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Sample records for atomic emission spectrometry

  1. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.

    1992-01-01

    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. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  3. Determination of Uranium in Apatite Minerals by Solvent Extraction--Inductively Coupled Plasma Atomic Emission Spectrometry

    OpenAIRE

    1993-01-01

    [Abstract] Solvent, extraction-ICP atomic emission spectrometry was applied to the determination of uranium in apatite minerals. Apatite minerals were treated with nitric acid. After removing a small quantity of insoluble residue, uranium was extracted with 0.05 mol/dm^3 1-phonyl-3-mcthyl-4-trifluoroacetyl-5-pyrazolonc-diisobutyl kctone at pH 0.8. The uranium content in the apatite was found to be (20.3〜132.9)×10^%.

  4. The Kalman filter approach to inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Van Veen, E. H.; Bosch, S.; De Loos-Vollebregt, M. T. C.

    1994-07-01

    This article is an electronic publication in Spectrochimica Acta Electronica (SAE), the electronic section of Spectrochimica Acta Part B (SAB). The hardcopy text, comprising the main article and two appendices, is accompanied by a disk containing the compiled program, a reference manual and data files. The work deals with data handling in inductively coupled plasma atomic emission spectrometry (ICP-AES). With this technique, the analyte signal is superimposed on a background signal. When separating the signals by manual or automated three-point background correction, there are many instances in which the data reduction fails. Based on scans recorded in a fast-scanning mode and on a library of pure-component scans, the Kaiman filter approach models the emission in the spectral window (about 100 pm) of the analyte and mathematically solves the problem of background correction. By using a criterion-based algorithm to correct for optical instability, the uncertainty in the determination of the interferent line signal is eliminated. Therefore, the present filter implementation yields more accurate and precise results, especially in the case of line overlap. The Kalman filter Approach to Atomic Spectrometry (KAAS) software automatically processes Perkin-Elmer Plasma 1000/2000 text files, but can also handle ASCII data files. Practical and comprehensive examples are given to evoke the "Kalman filter feeling" in the crucial step of creating the emission model.

  5. [Determination of total sulfur in coal by inductively coupled plasma atomic emission spectrometry].

    Science.gov (United States)

    Liu, Dong-yan; Zhang, Yuan-li

    2002-02-01

    A direct method was reported for the determination of total sulfur in coal by inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution conditions of coal samples as well as interference conditions of hydrochloric acid and matrix were studied. The recommended method not only proved to be simple and rapid than traditional gravimetric method but show satisfying precision and accuracy as well. The results of samples are as same as gravimetry. The recoveries are more than 96%, and the relative standard deviation of six samples are less than 3%.

  6. 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.

  7. Analysis of tungsten carbide coatings by UV laser ablation inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Kanicky, V.; Otruba, V.; Mermet, J.-M.

    2000-06-01

    Tungsten carbide coatings (thickness 0.1-0.2 mm) containing 8.0, 12.2, 17.2 and 22.9% Co were studied with laser ablation inductively coupled plasma atomic emission spectrometry (LA-ICP-AES). Composition of these plasma sprayed deposits on steel disks was determined using X-ray fluorescence spectrometry and electron microprobe energy/wavelength dispersive X-ray spectrometry. The coatings were ablated by means of a Q-switched Nd:YAG laser at 266 nm (10 Hz, 10 mJ per shot) coupled to an ICP echelle-based spectrometer equipped with a segmented charge-coupled device detector. Non-linear dependences of cobalt lines intensities on the Co percentage were observed both at a single spot ablation and at a sample translation. This behaviour could be attributed to a complex phase composition of the system W-C-Co. However, employing tungsten as internal standard the linear calibration was obtained for studied analytical lines Co II 228.616 nm, Co II 230.786 nm, Co II 236.379 nm and Co II 238.892 nm.

  8. Determination of additives in PVC material by UV laser ablation inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Hemmerlin, M.; Mermet, J. M.; Bertucci, M.; Zydowicz, P.

    1997-04-01

    UV laser ablation inductively coupled plasma atomic emission spectrometry (LA-ICP-AES) has been applied to the direct determination of additives in solid poly(vinyl chloride) materials. A Nd:YAG laser, operating at its fourth harmonic (266 nm), was used with a beam masking device, in the most reproducible conditions, to introduce solid particles into the plasma torch of a simultaneous ICP-AES system. Emphasis was placed on both precision and accuracy in the analysis of PVC materials by LA-ICP-AES. A series of six in-house PVC reference materials was prepared by incorporating several additives in increasing concentrations. Three alternative methods were evaluated to certify the amount of incorporated elements: ICP-AES with sample dissolution, NAA and XRF. Satisfactory results and good agreement were obtained for seven elements (Al, Ca, Cd, Mg, Sb, Sn and Ti) among the ten incorporated. Sample homogeneity appeared to be satisfactory, and calibration graphs obtained by LA-ICP-AES for several elements are presented. Finally, the performance of the technique in terms of repeatability (1.6-5%), reproducibility (2-5%), and limits of detection was investigated.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-05-10

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

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

    Science.gov (United States)

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

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Peterson, C. A.

    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 ..mu..g/g with the majority falling in the 0.01 to 0.1 ..mu..g/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 ..mu..m 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Yong Sam; Choi, Kwang Soon; Moon, Jong Hwa; Kim, Sun Ha; Lim, Jong Myoung; Kim, Young Jin [KAERI, Taejon (Korea, Republic of); Quraishi, Shamshad Begum [Bangladesh Atomic Energy Commission, Dhaka (Bangladesh)

    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)

  13. Gunshot residue testing in suicides: Part II: Analysis by inductive coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Molina, D Kimberley; Castorena, Joe L; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

    2007-09-01

    Several different methods can be employed to test for gunshot residue (GSR) on a decedent's hands, including scanning electron microscopy with energy dispersive x-ray (SEM/EDX) and inductive coupled plasma-atomic emission spectrometry (ICP-AES). In part I of this 2-part series, GSR results performed by SEM/EDX in undisputed cases of suicidal handgun wounds were studied. In part II, the same population was studied, deceased persons with undisputed suicidal handgun wounds, but GSR testing was performed using ICP-AES. A total of 102 cases were studied and analyzed for caliber of weapon, proximity of wound, and the results of the GSR testing. This study found that 50% of cases where the deceased was known to have fired a handgun immediately prior to death had positive GSR results by ICP/AES, which did not differ from the results of GSR testing by SEM/EDX. Since only 50% of cases where the person is known to have fired a weapon were positive for GSR by either method, this test should not be relied upon to determine whether someone has discharged a firearm and is not useful as a determining factor of whether or not a wound is self-inflicted or non-self-inflicted. While a positive GSR result may be of use, a negative result is not helpful in the medical examiner setting as a negative result indicates that either a person fired a weapon prior to death or a person did not fire a weapon prior to death.

  14. Analysis of tree leaves, bark and wood by sequential inductively coupled argon plasma atomic emission spectrometry

    Science.gov (United States)

    Verbeek, A. A.

    The analysis of extracts from tree leaf, bark and wood samples for Ca, Mg, K, Na, P, Mn, Fe, Al, B, Cu and Zn by inductively coupled argon plasma sequential emission spectrometry is described. Recovery percentages for simulated tree extracts and for spiked tree samples are presented together with typical analysis values for a leaf and a wood sample. The choice of analytical line for each element is discussed and spectral interferences, not listed in the ICP tables of Boumans, of Cu on the 214.9 nm line of P and of Fe on the 249.7 nm line of B are noted.

  15. Differentiation of colloidal and dissolved silica: Analytical separation using spectrophotometry and inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Lewis-Russ, A.; Ranville, J.; Kashuba, A.T.

    1991-01-01

    A method is described that differentiates between solutions containing silica-dominated colloids and solutions that are essentially free of colloids. Suspensions of tuff particles were treated to remove colloids by centrifugation, filtration or both. Agreement of silica concentrations determined by inductively coupled plasma atomic emission spectrometry and by a spectrophotometric method was taken as an indication of colloid-free solutions. For two tuffs, centrifugation was effective for removing colloids. For the third, highly altered tuff, filtration was more effective for removing colloids.

  16. 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

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

    Science.gov (United States)

    Montaser, A.

    This research follows a multifaceted approach, from theory to practice, to the investigation and development of novel helium plasmas, sample introduction systems, and diagnostic techniques for atomic and mass spectrometries. During the period January 1994 - December 1994, four major sets of challenging research programs were addressed that each included a number of discrete but complementary projects: (1) The first program is concerned with fundamental and analytical investigations of novel atmospheric-pressure helium inductively coupled plasmas (He ICPS) that are suitable for the atomization-excitation-ionization of elements, especially those possessing high excitation and ionization energies, for the purpose of enhancing sensitivity and selectivity of analytical measurements. (2) The second program includes simulation and computer modeling of He ICPS. The aim is to ease the hunt for new helium plasmas by predicting their structure and fundamental and analytical properties, without incurring the enormous cost for extensive experimental studies. (3) The third program involves spectroscopic imaging and diagnostic studies of plasma discharges to instantly visualize their prevailing structures, to quantify key fundamental properties, and to verify predictions by mathematical models. (4) The fourth program entails investigation of new, low-cost sample introduction systems that consume micro- to nanoliter quantity of sample solution in plasma spectrometries. A portion of this research involves development and applications of novel diagnostic techniques suitable for probing key fundamental properties of aerosol prior to and after injection into high-temperature plasmas. These efforts, still in progress, collectively offer promise of solving singularly difficult analytical problems that either exist now or are likely to arise in the future in the various fields of energy generation, environmental pollution, material science, biomedicine and nutrition.

  18. Determination of gaseous semi-and low-volatile organic halogen compounds by barrier-discharge atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    Yifei Sun; Nobuhisa Watanabe; Wei Wang; Tianle Zhu

    2013-01-01

    A group parameter approach using "total organic halogen" is effective for monitoring gaseous organic halogen compounds,including fluorine,chlorine,and bromine compounds,generated from combustion.We described the use of barrier-discharge radiofrequencyhelium-plasma/atomic emission spectrometry,for the detection of semi-and low-volatile organic halogen compounds (SLVOXs),which can be collected by CarbotrapTM adsorbents and analyzed using thermal desorption.The optimal carrier gas flow rates at the injection and desorption lines were established to be 100 mL/min.The detection range for SLVOXs in the gaseous samples was from 10 ng to tens of micrograms.Measuring F was more diflicult than measuring Cl or Br,because the wavelength ofF is dose to that of air.The barrierdischarge radiofrequency-helium-plasma/atomic emission spectrometry measured from 85% to 103% of the SLVOXs in the gas sample.It has been found that Carbotrap B is appropriate for high-boiling-point compounds,and Carbotrap C is suitable for the determination of organic halogen compounds with lower boiling points,in the range 200-230℃.Under optimal analysis conditions,a chlorinecontaining plastic was destroyed using different oxygen concentrations.Lower oxygen concentrations resulted in the production of lower amounts of organic halogen compounds.

  19. 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

  20. Evaluation of arsenic and selenium in Brazilian soluble coffee by inductively coupled plasma atomic emission spectrometry with hydride generation

    Directory of Open Access Journals (Sweden)

    Santos Éder José dos

    2001-01-01

    Full Text Available A method for the evaluation of arsenic and selenium in soluble coffee by inductively coupled plasma atomic emission spectrometry with continuous hydride generation to attend the Brazilian food legislation is described. Samples were digested with nitric acid and hydrogen peroxide in a focused microwave system. Slow heating eliminated nitric acid and selenium (VI was reduced to selenium (IV by addition of 6 mol/L hydrochloric acid and heating at 90° C under a reflux system. The influence of sample acidity on sensitivity was investigated. Hydrochloric acid 6 mol/L was the most suitable reaction medium. Practical detection limits of 2.0mug/L for As and 1.0mu g/L for Se were achieved and attended the Brazilian food legislation. The results of recoveries on spiked samples demonstrate the reliability and accuracy of the procedure.

  1. Determination of trace elements in refined gold samples by inductively coupled plasma atomic emission spectrometry

    Directory of Open Access Journals (Sweden)

    Steharnik Mirjana

    2013-01-01

    Full Text Available This paper presents a method for determination the trace contents of silver, copper, iron, palladium, zinc and platinum in refined gold samples. Simultaneous inductively coupled plasma atomic emission spectrometer with radial torch position and cross flow nebulizer was used for determination. In order to compare the different calibration strategies, two sets of calibration standards were prepared. The first set was based on matrix matched calibration standards and the second was prepared without the addition of matrix material. Detection limits for matrix matching calibrations were higher for some elements than those without matrix matching. In addition, the internal standardization method was applied and experiments indicated that indium was the best option as internal standard. The obtained results for gold sample by matrix matching and matrix free calibrations were compared with the obtained results by standard addition method. The accuracy of the methods was tested performing recovery test. Recoveries for spiked sample were in the range of 90-115 %. The accuracy of the methods was also tested by analysis of certified reference material of high pure goldAuGHP1. The best results were achieved by matrix free calibration and standard addition method using indium as internal standard at wavelength of 230 nm. [Projekat Ministarstva nauke Republike Srbije, br. 34024: Development of Technologies for Recycling of Precious, Rare and Associated Metals from Solid Waste in Serbia to High Purity Products

  2. Analysis of tungsten carbide coatings by infrared laser-induced argon spark with inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Kanický, V.; Otruba, V.; Mermet, J.-M.

    2000-10-01

    Infrared laser ablation was studied for application to the analysis of plasma-sprayed tungsten carbide/cobalt coatings. The potential of the laser induced argon-spark (LINA-Spark™), as a sample introduction device in inductively coupled plasma atomic emission spectrometry was studied. The use of an IR laser along with defocusing led to laser-induced microplasma-based ablation. The mass ablation rate, represented by the ICP emission intensity per laser beam unit area, exhibited a flat increase in the irradiance range 2-250 GW/cm 2. A low slope (0.5) of this dependence in log-log scale gave evidence of plasma shielding. The steep increase in the measured acoustic signal when focused in front of the sample, i.e. in argon, indicated a breakdown of argon. Consequently, considerably lower ICP emissions were observed within the same range of irradiance. The cobalt/tungsten line intensity ratio in the ICP was practically constant from 1.5 up to at least 250 GW/cm 2. Acceptable precision (R.S.D.<5%) was obtained without internal standardization for irradiance between 2 and 8 GW/cm 2. Optimization of the laser pulse energy, repetition rate, beam focusing and sample displacement during interaction led to the linearization of dependences of signal vs. cobalt percentage, at least up to the highest studied value of 23% Co.

  3. 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

  4. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry. Progress report, January 1, 1990--December 31, 1992

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.

    1992-09-01

    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. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  5. Determination of micro yttrium in an ytterbium matrix by inductively coupled plasma atomic emission spectrometry and wavelet transform

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoguo

    2005-01-01

    In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix by inductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line of yttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium. In this work, a method based on wavelet transform was proposed for the spectral interference correction. Haar wavelet was selected as the mother wavelet. The discrete detail after the third decomposition, D3,was chosen for quantitative analysis based on the consideration of both separation degree and peak height. The linear correlation coefficient between the height of the left positive peak in D3 and the concentration of Y was calculated to be 0.9926.Six synthetic samples were analyzed, and the recovery for yttrium varied from 96.3% to 110.0%. The amounts of yttrium in three ytterbium metal samples were determined by the proposed approach with an average relative standard deviation (RSD)of 2.5%, and the detection limit for yttrium was 0.016%. This novel correction technique is fast and convenient, since neither complicated model assumption nor time-consuming iteration is required. Furthermore, it is not affected by the wavelength drift inherent in monochromators that will severely reduce the accuracy of results obtained by some chemometric methods.

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

    Science.gov (United States)

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

    2014-01-02

    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 comparable to other traditional methods.

  7. 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).

  8. 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).

  9. Evaluation of vapor generation for the determination of nickel by inductively coupled plasma-atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Marrero, Julieta [Comision Nacional de Energia Atomica, Unidad de Actividad Quimica, Centro Atomico Constituyentes, Av. Gral. Paz 1499, 1650-San Martin, Pcia. de Buenos Aires (Argentina); Smichowski, Patricia [Comision Nacional de Energia Atomica, Unidad Proyectos Especiales de Suministros Nucleares, Av. Libertador 8250, 1429-Buenos Aires (Argentina)

    2002-09-01

    Volatile species of Ni were generated by merging acidified aqueous samples and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the inlet tube of the plasma torch. Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for detection. The operating conditions (chemical and physical parameters) and the concentrations of different acids were evaluated for the efficient generation of Ni vapor. The detection limit (3 {sigma}{sub blank}) was 1.8 ng mL{sup -1}. The precision (RSD) of the determination was 4.2% at a level of 500 ng mL{sup -1} and 7.3% for 20 ng mL{sup -1} (n=10). The efficiency of the generation process was estimated to be 51%. The possible interfering effect of transition metals (Cd, Co, Cu, Cr, Fe, Mn, Zn), hydride forming elements (As, Ge, Pb, Sb, Se, Sn, Te), and Hg on Ni signal was examined. This study has demonstrated that Ni vapor generation is markedly free of interferences. (orig.)

  10. Determination of {sup 233}U by inductively coupled argon plasma - atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Patwardhan, A.B.; Kulkarni, V.T.; Radhakrishnan, K.; Ramanujam, A.; Page, A.G. [Bhabha Atomic Research Centre, Bombay (India)

    1994-09-01

    The paper describes studies carried out for the determination of {sup 233}U at various stages during the recovery and purification of {sup 233}U from {sup 233}U-Al alloy scraps generated during the fabrication of {sup 233}U-Al alloy fuel. Employing a high resolution sequential spectrometer and Inductively Coupled argon Plasma (ICP) as the spectral excitation source, isotope shift for {sup 233}U with respect to {sup 238}U has been resolved and recorded. The shift for the 424.437 nm emission line of {sup 238}U is found to be of the order of 0.040 nm on the lower wavelength side for {sup 233}U and this isotopic effect has been utilised for the quantitative determination of {sup 233}U. The overall precision of the method is 5% RSD with the detection limit of 0.01 {mu}g/ml.

  11. Determination of trace amounts of molybdenum in plant tissue by solvent extraction-atomic-absorption and direct-current plasma emission spectrometry.

    Science.gov (United States)

    Lajunen, L H; Kubin, A

    1986-03-01

    Methods are presented for determination of molybdenum in plant tissue by flame and graphite-furnace atomic-absorption spectrometry and direct-current argon-plasma emission spectrometry. The samples are digested in HNO(3)-H(2)SO(4)-HC1O(4) mixture, and Mo is separated and concentrated by chelation and extraction. Three organic solvents (methyl isobutyl ketone, di-isobutyl ketone and isoamyl alcohol) and two ligands (8-hydroxyquinoline and toluene-3,4-dithiol) were studied. The procedure were tested on pine needle and birch leaf samples.

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

    OpenAIRE

    Dietz, Christian; Sanz Landaluze, Jon; Ximenez Embun, Pilar; Madrid Albarrán, Yolanda; Cámara, Carmen

    2004-01-01

    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 MCcolumn were in-house developed and multicapillary column was operated at moderate temperatures (30–100 ◦C). The method was...

  13. Determination of nickel in biological materials after microwave dissolution using inductively coupled plasma atomic emission spectrometry with prior extraction into butan-1-ol.

    Science.gov (United States)

    Vereda Alonso, E; García de Torres, A; Cano Pavón, J M

    1992-07-01

    A sensitive procedure has been developed for the determination of ultratrace amounts of nickel in biological materials by inductively coupled plasma atomic emission spectrometry after extraction of the nickel ion into butan-1-ol by using 1,5-bis(di-2-pyridylmethylene)thiocarbonohydrazide as the extracting reagent. Fast, efficient and complete sample digestion is achieved by an HNO3-HCl poly(tetrafluoroethylene) bomb dissolution technique using microwave heating. Results obtained for eleven certified reference materials agreed with the certified values.

  14. Inductively Coupled Plasma(ICP) Mass Spectrometry(MS) Hyphenated with Atomic Emission Spectrometry(AES) for Simultaneous Determination of Major, Minor and Micro Amounts of Elements in Geochemical Samples

    Institute of Scientific and Technical Information of China (English)

    HUANG Zhen-yu; ZHANG Qin; HU Ke; WU Jian-ling; YANG Peng-yuan

    2005-01-01

    @@ Introduction Geological resource survey demands for determining various constituents including major, minor, micro, trace and ultra-trace levels of elements for preparing the map of resource distribution of our country. As a powerful and popularly used technique for multi-element analysis, inductively coupled plasma(ICP) atomic emission spectrometry (AES) has been applied to this field for a period of time[1-3]. However, ICP spectrometric determination of those micro, trace and ultratrace elements needs enrichment procedures for improving the detection limit, which is unacceptable in case a great mass of samples should be analyzed as that in the task of geological resource survey. On the other hand, although ICP mass spectrometry(MS) is considered the most powerful method for trace elements determination[4,5], it is difficult for ICP-MS to be used to determine the trace and major analytes simultaneously in a spectrum.

  15. Calibration graphs for Ti, Ta and Nb in sintered tungsten carbide by infrared laser ablation inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    Kanický, V; Otruba, V; Mermet, J M

    2001-12-01

    Infrared laser ablation (IR-LA) has been studied as a sample introduction technique for the analysis of sintered cobalt-cemented tungsten carbide materials by inductively coupled plasma atomic emission spectrometry (ICP-AES). Fractionation of cobalt was observed. Linearity of calibration plots was verified at least up to 15% Ti, 8% Ta, and 3% Nb. Above 1% (m/m) Ti, Ta, and Nb, the repeatability of results was better than 3% R.S.D. The relative uncertainty at the centroid of the calibration line was in the range from +/- 3% to +/- 4% for Ti, Ta, and Nb with internal standardization by tungsten and up to +/- 5% without internal standardization. The limits of detection were 0.004% Ti, 0.001% Ta, and 0.004% Nb. Elimination of the cemented hardmetal dissolution procedure is the main advantage of this method.

  16. 电感耦合等离子体-原子发射光谱法的应用%Application of Inductively Coupled Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    时亮; 隋欣

    2013-01-01

    The application of inductively coupled plasma-atomic emission spectrometry in animal and plant analysis, environmental analysis, metallurgical analysis, electric power production, food analysis, lithium niobate analysis, harmful heavy metals detection in toys, and the cultural relics protection, etc, were summarized.%  综述了利用电感耦合高频等离子体作为激发光源的原子发射光谱法在动植物分析、环境分析、冶金分析、电力生产、食品分析、铌酸锂分析、玩具中有害重金属测定及文物保护科学研究等方面中的应用。

  17. Resonant laser ablation of metals detected by atomic emission in a microwave plasma and by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Cleveland, Danielle; Stchur, Peter; Hou, Xiandeng; Yang, Karl X; Zhou, Jack; Michel, Robert G

    2005-12-01

    It has been shown that an increase in sensitivity and selectivity of detection of an analyte can be achieved by tuning the ablation laser wavelength to match that of a resonant gas-phase transition of that analyte. This has been termed resonant laser ablation (RLA). For a pulsed tunable nanosecond laser, the data presented here illustrate the resonant enhancement effect in pure copper and aluminum samples, chromium oxide thin films, and for trace molybdenum in stainless steel samples, and indicate two main characteristics of the RLA phenomenon. The first is that there is an increase in the number of atoms ablated from the surface. The second is that the bandwidth of the wavelength dependence of the ablation is on the order of 1 nm. The effect was found to be virtually identical whether the atoms were detected by use of a microwave-induced plasma with atomic emission detection, by an inductively coupled plasma with mass spectrometric detection, or by observation of the number of laser pulses required to penetrate through thin films. The data indicate that a distinct ablation laser wavelength dependence exists, probably initiated via resonant radiation trapping, and accompanied by collisional broadening. Desorption contributions through radiation trapping are substantiated by changes in crater morphology as a function of wavelength and by the relatively broad linewidth of the ablation laser wavelength scans, compared to gas-phase excitation spectra. Also, other experiments with thin films demonstrate the existence of a distinct laser-material interaction and suggest that a combination of desorption induced by electronic transition (DIET) with resonant radiation trapping could assist in the enhancement of desorption yields. These results were obtained by a detailed inspection of the effect of the wavelength of the ablation laser over a narrow range of energy densities that lie between the threshold of laser-induced desorption of species and the usual analytical

  18. 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...

  19. [Characterization of dinosaur fossils and their surrounding rocks by atomic emission spectrometry and X-ray powder diffractometry].

    Science.gov (United States)

    Yang, Qun; Wang, Yi-lin; Li, Chao-zhen; Yuan, Bo

    2005-02-01

    More dinosaur fossils have been found in the Laochangqing valley, Lufeng county than anywhere else in the world, and the dinosaur fossils found here cover the longest time span (including the early and middle Jurassic ages). This excavation offers an ideal experimental base for prehistoric biology studies. This paper presents an elementary analysis of the components and structure of the dinosaur fossils in three different geologic-layers and their surrounding rocks in the above mentioned area. Atomic emission spectrum shows that the fossils are rich in the contents of calcium (>5%) and phosphor, but low in the content of silicon (3%-8%), while the surrounding rocks are high in the content of silicon (>10%). Furthermore, XRD results show that the major compound of the fossils is CaCO3 (66%), followed by SiO2 (17%); while that of the surrounding rocks is SiO2 (>80%), followed by CaCO3 (dinosaur fossils from other rocks. This paper provides valuable data for further zoological studies on the living conditions and evolution of the dinosaurs in the Laochangqing valley, Lufeng county.

  20. Investigations on the on-line determination of metals in air flows by capacitively coupled microwave plasma atomic emission spectrometry

    Science.gov (United States)

    Seelig, M.; Broekaert, J. A. C.

    2001-09-01

    Plasma optical emission spectrometry with a capacitively coupled microwave plasma (CMP) operated with air has been investigated with respect to its possibilities for real-time environmental monitoring of combustion processes. The unique feature is the possibility to operate the CMP with air as working gas, as is usually the case in exhaust gases of combustion processes. The CMP also is shown to be stable in the presence of large amounts of water and CO 2, which makes this source ideally suitable for this purpose. The detection limits obtained for the environmentally relevant elements Cd, Co, Cr, Fe, Mg, Ni and Pb show the possibility to monitor directly heavy metals in air in an on-line mode and down to the 2-160-μg m -3 level. These detection limits are generally lower than the threshold limit values of the 'Federal Law for Immission Protection' in Germany in the gaseous effluents of industrial plants. In order to investigate the influence of the water loading (32-222 g m -3) on the detection limits a comparison of results obtained with three different nebulizers (Légère nebulizer, hydraulic high-pressure nebulizer and ultrasonic nebulizer) was made, with which aerosols with different water loading are entered into the plasma. For the hydraulic high-pressure nebulizer and the ultrasonic nebulizer no desolvation unit was found to be necessary. It was shown that especially for elements with lines having high excitation energy (Cd) or for which ion lines are used (Mg II) the increase in water loading deteriorates the detection limits. The rotational temperatures ( Trot) and excitation temperatures ( Texe) in the case of different amounts of water are of the order of 3700-4900 K and 4700-7100 K, respectively. The temperatures show that changes in the geometry and temperature distribution in the case of Trot but also the values of Texe themselves are responsible for this increase in detection limits. Furthermore, different amounts of CO 2 mixed to the working gas (3

  1. Application of microwave plasma atomic emission spectrometry (MP-AES) for environmental monitoring of industrially contaminated sites in Hyderabad city.

    Science.gov (United States)

    Kamala C T; Balaram V; Dharmendra V; Satyanarayanan M; Subramanyam K S V; Krishnaiah A

    2014-11-01

    Recently introduced microwave plasma-atomic emission spectroscopy (MP-AES) represents yet another and very important addition to the existing array of modern instrumental analytical techniques. In this study, an attempt is made to summarize the performance characteristics of MP-AES and its potential as an analytical tool for environmental studies with some practical examples from Patancheru and Uppal industrial sectors of Hyderabad city. A range of soil, sediment, water reference materials, particulate matter, and real-life samples were chosen to evaluate the performance of this new analytical technique. Analytical wavelengths were selected considering the interference effects of other concomitant elements present in different sample solutions. The detection limits for several elements were found to be in the range from 0.05 to 5 ng/g. The trace metals analyzed in both the sectors followed the topography with more pollution in the low-lying sites. The metal contents were found to be more in ground waters than surface waters. Since a decade, the pollutants are transfered from Patancheru industrial area to Musi River. After polluting Nakkavagu and turning huge tracts of agricultural lands barren besides making people residing along the rivulet impotent and sick, industrialists of Patancheru are shifting the effluents to downstream of Musi River through an 18-km pipeline from Patancheru. Since the effluent undergoes primary treatment at Common Effluent Treatment Plant (CETP) at Patanchru and travels through pipeline and mixes with sewage, the organic effluents will be diluted. But the inorganic pollutants such as heavy and toxic metals tend to accumulate in the environmental segments near and downstreams of Musi River. The data generated by MP-AES of toxic metals like Zn, Cu, and Cr in the ground and surface waters can only be attributed to pollution from Patancheru since no other sources are available to Musi River.

  2. The use of ion chromatography-dc plasma atomic emission spectrometry for the speciation of trace metals

    Energy Technology Data Exchange (ETDEWEB)

    Urasa, I.T.

    1991-09-20

    The original objects of this research program were: to interface d.c. plasma atomic emission spectrometer with an ion chromatograph; to characterize and optimize the combined systems for application in the speciation of metals in aqueous solutions; to use this system in the study of the solution chemistry of various metals; and to find ways in which the measurement sensitivity of the method can be enhanced, thereby allowing the detection of metal species at low ppb concentration levels. This approach has been used to study the chemistry of and speciate several elements in solution including: arsenic, chromium, iron, manganese, nickel phosphorus, platinum, selenium, and vanadium. During the course of this research, we have found that the solution chemistry of the elements studied and the speciation data obtained can vary considerably depending on the solution, and the chromatographic conditions employed. The speciation of chromium, iron, and vanadium was found to be highly influenced by the acidity of the sample. The element selective nature of the d.c. plasma detector allows these changes to be monitored, thereby providing quantitative information on the new moieties formed. New approaches are being developed including the use of chelating ligands as preconcentration agents for purposes of reducing further the detection limits of the elements of interest and to improve the overall element speciation scheme. New thrusts are being directed towards the employment of post-column derivatization method coupled with colorimetric measurements to detect and quantify metal species eluting from the chromatographic column. The influence of sample acidity on these investigations will be carefully evaluated. These new thrusts are described in the accompanying Project Renewal Proposal.

