.F.; Pickford, C.J.

    1982-06-01

    As part of an interlaboratory collaborative exercise, certain trace and minor elements have been determined in a proposed zircaloy reference material using inductively-coupled plasma emission spectrometry. A dissolution procedure involving hydrochloric and hydrofluoric acids was used for determination of Hf, Cr, Fe and Sn. Data have also been obtained for Ni, Cu and Mn. Use of a high resolution monochromator in a scanning mode was found necessary for measurement of the emission intensities in order to resolve the spectral lines of interest from the intense and complex emission from the zirconium matrix. (author)

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-04-15

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2018-03-01

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

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

    Science.gov (United States)

    Zhang, Q L; Gao, G

    2016-04-20

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

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

    Science.gov (United States)

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

    2007-06-01

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

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

    Science.gov (United States)

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

    2016-09-14

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

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

    Science.gov (United States)

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

    2017-01-01

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

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

    International Nuclear Information System (INIS)

    Mermet, Jean-Michel

    2010-01-01

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

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

    International Nuclear Information System (INIS)

    Mandiwana, Khakhathi L.; Panichev, Nikolay

    2010-01-01

    Solid Certified Reference Materials (CRMs) with known vanadium(+5) content are currently not commercially available. Because of this, vanadium species have been determined in solid CRMs of soil, viz. CRM023-50, CRM024-50, CRM049-50, SQC001 and SQC0012. These CRMs are certified with only total vanadium content. Vanadium(+5) was extracted from soil reference materials with 0.1 M Na 2 CO 3 . The quantification of V(+5) was carried out by electrothermal atomic absorption spectrometry (ET-AAS). The concentration of V(+5) in the analyzed CRMs was found to be ranging between 3.60 and 86.0 μg g -1 . It was also found that SQC001 contains approximately 88% of vanadium as V(+5) species. Statistical evaluation of the results of the two methods by paired t-test was in good agreement at 95% level of confidence.

  7. Determination of Te in soldering tin using continuous flowing electrochemical hydride generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Jiang Xianjuan; Gan Wuer; Han Suping; He Youzhao

    2008-01-01

    An electrochemical hydride generation system was developed for the detection of Te by coupling an electrochemical hydride generator with atomic fluorescence spectrometry. Since TeH 2 is unstable and easily decomposes in solution, a reticular W filament cathode was used in the present system. The TeH 2 generated on the cathode surface was effectively driven out by sweeping gas from the cathode chamber. In addition, a low temperature electrochemical cell (10 deg. C) was applied to reduce the decomposition of TeH 2 in solution. The limit of detection (LOD) was 2.2 ng ml -1 and the relative standard deviation (RSD) was 3.9% for nine consecutive measurements of standard solution. This method was successfully employed for determination of Te in soldering tin material

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  9. Inductively coupled plasma atomic emission spectrometric determination of tin in canned food.

    Science.gov (United States)

    Sumitani, H; Suekane, S; Nakatani, A; Tatsuka, K

    1993-01-01

    Various canned foods were digested sequentially with HNO3 and HCl, diluted to 100 mL, and filtered, and then tin was determined by inductively coupled plasma atomic emission spectrometry (ICP/AES). Samples of canned Satsuma mandarin, peach, apricot, pineapple, apple juice, mushroom, asparagus, evaporated milk, short-necked clam, spinach, whole tomato, meat, and salmon were evaluated. Sample preparations did not require time-consuming dilutions, because ICP/AES has wide dynamic range. The standard addition method was used to determine tin concentration. Accuracy of the method was tested by analyzing analytical standards containing tin at 2 levels (50 and 250 micrograms/g). The amounts of tin found for the 50 and 250 micrograms/g levels were 50.5 and 256 micrograms/g, respectively, and the repeatability coefficients of variation were 4.0 and 3.8%, respectively. Recovery of tin from 13 canned foods spiked at 2 levels (50 and 250 micrograms/g) ranged from 93.9 to 109.4%, with a mean of 99.2%. The quantitation limit for tin standard solution was about 0.5 microgram/g.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-01

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

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

    International Nuclear Information System (INIS)

    Katskov, Dmitri

    2015-01-01

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

  12. Ultrafast atomic process in X-ray emission by using inner-shell ionization method for sodium and carbon atoms

    Energy Technology Data Exchange (ETDEWEB)

    Moribayashi, Kengo; Sasaki, Akira; Tajima, Toshiki [Japan Atomic Energy Research Inst., Neyagawa, Osaka (Japan). Kansai Research Establishment

    1998-07-01

    An ultrafast inner-shell ionization process with X-ray emission stimulated by high-intensity short-pulse X-ray is studied. Carbon and sodium atoms are treated as target matter. It is shown that atomic processes of the target determine the necessary X-ray intensity for X-ray laser emission as well as the features of X-ray laser such as wavelength and duration time. The intensity also depends on the density of initial atoms. Furthermore, we show that as the intensity of X-ray source becomes high, the multi-inner-shell ionization predominates, leading to the formation of hollow atoms. As the density of hollow atoms is increased by the pumping X-ray power, the emission of X-rays is not only of significance for high brightness X-ray measurement but also is good for X-ray lasing. New classes of experiments of pump X-ray probe and X-ray laser are suggested. (author)

  13. Determination of aluminium, scandium and rare earth elements by emission flame spectrometry

    International Nuclear Information System (INIS)

    Otruba, V.; Sommer, L.

    1989-01-01

    Emission spectrometry in nitrous oxide-acetylene flames in combination with a highly resolving double monochromator and sensitive detecting system enables simple, sensitive and selective determinations of aluminium, scandium and all rare earth elements with exception of cerium in complicated matrices. Calibration plots are linear for a large concentration interval (≤ 100 μgxml -1 ), detection limits are in ngxml -1 level and RSD does not exceed 3% on the optimal concentration level of the particular element. The determination of Al, Sc, Eu and Yb showed particular advantages as to methods using ICP-spectrometry. (orig.)

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

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination...... spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 sigma) achieved by the HPLC-FAAS system was 1 mg L-1 of selenium (100 mu L injections) for each of the four...

  15. Mercury in Environmental and Biological Samples Using Online Combustion with Sequential Atomic Absorption and Fluorescence Measurements: A Direct Comparison of Two Fundamental Techniques in Spectrometry

    Science.gov (United States)

    Cizdziel, James V.

    2011-01-01

    In this laboratory experiment, students quantitatively determine the concentration of an element (mercury) in an environmental or biological sample while comparing and contrasting the fundamental techniques of atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). A mercury analyzer based on sample combustion,…

  16. Study of atomic and molecular emission spectra of Sr by laser induced breakdown spectroscopy (LIBS).

    Science.gov (United States)

    Bhatt, Chet R; Alfarraj, Bader; Ayyalasomayajula, Krishna K; Ghany, Charles; Yueh, Fang Y; Singh, Jagdish P

    2015-12-01

    Laser Induced Breakdown Spectroscopy (LIBS) is an ideal analytical technique for in situ analysis of elemental composition. We have performed a comparative study of the quantitative and qualitative analysis of atomic and molecular emission from LIBS spectra. In our experiments, a mixture of SrCl2 and Al2O3 in powder form was used as a sample. The atomic emission from Sr and molecular emission from SrCl and SrO observed in LIBS spectra were analyzed. The optimum laser energies, gate delays, and gate widths for selected atomic lines and molecular bands were determined from spectra recorded at various experimental parameters. These optimum experimental conditions were used to collect calibration data, and the calibration curves were used to predict the Sr concentration. Limits of detection (LODs) for selected atomic and molecular emission spectra were determined.

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

    Czech Academy of Sciences Publication Activity Database

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

    2017-01-01

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

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

    Science.gov (United States)

    Pfennig, Brian W.; Schaefer, Amy K.

    2011-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2017-01-01

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

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

    NARCIS (Netherlands)

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

    1989-01-01

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

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

    International Nuclear Information System (INIS)

    Vrebos, B.

    1996-01-01

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

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

    International Nuclear Information System (INIS)

    Jiang, X.; Smith, D.L.

    1987-01-01

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

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

    International Nuclear Information System (INIS)

    Konecna, Marie; Komarek, Josef

    2007-01-01

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

  4. Frequency shifts in spontaneous emission from two interacting atoms

    International Nuclear Information System (INIS)

    James, D.F.V.

    1993-01-01

    A model radiating system consisting of two atoms in close proximity is analyzed. This system demonstrates the influence of spatial coherence on the spectrum of the radiation field. Explicit expressions for the degree of coherence, the source spectrum, and the spectrum of the radiation field are derived. The results are discussed in terms of Wolf's work [Phys. Rev. Lett. 56, 1370 (1986)] on this effect, which can be considered in terms of a multiple-atom analog of the effects of radiation reaction on a single atom, i.e., spontaneous decay and the Lamb shift

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

    Science.gov (United States)

    Sirirat, Natnicha; Tetbuntad, Kornrawee; Siripinyanond, Atitaya

    2017-03-01

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

  6. Localization of the relative position of two atoms induced by spontaneous emission

    International Nuclear Information System (INIS)

    Zheng, L.; Li, C.; Li, Y.; Sun, C.P.

    2005-01-01

    We reexamine the back-action of emitted photons on the wave packet evolution about the relative position of two cold atoms. We show that photon recoil resulting from the spontaneous emission can induce the localization of the relative position of the two atoms through the entanglement between the spatial motion of individual atoms and their emitted photons. The obtained result provides a more realistic model for the analysis of the environment-induced localization of a macroscopic object

  7. Visible Light Emission from Atomic Scale Patterns Fabricated by the Scanning Tunneling Microscope

    DEFF Research Database (Denmark)

    Thirstrup, C.; Sakurai, M.; Stokbro, Kurt

    1999-01-01

    Scanning tunneling microscope (STM) induced light emission from artificial atomic scale structures comprising silicon dangling bonds on hydrogen-terminated Si(001) surfaces has been mapped spatially and analyzed spectroscopically in the visible spectral range. The light emission is based on a novel...

  8. Electron and X-ray emission in collisions of multiply charged ions and atoms

    International Nuclear Information System (INIS)

    Woerlee, P.H.

    1979-01-01

    The author presents experimental results of electron and X-ray emission following slow collisions of multiply charged ions and atoms. The aim of the investigation was to study the mechanisms which are responsible for the emission. (G.T.H.)

  9. The influence of atomic alignment on absorption and emission spectroscopy

    Science.gov (United States)

    Zhang, Heshou; Yan, Huirong; Richter, Philipp

    2018-06-01

    Spectroscopic observations play essential roles in astrophysics. They are crucial for determining physical parameters in the universe, providing information about the chemistry of various astronomical environments. The proper execution of the spectroscopic analysis requires accounting for all the physical effects that are compatible to the signal-to-noise ratio. We find in this paper the influence on spectroscopy from the atomic/ground state alignment owing to anisotropic radiation and modulated by interstellar magnetic field, has significant impact on the study of interstellar gas. In different observational scenarios, we comprehensively demonstrate how atomic alignment influences the spectral analysis and provide the expressions for correcting the effect. The variations are even more pronounced for multiplets and line ratios. We show the variation of the deduced physical parameters caused by the atomic alignment effect, including alpha-to-iron ratio ([X/Fe]) and ionisation fraction. Synthetic observations are performed to illustrate the visibility of such effect with current facilities. A study of PDRs in ρ Ophiuchi cloud is presented to demonstrate how to account for atomic alignment in practice. Our work has shown that due to its potential impact, atomic alignment has to be included in an accurate spectroscopic analysis of the interstellar gas with current observational capability.

  10. Direct isotope ratio measurement of uranium metal by emission spectrometry on a laser-produced plasma

    International Nuclear Information System (INIS)

    Pietsch, W.; Petit, A.; Briand, A.

    1995-01-01

    The method of Optical Emission Spectrometry on a Laser-Produced Plasma (OES/LPP) at reduced pressure has been studied for the determination of the uranium isotope ratio ( 235 U/ 238 U). Spectral profiles of the investigated transition U-II 424.437 nm show the possibility to obtain an isotopic spectral resolution in a laser-produced plasma under exactly defined experimental conditions. Spectroscopic data and results are presented. (author)

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

    Science.gov (United States)

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

    2018-05-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  13. Steelmaking process control using remote ultraviolet atomic emission spectroscopy

    Science.gov (United States)

    Arnold, Samuel

    Steelmaking in North America is a multi-billion dollar industry that has faced tremendous economic and environmental pressure over the past few decades. Fierce competition has driven steel manufacturers to improve process efficiency through the development of real-time sensors to reduce operating costs. In particular, much attention has been focused on end point detection through furnace off gas analysis. Typically, off-gas analysis is done with extractive sampling and gas analyzers such as Non-dispersive Infrared Sensors (NDIR). Passive emission spectroscopy offers a more attractive approach to end point detection as the equipment can be setup remotely. Using high resolution UV spectroscopy and applying sophisticated emission line detection software, a correlation was observed between metal emissions and the process end point during field trials. This correlation indicates a relationship between the metal emissions and the status of a steelmaking melt which can be used to improve overall process efficiency.