  3. 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.

  4. Slurry sampling fluorination assisted electrothermal vaporization-inductively coupled plasma-atomic emission spectrometry for the direct determination of metal impurities in aluminium oxide ceramic powders.

    Science.gov (United States)

    Peng, T; Chang, G; Wang, L; Jiang, Z; Hu, B

    2001-03-01

    A new analytical procedure for the direct determination of metal impurities (Cr, Cu, Fe and V) in aluminium oxide ceramic powders by slurry sampling fluorination assisted electrothermal vaporization-inductively coupled plasma-atomic emission spectrometry (ETV-ICP-AES) is reported. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating reagent to promote the vaporization of impurity elements in aluminium oxide ceramic powders from the graphite tube. A vaporization stage with a long ramp time and a short hold time provided the possibility of temporal analyte-matrix separation. The experimental results indicated that a 10 microL 1% m/v slurry of aluminium oxide could be destroyed and vaporized completely with 600 micrograms PTFE under the selected conditions. Two aluminium oxide ceramic powder samples were used without any additional pretreatment. Analytical results obtained by using standard addition method with aqueous standard solution were checked by comparison of the results with pneumatic nebulization (PN)-ICP-AES based on the wet-chemical decomposition and analyte-matrix separation. The limits of detection (LODs) between 0.30 microgram g-1 (Fe) and 0.08 microgram g-1 (Cu) were achieved, and, the repeatability of measurements was mainly better than 10%.

  5. 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).

  6. 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.

  7. Multielement determination of heavy metals in water samples by continuous powder introduction microwave-induced plasma atomic emission spectrometry after preconcentration on activated carbon

    Science.gov (United States)

    Jankowski, Krzysztof; Yao, Jun; Kasiura, Krzysztof; Jackowska, Adrianna; Sieradzka, Anna

    2005-03-01

    A novel continuous powder introduction microwave-induced plasma atomic emission spectrometry method (CPI-MIP-AES) has been developed for trace determination of metals in ground and tap water samples after preconcentration on activated carbon. The experimental setup consisted of integrated rectangular cavity TE 101 and vertically positioned plasma torch. The technical arrangement of the sample introduction system has been designed based on the fluidized bed concept. The satisfactory signal stability required for sequential analysis was attained owing to the vertical plasma configuration, as well as the plasma gas flow rate compatibility with sample introduction flow rate. The elements of interest (Cd, Cu, Cr, Fe, Mn, Pb, Zn) were preconcentrated in a batch procedure at pH 8-8.5 after addition of activated carbon and then, after filtering and drying of the activated carbon suspension, introduced to the MIP by the CPI system. An enrichment factor of about 1000-fold for a sample volume of 1 l was obtained. The detection limit values for the proposed method were 17-250 ng l -1. The proposed method was validated by analyzing the certified reference materials: SRW "Warta" Synthetic River Water and BCR CRM 399 major elements in freshwater. The method was successfully applied to the determination of the heavy metals in tap water samples.

  8. Multielement determination of heavy metals in water samples by continuous powder introduction microwave-induced plasma atomic emission spectrometry after preconcentration on activated carbon

    Energy Technology Data Exchange (ETDEWEB)

    Jankowski, Krzysztof [Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, 00-664 Warsaw, ul. Noakowskiego 3 (Poland)]. E-mail: kj@ch.pw.edu.pl; Yao Jun [College of Chemistry and Chemical Engineering, Jishou University, 120 Renmin South Road, Jishou 416000 (China); Kasiura, Krzysztof [Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, 00-664 Warsaw, ul. Noakowskiego 3 (Poland); Jackowska, Adrianna [Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, 00-664 Warsaw, ul. Noakowskiego 3 (Poland); Sieradzka, Anna [Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, 00-664 Warsaw, ul. Noakowskiego 3 (Poland)

    2005-03-31

    A novel continuous powder introduction microwave-induced plasma atomic emission spectrometry method (CPI-MIP-AES) has been developed for trace determination of metals in ground and tap water samples after preconcentration on activated carbon. The experimental setup consisted of integrated rectangular cavity TE{sub 101} and vertically positioned plasma torch. The technical arrangement of the sample introduction system has been designed based on the fluidized bed concept. The satisfactory signal stability required for sequential analysis was attained owing to the vertical plasma configuration, as well as the plasma gas flow rate compatibility with sample introduction flow rate. The elements of interest (Cd, Cu, Cr, Fe, Mn, Pb, Zn) were preconcentrated in a batch procedure at pH 8-8.5 after addition of activated carbon and then, after filtering and drying of the activated carbon suspension, introduced to the MIP by the CPI system. An enrichment factor of about 1000-fold for a sample volume of 1 l was obtained. The detection limit values for the proposed method were 17-250 ng l{sup -1}. The proposed method was validated by analyzing the certified reference materials: SRW 'Warta' Synthetic River Water and BCR CRM 399 major elements in freshwater. The method was successfully applied to the determination of the heavy metals in tap water samples.

  9. Element analysis and characteristic identification of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. using microwave digestion-inductively coupled plasma atomic emission spectrometry combined with Fourier transform infrared spectrometry

    Directory of Open Access Journals (Sweden)

    Yajing Lou

    2014-01-01

    Full Text Available Background: Sulfur-fumigation may induce chemical transformation of traditional Chinese medicines leading to harmful effects following patient ingestion. For quality control, it is urgently needed to develop a reliable and efficient method for sulfur-fumigation identification. Materials and Methods: The spectrochemical identification of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. was carried out to evaluate inorganic elements and organic components. The concentrations of 12 elements, including Zn, Mn, Cu, Fe, Li, Mg, Sr, Pb, As, Cd, Hg, and S of samples were determined by microwave digestion - inductively coupled plasma atomic emission spectrometry (ICP-AES. Meanwhile, Fourier transform infrared spectrometry (FTIR was used for the study of chemical group characteristic reactions after sulfur-fumigation. Results: The concentrations of Fe, Mg, Hg, and S elements showed significant differences between non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. The characteristic stretching vibrations of some groups in FTIR spectra, such as -OH, -S = O and -S-O, provided the identification basis for the discrimination of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. Conclusion: The application of microwave digestion - ICP-AES was successfully used in combination with FTIR to authenticate and evaluate the quality of medicinal Fritillaria thunbergii Miq. Further applications of this technique should be explored.

  10. A novel methodology for rapid digestion of rare earth element ores and determination by microwave plasma-atomic emission spectrometry and dynamic reaction cell-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Helmeczi, Erick; Wang, Yong; Brindle, Ian D

    2016-11-01

    Short-wavelength infrared radiation has been successfully applied to accelerate the acid digestion of refractory rare-earth ore samples. Determinations were achieved with microwave plasma-atomic emission spectrometry (MP-AES) and dynamic reaction cell - inductively coupled plasma-mass spectrometry (DRC-ICP-MS). The digestion method developed was able to tackle high iron-oxide and silicate matrices using only phosphoric acid in a time frame of only 8min, and did not require perchloric or hydrofluoric acid. Additionally, excellent recoveries and reproducibilities of the rare earth elements, as well as uranium and thorium, were achieved. Digestions of the certified reference materials OREAS-465 and REE-1, with radically different mineralogies, delivered results that mirror those obtained by fusion processes. For the rare-earth CRM OKA-2, whose REE data are provisional, experimental data for the rare-earth elements were generally higher than the provisional values, often exceeding z-values of +2. Determined values for Th and U in this reference material, for which certified values are available, were in excellent agreement.

  11. Separation and preconcentration of ultra trace amounts of beryllium in water samples using mixed micelle-mediated extraction and determination by inductively coupled plasma-atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Beiraghi, Assadollah [Faculty of Chemistry, Tarbiat Moallem University, Mofatteh Avenue, No. 49, P.O. Box 15614, Tehran (Iran, Islamic Republic of)], E-mail: Beiraghi@Saba.tmu.ac.ir; Babaee, Saeed [Faculty of Chemistry, Tarbiat Moallem University, Mofatteh Avenue, No. 49, P.O. Box 15614, Tehran (Iran, Islamic Republic of)

    2008-01-28

    In the present study a cloud point extraction process using mixed micelle of the cationic surfactant cetyl-pyridinium chloride (CPC) and non-ionic surfactant Triton X-114 for extraction of beryllium from aqueous solutions is developed. The extraction of analyte from aqueous samples was performed in the presence of 1,8-dihydroxyanthrone as chelating agent in buffer media of pH 9.5. After phase separation, the surfactant-rich phase was diluted with 0.4 mL of a 60:40 methanol-water mixture containing 0.03 mL HNO{sub 3}. Then, the enriched analyte in the surfactant-rich phase was determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The different variables affecting the complexation and extraction conditions were optimized. Under the optimum conditions (i.e. 1.6 x 10{sup -4} mol L{sup -1} 1,8-dihydroxyanthrone, 1.2 x 10{sup -4} mol L{sup -1} CPC, 0.15% (v/v) Triton X-114, 50 deg. C equilibrium temperature) the calibration graph was linear in the range of 0.006-80 ng mL{sup -1} with detection limit of 0.001 ng mL{sup -1} and the precision (R.S.D.%) for five replicate determinations at 18 ng mL{sup -1} of Be(II) was better than 2.9%. In this manner the preconcentration and enrichment factors were 16.7 and 24.8, respectively. Under the presence of foreign ions no significant interference was observed. Finally, the proposed method was successfully utilized for the determination of this cation in water samples.

  12. Ultrasound bath-assisted enzymatic hydrolysis procedures as sample pretreatment for the multielement determination in mussels by inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    Peña-Farfal, Carlos; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Adela; Bermejo-Barrera, Pilar; Pinochet-Cancino, Hugo; de Gregori-Henríquez, Ida

    2004-07-01

    Ultrasound energy has been applied to speed up enzymatic hydrolysis processes of mussel tissue in order to determine trace and ultratrace elements (As, Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn). The element releases, by action of three proteases (pepsin, pancreatin, trypsin), lipase, and alpha-amylase, have been evaluated by inductively coupled plasma atomic emission spectrometry. Different variables such as pH, sonication temperature, ionic strength, hydrolysis time, ultrasound frequency, extracting volume, and enzyme mass were simultaneously studied by applying an experimental design approach (Plackett-Burman design and central composite design). Results showed that the hydrolysis time was statistically nonsignificant (confidence interval of 95%) for most of the elements and enzymes, meaning that the hydrolysis procedure can be finished within a 30-60-min range. These hydrolysis times are far shorter than those obtained when using thermostatic cameras, between 12 and 24 h. Statistically significant factors were the ultrasound frequency (the highest metals releasing at high-ultrasound frequency), pH, sonication temperature, and ionic strength. All metals can be extracted using the same operating conditions (pH of 1.0 and sodium chloride at 1.0% for pepsin; pH of 7.5, temperature at 37 degrees C, and 0.4 M potassium dihydrogen phosphate/potassium hydrogen phosphate buffer for amylase; pH of 8.0 and 0.5 M potassium dihydrogen phosphate/potassium hydrogen phosphate buffer for pancreatin; pH of 5.0 and 0.5 M potassium dihydrogen phosphate/potassium hydrogen phosphate buffer for lipase; pH of 8.0 and 0.2 M potassium dihydrogen phosphate/potassium hydrogen phosphate buffer for trypsin). Analytical performances, such as limits of detection and quantification, repeatability of the overall procedure, and accuracy, by analyzing DORM-1, DORM-2, and TORT-1 certified reference materials, were finally assessed for each enzyme.

  13. 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)

  14. Separation and preconcentration of ultra trace amounts of beryllium in water samples using mixed micelle-mediated extraction and determination by inductively coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Beiraghi, Assadollah; Babaee, Saeed

    2008-01-28

    In the present study a cloud point extraction process using mixed micelle of the cationic surfactant cetyl-pyridinium chloride (CPC) and non-ionic surfactant Triton X-114 for extraction of beryllium from aqueous solutions is developed. The extraction of analyte from aqueous samples was performed in the presence of 1,8-dihydroxyanthrone as chelating agent in buffer media of pH 9.5. After phase separation, the surfactant-rich phase was diluted with 0.4mL of a 60:40 methanol-water mixture containing 0.03 mL HNO(3). Then, the enriched analyte in the surfactant-rich phase was determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The different variables affecting the complexation and extraction conditions were optimized. Under the optimum conditions (i.e. 1.6 x 10(-4) molL(-1) 1,8-dihydroxyanthrone, 1.2 x 10(-4) molL(-1) CPC, 0.15% (v/v) Triton X-114, 50 degrees C equilibrium temperature) the calibration graph was linear in the range of 0.006-80 ngmL(-1) with detection limit of 0.001 ngmL(-1) and the precision (R.S.D.%) for five replicate determinations at 18 ngmL(-1) of Be(II) was better than 2.9%. In this manner the preconcentration and enrichment factors were 16.7 and 24.8, respectively. Under the presence of foreign ions no significant interference was observed. Finally, the proposed method was successfully utilized for the determination of this cation in water samples.

  15. 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.

  16. On-line cloud point extraction combined with electrothermal vaporization inductively coupled plasma atomic emission spectrometry for the speciation of inorganic antimony in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)]. E-mail: binhu@whu.edu.cn; Jiang Zucheng [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2006-08-25

    A new method for the determination of inorganic Sb species by on-line cloud point extraction combined with electrothermal vaporization inductively coupled plasma atomic emission spectrometry (ETV-ICP-AES) is presented and evaluated. The method is based on the complexation of Sb(III) with pyrrolidine dithiocarbamate (PDC) which form an hydrophobic complex at pH 5.5 and subsequently enter surfactant-rich phase at pH 5.5, whereas Sb(V) remained in aqueous solutions. The preconcentration step is mediated by micelles of the non-ionic surfactant Triton X-114 with ammonium pyrrolidine dithiocarbamate (APDC). The micellar system containing the complex was loaded into the FIA manifold at a flow rate of 2.5 mL min{sup -1}, and the surfactant-rich phase was retained in a microcolumn packed with absorbent cotton, at pH 5.5. After the surfactant-rich phase was eluted with 100 {mu}L acetonitrile, it was determined by ETV-ICP-AES. Sb(V) is reduced to Sb(III) by L-cysteine prior to determined total Sb, and its assay is based on subtracting Sb(III) from total antimony. The main factors affecting separation/preconcentration and the vaporization behavior of analyte in graphite tube were investigated in detail. Under the optimized conditions, the precision relative standard deviation (R.S.D.) for eight replicate measurements of 0.2 {mu}g mL{sup -1} Sb(III) was 4.3%. The apparent concentration factor, which is defined as the concentration ratio of the analyte in the final diluted surfactant-rich extract ready for ETV-ICP-AES detection and in the initial solution, was 872 for Sb(III). The limit of detection (LOD) for Sb(III) was 0.09 {mu}g L{sup -1}. The proposed method was successfully applied for the speciation of inorganic antimony in different water samples and urine sample with satisfactory results.

  17. 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

  18. The rewards of fundamental atomic spectrometry research.

    Science.gov (United States)

    Slavin, W

    2000-04-01

    Atomic spectrometry research is the life-blood of the atomic spectrometry instrument industry. The instrument designer can be expected to innovate in the execution of instrumentation and should be expected to be the expert in optical, electronic and software engineering. Fundamentally new technology has required too long a period of gestation to be compatible with commercial time scales and budgets. But in the past decade, the pressure from stockholders for increased return on investments has put increasingly strong pressure on management to reduce expenses and focus increasingly on projects that guarantee a fast payback. This pressure falls particularly heavily on the larger companies; the same companies that a decade or more ago were the ones that brought the more far-reaching and expensive new concepts to market. Fundamental research in atomic spectrometry has been accomplished in the past several decades mostly in the academic environment and in research institutions that are Federally funded. All of the Federally funded research institutions have been forced to alter their missions to more tangible and immediate goals, and many have also seen severe financial reductions.

  19. The Rewards of Fundamental Atomic Spectrometry Research

    Institute of Scientific and Technical Information of China (English)

    Walter Slavin

    2000-01-01

    Atomic spectrometry research is the life-blood of the atomic spectrometry instrument industry.The instrument designer can be expected to innovate in the execution of instrumentation and should be expected to be the expert in optical,electronic and software engineering.Fundamentally new technology has required too long a period of gestation to be compatible with commercial time scales and budgets.But in the past decade,the pressure from stockholders for increased return on investments has put increasingly strong pressure on management to reduce expenses and focus increasingly on projects that guarantee a fast payback.This pressure falls particularly heavily on the larger companies;the same companies that a decade or more ago were the ones that brought the more far-reaching and expensive new concepts to market. Fundamental research in atomic spectrometry has been accomplished in the past several decades mostly in the academic environment and in research institutions that are Federally funded.All of the Federally funded research institutions have been forced to alter their missions to more tangible and immediate goals,and many have also seen severe financial reductions.

  20. Evaluation of analyte additions method for sodium determination in fuel ethanol by flame atomic emission spectrometry; Avaliacao do metodo das adicoes de analito para a determinacao de sodio em alcool combustivel por espectrometria de emissao atomica em chama

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Adriana Paiva de; Okumura, Leonardo Luiz; Gomes Neto, Jose Anchieta [UNESP, Araraquara, SP (Brazil). Inst. de Quimica. Dept. de Quimica Analitica

    2002-07-01

    The analyte additions method was applied for sodium determination in fuel ethanol by atomic emission spectrometry. Graphics involving emission intensity versus analyte concentration in the 0 - 0.300 mg Na L{sup -1} interval concentration range containing 2.1 g K L{sup -1} as an ionisation buffer. Twenty samples of commercial fuel ethanol were collected in different gas stations located in Araraquara city, analyzed and results obtained varied from 0.0072 to 1.55 mg Na L{sup -1}. The limits of detection (L.O.D.) varied from 0.0026 to 0.0239 mg Na L{sup -1}. Recoveries varied in the 95 - 104 % interval. The relative standard deviations (n=12) for three analyte additions in all samples were {<=}4,1 %. (author)

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

    Directory of Open Access Journals (Sweden)

    Iracema Takase

    2002-12-01

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

  2. Purge-and-trap isothermal multicapillary gas chromatographic sample introduction accessory for speciation of mercury by microwave-induced plasma atomic emission spectrometry.

    Science.gov (United States)

    Rodriguez Pereiro, I; Wasik, A; Lobiński, R

    1998-10-01

    A compact device based on purge-and-trap multicapillary gas chromatography was developed for sensitive species-selective analysis of methylmercury and Hg2+ by atomic spectrometry. The operating mode includes in situ conversion of the analyte species to MeEtHg and HgEt2 and cryotrapping of the derivatives formed in a 0.53-mm-i.d. capillary, followed by their flash ( 60 mL min-1) compatible with an MIP AES detector (no dilution with a makeup gas is required). Developments regarding each of the steps of the analytical procedure and effects of operational variables (sample volume, purge flow, trap temperature, separation conditions) are discussed. The device allows speciation of MeHg+ and Hg2+ down to 5 pg g-1 in urine and, after a rapid microwave-assisted hydrolysis, down to 0.1 ng g-1 in solid biological samples with a throughput of 6 samples/h. The analytical protocols developed were validated by the analysis of DORM-1 (dogfish muscle), TORT-1 (lobster hepatopancreas), and Seronorm urine certified reference materials.

  3. Development of open-air type electrolyte-as-cathode glow discharge-atomic emission spectrometry for determination of trace metals in water

    Science.gov (United States)

    Kim, Hyo J.; Lee, Jeong H.; Kim, Myung Y.; Cserfalvi, T.; Mezei, P.

    2000-07-01

    The open-air type electrolyte cathode atomic glow discharge (ELCAD) has been developed and studied for fundamental and analytical applications for determination of trace heavy metals in water. The normal closed-type discharge cell shows some problems such as unstable plasma due to changes in the pressure inside the cell during the discharge, and water vapor condensing onto the window. Applying approximately 1500 V to the several-millimeter gap between the electrolyte solution cathode and a Pt rod anode in atmospheric air pressure produced a stable plasma and significantly improved sensitivity. The emission spectrum of de-ionized water containing 100 mg/l Cu was measured and some emission lines were found from Cu I (324.7 nm, 327.4 nm and 510.5 nm) and Cu II (224.7 nm and 229.4 nm). The LODs of Cr, Cu, Fe, Mn, Ni, Pb, and Zn are in the ranges from 0.01 mg/l to 0.6 mg/l. The LODs of Cu, Mn, Pb and Zn improve by approximately one order of magnitude compared to the previous closed-type ELCAD.

  4. 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.

  5. 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

    Science.gov (United States)

    Holá, Markéta; Otruba, Vítězslav; Kanický, Viktor

    2006-05-01

    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

  6. 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

  7. 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}.

  8. High-temperature liquid chromatography inductively coupled plasma atomic emission spectrometry hyphenation for the combined organic and inorganic analysis of foodstuffs.

    Science.gov (United States)

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

    2010-10-01

    The coupling of a High-Temperature Liquid Chromatography system (HTLC) with an Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES) is reported for the first time. This hyphenation combines the separation efficiency of HTLC with the detection power of a simultaneous ICP-AES system and allows the combined determination of organic compound and metals. The effluents of the column were introduced into the spectrometer and the chromatograms for organic compounds were obtained by plotting the carbon emission signal at a characteristic wavelength versus time. As regards metals, they were determined by injecting a small sample volume between the exit of the column and the spectrometer and taking the emission intensity for each one of the elements simultaneously. Provided that in HTLC the effluents emerged at high temperatures, an aerosol was easily generated at the exit of the column. Therefore, the use of a pneumatic nebulizer as a component of a liquid sample introduction system in the ICP-AES could be avoided, thus reducing the peak dispersion and limits of detection by a factor of two. The fact that a hot liquid stream was nebulized made it necessary to use a thermostated spray chamber so as to avoid the plasma cooling as a cause of the excessive mass of solvent delivered to it. Due to the similarity in sample introduction, an Evaporative Light Scattering Detector (ELSD) was taken as a reference. Comparatively speaking, limits of detection were of the same order for both HTLC-ICP-AES and HTLC-ELSD, although the latter provided better results for some compounds (from 10 to 20 mg L(-1) and 5-10 mg L(-1), respectively). In contrast, the dynamic range for the new hyphenation was about two orders of magnitude wider. More importantly, HTLC-ICP-AES provided information about the content of both organic (glucose, sucrose, maltose and lactose at concentrations from roughly 10 to 400 mg L(-1)) as well as inorganic (magnesium, calcium, sodium, zinc, potassium and

  9. Simultaneous determination of some trace metal impurities in high-purity sodium tungstate using coprecipitation and inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoguo; KUANG Tongchun; LIU Qianjun

    2004-01-01

    A method based on the combination of coprecipitation with inductively coupled plasma atomic emission spec trometry (ICP-AES) was developed for the determination of impurities in high-purity sodium tungstate. Six elements (Co,Cu, Fe, Mn, Ni, and Pb) were coprecipitated by lanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of some factors on the recoveries of the analytes and on the residual amount of sodium tungstate were investigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matching calibration curve method was used for the analysis. It is shown that the elements mentioned above can be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4, 0.2, 0.1, 0.6, and 1.3 μg.g-1, respectively. The recoveries vary from 92.5% to 108%, and the relative standard deviations (RSDs) are in the range of 3.1%-5.5%.

  10. 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.

  11. The use of ion chromatography-dc plasma atomic emission spectrometry for the speciation of trace metals. Annual performance report, February 1, 1989--January 31, 1992

    Energy Technology Data Exchange (ETDEWEB)

    Urasa, I.T.

    1991-09-20

    The original objects of this research program were: to interface d.c. plasma atomic emission spectrometer with an ion chromatograph; to characterize and optimize the combined systems for application in the speciation of metals in aqueous solutions; to use this system in the study of the solution chemistry of various metals; and to find ways in which the measurement sensitivity of the method can be enhanced, thereby allowing the detection of metal species at low ppb concentration levels. This approach has been used to study the chemistry of and speciate several elements in solution including: arsenic, chromium, iron, manganese, nickel phosphorus, platinum, selenium, and vanadium. During the course of this research, we have found that the solution chemistry of the elements studied and the speciation data obtained can vary considerably depending on the solution, and the chromatographic conditions employed. The speciation of chromium, iron, and vanadium was found to be highly influenced by the acidity of the sample. The element selective nature of the d.c. plasma detector allows these changes to be monitored, thereby providing quantitative information on the new moieties formed. New approaches are being developed including the use of chelating ligands as preconcentration agents for purposes of reducing further the detection limits of the elements of interest and to improve the overall element speciation scheme. New thrusts are being directed towards the employment of post-column derivatization method coupled with colorimetric measurements to detect and quantify metal species eluting from the chromatographic column. The influence of sample acidity on these investigations will be carefully evaluated. These new thrusts are described in the accompanying Project Renewal Proposal.

  12. An analytical method for hydrogeochemical surveys: Inductively coupled plasma-atomic emission spectrometry after using enrichment coprecipitation with cobalt and ammonium pyrrolidine dithiocarbamate

    Science.gov (United States)

    Hopkins, D.M.

    1991-01-01

    Trace metals that are commonly associated with mineralization were concentrated and separated from natural water by coprecipitation with ammonium pyrollidine dithiocarbamate (APDC) and cobalt and determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The method is useful in hydrogeochemical surveys because it permits preconcentration near the sample sites, and selected metals are preserved shortly after the samples are collected. The procedure is relatively simple: (1) a liter of water is filtered; (2) the pH is adjusted; (3) Co chloride and APDC are added to coprecipitate the trace metals; and (4) later, the precipitate is filtered, dissolved, and diluted to 10 ml for a 100-fold concentration enrichment of the separated metals. Sb(III), As(III), Cd, Cr, Cu, Fe, Pb, Mo, Ni, Ag, V, and Zn can then be determined simultaneously by ICP-AES. In an experiment designed to measure the coprecipitation efficiency, Sb(III), Cd and Ag were recovered at 70 to 75% of their original concentration. The remaining metals were recovered at 85 to 100% of their original concentrations, however. The range for the lower limits of determination for the metals after preconcentration is 0.1 to 3.0 ??g/l. The precision of the method was evaluated by replicate analyses of a Colorado creek water and two simulated water samples. The accuracy of the method was estimated using a water reference standard (SRM 1643a) certified by the U.S. National Bureau of Standards. In addition, the method was evaluated by analyzing groundwater samples collected near a porphyry copper deposit in Arizona and by analyzing meltwater from glacier-covered areas favorable for mineralization in south-central Alaska. The results for the ICP-AES analyses compared favorably with those obtained using the sequential technique of GFAAS on the acidified but unconcentrated water samples. ICP-AES analysis of trace-metal preconcentrates for hydrogeochemical surveys is more efficient than GFAAS because a

  13. 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

  14. Determination of borax in yuba by inductively coupled plasma atomic emission spectrometry with microwave digestion%微波消解-等离子体发射光谱法测定腐竹中硼砂

    Institute of Scientific and Technical Information of China (English)

    黄子伟; 王世平; 汤大鹏

    2012-01-01

    The dielectric assisted microwave digestion conditions were selected by orthogonal design, the experimental design was used to investigate the effect of four parameters: microwave power, mixed acid ratio, mixed acid volume and digestion time. And the borax in Yuba was determination with Inductively Coupled Plasma Atomic Emission Spectrometry after microwave digestion. The detection limit of the method was 0.4 mg/kg, the recoveries were in the rang of 91.2%~103.9%, and relative standard deviations were less than 2%.%采用正交试验设计优化介质辅助微波消解样品的条件,以电感耦合等离子体发射光谱法(ICP-AES)测定腐竹中硼砂。考察了微波消解功率、混合酸的比例、混合酸用量、试样消解时间4个因素在不同水平条件下对仪器响应值的影响。在优化了微波消解条件下测定实际样品,方法检出限为0.4mg/kg,加标回收率为91.2%~103.9%,相对标准偏差〈2%。

  15. ICP-AES法测定土壤中的钾、锌、钒和钴%Determination of Potassium,Zinc,Vanadium,and Cobalt in Soil by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES)

    Institute of Scientific and Technical Information of China (English)

    张继华; 张加萍

    2014-01-01

    Hydrochloric acid,nitric acid,hydrofluoric acid,and perchloric acid were applied to digest heavy met-als in soil sample.Inductively coupled plasma-atomic emission spectrometry (ICP-AES)method was employed to determine the contents of potassium,zinc,vanadium,and cobalt.The precision of this method to these four heavy metals was 3.09%for potassium,4.14%for zinc,3.76%for vanadium,and 3.85%for cobalt respective-ly.Generally,this method is simple and quick with wide linear range and few distractions.%采用盐酸-硝酸-氢氟酸-高氯酸全分解的方法消解,在选定的条件下以ICP-AES测定溶液中的K、Zn 、V 和Co含量,对国家标准物进行测定,方法精密度(RSD,n=16)为K 3.09%、Zn 4.14%、V 3.76%、Co3.85%。该方法具有线性范围宽、干扰少、快速、简便等优点,用于实样分析,结果令人满意。

  16. Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    Holá, Markéta; Kanický, Viktor; Mermet, Jean-Michel; Otruba, Vítezslav

    2003-12-01

    The potential of the laser-induced argon spark atomizer (LINA-Spark atomizer) coupled with ICP-AES as a convenient device for direct analysis of WC/Co powdered precursors of sintered hardmetals was studied. The samples were presented for the ablation as pressed pellets prepared by mixing with powdered silver binder containing GeO2 as internal standard. The pellets were ablated with the aid of a Q-switched Nd:YAG laser (1064 nm) focused 16 mm behind the target surface with a resulting estimated power density of 5 GW cm(-2). Laser ablation ICP-AES signals were studied as a function of ablation time, and the duration of time prior to measurement (pre-ablation time) which was necessary to obtain reliable results was about 40 s. Linear calibration plots were obtained up to 10% (m/m) Ti, 9% Ta and 3.5% Nb both without internal standardization and by using germanium as an added internal standard or tungsten as a contained internal standard. The relative uncertainty at the centroid of the calibration line was in the range from +/- 6% to +/- 11% for Nb, Ta and Ti both with and without internal standardisation by Ge. A higher spread of points about the regression was observed for cobalt for which the relative uncertainty at the centroid was in the range from +/- 9% to +/- 14%. Repeatability of results was improved by the use of both Ge and W internal standards. The lowest determinable quantities calculated for calibration plots were 0.060% Co, 0.010% Nb, 0.16% Ta and 0.030% Ti with internal standardization by Ge. The LA-ICP-AES analyses of real samples led to good agreement with the results obtained by solution-based ICP determination with a relative bias not exceeding 10%. The elimination of the dissolution procedure of powdered tungsten (Nb, Ta, Ti) carbide is the principal advantage of the developed LA-ICP-AES method.

  17. Sequential-injection on-line preconcentration using chitosan resin functionalized with 2-amino-5-hydroxy benzoic acid for the determination of trace elements in environmental water samples by inductively coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Sabarudin, Akhmad; Lenghor, Narong; Oshima, Mitsuko; Hakim, Lukman; Takayanagi, Toshio; Gao, Yun-Hua; Motomizu, Shoji

    2007-07-31

    A new chelating resin using chitosan as a base material was synthesized. Functional moiety of 2-amino-5-hydroxy benzoic acid (AHBA) was chemically bonded to the amino group of cross-linked chitosan (CCTS) through the arm of chloromethyloxirane (CCTS-AHBA resin). Several elements, such as Ag, Be, Cd, Co, Cu, Ni, Pb, U, V, and rare earth elements (REEs), could be adsorbed on the resin. To use the resin for on-line pretreatment, the resin was packed in a mini-column and installed into a sequential-injection/automated pretreatment system (Auto-Pret System) coupled with inductively coupled plasma-atomic emission spectrometry (ICP-AES). The sequential-injection/automated pretreatment system was a laboratory-assembled, and the program was written using Visual Basic software. This system can provide easy operation procedures, less reagent consumption, as well as less waste production. Experimental variables considered as effective factors in the improvement sensitivity, such as an eluent concentration, a sample and an eluent flow rate, pH of samples, and air-sandwiched eluent were carefully optimized. The proposed system provides excellent on-line collection efficiency, as well as high concentration factors of analytes in water samples, which results in highly sensitive detection of ultra-trace and trace analysis. Under the optimal conditions, the detection limits of 24 elements examined are in the range from ppt to sub-ppb levels. The proposed method was validated by using the standard reference material of a river water, SLRS-4, and the applicability was further demonstrated to the on-line collection/concentration of trace elements, such as Ag, Be, Cd, Co, Cu, Ni, Pb, U, V, and REEs in water samples.

  18. Determination of La,Mg in Co-based alloys by inductively coupled plasma atomic emission spectrometry%ICP-AES法测定钴基合金中La、Mg元素的含量

    Institute of Scientific and Technical Information of China (English)

    高颂; 庞晓辉; 许维兵

    2014-01-01

    A method for determination of principal elements lanthanum and magnesium in Co-based al-loys by inductively coupled plasma atomic emission spectrometry is proposed .In this method ,the micro-wave digestion is used to reduce the background .Matrix-matching method is used to eliminated spectral interference .The experiments of instrument parameters ,sample dissolution ,selection of analysis lines , and the effect of matrix on the determination ,and the comparison of reference materials and the analytical results are carried out .T he recovery rate is at the range of 90%-99% ,RSD≤4% .%研究了钴基合金样品的溶解方法,采用盐酸、硝酸、氢氟酸溶解,使用微波消解溶解方法,控制试剂用量,降低了空白;考察了基体和主量元素对待测元素的影响,选择待测元素灵敏度高、光谱干扰少的谱线 La 408.672nm、Mg 279.553nm为分析线,校准曲线溶液采用基体匹配消除了基体效应影响,实现了用电感耦合等离子体原子发射光谱法测定钴基合金中La、Mg元素含量,方法的检出限可达0.002μg/mL ,进行了标准物质对照试验,与标准值相符,进行了加入回收试验,回收率90~99%,RSD<4%。

  19. 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.

    Science.gov (United States)

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

    2014-09-01

    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 between the summation of leached concentrations of TE in gastric juice plus the residual fraction and the total concentration of the overall assayed metals determined by microwave digestion. These results showed the reliability and lack of bias (trueness) of the automatic biomimetic extraction approach using digestive juices.

  20. 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 an

  1. A Thermo-Chemical Reactor for analytical atomic spectrometry

    Science.gov (United States)

    Gilmutdinov, A. Kh.; Nagulin, K. Yu.

    2009-01-01

    A novel atomization/vaporization system for analytical atomic spectrometry is developed. It consists of two electrically and thermally separated parts that can be heated separately. Unlike conventional electrothermal atomizers in which atomization occurs immediately above the vaporization site and at the same instant of time, the proposed system allows analyte atomization via an intermediate stage of fractional condensation as a two stage process: Vaporization → Condensation → Atomization. The condensation step is selective since vaporized matrix constituents are mainly non-condensable gases and leave the system by diffusion while analyte species are trapped on the cold surface of a condenser. This kind of sample distillation keeps all the advantages of traditional electrothermal atomization and allows significant reduction of matrix interferences. Integration into one design a vaporizer, condenser and atomizer gives much more flexibility for in situ sample treatment and thus the system is called a Thermo-Chemical Reactor (TCR). Details of the design, temperature measurements, vaporization-condensation-atomization mechanisms of various elements in variety of matrices are investigated in the TCR with spectral, temporal and spatial resolution. The ability of the TCR to significantly reduce interferences and to conduct sample pyrolysis at much higher temperatures as compared to conventional electrothermal atomizers is demonstrated. The analytical potential of the system is shown when atomic absorption determination of Cd and Pb in citrus leaves and milk powder without the use of any chemical modification.

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

    OpenAIRE

    Marschner, K; Musil, S. (Stanislav); Dědina, J. (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 NaBH4 in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were ...

  3. Study on Atomic Fluorescence Spectrometry Excited by Synchrotron Radiation

    Institute of Scientific and Technical Information of China (English)

    Jia-jia Guo; Wu-er Gan; Guo-bin Zhang; Qing-de Su

    2008-01-01

    A novel analysis approach using atomic fluorescence excited by synchrotron radiation is presented. A system for synchrotron radiation-atomic fluorescence spectrometry is developed, and experimental conditions such as flow rate, analyte acidity, concentration of pre-reducing and hydrogenation system are optimized. The proposed method is successfully applied to get an excitation spectrum of arsenic. Seven of ten primary spectral lines, four of which have never been reported by means of atomic fluorescence spectrometry, agree well with the existing reports. The other three are proposed for the first time. Excitation potentials and possible transitions are investigated. Especially for the prominent line at 234.99 nm, the mechanism of generation is discussed and a model of energy transition processes is proposed.

  4. 电感耦合等离子体原子发射光谱法测定炼锑泡渣中碲%Determination of tellurium in refined antimony slag by inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    张忠亭; 邓飞跃; 蒋苏琼; 刘逸群; 李彪

    2011-01-01

    建立了用电感耦合等离子体原子发射光谱法(ICP-AES)测定炼锑泡渣中碲的方法.选择波长为214.281 nm的谱线作为碲的分析线,只有La 214.281 nm,V 214.274 nm,Pt214.250 nm,Nb 214.291 nm和Re 214.297 nm线有干扰,但炼锑泡渣中La、V、Pt、Nb、Re含量都很低,其影响可以忽略,因此不需要进行预分离,样品用王水溶解后可直接进行ICP-AES测定.考察了仪器工作参数对测定结果的影响,并确定了最佳工作条件:观测高度为15 mm,雾化气流速为0.8 L/min,射频功率为1 300 W.方法线性范围为0.01~100 mg/L,线性相关系数为1.000 0,检出限(3σ)为0.007 2 mg/L,样品测定结果的相对标准偏差(RSD)为0.16%,加标回收率为97%~102%.%The determination method of tellurium in refined antimony slag by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The spectral line of 214. 281 nm was used as the analytical line of tellurium. Only La 214. 281 nm, V 214. 274 nm, Pt 214. 250 nm, Nb 214. 291 nm and Re 214. 297 nm lines had interference. However, the content of La, V, Pt, Nb and Re in refined antimony slag were very low, so their influence could be ignored and the pre-separation was not necessary. After dissolving with aqua regia, the sample solution was directly determined by ICP-AES. The effect of instrumental working parameters on determination results was investigated. The optimal working conditions were as follows: observation height, 15 mm; flow rate of atomizing gas, 0.8 L/min; radio frequency power, 1 300 W. The linear range of method was 0. 01-100 mg/L with correlation coefficient of 1. 000 0. The detection limit (3a) was 0. 007 2 mg/L. The relative standard deviation (RSD) was 0. 16 %, and the recoveries of standard addition were 97 %-102 %.

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

    Science.gov (United States)

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

    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(NO3)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 microg 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).

  6. 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)

  7. Spontaneous emission of two interacting atoms near an interface

    Institute of Scientific and Technical Information of China (English)

    Dehua Wang

    2009-01-01

    The spontaneous emission rate of two interacting excited atoms near a dielectric interface is studied using the photon closed-orbit theory and the dipole image method.The total emission rate of one atom during the emission process is calculated as a function of the distance between the atom and the interface.The results suggest that the spontaneous emission rate depends not only on the atomic-interface distances,but also on the orientation of the two atomic dipoles and the initial distance between the two atoms.The oscillation in the spontaneous emission rate is caused by the interference between the outgoing electromagnetic wave emitted from one atom and other waves arriving at this atom after traveling along various classical orbits.Each peak in the Fourier transformed spontaneous emission rate corresponds with one action of photon classical orbit.

  8. 电感耦合等离子体发射光谱法测定油田水中的硼%Determination of Boron in Oil Field Water by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    宋继芳

    2012-01-01

    样品经硝酸酸化、滤膜过滤处理后,用电感耦合等离子体发射光谱法直接测定其中硼的含量.通过正交实验优选仪器参数和分析谱线,在选定的波长208.959nm下,对样品稀释倍数和介质酸种类进行选择,结果表明,硼含量低于10mg/L的样品不用稀释,高于10mg/L的样品一般稀释20倍,介质选用硝酸可使测定结果更加准确.对油田水中共存的7种主要金属元素进行了干扰试验,样品中存在20mg/L的Sr、Ba、Fe,50mg/L的Mg、Ca,100mg/L的K,200mg/L的Na对待测元素的测定没有影响.选取油田水样品进行加标回收试验,方法平均回收率为95.3%~102.0%,精密度(RSD,n=11)为0.43%~0.92%,检出限为0.0020mg/L.方法简便、快速,结果令人满意,与姜黄素分光光度法比较,克服了分析流程长、使用试剂较多且不易操作的不足.%Boron in oil field water has been directly determined by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) after sample were treated with nitric acid and filtrated. This method overcomes the problems of spectrophotometry such as long analysis flow, more reagent and difficulty in controlling the chemical procedure. The working parameters and the spectral line were optimized by orthogonal tests. The dilute multiple and acid medium were analyzed using the selected 208.959 nm frequency. The results show that it is not necessary to dilute the sample when the content of B is less than 10 mg/L, and the dilution factor is 20 when B is greater than 10 mg/L. The selected HNO3 as the acid medium, improved the accuracy of the results. The interference tests were carried out for 7 major metals in oil field water. 20 mg/L Sr, Ba and Fe, 50 mg/L Mg and Ca, 100 mg/L K and 200 mg/L Na have no interference for the measurements of the target element. The detection limit of boron was 0.0020 mg/L and the recoveries ranged from 95.3% to 102.0% with a precision in the range of 0.43% - 0.92% ( RSD, n = 11

  9. Emission Probability of the Cascade Three-Level-Atom Mazer with Injected Atomic Coherence

    Institute of Scientific and Technical Information of China (English)

    熊锦; 张智明

    2002-01-01

    We investigate the effects of the injected atomic coherence on the atomic emission probability of the micromaser injected with ultracold cascade three-level atoms by considering that the atoms are initially in the coherent superposition states of the two upper levels. We show that there is no interference between the transitions from the two upper levels to the lowest level. In the large atom-field-detuning case, the atomic emission probability decreases as the coherent parameter increases. In the zero atom-field-detuning case, the atomic emission probability has three sets of resonance peaks. The reason for these results has been explained.

  10. Simulation of Rutherford backscattering spectrometry from arbitrary atom structures

    Science.gov (United States)

    Zhang, S.; Nordlund, K.; Djurabekova, F.; Zhang, Y.; Velisa, G.; Wang, T. S.

    2016-10-01

    Rutherford backscattering spectrometry in a channeling direction (RBS/C) is a powerful tool for analysis of the fraction of atoms displaced from their lattice positions. However, it is in many cases not straightforward to analyze what is the actual defect structure underlying the RBS/C signal. To reveal insights of RBS/C signals from arbitrarily complex defective atomic structures, we develop here a method for simulating the RBS/C spectrum from a set of arbitrary read-in atom coordinates (obtained, e.g., from molecular dynamics simulations). We apply the developed method to simulate the RBS/C signals from Ni crystal structures containing randomly displaced atoms, Frenkel point defects, and extended defects, respectively. The RBS/C simulations show that, even for the same number of atoms in defects, the RBS/C signal is much stronger for the extended defects. Comparison with experimental results shows that the disorder profile obtained from RBS/C signals in ion-irradiated Ni is due to a small fraction of extended defects rather than a large number of individual random atoms.

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

    Science.gov (United States)

    Parsons, Patrick J.; Slavin, Walter

    1999-05-01

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

  12. X-ray Emission of Hollow Atoms

    Institute of Scientific and Technical Information of China (English)

    ZhaoYongtao; XiaoGuoqing; ZhangXiaoan; YangZhihu; ChenXimeng; ZhangYanping

    2003-01-01

    We have systematically investigated the X-rays emission of hollow atoms (HA) which formed in the interaction of highly charged ions with a variety of solid surfaces at the atomic physics experimental setup of IMP. The X-ray spectra were measured by Si(Li) detectors with effective energy ranging from 1 keV to 60 keV. The results show that, the X-ray emission from the formed HA is closely correlated with the charge state of the projectile ions, and weakly correlated with the velocity of the projectile ions. For example, it was found that when Ar18+ ions interact with Be-target, the yield of K X-ray with character energy of 3.0 keV is 7.2×10-3 per ion, which is two times and 5 order of magnitude higher than those in the interactions of Ar17+ and Ar16+ ions respectively. When Ar15+ ions interact with the same targets, the Argon K X-ray would be too feeble to be detected. The X-ray yield with single ion in this experiment can be represented by the following equation,

  13. 40 CFR Table 4 to Subpart Uuu of... - Requirements for Performance Tests for Metal HAP Emissions From Catalytic Cracking Units Not...

    Science.gov (United States)

    2010-07-01

    ... Plasma-Atomic Emission Spectrometry, EPA Method 6020, Inductively Coupled Plasma-Mass Spectrometry, EPA Method 7520, Nickel Atomic Absorption, Direct Aspiration, and EPA Method 7521, Nickel Atomic...

  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. 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

    2016-09-29

    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.

  16. Stimulated Emission of an Atom in Circularly Polarized Light

    Institute of Scientific and Technical Information of China (English)

    李锦茴; 曾高坚; 叶永华

    2003-01-01

    We study the stimulated emission of a two-level atom in an electromagnetic wave of circular polarization. The correlation function G(r1t, r2t) = of atom radiation fields at dipole approximation are computed. Under the resonance condition, the atom stimulated emission is influenced by the circularly polarized electromagnetic wave discussed. We have found that the time-averaged value of energy density does not depend on the initial conditions. We have also deduced the relation between the emission power of an atom and the Rabi frequency Ω.

  17. 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...

  18. 中国原子光谱发展近况概述%Recent Development of Atomic Spectrometry in China

    Institute of Scientific and Technical Information of China (English)

    肖元芳; 王小华; 杭纬

    2015-01-01

    As an important part of modern analytical techniques,atomic spectrometry occupies a decisive status in the whole an-alytical field.The development of atomic spectrometry also reflects the continuous reform and innovation of analytical tech-niques.In the past fifteen years,atomic spectrometry has experienced rapid development and been applied widely in many fields in China.This review has witnessed its development and remarkable achievements.It contains several directions of atomic spec-trometry,including atomic emission spectrometry (AES),atomic absorption spectrometry (AAS),atomic fluorescence spec-trometry (AFS),X-ray fluorescence spectrometry (XRF),and atomic mass spectrometry (AMS).Emphasis is put on the inno-vation of the detection methods and their applications in related fields,including environmental samples,biological samples,food and beverage,and geological materials,etc.There is also a brief introduction to the hyphenated techniques utilized in atomic spectrometry.Finally,the prospects of atomic spectrometry in China have been forecasted.%原子光谱技术作为现代分析检测技术中的一个重要组成部分,在分析领域中占据着举足轻重的地位,而其发展也反映了分析技术的不断改革与创新。综述了中国原子光谱技术近15年来(2000年—2014年)的研究与应用进展。内容涉及原子光谱的多个分支领域,包括原子发射光谱(atomic emission spectrometry, AES),原子吸收光谱(atomic absorption spectrometry,AAS),原子荧光光谱(atomic fluorescence spectrome-try,AFS),X 射线荧光光谱(X-ray fluorescence spectrometry,XRF)以及原子质谱(atomic mass spectrome-try,AMS)五种原子光谱技术,重点关注各技术在检测方法上的创新及其在环境样品、生物样品、食品饮料以及地质材料等相关领域中的应用,并对原子光谱分析中利用到的各种联用技术进行了简要介绍。最后展望了今后我

  19. Improvement of determination for the content of potassium and sodium in food by Flame Atomic ;Emission Spectrometry%火焰原子发射光谱法测定食品中钾和钠含量的方法改进

    Institute of Scientific and Technical Information of China (English)

    林凯; 刘桂华; 张慧敏; 张红宇; 许欣欣; 姜杰

    2015-01-01

    目的对火焰原子发射光谱法测定食品中钾和钠含量的方法进行改进和探讨。方法采用高压密闭消解样品后,用火焰原子发射光谱法测定其中钾和钠的含量,并与原子吸收光谱法进行对比。结果在优化实验条件下,钾和钠的发射光谱法线性范围为0.1~4.0 mg/L,标准曲线线性关系良好,钾、钠的检出限分别为0.2 mg/100g和0.8mg/100g;各种食品基质标准物质的测定值均在证书参考值范围内,RSD<4%,原子发射光谱法与原子吸收光谱法的测定结果无差异。结论该方法准确、简便快速,精密度高,适用于食品中钾和钠含量的测定。%Objective To improve and discuss the flame atomic emission spectrometry method to determine the content of Potassium(K) and Sodium(Na) in food.Method The samples were digested in airtight pressure closed vessel,then were analyzed by flame atomic emission spectrometry.The results obtained by this method were compared with flame atomic absorption spectrometry meanwhile. Results Under the optimized condition, the determine range of K and Na was 0.1~4.0 mg/L,the calibration curve showed good,and the detection limit were 0.2mg/100g and 0.8mg/100g respectively.The determination value of various food matrix material were within the range of certificate value,RSD<4% ,no difference between two methods’ results were found.Conclusion This method is accurate ,simple and rapid, and has high precision,suitable for determinating the content of K and Na in food.

  20. The emission properties of an atom inside a cavity when manipulating the atoms outside the cavity

    Institute of Scientific and Technical Information of China (English)

    ZHANG Wen; YE Liu; XIONG Kuang-wei; ZHANG Jin

    2003-01-01

    Considering three two-level atoms initially in the GHZ state, then one atom of them is put into an initially empty cavity and made resonant interaction. It is shown that the emission properties of the atom inside the cavity can be affected only when both of the atoms outside the cavity have been manipulated. This conclusion can also be generalized to n two-level atoms.

  1. Determinação de Cd, Ni e Zn por espectrometria de emissão atômica com plasma indutivamente acoplado, após separação e pré-concentração em coluna contendo p-dimetilaminobenzilidenorodanina adsorvida sobre sílica gel Determination of Cd, Ni and Zn by inductively coupled plasma emission atomic spectrometry after separation and preconcentration in column packed with 5-(4-dimethylaminobenzylidene rhodanine adsorbed on silica gel

    Directory of Open Access Journals (Sweden)

    Laerte da Cunha Azeredo

    1999-07-01

    Full Text Available A column packed with 5-(4-dimethylaminobenzylidenerhodanine adsorbed on silica gel was used for the preconcentration of Cd, Ni and Zn at different spiked solutions prior to their determination by inductively coupled plasma atomic emission spectrometry. This column allowed recoveries over than 98% for the above elements and accurate analyses of coastal sea-water certified reference material were also achieved.

  2. 电感耦合等离子体原子发射光谱法测定银合金中的铂钯%Determination of Platinum and Palladium in Silver Alloy by Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    佡云; 褚晓君

    2016-01-01

    采用硝酸溶解样品,盐酸沉淀分离银,过滤洗涤后,在5%(体积分数)硝酸介质中,用电感耦合等离子体原子发射光谱法(ICP-AES)测定银合金样品中的铂、钯,该方法用于多个银合金中铂钯的测定,加标回收率在96%~101%,相对标准偏差(RSD,n=10)小于5%。%The sample was dissolved with nitric acidhydrochloric acid was added to the sample to produce precipitation of silver chloridethen filter and wash it.Platinum and palladium in silver alloy samples are determinated by inductively coupled plasma atomic emission spectrometryICP-AES in a 5% volume fraction nitric acid .The method was applied to the determination of platinum and palladium in silver al-lay samples.The recovery rate was in the range of 96%~101% and the relative standard deviationRSDn=10 was less than 5%.

  3. Determination of Elements by Atomic Absorption Spectrometry in Medicinal Plants Employed to Alleviate Common Cold Symptoms

    Institute of Scientific and Technical Information of China (English)

    F Zehra Küçükbay; Ebru Kuyumcu

    2014-01-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of com-mon cold have been studied for their mineral contents .Eleven minor and major elements (essential ,non-essen-tial and toxic) were identified in the Asplenium adiantum-nigrum L .,Althaea of ficinalis L .,Verbascum phlomoides L .,Euphorbiachamaesyce L .,Zizyphus jujube Miller ,Peganum harmala L .,Arum dioscori-dis Sm .,Sambucus nigra L .,Piper longum L .,Tussilago farfara L .and Elettariacardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrom-etry .Microwave digestion procedure for total concentration was applied under optimized conditions for dissolu-tion of medicinal plants .Plant based biological certified reference materials (CRMs) served as standards for quantification .These elements are found to be present in varying concentrations in the studied plants .The baseline data presented in this work can be used in understanding the role of essential ,non-essential and toxic elements in nutritive ,preventive and therapeutic properties of medicinal plants .

  4. Iodine Determination by Microwave Plasma Torch Atomic Emission Spectrometer Coupled with Online Preconcentration Vapor Generation Technique

    Institute of Scientific and Technical Information of China (English)

    FEI Yan-qun; LUO Gui-min; FENG Guo-dong; CHEN Huan-wen; FEI Qiang; HUAN Yan-fu; JIN Qin-han

    2008-01-01

    This article focuses on iodine determination by microwave plasma torch atomic emission spectrometry (MPT-AES) coupled with online preconcentration vapor generation method.A new desolvation device,multistrand Nation dryer,was used as the substitute for condenser desolvation system.Some experimental conditions,such as preconcentration time,acidity of sample solution,rinsing solution acidity and dynamic linear range were investigated and optimized.The new desolvation system eliminates the problem of decreasing emission intensity of I(I) 206.238 nm line with the increase of working time on a conventional condenser desolvation system,thus greatly improving the reproducibility.

  5. 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.

  6. Spreadsheet-Based Program for Simulating Atomic Emission Spectra

    Science.gov (United States)

    Flannigan, David J.

    2014-01-01

    A simple Excel spreadsheet-based program for simulating atomic emission spectra from the properties of neutral atoms (e.g., energies and statistical weights of the electronic states, electronic partition functions, transition probabilities, etc.) is described. The contents of the spreadsheet (i.e., input parameters, formulas for calculating…

  7. 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.

  8. Graviton Emission and Absorption by Atomic Hydrogen

    CERN Document Server

    Rothman, S B T

    2006-01-01

    Graviton absorption cross sections and emission rates for hydrogen are calculated by both semi-classical and field theoretic methods. We point out several mistakes in the literature concerning spontaneous emission of gravitons and related phenomena, some of which are due to a subtle issue concerning gauge invariance of the linearized interaction Hamiltonian.

  9. High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

    2017-03-01

    In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

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

    Science.gov (United States)

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

    2006-03-01

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

  11. Hyphenated techniques in speciation analysis of polyoxometalates: identification of individual [PMo12-xVxO40](-3-x) (x = 1-3) in the reaction mixtures by high performance liquid chromatography and atomic emission spectrometry with inductively coupled plasma.

    Science.gov (United States)

    Shuvaeva, O V; Zhdanov, A A; Romanova, T E; Abramov, P A; Sokolov, M N

    2017-03-14

    Unambiguous identification of polyoxometalate (POM) species generated in self-assembly reactions in solution is rather problematic due to close similarity of their properties such as solubility and spectral characteristics. The situation is made more complex by protonation equilibria (which can change their analytical signals) and the lack of individual compounds to serve as standards for individual members of these mixtures. In the present work a new approach to the study of such POMs has been suggested, taking molybdovanadates [PMo12-xVxO40](-3-x) as a model. The key feature of this approach consists of generation of so-called "conditional model systems" that include most of the expected components of a mixture formed by self-assembly, tracked down by reliable detection techniques, e.g., (51)V NMR-spectroscopy in this particular case. Then the proposed composition of the mixture is verified and corrected by means of high-performance liquid chromatography coupled with inductively coupled plasma atomic emission spectrometry (HPLC-ICP-AES).

  12. Determination of Trace Elements in Pomegranate Peel and Pomegranate Seed by Inductively Coupled Plasma-Atomic Emission Spectrometry with Microwave Digestion%微波消解-等离子体原子发射光谱法测定石榴皮和石榴籽中微量元素

    Institute of Scientific and Technical Information of China (English)

    吴佳; 解成喜

    2012-01-01

    采用微波消解样品,电感耦合等离子体原子发射光谱法(ICP-AES)测定了石榴皮和石榴籽中K、Ca、Mg、Fe、A1、Cu、Zn、Mn、Na、Li、P、S12种微量元素的含量.在最佳仪器工作条件下,各元素的加标回收率为91.8%~103.1%,相对标准偏差(RSD)为0.70%~2.68%.实验结果可为石榴皮和石榴籽中微量元素与其药效的相关性提供科学依据.%The trace elements of K,Ca,Mg,Fe, Al,Cu,Zn,Mn,Na,Li,P and S in the pomegranate peel and pomegranate seed were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) with microwave digestion. Under the optimal working conditions of the equipment, the element recoveries of standard addition are 91. 8% ~ 103. l%,and the relative standard deviations (RSDs) are 0. 70%~2. 68%.

  13. 电感耦合等离子体发射光谱法测定镍矿石中镍铜铅锌%Determination of Ni,Cu,Pb and Zn in nickel ores by inductive coupling plasma-atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    郭爽; 金震宇; 杨婷; 于微

    2012-01-01

    The authors dissolved the sample of the nickle ore with hydrofluoric acid,nitric acid,hydrochloric acid and high chloride acid.Dissolved the salt with aqua regia.To determine the elements of nickel,copper,lead and zinc in the solution by inductive coupling plasma-atomic emission spectrometry,to interfere survey the target elements in spectrum lines,and to select the suitable analytical spectral lines.The result of the experiment proves that the nickel can increase the spectrum line background and overlapping peak of the target elements,In addition,the recovery rate ranges from 98% to 103%,and the relative deviation less than 3.%选用氢氟酸、硝酸、盐酸、高氯酸对镍矿石样品进行溶样,用王水溶解盐类,电感耦合等离子体发射光谱法测定溶液中镍、铜、铅、锌元素,对目标元素进行谱线干扰考察,选择合适的分析谱线,结果表明镍会使目标元素谱线背景和叠加峰轻度增高,回收率都在98%~103%,相对偏差小于3。

  14. Determination of Twelve Trace Elements in Children`s hair by Inductively Coupled Plasma Atomic Emission Spectrometry%电感耦合等离子体发射光谱法测定儿童发样中十二种微量元素

    Institute of Scientific and Technical Information of China (English)

    代建强; 杨诗佳

    2013-01-01

    This paper uses the nitric acid and hydrogen peroxide sample digestionarticle, Determination of aluminum, calcium, chromium, copper, iron, potassium, magnesium, sodium, manganese, lead, nickel, zinc and other trace elements in children's hair by inductively coupled plasma atomic emission spectrometry.The recovery rate of 95%~105%,The detection limit of element (ug/ml) in 0.0010-0.011,The relative standard deviation (RSD, n=9) is less than 4%,After verification of human hair in national standard reference samples, The measured value had no significant difference with standard value.%采用硝酸-过氧化氢消解试样,电感耦合等离子体发射光谱法测定儿童发样中铝、钙、铬、铜、铁、钾、镁、锰、钠、铅、镍、锌等十二种微量元素。方法回收率95%~105%,各元素检出限(ug/mL)在0.0010~0.011之间,相对标准偏差(RSD,n=9)小于4%,经人发国家一级标准物质验证,测定值与标准认定值无明显差异。

  15. Separation and preconcentration of Cd(II), Cu(II), Ni(II), and Pb(II) in water and food samples using Amberlite XAD-2 functionalized with 3-(2-nitrophenyl)-1H-1,2,4-triazole-5(4H)-thione and determination by inductively coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Kumar, Bommana Naresh; Ramana, D K Venkata; Harinath, Yapati; Seshaiah, Kalluru; Wang, M C

    2011-10-26

    A separation and preconcentration procedure was developed for the determination of trace amounts of Cd(II), Cu(II), Ni(II), and Pb(II) in water and food samples using Amberlite XAD-2 fuctionalized with a new chelating ligand, 3-(2-nitrophenyl)-1H-1,2,4-triazole-5(4H)-thione (Amberlite XAD-2-NPTT). The chelating resin was characterized by Fourier transform infrared spectroscopy (FT-IR) and used as a solid sorbent for enrichment of analytes from samples. The sorbed elements were subsequently eluted with 10 mL of 1.0 M HNO(3), and the eluates were analyzed by inductively coupled plasma-atomic emission spectrometry. The influences of the analytical parameters including pH, amount of adsorbent, eluent type and volume, flow rate of the sample solution, volume of the sample solution, and effect of matrix on the preconcentration of metal ions have been studied. The optimum pH for the sorption of four metal ions was about 6.0. The limits of detection were found to be 0.22, 0.18, 0.20, and 0.16 μg L(-1) for Cd(II), Cu(II), Ni(II), and Pb(II), respectively, with a preconcentration factor 60. The proposed method was applied successfully for the determination of metal ions in water and food samples.