  14. Rainbow Emission from an Atomic Transition in Doped Quantum Dots.

    Science.gov (United States)

    Hazarika, Abhijit; Pandey, Anshu; Sarma, D D

    2014-07-03

    Although semiconductor quantum dots are promising materials for displays and lighting due to their tunable emissions, these materials also suffer from the serious disadvantage of self-absorption of emitted light. The reabsorption of emitted light is a serious loss mechanism in practical situations because most phosphors exhibit subunity quantum yields. Manganese-based phosphors that also exhibit high stability and quantum efficiency do not suffer from this problem but in turn lack emission tunability, seriously affecting their practical utility. Here, we present a class of manganese-doped quantum dot materials, where strain is used to tune the wavelength of the dopant emission, extending the otherwise limited emission tunability over the yellow-orange range for manganese ions to almost the entire visible spectrum covering all colors from blue to red. These new materials thus combine the advantages of both quantum dots and conventional doped phosphors, thereby opening new possibilities for a wide range of applications in the future.

  15. Frequency lock of a dye laser emission on iron atomic line top

    International Nuclear Information System (INIS)

    Durand, P.

    1995-03-01

    The aim of this thesis is to realize a frequency lock of a dye laser emission on iron atomic line top. To reach that goal, the author first presents the calculation of atomic vapour density by means of laser absorption ratio measure and studies the dye laser working. It is then necessary to find a device giving the required precision on the frequency of the absorption line choosen. It is obtained thanks to the atomic line reconstitution by optogalvanic effect which gives the reference. Besides, the author presents the necessity of a laser emission power regulation which is obtained thanks to a device including an acoustic and optic modulator. A reliable and accurate captor is choosen and adjusted testing various hollow cathode lamps. The method to obtain the frequency lock of laser emission on iron atomic line top is described. (TEC). 18 refs., 64 figs

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

    Czech Academy of Sciences Publication Activity Database

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

    2002-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-12-05

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

  18. Emission Channeling Studies of the Lattice Site of Oversized Alkali Atoms Implanted in Metals

    CERN Multimedia

    2002-01-01

    % IS340 \\\\ \\\\ As alkali atoms have the largest atomic radius of all elements, the determination of their lattice configuration following implantation into metals forms a critical test for the various models predicting the lattice site of implanted impurity atoms. The site determination of these large atoms will especially be a crucial check for the most recent model that relates the substitutional fraction of oversized elements to their solution enthalpy. Recent exploratory $^{213}$Fr and $^{221}$Fr $\\alpha$-emission channeling experiments at ISOLDE-CERN and hyperfine interaction measurements on Fr implanted in Fe gave an indication for anomalously large substitutional fractions. To investigate further the behaviour of Fr and other alkali atoms like Cs and Rb thoroughly, more on-line emission channeling experiments are needed. We propose a number of shifts for each element, where the temperature of the implanted metals will be varied between 50$^\\circ$ and 700$^\\circ$~K. Temperature dependent measurements wi...

  19. Spontaneous emission spectrum of a four-level atom coupled by three kinds of reservoirs

    International Nuclear Information System (INIS)

    Yang Dong; Wang Jian; Zhang, Hanzhuang; Yao Jinbo

    2007-01-01

    A model of a four-level atom embedded in a double-band photonic crystal (PC) is presented. The atomic transitions from the upper two levels to the lower two levels are coupled by the same reservoir which is assumed in turn to be isotropic PC modes, anisotropic PC modes and free vacuum modes. The effects of the fine structure of the atomic ground state levels and the quantum interference on the spontaneous emission spectrum of an atom are investigated in detail. Most interestingly, it is shown for the first time that new spontaneous emission lines are produced from the fine splitting of atomic ground state levels in the isotropic PC case. Quantum interference induces additional narrow spontaneous lines near the transition from the empty upper level to the lower levels

  20. Efficient high-resolution X-ray emission spectrometry using synchrotron radiation

    International Nuclear Information System (INIS)

    Unterumsberger, Rainer

    2015-01-01

    The aim of the present work is to get access to high-resolution X-Ray Emission Spectrometry (XES) at nanoscaled materials, consisting of light elements and transition metals, by the increase of the sensitivity of a Wavelength-Dispersive Spectrometer (WDS) in the soft X-Ray range. The increase of the sensitivity was achieved by a refocusing of the incident radiation. With the increased sensitivity of the WDS, it was possible to determine the chemical species of different, nominal 100 nm thin titanium oxides. The combination of the refocusing optic and calibrated spectrometer enabled the detection and deconvolution of the L-fluorescence radiation of these nanoscaled titanium oxides. Due to the calibration of the spectrometer, a reliable determination of the transition probabilities of the titanium La- and Ll-fluorescence lines as a function of the chemical state is possible. To the best of my knowledge, the determination of the transition probabilities as a function of the chemical state in the soft X-Ray range has not been investigated yet. The quality of the refocusing was characterized using different diagnostic tools. Vertical full width at half maximum (FWHM) values of the focused beam between 10 μm to 20 μm and horizontal FWHM values between 12 μm and 25 μm could be achieved over an energy range of 180 eV to 1310 eV. Using calibrated photodiodes, it was possible to determine the absolute transmission of the used single bounce monocapillary as well as to monitor the absolute photon flux. By means of the refocusing, it was possible to increase the photon flux by a factor of 4.9 experimentally. The increase of the photon flux enables the analysis of nanoscaled materials with the used spectrometer. This could be shown based on the determination of the lower limit of detection of boron Ka and titanium La. In both cases, the lower limit of detection of 0.4 nm equivalent layer thickness was achieved (about 1.10 -7 g/cm 2 to 2.10 -7 g/cm 2 or 3.10 15 atoms/cm 2 to

  1. On the role of coulomb forces in atomic radiative emission

    International Nuclear Information System (INIS)

    Yngstroem, S.

    1988-10-01

    It is shown how the generalized Coulomb interaction (electric and magnetic fields of force) competes with the radiative interaction causing overall inhibition of the radiative capability of atoms and ions in a gaseous sample of matter. Basic quantum mechanical aspects of the electromagnetic interaction are discussed in a heuristic introduction followed by a more precise treatment in the formalism of relativistic quantum electrodynamics. (author)

  2. Teleporting the one-qubit state via two-level atoms with spontaneous emission

    Energy Technology Data Exchange (ETDEWEB)

    Hu Mingliang, E-mail: mingliang0301@xupt.edu.cn, E-mail: mingliang0301@163.com [School of Science, Xi' an University of Posts and Telecommunications, Xi' an 710061 (China)

    2011-05-14

    We study quantum teleportation via two two-level atoms coupled collectively to a multimode vacuum field and prepared initially in different atomic states. We concentrated on the influence of the spontaneous emission, collective damping and dipole-dipole interaction of the atoms on fidelity dynamics of quantum teleportation and obtained the region of spatial distance between the two atoms over which the state can be teleported nonclassically. Moreover, we showed through concrete examples that entanglement of the channel state is the prerequisite but not the only essential quantity for predicting the teleportation fidelity.

  3. Coherent effects on two-photon correlation and directional emission of two two-level atoms

    International Nuclear Information System (INIS)

    Ooi, C. H. Raymond; Kim, Byung-Gyu; Lee, Hai-Woong

    2007-01-01

    Sub- and superradiant dynamics of spontaneously decaying atoms are manifestations of collective many-body systems. We study the internal dynamics and the radiation properties of two atoms in free space. Interesting results are obtained when the atoms are separated by less than half a wavelength of the atomic transition, where the dipole-dipole interaction gives rise to new coherent effects, such as (a) coherence between two intermediate collective states, (b) oscillations in the two-photon correlation G (2) , (c) emission of two photons by one atom, and (d) the loss of directional correlation. We compare the population dynamics during the two-photon emission process with the dynamics of single-photon emission in the cases of a Λ and a V scheme. We compute the temporal correlation and angular correlation of two successively emitted photons using the G (2) for different values of atomic separation. We find antibunching when the atomic separation is a quarter wavelength λ/4. Oscillations in the temporal correlation provide a useful feature for measuring subwavelength atomic separation. Strong directional correlation between two emitted photons is found for atomic separation larger than a wavelength. We also compare the directionality of a photon spontaneously emitted by the two atoms prepared in phased-symmetric and phased-antisymmetric entangled states vertical bar ±> k 0 =e ik 0 ·r 1 vertical bar a 1 ,b 2 >±e ik 0 ·r 2 vertical bar b 1 ,a 2 > by a laser pulse with wave vector k 0 . Photon emission is directionally suppressed along k 0 for the phased-antisymmetric state. The directionality ceases for interatomic distances less than λ/2

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-06-01

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

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

    Directory of Open Access Journals (Sweden)

    Prkić Ante

    2017-08-01

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

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

    International Nuclear Information System (INIS)

    Naeemullah, A.; Kazi, T.G.

    2011-01-01

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

  7. Determination of mercury in rice by cold vapor atomic fluorescence spectrometry after microwave-assisted digestion

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Maria Jose da [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain); Departamento de Quimica Fundamental, Universidade Federal de Pernambuco, Cidade Universitaria, 50740-550 Recife, PE (Brazil); Paim, Ana Paula S. [Departamento de Quimica Fundamental, Universidade Federal de Pernambuco, Cidade Universitaria, 50740-550 Recife, PE (Brazil); Pimentel, Maria Fernanda [Departamento de Engenharia Quimica, Universidade Federal de Pernambuco, Recife, PE (Brazil); Cervera, M. Luisa, E-mail: m.luisa.cervera@uv.es [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain); Guardia, Miguel de la [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain)

    2010-05-14

    A cold vapor atomic fluorescence spectrometry method (CV-AFS) has been developed for the determination of Hg in rice samples at a few ng g{sup -1} concentration level. The method is based on the previous digestion of samples in a microwave oven with HNO{sub 3} and H{sub 2}O{sub 2} followed by dilution with water containing KBr/KBrO{sub 3} and hydroxylamine and reduction with SnCl{sub 2} in HCl using external calibration. The matrix interferences and the effect of nitrogen oxide vapors have been evaluated and the method validated using a certified reference material. The limit of detection of the method was 0.9 ng g{sup -1} with a recovery percentage of 95 {+-} 4% at an added concentration of 5 ng g{sup -1}. The concentration level of Hg found in 24 natural rice samples from different origin ranged between 1.3 and 7.8 ng g{sup -1}.

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

    International Nuclear Information System (INIS)

    Mashhadian, N.V.

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  11. Determination of iron in natural and mineral waters by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    ROLANDAS KAZLAUSKAS

    2004-05-01

    Full Text Available Simple methods for the determination of Fe in natural and mineral waters by flame atomic absorption spectrometry (AAS are suggested. The results of the investigation of selectivity of the proposed AAS method proved that this procedure is not affected by high concentrations of other metals. The calibration graph for iron was linear at levels near the detection limit up to at least 0.10 mg ml-1. For the determination of microamounts of iron in mineral waters, an extraction AAS technique was developed. Iron was retained as Fe-8-oxyquinoline complex and extracted into chloroform. The optimal conditions for the extraction of the iron complex were determined. The AAS method was applied to the determination of Fe in mineral waters and natural waters from different areas of Lithuania. The accuracy of the developed method was sufficient and evaluated in comparison with a photometric method. The obtained results demonstrated that the procedure could be successfully applied for the analysis of water samples with satisfactory accuracy.

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

    Science.gov (United States)

    Gokce, Kaya; Mehmet, Yaman

    2012-01-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2016-04-15

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

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

    International Nuclear Information System (INIS)

    Yaman, Mehmet; Kaya, Gokce

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-09-14

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

  18. [Novel Hyphenated Techniques of Atomic Spectrometry for Metal Species Interaction with Biomolecules].

    Science.gov (United States)

    Li, Yan; Yan, Xiu-ping

    2015-09-01

    Trace metals may be adopted by biological systems to assist in the syntheses and metabolic functions of genes (DNA and RNA) and proteins in the environment. These metals may be beneficial or may pose a risk to humans and other life forms. Novel hybrid techniques are required for studies on the interaction between different metal species and biomolecules, which is significant for biology, biochemistry, nutrition, agriculture, medicine, pharmacy, and environmental science. In recent years, our group dwells on new hyphenated techniques based on capillary electrophoresis (CE), electrothermal atomic absorption spectrometry (ETAAS), and inductively coupled plasma mass spectroscopy (ICP-MS), and their application for different metal species interaction with biomolecules such as DNA, HSA, and GSH. The CE-ETAAS assay and CE-ICP-MS assay allow sensitively probing the level of biomolecules such as DNA damage by different metal species and extracting the kinetic and thermodynamic information on the interactions of different metal species with biomolecules, provides direct evidences for the formation of different metal species--biomolecule adducts. In addition, the consequent structural information were extracted from circular dichroism (CD) and X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and Fourier transform infrared (FTIR) spectroscopy. The present works represent the most complete and extensive study to date on the interactions between different metal species with biomolecules, and also provide new evidences for and insights into the interactions of different metal species with biomolecules for further understanding of the toxicological effects of metal species.

  19. Line emission processes in atomic and molecular shocks

    International Nuclear Information System (INIS)

    Shull, J.M.