  16. 电感耦合等离子体原子发射光谱法同时测定饮用水的硬度和碱度%Simultaneous determination of the hardness and alkalinity in drinking water by inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    霍建中; 段旭川

    2013-01-01

    The feasibility of simultaneous determination of hardness and alkalinity of drinking water by inductively coupled plasma atomic emission spectrometry (ICP-AES) was studied.the water sample was acidified off-line with diluted hydrochloric acid.The bicarbonates in water sample were in-situ converted into carbon dioxide,which was also dissolved in original water.Then,the solution was sampled by conventional single tube of inductively coupled plasma atomic emission spectrometer.The simultaneous sampling of CO2,Ca and Mg was realized at relatively low atomizer pressure.Among them,CO2 was sampled in gas state,while Ca and Mg were sampled in atomizing state.In this study,the bicarbonates with low sampling efficiency in atomizing method were converted into gas carbon dioxide,which had high sampling efficiency,thus the determination sensitivity of carbon was increased,realizing the accurate determination.The measured content of inorganic carbon was converted to the content of bicarbonates,so the alkalinity of drinking water was obtained.Meanwhile,the content of Ca and Mg was converted to the content of calcium carbonate to calculate the hardness of water.Under the optimal experimental conditions,i.e.,atomizer pressure of 241.3 kPa and dilution ratio of 5for water sample,the hardness and alkalinity of drinking water were simultaneously determined by this method.The found results were consistent with those obtained by titration method.%研究了使用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定饮用水的硬度和碱度可行性.通过用稀盐酸离线酸化水样,使水样中的碳酸氢根原位转化为二氧化碳并继续溶解在原水中,然后使用ICP-AES仪器上常规的单管吸取溶液,在比较低的雾化器压力下实现了CO2、Ca、Mg的同时进样.其中CO2属于气态进样,而钙、镁属于雾化进样.由于方法将雾化法进样效率低的碳酸氢根转化成进样效率高的二氧化碳气态,因此碳的测定灵敏

  17. Emission spectrum of the atomic chain excited by channeled particle

    CERN Document Server

    Epp, V

    2014-01-01

    Basic properties of radiation of the atomic chains excited by a channeled particle are considered. Using a very simple two-dimensional model of a crystal lattice we have shown that the main part of this radiation is generated on the frequency of oscillations of a channeled particle between the crystal planes, shifted by the Doppler effect. Spectral and angular distribution and spectral distribution of the radiation of the atomic chain excited by channeled particle were calculated. Emission spectrum of the atomic chain excited by channeled particle was plotted.

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

    Science.gov (United States)

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

    2015-01-01

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

  19. Atomic Coherence in the Micromaser Injected with Slow V-type Three-State Atoms: Emission Probability

    Institute of Scientific and Technical Information of China (English)

    ZHANG Zhi-Ming; LIANG Wen-Qing; XIE Sheng-Wu

    2001-01-01

    The effects of atomic coherence on the single-mode two-photon rnicromaser injected with slow V-type three-state atoms are studied for the first time. It is shown that the atomic coherence can modify the atomic emission probability. The effects of the atomic centre-of-mass momentum, the cavity length and other parameters are also studied.

  20. Padronização interna em espectrometria de absorção atômica Internal standardization in atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Kelly G. Fernandes

    2003-03-01

    Full Text Available This paper describes a review on internal standardization in atomic absorption spectrometry with emphasis to the systematic and random errors in atomic absorption spectrometry and applications of internal standardization in flame atomic absorption spectrometry and electrothermal atomic absorption spectrometry. The rules for selecting an element as internal standard, limitations of the method, and some comments about the application of internal standardization in atomic absorption spectrometry and the future of this compensation strategy are critically discussed.

  1. Theory of analytical curves in atomic fluorescence flame spectrometry

    NARCIS (Netherlands)

    Hooymayers, H.P.

    1968-01-01

    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 bro

  2. 电感耦合等离子体原子发射光谱法测定新疆洋葱籽中常量/微量元素%Determination of Major/Trace Elements in the Xinjiang Allium cepa L.Seeds by Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    孙凤; 邓丽霜; 童红; 王强

    2013-01-01

    Six samples were pretreated by microwave digestion method and analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES). And 18 kinds of major/trace elements in Xinjiang Allium cepa L. seeds were determined including Co, Cr, Ca, K, Mg, P, Fe, Mn, Na, Ni, Sn, Zn, Cd, As,Se, Cu, Mo and V. Results indicated that Allium cepa L. seeds were riched in major elements such as K,Mg,P,Ca and Na, besides, the trace elements Fe, Mn,Zn,Cr,Ni,and Cu were also relatively abundant. Allium cepa L. seeds contain a lot of major and trace elements which are beneficial to human body and have high medicinal value.%采用微波消解法处理样品,以电感耦合等离子体原子发射光谱法(ICP AES)测定新疆洋葱籽样品中Co、Cr、Ca、K、Mg、P、Fe、Mn、Na、Ni、Sn、Zn、Cd、As、Se、Cu、Mo和V 18种常量/微量元素.结果显示,新疆洋葱籽中含有丰富的K、Mg、P、Ca和Na等常量元素,此外微量元素Fe、Mn、Zn、Cr、Ni、Cu的含量也较丰富.新疆洋葱籽中含有很多对人体有益的常量及微量元素,有较高的药用价值.

  3. Determination of Heavy Metals in Electroplating Sludge Leaching Liquid by Inductively Coupled Plasma Atomic Emission Spectrometry%电感耦合等离子体原子发射光谱法测定电镀污泥浸出液中的重金属

    Institute of Scientific and Technical Information of China (English)

    徐国津; 樊颖果; 赵倩

    2014-01-01

    Heavy metals in electroplating sludge leaching liquid such as Cu,Zn,Ni,Cr,Pb,Cd and Ba were determined by inductively coupled plasma atomic emission spectrometry with sulfuric acid-nitric acid extraction. The working conditions of the instrument and interference factors and elimination method were studied. Under the selected conditions,the linear correlation coefficients were all 0.999 9,the detection limits were between 0.002 mg/L and 0.01 mg/L,recoveries ranged from 93.5%to 106.0%,and the relative standard deviations of determination results were less than 10%(n=6). The method could quickly and accurately detect some heavy metals in electroplating sludge leaching liquid.%采用硫酸-硝酸溶液浸提电镀污泥中的重金属,建立电感耦合等离子体原子发射光谱法(ICP-AES)测定电镀污泥浸出液中铜、锌、镍、铬、铅、镉、钡元素的分析方法。研究了仪器的工作条件及影响检测方法的干扰因素和消除。在选定的条件下,线性相关系数均为0.9999,检出限为0.002~0.01 mg/L,加标回收率为93.5%~106.0%,测定结果的相对标准偏差小于10%(n=6)。该方法准确快速,可用于电镀污泥浸出液中多种重金属的含量测定。

  4. A NEW GENERATION OF INSTRUMENTATION AND CAPABILITIES FOR ATOMIC MASS SPECTROMETRY

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    @@ Atomic mass spectrometry,embodied usually as inductively coupled plasma mass spectrometry (ICPMS) or glow-discharge mass spectrometry (GDMS),has become a widely accepted tool for trace and ultra-trace elemental analysis.ICPMS offers detection limits below 1 ppt in solution,a dynamic concentration levels,isotope-analysis and isotope-dilution capabilities,modest matrix interferences,understandable spectral interferences (isobaric overlaps),precision in range of 2—5%,and rapid measurements (typically 10 seconds per isotope).

  5. 碱熔—电感耦合等离子体原子发射光谱法测定红土镍矿中硅钙镁铝锰钛铬镍钴%Determination of silicon, calcium, magnesium, aluminium, manganese,titanium, chromium, nickel and cobalt in laterite nickel ore by alkali fusion-inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    高亮

    2013-01-01

    The determination method of nine elements (silicon, calcium, magnesium, aluminium, manganese, titanium, chromium, nickel and cobalt) in laterite nickel ore by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The laterite nickel ore sample was fused by anhydrous Na2CO3-H3BO3 mixed flux, then acidified and leached by hydrochloric acid. The high salt atomizer and cyclone chamber were used. Under the selected measurement conditions, the content of nine elements in sample solution was determined by ICP-AES. The influence of salts introduced by matrix iron and sample treatment could be eliminated by matrix matching method. The precision test results showed that, the relative standard deviations (RSD) of elements were smaller than 5 %. The proposed method was applied to the determination of reference material, and the determination results of nine elements were basically consistent with the certified values.%建立了红土镍矿中Si、Ca、Mg、Al、Mn、Ti、Cr、Ni、Co 9种元素的电感耦合等离子体原子发射光谱测定方法.红土镍矿样品用无水Na2CO3-H3BO3混合熔剂熔融,盐酸浸取、酸化,选用高盐雾化器和旋流雾室,在选定的测量条件下,用电感耦合等离子体原子发射光谱法测定试液中9种元素含量.基体铁和处理样品时引入试液中的盐分对测定的影响可以通过基体匹配的方法消除.精密度试验结果表明,样品中各元素测定结果的相对标准偏差小于5%.用本法测定标准样品,9种元素的测定值与认定值基本一致.

  6. Atomic Dipole Traps with Amplified Spontaneous Emission: A Proposal

    CERN Document Server

    Clément, Jean-François; Garreau, Jean Claude; Szriftgiser, Pascal

    2010-01-01

    We propose what we believe to be a novel type of optical source for ultra-cold atomic Far Off-Resonance optical-dipole Traps (FORTs). The source is based on an Erbium Amplified Spontaneous Emission (ASE) source that seeds a high power Erbium Doped Fiber Amplifier (EDFA). The main interest of this source is its very low coherence length, thus allowing an incoherent superposition of several trapping beams without any optical interference. The behavior of the superimposed beams is then a scalar sum greatly simplifying complex configurations. As an illustration, we report an estimation of the intensity noise of this source and an estimation of the atomic excess heating rate for an evaporative cooling experiment application. They are both found to be suitable for cold atoms experiments.

  7. 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.

  8. 碱熔-电感耦合等离子体发射光谱法测定大气颗粒物样品中无机元素%Quantification of Inorganic Elements in Aerosol Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry with Alkali Melting

    Institute of Scientific and Technical Information of China (English)

    付爱瑞; 陈庆芝; 罗治定; 姜云军; 金倩; 王芸

    2011-01-01

    大气颗粒物(TSP和PM10)中Si、Al、Ca、Mg、K、Fe、Na等元素含量较高,是颗粒物源分析的指示性元素.目前分析大气颗粒物样品中无机元素的方法有中子活化分析法、X射线荧光光谱法、微波消解(或高压釜消解)电感耦合等离子体发射光谱法和电感耦合等离子体质谱法.本文建立了碱熔-电感耦合等离子体发射光谱法测定大气颗粒物样品中Si、Al、Ca、Mg、Fe、Ti、Ba、Sr、Zr等无机元素的分析方法,样品于镍坩埚中530~550℃灰化60 min后用NaOH融熔,水提取,再用2 mL 50%的HCl酸化,钠基体匹配消除干扰,解决了大气颗粒物滤膜样品中Si易产生的溶解不完全等问题,提高了Ti、Ba、Sr、Zr等主、次量元素测定的精密度和准确度.讨论了坩埚和熔剂的选择、灰化温度、灰化时间、酸度、干扰等影响因素.在选定条件下,测定结果相对误差(RE)﹤4%,相对标准偏差(RSD,n=12)﹤5%,检出限为0.0047~1.2 ng/g.方法所需设备简单,分析成本低,快速简便,精密度好,准确度高,适宜批量样品的测定.%In atmospheric particles ( TSP and PM10 ), the high contents of some inorganic elements including Si, Al, Ca, Mg, K, Fe and Na are the proxy elements for the particles source analysis. At present, there are several methods to analyze inorganic elements for atmospheric particles such as neutron activation analysis, X-ray Fluorescence Spectrometry ( XRF ), Inductively Coupled Plasma-Atomic Emission Spectrometry ( ICP-AES ) and Inductively Coupled Plasma-Mass Spectrometry ( ICP-MS ) after dissolving by microwave ( or high-pressured cauldron ). The established method for determining Si, Al, Ca, Mg, Fe, Ti, Sr, Ba and Zr in aerosols by ICP-AES with alkali melting solved the problems of incomplete dissolving for Si caught in an atmospheric particles filter diaphragm, and improved the precision and accuracy of the determinations of major and trace elements such as Ti, Ba, Sr, Zr. In

  9. 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...

  10. Saturation of Energy Levels in Analytical Atomic Fluorescence Spectrometry. II. Experimental.

    Science.gov (United States)

    1981-01-30

    RESEARCH Contract N14-76-C-0838 Task Ao. NR 051-622 TECHNICAL REPORT NO. 34 SATURATION OF ENERGY LEVELS IN ANALYTICAL ATOMIC FLUORESCENCE SPECTROMETRY II...an assumption which is valid only if the daral o’l of 111, cxcilIatio n pulse is mucl ) longer than the fluorescence life- time of the tjaii!,ition

  11. A new heating strategy in electrothermal atomic absorption spectrometry for better absorbance-time curves at high atomization rate

    Energy Technology Data Exchange (ETDEWEB)

    Torsi, Giancarlo [Department of Chemistry G. Ciamician, University of Bologna, Via F. Selmi 2, 40126 Bologna (Italy)]. E-mail: giancarlo.torsi@unibo.it; Zattoni, Andrea [Department of Chemistry G. Ciamician, University of Bologna, Via F. Selmi 2, 40126 Bologna (Italy); Locatelli, Clinio [Department of Chemistry G. Ciamician, University of Bologna, Via F. Selmi 2, 40126 Bologna (Italy); Valcher, Sergio [Department of Chemistry G. Ciamician, University of Bologna, Via F. Selmi 2, 40126 Bologna (Italy)

    2005-03-31

    The results previously obtained by using fast heating in electrothermal atomic absorption spectrometry are considerably improved by using a new heating sequence which can be summarized as transverse-longitudinal heating mode. The absorbance vs. time curves, obtained with the new heating mode, follow almost perfectly a simple model in which only diffusion is considered as the force acting on the atomic vapor. From the fitting of the experimental absorbance vs. time data points with theoretical values, it is possible to calculate both the absorbance, when all atoms injected are assumed to be present, and their diffusion coefficient. Both values can be calculated by a simple software approach without the operator intervention. The asymptotic absorbance calculated in this way is the maximum absorbance physically obtainable and is the basis for standardless analysis.

  12. Determination of eight impurity elements in industrial silicon by inductively coupled plasma atomic emission spectrometry%电感耦合等离子体原子发射光谱法测定工业硅中8种杂质元素

    Institute of Scientific and Technical Information of China (English)

    张云晖; 杨晓静; 亢若谷; 赵建为; 金波

    2013-01-01

    The inert sample injection system resistant hydrofluoric acid of inductively coupled plasma atomic emission spectrometer was used. The sample solution was injected directly without removing hydrofluoric acid and silicon matrix after sample was dissolved in hydrofluoric acid, nitric acid and perchloric acid. Eight impurities including iron, aluminum, calcium, titanium, manganese, nickel, boron and phosphorus in industrial silicon powder were simultaneously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Most of matrix silicon had been volatilized and removed in sample dissolution process, so the matrix effect had no influence on the determination of i-ron, aluminum, calcium, titanium, manganese and nickel. However, the determination of boron and phosphorus was still affected, which could be eliminated by vertical observation method. The detection limit of the method was calculated by three times of standard deviation of blank. The detection limits (w/%) for iron, aluminum, calcium, titanium, manganese, nickel, boron and phosphorus were 0. 004, 0. 001, 0. 004, 0. 001, 0. 0001, 0. 0001, 0. 000 04 and 0. 000 06, respectively. The proposed method was applied to the determination of eight impurities in industrial silicon. The found results were consistent with the certified values or those obtained by standard method (GB/T 14849. 4-2008).%采用电感耦合等离子体原子发射光谱仪的耐氢氟酸惰性进样系统,在样品用氢氟酸、硝酸、高氯酸溶解完全后无需赶尽氢氟酸和硅基体,直接进样,电感耦合等离子体原子发射光谱法同时测定了工业硅粉中铁、铝、钙、钛、锰、镍、硼和磷8种杂质元素.因为在溶样过程中大部分基体硅已挥发除去,基体效应对铁、铝、钙、钛、锰、镍的测定没有影响,但是对硼和磷的测定仍有影响,这种影响可以采用垂直观测方式克服.按照空白值的3倍标准偏差计算方法的检测限,得到

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

    OpenAIRE

    Musil, S. (Stanislav); Dědina, J. (Jiří)

    2013-01-01

    Sapphire was tested as a new material for volatile species atomizers and bismuthine was chosen as a convenient model for volatile species. Its performance was compared with a quartz atomizer in both modes of operation - on-line atomization versus in situ collection.

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

    Science.gov (United States)

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

    2005-05-01

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

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

    Science.gov (United States)

    Titretir, Serap; Kendüzler, Erdal; Arslan, Yasin; Kula, İbrahim; Bakırdere, Sezgin; Ataman, O. Yavuz.

    2008-08-01

    An electrically heated tungsten coil was used as a trap in the determination of antimony. The technique consists of three steps. Initially, SbH 3 is formed by hydride generation procedure; then the analyte species in vapor form are transported to W-coil trap heated at 370 °C. Following the preconcentration step, the trap is heated to 895 °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 4 solutions, H 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 - 1 using a sample of 36 ml collected in 4.0 min. Enhancement factor in sensitivity was 17.

  16. 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.

  17. Infrared [Fe II] Emission Lines from Radiative Atomic Shocks

    CERN Document Server

    Koo, Bon-Chul; Kim, Hyun-Jeong

    2016-01-01

    [Fe II] emission lines are prominent in the infrared (IR), and they are important diagnostic tools for radiative atomic shocks. We investigate the emission characteristics of [Fe II] lines using a shock code developed by Raymond (1979) with updated atomic parameters. We first review general characteristics of IR [Fe II] emission lines from shocked gas, and derive [Fe II] line fluxes as a function of shock speed and ambient density. We have compiled the available IR [Fe II] line observations of interstellar shocks and compare them to the ratios predicted from our model. The sample includes both young and old supernova remnants in the Galaxy and the Large Magellanic Cloud and several Herbig-Haro objects. We find that the observed ratios of IR [Fe II] lines generally fall on our grid of shock models, but the ratios of some mid-infrared lines, e.g., [Fe II] 35.35 um/[Fe II] 25.99 um, [Fe II] 5.340 um/[Fe II] 25.99 um, and [Fe II] 5.340 um/[Fe II] 17.94 um, are significantly offset from our model grid. We discuss ...

  18. Chlorine Analysis by Diode Laser Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    Joachim Koch; Aleksandr Zybin; Kay Niemax

    2000-01-01

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

  19. 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.

  20. Affirmation of the Method that Simultaneous Determination of Copper, Lead, Zinc, Cobalt and Nickel in Copper, Lead and Zinc Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry%电感耦合等离子体发射光谱法同时测定铜铅锌矿石中铜铅锌钴镍等元素方法确认

    Institute of Scientific and Technical Information of China (English)

    熊英; 王晓雁; 胡建平

    2011-01-01

    文章在修订GB/T 14353-1993研究工作中,建立了电感耦合等离子体发射光谱同时测定铜铅锌矿石中铜铅锌钴镍等元素的标准分析方法.通过控制试样量和制备试样溶液的体积,可实现主量元素铜、铅、锌与次量元素钴、镍的同时测定.测定范围为铜0.002%~8.5%,铅0.01%~5%,锌0.005%~3%,钴0.001 5%~0.5%,镍0.003%~0.5%.按照相关国家标准对测量方法与结果的准确度进行8个实验室协同参加的准确度试验,统计参数结果表明在限定水平范围内方法偏倚不显著;利用方法重复性限参数,计算可能产生的最大相对偏差.分析方法精密度满足的要求.%A standard analysis method for simultaneous detecting copper, lead, zinc, cobalt, nickel and other elements by inductively coupled plasma-atomic emission spectrometry (ICP-AES) was developed when improving GB/T 14353-1993 , the method for chemical analysis of copper ore, lead ore and zinc ore. The major elements such as copper, lead, zinc and the minor elements of cobalt and nickel can be simultaneous detected by adjusting the test portion amounts and reagent solution volumes. The determination ranges of copper, lead, zinc, cobalt and nickel are respectively 0.002% -8.5% , 0. 01% - 5% , 0. 005% - 3% , 0. 001 5% - 0. 5% and 0. 003% - 0. 5%. According to relevant national standards, this method was tested by eight cooperation laboratories. Statistical results indicated that the method is impartial within a definitive range. The repeatability limit parameter was used to calculate the possible maximum deviations. The precision of the method satisfied the requirement of "The specification of testing quality management for geological laboratoris".

  1. 电感耦合等离子体发射光谱法测定红土镍矿中镍钻铜%Determination of Ni, Co and Cu in Laterite-Nickel Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    王国新; 许玉宇; 王慧; 刘烽; 吴骋; 胡清

    2011-01-01

    A method for the determination of Ni, Co and Cu contents in laterite is presented in this paper. Laterite samples were fused with a mixed flux of Na2CO3-Na2B4O7, then the analytes were extracted by HC1 acid. The sample solution was measured by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The internal standard method was used to avoid matrix interference based on choosing Y 371. 030 nm as the internal calibration line for Cu (324.754 nm) and Y 224.306 nm for Ni (231.604 nm) and Co (228.616 nm). The detection limits for Ni, Co and Cu were 0. 5 μg/g, 1.0 μg/g and 1.0 μg/g, respectively. The relative standard deviations (RSD) of the test result were 1. 2% -2. 0% (n =7) , and the recoveries ranged from 95% to 103.6%, which met the requirements of analysis for laterite.%红土镍矿样品用无水Na2 CO3 - Na2 B4 O7混合熔剂熔融,HCl浸出酸化,电感耦合等离子体发射光谱法直接测定样品中镍、钴、铜的含量.Cu 324.754 nm使用Y 371.030 nm作为内标线,Ni 231.604 nm、Co 228.616 nm使用Y 224.306 nm作为内标线校正基体干扰,方法检出限镍为0.5μg/g、钴为1.0 μg/g、铜为1.0μg/g,相对标准偏差( RSD,n=7)为1.2% ~2.0%,加标回收率为95.0% ~ 103.6%,能满足红土镍矿的分析要求.

  2. 电感耦合等离子体原子发射光谱法测定镍基钎焊料中铬和硅%Determination of chromium and silicon in nickel-based brazing material by inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    杨丽; 王金阳; 张庸

    2013-01-01

    The analysis conditions of chromium and silicon in nickel-based brazing material by inductively coupled plasma atomic emission spectrometry (ICP-AES) were discussed.After the nickelbased brazing material was dissolved with aqua regia-hydrofluoric acid mixed acid,and matrix effect was reduced by matrix matching,chromium and silicon in the sample were determined by ICP-AES with spectral line of 267.716(125) nm and 251.612(133) nm as the analytical lines for chromium and silicon respectively.This proposed method was applied to the determination of chromium and silicon in actual samples and the results were consistent with those obtained by ammonium persulfate oxidization titration method and perchloric acid dehydration method.The relative standard deviation (RSD,n =6) of chromium and silicon was 0.55%-0.73% and 0.71%-1.0%,respectively.The recoveries were 100%-101% and 99%-100%,respectively.%探讨了电感耦合等离子体原子发射光谱法(ICP-AES)测定镍基钎焊料中铬和硅的分析条件.试样经王水和氢氟酸混合酸溶解,选择267.716(125) nm和251.612(133) nm的光谱线分别作为铬和硅的分析线,并采用基体匹配法降低了基体效应,ICP-AES测定了镍基钎焊料中铬和硅含量.实际样品中铬和硅的测定结果与过硫酸铵氧化滴定法和高氯酸脱水法相符,铬和硅的相对标准偏差(n=6)分别为0.55%~0.73%和0.71%~1.0%,加标回收率分别为100%~101%和99%~100%.

  3. 碱熔融电感耦合等离子体原子发射光谱法测定生铁中硅锰磷含量%Determination of Silicon Manganese and Phosphorus in Pig Iron with Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    吴金龙; 金献忠

    2014-01-01

    A method was proposed for the determination of silicon, manganese, and phosphorus in pig iron with inductively coupled plasma atomic emission spectrometry . Samples were fused with sodium hydroxide and sodium peroxide in zirconium crucibles and leached out with hydrochloric acid solution. The matrix effect were investigated, no effect on the measured elements by sodium between 5.0 mg/mL and 6.0 mg/mL, zirconium in 20μg/mL and other elements in pig iron was found. Acidity effect was discussed and the effect of the volume of hydrochloric acid between 8 percent and 12 percent was able to be ignored. CRMs of pig iron were analyzed, and good agreements were achieved on the detected levels and the certified values with RSDs (n=5) being in the range of 0.3%-1.0%.%提出了一种电感耦合等离子体原子发射光谱法测定生铁中硅、锰、磷含量的方法。生铁样品采用氢氧化钠和过氧化钠在锆坩埚内熔融,盐酸浸取;研究了共存元素的影响,浓度在5.0 mg/mL-6.0 mg/mL之间的钠元素、20μg/mL的锆元素以及样品中其他共存元素对各元素的测定结果无影响;考察了酸度效应,盐酸用量在体积分数8%-12%时,对各元素测定的影响可以忽略。以生铁标准物质作为样品进行分析,测定值和认定值相吻合,RSD(n=5)为0.3%-1.0%。

  4. Methods of Cold Soaking, Foam Plastics Enrichment and Inductive Coupling Plasma Atomic Emission Spectrometry%冷浸取--泡塑富集-电感耦合等离子体发射光谱法测定化探样品中的超痕量金铂钯研究

    Institute of Scientific and Technical Information of China (English)

    闵慧英; 袁蕙霞; 郭玉翠

    2015-01-01

    建立了冷浸--泡沫塑料富集,采用 ICP-AES 测定地球化学勘探样品中超痕量金、铂、钯的方法,并试验了冷浸取、泡沫塑料富集时各种因素的影响;确定了采用氯化钠、盐酸和高锰酸钾冷浸取分解试样,以泡沫塑料富集、灰化,残渣用王水溶解,用电感耦合等离子体发射光谱法测定的条件。该方法检出限分别为:Au 0.039ng/g,Pt 0.040ng/g,Pd 0.058ng/g;回收率为95.6%~102.5%之间;测量精密度( RSD%)为:Au 4.85%,Pt 5.76%,Pd 6.45%。采用该方法测定了国家一级地球化学标准物质中的痕量 Au,Pt,Pd,测定值与标准值符合规范要求。%In this paper, we set up the enrichment of cold soaking foam plastics by adopting the method of ICP-AES to test the ultra-trace of gold, platinum and palladium from the geochemical exploration sample and studied all kinds of effective factors in cold soaking foam plastics enrichment. And we confirmed the requirements of using sodi-um chloride, hydrochloric acid and potassium permanganate cold soak-ing to decompose the sample, using foam plastics to enrich and ash, aqua regia to dissolve residue, and measuring by inductive coupling Plasma Atomic Emission Spectrometry. The detection limits of this method are as follows: detection limit: Au 0.039ng/g, Pt 0.040ng/g, Pd 0.058ng/g; recovery rate: between 95.9% and 102.2%; relative stan-dard deviation (RSD%): Au 4.85%,Pt 5.76%,Pd 6.45%.We tested the trace amount of Au, Pt and Pd in the country-level geochemistry stan-dard substance. The measured value is consistent with the normalized value.

  5. Determination of Chromium,Zirconium,Vanadium and Hafnium in Polyethylene and Polypropylene by Inductively Coupled Plasma Atomic Emission Spectrometry%电感耦合等离子体原子发射光谱法测定聚乙烯、聚丙烯中铬、锆、钒和铪

    Institute of Scientific and Technical Information of China (English)

    陈金凤; 陈章捷; 钟坚海; 郑宗展

    2011-01-01

    采用微波消解技术对以聚乙烯、聚丙烯为原料制作的食品容器、食品包装薄膜进行预处理,确定了溶样酸介质及其用量、微波消解温度、时间等关键因素,建立了一种快速测定聚乙烯、聚丙烯材料中铬、锆、钒和铪含量的电感耦合等离子体原子发射光谱法。实验结果表明,5mL硝酸和1mL过氧化氢的混合溶液即可实现样品的完全消解,同时通过优化光谱分析条件,得到铬、锆、钒和铪的检测限分别为1.0 mg/kg,0.7mg/kg,0.7 mg/kg,1.4 mg/kg。该法加标回收率在88%-103%之间,相对标准偏差(n=3)为0.84-6.4%。用于实际样品的测定,所得结果与标准样品的参考值相符。%A method for the rapid determination of chromium,zirconium,vanadium and hafnium in polyethylene and polypropylene by inductively coupled plasma atomic emission spectrometry was established.The samples made of polyethylene and polypropylene used as food container or food wrapper was pretreated by microwave digestion.The effects of digestion media and it's use amount,digestion temperature and holding time on digestion results were investigated.It was experimentally indicated that the samples could be thoroughly digested in a mixture of 5 mL of nitric acid and 2 mL of hydrogen peroxide.Under the optimal conditions,the detection limits of chromium,zirconium,vanadium and hafnium were 1.0 mg/kg,0.7 mg/kg,0.7 mg/kg and 1.4 mg/kg respectively.The recoveries of standards in polyethylene and polypropylene samples were from 88% to 103%,with the RSDs of 0.84%-6.4%(n=3).This method was employed in the determination of real samples,the analytical results was accorded with the certified results.

  6. Negative spontaneous emission by a moving two-level atom

    Science.gov (United States)

    Lannebère, Sylvain; Silveirinha, Mário G.

    2017-01-01

    In this paper we investigate how the dynamics of a two-level atom is affected by its interaction with the quantized near field of a plasmonic slab in relative motion. We demonstrate that for small separation distances and a relative velocity greater than a certain threshold, this interaction can lead to a population inversion, such that the probability of the excited state exceeds the probability of the ground state, corresponding to a negative spontaneous emission rate. It is shown that the developed theory is intimately related to a classical problem. The problem of quantum friction is analyzed and the differences with respect to the corresponding classical effect are highlighted.

  7. Determination of cadmium and lead in urine by derivative flame atomic absorption spectrometry using the atom trapping technique

    Science.gov (United States)

    Han-wen, Sun; De-qiang, Zhang; Li-li, Yang; Jian-min, Sun

    1997-06-01

    A method is described for the determinations of cadmium and lead in urine by derivative flame atomic absorption spectrometry with a modified water-cooled stainless steel atom trapping tube. The effects of the trap position, the flame conditions, the coolant flow rates, and the collection time were studied. With a 1 min collection time, the characteristic concentrations (derivative absorbance of 0.0044) for cadmium and lead were 0.028 and 1.4 μg L -1, the detection limits (3σ) were 0.02 and 0.27 μg L -1, respectively. The detection limits and sensitivities of the proposed method were 2 and 3 orders of magnitude higher for 1-3 min collection time than those of conventional flame atomic absorption spectrometry for cadmium and lead, respectively. Urine samples from a small population of normal individuals have been analyzed for cadmium and lead by the proposed method. Satisfactory recoveries of 91-110% and 91-106%, for Cd and Pb were obtained with these urine samples.

  8. 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.

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

    Science.gov (United States)

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

  10. Determination of cadmium in rice and water by tungsten coil electrothermal vaporization-atomic fluorescence spectrometry and tungsten coil electrothermal atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Wen Xiaodong [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Wu Peng [Analytical and Testing Center, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Chen Li [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Hou Xiandeng, E-mail: houxd@scu.edu.cn [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Analytical and Testing Center, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China)

    2009-09-14

    In this work, the microsampling nature of tungsten coil electrothermal vaporization Ar/H{sub 2} flame atomic fluorescence spectrometry (W-coil ETV-AFS) as well as tungsten coil electrothermal atomic absorption spectrometry (W-coil ET-AAS) was used with cloud point extraction (CPE) for the ultrasensitive determination of cadmium in rice and water samples. When the temperature of the extraction system is higher than the cloud point temperature of the selected surfactant Triton X-114, the complex of cadmium with dithizone can be quantitatively extracted into the surfactant-rich phase and subsequently separated from the bulk aqueous phase by centrifugation. The main factors affecting the CPE, such as concentration of Triton X-114 and dithizone, pH, equilibration temperature and incubation time, were optimized for the best extract efficiency. Under the optimal conditions, the limits of detection for cadmium by W-coil ETV-AFS and W-coil ET-AAS were 0.01 and 0.03 {mu}g L{sup -1}, with sensitivity enhancement factors of 152 and 93, respectively. The proposed methods were applied to the determination of cadmium in certified reference rice and water samples with analytical results in good agreement with certified values.

  11. Determination of Metal Ions in Environmental Samples by Matrix-Assisted Microwave Induced Plasma Surface Sampling Atomic Emission Spectrometry%基体辅助微波诱导等离子体表面进样原子发射光谱检测环境样品

    Institute of Scientific and Technical Information of China (English)

    袁欣; 段忆翔

    2015-01-01

    采用基体辅助等离子体表面进样原子发射光谱技术对环境样品中的13种金属元素( Ag, Au, Ba, Cd, Cr, Cu, Eu, La, Mn, Ni, Pb, Sr, Y)进行检测。实验采用滤纸作为样品基体,样品直接滴加在滤纸上。将等离子体射流尾焰烧蚀滤纸表面,滤纸受热燃烧并释放出燃烧热,样品在等离子体辐射热和滤纸燃烧热的共同作用下原子化并激发,即可得到样品的特征光谱。液/固态样品均采用表面进样的方式实现样品引入,无需复杂的流动进样系统,并简化了繁琐的样品处理过程。本方法具有分析速度快(≤15 s)、用样量少(微升/微克级)、装置简洁、操作简单等优点,可实现对大量环境样品的现场高通量分析。在实验优化条件下,样品体积为1μL 时,本方法对以上13种元素的检出限为1.0~88 ng/mL,相对标准偏差为2.3%~6.8%(n=10)。该技术成功用于水样、土壤、海底沉积物等环境样品中金属元素的分析,结果均与理论值吻合。%A novel method for the determination of metallic elements in environmental samples was developed based on the matrix-assisted plasma surface sampling atomic emission spectrometry ( AES system) . A piece of filter paper was used as sample substrate. By direct interaction of the plasma tail plume with the filter paper surface, the filter paper absorbed energy from the plasma source and released combustion heating to the analytes originally present on its surface, thus to promote the atomization and excitation process. Surface sampling was performed in both cases of liquid and solid state analytes. Therefore, no flow injection system was required and sample pretreatment process was simplified. The proposed method provides several advantages, including fast analysis speed ( about 240 samples/h ) , little sample consumption (μL or μg level) , simplicity in instrument design, and also ease of system operation. These advantages made it attractive as a

  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. 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...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-04-15

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

  15. Literature study of microwave-assisted digestion using electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Chakraborty, R; Das, A K; Cervera, M L; De La Guardia, M

    1996-05-01

    The literature on the use of microwave-assisted digestion procedures for subsequent sample analysis by means of electrothermal atomic absorption spectrometry (ETAAS) is reviewed. The literature survey reveals that this digestion technique has been applied mainly for biological materials. The elements most extensively determined by this method are cadmium and lead followed by copper, chromium, nickel and iron. The microwave digestion conditions, ETAAS furnace programmes and analytical details of the developed methodologies have been carefully revised.

  16. Determination of Trace Iron in High Purity Sodium Fluoride by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A method is described for the direct determination of iron in high purity sodium fluoride using graphite furnace atomic absorption spectrometry. Interferences caused by the matrix are investigated. It is shown that the ashing temperature can be increased to 1 400°C and matrix interferences eliminated, the sensi tivity of iron increased in 1.27 fold by the addition of nickel nitrate. The method is applied to the determina tion of iron in sodium fluoride and satisfactory results are obtained.

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

    OpenAIRE

    Turlakiewicz, Z; Jakubowski, M.; Chmielnicka, J

    1985-01-01

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

  18. EVALUATION OF HEAVY METALS CONTENT IN EDIBLE MUSHROOMS BY MICROWAVE DIGESTION AND FLAME ATOMIC ABSORPTION SPECTROMETRY

    OpenAIRE

    Cristiana Radulescu; Claudia Stihi; Valerica Gh. Cimpoca; Popescu, Ion V.; Gabriela Busuioc; Ana Irina Gheboianu

    2011-01-01

    The aim of this work was to determine the heavy metal (Cd, Cr, Ni, Pb, Mn, Zn, Fe and Cu) content of the fruiting bodies (cap and stipe) of four species (Amanita caesarea, Pleurotus ostreatus, Fistulina hepatica and Armillariella mellea) and their substrate, collected from forest sites in Dâmboviţa County, Romania. The elements were determined by Flame Atomic Absorption Spectrometry (FAAS) after microwave assisted digestion. From the same collecting point were taken n = 5 samples of young and...

  19. Atomization mechanisms and gas phase reactions in graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Frech, W.; Lindberg, A.O.; Lundberg, E.; Cedergren, A.

    1986-04-01

    The amounts of carbon monoxide as well as the total amounts of hydrocarbons generated in different types of graphite tubes were investigated under various experimental conditions. Depending on whether or not a matrix like 50 ..mu..g of sodium nitrate was added the amount of carbon monoxide formed during atomization at 1,700 K in a pyrocoated tube was in the range 60 to 600 nmoles when using a thermal pretreatment temperature of 1,200 K. The corresponding values for an uncoated tube were 250 to 1,300 nmoles. The effect of carbon monoxide on the atomization behaviour of silver, bismuth, chromium, copper and lead was investigated experimentally and the results were evaluated by means of thermodynamically based models. In accordance with theoretical predications, only lead, bismuth and chromium, which are assumed to be atomized by oxide decomposition, showed substantial shifts in their appearance temperatures in different gas mixtures, and changes in activation energies.

  20. 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.

  1. 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.

  2. Field-emission spectroscopy of beryllium atoms adsorbed on tungsten

    Energy Technology Data Exchange (ETDEWEB)

    Czyzewski, J.J.; Grzesiak, W.; Krajniak, J. (Politechnika Wroclawska (Poland))

    1981-01-01

    Field emission energy distributions (FEED) have been measured for the beryllium-tungsten (023) adsorption system over the 78-450 K temperature range. A temperature dependence of the normalized half-width, ..delta../d, of FEED peaks changed significantly due to beryllium adsorption; and the curve, ..delta../d vs p, for the Be/W adsorption system was identical in character to the calculated curve based on the free electron model in contrast to the curve for the clean tungsten surface. In the last part of this paper Gadzuk's theory of the resonance-tunneling effect is applied to the beryllium atom on tungsten. Experimental and theoretical curves of the enhancement factor as a function of energy have been discussed.

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

    Science.gov (United States)

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

    2016-11-01

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

  4. Chemical Characterisation of Bulk and Melt-spun Ribbons of NiMnIn Alloy using Inductively Coupled Plasma Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    S.S. Kalyan Kamal

    2011-05-01

    Full Text Available Method development for the analysis of NiMnIn, a new magnetocaloric effect (MCE material using inductively-coupled plasma optical emission spectrometry (ICPOES is discussed. Spectral interference of Ni and Mn on the analysis of In were studied. The process of method validation was carried out using various analytical techniques like conventional wet chemical techniques and instrumental techniques such as atomic absorption spectrometry. All the techniques show a close agreement in values, thus this method could be applied for regular analysis of NiMnIn alloys. A comparative chemical analysis of bulk and melt-spun ribbons of this alloy is also discussed.

  5. 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

  6. 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.

  7. Determination of elements in tea seeds by inductively coupled plasma atomic emission spectrometry%电感耦合等离子体发射光谱(ICP-OES)法快速测定茶叶籽中多种元素

    Institute of Scientific and Technical Information of China (English)

    董海胜; 臧鹏; 王妮; 黄贱英

    2014-01-01

    Objective To analyze the etal elements in tea seed, so as to provide a reference for tea seed utilization. Methods Rapid quantitative analysis for elements As, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Pb, Se and Zn in tea seeds was carried out by the high-pressure sealed microwave digestion combined with inductively coupled plasma atomic emission spectrometry. Results The content of each element in tea seed were as fol-lowing:Mg (1652.23 mg/kg), Ca (1 026.36 mg/kg), Mn (122.44 mg/kg), Na (37.77 mg/kg) , Cr (7.58 mg/kg), Cu (9.11 mg/kg), Fe (58.17 mg/kg), Zn (17.59 mg/kg) and K (9191.29 mg/kg), while, As, Cd, Pb and Se were not detected. Method recoveries for all the elements used in this research were between 89%and 113%. Con-clusion The method established in this research satisfies the analysis requirements of element in tea seed. Contents of potassium, magnesium and calcium are of high lever in tea seed, while sodium content is relatively low. Tea seed is rich in minor elements such as manganese, iron, zinc and chromium.%目的:对茶叶籽中金属元素进行分析,为茶叶籽综合利用提供参考。方法采用高压密闭微波消解结合电感耦合等离子体发射光谱法对茶叶籽中As、Ca、Cd、Cr、Cu、Fe、K、Mg、Mn、Na、Pb、Se及Zn等元素进行了同时快速定量分析。结果茶叶籽中各元素含量: Mg(1652.23 mg/kg)、Ca(1026.36 mg/kg)、Mn(122.44 mg/kg)、Na(37.77 mg/kg)、Cr(7.58 mg/kg)、Cu(9.11 mg/kg)、Fe(58.17 mg/kg)、Zn(17.59 mg/kg)、K (9191.29 mg/kg)。As、Cd、Pb及Se未检出。方法加标回收率89%~113%。结论此方法满足茶叶籽样品中所述元素的分析要求。茶叶籽中钾、镁及钙含量较高,钠含量相对较低;锰、铁、锌及铬元素含量丰富。

  8. 溴-甲醇提取-电感耦合等离子体原子发射光谱法测定红土镍矿还原产物中金属镍%Determination of metallic nickel in reducing products of nickel laterite ore by inductively coupled plasma atomic emission spectrometry after bromine-methanol extraction

    Institute of Scientific and Technical Information of China (English)

    李博; 王华; 魏永刚

    2011-01-01

    The metallic nickel in reducing products of nickel laterite ore was extracted by bromine-methanol. After filtering and separating the insoluble residue, the filtrate was evaporated to dryness. The residual was then dissolved in hydrochloric acid. The 231. 604 nm was selected as analytical spectral line of nickel. The content of nickel in solution was determined by inductively coupled plasma a-tomic emission spectrometry under optimal instrumental conditions. Hence, the content of metallic nickel could be calculated. The influence of sample size, extraction time, bromine concentration, dosage of bromine-methanol and interference elements on determination results was studied. Moreover, the sample analysis and recovery test were performed. The results showed that, when the sample size was smaller than 0.1 mm, and the metallic nickel was extracted with 100 mL of 5 % (V/V) bromine-methanol for 90 min, the determination results were best. Under this condition, some other active metal elements such as magnesium, aluminum and iron could be also extracted. Since their spectral lines would be overlapped with that of nickel, the determination of nickel would be affected. However, the interference could be eliminated by background correction method. The proposed method was applied to the determination of metallic nickel in reducing products of nickel laterite ore. The relative standard deviations (RSD) of determination results were in the range of 0. 96 % -5. 9 %. The recoveries of standard addition were 97. 8% -103. 8%.%采用溴-甲醇提取红土镍矿还原产物中金属镍,过滤分离不溶残渣,滤液蒸干后用盐酸溶解,选择231.604nm作为镍的分析谱线,在最佳的仪器条件下用电感耦合等离子体原子发射光谱法测定溶液中镍的含量,然后通过计算得出金属镍的含量.研究了样品粒度、提取时间、溴浓度、溴-甲醇用量、干扰元素对测定结果的影响,并进行了样品分析和回收率实验.结

  9. 电感耦合等离子体发射光谱法测定镍矿石中镍铝磷镁钙%Determination of Ni, AI, P, Mg and Ca in Nickel Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    张超; 李享

    2011-01-01

    The simultaneous determination of Ni, Al, P, Mg, and Ca in nickel ores by inductively coupled plasma atomic emission spectrometry (ICP-AES) has been developed and is described in this paper. The sample was dissolved in nitric acid with hydrofluoric acid as flux. Perchloric acid was added and heated in order to remove hydrofluoric acid. After dissolving the salts with hydrochloric, Ni, Al, P, Mg and Ca were determined by ICP-AES. The selected spectral lines forNi, Al, P, Mg and Ca were 221. 6 nm, 396.1 nm, 178. 2 nm, 285. 2 nm and 393. 3 nm, respectively. The matrix effect was corrected by adding the same amount of Fe as the measured sample into the standard curve. The recoveries were 98. 00% -100.50%. The precisions of Ni, Al, P, Mg and Ca were all less than 1 % and the detection limits were 0. 0054 μg/mL, 0. 0028 μg/mL, 0. 0060 μg/mL, 0. 0030 μg/mL and 0. 0013 μg/mL, respectively. Compared with other methods, this method increased sensitivity and decreased the detection limit. It was applied to the determination of nickel ores from Indonesia, and the measured results were consistent with the standard values and RSD was below 1 % ( n = 6 ).%样品用硝酸溶解,氢氟酸助溶,高氯酸冒烟除去氢氟酸,盐酸溶解盐类后,在选定的测量条件下用电感耦合等离子体发射光谱法( ICP - AES)测定镍矿中镍、铝、磷、镁、钙.选择Ni 221.6 nm、Al 396.1nm、P 178.2 nm、Mg 285.2 nm、Ca 393.3 nm分别作为镍、铝、磷、镁、钙的分析线;通过在标准曲线中加入与待测样品等量的铁,消除基体干扰的影响.方法回收率为98.0% ~ 100.5%,镍、铝、磷、镁、钙的精密度均小于1%,检出限分别为0.0054、0.0028、0.0060、0.0030、0.0013 μg/mL.与同类ICP - AES方法比较,本法灵敏度提高,检出限降低.方法用于测定印度尼西亚的两批次镍矿石样品,结果与化学法的测定值基本一致,相对标准偏差小于1%(n=6).

  10. Determination of platinum and palladium in copper leaching residue by inductively coupled plasma atomic emission spectrometry with lead fire assaying%铅试金-电感耦合等离子体原子发射光谱法测定铜浸出渣中铂钯

    Institute of Scientific and Technical Information of China (English)

    魏巍; 柴徐彬

    2015-01-01

    Platinum and palladium in copper leaching residue were captured into gold-silver composite granule by lead fire assaying method. Then, the gold-silver composite granule was dissolved with nitric acid (1+7). After the solution was pouring out, the residues were dissolved with aqua regia(1+1). Merging the solutions above, the hy-drochloric acid (1+1) was added to precipitate the silver. After filtration, the content of platinum and palladium in filtrate was determined. Thus, a method was established for determination of platinum and palladium in copper leaching residue by inductively coupled plasma atomic emission spectrometry ( ICP-AES) . The interference tests of gold and silver in gold-silver composite granule indicated that the absorption of platinum and palladium by silver chloride precipitate could be eliminated through continuous stirring in precipitation process. Meanwhile, gold in so-lution had no interference with the determination. The proposed method was applied to the determination of copper leaching residue actual samples. The relative standard deviations of the results (RSD, n=11) were 5. 6%-9. 7%, and the recoveries were between 94% and 104%. The content of platinum and palladium in control samples of cop-per leaching residue was determined by proposed method. The results were consistent with the reference values.%采用铅试金法将铜浸出渣中的铂和钯捕集于金银合粒中,用硝酸(1+7)溶解金银合粒,倾出硝酸溶解液,用王水(1+1)溶解剩余的残渣,合并两次溶解液,加入盐酸(1+1)沉淀银,过滤,对溶液中铂和钯进行测定,建立了电感耦合等离子体原子发射光谱法( ICP-AES )测定铜浸出渣中铂和钯的分析方法。金银合粒中金和银的干扰试验表明:在沉淀过程中不断搅拌可消除氯化银沉淀对铂和钯吸附的影响,同时溶液中的金对测定不产生干扰。方法用于铜浸出渣实际样品分析,测得结果的相对标准偏差(RSD,n=11)为5.6%~9.7%,

  11. Determination of Cr, V and P in Ilmenite by Inductively Coupled Plasma-Atomic Emission Spectrometry with Sodium Peroxide Fusion%过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铁矿中铬磷钒

    Institute of Scientific and Technical Information of China (English)

    王卿; 赵伟; 张会堂; 周长祥; 回寒星

    2012-01-01

    An analytical method for the determination of trace elements of Cr, P and V in ilmenite with sodium peroxide by Inductively Coupled Plasma-Atomic Emission Spectrometry ( ICP-AES ) is proposed. The sample was digested by sodium peroxide fusion following which, the clear top solution was acidized to measure Cr, P and V by ICP-AES. The optimum instrumental conditions and selection of spectral lines for the elemental analysis were studied. The large dilution of 1000 and calibration standard solution by adding sodium as the matrix were conducted to eliminate the matrix effect. 2 mL HC1 was loaded to acidize the sample solution in order to avoid eroding the machines sampling system by the strong basicity of the solution by sodium peroxide fusion. The detection limit of this method was 4.46 -23.55 fig/g. According to the validation by national standard materials, the accuracy of the method (relative error) was less than 10% , and precision (RSD, n = 12) was 0.68% to 9. 90%. Compared with the spectrophotometer method for single element determination, this method showed many advantages, such as a low detection limit, high sensitivity, a wide measuring range, convenient operation, and was suitable for batch samples.%样品经过氧化钠碱熔,溶解后的上层清液直接酸化,用电感耦合等离子体发射光谱测定钛铁矿中铬、磷、钒的含量.确定了钛铁矿石中Cr、P、V的分析谱线、光谱级次;为了消除钠盐基体的影响,确定稀释因子为1000,标准曲线基体与样品基体保持一致;为避免过氧化钠熔矿后溶液碱性较大对选样系统造成腐蚀,加入2.00 mL盐酸对溶液进行酸化.方法检出限为4.46 ~23.55μg/g,采用国家一级标准物质进行验证,方法准确度小于10%,精密度为0.68%~9.90%.本法与分光光度法单一元素测定相比较,具有测量范围宽、结果准确、操作简便、省时省力、适合大批量样品测定等突出的优点.

  12. Characterization of polycyclic aromatic hydrocarbon emissions in the particulate phase from burning incenses with various atomic hydrogen/carbon ratios

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Tzu-Ting, E-mail: d89844001@ntu.edu.tw [Department of Environmental Engineering and Health, Yuanpei University, No. 306, Yuanpei St., Hsin Chu, 300, Taiwan (China); Lin, Shaw-Tao [Department of Applied Chemistry, Providence University, 200 Chung-Chi Rd., Salu Dist., Taichung City 43301, Taiwan (China); Lin, Tser-Sheng [Department of Safety, Health, and Environmental Engineering, National United University, 2 Lien Da, Maioli, 360, Taiwan (China); Hong, Wei-Lun [Department of Environmental Engineering and Health, Yuanpei University, No. 306, Yuanpei St., Hsin Chu, 300, Taiwan (China)

    2012-01-01

    Polycyclic aromatic hydrocarbons in the particulate phase generated from burning various incense was investigated by a gas chromatography/mass spectrometry. Among the used incenses, the atomic H/C ratio ranged from 0.51 to 1.69, yielding the emission factor ranges for total particulate mass and PAHs of 4.19-82.16 mg/g and 1.20-9.50 {mu}g/g, respectively. The atomic H/C ratio of the incense was the key factor affecting particulate mass and the PAHs emission factors. Both the maximum emission factor and the slowest burning rate appear at the H/C ratio of 1.57. The concentrations of the four-ring PAHs predominated and the major species among the 16 PAHs were fluoranthene, phenanthrene, pyrene, and chrysene for most incense types. The benzo[a]pyrene, benzo[a]anthracene, benzo[b]fluoranthene, and dibenzo[a,h]anthracene accounted for 87.08-93.47% of the total toxic equivalency emission factor. - Highlights: Black-Right-Pointing-Pointer The atomic H/C ratio of incense was the key factor affecting PAHs emission factors. Black-Right-Pointing-Pointer Burning incense with lower atomic H/C ratio minimized the production of total PAHs. Black-Right-Pointing-Pointer The BaP, BaA, BbF, and DBA accounted for 87.08-93.47% of the TEQ emission factor. Black-Right-Pointing-Pointer Special PAH ratios were regarded as characteristic ratios for burning incense.

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

    Energy Technology Data Exchange (ETDEWEB)

    Morzan, Ezequiel; Piano, Ornela; Stripeikis, Jorge; Tudino, Mabel, E-mail: tudino@qi.fcen.uba.ar

    2012-11-15

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

  14. Determination of total magnesium in biological samples using electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Hulanicki, Adam; Godlewska, Beata; Brzóska, Malgorzata

    1995-11-01

    Magnesium content is an important diagnostic parameter in medicine. It is recognized that its determination in one compartment is not sufficient for reliable information about the magnesium status in the body. In addition to the common procedures of magnesium determination in blood by flame atomic absorption spectrometry, the procedure of electrothermal atomization has also been developed and applied to the analysis of blood fractions, mononuclear cells and isolated nuclei of liver cells. Electrothermal atomization is preferred in cases where the sample size is limited and the magnesium content low. The total errors are in the order of 3-4%. Various techniques of sample pretreatment have been tested and direct dilution with 0.05 mol l -1 nitric acid was optimal when the samples were not mineralized. The calibration graph based on standards containing albumin was found to give the best results, as the form of magnesium in the samples may influence the ashing and atomization processes. Good agreement was obtained for determination of magnesium in standard serum. The results are compared with those obtained by the standard flame atomization technique.

  15. 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) are pres......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...

  16. 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.

  17. 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....../preconcentration procedures have been suggested and applied, such as liquid-liquid extraction, (co)precipitation with collection in knotted reactors, adsorption, hydride generation, or ion-exchange. Selected examples of some of these procedures will be discussed. Emphasis will be placed on the use of FI...

  18. Spontaneous Emission of an Atom in a Spacetime with Two Parallel Reflecting Boundaries

    Institute of Scientific and Technical Information of China (English)

    HUANG Tie-Tie; ZHU Zhi-Ying; ZHU Yun-Feng; YU Hong-Wei

    2009-01-01

    @@ We consider an inertial two-level atom in interaction with a real massless scalar quantum field in a spacetime between two parallel reflecting plane boundaries, and calculate the contributions of vacuum fluctuations and radiation reaction to the rate of change of the atomic energy. Our results show that there exists a regime of the separation L between the two boundaries such that the excited atom's spontaneous emission is impossible. There also exist certain values of the atom's position such that the corrections due to the presence of boundaries balance each other, so that the atom's spontaneous emission rate is the same as if there were no boundaries at all.

  19. 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.)

  20. Freon (CHF3)-assisted atomization for the determination of titanium using ultrasonic slurry sampling-graphite furnace atomic absorption spectrometry (USS-GFAAS): a simple and advantageous method for solid samples.

    Science.gov (United States)

    Asfaw, Alemayehu; Wibetoe, Grethe

    2004-06-01

    A simple and advantageous method for the determination of titanium using graphite furnace atomic absorption spectrometry with slurry sampling has been developed. Titanium is one of the refractory elements that form thermally stable carbides in the graphite tube, which leads to severe memory effects. Trifluoromethane (Freon-23) was applied in the purge gas during the atomization step or alternatively just prior to the atomization to successfully eliminate the problems of carbide formation and increase the lifetime of the furnace tube which could be used for more than 600 heating cycles. A flow rate of 40 mL min(-1) (5% of Freon in argon) was used to obtain symmetrical peaks with no tailing. However, when the gas flow rate was too high (250 mL min(-1)) the peak-tailing and memory effects reappeared. Ti was determined in various materials covering a wide range of concentrations, from 2.8 microg g(-1) to 12% (m/m) Ti. The accuracy of the method was confirmed by analyzing certified reference materials (CRMs) or by comparing the results with those obtained using inductively coupled plasma-atomic emission spectrometry (ICP-AES) after decomposition of the samples. The materials analyzed were soil, plant, human hair, coal, urban particulate matters, toothpaste, and powdered paint.

  1. Constraining Anthropogenic and Biogenic Emissions Using Chemical Ionization Mass Spectrometry

    Science.gov (United States)

    Spencer, Kathleen M.

    Numerous gas-phase anthropogenic and biogenic compounds are emitted into the atmosphere. These gases undergo oxidation to form other gas-phase species and particulate matter. Whether directly or indirectly, primary pollutants, secondary gas-phase products, and particulate matter all pose health and environmental risks. In this work, ambient measurements conducted using chemical ionization mass spectrometry are used as a tool for investigating regional air quality. Ambient measurements of peroxynitric acid (HO2NO2) were conducted in Mexico City. A method of inferring the rate of ozone production, PO3, is developed based on observations of HO2NO 2, NO, and NO2. Comparison of this observationally based PO3 to a highly constrained photochemical box model indicates that regulations aimed at reducing ozone levels in Mexico City by reducing NOx concentrations may be effective at higher NO x levels than predicted using accepted photochemistry. Measurements of SO2 and particulate sulfate were conducted over the Los Angeles basin in 2008 and are compared to measurements made in 2002. A large decrease in SO2 concentration and a change in spatial distribution are observed. Nevertheless, only a modest reduction in sulfate concentration is observed at ground sites within the basin. Possible explanations for these trends are investigated. Two techniques, single and triple quadrupole chemical ionization mass spectrometry, were used to quantify ambient concentrations of biogenic oxidation products, hydroxyacetone and glycolaldehyde. The use of these techniques demonstrates the advantage of triple quadrupole mass spectrometry for separation of mass analogues, provided the collision-induced daughter ions are sufficiently distinct. Enhancement ratios of hydroxyacetone and glycolaldehyde in Californian biomass burning plumes are presented as are concentrations of these compounds at a rural ground site downwind of Sacramento.

  2. Slurry sampling techniques for the determination of lead in Bangladeshi fish samples by electrothermal atomic absorption spectrometry with a metal tube atomizer.

    Science.gov (United States)

    Rahman, Mohammad Arifur; Kaneco, Satoshi; Suzuki, Tohru; Katsumata, Hideyuki; Ohta, Kiyohisa

    2005-05-01

    Ultrasonic slurry sampling electrothermal atomic absorption spectrometry with a metal tube atomizer has been applied to the determination of lead in Bangladeshi fish samples. The slurry sampling conditions, such as slurry stabilizing agent, slurry concentration, pyrolysis temperature for the slurried fish samples, particle size and ultrasonic agitation time, were optimized for electrothermal atomic absorption spectrometry with the Mo tube atomizer. Thiourea was used as the chemical modifier for the interference of matrix elements. The detection limit was 53 fg (3S/N). The determined amount of lead in Bangladeshi fish samples was consistent with those measured in the dissolved acid-digested samples. The advantages of the proposed methods are easy calibration, simplicity, low cost and rapid analysis.