    1988-01-01

    The review discusses the observations and theoretical models of interstellar shock waves in diffuse and molecular clouds. After summarizing the relevant gas dynamics, atomic, molecular and grain processes, and physics of radiative and magnetic precursors, the author describes observational diagnostics of shocks. This paper concludes with a discussion of two topics: unstable or non-steady shocks and thermal conduction in metal-rich shocks

  20. Low-energy neutral atom emission from the Earth's magnetosphere

    International Nuclear Information System (INIS)

    Moore, K.R.; Scime, E.E.; Funsten, H.O.; McComas, D.J.; Thomsen, M.F.

    1994-01-01

    Imaging of the terrestrial magnetosphere is possible through the detection of low-energy neutral atoms (LENAs) produced by charge exchange between magnetospheric plasma ions and neutral atoms of the Earth's geocorona. The authors present calculations of both hydrogen and oxygen line-of-sight LENA fluxes expected on orbit for various plasma regimes as predicted by the Rice University Magnetospheric Specification Model. To decrease the required computation time, they are in the process of adapting their code for massively parallel computers. The speed gains achieved from parallel algorithms are substantial, and they present results from computational runs on the Connection Machine CM-2 data parallel supercomputer. They also estimate expected image count rates and image quality based on realistic instrument geometric factors, energy passbands, neutral atom scattering in the instrument, and image accumulation intervals. The results indicate that LENA imaging instruments will need a geometric factor (G) on the order of 0.1 cm 2 sr eV/eV to be capable of imaging storm time ring currents, and a G of 1.0 cm 2 sr eV/eV in order to image the quiet time ring current fluxes, ion injections from the tail, and subsequent ion drifts toward the dayside magnetopause

  1. Two-photon emission and multiphoton absorption by atoms

    International Nuclear Information System (INIS)

    Mu, X.

    1988-01-01

    This thesis consists of investigations of two problems concerning photon-atom interactions. The first topic deals with two-photon transitions in atomic inner shells. An independent-particle model has been used to describe the two-photon transitions between different inner-shell electron states. The first relativistic self-consistent-field calculation of these transition rates in Ag, Mo, and Xe has been carried out. The theoretical results are compared with recent measurements. Good agreement with measured rates is found except in some cases where more reliable experiments still need to be done. The second topic is multiphoton multiionization of atoms. The maximum entropy principle has been employed in this theoretical investigation. A detailed statistical analysis of measured ionic charge distributions produced in strong laser pulses has been carried out. The results of this analysis indicates that the charge-state distribution is a Poissonian, rather than the binomial which prevails under infrared radiation, and hence that ionization occurs stepwise during the pulse. This result is shown to be consistent with experimental data

  2. Electron emission in collisions of intermediate energy ions with atoms

    International Nuclear Information System (INIS)

    Garibotti, C.R.

    1988-01-01

    The aim of this work, is the analysis of the processes of electronic emission produced in the collisions of small ions (H + , He ++ ) of intermediate energy (50 a 200 KeV/amu) with light gaseous targets. (A.C.A.G.) [pt

  3. Time evolution, Lamb shift, and emission spectra of spontaneous emission of two identical atoms

    International Nuclear Information System (INIS)

    Wang Dawei; Li Zhenghong; Zheng Hang; Zhu Shiyao

    2010-01-01

    A unitary transformation method is used to investigate the dynamic evolution of two multilevel atoms, in the basis of symmetric and antisymmetric states, with one atom being initially prepared in the first excited state and the other in the ground state. The unitary transformation guarantees that our calculations are based on the ground state of the atom-field system and the self-energy is subtracted at the beginning. The total Lamb shifts of the symmetric and antisymmetric states are divided into transformed shift and dynamic shift. The transformed shift is due to emitting and reabsorbing of virtual photons, by a single atom (nondynamic single atomic shift) and between the two atoms (quasi-static shift). The dynamic shift is due to the emitting and reabsorbing of real photons, by a single atom (dynamic single atomic shift) and between the two atoms (dynamic interatomic shift). The emitting and reabsorbing of virtual and real photons between the two atoms result in the interatomic shift, which does not exist for the one-atom case. The spectra at the long-time limit are calculated. If the distance between the two atoms is shorter than or comparable to the wavelength, the strong coupling between the two atoms splits the spectrum into two peaks, one from the symmetric state and the other from the antisymmetric state. The origin of the red or blue shifts for the symmetric and antisymmetric states mainly lies in the negative or positive interaction energy between the two atoms. In the investigation of the short time evolution, we find the modification of the effective density of states by the interaction between two atoms can modulate the quantum Zeno and quantum anti-Zeno effects in the decays of the symmetric and antisymmetric states.

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

    OpenAIRE

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

    2005-01-01

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

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

    International Nuclear Information System (INIS)

    Alduan, F. A.; Capdevilla, C.

    1980-01-01

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

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

    International Nuclear Information System (INIS)

    Fernandes, E.A.N.

    1981-01-01

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

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

    International Nuclear Information System (INIS)

    Sardans, Jordi; Montes, Fernando; Penuelas, Josep

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Sardans, Jordi, E-mail: j.sardans@creaf.uab.ca [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain); Montes, Fernando [Departamento de Ciencias Analiticas, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia (UNED), C/ Senda del Rey 9. 28040 Madrid (Spain); Penuelas, Josep [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain)

    2010-02-15

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

  9. Photon emission spectroscopy of ion-atom collisions

    International Nuclear Information System (INIS)

    Nystroem, B.

    1995-10-01

    Emission cross sections for the 1snp 1 P 1 -levels have been measured by photon emission spectroscopy for the collision systems He + + He at 10 keV and He 2+ + He at 10-35 keV. Photon spectra of Krypton (Kr VIII) and Xenon (Xe V - IX) have also been obtained using 10q keV beams of Kr q+ (q=7-9) and Xe q+ (q=5-9) colliding with Helium and Argon. The Lifetimes of 3p 2 P-levels in Na-like Nb are reported together with lifetime for the 3s3p 3 P 1 -level in Mg-like Ni, Kr, Y, Zr and Nb where this level has an intercombination transition to the ground state. 45 refs, 20 figs

  10. Photon emission spectroscopy of ion-atom collisions

    Energy Technology Data Exchange (ETDEWEB)

    Nystroem, B

    1995-10-01

    Emission cross sections for the 1snp{sup 1}P{sub 1}-levels have been measured by photon emission spectroscopy for the collision systems He{sup +} + He at 10 keV and He{sup 2+} + He at 10-35 keV. Photon spectra of Krypton (Kr VIII) and Xenon (Xe V - IX) have also been obtained using 10q keV beams of Kr{sup q+} (q=7-9) and Xe{sup q+} (q=5-9) colliding with Helium and Argon. The Lifetimes of 3p{sup 2}P-levels in Na-like Nb are reported together with lifetime for the 3s3p{sup 3}P{sub 1}-level in Mg-like Ni, Kr, Y, Zr and Nb where this level has an intercombination transition to the ground state. 45 refs, 20 figs.

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  12. Direct determination of arsenic in petroleum derivatives by graphite furnace atomic absorption spectrometry: A comparison between filter and platform atomizers

    OpenAIRE

    Becker, Emilene M.; Rampazzo, Roger T.; Dessuy, Morgana B.; Vale, Maria Goreti R.; Silva, Márcia M. da; Welz, Bernhard; Katskov, Dmitri A.

    2011-01-01

    Acesso restrito: Texto completo. In the present work a direct method for the determination of arsenic in petroleum derivatives has been developed, comparing the performance of a commercial transversely heated platform atomizer (THPA) with that of a transversely heated filter atomizer (THFA). The THFA results in a reduction of background absorption and an improved sensitivity as has been reported earlier for this atomizer. The mixture of 0.1% (m/v) Pd+0.03% (m/v) Mg+0.05% (v/v) Triton X-...

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

    Science.gov (United States)

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

    2017-06-01

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

  14. Speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-02-23

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

  15. Speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Li Xun; Jia Jing; Wang Zhenghao

    2006-01-01

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

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

  17. Atomic carbon emission from photodissociation of CO2. [planetary atmospheric chemistry

    Science.gov (United States)

    Wu, C. Y. R.; Phillips, E.; Lee, L. C.; Judge, D. L.

    1978-01-01

    Atomic carbon fluorescence, C I 1561, 1657, and 1931 A, has been observed from photodissociation of CO2, and the production cross sections have been measured. A line emission source provided the primary photons at wavelengths from threshold to 420 A. The present results suggest that the excited carbon atoms are produced by total dissociation of CO2 into three atoms. The cross sections for producing the O I 1304-A fluorescence through photodissociation of CO2 are found to be less than 0.01 Mb in the wavelength region from 420 to 835 A. The present data have implications with respect to photochemical processes in the atmospheres of Mars and Venus.

  18. Emission and electron transitions in an atom interacting with an ultrashort electromagnetic pulse

    International Nuclear Information System (INIS)

    Matveev, V.I.

    2003-01-01

    Electron transitions and emission of an atom interacting with a spatially inhomogeneous ultrashort electromagnetic pulse are considered. The excitation and ionization probabilities are obtained as well as the spectra and cross sections of the reemission of such a pulse by atoms. By way of an example, one- and two-electron inelastic processes accompanying the interaction of ultrashort pulses with hydrogen- and helium-like atoms are considered. The developed technique makes it possible to take into account exactly the spatial nonuniformity of the ultrashort pulse field and photon momenta in the course of reemission

  19. Measurement of Apparent Temperature in Post-Detonation Fireballs Using Atomic Emission Spectroscopy

    Science.gov (United States)

    2011-02-01

    thermometric species into burners.3,12 Interestingly, Wilkin- son et al.6 have recently observed Al atomic emission lines in the spectrum of aluminum...candidate thermometric species must produce several strong emission lines in the spectrum that originate from different upper energy levels in order to...allow the populations of the associated states to be determined. Barium nitrate was chosen as a thermometric impurity for the current work since Ba

  20. Automated installation for atomic emission determination of gold, silver and platinum group metals

    International Nuclear Information System (INIS)

    Zayakina, S.B.; Anoshin, G.N.; Gerasimov, P.A.; Smirnov, A.V.

    1999-01-01

    An automated installation for the direct atomic emission determination of silver, gold and platinum-group metals (Ru) in geological and geochemical materials with software for automated data acquisition and handling is designed and developed. The installation consists of a DFS-458 diffraction spectrograph, a MAES-10 multichannel analyzer of emission spectra, and a dual-jet plasmatron. A library of spectral lines of almost all elements excited in the dual-jet plasmatron is complied [ru

  1. Chemical Analysis of Impurity Boron Atoms in Diamond Using Soft X-ray Emission Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Muramatsu, Yasuji; Iihara, Junji; Takebe, Toshihiko; Denlinger, Jonathan D.

    2008-03-29

    To analyze the local structure and/or chemical states of boron atoms in boron-doped diamond, which can be synthesized by the microwave plasma-assisted chemical vapor deposition method (CVD-B-diamond) and the temperature gradient method at high pressure and high temperature (HPT-B-diamond), we measured the soft X-ray emission spectra in the CK and BK regions of B-diamonds using synchrotron radiation at the Advanced Light Source (ALS). X-ray spectral analyses using the fingerprint method and molecular orbital calculations confirm that boron atoms in CVD-B-diamond substitute for carbon atoms in the diamond lattice to form covalent B-C bonds, while boron atoms in HPT-B-diamond react with the impurity nitrogen atoms to form hexagonal boron nitride. This suggests that the high purity diamond without nitrogen impurities is necessary to synthesize p-type B-diamond semiconductors.

  2. Chemically assisted release of transition metals in graphite vaporizers for atomic spectrometry

    International Nuclear Information System (INIS)

    Katskov, Dmitri; Darangwa, Nicholas; Grotti, Marco

    2006-01-01

    The processes associated with the vaporization of microgram samples and modifiers in a graphite tube ET AAS were investigated by the example of transition metals. The vapor absorption spectra and vaporization behavior of μg-amounts Cd, Zn, Cu, Ag, Au, Ni, Co, Fe, Mn and Cr were studied using the UV spectrometer with CCD detector, coupled with a continuum radiation source. The pyrocoated, Ta or W lined tubes, with Ar or He as internal gases, and filter furnace were employed in the comparative experiments. It was found that the kinetics of atomic vapor release changed depending on the specific metal-substrate-gas combination; fast vaporization at the beginning was followed by slower 'tailing.' The absorption continuum, overlapped by black body radiation at longer wavelengths, accompanied the fast vaporization mode for all metals, except Cd and Zn. The highest intensity of the continuum was observed in the pyrocoated tube with Ar. For Cu and Ag the molecular bands overlapped the absorption continuum; the continuum and bands were suppressed in the filter furnace. It is concluded that the exothermal interaction of sample vapor with the material of the tube causes the energy evolution in the gas phase. The emitted heat is dispersed near the tube wall in the protective gas and partially transferred back to the surface of the sample, thus facilitating the vaporization. The increased vapor flow causes over-saturation and gas-phase condensation in the absorption volume at some distance from the wall, where the gas temperature is not affected by the reaction. The condensation is accompanied by the release of phase transition energy via black body radiation and atomic emission. The particles of condensate and molecular clusters cause the scattering of light and molecular absorption; slow decomposition of the products of the sample vapor-substrate reaction produces the 'tailing' of atomic absorption signal. The interaction of graphite with metal vapor or oxygen, formed in the

  3. X-ray fluorescence analysis and optical emission spectrometry of an roman mirror from Tomis, Romania

    International Nuclear Information System (INIS)

    Belc, M.; Bogoi, M.; Ionescu, D.; Guita, D.; Caiteanu, S.; Caiteanu, D.