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

    Science.gov (United States)

    Chen, Li-dan; Chen, Kai-kao

    2012-01-01

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

  4. Atomic force microscopy fishing and mass spectrometry identification of gp120 on immobilized aptamers

    Directory of Open Access Journals (Sweden)

    Ivanov YD

    2014-10-01

    Full Text Available Yuri D Ivanov,1 Natalia S Bukharina,1 Tatyana O Pleshakova,1 Pavel A Frantsuzov,1 Elena Yu Andreeva,1 Anna L Kaysheva,1,2 Victor G Zgoda,1 Alexander A Izotov,1 Tatyana I Pavlova,1 Vadim S Ziborov,1 Sergey P Radko,1 Sergei A Moshkovskii,1 Alexander I Archakov1 1Department of Personalized Medicine, Orekhovich Institute of Biomedical Chemistry of the Russian Academy of Medical Sciences, Moscow, Russia; 2PostgenTech Ltd., Moscow, Russia Abstract: Atomic force microscopy (AFM was applied to carry out direct and label-free detection of gp120 human immunodeficiency virus type 1 envelope glycoprotein as a target protein. This approach was based on the AFM fishing of gp120 from the analyte solution using anti-gp120 aptamers immobilized on the AFM chip to count gp120/aptamer complexes that were formed on the chip surface. The comparison of image contrasts of fished gp120 against the background of immobilized aptamers and anti-gp120 antibodies on the AFM images was conducted. It was shown that an image contrast of the protein/aptamer complexes was two-fold higher than the contrast of the protein/antibody complexes. Mass spectrometry identification provided an additional confirmation of the target protein presence on the AFM chips after biospecific fishing to avoid any artifacts. Keywords: gp120 HIV-1 envelope glycoprotein, aptamer, atomic force microscopy, mass spectrometry

  5. The emission of atoms and molecules accompanying fracture of single-crystal MgO

    Science.gov (United States)

    Dickinson, J. T.; Jensen, L. C.; Mckay, M. R.; Freund, F.

    1986-01-01

    The emission of particles due to deformation and fracture of materials has been investigated. The emission of electrons (exoelectron emission), ions, neutral species, photons (triboluminescence), as well as long wavelength electromagnetic radiation was observed; collectively these emissions are referred to as fractoemission. This paper describes measurements of the neutral emission accompanying the fracture of single-crystal MgO. Masses detected are tentatively assigned to the emission of H2, CH4, H2O, CO, O2, CO2, and atomic Mg. Other hydrocarbons are also observed. The time dependencies of some of these emissions relative to fracture are presented for two different loading conditions.

  6. Investigation of the atomic emission spectroscopy of F atoms and CF2 molecules in CF4 plasma processing

    Science.gov (United States)

    Jin, Huiliang; Li, Jie; Tang, Caixue; Deng, Wenhui; Chen, Xianhua

    2016-10-01

    The surface chemistry reaction involved in the processing of Atmospheric Pressure Plasma Jet (APPJ) produced from CF4 precursor has been explored. The atomic emission spectroscopy of F atoms and CF2 molecules was investigated as they contribute to substrate etching and FC film formation during APPJ processing. Optical emission spectroscopy (OES) spectra were acquired for CF4 plasma, relative concentrations of excited state species of F atoms and CF2 molecules were also dependent upon plasma parameters. The densities of F atoms increased dramatically with increasing applied RF power, whereas CF2 molecules decreased monotonically over the same power range, the subsequent electron impacted decomposition of plasma species after CF4 precursor fragmentation. The spectrum of the F atoms and CF2 molecules fallowed the same tendency with the increasing concentration of gas CF4, reaching the maximum at the 20sccm and 15sccm respectively, and then the emission intensity of reactive atoms decreased with more CF4 molecules participating. Addition certain amount O2 into CF4 plasma resulted in promoting CF4 dissociation, O2 can easily react with the dissociation product of CF2 molecules, which inhibit the compound of the F atoms, so with the increasing concentration of O2, the concentration of the CF2 molecules decreased and the emission intensities of F atoms showed the maximum at the O2/CF4 ratio of 20%. These results have led to the development of a scheme that illustrates the mechanisms of surface chemistry reaction and the affection of plasma parameters in CF4 plasma systems with respect to F and CF2 gas-phase species.

  7. Determination of cobalt, nickel, iron, niobium, tantalum, vanadium and chrome in tungsten-based hard alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry%微波消解-电感耦合等离子体原子发射光谱法测定钨基硬质合金中钴镍铁铌钽钒铬

    Institute of Scientific and Technical Information of China (English)

    成勇; 彭慧仙; 袁金红; 胡金荣

    2013-01-01

    以硝酸和磷酸(V(HNO3)∶V(H3PO4)=5∶1)作为消解试剂,采取高压密闭微波加热方法对钨钴或钨镍类钨基硬质合金样品进行消解,消解液用水定容后直接以电感耦合等离子体原子发射光谱法(ICP-AES)测定0.005%~10% Co、Ni和0.005%~1% Fe、Nb、Ta、V、Cr、Mo的含量.考察了消解试剂中的硝酸和磷酸量对试样消解的影响以及微波控制参数等最佳消解条件,建立了微波消解-无机试剂络合基体钨的样品消解方法,从而避免了因钨酸沉淀析出而导致部分待测元素损失和使用有机络合剂对光谱测定的干扰影响.实验结果表明:采用以5 min升温至130℃并保持5 min,再以5 min升温至190℃并保持15 min的消解程序,样品的消解效果较好.试验通过优选元素分析谱线,基体匹配和同步背景校正法消除了高钨基体的影响和光谱干扰,确保了方法的可靠性.背景等效浓度值从5 μg/L (Nb)至18 μg/L(Fc),元素检出限从4 μg/L (Nb)至13 μg/L (Fe).方法用于钨基硬质合金样品中上述合金或杂质元素的测定,RSD<3%,加标回收率在97%~104%之间,测定结果与国家标准方法检测结果对照一致.%The tungsten-based hard alloy samples (such as tungsten-cobalt and tungsten-nickel) were digested by high pressure closed microwave heating method using nitric acid-phosphoric acid (V(HNO3) : V(H3PO4)=5 :1) as digestion reagent. After dilution with water, the content of Co, Ni (0.005%-10%), Fe, Nb, Ta, V, Cr and Mo (0. 005%-l%) in digestion solution was directly determined by microwave digestion-inductively coupled plasma atomic emission spectrometry (ICP-AES). The effect of nitric acid and phosphoric acid concentration on sample digestion was investigated. The optimal digestion conditions such as microwave control parameters were studied. The sample digestion method by microwave digestion was established. The matrix tungsten was complexed with inorganic reagents

  8. 超声辅助萃取-电感耦合等离子体原子发射光谱仪联用同时测定水样中多种金属离子%Simultaneous determination of metal ions in water samples by ultrasound-assisted extraction coupled with inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    宋杨; 孟楚桥; 朱田; 高庆历; 聂红霞; 谭彩云; 祁艳霞; 赵前程

    2015-01-01

    目的:优化超声辅助乳化萃取结合电感耦合等离子体(inductively coupled plasma, ICP)原子发射法,同时测定水样中镉、钴、镍、锌4种金属离子。方法采用吡咯烷二硫代氨基甲酸铵(APDC)溶液作为螯合剂,超声条件下采用二氯甲烷对重金属螯合物进行萃取。优化了缓冲液的 pH 值,测定了不同加标浓度下方法的回收率。并对自来水、矿泉水、海水等水样进行了测定。结果该方法对Cd、Co、Ni、Zn 4种金属离子在200μg/L加标条件下绝对回收率为27.0%~91.0%,检出限为Cd为0.81μg/L, Co为1.03μg/L, Ni为1.28μg/L, Zn为0.14μg/L。检测实际自来水样,镉、钴、镍、锌4种金属离子相对回收率分别为96.4%、77.4%、120.2%、85.6%,所测自来水中镉、钴、镍、锌4种金属含量分别为1μg/L、0μg/L、2μg/L和146μg/L,均符合国标要求。对矿泉水中镉、钴、镍的相对回收率分别为77.8%,89.9%和74.2%。矿泉水中没有检测到镉、钴两种金属离子,镍含量为1μg/L。结论该方法适合于自来水和矿泉水中部分金属离子的测定,不适合于对海水中金属离子的测定。%Objective To optimize the ultrasonic-assisted emulsification extraction combined with inductively coupled plasma atomic emission spectrometry (ICP-OES) in order to determinate the concentration of cadmium, cobalt, nickel and zinc in water simultaneously.MethodsAmmonium pyrrolidinedithio carbamate (APDC) was used as a chelating agent, and dichloromethane was used as the extraction reagent of the heavy metal chelating ultrasonic extraction. The pH of the buffer was optimized, and the recovery of every metal ion was measured at different spiked concentration. And the concentration of metal ions in tap water, mineral water and sea water were determined. Results The absolute recovery of Cd, Co, Ni, Zn 4 kinds of metal ions in 200 μg/L spiked conditions were between 27.0%~91.0%, and the detection limits of method were Cd 0

  9. Arsenic species analysis in porewaters and sediments using hydride generation atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    LIAO Meng-xia; DENG Tian-long

    2006-01-01

    It was observed that the atomic fluorescence emission due to As(Ⅴ) could has a 10% to 40% of fluorescence emission signal during the determination of As(Ⅲ) in the mixture of As(Ⅲ) and As(Ⅴ). Besides, interferes from heavy metals such as Pb(Ⅱ),Cu(Ⅱ) can cause severe increase of the signals as compared to the insignificant effects caused by Cd(Ⅱ), Zn(Ⅱ), Mn(Ⅱ) and Fe(Ⅲ). On the basis of further studies, the masking agent of 8-hydroxyquinoline was used as an efficient agent to eliminate interference of As(Ⅴ)emission and the heavy metal of Cu2+ and Pb2+ in the measurements of arsenic species. After a series standard additions and CRM researches, a sensitive and interference-free analytical procedure was developed for the speciation of arsenic in samples ofporewaters and sediments in Poyang Lake, China.

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

    Science.gov (United States)

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

    2002-04-01

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

  11. Dynamics of secondary ion emission: Novel energy and angular spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jalowy, T. E-mail: jalowy@hsb.uni-frankfurt.de; Neugebauer, R.; Hattass, M.; Fiol, J.; Afaneh, F.; Pereira, J.A.M.; Collado, V.; Silveira, E.F. da; Schmidt-Boecking, H.; Groeneveld, K.O

    2002-06-01

    A new spectrometer has been developed based on the combination of standard time-of-flight technique and position sensitive delay line detectors. The basic features of the spectrometer, particularly of the multi-hit capable detector, are described. To demonstrate the performance of this new system, the dynamic emission characteristics, i.e. the three-dimensional velocity distribution, of desorbed H{sub 2}{sup +} from Al target by Ar{sup 0} impact (570 keV) is presented. It is found that the desorption yield is maximum for radial and axial emission velocities at 1.2 and 12 km/s respectively, corresponding to 1.5 eV ions emitted at 57 deg. to normal (following the projectile radial direction). The initial energy distribution spreads out over 16 eV.

  12. Dynamics of secondary ion emission Novel energy and angular spectrometry

    CERN Document Server

    Jalowy, T; Hattass, M; Fiol, J; Afaneh, F; Pereira, J A M; Collado, V; Silveira, E F D; Schmidt-Böcking, H; Groeneveld, K O

    2002-01-01

    A new spectrometer has been developed based on the combination of standard time-of-flight technique and position sensitive delay line detectors. The basic features of the spectrometer, particularly of the multi-hit capable detector, are described. To demonstrate the performance of this new system, the dynamic emission characteristics, i.e. the three-dimensional velocity distribution, of desorbed H sub 2 sup + from Al target by Ar sup 0 impact (570 keV) is presented. It is found that the desorption yield is maximum for radial and axial emission velocities at 1.2 and 12 km/s respectively, corresponding to 1.5 eV ions emitted at 57 deg. to normal (following the projectile radial direction). The initial energy distribution spreads out over 16 eV.

  13. Detection of emissions from surfaces using ion mobility spectrometry.

    Science.gov (United States)

    Vautz, Wolfgang; Baumbach, Jörg Ingo; Uhde, Erik

    2006-02-01

    Emissions from surfaces (from furniture, wall paintings or floor coverings for instance) significantly influence indoor air quality and therefore the wellbeing or even the health of the occupants. Together with metabolites from mold they are responsible for the well-known "sick building syndrome". Therefore, it is in the interest of the manufacturer as well as of the occupants to have a fast and accurate method for the detection of substances relevant to this syndrome in order to be able to monitor and control product quality and indoor air quality. The use of small and easy-to-transport ion mobility spectrometers that use UV light as the ionization source enables rapid in situ detection of such substances with high selectivity and sensitivity (detection limits in the lower ppb range). If a multicapillary column is used for preseparation as well, the selectivity is increased and the unwanted influence of humidity on the spectra can be eliminated, thus enabling the use of the instruments under normal ambient conditions. Furthermore, the use of air as carrier gas avoids the need for other sources of high-purity gas. An emission cell with a homogeneous and constant air flow over the surface to be investigated was developed in order to ensure reproducible results. Investigations of emissions from wooden surfaces with and without additional contamination as well as from complex mixtures are presented. The results demonstrate that relevant emissions can be identified and quantified with high sensitivity and selectivity in under five minutes. Therefore, the method is useful for indoor air quality monitoring, especially when miniaturized instruments are applied.

  14. Atomic force microscope controlled topographical imaging and proximal probe thermal desorption/ionization mass spectrometry imaging.

    Science.gov (United States)

    Ovchinnikova, Olga S; Kjoller, Kevin; Hurst, Gregory B; Pelletier, Dale A; Van Berkel, Gary J

    2014-01-21

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

  15. Development of rapid slurry methods for flame and direct current plasma emission and graphite furnace atomic absorption analysis of solid animal tissue

    Energy Technology Data Exchange (ETDEWEB)

    Fietkau, R.

    1986-01-01

    Studies are presented describing developments in the rapid, direct atomic spectrochemical analysis of meat samples by the technique of slurry atomization. The number of elements that can be determined in meat slurry samples has been increased and the concentration range that can be detected extended to included analysis at the part per billion as well as the percent level. Slurry atomization involves the rapid preparation procedure whereby the sample is simple homogenized with deionized distilled water prior to analysis. In this manner, rapid, quantitative analysis of hot dogs (processed meat) for dietary salt (Na, K) was achieved by premixed air-natural gas flame emission spectrometry. Quantitative analysis of mechanically separated meat for residual bone fragments (as Ca) was attained using a simple photometer when the premixed air-acetylene flame was used. The phosphate interference of the Ca emission signal was overcome by placing an insert in the spray chamber which decreased the droplet size of the aerosol reaching the flame. Slight matrix modification in the form of 2% nitric acid was necessary to solubilize the Ca from the bone fragments. Determining elements present at very low concentrations i.e. part per billion levels, in homogenized beef liver was evaluated using graphite furnace atomic absorption and shown to be viable for determinations of Pb, Cd, Cr, and Ni. Qualitative multielement analysis of several types of meat slurries by direct current plasma (DCP) emission spectrometry using both photographic and electronic modes of detection was reported for the first time.

  16. Non-dispersive atomic-fluorescence spectrometry of trace amounts of bismuth by introduction of its gaseous hydride into a premixed argon (entrained air)-hydrogen flame.

    Science.gov (United States)

    Kobayashi, S; Nakahara, T; Musha, S

    1979-10-01

    A method has been developed for the determination of bismuth by generation of its gaseous hydride and introduction of the hydride into a premixed argon (entrained air)-hydrogen flame, the atomic-fluorescence lines from which are all detected by use of a non-dispersive system. The detection limit is 5 pg/ml, or 0.1 ng of bismuth, but the reagent blank found in a 20-ml sample volume was approximately 2 ng of bismuth. Analytical working curves obtained by measuring peak-heights and integrated peak-areas of the signals are linear over a range of about four orders of magnitude from the detection limit. Perchloric, phosphoric and sulphuric acids up to 2.0M concentration give no interference, but nitric acid gives slight depression of the signal. The presence of silver, gold, nickel, palladium, platinum, selenium and tellurium in 1000-fold ratio to bismuth causes pronounced depression of the signal, whereas mercury and tin slightly enhance the atomic-fluorescence signal. The method has been applied to the determination of bismuth in aluminium-base alloys and sulphide ores with use of the standard additions method. The results are in good agreement with those obtained by flame atomic-absorption spectrometry and optical emission spectrometry with an inductively coupled plasma.

  17. 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)

  18. Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2008-01-01

    Full Text Available A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU, copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS. Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4 of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

  19. Preconcentration and Determination of Chromium Species Using Octadecyl Silica Membrane Disks and Flame Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    MOGHIMI Ali; SABER-TEHRANI Mohammad; WAQIF-HUSAIN Syed; MOHAMMADHOSSEINI Majid

    2007-01-01

    A novel and selective method for the fast determination of trace amounts of chromium species in water samples has been developed.The procedure is based on the selective formation of chromium diethyldithiocarbamate complexes at different pH in the presence of Mn(Ⅱ) as an enhancement agent of chromium signals followed by elutionwith organic eluents and determination by atomic flame absorption spectrometry.The maximum capacity of the employed disks was found to be (3964±3) μg and (376±2) μg for Cr(Ⅲ) and Cr(Ⅵ),respectively.The detection limit of the proposed method is 49 and 43 ng·L-1 for Cr(Ⅲ) and Cr(Ⅵ),respectively.The proposed method was successfully applied for determination of chromium species Cr(Ⅲ) and Cr(Ⅵ) in different water samples.

  20. Preconcentration of Vanadium(Ⅴ) on Crosslinked Chitosan and Determination by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol*L-1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0-12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg*L-1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.

  1. [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.

  2. Determination of sodium in foods by flame atomic absorption spectrometry after microwave digestion: NMKL interlaboratory study.

    Science.gov (United States)

    Julshamn, Kaare; Lea, Per; Norli, Hilde Skaar

    2005-01-01

    Nine laboratories participated in an interlaboratory method performance (collaborative) study of a method for the determination of sodium in foods by flame atomic absorption spectrometry after wet digestion, using a microwave oven technique. Before the study, the laboratories were able to practice on samples with defined sodium levels (pretrial test). The method was tested on a total of 6 foods (broccoli, carrot, bread, saithe fillet, pork, and cheese) with sodium concentrations of 1480-8260 mg/kg. The materials were presented to the participants in the study as blind duplicates, and the participants were asked to perform single determinations for each sample. The repeatability relative standard deviations (RSDr) for sodium ranged from 1.9 to 6.5%. The reproducibility relative standard deviations (RSDR) ranged from 4.2 to 6.9%. The HorRat values ranged from 0.9 to 1.6.

  3. Determination of barium in bottled drinking water by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Fagioli, F.; Locatelli, C.; Lanciotti, E.; Vallone, G.; Mazzotta, D.; Mugelli, A.

    1988-11-01

    In relation to the wide environmental spread of barium and to its cardiovascular effects, barium levels were determined by graphite furnace atomic absorption spectrometry in 60 different brands of bottled water marketed in Italy. Matrix interferences were investigated in order to evaluate the use of an analytical calibration function rather than the much more time consuming addition technique. The barium content ranged from limit of detection C/sub L/ (7.0 ..mu..g/1) up to 660 ..mu..g/1, the median value being 80 ..mu..g/l, while the recovery tests varied between 90 and 110% and the precision of the method (s/sub yx/) was 2.5%.

  4. [Atomic force microscopy fishing of gp120 on immobilized aptamer and its mass spectrometry identification].

    Science.gov (United States)

    Bukharina, N S; Ivanov, Yu D; Pleshakova, T O; Frantsuzov, P A; Andreeva, E Yu; Kaysheva, A L; Izotov, A A; Pavlova, T I; Ziborov, V S; Radko, S P; Archakov, A I

    2015-01-01

    A method of atomic force microscopy-based fishing (AFM fishing) has been developed for protein detection in the analyte solution using a chip with an immobilized aptamer. This method is based on the biospecific fishing of a target protein from a bulk solution onto the small AFM chip area with the immobilized aptamer to this protein used as the molecular probe. Such aptamer-based approach allows to increase an AFM image contrast compared to the antibody-based approach. Mass spectrometry analysis used after the biospecific fishing to identify the target protein on the AFM chip has proved complex formation. Use of the AFM chip with the immobilized aptamer avoids interference of the antibody and target protein peaks in a mass spectrum.

  5. Selenosugar determination in porcine liver using multidimensional HPLC with atomic and molecular mass spectrometry.

    Science.gov (United States)

    Lu, Ying; Pergantis, Spiros A

    2009-01-01

    A methodology based on liquid chromatography coupled online with atomic and molecular mass spectrometry was developed for identifying trace amounts of the selenosugar methyl 2-acetamido-2-deoxy-1-seleno-β-D-galactopyranoside (SeGalNAc) in porcine liver, obtained from an animal that had not received selenium supplementation. Sample preparation was especially critical for the identification of SeGalNAc by molecular mass spectrometry. This involved liver extraction using a Tris buffer, followed by sequential centrifugations. The resulting cytosolic fraction was pre-concentrated and the low molecular weight selenium (LMWSe) fraction obtained from a size exclusion column was collected, concentrated, and subsequently analyzed using a tandem dual-column HPLC-ICP-MS system which consisted of strong cation exchange (SCX) and reversed phase (RP) columns coupled in tandem. Hepatocytosolic SeGalNAc was tentatively identified by retention time matching and spiking. Its identity was further confirmed by using the same type of chromatography on-line with atmospheric pressure chemical ionization tandem mass spectrometry operated in the selected reaction monitoring (SRM) mode. Four SRM transitions, characteristic of SeGalNAc, were monitored and their intensity ratios determined in order to confirm SeGalNAc identification. Instrument limits of detection for SeGalNAc by SCX-RP HPLC-ICP-MS and SCX-RP HPLC-APCI-MS/MS were 3.4 and 2.9 μg Se L(-1), respectively. Selenium mass balance analysis revealed that trace amounts of SeGalNAc, 2.16±0.94 μg Se kg(-1) liver (wet weight) were present in the liver cytosol, corresponding to 0.4% of the total Se content in the porcine liver.

  6. Emission of fast non-Maxwellian hydrogen atoms in low-density laboratory plasma

    Science.gov (United States)

    Brandt, Christian; Marchuk, Oleksandr; Pospieszczyk, Albrecht; Dickheuer, Sven

    2017-03-01

    The source of strong and broad emission of the Balmer-α line in mixed plasmas of hydrogen (or deuterium) and noble gases in front of metallic surfaces is a subject of controversial discussion of many plasma types. In this work the excitation source of the Balmer lines is investigated by means of optical emission spectroscopy in the plasma device PSI-2. Neutral fast non-Maxwellian hydrogen atoms are produced by acceleration of hydrogen ions towards an electrode immersed into the plasma. By variation of the electrode potential the energy of ions and in turn of reflected fast atoms can be varied in the range of 40-300 eV. The fast atoms in front of the electrode are observed simultaneously by an Echelle spectrometer (0.001 nm/channel) and by an imaging spectrometer (0.01 nm/channel) up to few cm in the plasma. Intense excitation channels of the Balmer lines are observed when hydrogen is mixed with argon or with krypton. Especially in Ar-H and Ar-D mixed plasmas the emission of fast hydrogen atoms is very strong. Intermixing hydrogen with other noble gases (He, Ne or Xe) one observes the same effect however the emission is one order of magnitude less compared to Kr-H or Kr-D plasmas. It is shown, that the key process, impacting this emission, is the binary collision between the fast neutral hydrogen atom and the noble gas atom. Two possible sources of excitation are discussed in details: one is the excitation of hydrogen atoms by argon atoms in the ground state and the second one is the process of the so-called excitation transfer between the metastable states of noble gases and hydrogen. In the latter case the atomic data for excitation of Balmer lines are still not available in literature. Further experimental investigations are required to conclude on the source process of fast atom emission.

  7. 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

  8. 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,…

  9. 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…

  10. Evaluation of the mineral profile of textile materials using inductively coupled plasma optical emission spectrometry and chemometrics

    Energy Technology Data Exchange (ETDEWEB)

    Menezes, E.A.; Carapelli, R.; Bianchi, S.R. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Embrapa Pecuaria Sudeste, C.P. 339, Sao Carlos, SP 13560-970 (Brazil); Souza, S.N.P. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Matos, W.O. [Departamento de Quimica Analitica e Fisico-Quimica, Universidade Federal do Ceara, Fortaleza, CE (Brazil); Pereira-Filho, E.R. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Nogueira, A.R.A., E-mail: anarita@cppse.embrapa.br [Embrapa Pecuaria Sudeste, C.P. 339, Sao Carlos, SP 13560-970 (Brazil)

    2010-10-15

    The content of Al, Ba, Ca, Cr, Cu, Fe, Ni, P, Zn, Cd and Pb was determined in textile material samples after microwave-assisted decomposition in a cavity oven and extraction with an artificial sweat solution. Radial viewing inductively coupled plasma optical emission spectrometry (ICP OES) was the main detection technique, but Cd and Pb were determined by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to increase the sensitivity. Principal components analysis (PCA) was applied to the data sets to characterize the samples with respect to their geographic origin and color difference. The PCA for Brazilian single-color samples showed separation, with one group consisting of blue and green textiles and another with all the other materials evaluated. The geographic origin study showed a clear separation between Brazilian and Chinese textiles. The metals amount extracted with sweat extractable solution were lower than limits values pointed by the International Testing and Certification System for Textiles, Oko Tex Standard 100, in the all considered classes. Recoveries varied from 85 to 112% for additions ranging from 3.0 to 25 mg kg{sup -1} for Ca and from 0.3 to 7.0 mg kg{sup -1} for all other analytes through the microwave-assisted decomposition procedure.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-02-11

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

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

    Science.gov (United States)

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

    2012-05-01

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

  13. Determination of lead in fine particulates by slurry sampling electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Yu, J C; Ho, K F; Lee, S C

    2001-01-02

    A simple method for determining lead in fine particulates (PM2.5) by using electrothermal atomic absorption spectrometry (ETAAS) has been developed. Particulates collected on Nuclepore filter by using a dichotomous sampler were suspended in diluted nitric acid after ultrasonic agitation. The dislodging efficiency is nearly 100% after agitation for 5 min. In order to study the suspension behavior of PM2.5 in solvents, a Brookhaven ZetaPlus Particle Size Analyzer was used to determine the particle size distribution and suspension behavior of air particulates in the solvent. The pre-digestion and modification effect of nitric acid would be discussed. Palladium was added as a chemical modifier and the temperature program of ETAAS was changed in order to improve the recovery. The slurry was introduced directly into a graphite tube for atomization. The metal content in the sample was determined by the standard addition method. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling method. It offers a quick and efficient alternative method for heavy metal characterization in fine particulates.

  14. 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.

  15. X-ray emission from charge exchange of highly-charged ions in atoms and molecules

    Science.gov (United States)

    Greenwood, J. B.; Williams, I. D.; Smith, S. J.; Chutjian, A.

    2000-01-01

    Charge exchange followed by radiative stabilization are the main processes responsible for the recent observations of X-ray emission from comets in their approach to the Sun. A new apparatus was constructed to measure, in collisions of HCIs with atoms and molecules, (a) absolute cross sections for single and multiple charge exchange, and (b) normalized X-ray emission cross sections.

  16. Radiative emission of neutrino pair from nucleus and inner core electrons in heavy atoms

    CERN Document Server

    Yoshimura, M

    2013-01-01

    Radiative emission of neutrino pair (RENP) from atomic states is a new tool to experimentally investigate undetermined neutrino parameters such as the smallest neutrino mass, the nature of neutrino masses (Majorana vs Dirac), and their CP properties. We study effects of neutrino pair emission either from nucleus or from inner core electrons in which the zero-th component of quark or electron vector current gives rise to large coupling. Both the overall rate and the spectral shape of photon energy are given for a few cases of interesting target atoms. Calculated rates exceed those of previously considered target atoms by many orders of magnitudes.

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

    Energy Technology Data Exchange (ETDEWEB)

    Docekal, Bohumil [Institute of Analytical Chemistry, Academy of Sciences of the Czech Republic, Veveri 97, CZ-61142, Brno (Czech Republic)], E-mail: docekal@iach.cz; Vojtkova, Blanka [Institute of Materials Science, Faculty of Chemistry, Brno University of Technology, Purkynova 118, CZ-61200 Brno (Czech Republic)

    2007-03-15

    A true direct solid sampling electrothermal atomic absorption spectrometry method with Zeeman-effect background correction (Analytik Jena ZEEnit 60 AAS) was developed for the determination of As, Cd, Hg, Pb, Sb and Zn in powdered titanium dioxide of pharmaceutical, food and cosmetics grade. The interaction of the titanium matrix and graphite surface of the sample carrier boat in a transversely heated graphite tube atomizer was investigated. Conversion of titanium dioxide to interfering TiO{sub 2}-TiC-liquid phase, running out the sampling boat, was observed at temperatures above 2000 deg. C. The temperature program was optimized accordingly for these volatile analytes in atomization and cleaning steps in order to prevent this interference and to prolong significantly the analytical lifetime of the boat to more than one thousand runs. For all elements, calibration by aqueous standard addition method, by wet-chemically analyzed samples with different content of analytes and/or by dosing one sample in different amounts, were proved as adequate quantification procedures. Linear dynamic calibration working ranges can be considerably expanded up to two orders of magnitude within one measurement run by applying three-field dynamic mode of the Zeeman background correction system. The results obtained by true direct solid sampling technique are compared with those of other independent, mostly wet-chemical methods. Very low limits of detection (3{sigma} criterion) of true solid sampling technique of 21, 0.27, 24, 3.9, 6.3 and 0.9 ng g{sup -1} were achieved for As, Cd, Hg, Pb, Sb and Zn, respectively.

  18. Determination of Fe_2O_3,TiO_2 and SiO_2 in bauxite by inductivelycoupled plasma-atomic emission spectrometry%ICP-AES法测定矾土中Fe2O3、TiO2和SiO2

    Institute of Scientific and Technical Information of China (English)

    郝荷芳; 苑利

    2011-01-01

    采用四硼酸锂熔融试样,电感耦合等离子体原子发射光谱法(ICP-AES法)测定矾土中Fe2 O3、TiO2和SiO2。通过对熔样方法选择、铝基体以及背景的研究,确定了分析条件。结果表明,该法具有良好的精密度和准确性,回收率在94%~108%。%A method based on inductively coupled plasma-atomic emission spectrometry(ICP-AES) was established for the determination of Fe2O3,TiO2 and SiO2 in bauxite.The sample was melted into lithium tetraborate.The analysis conditions were obtained by studying the melted methods,Al matrix and background.The recommended method showed satisfying precision and accuracy as well.The recovery percents detected by standard addition method were in range of 94%~108%.

  19. Simulation of UV atomic radiation for application in exhaust plume spectrometry

    Science.gov (United States)

    Wallace, T. L.; Powers, W. T.; Cooper, A. E.

    1993-06-01

    Quantitative analysis of exhaust plume spectral data has long been a goal of developers of advanced engine health monitoring systems which incorporate optical measurements of rocket exhaust constituents. Discussed herein is the status of present efforts to model and predict atomic radiation spectra and infer free-atom densities from emission/absorption measurements as part of the Optical Plume Anomaly Detection (OPAD) program at Marshall Space Flight Center (MSFC). A brief examination of the mathematical formalism is provided in the context of predicting radiation from the Mach disk region of the SSME exhaust flow at nominal conditions during ground level testing at MSFC. Computational results are provided for Chromium and Copper at selected transitions which indicate a strong dependence upon broadening parameter values determining the absorption-emission line shape. Representative plots of recent spectral data from the Stennis Space Center (SSC) Diagnostic Test Facility (DTF) rocket engine are presented and compared to numerical results from the present self-absorbing model; a comprehensive quantitative analysis will be reported at a later date.

  20. Dispersive liquid–liquid microextraction combined with laser-induced breakdown spectrometry and inductively coupled plasma optical emission spectrometry to elemental analysis

    OpenAIRE

    Gaubeur, Ivanise; Aguirre Pastor, Miguel Ángel; Kovachev, Nikolay; Hidalgo Núñez, Montserrat; Canals Hernández, Antonio

    2015-01-01

    In this paper, two analytical methodologies based on the combination of dispersive liquid–liquid microextraction with inductively coupled plasma optical emission spectrometry and laser-induced breakdown spectrometry, respectively, were evaluated for simultaneous preconcentration and detection of Cd, Co, Ni, Pb and Zn. The microextraction procedure was based on the injection of appropriate quantities of 1-undecanol and methanol into the sample solution containing the complexes formed between m...

  1. Spontaneous emission spectrum of a four-level atom in a double-band photonic crystal

    Institute of Scientific and Technical Information of China (English)

    Wang Jian; Yang Dong; Zhang Han-Zhang

    2005-01-01

    The spontaneous emission spectrum from a four-level atom in a double-band photonic crystal has been investigated.We use the model which assumes three atomic transitions. One of the transitions interacts with the free vacuum modes,and the other two transitions couple to the modes of the isotropic photonic band gap (PBG), the anisotropic PBG and another free vacuum. The effects of the fine structure of the lower levels on the spontaneous emission spectrum of an atom are investigated in detail in the three cases. New features of four (two) transparencies with two (one) spontaneous emission peaks, resulting from the fine structure of the lower levels of an atom, are predicted in the case of isotropic PBG modes.

  2. 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...

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

    Science.gov (United States)

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

    2013-03-15

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

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

    Science.gov (United States)

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

    2001-10-01

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

  5. Characteristics of Spontaneous Emission of Polarized Atoms in Metal-Dielectric Multiple Layer Structures

    Institute of Scientific and Technical Information of China (English)

    ZHAO Li-Ming; GU Ben-Yuan; ZHOU Yun-Song

    2007-01-01

    The spontaneous emission (SE) progress of polarized atoms in a stratified structure ofair-dielectric(D0)-metal(M)-dielectric(D1)-air can be controlled effectively by changing the thickness of the D1 layer and rotating the polarized direction of atoms. It is found that the normalized SE rate of atoms located inside the D0 layer crucially depends on the atomic position and the thickness of the D1 layer. When the atom is located near the D0-M interface, the normalized atomic SE rate as a function of the atomic position is abruptly onset for the thin D1 layer. However, with the increasing thickness of the D1 layer, the corresponding curve profile exhibits plateau and stays nearly unchanged. The substantial change of the SE rate stems from the excitation of the surface plasmon polaritons in metal-dielectric interface, and the feature crucially depends on the thickness of D1 layer. If atoms are positioned near the D0-air interface, the substantial variation of the normalized SE rate appears when rotating the polarized direction of atoms. These findings manifest that the atomic SE processes can be flexibly controlled by altering the thickness of the dielectric layer D1 or rotating the orientation of the polarization of atoms.

  6. Chemical Characterisation of Bulk and Melt-spun Ribbons of NiMnIn alloy using Inductively Coupled Plasma Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    S.S. Kalyan Kamal

    2011-04-01

    Full Text Available Method development for the analysis of NiMnIn, a new magnetocaloric effect (MCE material using inductively coupled plasma optical emission spectrometry (ICPOES is discussed. Spectral interference of Ni and Mn on the analysis of In were studied. The process of method validation was carried out using various analytical techniques like conventional wet chemical techniques and instrumental techniques such as atomic absorption spectrometry. All the techniques show a close agreement in values, thus this method could be applied for regular analysis of NiMnIn alloys. A comparative chemical analysis of bulk and melt-spun ribbons of this alloy is also discussed.Defence Science Journal, 2011, 61(3, pp.270-274, DOI:http://dx.doi.org/10.14429/dsj.61.397

  7. Gas chromatography coupled with atomic absorption spectrometry — a sensitive instrumentation for mercury speciation

    Science.gov (United States)

    Emteborg, Håkan; Sinemus, Hans-Werner; Radziuk, Bernard; Baxter, Douglas C.; Frech, Wolfgang

    1996-07-01

    New instrumentation for the speciation of mercury is described, and is applied to the analysis of natural water samples. The separation of mercury species is effected using gas chromatography of derivatized mercury species on a widebore capillary column. The solvent is vented using a bypass valve and the separated mercury species are pyrolysed on-line at 800°C for production of mercury atoms. These are then detected by atomic absorption spectrometry (AAS) at the 253.7 and 184.9 nm lines simultaneously in a quartz cuvette. The use of the 184.9 nm line provides a more than five-fold increase in sensitivity compared with the conventional 253.7 nm line and an absolute detection limit of 0.5 pg of mercury. The dynamic range of the combined analytical lines provides a linear response over more than three orders of magnitude. A number of organic compounds not containing mercury are also detected following pyrolysis, especially at the 184.9 nm line. These background species must not co-elute at the retention times for methyl- and inorganic mercury, as otherwise a positive interference would result. By maximizing the chromatographic resolution and minimizing the band broadening in the cuvette by use of a make-up gas, the retention times of interest are freed from co-eluting background peaks. The instrumentation has been applied to the determination of ng l -1 concentrations of methyl- and inorganic mercury in Lake Constance, Germany and within the Lake Constance drinking water supply organization, Bodenseewasserversorgung (BWV). The accuracy for the sum of methyl- and inorganic mercury has been assessed by comparison with an independent method for total mercury based on AAS detection implemented at BWV. Relative detection limits using 1 litre water samples and 15 ml injections of the final hexane extract were 0.03 ng l -1 for methylmercury and 0.4 ng l -1 for inorganic mercury based on the 3j criterion.

  8. [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.

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

    Science.gov (United States)

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

    2010-03-01

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

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

    Science.gov (United States)

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

    1992-08-01

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

  11. Speciation analysis of iron in traditional Chinese medicine by flame atomic absorption spectrometry.

    Science.gov (United States)

    Li, Shun-Xing; Deng, Nan-Sheng

    2003-04-24

    In view of octanol, a long-chain alkanol, resembled as the configuration of carbohydrate and adipose in human body, the octanol-solubility and water-solubility were used to define the species of iron in medicine, to identify the lipophily and bioavailability of coordinated iron complex, and octanol-water system was adopted to study the distribution of iron in decoction of eight single medicines and compatibility of semen persicae and flos carthami in stomach and intestine. To study the effect of compatibility of medicines, the different acidity of stomach and intestine on the species of iron in phytomedicine decoction, the total concentration, octanol- and water-solubility concentration of iron in medicinal materials or decoctions under gastric and intestinal acidity, were determined, respectively, by flame atomic absorption spectrometry, analyzed and compared. The different acidity of digestive site, the different composition of medicine, and the compatibility of medicines, have greatly affected the species of iron, the pharmacological activity of coordinated iron complex in decoctions. Such factors, especially the concentration of octanol-solubility iron, could be the basis of the dosage to avoid iron overload.

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

    Energy Technology Data Exchange (ETDEWEB)

    Yaman, Mehmet [Department of Chemistry, Science and Arts Faculty, Firat University, Elazig (Turkey)]. E-mail: myaman@firat.edu.tr; Kaya, Gokce [Department of Chemistry, Science and Arts Faculty, Firat University, Elazig (Turkey)

    2005-05-17

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

  13. [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.

  14. 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}.

  15. Direct solid sampling electrothermal atomic absorption spectrometry for the analysis of high-purity niobium pentaoxide.

    Science.gov (United States)

    Huang, M D; Krivan, V

    2000-01-01

    A direct solid sampling electrothermal atomic absorption spectrometry (SoS-ETAAS) method for ultratrace analysis of powdered niobium pentaoxide for Al, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni and Zn has been developed. The elements K, Mg, Na and Zn could be determined without any chemical modification. However, in the determination of the elements Al, Co, Cr, Cu, Fe, Mn and Ni, serious matrix-caused non-spectral interferences and background occurred which made their determination impossible. This problem was remedied by conversion of the niobium pentaoxide matrix into the thermally stable niobium carbide by using methane atmosphere during the pyrolysis stage. The development resulted in establishing an extraordinary powerful method for the analysis of niobium pentaoxide in term of limits of detection, accuracy, simplicity and analysis time. Quantification was performed using calibration curves measured with aqueous standard solutions. The accuracy was checked by comparing the results with those obtained by ETAAS in analysis of slurries and digests of the sample. Due to almost complete freedom of blank and high applicable sample amounts (up to 15 mg), extremely low limits of detection (0.5-2 ng/g) were achieved.

  16. Determination of selenium and tellurium in the gas phase using specific columns and atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Muangnoicharoen, S.; Chiou, K.Y.; Manuel, O.K.

    1986-11-01

    Total selenium and tellurium in the gas phase were analyzed after adsorption on gold-coated beads and charcoal. The thermally eluting gas was trapped on columns filled with quartz beads that were cooled in an ice bath. The beads were boiled in dilute HCl, and the resulting solution was analyzed for Se and Te by graphite furnace atomic absorption spectrometry. Their results demonstrate that gold-coated beads efficiently trap gaseous Se and Te at a low gas flow rate, but at higher flow rates charcoal traps are more expedient. With charcoal traps, it was found that local air samples contain Se in the range of 0.92-3.05 ng m/sup -3/ and Te in the range of 0.10-0.34 ng m/sup -3/. Detection limits down to about 0.1 ng m/sup -3/ allow the ready detection of Se and Te in rural air with a precision of about +/- 6% at the nanogram level of Te and about +/- 4% at the nanogram level of Se.

  17. Speciation Analysis of Serum Copper by Ultrafiltration Com-bined with Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    WANG Zhi-Hua; MA Hui-Min; MA Quan-Li; LIANG Shu-Chuan

    2001-01-01

    UItrafiltration combined with graphite furnace atomic absorp-tion spectrometry(GFAAS)was used to study protein binding and speciation of copper in human serum..UItrafiltration was carried out using a cell unit ultrafiltration membraoes having a nominal cut-off of 10,000Dalton.The effects of var-ious experimental factors including the kind and concentration of electrolyte,sample storge,pH,pressure and the precon-ditioning of the membranes on the speciation analysis of serum copper by ultrafiltration were examined.It was observed that 4.5±2.3% of the total copper in serum was ultrafiltrable and this value did not seem to be influenced by the total serum ele-mental concentration,the PH (6.5——10) adn the pressure(≤1.5kg/cm2).the preconditioning of the ultrafiltration system with 0.1mol/L calcium nitrate can overcome the adsorption loss of copper effectively,and the addition of tris-HCI sohtion (pH 7.4)to serum accelerates the ultrafiltration.The present method was proved to be suitable for speciation analysis for its simplicity,rapidity,small sample reuqirement and easy con-trol.The results obtained with the method are accurate and reliable.

  18. [Determination of mercury in shark liver by cold atom fluorescence spectrometry after microwave dissolution].

    Science.gov (United States)

    Weng, Di

    2005-12-01

    The conditions for the determination of mercury in shark liver by cold atom fluorescence spectrometry (CAFS) with microwave dissolution were studied. After being dried completely, the method employed 2 mol x L(-1) HNO3-4 mol x L(-1) HCl as an oxidant, and with catalysis by V2O5, the samples were digested in a microwave oven. The mercury in absorption solution was reduced by SnCl2, and then was determined by CAFS at wavelength of 253.7 nm. 10% SnCl2 solution was used as a reductive agent for mercury. The linear range was 0-2.0 ng x mL(-1) mercury (r = 0.999 7). The detection limit was 0.05 ng x mL(-1), the relative standard deviation was 0.86%-2.22%, and the average recovery rate was 96.0%-108.5%. The method was suitable for the determination of mercury in shark liver.

  19. Use of Atomic Absorption Spectrometry in Assessment of Biomonitor Plants for Lead, Cadmium and Copper Pollution

    Institute of Scientific and Technical Information of China (English)

    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 · kg-1,respectively.Significantly increased lead concentration up to 2 750 mg · 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 angustifolia 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.

  20. 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.

  1. Novel Method for Indirect Determination of Iodine in Marine Products by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    LU Jian-ping; TAN Fang-wei; TANG Qiong; JIANG Tian-cheng

    2013-01-01

    A method for the determination of iodine based upon compound H2HgI4,formed between I-and Hg2+ in nitric acid and extracted in methyl isobutyl ketone(MIBK),was developed via atomic fluorescence spectrometry(AFS).After the compound is reduced with potassium borohydrid(KBH4),the resultant mercury vapor was injected into the instrument and iodine was,therefore,indirectly determined.Experimental parameters such as the conditions of extraction reagents,aqueous phase acidity,elemental mercury diffusion temperature in a vial and other factors were investigated and optimized.Under the optimum experimental conditions,this method shows a detection limit of 0.038 μg/L iodine and a linear relationship between 0.04-20 μg/L.The method was applied to determining the iodine content in marine duck eggs,kelps,laver and Ganoderma lucidum spirulina,showing a relative standard deviation(RSD) of 2.15% and the recoveries in the range of 98.1%-102.5%.

  2. EVALUATION OF HEAVY METALS CONTENT IN EDIBLE MUSHROOMS BY MICROWAVE DIGESTION AND FLAME ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Cristiana Radulescu

    2011-05-01

    Full Text Available The aim of this work was to determine the heavy metal (Cd, Cr, Ni, Pb, Mn, Zn, Fe and Cu content of the fruiting bodies (cap and stipe of four species (Amanita caesarea, Pleurotus ostreatus, Fistulina hepatica and Armillariella mellea and their substrate, collected from forest sites in Dâmboviţa County, Romania. The elements were determined by Flame Atomic Absorption Spectrometry (FAAS after microwave assisted digestion. From the same collecting point were taken n = 5 samples of young and mature fruiting bodies of mushrooms and their substrate. The high concentrations of lead, chrome and cadmium (Pb: 0.25 – 1.89 mg.kg-1, Cr: 0.36 – 1.94 mg.kg-1, Cd: 0.23 – 1.13 mg.kg-1 for all collected wild edible mushrooms, were determined. These data were compared with maximum level for certain contaminants in foodstuffs established by the commission of the European Committees (EC No 466/2001. A quantitative evaluation of the relationship of element uptake by mushrooms from substrate was made by calculating the accumulation coefficient (Ka. The moderately acid pH value of soil influenced the accumulation of Zn and Cd inside of the studied species. The variation of heavy metals content between edible mushrooms species is dependent upon the ability of the species to extract elements from the substrate and on the selective uptake and deposition of metals in tissue.

  3. 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.

  4. 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.

  5. Methane Oxidation to Methanol without CO2 Emission: Catalysis by Atomic Negative Ions

    CERN Document Server

    Tesfamichael, Aron; Felfli, Zineb; Msezane, Alfred Z

    2014-01-01

    The catalytic activities of the atomic Y-, Ru-, At-, In-, Pd-, Ag-, Pt-, and Os- ions have been investigated theoretically using the atomic Au- ion as the benchmark for the selective partial oxidation of methane to methanol without CO2 emission. Dispersion-corrected density-functional theory has been used for the investigation. From the energy barrier calculations and the thermodynamics of the reactions, we conclude that the catalytic effect of the atomic Ag-, At-, Ru-, and Os- ions is higher than that of the atomic Au- ion catalysis of CH4 conversion to methanol. By controlling the temperature around 290K (Os-), 300K (Ag-), 310K (At-), 320K (Ru-) and 325K (Au-) methane can be completely oxidized to methanol without the emission of CO2. We conclude by recommending the investigation of the catalytic activities of combinations of the above negative ions for significant enhancement of the selective partial oxidation of methane to methanol.

  6. Determination of cadmium and lead in edible oils by electrothermal atomic absorption spectrometry after reverse dispersive liquid-liquid microextraction.

    Science.gov (United States)

    López-García, Ignacio; Vicente-Martínez, Yesica; Hernández-Córdoba, Manuel

    2014-06-01

    The dispersive liquid-liquid microextraction of edible oils with a low volume of an acidic solution in the presence of isopropyl alcohol allows cadmium and lead to be completely separated into the aqueous phase. After centrifugation, the metals are determined by electrothermal atomization atomic absorption spectrometry using a palladium salt for chemical modification in the heating cycle. Using a 10 g oil sample, the enrichment factor is 140, which permits detection limits of 0.6 and 10 ng kg(-1) for cadmium and lead, respectively. The results agree with those obtained after sample mineralization. Data for the cadmium and lead levels for 15 samples of different characteristics are given.

  7. 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...

  8. Single-Photon Emission of a Hydrogenlike Atom

    Science.gov (United States)

    Skobelev, V. V.

    2016-11-01

    Implementing a previously obtained, original solution of the Dirac equation for an electron in the field of a nucleus ( Ze) expressed in terms of the wave function of the corresponding Schrödinger equation and its derivatives in spherical coordinates and the spin projection operator Σ3 associated with the eigenfunction, taking into account in each component of the spinor the leading term of the expansion in the small parameter ( Zα), α = e 2 / ħc ≈ 1 / 137, the partial probabilities W of emission of a photon ( Zα)* → ( Zα) + γ have been calculated. Here two orthogonal states of the linear polarization of the photon, and also the spin states of the electron, which previously had not been taken into consideration, have been taken into account in the transverse gauge. It turns out that the probabilities W of emission of a photon per unit time for any allowed transitions are proportional to (Zα)4, as was previously accepted, and the selection rules for the quantum number m have the usual form ∆ m = 0,±1. It was found that a spin flip does not take place during emission. In contrast to the customary situation with the selection rules for the quantum number l being of the form ∆ l = ±1, for ∆ m = ±1 there also exist integrals over dcosθ which are not equal to zero for undetermined odd values of ∆ l. In this, and also in a fundamentally different dependence of the amplitude on the quantum numbers consist the differences from the traditional approach to the problem. Necessary conditions are formulated, under the fulfillment of which the selection rules for l are not changed, having values ∆ l = ±1 for arbitrary ∆ m, but it was not possible, however, to give a complete proof of these rules.

  9. 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

  10. Kinetic model of atomic and molecular emissions in laser-induced breakdown spectroscopy of organic compounds.

    Science.gov (United States)

    Ma, Qianli; Dagdigian, Paul J

    2011-07-01

    A kinetic model previously developed to predict the relative intensities of atomic emission lines in laser-induced breakdown spectroscopy has been extended to include processes related to CN and C(2) molecular emissions. Simulations with this model were performed to predict the relative excited-state populations. The results from the simulations are compared with experimentally determined excited-state populations from 1,064 nm laser irradiation of organic residues on aluminum foil. The model reasonably predicts the relative intensity of the molecular emissions. Significantly, the model reproduces the vastly different temporal profiles of the atomic and molecular emissions. The latter are found to extend to much longer times after the laser pulse, and this appears to be due to the increasing concentration of the molecules versus time. From the simulations, the important processes affecting the CN and C(2) concentrations are identified.

  11. Three-body entanglement induced by spontaneous emission in a three two-level atoms system

    Institute of Scientific and Technical Information of China (English)

    Liao Xiang-Ping; Fang Mao-Fa; Zheng Xiao-Juan; Cai Jian-Wu

    2006-01-01

    We study three-body entanglement induced by spontaneous emission in a three two-level atoms system by using the entanglement tensor approach. The results show that the amount of entanglement is strongly dependent on the initial state of the system and the species of atoms. The three-body entanglement is the result of the coherent superposition of the two-body entanglements. The larger the two-body entanglement is, the stronger the three-body entanglement is. On the other hand, if there exists a great difference in three two-body entanglement measures, the three-body entanglement is very weak. We also find that the maximum of the two-body entanglement obtained with nonidentical atoms is greater than that obtained with identical atoms via adjusting the difference in atomic frequency.

  12. 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

    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......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...... of 1300 W. The limit of detection achieved under these conditions was 1 mu g L-1 (100 mu L injections). The HPLC-ICP-MS system was used for selenium speciation of selenite and selenate in aqueous solutions during a BCR certification exercise and for selenium speciation in the certified reference material...

  13. Spontaneous emission from a microwave-driven four-level atom in an anisotropic photonic crystal

    Science.gov (United States)

    Jiang, Li; Wan, Ren-Gang; Yao, Zhi-Hai

    2016-10-01

    The spontaneous emission from a microwave-driven four-level atom embedded in an anisotropic photonic crystal is studied. Due to the modified density of state (DOS) in the anisotropic photonic band gap (PBG) and the coherent control induced by the coupling fields, spontaneous emission can be significantly enhanced when the position of the spontaneous emission peak gets close to the band gap edge. As a result of the closed-loop interaction between the fields and the atom, the spontaneous emission depends on the dynamically induced Autler-Townes splitting and its position relative to the PBG. Interesting phenomena, such as spectral-line suppression, enhancement and narrowing, and fluorescence quenching, appear in the spontaneous emission spectra, which are modulated by amplitudes and phases of the coherently driven fields and the effect of PBG. This theoretical study can provide us with more efficient methods to manipulate the atomic spontaneous emission. Project supported by the National Natural Science Foundation of China (Grant Nos. 11447232, 11204367, 11447157, and 11305020).

  14. CHIANTI - An atomic database for Emission Lines. Version 8

    CERN Document Server

    Del Zanna, G; Young, P R; Landi, E; Mason, H E

    2015-01-01

    We present version 8 of the CHIANTI database. This version includes a large amount of new data and ions, which represent a significant improvement in the soft X-ray, EUV and UV spectral regions, which several space missions currently cover. New data for neutrals and low charge states are also added. The data are assessed, but to improve the modelling of low-temperature plasma the effective collision strengths for most of the new datasets are not spline-fitted as previously, but are retained as calculated. This required a change of the format of the CHIANTI electron excitation files. The format of the energy files has also been changed. Excitation rates between all the levels are retained for most of the new datasets, so the data can in principle be used to model high-density plasma. In addition, the method for computing the differential emission measure used in the CHIANTI software has been changed.

  15. 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.

  16. Structure determination of adipokinetic hormones using fast atom bombardment tandem mass spectrometry; An unknown adipokinetic hormone (AKH-III) from Locusta migratoria

    Energy Technology Data Exchange (ETDEWEB)

    Heerma, W.; Versluis, C.; Lankhof, H. (Utrecht University (Netherlands). Faculty of Chemistry, Department of Analytical Molecular Spectrometry); Oudejans, R.C.H.M.; Kooiman, F.P.; Beenakkers, A.M.T. (Utrecht University (Netherlands). Department of Experimental Zoology)

    1991-08-01

    Fast atom bombardment mass spectrometry combined with various tandem mass spectrometric techniques and accurate mass measurement were used to elucidate the structure of an unknown biologically active peptide isolated from Locusa migratoria. (author). 23 refs.; 6 figs.; 2 schemes.

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

    Energy Technology Data Exchange (ETDEWEB)

    Jesus, Alexandre de; Zmozinski, Ariane Vanessa [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Damin, Isabel Cristina Ferreira [Faculdade Dom Bosco de Porto Alegre, 90520-280, Porto Alegre, RS (Brazil); Silva, Marcia Messias, E-mail: mmsilva@iq.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, 40170-115 Salvador, BA (Brazil); Vale, Maria Goreti Rodrigues [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, 40170-115 Salvador, BA (Brazil)

    2012-05-15

    In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 {mu}g kg{sup -1} for arsenic and 0.2 {mu}g kg{sup -1} for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a 'cold finger' was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis. - Highlights: Black-Right-Pointing-Pointer A direct sampling GF AAS method to determine As and Cd in crude oil was proposed. Black-Right-Pointing-Pointer The conventional chemical modifier Pd/Mg has been used to stabilize As and Cd. Black

  18. Determination of some antihistaminic drugs by atomic absorption spectrometry and colorimetric methods.

    Science.gov (United States)

    El-Kousy, N; Bebawy, L I

    1999-08-01

    Atomic absorption spectrometry (AAS) and colourimetric methods have been developed for the determination of pizotifen (I), ketotifen (II) and loratadine (III). The first method depends on the reaction of the three drugs (I); (II) and (III) with cobalt thiocyanate reagent at pH 2 to give ternary complexes. These complexes are readily extracted with organic solvent and estimated by indirect atomic absorption method via the determination of the cobalt content in the formed complex after extraction in 0.1 M hydrochloric acid. It was found that the three drugs can be determined in the concentration ranges from 10 to 74, 12 to 95 and 10 to 93 microg ml(-1) with mean percentage recovery of 99.71+/-0.87, 99.70+/-0.79 and 99.62+/-0.75%, respectively. The second method is based on the formation of orange red ion pairs as a result of the reaction between (I); (II) and (III) and molybdenum thiocyanate with maximum absorption at 469.5 nm in dichloromethane. Appropriate conditions were established for the colour reaction. Under the proposed conditions linearity was obeyed in the concentration ranges 3.5-25, 5-37.5 and 2.5-22.5 microg ml(-1) with mean percentage recovery of 99.60+/-0.41, 100.11+/-0.43 and 99.31+/-0.47% for (I): (II) and (III), respectively. The third method depends on the formation of radical ion using 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ). The colour formed was measured at 588 nm for the three drugs (I); (II) and (III), respectively. The method is valid in concentration range 10-80 microg ml(-1) with mean percentage recovery 99.75+/-0.44, 99.94+/-0.72 and 99.17+/-0.36% for (I); (II) and (III), respectively. The proposed methods were applied to the analysis of pharmaceutical preparations. The results obtained were statistically analysed and compared with those obtained by applying the official and reference methods.

  19. 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

  20. 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

  1. Determination of Inorganic Arsenic Species by Electrochemical Hydride Generation Atomic Absorption Spectrometry with Selective Electrochemical Reduction

    Institute of Scientific and Technical Information of China (English)

    LI Xun; WANG Zheng-Hao

    2007-01-01

    A new direct procedure for the determination of inorganic arsenic species was developed by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS) with selective electrochemical reduction. The determination of inorganic arsenic species is based on the fact that As(Ⅲ) shows significantly higher absorbance at low electrolytic currents than As(Ⅴ) in 0.3 mol·L-1 H2SO4.The electrolytic current used for the determination of As(Ⅲ) without considerable interferences of As(V) was 0.4 A, whereas the current for the determination of As(Ⅲ)and As(V) was 1.2 A. For equal concentrations of As(Ⅲ) and As(V) in a sample, the interferences of As(V) during the As(Ⅲ) determination were smaller than 5%. The absorbance for As(V) could be calculated by subtracting that for As(Ⅲ) measured at 0.4 A from the total absorbance for As(Ⅲ) and As(V) measured at 1.2 A, and then the concentration of As(V) can be obtained by its calibration curve at 1.2 A. The methodology developed provided the detection limits of 0.3 and 0.6 ng·ml-1 for As(Ⅲ) and As(V) respectively.The relative standrad deviations were of 3.5% for 20 ng·ml-1 As(Ⅲ) and 302% for 20 ng·ml-1 As(V).The method was successfully applied to determination of soluble inorganic arsenic species in Chinese medicine.

  2. Investigation of aging processes of graphite tubes modified with iridium and rhodium used for atomic spectrometry

    Science.gov (United States)

    Bulska, Ewa; Piaścik, Marek; Katskov, Dmitri; Darangwa, Nicholas; Grotti, Marco

    2007-11-01

    UV spectrometry (187-380 nm) with charge coupled device (CCD) detection was used to study the evolution of absorption spectra during the vaporization of various species in the pyrocoated graphite furnace, with electrodeposited Ir and Rh as modifiers. In order to mimic a typical matrix composition, various salts of aluminum, manganese, copper, magnesium, sodium, and lead were used in microgram amounts. Changes in spectra and vapor release rate, along with aging of the tubes in the repetitive temperature cycles, were observed. Compared to the unmodified pyrocoated tubes, the presence of Ir or Rh causes a significant reduction in the vaporization efficiency, especially for microgram amounts of copper and aluminum introduced as nitrates, and manganese introduced as a sulfate. The vaporization efficiency, for magnesium and sodium as chlorides, and for lead as a sulfate, remained unchanged. Interestingly, the aging of the tubes was accompanied by partial restoration of the spectral characteristics for unmodified tubes. For example, with unmodified pyrocoated tubes, the vaporization spectrum, appearing as a consequence of the decomposition of aluminum nitrate, consisted of Al2O bands overlapped by Al atomic lines. In the freshly modified tubes, intensities of those lines and bands were substantially reduced, and in this case, the dominance of AlO molecules was observed. The efficiency of vaporization of aluminum species increased in the aged modified tubes. The scanning electron microscopy (SEM) images of the modified surfaces for the new and aged tubes indicated that aging of the tubes is accompanied by the destruction of the pyrocoating, formation of pyrographite shells around the areas where the modifier was electrodeposited, and finally, complete substitution of the metal on the graphite surface by pyrographite debris.