    2000-01-01

    The miscellaneous population of Roman Empire, their diverse cultural tradition, their ability to assimilate the roman civilization spirits, had determined a permanent reassessment superimposed upon the roman contribution. Analysis was undertaken using optical emission spectrometry and non-destructive X-ray fluorescence. X-ray fluorescence analysis is a well-established method and is often used in archaeometry and other work dealing with valuable objects pertaining to the history of art and civilization. Roman mirror analysed has been found not to be made of speculum (a high tin bronze). (authors)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-12-15

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

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

    Science.gov (United States)

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

    2010-12-15

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

  6. Atomic nuclei decay modes by spontaneous emission of heavy ions

    International Nuclear Information System (INIS)

    Poenaru, D.N.; Ivascu, M.; Sandulescu, A.

    1984-01-01

    The great majority of the known nuclei, including the so-called stable nuclides, are in fact metastable with respect to several modes of spontaneous superasymmetric splitting. If the lifetime against these processes is larger than 10 30 s, the phenomenon is not detectable with available experimental techniques, hence one can admit stability from the practical point of view. A model extended from the fission theory of alpha decay allows one to estimate the lifetimes and the branching ratios relatively to the alpha decay for these natural radioactivities. From a huge amount of systematical calculations it is concluded that the process should proceed with maximum intensity in the trans-lead nuclei, where the minimum lifetime is obtained for parent nuclei - heavy clusters leading to a magic ( 208 Pb) or almost daughter nucleus. More than 140 nuclides with atomic number smaller than 25 are possible candidates to be emitted from heavy nuclei, with half-life n the 10 10 -10 30 s range. The shell structure and pairing effects are clearly manifested in these new decay modes

  7. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part I. Theoretical considerations

    International Nuclear Information System (INIS)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-01-01

    Highlights: • Tutorial review addressed to beginners or more experienced analysts. • Theoretical background of effects caused by organic matrices on ICP techniques. • Spatial distribution of carbon species and analytes in plasma. • Carbon spectroscopic and non-spectroscopic interferences in ICP. - Abstract: Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical “matrix removal” approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the

  8. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part I. Theoretical considerations.

    Science.gov (United States)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-07-23

    Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical "matrix removal" approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the plasma with respect to analytes repartition; (iii) the subsequent modifications of plasma fundamental properties; and (iv) the resulting spectroscopic and non spectroscopic interferences. This first part of this tutorial review is addressed either to beginners or to more experienced scientists who are interested in the

  9. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part I. Theoretical considerations

    Energy Technology Data Exchange (ETDEWEB)

    Leclercq, Amélie, E-mail: amelie.leclercq@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Nonell, Anthony, E-mail: anthony.nonell@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Todolí Torró, José Luis, E-mail: jose.todoli@ua.es [Universidad de Alicante, Departamento de Quimica Analitica, Nutricion y Bromatología, Ap. de Correos, 99, 03080 Alicante (Spain); Bresson, Carole, E-mail: carole.bresson@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vio, Laurent, E-mail: laurent.vio@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vercouter, Thomas, E-mail: thomas.vercouter@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Chartier, Frédéric, E-mail: frederic.chartier@cea.fr [CEA Saclay, DEN, DANS, DPC, 91191 Gif-sur-Yvette (France)

    2015-07-23

    Highlights: • Tutorial review addressed to beginners or more experienced analysts. • Theoretical background of effects caused by organic matrices on ICP techniques. • Spatial distribution of carbon species and analytes in plasma. • Carbon spectroscopic and non-spectroscopic interferences in ICP. - Abstract: Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical “matrix removal” approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the

  10. Simple, sensitive nitrogen analyzer based on pulsed miniplasma source emission spectrometry

    International Nuclear Information System (INIS)

    Jin Zhe; Duan Yixiang

    2003-01-01

    The development of pulsed miniplasma source emission spectrometry for trace nitrogen determination in inert gases is described in this article. The instrument consists of a pulsed miniplasma source generated by an in-house fabricated portable high-voltage supply, an optical beam collection system, an integrated small spectrometer with a charge-coupled-device detector, an interface card, and a notebook computer for controlling spectrometer parameters and signal processing. Trace nitrogen in the inert gases, such as helium and argon, was determined by monitoring the emission intensities from nitrogen molecules at 357 and 337 nm. The analytical performance was examined under various experimental conditions. The system has a detection limit of about 15 ppb (v/v) for nitrogen in helium with a relative standard deviation of 1.5%. The newly developed instrument offers a simple, low-cost, and sensitive method for continuously monitoring trace nitrogen in high-purity inert gases

  11. Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry

    Science.gov (United States)

    Todorov, Todor I.; Wolf, Ruth E.; Adams, Monique

    2014-01-01

    Typically, 27 major, minor, and trace elements are determined in natural waters, acid mine drainage, extraction fluids, and leachates of geological and environmental samples by inductively coupled plasma-optical emission spectrometry (ICP-OES). At the discretion of the analyst, additional elements may be determined after suitable method modifications and performance data are established. Samples are preserved in 1–2 percent nitric acid (HNO3) at sample collection or as soon as possible after collection. The aqueous samples are aspirated into the ICP-OES discharge, where the elemental emission signals are measured simultaneously for 27 elements. Calibration is performed with a series of matrix-matched, multi-element solution standards.

  12. Alpha-particle emission probabilities of ²³⁶U obtained by alpha spectrometry.

    Science.gov (United States)

    Marouli, M; Pommé, S; Jobbágy, V; Van Ammel, R; Paepen, J; Stroh, H; Benedik, L

    2014-05-01

    High-resolution alpha-particle spectrometry was performed with an ion-implanted silicon detector in vacuum on a homogeneously electrodeposited (236)U source. The source was measured at different solid angles subtended by the detector, varying between 0.8% and 2.4% of 4π sr, to assess the influence of coincidental detection of alpha-particles and conversion electrons on the measured alpha-particle emission probabilities. Additional measurements were performed using a bending magnet to eliminate conversion electrons, the results of which coincide with normal measurements extrapolated to an infinitely small solid angle. The measured alpha emission probabilities for the three main peaks - 74.20 (5)%, 25.68 (5)% and 0.123 (5)%, respectively - are consistent with literature data, but their precision has been improved by at least one order of magnitude in this work. © 2013 Published by Elsevier Ltd.

  13. Double differential distributions of electron emission in ion-atom and electron-atom collisions using an electron spectrometer

    International Nuclear Information System (INIS)

    Misra, Deepankar; Thulasiram, K.V.; Fernandes, W.; Kelkar, Aditya H.; Kadhane, U.; Kumar, Ajay; Singh, Yeshpal; Gulyas, L.; Tribedi, Lokesh C.

    2009-01-01

    We study electron emission from atoms and molecules in collisions with fast electrons and heavy ions (C 6+ ). The soft collision electrons (SE), two center electron emission (TCEE), the binary encounter (BE) events and the KLL Auger lines along with the elastically scattered peaks (in electron collisions) are studied using a hemispherical electrostatic electron analyzer. The details of the measurements along with description of the spectrometer and data acquisition system are given. The angular distributions of the low energy (few eV) electrons in soft collisions and the binary encounter electrons at keV energies are compared with quantum mechanical models based on the first Born (B1) and the continuum distorted wave-Eikonal initial state approximation (CDW-EIS).

  14. Fourier transform infrared emission spectra of atomic rubidium: g- and h-states

    Czech Academy of Sciences Publication Activity Database

    Civiš, Svatopluk; Ferus, Martin; Kubelík, Petr; Chernov, Vladislav E.; Zanozina, Ekaterina M.

    2012-01-01

    Roč. 45, č. 17 (2012), s. 175002 ISSN 0953-4075 R&D Projects: GA AV ČR IAAX00100903 Institutional support: RVO:61388955 Keywords : Fourier transform infrared emission spectra * atomic rubidium * physical chemistry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.031, year: 2012

  15. Determination of rare earth elements in aluminum by inductively coupled plasma-atomic emission spectroscopy

    International Nuclear Information System (INIS)

    Mahanti, H.S.; Barnes, R.M.

    1983-01-01

    Inductively coupled plasma-atomic emission spectroscopy is evaluated for the determination of 14 rare earth elements in aluminum. Spectral line interference, limit of detection, and background equivalent concentration values are evaluated, and quantitative recovery is obtained from aluminum samples spiked with rare earth elements. The procedure is simple and suitable for routine process control analysis. 20 references, 5 tables

  16. Exact results for emission from one and two atoms in an ideal cavity at multiphoton resonance

    International Nuclear Information System (INIS)

    Fam Le Kien; Shumovskij, A.S.; Tran Quang.

    1987-01-01

    The emission from the system of one or two two-level atoms in an ideal cavity with one mode at mutiphoton resonance is examined. Exact results for the two-time dipole correlation function and the time-dependent spectra of multiphoton-induced fluorescence are presented

  17. Atomic emission lines in the near ultraviolet; hydrogen through krypton, section 2

    Science.gov (United States)

    Kelly, R. L.

    1979-01-01

    A compilation of spectra from the first 36 elements was prepared from published literature available through October 1977. In most cases, only those lines which were actually observed in emission or absorption are listed. The wavelengths included range from 2000 Angstroms to 3200 Angstroms with some additional lines up to 3500 Angstroms. Only lines of stripped atoms are reported; no molecular bands are included.

  18. Atomic emission lines in the near ultraviolet; hydrogen through krypton, section 1

    Science.gov (United States)

    Kelly, R. L.

    1979-01-01

    A compilation of spectra from the first 36 elements was prepared from published literature available through October 1977. In most cases, only those lines which were actually observed in emission or absorption are listed. The wavelengths included range from 2000 Angstroms to 3200 Angstroms with some additional lines up to 3500 Angstroms. Only lines of stripped atoms are reported; no molecular bands are included.

  19. Atomic emission spectroscopy for the on-line monitoring of incineration processes

    NARCIS (Netherlands)

    Timmermans, E.A.H.; de Groote, F.P.J.; Jonkers, J.; Gamero, A.; Sola, A.; Mullen, van der J.J.A.M.

    2003-01-01

    A diagnostic measurement system based on atomic emission spectroscopy has been developed for the purpose of on-line monitoring of hazardous elements in industrial combustion gases. The aim was to construct a setup with a high durability for rough and variable experimental conditions, e.g. a strongly

  20. In situ calibration of inductively coupled plasma-atomic emission and mass spectroscopy

    Science.gov (United States)

    Braymen, Steven D.

    1996-06-11

    A method and apparatus for in situ addition calibration of an inductively coupled plasma atomic emission spectrometer or mass spectrometer using a precision gas metering valve to introduce a volatile calibration gas of an element of interest directly into an aerosol particle stream. The present situ calibration technique is suitable for various remote, on-site sampling systems such as laser ablation or nebulization.

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

    Science.gov (United States)

    Nerdy

    2018-01-01

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

  2. Study on the application of electrothermal atomization atomic absorption spectrometry for the determination of metallic Cu, Pb, Zn, Cd traces in sea water samples

    International Nuclear Information System (INIS)

    Nguyen Thi Kim Dung; Doan Thanh Son; Tran Thi Ngoc Diep

    2004-01-01

    The trace amount of some heavy metallic elements (Cu, Zn, Pb, Cd) in sea water samples were determined directly (without separation) and quantitatively by using Electro-Thermal Atomization Atomic Absorption Spectrometry (ETA-AAS). The effect of mainly major constituents such as Na, Mg, Ca, K, and the mutual effect of the trace elements, which were present in the matrix on the absorption intensity of each analyzed element was studied. The adding of a certain chemical modification for each trace element was also investigated in order to eliminate the overall effect of the background during the pyrolysis and atomization. The sea water sample after fitrating through a membrane with 0.45 μm-hole size was injected in to the graphite tube via an autosampler (MPE50). The absorption intensity of each element was then measured on the VARIO-6 under the optimum parameters for spectrometer such as: maximum wavelength, current of hollow cathode lamp, and that for graphite furnace such as dry temperature, pyrolysis temperature, atomization temperature, ect. The analytical procedures were set-up and applied for the determination of these above mentioned elements in the synthesized sea water sample and in the real sea water samples with high precision and accuracy. (author)

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

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Dědina, Jiří

    2015-01-01

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

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

    Science.gov (United States)

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

    2004-12-01

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

  5. Determination of concentration of heavy metals (Pb, Cd, Fe) in animal tissues using atomic absorption spectrometry

    International Nuclear Information System (INIS)

    RAZAFINTSALAMA, V.T.

    2009-01-01

    Heavy metals are classified among the inorganic compounds. The latter type of metal is found in rocks, fertilizers, urban mud but may also originate from the atmospheric pollution. A particular characteristic of heavy metals is their bioaccumulation in the food chain. Therefore, lead and cadmium, which are classified as heavy metals may be easily found in animal products and can lead to food poisoning if their concentrations are higher than the maximum permissible values as requested by international agencies such as the c odex alimentarius . The values are set down and differ according to types of food for human consuption and the trading companies take action accordingly. Therefore, it is necessary to set up a quality control system through analytical laboratory measurements and testings. This study underlies the method of determination of lead, cadmium and iron in animal tissues by atomic absorption spectrometry. The results showed that the method is sensitive and reliable. For each analyte, the Z-score lies between -2 and 2, indicating that the method is working properly. The analytical results showed that: (i) only beef and chicken meats and beef liver contain lead [0,09μg.g - 1; 0,29μg.g - 1]. The limit value of 0,1μg.g - 1 is almost reached in beef and chicken meats, (ii) as far as cadmium is concerned, the five studied samples contain this analyte [0,02μg.g - 1; 0,9μg.g - 1]. Except the chicken liver of which the concentration (0,15μg.g - 1) exceeds the maximum permissible value (0,1μg.g - 1), the others are in conformity with the standards and appropriate to be consumed,(iii) iron is higher in the liver and kidney samples: beef liver 282mg.g - 1, chicken liver 250 mg.g - 1, pork kidney 247mg.g - 1. The study also showed that the calcium concentration in animal tissues is low and they can be classified as poor-calcium food. [fr

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  7. Speciation analysis of organomercurial compounds in Fish Tissue by capillary gas chromatography coupled to microwave-induced plasma atomic emission detection

    Directory of Open Access Journals (Sweden)

    Dorfe Díaz

    Full Text Available This paper describes a novel approach for analysis of mercury speciation in fish using gas chromatography coupled with microwave-induced plasma optical emission spectrometry (GC-MIP-OES in surfatron resonant cavity. Sample treatment was based on quantitative leaching of mercury species from fish tissue with ultrasound-assisted acid-toluene extraction. The extracted mercury species analyzed with GC-MIP-OES attained detection limits of 5 and 9 pg for methylmercury (MeHg and ethylmercury (EtHg, respectively. A complete chromatogram could be completed in 1.5 min. MeHg values obtained with GC-MIP-OES were matched with organic mercury values obtained with selective reduction cold vapour- atomic absorption spectrometry (CV-AAS.

  8. Atom probe field ion microscopy and related topics: A bibliography 1991

    International Nuclear Information System (INIS)

    Russell, K.F.; Miller, M.K.

    1993-01-01

    This report contains a bibliography for 1991 on the following topics: Atom probe field ion microscopy; field desorption mass spectrometry; field emission; field ion microscopy; and field emission theory

  9. Cold excitation and determination of hydrogen sulfide by dielectric barrier discharge molecular emission spectrometry.

    Science.gov (United States)

    Wu, Zhongchen; Jiang, Jie; Li, Na

    2015-11-01

    A low-temperature microplasma generated in a dielectric barrier discharge (DBD) was used as a radiation source for the excitation of hydrogen sulfide and its determination by molecular emission spectrometry (MES). The excitation/emission chamber was enclosed to eliminate spectral interference from ambient air. The spectral emission lines of hydrogen sulfide were clearly discriminated from the background spectrum, and the emission line at 365.06 nm was selected for parameter optimization and quantitative analysis. The S(2-) ions in aqueous samples were reacted with acid to generate hydrogen sulfide and then determined. The experimental parameters affecting the determination of hydrogen sulfide and S(2-) were optimized. The limits of detection were 1.4 mg m(-3) for H2S and 11.2 mg L(-1) for S(2-). The repeatability of the method was satisfactory, as the RSD values were 2.3% for H2S and 1.8% for S(2-). The enclosed DBD-MES system was demonstrated to be a useful tool for the determination of hydrogen sulfide in gas samples and S(2-) in aqueous samples. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2015-10-01

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

  11. On the deviation from the sech2 superradiant emission law in a two-level atomic system

    International Nuclear Information System (INIS)

    Goncalves, A.E.

    1990-01-01

    The atomic superradiant emission is treated in the single particle mean field approximation. A single particle Hamiltonian, which represents a dressed two-level atom in a radiation field, can be obtained and it is verified that it describes the transient regime of the emission process. While the line shape emission for a bare atom follows the sech 2 law, for the dressed atom the line shape deviates appreciably from this law and it is verified that the deviation depends crucially on the ratio of the dynamic frequency shift to the transition frequency. This kind of deviation is observed in experimental results. (Author) [pt

  12. Inductively coupled plasma-atomic emission spectroscopy glovebox assembly system at the West Valley Demonstration Project

    International Nuclear Information System (INIS)

    Marlow, J.H.; McCarthy, K.M.; Tamul, N.R.

    1999-01-01

    The inductively coupled plasma/atomic emission spectroscopy [ICP/AES (ICP)] system for elemental analyses in support of vitrification processing was first installed in 1986. The initial instrument was a Jobin Yvon (JY) Model JY-70 ICP that consisted of sequential and simultaneous spectrometers for analysis of nonradioactive samples as radioactive surrogates. The JY-70 ICP continued supporting nonradioactive testing during the Functional and Checkout Testing of Systems (FACTS) using the full-scale melter with ''cold'' (nonradioactive) testing campaigns. As a result, the need for another system was identified to allow for the analysis of radioactive samples. The Mass Spec (Spectrometry) Lab was established for the installation of the modified ICP system for handling radioactive samples. The conceptual setup of another ICP was predicated on the use of a hood to allow ease of accessibility of the torch, nebulizer, and spray chamber, and the minimization of air flow paths. However, reconsideration of the radioactive sample dose rate and contamination levels led to the configuration of the glovebox system with a common transfer interface box for the ICP and the inductively coupled plasma-mass spectrometer (ICP-MS) glovebox assemblies. As a result, a simultaneous Model JY-50P ICP with glovebox was installed in 1990 as a first generation ICP glovebox system. This was one of the first ICP glovebox assemblies connected with an ICP-MS glovebox system. Since the economics of processing high-level radioactive waste (HLW) required the availability of an instrument to operate 24 hours a day throughout the year without any downtime, a second generation ICP glovebox assembly was designed, manufactured, and installed in 1995 using a Model JY-46P ICP. These two ICP glovebox systems continue to support vitrification of the HLW into canisters for storage. The ICP systems have been instrumental in monitoring vitrification batch processing. To date, remote sample preparation and

  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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-01

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

  14. Arsenic speciation in edible alga samples by microwave-assisted extraction and high performance liquid chromatography coupled to atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Salgado, S. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Quijano, M.A., E-mail: marian.quijano@upm.es [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Bonilla, M.M. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain)

    2012-02-10

    Highlights: Black-Right-Pointing-Pointer Total As and As species were analyzed in edible marine algae. Black-Right-Pointing-Pointer A microwave-assisted extraction method with deionized water was applied. Black-Right-Pointing-Pointer As compounds identified comprised DMA, As(V) and four arsenosugars Black-Right-Pointing-Pointer Considerably high As(V) concentrations were found in the most of the algae studied. - Abstract: Twelve commercially available edible marine algae from France, Japan and Spain and the certified reference material (CRM) NIES No. 9 Sargassum fulvellum were analyzed for total arsenic and arsenic species. Total arsenic concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) after microwave digestion and ranged from 23 to 126 {mu}g g{sup -1}. Arsenic species in alga samples were extracted with deionized water by microwave-assisted extraction and showed extraction efficiencies from 49 to 98%, in terms of total arsenic. The presence of eleven arsenic species was studied by high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation atomic-fluorescence spectrometry (HPLC-(UV)-HG-AFS) developed methods, using both anion and cation exchange chromatography. Glycerol and phosphate sugars were found in all alga samples analyzed, at concentrations between 0.11 and 22 {mu}g g{sup -1}, whereas sulfonate and sulfate sugars were only detected in three of them (0.6-7.2 {mu}g g{sup -1}). Regarding arsenic toxic species, low concentration levels of dimethylarsinic acid (DMA) (<0.9 {mu}g g{sup -1}) and generally high arsenate (As(V)) concentrations (up to 77 {mu}g g{sup -1}) were found in most of the algae studied. The results obtained are of interest to highlight the need to perform speciation analysis and to introduce appropriate legislation to limit toxic arsenic species content in these food products.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  16. Control of spontaneous emission from a microwave-field-driven four-level atom in an anisotropic photonic crystal

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Duo, E-mail: zhangduo10@gmail.com [Wuhan National Laboratory for Optoelectronics and School of Physics, Huazhong University of Science and Technology, Wuhan 430074 (China); School of Electrical and Electronic Engineering, Wuhan Polytechnic University, Wuhan 430023 (China); Li, Jiahua, E-mail: huajia_li@163.com [Wuhan National Laboratory for Optoelectronics and School of Physics, Huazhong University of Science and Technology, Wuhan 430074 (China); Ding, Chunling; Yang, Xiaoxue [Wuhan National Laboratory for Optoelectronics and School of Physics, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2012-05-21

    The spontaneous emission properties of a microwave-field-driven four-level atom embedded in anisotropic double-band photonic crystals (PCs) are investigated. We discuss the influences of the band-edge positions, Rabi frequency and detuning of the microwave field on the emission spectrum. It is found that several interesting features such as spectral-line enhancement, spectral-line suppression, spectral-line overlap, and multi-peak structures can be observed in the spectra. The proposed scheme can be achieved by use of a microwave-coupled field into hyperfine levels in rubidium atom confined in a photonic crystal. These theoretical investigations may provide more degrees of freedom to manipulate the atomic spontaneous emission. -- Highlights: ► Spontaneous emission properties of an atom embedded in PCs are investigated. ► Spectral-line enhancement, suppression and overlapping are observed. ► The results provide more degrees of freedom to control atomic spontaneous emission.

  17. Control of spontaneous emission from a microwave-field-driven four-level atom in an anisotropic photonic crystal

    International Nuclear Information System (INIS)

    Zhang, Duo; Li, Jiahua; Ding, Chunling; Yang, Xiaoxue

    2012-01-01

    The spontaneous emission properties of a microwave-field-driven four-level atom embedded in anisotropic double-band photonic crystals (PCs) are investigated. We discuss the influences of the band-edge positions, Rabi frequency and detuning of the microwave field on the emission spectrum. It is found that several interesting features such as spectral-line enhancement, spectral-line suppression, spectral-line overlap, and multi-peak structures can be observed in the spectra. The proposed scheme can be achieved by use of a microwave-coupled field into hyperfine levels in rubidium atom confined in a photonic crystal. These theoretical investigations may provide more degrees of freedom to manipulate the atomic spontaneous emission. -- Highlights: ► Spontaneous emission properties of an atom embedded in PCs are investigated. ► Spectral-line enhancement, suppression and overlapping are observed. ► The results provide more degrees of freedom to control atomic spontaneous emission.

  18. Simultaneous determination of Cr, Ni and V in urine by electrothermal atomic absorption spectrometry (ET AAS); Determinacion simultanea de Cr, Ni y V en orina mediante et aas

    Energy Technology Data Exchange (ETDEWEB)

    Alvarez, Maria A.; Hermida, Jeymi [Universidad Central de Venezuela, Caracas (Venezuela, Bolivarian Republic of). Escuela de Quimica. Centro de Quimica Analitica

    2011-07-01

    A procedure for the simultaneous determination of Cr, Ni, and V in urine by electrothermal atomic absorption spectrometry (ET AAS) was optimized by factorial design, and performed at a pyrolysis and atomization temperatures of 1300 and 2500 deg C, respectively, using 15 {mu}g de Mg(NO{sub 3}){sub 2} as chemical modifier. Characteristics mass of 14, 6 and 220 {rho}g and detection limits of the method of 0.07, 0.38 and 0.75 {mu}g L{sup -1} were obtained for Cr, Ni and V respectively. The methodology was validated using a Liphochek Urine Metals Control sample (Bio-Rad) (P=0.05). The methodology was applied to samples of voluntary Venezuelan people, not environmentally exposed to specific emissions, and results ranging from < LOD-1.1 and 1.3-3.3 {mu}g L{sup -1} was observed for Cr and V, respectively, and not detectable levels for Ni. (author)

  19. Direct determination of arsenic in petroleum derivatives by graphite furnace atomic absorption spectrometry: A comparison between filter and platform atomizers

    Energy Technology Data Exchange (ETDEWEB)

    Becker, Emilene; Rampazzo, Roger T.; Dessuy, Morgana B. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq - INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Silva, Marcia M. da [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Welz, Bernhard [Instituto Nacional de Ciencia e Tecnologia do CNPq - INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Katskov, Dmitri A. [Tshwane University of Technology (TUT), Faculty of Science, Chemistry Department, Pretoria 0001 (South Africa)

    2011-05-15

    In the present work a direct method for the determination of arsenic in petroleum derivatives has been developed, comparing the performance of a commercial transversely heated platform atomizer (THPA) with that of a transversely heated filter atomizer (THFA). The THFA results in a reduction of background absorption and an improved sensitivity as has been reported earlier for this atomizer. The mixture of 0.1% (m/v) Pd + 0.03% (m/v) Mg + 0.05% (v/v) Triton X-100 was used as the chemical modifier for both atomizers. The samples (naphtha, gasoline and petroleum condensate) were stabilized in the form of a three-component solution (detergentless microemulsion) with the sample, propan-1-ol and 0.1% (v/v) HNO{sub 3} in a ratio of 3.0:6.4:0.6. The characteristic mass of 13 pg found in the THFA was about a factor of two better than that of 28 pg obtained with the THPA; however, the limits of detection (LOD) and quantification (LOQ) were essentially the same for both atomizers (1.9 and 6.2 {mu}g L{sup -1}, respectively, for THPA, and 1.8 and 5.9 {mu}g L{sup -1}, respectively, for THFA) due to the increased noise observed with the THFA. A possible explanation for that is a partial blockage of the radiation from the hollow cathode lamp by the narrow inner diameter of this tube and the associated loss of radiation energy. Due to the lack of an appropriate certified reference material, recovery tests were carried out with inorganic and organic arsenic standards and the results were between 89% and 111%. The only advantage of the THFA found in this work was a reduction of the total analysis time by about 20% due to the 'hot injection' that could be realized with this furnace. The arsenic concentrations varied from < LOQ to 43.3 {mu}g L{sup -1} in the samples analyzed in this work.

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

    Science.gov (United States)

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

    2015-06-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1995-01-01

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

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

    Science.gov (United States)

    Strong, B; Murray-Smith, R

    1974-12-01

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

  5. Induced absorption and stimulated emission in a driven two-level atom

    International Nuclear Information System (INIS)

    Mavroyannis, C.

    1992-01-01

    We have considered the induced processes that occur in a driven two-level atom, where a laser photon is absorbed and emitted by the ground and by the excited states of the atom, respectively. In the low-intensity limit of the laser field, the induced spectra arising when a laser photon is absorbed by the ground state of the atom consist of two peaks describing induced absorption and stimulated-emission processes, respectively, where the former prevails over the latter. Asymmetry of the spectral lines occurs at off-resonance and its extent depends on the detuning of the laser field. The physical. process where a laser photon is emitted by the excited state is the reverse of that arising from the absorption of a laser photon by the ground state of the atom. The former differs from the latter in that the emission of a laser photon by the excited state occurs in the low frequency regime and that the stimulated-emission process prevails over that of the induced absorption. In this case, amplification of ultrashort pulses is likely to occur without the need of population inversion between the optical transitions. The computed spectra are graphically presented and discussed. (author)

  6. [Applications of atomic emission spectrum from liquid electrode discharge to metal ion detection].

    Science.gov (United States)

    Mao, Xiu-Ling; Wu, Jian; Ying, Yi-Bin

    2010-02-01

    The fast and precise detection of metal ion is an important research project concerning studies in diverse academic fields and different kinds of detecting technologies. In the present paper, the authors review the research on atomic emission spectrum based on liquid electrode discharge and its applications in the detection of metal ion. In the first part of this paper the principles and characteristics of the methods based on electrochemistry and spectroscopy were introduced. The methods of ion-selective electrode (ISE), anodic stripping voltammetry, atomic emission spectrum and atomic absorption spectrum were included in this part and discussed comparatively. Then the principles and characteristics of liquid electrode spectra for metal ion detection were introduced. The mechanism of the plasma production and the characteristics of the plasma spectrum as well as its advantages compared with other methods were discussed. Secondly, the authors divided the discharge system into two types and named them single liquid-electrode discharge and double-liquid electrode respectively, according to the number of the liquid electrode and the configuration of the discharge system, and the development as well as the present research status of each type was illustrated. Then the characteristics and configurations of the discharge systems including ECGD, SCGD, LS-APGD and capillary discharge were discussed in detail as examples of the two types. By taking advantage of the technology of atomic emission spectrum based on liquid electrode discharge, the detecting limit of heavy metals such as copper, mercury and argent as well as active metal ions including sodium, potass and magnesium can achieve microg x L(-1). Finally, the advantages and problems of the liquid-electrode discharge applied in detection of metal ion were discussed. And the applications of the atomic emission spectrum based on liquid electrode discharge were prospected.

  7. Superradiant cascade emissions in an atomic ensemble via four-wave mixing

    Energy Technology Data Exchange (ETDEWEB)

    Jen, H.H., E-mail: sappyjen@gmail.com

    2015-09-15

    We investigate superradiant cascade emissions from an atomic ensemble driven by two-color classical fields. The correlated pair of photons (signal and idler) is generated by adiabatically driving the system with large-detuned light fields via four-wave mixing. The signal photon from the upper transition of the diamond-type atomic levels is followed by the idler one which can be superradiant due to light-induced dipole–dipole interactions. We then calculate the cooperative Lamb shift (CLS) of the idler photon, which is a cumulative effect of interaction energy. We study its dependence on a cylindrical geometry, a conventional setup in cold atom experiments, and estimate the maximum CLS which can be significant and observable. Manipulating the CLS of cascade emissions enables frequency qubits that provide alternative robust elements in quantum network. - Highlights: • Superradiance from a cascade atomic transition. • Correlated photon pair generation via four-wave mixing. • Dynamical light–matter couplings in a phased symmetrical state. • Cooperative Lamb shift in a cylindrical atomic ensemble.

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-11-15

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    1976-01-01

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

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

    Directory of Open Access Journals (Sweden)

    A. A. Asweisi

    2010-01-01

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

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

    International Nuclear Information System (INIS)

    Khalid, N.; Chaudhri, S.A.

    1999-01-01

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

  14. Ultra fast atomic process in X-ray emission by inner-shell ionization

    Energy Technology Data Exchange (ETDEWEB)

    Moribayashi, Kengo; Sasaki, Akira [Japan Atomic Energy Research Inst., Neyagawa, Osaka (Japan). Kansai Research Establishment; Tajima, T

    1998-03-01

    An ultra-fast atomic process together with X-ray emission by inner-shell ionization using high intensity (10{sup 18} W/cm{sup 2}) short pulse (20fs) X-ray is studied. A new class of experiment is proposed and a useful pumping source is suggested. In this method, it is found that the gain value of X-ray laser amounts to larger than 1000(1/cm) with use of the density of 10{sup 22}/cm{sup 3} of carbon atom. Electron impact ionization effect and initial density effect as well as intensity of pumping source effect are also discussed. (author)

  15. Dielectric barrier discharge micro-plasma emission spectrometry for the detection of acetone in exhaled breath.

    Science.gov (United States)

    Yang, Ting; Gao, Dong-Xue; Yu, Yong-Liang; Chen, Ming-Li; Wang, Jian-Hua

    2016-01-01

    Acetone is a predominant volatile organic compound (VOC) in the exhaled breath and a promising biomarker for diabetes and ketoacidosis. A non-thermal micro-plasma generated in a planar dielectric barrier discharge (DBD) is used as a radiation source for the excitation of gaseous acetone followed by its quantification with optical emission spectrometry (OES). Gaseous acetone can be directly sampled, while liquid acetone is evaporated by heated tungsten coil and then introduced into the DBD micro-plasma by a helium carrier flow for performing optical emission and detection at a 519 nm emission line. In the present study, the exhaled breath is collected and transferred into aqueous medium for sampling. With a sampling volume of 7 μL in a micro-drop, a linear range of 40-1600 mg L(-1) is obtained along with a detection limit of 44 ng and a precision of 5.7% RSD. The present system is successfully applied to the determination of breath acetone for both diabetic patients and healthy volunteers. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Fara, M.; Novak, F. [EGU Prague, PLC, Bichovice, Prague (Czechoslovakia)

    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).

  17. The Diagnosis of Plasma Parameters in Surface Alloying Technique by Optical Emission Spectrometry

    International Nuclear Information System (INIS)

    Fu Yabo; Zhang Yuefei; Chen Qiang; Zhang Guangqiu; Gao Yuan; Wang Jianzhong; Kui Xiaoyun

    2006-01-01

    Electron density (Ne) in a glow discharge plasma for the surface alloying technique is diagnosed by optical emission spectrometry (OES). With CH 4 as the feeding gas, Ne is obtained by comparing the Hβ spectrum according to the Stark broadening effect. It is noticed that Ne varies with the working pressures (30 Pa to 70 Pa) and cathode voltages (500 V to 1000 V), respectively. Due to an abnormal glow discharge, Ne is between 1.71x10 15 /cm 3 to 6.64x10 15 /cm 3 and increases rapidly with working gas pressures and cathode voltages. The results show that OES is a useful method to measure the plasma parameters in a surface alloying glow discharge plasma

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Liliane Catone Soares

    2015-08-01

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

  20. Green method for ultrasensitive determination of Hg in natural waters by electrothermal-atomic absorption spectrometry following sono-induced cold vapor generation and 'in-atomizer trapping'

    International Nuclear Information System (INIS)

    Gil, Sandra; Lavilla, Isela; Bendicho, Carlos

    2007-01-01

    Sono-induced cold vapor generation (SI-CVG) has been used for the first time in combination with a graphite furnace atomizer for determination of Hg in natural waters by electrothermal-atomic absorption spectrometry after in situ trapping onto a noble metal-pretreated platform (Pd, Pt or Rh) inserted into a graphite tube. The system allows 'in-atomizer trapping' of Hg without the use of conventional reduction reactions based on sodium borohydride or tin chloride in acid medium for cold vapor generation. The sono-induced reaction is accomplished by applying ultrasound irradiation to the sample solution containing Hg(II) in the presence of an organic compound such as formic acid. As this organic acid is partly degraded upon ultrasound irradiation to yield CO, CO 2 , H 2 and H 2 O, the amount of lab wastes is minimized and a green methodology is achieved. For this purpose, experimental variables influencing the generation/trapping process are fully investigated. The limit of detection for a 10 min trapping time and 10 mL sample volume was 0.03 μg L -1 (Integrated absorbance) and the repeatability expressed as relative standard deviation was about 3%. Carbonates and chlorides at 100 mg L -1 level caused a signal depression by 20-30%. The enhanced trapping efficiency observed with the sono-induced cold vapor generation as compared with 'in-atomizer trapping' methods employing chemical vapor generation is discussed. A reaction pathway for SI-CVG is proposed on the basis of the current knowledge for synthesis of noble metal nanoparticles by ultrasound

  1. Secondary electron emission from Au by medium energy atomic and molecular ions

    CERN Document Server

    Itoh, A; Obata, F; Hamamoto, Y; Yogo, A

    2002-01-01

    Number distributions of secondary electrons emitted from a Au metal surface have been measured for atomic and molecular ions of H sup + , He sup + , C sup + , N sup + , O sup + , H sup + sub 2 , H sup + sub 3 , HeH sup + , CO sup + and O sup + sub 2 in the energy range 0.3-2.0 MeV. The emission statistics obtained are described fairly well by a Polya function. The Polya parameter b, determining the distribution shape, is found to decrease monotonously with increasing emission yield gamma, revealing a surprising relationship of b gamma approx 1 over the different projectile species and impact energies. This finding supports certainly the electron cascading model. Also we find a strong negative molecular effect for heavier molecular ions, showing a significant reduction of gamma compared to the estimated values using constituent atomic projectile data.

  2. Effect of Cs and Li atom adsorption on MgO: Secondary emission and work function

    International Nuclear Information System (INIS)

    Bagraev, N.T.; Borisov, V.L.

    1980-01-01

    Adsorption of Cs and Li atoms on the surface of single crystal magnesium oxide films has been investigated using Auger, LEED and contact difference techniques. A decreased work function for a single crystal MgO film grown on the Mo (100) face was observed to be accompanied by an increased secondary electron emission yield shown to be due to a larger escape depth for secondary electrons. LEED showed well ordered layers of adsorbed Cs on the MgO film surface. A model to explain the behaviour of Cs atoms on the film surface is proposed. It is shown that the stability of the Cs coating is not dependent on a prolonged bombardment of the film by incident electron beams of high current density. Depositing and implanting of thin single crystal MgO films with Li were found to result in an increased secondary electron emission yield, with Li adsorption on the MgO film surface being disordered. (orig.)

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

    Science.gov (United States)

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

    1999-06-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-09-15

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

  5. Search for two-photon emission from 2S states of low-Z muonic atoms

    International Nuclear Information System (INIS)

    Carter, A.L.; Hincks, E.P.; Cox, C.R.; Dodson, G.W.; Eckhause, M.; Kane, J.R.; Rushton, A.M.; Siegel, R.T.; Welsh, R.E.; Hargrove, C.K.; Mes, H.; Dixit, M.S.; National Research Council of Canada, Ottawa, Ontario)

    1983-01-01

    A search for two-photon emission from 2S states of low-Z muonic atoms has been made. Intrinsic Ge detectors were positioned around target of Li, Be, B, or their hydrides, or a vessel containing B 2 H 6 , H 2 , or O 2 . Upper limits on the fraction of stopping muons which formed metastable 2S states range from approx.= 10 - 3 to 10 - 5 . (orig.)

  6. Search for two-photon emission from 2S states of low-Z muonic atoms

    Energy Technology Data Exchange (ETDEWEB)

    Carter, A.L.; Hincks, E.P. (Carleton Univ., Ottawa, Ontario (Canada). Dept. of Physics); Cox, C.R.; Dodson, G.W.; Eckhause, M.; Kane, J.R.; Rushton, A.M.; Siegel, R.T.; Welsh, R.E. (College of William and Mary, Williamsburg, VA (USA). Dept. of Physics); Hargrove, C.K.

    1983-05-12

    A search for two-photon emission from 2S states of low-Z muonic atoms has been made. Intrinsic Ge detectors were positioned around target of Li, Be, B, or their hydrides, or a vessel containing B/sub 2/H/sub 6/, H/sub 2/, or O/sub 2/. Upper limits on the fraction of stopping muons which formed metastable 2S states range from approximately = 10/sup -3/ to 10/sup -5/.

  7. Atomic emission spectroscopic investigations for determining depth profiles at boride layers on iron materials

    International Nuclear Information System (INIS)

    Danzer, K.; Marx, G.

    1980-01-01

    A combination of atomic emission spectroscopic surface analysis and mechanical removement of defined surface areas in layers by grinding yields information about the depth distribution of boron in iron. In addition, the evaluation with the aid of the two-dimensional variance analysis leads to statements on the homogeneous distribution within individual layers at different depth. The results obtained in this way are in agreement with those of other methods

  8. Inductively coupled plasma for atomic emission spectroscopy at the Savannah River Plant

    International Nuclear Information System (INIS)

    Coleman, J.T.

    1986-01-01

    The Savannah River Plant atomic emission spectroscopy laboratory has been in operation for over 30 years. Routine analytical methods and instrumentation are being replaced with current technology. Laboratory renovation will include the installation of contained dual excitation sources (inductively coupled plasma and d-c arc) with a direct reading spectrometer. The instrument will be used to provide impurity analyses of plutonium, uranium, and other nuclear fuel cycle materials

  9. Direct atomic-emission determination of tungsten in molybdenum oxide in dc arc

    International Nuclear Information System (INIS)

    Zolotareva, N.I.; Grazhulene, S.S.

    2007-01-01

    A method of direct atomic-emission determination of tungsten impurity in molybdenum trioxide of high purity in dc arc is presented. Chemically active additives of elementary sulfur and gallium oxide are used to optimize W evaporation rate and residence time in the arc plasma. The procedure is easy to use and provides the limit of W determination at a level of 2x10 -4 wt. % [ru

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

    Science.gov (United States)

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

    2016-02-01

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

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

    Science.gov (United States)

    Zurynková, Pavla; Dědina, Jiří; Kratzer, Jan

    2018-06-20

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

  12. Angle and Spin Resolved Auger Emission Theory and Applications to Atoms and Molecules

    CERN Document Server

    Lohmann, Bernd

    2009-01-01

    The Auger effect must be interpreted as the radiationless counterpart of photoionization and is usually described within a two-step model. Angle and spin resolved Auger emission physics deals with the theoretical and numerical description, analysis and interpretation of such types of experiments on free atoms and molecules. This monograph derives the general theory applying the density matrix formalism and, in terms of irreducible tensorial sets, so called state multipoles and order parameters, for parameterizing the atomic and molecular systems, respectively. Propensity rules and non-linear dependencies between the angular distribution and spin polarization parameters are included in the discussion. The numerical approaches utilizing relativistic distorted wave (RDWA), multiconfigurational Dirac-Fock (MCDF), and Greens operator methods are described. These methods are discussed and applied to theoretical predictions, numerical results and experimental data for a variety of atomic systems, especially the rare...

  13. Determination of Cr, Mn, Si, and Ni in carbon steels by optical emission spectrometry with spark source

    International Nuclear Information System (INIS)

    Garcia Gonzalez, M.A.; Pomares Alfonso, M.; Mora Lopez, L.

    1995-01-01

    Elemental composition of steels determines some important of his characteristic moreover it is necessary to obtain their quality certification. Analytical procedure has performed for determination of Cr, Mn, Si and Ni in carbon steels by optical emission spectrometry with spark source. reproducibility of results is 5-11 %. Exactitude has tested with results that have obtained by internationally recognised methods-

  14. Spontaneous emission spectra and simulating multiple spontaneous generation coherence in a five-level atomic medium

    International Nuclear Information System (INIS)

    Li Jiahua; Liu Jibing; Qi Chunchao; Chen Aixi

    2006-01-01

    We investigate the features of the spontaneous emission spectra in a coherently driven cold five-level atomic system by means of a radio frequency (rf) or microwave field driving a hyperfine transition within the ground state. It is shown that a few interesting phenomena such as spectral-line narrowing, spectral-line enhancement, spectral-line suppression, and spontaneous emission quenching can be realized by modulating the frequency and intensity of the rf-driving field in our system. In the dressed-state picture of the coupling and rf-driving fields, we find that this coherently driven atomic system has three close-lying levels so that multiple spontaneously generated coherence (SGC) arises. Our considered atomic model can be found in real atoms, such as rubidium or sodium, so a corresponding experiment can be done to observe the expected phenomena related to SGC reported by Fountoulakis et al. [Phys. Rev. A 73, 033811 (2006)], since no rigorous conditions are required

  15. Atoms

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2014-10-01

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

  17. An improved microstrip plasma for optical emission spectrometry of gaseous species

    Energy Technology Data Exchange (ETDEWEB)

    Schermer, Susanne; Bings, Nicolas H.; Bilgic, Attila M.; Stonies, Robert; Voges, Edgar; Broekaert, Jose A.C. E-mail: jose.broekaert@chemie.uni-hamburg.de

    2003-09-26

    A modified compact 2.45 GHz microstrip plasma (MSP) operated with Ar as working gas at atmospheric pressure has been characterized and examined for its suitability for the determination of Hg as gaseous species by optical emission spectrometry. As a formerly described MSP the new device is provided on a sapphire substrate. The areas of plasma stability in terms of gas flow rates and microwave power for both MSPs with respect to plasma form and reflected power were investigated. Power levels of 5-40 W and Ar flow rates of 15-60 l/h were used. The modified MSP, which extends out of the channel in the sapphire substrate, was used for the recording of emission spectra for Hg vapor at different working conditions. Using optimized parameters a detection limit for Hg of less than 10 ng Hg/l Ar is obtained. The attainable excitation temperatures in the modified MSP at different microwave power were determined under the use of Fe as thermometric species and introducing ferrocene into the plasma. They were found to be at the order of 6000-7000 K for a power of 10-40 W and a gas flow of 15 l/h. It was shown that the modified MSP source can be combined with both a conventional monochromator with photomultiplier detection and a miniaturized spectrometer with CCD detection, whereby space-angle limitations are not stringent.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-11-15

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

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

    Czech Academy of Sciences Publication Activity Database

    Zurynková, Pavla; Dědina, Jiří; Kratzer, Jan

    2018-01-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-15

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

  2. Charging induced emission of neutral atoms from NaCl nanocube corners

    International Nuclear Information System (INIS)

    Ceresoli, Davide; Zykova-Timan, Tatyana; Tosatti, Erio

    2008-01-01

    Detachment of neutral cations/anions from solid alkali halides can in principle be provoked by donating/subtracting electrons to the surface of alkali halide crystals, but generally constitutes a very endothermic process. However, the amount of energy required for emission is smaller for atoms located in less favorable positions, such as surface steps and kinks. For a corner ion in an alkali halide cube the binding is the weakest, so it should be easier to remove that atom, once it is neutralized. We carried out first principles density functional calculations and simulations of neutral and charged NaCl nanocubes, to establish the energetics of extraction of neutralized corner ions. Following hole donation (electron removal) we find that detachment of neutral Cl corner atoms will require a limited energy of about 0.8 eV. Conversely, following the donation of an excess electron to the cube, a neutral Na atom is extractable from the corner at the lower cost of about 0.6 eV. Since the cube electron affinity level (close to that a NaCl(100) surface state, which we also determine) is estimated to lie about 1.8 eV below vacuum, the overall energy balance upon donation to the nanocube of a zero-energy electron from vacuum will be exothermic. The atomic and electronic structure of the NaCl(100) surface, and of the nanocube Na and Cl corner vacancies are obtained and analyzed as a byproduct

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

    Energy Technology Data Exchange (ETDEWEB)

    Vilar Farinas, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Barciela Garcia, J. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Garcia Martin, S. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena Crecente, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Herrero Latorre, C. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)]. E-mail: cherrero@lugo.usc.es

    2007-05-22

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO{sub 3}){sub 2} and (NH{sub 4})H{sub 2}PO{sub 4}-Mg(NO{sub 3}){sub 2}] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 {mu}g L{sup -1}), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-08-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO 3 ) 2 and (NH 4 )H 2 PO 4 -Mg(NO 3 ) 2 ] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 μg L -1 ), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged -1

  6. Trace element determination using static high-sensitivity inductively coupled plasma optical emission spectrometry (SHIP-OES).

    Science.gov (United States)

    Engelhard, Carsten; Scheffer, Andy; Nowak, Sascha; Vielhaber, Torsten; Buscher, Wolfgang

    2007-02-05

    A low-flow air-cooled inductively coupled plasma (ICP) design for optical emission spectrometry (OES) with axial plasma viewing is described and an evaluation of its analytical capabilities in trace element determinations is presented. Main advantage is a total argon consumption of 0.6 L min(-1) in contrast to 15 L min(-1) using conventional ICP sources. The torch was evaluated in trace element determinations and studied in direct comparison with a conventional torch under the same conditions with the same OES system, ultrasonic nebulization (USN) and single-element optimization. A variety of parameters (x-y-position of the torch, rf power, external air cooling, gas flow rates and USN operation parameters) was optimized to achieve limits of detection (LOD) which are competitive to those of a conventional plasma source. Ionic to atomic line intensity ratios for magnesium were studied at different radio frequency (rf) power conditions and different sample carrier gas flows to characterize the robustness of the excitation source. A linear dynamic range of three to five orders of magnitude was determined under compromise conditions in multi-element mode. The accuracy of the system was investigated by the determination of Co, Cr, Mn, Zn in two certified reference materials (CRM): CRM 075c (Copper with added impurities), and CRM 281 (Trace elements in rye grass). With standard addition values of 2.44+/-0.04 and 3.19+/-0.21 microg g(-1) for Co and Mn in the CRM 075c and 2.32+/-0.09, 81.8+/-0.4, 32.2+/-3.9 for Cr, Mn and Zn, respectively, were determined in the samples and found to be in good agreement with the reported values; recovery rates in the 98-108% range were obtained. No influence on the analysis by the matrix load in the sample was observed.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-01-15

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

  8. Assessing the role of "bottom-up" emissions and simplified chemical mechanisms in reconciling CESM2.0 with TOGA observations from the ORCAS and ATom-2 campaigns

    Science.gov (United States)

    Asher, E.; Emmons, L. K.; Kinnison, D. E.; Tilmes, S.; Hills, A. J.; Hornbrook, R. S.; Stephens, B. B.; Apel, E. C.

    2017-12-01

    Surface albedo and precipitation over the Southern Ocean are sensitive to parameterizations of aerosol formation and cloud dynamics in global climate models. Observations of precursor gases for natural aerosols can help constrain the uncertainty in these parameterizations, if used in conjunction with an appropriately simplified chemical mechanism. We implement current oceanic "bottom-up" emission climatologies of dimethyl sulfide (DMS) and isoprene in CESM2.0 (Lana et al. 2016; Archer et al. 2009) and compare modeled constituents from two separate chemical mechanisms with data obtained from the Trace Organic Gas Analyzer (TOGA) on the O2/N2 Ratios and CO2 Airborne Study in the Southern Ocean (ORCAS) and the Atmospheric Tomography Mission 2 (ATom-2). We use ORCAS measurements of DMS, isoprene, methyl vinyl ketone (MVK) and methacrolein (MACR) from over 10 flights in Jan. - Feb. 2016 as a training dataset to improve "bottom-up" emissions. Thereafter, we evaluate the scaled "top-down" emissions in CESM with TOGA data obtained from the Atmospheric Tomography Mission (ATom-2) in Feb. 2017. Recent laboratory studies at NCAR confirm that TOGA surpasses proton transfer reaction mass spectrometry (PTR-MS) and commercial gas chromatography (GC) instruments with respect to accurate measurements of oxygenated VOCs in low nitrogen oxide (NO) environments, such as MVK and MACR.

  9. Arsenic speciation in edible alga samples by microwave-assisted extraction and high performance liquid chromatography coupled to atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    García-Salgado, S.; Quijano, M.A.; Bonilla, M.M.

    2012-01-01

    Highlights: ► Total As and As species were analyzed in edible marine algae. ► A microwave-assisted extraction method with deionized water was applied. ► As compounds identified comprised DMA, As(V) and four arsenosugars ► Considerably high As(V) concentrations were found in the most of the algae studied. - Abstract: Twelve commercially available edible marine algae from France, Japan and Spain and the certified reference material (CRM) NIES No. 9 Sargassum fulvellum were analyzed for total arsenic and arsenic species. Total arsenic concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) after microwave digestion and ranged from 23 to 126 μg g −1 . Arsenic species in alga samples were extracted with deionized water by microwave-assisted extraction and showed extraction efficiencies from 49 to 98%, in terms of total arsenic. The presence of eleven arsenic species was studied by high performance liquid chromatography–ultraviolet photo-oxidation–hydride generation atomic–fluorescence spectrometry (HPLC–(UV)–HG–AFS) developed methods, using both anion and cation exchange chromatography. Glycerol and phosphate sugars were found in all alga samples analyzed, at concentrations between 0.11 and 22 μg g −1 , whereas sulfonate and sulfate sugars were only detected in three of them (0.6-7.2 μg g −1 ). Regarding arsenic toxic species, low concentration levels of dimethylarsinic acid (DMA) ( −1 ) and generally high arsenate (As(V)) concentrations (up to 77 μg g −1 ) were found in most of the algae studied. The results obtained are of interest to highlight the need to perform speciation analysis and to introduce appropriate legislation to limit toxic arsenic species content in these food products.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-01

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

  12. The use of double laser pulses for the atomic-emission spectral estimation of uranium content in biological samples

    International Nuclear Information System (INIS)

    Patapovich, M.P.; Umreiko, D.S.; Zajogin, A.P.; Buloichik, J.I.

    2012-01-01

    This paper is aimed at the development of the techniques for estimation of the uranium content in biological objects (hair) using the atomic-emission laser analysis with a sufficient accuracy and high processing rate. (authors)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-05-15

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

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

    International Nuclear Information System (INIS)

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

    1975-01-01

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

  15. REVIEW: Spontaneous emission of an atom in the presence of nanobodies

    Science.gov (United States)

    Klimov, Vasilii V.; Ducloy, M.; Letokhov, V. S.

    2001-07-01

    The effect of nanobodies, i.e., the bodies whose size is small compared to the emission wavelength, on spontaneous emission of an atom located near them is considered. The results of calculations performed within the framework of quantum and classical electrodynamics are presented both in analytic and graphical forms and can be readily used for planning experiments and analysis of experimental data. It is shown that nanobodies can be used to control efficiently the rate of spontaneous transitions. Thus, an excited atom located near a nanocylinder or a nanospheroid pole, whose transition dipole moment is directed normally to the nanobody surface, can decay with the rate that is tens and hundreds times higher than the decay rate in a free space. In the case of some (negative) dielectric constants, the decay rate can increase by a factor of 105—106 and more. On the other hand, the decay of an excited atom whose transition dipole moment is directed tangentially to the nanobody surface substantially slows down. The probability of nonradiative decay of the excited state is shown to increase substantially in the presence of na-nobodies possessing losses.

  16. Atomic hydrogen determination in medium-pressure microwave discharge hydrogen plasmas via emission actinometry

    International Nuclear Information System (INIS)

    Geng Zicai; Xu Yong; Yang Xuefeng; Wang Weiguo; Zhu Aimin

    2005-01-01

    Atomic hydrogen plays an important role in the chemical vapour deposition of functional materials, plasma etching and new approaches to the chemical synthesis of hydrogen-containing compounds. This work reports experimental determinations of atomic hydrogen in microwave discharge hydrogen plasmas formed from the TM 01 microwave mode in an ASTeX-type reactor, via optical emission spectroscopy using Ar as an actinometer. The relative intensities of the H atom Balmer lines and Ar-750.4 nm emissions as functions of input power and gas pressure have been investigated. At an input microwave power density of 13.5 W cm -3 , the approximate hydrogen dissociation fractions calculated from electron-impact excitation and quenching cross sections in the literature, decreased from ∼0.08 to ∼0.03 as the gas pressure was increased from 5 to 25 Torr. The influences of the above cross sections, and the electron and gas temperatures of the plasmas on the determination of the hydrogen dissociation fraction data have been discussed

  17. Halogenated salicylaldehyde azines: The heavy atom effect on aggregation-induced emission enhancement properties

    International Nuclear Information System (INIS)

    Chen, Xiao-tong; Tong, Ai-jun

    2014-01-01

    This study investigates the heavy-atom effect (HAE) on aggregation-induced emission enhancement (AIEE) properties of salicylaldehyde azines. For this purpose, a series of halogenated salicylaldehyde azine derivatives, namely, chloro-salicylaldehyde azine (1), bromo-salicylaldehyde azine (2) and iodo-salicylaldehyde azine (3) are synthesized. 1 and 2 display typical AIEE characteristics of salicylaldehyde azine compounds; whereas for the iodo-substituent in 3, is found to be effective “external” heavy atom quenchers to salicylaldehyde azine fluorescence in aggregated state. Based on its weak fluorescence in aggregated state and relative strong fluorescence in dispersed state, 3 can also be applied as a turn-on fluorescence probe for egg albumin detection attributed to hydrophobic interaction. -- Highlights: • This study investigates the heavy-atom effect (HAE) on aggregation-induced emission enhancement (AIEE) properties of salicylaldehyde azines. • Chloro- and bromo-salicylaldehyde display typical AIEE properties of salicylaldehyde azine, whereas the iodo-substitute quenches AIEE in aggregated state. • Iodo-salicylaldehyde can be applied as a turn-on fluorescence probe for egg albumin detection attributed to hydrophobic interaction

  18. On I(5577 Å and I (7620 Å auroral emissions and atomic oxygen densities

    Directory of Open Access Journals (Sweden)

    R. L. Gattinger

    1996-07-01

    Full Text Available A model of auroral electron deposition processes has been developed using Monte Carlo techniques to simulate electron transport and energy loss. The computed differential electron flux and pitch angle were compared with in situ auroral observations to provide a check on the accuracy of the model. As part of the energy loss process, a tally was kept of electronic excitation and ionization of the important atomic and molecular states. The optical emission rates from these excited states were computed and compared with auroral observations of η(3914 Å, η(5577 Å, η(7620 Å and η(N2VK. In particular, the roles played by energy transfer from N2(A3Σ+u and by other processes in the excitation of O(1S and O2(b1Σ+g were investigated in detail. It is concluded that the N2(A3Σ+u mechanism is dominant for the production of OI(5577 Å in the peak emission region of normal aurora, although the production efficiency is much smaller than the measured laboratory value; above 150 km electron impact on atomic oxygen is dominant. Atomic oxygen densities in the range of 0.75±0.25 MSIS-86 [O] were derived from the optical comparisons for auroral latitudes in mid-winter for various levels of solar and magnetic activity.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-04-15

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

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

    Science.gov (United States)

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

    2016-01-15

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

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Nielsen, Steffen

    1998-01-01

    One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atom...

  2. Nanocluster formation by spin coating : quantitative atomic force microscopy and Rutherford backscattering spectrometry analysis

    NARCIS (Netherlands)

    Partridge, A.; Toussaint, S.L.G.; Flipse, C.F.J.; IJzendoorn, van L.J.; Oetelaar, van den L.C.A.

    1996-01-01

    A recently developed spin coating method has been employed to produce a homogeneous distribution of nanometer-sized metal clusters onto a flat oxidic support. The particle size and distribution, and the total amount of material deposited has been studied by comparing the results of atomic force

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

    Science.gov (United States)

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

    1984-01-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

    The soil samples of nine different sites in Islamabad were studied for their elemental composition. Instrumental neutron activation analysis and atomic absorption spectrometry were employed and 33 elements were determined. The acquired data were analyzed using descriptive statistics, principal component analysis, cluster analysis, pollution level index and enrichment factor. A perusal of results shows a distribution of elemental concentration in two major groups, one along the highway and the other in industrial area of Islamabad. The soil along the highway sites was found to be relatively less polluted than at the sites in the industrial area. The enrichment factor indicates the presence of As, Pb, Sb, Se and Sn at higher levels. The method validation was done by analyzing IAEA reference materials SL-1 (lake sediment) and S7 (soil). (orig.)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

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

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Ekelund, J.

    1989-01-01

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

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

    International Nuclear Information System (INIS)

    Tran Bang Diep; Tran Dai Nghiep

    2005-01-01

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

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

    Science.gov (United States)

    Viets, J.G.

    1978-01-01

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

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

    International Nuclear Information System (INIS)

    Sekerka, I.; Lechner, J.F.

    1991-01-01

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

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

    Science.gov (United States)

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

    2008-04-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    Science.gov (United States)

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

    2014-08-13

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

  14. Effect of atomic-state coherence and spontaneous emission on three-level dynamics

    International Nuclear Information System (INIS)

    Cardimona, D.A.

    1990-01-01

    For a three-level atom in the ssV configuration (i.e., having two excited states each dipole-coupled to a common ground state), we have found a particular linear combination of bare-atom states in which Rabi oscillations and their associated collapses and revivals do not occur. Moving to a dressed-state picture, we discover that this particular linear combination state is just that dressed state which is decoupled from all the field modes. It is a dressed state for which the transition dipole moments with the other dressed states are zero. The existence of this decoupled dressed state depends on the tuning of the dressing laser field, which in turn depends on the bare-atom excited-state dipole moments and energy-level separation. When we include spontaneous emission, the population decays from the other dressed states into this decoupled state and remains coherently trapped there, producing a system that experiences no dynamical behavior. This is exact for δ-function photon statistics (i.e., if there is no intensity uncertainty). The trapping becomes less perfect as the photon statistics are allowed to have a greater bandwidth. Also, if the applied field is tuned incorrectly, the spontaneous realignment of the atomic state amplitudes does not result in a totally decoupled dressed state, and the dynamics proceed normally

  15. CHIANTI—AN ATOMIC DATABASE FOR EMISSION LINES. XII. VERSION 7 OF THE DATABASE

    International Nuclear Information System (INIS)

    Landi, E.; Del Zanna, G.; Mason, H. E.; Young, P. R.; Dere, K. P.

    2012-01-01

    The CHIANTI spectral code consists of an atomic database and a suite of computer programs to calculate the optically thin spectrum of astrophysical objects and carry out spectroscopic plasma diagnostics. The database includes atomic energy levels, wavelengths, radiative transition probabilities, collision excitation rate coefficients, and ionization and recombination rate coefficients, as well as data to calculate free-free, free-bound, and two-photon continuum emission. Version 7 has been released, which includes several new ions, significant updates to existing ions, as well as Chianti-Py, the implementation of CHIANTI software in the Python programming language. All data and programs are freely available at http://www.chiantidatabase.org, while the Python interface to CHIANTI can be found at http://chiantipy.sourceforge.net.

  16. CHIANTI-AN ATOMIC DATABASE FOR EMISSION LINES. XII. VERSION 7 OF THE DATABASE

    Energy Technology Data Exchange (ETDEWEB)

    Landi, E. [Department of Atmospheric, Oceanic and Space Sciences, University of Michigan, Ann Arbor, MI 48109 (United States); Del Zanna, G.; Mason, H. E. [Department of Applied Mathematics and Theoretical Physics, University of Cambridge, Wilberforce Road, Cambridge CB3 0WA (United Kingdom); Young, P. R. [College of Science, George Mason University, 4400 University Drive, Fairfax, VA, 22030 (United States); Dere, K. P. [School of Physics, Astronomy and Computational Sciences, MS 6A2, George Mason University, 4400 University Drive, Fairfax, VA 22030 (United States)

    2012-01-10

    The CHIANTI spectral code consists of an atomic database and a suite of computer programs to calculate the optically thin spectrum of astrophysical objects and carry out spectroscopic plasma diagnostics. The database includes atomic energy levels, wavelengths, radiative transition probabilities, collision excitation rate coefficients, and ionization and recombination rate coefficients, as well as data to calculate free-free, free-bound, and two-photon continuum emission. Version 7 has been released, which includes several new ions, significant updates to existing ions, as well as Chianti-Py, the implementation of CHIANTI software in the Python programming language. All data and programs are freely available at http://www.chiantidatabase.org, while the Python interface to CHIANTI can be found at http://chiantipy.sourceforge.net.

  17. Dynamical Evolution of Properties for Atom and Field in the Process of Two-Photon Absorption and Emission Between Atomic Levels

    Science.gov (United States)

    Wang, Jian-ming; Xu, Xue-xiang

    2018-04-01

    Using dressed state method, we cleverly solve the dynamics of atom-field interaction in the process of two-photon absorption and emission between atomic levels. Here we suppose that the atom is initially in the ground state and the optical field is initially in Fock state, coherent state or thermal state, respectively. The properties of the atom, including the population in excited state and ground state, the atom inversion, and the properties for optical field, including the photon number distribution, the mean photon number, the second-order correlation function and the Wigner function, are discussed in detail. We derive their analytical expressions and then make numerical analysis for them. In contrast with Jaynes-Cummings model, some similar results, such as quantum Rabi oscillation, revival and collapse, are also exhibit in our considered model. Besides, some novel nonclassical states are generated.

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

    Science.gov (United States)

    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.

  19. Introduction of Flame Atomic Absorption Spectrometry (FAAS) For River Water Samples Analysis

    International Nuclear Information System (INIS)

    Shakirah Abd Shukor; Mohd Suhaimi Hamzah; Shamsiah Abdul Rahman

    2015-01-01

    Metal contamination in water is a major component in the determination of water quality monitoring. In spite of the viability of several other metal ion analysis techniques for river water, atomic absorption spectroscopy (AAS) method is most commonly used due to the reproducibility results, short analysis time, cost effective, lower level detection and robust. Therefore, this article gives an overview on the principles, instrumentation techniques, sample preparations, instrument calibration and data analysis in a simple manner for beginner. (author)

  20. Study of thermoelectron emission of oxidized tungsten sponge in cesium atom flow

    International Nuclear Information System (INIS)

    Tursunmetov, K.A.; Sabirov, A.K.

    1993-01-01

    Thermoelectron emission of a tungsten sponge with 30-40% porosity is studied. The tungsten sponge is produced of fine-grain tungsten powder (diameter - 1-2 μm) according to standard technology. It is shown that tungsten sponge oxidation at T=1000 K with subsequent heating in vacuum at T=1100 K allows one to obtain the minimal stable and reproducible work function at the level of 1.03-1.05 eV in a flux of cesium atoms. Estimations show that effective emitting surface is 15-20 times as much as the polycrystal surface