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

    Science.gov (United States)

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

    2016-01-01

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

  4. Flow injection-chemical vapor generation atomic fluorescence spectrometry hyphenated system for organic mercury determination: A step forward

    Energy Technology Data Exchange (ETDEWEB)

    Angeli, Valeria [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Biagi, Simona [National Research Council of Italy, C.N.R., Istituto per i Processi Chimico-Fisici - IPCF-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Ghimenti, Silvia [University of Pisa, Department of Chemistry and Industrial Chemistry, Via Risorgimento 35, 56126 Pisa (Italy); Onor, Massimo; D' Ulivo, Alessandro [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Bramanti, Emilia, E-mail: bramanti@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2011-11-15

    Monomethylmercury and ethylmercury were determined on line using flow injection-chemical vapor generation atomic fluorescence spectrometry without neither requiring a pre-treatment with chemical oxidants, nor UV/MW additional post column interface, nor organic solvents, nor complexing agents, such as cysteine. Inorganic mercury, monomethylmercury and ethylmercury were detected by atomic fluorescence spectrometry in an Ar/H{sub 2} miniaturized flame after sodium borohydride reduction to Hg{sup 0}, monomethylmercury hydride and ethylmercury hydride, respectively. The effect of mercury complexing agent such as cysteine, ethylendiaminotetracetic acid and HCl with respect to water and Ar/H{sub 2} microflame was investigated. The behavior of inorganic mercury, monomethylmercury and ethylmercury and their cysteine-complexes was also studied by continuous flow-chemical vapor generation atomic fluorescence spectrometry in order to characterize the reduction reaction with tetrahydroborate. When complexed with cysteine, inorganic mercury, monomethylmercury and ethylmercury cannot be separately quantified varying tetrahydroborate concentration due to a lack of selectivity, and their speciation requires a pre-separation stage (e.g. a chromatographic separation). If not complexed with cysteine, monomethylmercury and ethylmercury cannot be separated, as well, but their sum can be quantified separately with respect to inorganic mercury choosing a suitable concentration of tetrahydroborate (e.g. 10{sup -5} mol L{sup -1}), thus allowing the organic/inorganic mercury speciation. The detection limits of the flow injection-chemical vapor generation atomic fluorescence spectrometry method were about 45 nmol L{sup -1} (as mercury) for all the species considered, a relative standard deviation ranging between 1.8 and 2.9% and a linear dynamic range between 0.1 and 5 {mu}mol L{sup -1} were obtained. Recoveries of monomethylmercury and ethylmercury with respect to inorganic mercury were

  5. Flow injection-chemical vapor generation atomic fluorescence spectrometry hyphenated system for organic mercury determination: A step forward

    Science.gov (United States)

    Angeli, Valeria; Biagi, Simona; Ghimenti, Silvia; Onor, Massimo; D'Ulivo, Alessandro; Bramanti, Emilia

    2011-11-01

    Monomethylmercury and ethylmercury were determined on line using flow injection-chemical vapor generation atomic fluorescence spectrometry without neither requiring a pre-treatment with chemical oxidants, nor UV/MW additional post column interface, nor organic solvents, nor complexing agents, such as cysteine. Inorganic mercury, monomethylmercury and ethylmercury were detected by atomic fluorescence spectrometry in an Ar/H 2 miniaturized flame after sodium borohydride reduction to Hg 0, monomethylmercury hydride and ethylmercury hydride, respectively. The effect of mercury complexing agent such as cysteine, ethylendiaminotetracetic acid and HCl with respect to water and Ar/H 2 microflame was investigated. The behavior of inorganic mercury, monomethylmercury and ethylmercury and their cysteine-complexes was also studied by continuous flow-chemical vapor generation atomic fluorescence spectrometry in order to characterize the reduction reaction with tetrahydroborate. When complexed with cysteine, inorganic mercury, monomethylmercury and ethylmercury cannot be separately quantified varying tetrahydroborate concentration due to a lack of selectivity, and their speciation requires a pre-separation stage (e.g. a chromatographic separation). If not complexed with cysteine, monomethylmercury and ethylmercury cannot be separated, as well, but their sum can be quantified separately with respect to inorganic mercury choosing a suitable concentration of tetrahydroborate (e.g. 10 - 5 mol L - 1 ), thus allowing the organic/inorganic mercury speciation. The detection limits of the flow injection-chemical vapor generation atomic fluorescence spectrometry method were about 45 nmol L - 1 (as mercury) for all the species considered, a relative standard deviation ranging between 1.8 and 2.9% and a linear dynamic range between 0.1 and 5 μmol L - 1 were obtained. Recoveries of monomethylmercury and ethylmercury with respect to inorganic mercury were never less than 91%. Flow injection

  6. On-line analysis of penicillin blood levels in the live rat by combined microdialysis/fast-atom bombardment mass spectrometry.

    OpenAIRE

    Caprioli, R.M.; Lin, S. N.

    1990-01-01

    The combination of microdialysis and fast-atom bombardment mass spectrometry has been used to follow the pharmacokinetics of penicillin G directly in the blood-stream of a live rat. After the intramuscular injection of the antibiotic, the blood dialysate was allowed to flow into the mass spectrometer via the continuous-flow/fast-atom bombardment interface. Tandem mass spectrometry provided the means for isolating and recording the ion fragments produced from the drug as the dialysate was expo...

  7. Atomic nuclei decay modes by spontaneous emission of heavy ions

    Energy Technology Data Exchange (ETDEWEB)

    Poenaru, D.N.; Ivascu, M.; Sndulescu, A.; Greiner, W.

    1985-08-01

    The great majority of the known nuclides with Z>40, including the so-called stable nuclides, are metastable with respect to several modes of spontaneous superasymmetric splitting. A model extended from the fission theory of alpha decay allows one to estimate the lifetimes and the branching ratios relative to the alpha decay for these natural radioactivities. From a huge amount of systematic calculations it is concluded that the process should proceed with maximum intensity in the trans-lead nuclei, where the minimum lifetime is obtained from parent-emitted heavy ion combinations leading to a magic (/sup 208/Pb) or almost magic daughter nucleus. More than 140 nuclides with atomic number smaller than 25 are possible candidates to be emitted from heavy nuclei, with half-lives in the range of 10/sup 10/--10/sup 30/ s: /sup 5/He, /sup 8en-dash10/Be, /sup 11,12/B, /sup 12en-dash16/C, /sup 13en-dash17/N, /sup 15en-dash22/O, /sup 18en-dash23/F, /sup 20en-dash26/Ne, /sup 23en-dash28/Na, /sup 23en-dash30/Mg, /sup 27en-dash32/Al, /sup 28en-dash36/Si, /sup 31en-dash39/P, /sup 32en-dash42/S, /sup 35en-dash45/Cl, /sup 37en-dash47/Ar, /sup 40en-dash49/ K, . .Ca, /sup 44en-dash53/ Sc, /sup 46en-dash53/Ti, /sup 48en-dash54/V, and /sup 49en-dash55/ Cr. The shell structure and the pairing effects are clearly manifested in these new decay modes.

  8. 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.

  9. Atom-atom entanglement generated at early times by two-photon emission

    Energy Technology Data Exchange (ETDEWEB)

    Leon, Juan; Sabin, Carlos [Instituto de Fisica Fundamental, CSIC, Serrano 113-bis, 28006 Madrid (Spain)], E-mail: leon@imaff.cfmac.csic.es, E-mail: csl@imaff.cfmac.csic.es

    2009-07-15

    We analyze entanglement generation between a pair of neutral two-level atoms that are initially excited in a common electromagnetic vacuum. The nonlocal correlations that appear due to the interaction with the field can become entanglement when the field state is known. We distinguish two different situations: in the first, the field remains in the vacuum state and in the second, two photons are present in the final state. In both cases, we study the dependence of the entanglement on time and interatomic distance, at ranges related with locality issues.

  10. Electron emission in energetic ion-atom collisions in the presence of coherent electromagnetic radiation

    Energy Technology Data Exchange (ETDEWEB)

    Ciappina, M F [CONICET and Departamento de Fisica, Av. Alem 1253 (8000) BahIa Blanca (Argentina); Madsen, L B [Department of Physics and Astronomy, University of Aarhus, 8000 Aarhus C (Denmark)

    2006-12-28

    We consider the effect of a low-frequency electromagnetic field on the spectra of electron emission in energetic nonrelativistic ion-atom collisions. The field is assumed to have linear polarization and to be weak compared to the typical atomic field. The incorporation of the projectile interaction opens a new scenario to the combined study of electromagnetic and atomic interactions. Our work suggests that the electromagnetic field can have a profound effect on two of the most important structures that appear in the electron emission spectra: the electron capture into the continuum and binary encounter (BE) peaks. We show that in the BE peak region the result for the laser-assisted scattering depends on the theory applied for the collision part, the first Born approximation or the distorted wave Born approximation.

  11. 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.

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

    Science.gov (United States)

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

    2007-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-03-15

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

  14. Model for Atomic Oxygen Visible Line Emissions in Comet C/1995 O1 Hale-Bopp

    CERN Document Server

    Raghuram, Susarla

    2012-01-01

    We have recently developed a coupled chemistry-emission model for the green and red-doublet emissions of atomic oxygen on comet Hyakutake. In the present work we applied our model to comet Hale-Bopp, which had an order of magnitude higher H2O production rate than comet Hyakutake, to evaluate the photochemistry associated with the production and loss of O(1S) and O(1D) atoms and emission processes of green and red-doublet lines. We present the wavelength-dependent photo-attenuation rates for different photodissociation processes forming O(1S) and O(1D). The calculated radiative efficiency profiles of O(1S) and O(1D) atoms show that in comet Hale-Bopp the green and red-doublet emissions are emitted mostly above radial distances of 10^3 and 10^4 km, respectively. The model calculated [OI] 6300 A emission surface brightness and average intensity over the Fabry-P{\\'e}rot spectrometer field of view are consistent with the observation of Morgenthaler et al. (2001), while the intensity ratio of green to red-doublet e...

  15. Photon absorption and emission statistics of a two-level atom in a cavity

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Chang J. [Sun Moon University, Asan (Korea, Republic of)

    2012-03-15

    The absorption and the emission of photons by an atom involves quantum jumps between states. We investigate the quantum jump statistics for the system of a two-level atom and a single-mode cavity field. We use the Jaynes-Cummings model for this problem, perform Monte Carlo numerical simulations, and give a detailed exact analysis on these simulations. These studies reveal that the waiting-time distribution (WTD) for photon absorptions (emissions) has a unique novel statistic, and that the photon absorption (emission) rate is not uniform, but counter-intuitively depends on the position in the Rabi cycle. The effects of the nonclassical nature of the field on the WTD is discussed.

  16. Visible light emission in collisions between O5+ ions and He atoms

    Institute of Scientific and Technical Information of China (English)

    李大万; 潘广炎; 杨锋; 刘占稳; 周嗣信; 张文; 张雪珍; 郭晓虹; 王友德; 杨治虎; 马新文; 刘惠萍; 赵孟春

    1997-01-01

    Visible light emission spectra during collisions between O5 + ions and He atoms in the range of 200-800 nm at different projectile energies (4.06-5.31 keV·u 1) have been measured. Emission spectra show that there arc three channels of excitation in the O5+ -He collision system; (i) single-electron capture into excited states; (ii) double-electron capture into excited states; (iii) direct excitation of target atoms. There are transitions between states with comparably high quantum numbers nl The absolute emission cross-sections of every spectral line are calculated. The relations of these cross-sect ions with the energy of the projectiles are studied.

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

    Science.gov (United States)

    Musil, Stanislav; Matoušek, Tomáš; Currier, Jenna M; Stýblo, Miroslav; Dědina, Jiří

    2014-10-21

    This work describes the method of a selective hydride generation-cryotrapping (HG-CT) coupled to an extremely sensitive but simple in-house assembled and designed atomic fluorescence spectrometry (AFS) instrument for determination of toxicologically important As species. Here, an advanced flame-in-gas-shield atomizer (FIGS) was interfaced to HG-CT and its performance was compared to a standard miniature diffusion flame (MDF) atomizer. A significant improvement both in sensitivity and baseline noise was found that was reflected in improved (4 times) limits of detection (LODs). The yielded LODs with the FIGS atomizer were 0.44, 0.74, 0.15, 0.17 and 0.67 ng L(-1) for arsenite, total inorganic, mono-, dimethylated As and trimethylarsine oxide, respectively. Moreover, the sensitivities with FIGS and MDF were equal for all As species, allowing for the possibility of single species standardization with arsenate standard for accurate quantification of all other As species. The accuracy of HG-CT-AFS with FIGS was verified by speciation analysis in two samples of bottled drinking water and certified reference materials, NRC CASS-5 (nearshore seawater) and SLRS-5 (river water) that contain traces of methylated As species. As speciation was in agreement with results previously reported and sums of all quantified species corresponded with the certified total As. The feasibility of HG-CT-AFS with FIGS was also demonstrated by the speciation analysis in microsamples of exfoliated bladder epithelial cells isolated from human urine. The results for the sums of trivalent and pentavalent As species corresponded well with the reference results obtained by HG-CT-ICPMS (inductively coupled plasma mass spectrometry).

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

    Science.gov (United States)

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

    2015-03-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

  20. 微波消解-耐氢氟酸系统进样电感耦合等离子体发射光谱法测定锰矿中铝磷镁铁锌镍%Determination of aluminum, phosphorus, magnesium, iron, zinc and nickel in manganese ore by inductively coupled plasma atomic emission spectrometry with hydrofluoric add resistant sampling system after microwave digestion

    Institute of Scientific and Technical Information of China (English)

    邓全道; 许光; 林冠春; 刘建发; 刘灵芝

    2011-01-01

    采用混合酸作溶剂微波消解试样,样液定客后,直接用耐氢氟酸进样系统(Duo HF KIT)进样,电感耦合等离子体发射光谱法(ICP-AES)测定锰矿石试液中的铝、磷、镁、铁、锌、镍,避免因为引入硼酸掩蔽氟离子而带来的基体干扰,缩短了检测时间.测定时选择波长为369.152 nm{85}、186.942 nm{481}、280.270 nm{120}、240.488 nm{140}、213.856 nm{457}和341.476 nm{99}光谱线分别作为Al、P、Mg、Fe、Zn、Ni分析线,采用基体匹配方法来消除锰的基体效应.本法已测定国家锰矿标准物质中铝、磷、镁、铁、锌、镍,并与国标方法测定结果相比对,分析结果与认定值及国标方法的测定值相符,且重复性好.各元素的加标回收率为94%~107%,测定结果的相对标准偏差(RSD,n=12)小于1.1%.%The samples were dissolved by microwave digestion using mixed acid as solvent. After dilution, the aluminum, phosphorus, magnesium, iron, zinc and nickel in manganese ore were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) using hydrofluoric acid resistant sampling system (Duo HF KIT). The matrix effect of boric acid introduced for masking fluorine ion was prevented , and the detection time was shortened. The spectral lines for Al, P, Mg, Fe, Zn and Ni were 369. 152 nm{ 85 } , 186. 942 nm{ 481 } , 280. 270 nm{120} , 240. 488 nm {140} , 213. 856 nm {457} and 341. 476 nm {99}, respectively. The matrix effect of manganese was eliminated by matrix matching method. The proposed method had been applied to the determination of aluminum, phosphorus, magnesium, iron, zinc and nickel in certified reference materials of manganese ore. The determination results were compared with those obtained by national standard method. It was found that the analytical results were consistent with the certified values and those obtained by national standard method. Moreover, the repeatability was good. The recoveries of elements were 94%-107

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

    Energy Technology Data Exchange (ETDEWEB)

    Zeini Jahromi, Elham [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Bidari, Araz [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Assadi, Yaghoub [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of) and Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of)]. E-mail: y_assadi@iust.ac.ir; Milani Hosseini, Mohammad Reza [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Jamali, Mohammad Reza [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of)

    2007-03-07

    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 {mu}L methanol (disperser solvent) containing 34 {mu}L 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 {mu}L). Then a 20 {mu}L 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{sup -1} with detection limit of 0.6 ng L{sup -1}. The relative standard deviation (R.S.D.s) for ten replicate measurements of 20 ng L{sup -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{sup -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

  2. 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.

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

    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.

  4. 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.

  5. Spontaneous emission spectrum of a three-level atom embedded in photonic crystal

    Institute of Scientific and Technical Information of China (English)

    刘国强; 王健; 张汉壮

    2005-01-01

    The two models of three-level (one upper level and two lower levels, or two upper levels and one lower level) atom embedded in a double-band photonic crystal are adopted. The atomic transitions from the upper levels to the lower levels are assumed to be coupled by the same reservoir which are respectively the isotropic photonic band gap (PBG)modes, the anisotropic PBG modes and the free vacuum modes. The effects of the fine structure of the atomic ground state levels in the model with one upper level and two lower levels, and the quantum interferences in the model with two upper levels and one lower level on the spontaneous emission spectrum of an atom are investigated in detail. Most interestingly, it is shown that new spontaneous emission lines are produced from the fine splitting of atomic ground state levels in the isotropic PBG case. The quantum interferences induce additional narrow spontaneous lines near the transition from the empty upper level to the lower level.

  6. 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)

  7. Electron ionization of metastable nitrogen and oxygen atoms in relation to the auroral emissions

    Science.gov (United States)

    Pandya, Siddharth; Joshipura, K. N.

    Atomic and molecular excited metastable states (EMS) are exotic systems due to their special properties like long radiative life-time, large size (average radius) and large polarizability along with relatively smaller first ionization energy compared to their respective ground states (GS). The present work includes our theoretical calculations on electron impact ionization of metastable atomic states N( (2) P), N( (2) D) of nitrogen and O( (1) S), O( (1) D) of oxygen. The targets of our present interest, are found to be present in our Earth's ionosphere and they play an important role in auroral emissions observed in Earth’s auroral regions [1] as also in the emissions observed from cometary coma [2, 3] and airglow emissions. In particular, atomic oxygen in EMS can radiate, the visible O( (1) D -> (3) P) doublet 6300 - 6364 Å red doublet, the O( (1) S -> (1) D) 5577 Å green line, and the ultraviolet O( (1) S -> (3) P) 2972 Å line. For metastable atomic nitrogen one observes the similar emissions, in different wavelengths, from (2) D and (2) P states. At the Earth's auroral altitudes, from where these emissions take place in the ionosphere, energetic electrons are also present. In particular, if the metastable N as well as O atoms are ionized by the impact of electrons then these species are no longer available for emissions. This is a possible loss mechanism, and hence it is necessary to analyze the importance of electron ionization of the EMS of atomic O and N, by calculating the relevant cross sections. In the present paper we investigate electron ionization of the said metastable species by calculating relevant total cross sections. Our quantum mechanical calculations are based on projected approximate ionization contribution in the total inelastic cross sections [4]. Detailed results and discussion along with the significance of these calculations will be presented during the COSPAR-2014. References [1] A.Bhardwaj, and G. R. Gladstone, Rev. Geophys., 38

  8. 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)

  9. Approximate Toffoli Gate Originated from a Single Resonant Interaction of Cavity Dissipation and Atomic Spontaneous Emission

    Institute of Scientific and Technical Information of China (English)

    GU Xiao-Yan; CHEN Chang-Yong; SUN Jian-Qiang

    2008-01-01

    We propose a potentially practical scheme to implement an approximate three-qubit Toffoli gate by a single resonant interaction in dissipative cavity QED in which the cavity mode decay and atomic spontaneous emission are considered. The scheme does not require two-qubit controlled-NOT gates but uses a three-qubit phase gate and two Hadamard gates, where the approximate phase gate can be implemented by only a single dissipative resonant interaction of atoms with the cavity mode. Discussions are made for the advantages and the experimental feasibility of our scheme.

  10. Extracting Oscillation Frequencies in Spontaneous Emission Rate of an Atom Between Two Mirrors

    Institute of Scientific and Technical Information of China (English)

    ZHAO Hai-Jun; DU Meng-Li

    2007-01-01

    For an atom in a medium with refractive index n sandwiched between two parallel mirrors, we derive an analytical formula for the spontaneous emission rate based on Fermi's golden rule. The oscillations are not transparent in this formula. By performing Fourier transform on scaling variable measuring system size while holding system configuration fixed, we extracted the frequencies of many oscillations in this system. We show that these oscillations correspond to emitted photon closed-orbits going away from and returning to the emitting atom.

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

    OpenAIRE

    Andrada,Daniel; Pinto,Frederico G.; Magalhães, Cristina Gonçalves; Nunes,Berta R.; Franco,Milton B.; Silva,José Bento Borba da

    2006-01-01

    The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ET AAS). Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 µL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO3 1% v/v and 0.02% v/v of cetil trimethyl ammonium chloride (CTAC) were prepared directly in the autosampler cup...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-11-01

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

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

    Science.gov (United States)

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

    2002-11-01

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

  14. Trace elemental composition of curry by inductively coupled plasma optical emission spectrometry (ICP-OES).

    Science.gov (United States)

    Gonzálvez, A; Armenta, S; De La Guardia, M

    2008-01-01

    A methodology based on inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted acid digestion was developed to determine the content of traces elements in curry samples from the Spanish market. The methodology was validated in terms of accuracy by the analysis of citrus and tomato leaf reference materials achieving comparable results with the certified values. The trace metal content of curry samples was compared with data available from previously published reports concerning Indian samples, especially in terms of heavy metal composition, in order to guarantee the quality of the commercially available spices in the European countries. Values found for the analysis of arsenic, lead and cadmium were significantly lower than the maximum limit allowed by European Union statutory limits for heavy metals and lower than those obtained for Indian curry leaves reported by Indian research teams by using neutron activation and γ-ray analysis.

  15. 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

  16. Photochemistry of atomic oxygen green and red-doublet emissions in comets at larger heliocentric distances

    CERN Document Server

    Raghuram, Susarla

    2014-01-01

    In comets the atomic oxygen green to red-doublet emission intensity ratio (G/R ratio) of 0.1 has been used to confirm H$_2$O as the parent species producing oxygen emission lines. The larger ($>$0.1) value of G/R ratio observed in a few comets is ascribed to the presence of higher CO$_2$ and CO relative abundances in the cometary coma. We aim to study the effect of CO$_2$ and CO relative abundances on the observed G/R ratio in comets observed at large ($>$2 au) heliocentric distances by accounting for important production and loss processes of O($^1$S) and O($^1$D) in the cometary coma. Recently we have developed a coupled chemistry-emission model to study photochemistry of O($^1$S) and O($^1$D) atoms and the production of green and red-doublet emissions in comets Hyakutake and Hale-Bopp. In the present work we applied the model to six comets where green and red-doublet emissions are observed when they are beyond 2 au from the Sun. In a water-dominated cometary coma and with significant ($>$10%) CO$_2$ relati...

  17. Half lives for spontaneous emission of heavy ions from atomic nuclei

    Energy Technology Data Exchange (ETDEWEB)

    Poenaru, D.N.; Ivascu, M.; Greiner, W.

    1986-01-01

    The analytical superasymmetric fission model is used to estimate the half lives for spontaneous emission of heavy clusters from atomic nuclei. One gets a unified description of the new radioactivities, alpha decay and fission processes. Life-times shorter than 10/sup 30/s are found for the emission of more than 140 different clusters with 2-24 proton numbers and 3-31 neutron numbers. Even the 'stable' nuclides with Z > 40 are metastable with respect to several new decay modes. Solid state nuclear track detectors allow a good discrimination against other disintegration processes.

  18. 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).

  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. A espectrometria atômica e a determinação de elementos metálicos em material polimérico Atomic spectrometry and the determination of metals in polymeric materials

    Directory of Open Access Journals (Sweden)

    Solange Cadore

    2008-01-01

    Full Text Available Polymeric materials are widely used in the chemical industry and are part of our daily lives. Inorganic species may be added to them as additives, anti-oxidizing agents, stabilizers, plasticizers, colorants and catalysts and may be present in a wide range of concentrations. Their determination demands the development of analytical methods considering different kinds of polymeric materials, their composition and the final use of the material. Although many different analytical techniques may be used, this review emphasizes those based on atomic absorption and emission spectrometry. Solid sampling techniques and digestion methods are described and discussed and compared considering published results.

  1. Determination of cadmium by electrothermal atomic absorption spectrometry after microwave-assisted digestion of animal tissues and sewage sludges.

    Science.gov (United States)

    Chakraborty, R; Das, A K; Cervera, M L; De La Guardia, M

    1996-04-01

    The determination of cadmium in different sample types has been carried out by electrothermal atomization atomic absorption spectrometry with D(2)-background correction using a unpyrocoated graphite tube, after pressurized microwave-assisted digestion. Five chemical modifiers [(NH(4))(2)HPO(4), Pd(NO)(3))(2), Ni(NO(3))(2), thiourea and Triton X-100] have been assayed and nickel nitrate has been found to be most effective for an accurate determination of cadmium in mussel tissue, pig kidney and sewage sludge. The characteristic mass of the method is of the order of 1 pg and the limit of detection is lower than 0.1 ng/ml.

  2. 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.

  3. X-ray emission simulation from hollow atoms produced by high intensity laser irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Moribayashi, Kengo; Sasaki, Akira; Zhidkov, A. [Japan Atomic Energy Research Inst., Kansai Research Establishment, Neyagawa, Osaka (Japan); Suto, Keiko [Nara Women' s Univ., Graduate School of Human Culture, Nara (Japan); Kagawa, Takashi [Nara Women' s Univ., Department of Physics, Nara (Japan)

    2001-10-01

    We theoretically study the x-ray emission from hollow atoms produced by collisions of multiply charged ions accelerated by a short pulse laser with a solid or foil. By using the multistep-capture-and-loss (MSCL) model a high conversion efficiency to x-rays in an ultrafast atomic process is obtained. It is also proposed to apply this x-ray emission process to the x-ray source. For a few keV x-rays this x-ray source has a clear advantage. The number of x-ray photons increases as the laser energy becomes larger. For a laser energy of 10 J, the number of x-ray photons of 3x10{sup 11} is estimated. (author)

  4. Laser sampling system for an inductively-coupled atomic emission spectrometer. Final report

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1998-02-15

    A laser sampling system was attached to a Perkin Elmer Optima 3000 inductively-coupled plasma, atomic emission spectrometer that was already installed and operating in the Chemistry and Geochemistry Department at the Colorado School of Mines. The use of the spectrometer has been highly successful. Graduate students and faculty from at least four different departments across the CSM campus have used the instrument. The final report to NSF is appended to this final report. Appendices are included which summarize several projects utilizing this instrument: acquisition of an inductively-coupled plasma atomic emission spectrometer for the geochemistry program; hydrogen damage susceptibility assessment for high strength steel weldments through advanced hydrogen content analysis, 1996 and 1997 annual reports; and methods for determination of hydrogen distribution in high strength steel welds.

  5. ANALYSIS OF TRACE-LEVEL ORGANIC COMBUSTION PROCESS EMISSIONS USING NOVEL MULTIDIMENSIONAL GAS CHROMATOGRAPHY-MASS SPECTROMETRY PROCEDURES

    Science.gov (United States)

    The paper discusses the analysis of trace-level organic combustion process emissions using novel multidimensional gas chromatography-mass spectrometry (MDGC-MS) procedures. It outlines the application of the technique through the analyses of various incinerator effluent and produ...

  6. 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...

  7. [Determination of high content of tin in geochemical samples by solid emission spectrometry].

    Science.gov (United States)

    Yao, Jian-Zhen; Hao, Zhi-Hong; Tang, Rui-Ling; Li, Xiao-Jing; Li, Wen-Ge; Zhang, Qin

    2013-11-01

    A method for the determination of high content of tin in geochemical samples by solid emission spectrometry was presented. The dedicated high content tin spectrum standard series was developed. K2S2O7, NaF, Al2O3 and carbon powder were used as buffers and Ge was used as internal standard, and the ratio of sample/matrix/buffer is 1 : 1 : 2. A weak sensitive line (Sn 242. 170 0 nm) was used as the analytical line. The technologies of vertical electrodes, AC arc overlap spectrograph, interception of the exposure, quantitative computer translation spectrum and background correction were used. The determination range is 100-22 350 microg x g(-1), the detection limit is 16.64 microg x g(-1), and the precision is (RSD, n = 12) 4.11%-6.46%. The accuracy of the method has been verified by determination of high content of tin in national geochemical standard samples and the results are in agreement with certified value. The method can be used for measurement directly without dilution of high content of tin in geochemical samples, and it greatly improved the detection upper limit for the determination of tin with solid emission spectroscopy and has certain practical value.

  8. 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.

  9. Contents of cadmium, mercury and lead in fish from the Atlantic sea (Morocco) determined by atomic absorption spectrometry.

    Science.gov (United States)

    Chahid, Adil; Hilali, Mustapha; Benlhachimi, Abdeljalil; Bouzid, Taoufiq

    2014-03-15

    As a part of a specific monitoring program, lead (Pb) cadmium (Cd) and mercury (Hg) concentrations in important species of fish from various fishing ports of the southern Kingdom of Morocco (Sardina pilchardus, Scomber scombrus, Plectorhinchus mediterraneus, Trachurus trachurus, Octopus vulgaris, Boops boops, Sarda sarda, Trisopterus capelanus, and Conger conger) were investigated by the Moroccan Reference Laboratory (NRL) for trace elements in foodstuffs of animal origin. The samples were analysed for lead and cadmium by a graphite furnace atomic absorption spectrometry (GFAAS); and for mercury by cold vapour atomic absorption spectrometry (CVAAS). The results were expressed as μg/g of wet weight (w/w). The levels of Cd, Pb and Hg in muscles of fish were 0.009-0.036, 0.013-0.114 and 0.049-0.194 μg/g, respectively. The present study showed that different metals were present in the sample at different levels but within the maximum residual levels prescribed by the EU for the fish and shellfish from these areas, in general, should cause no health problems for consumers.

  10. Determination of lead in wine by hydride generation atomic fluorescence spectrometry in the presence of hexacyanoferrate(III).

    Science.gov (United States)

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

    2007-06-01

    A rapid, accurate, and precise method is described for the determination of Pb in wine using continuous-flow hydride generation atomic fluorescence spectrometry (CF-HGAFS). Sample pretreatment consists of ten-fold dilution of wine followed by direct plumbane generation in the presence of 0.1 mol L(-1) HCl and 1% m/v K(3)[Fe(CN)(6)] with 1% m/v NaBH(4) as reducing agent. An aqueous standard calibration curve is recommended for Pb quantification in wine sample. The method provides a limit of detection and a limit of quantification of 0.3 microg L(-1) and 1 microg L(-1), respectively. The relative standard deviation varies between 2-6% (within-run) and 4-11% (between-run) at 3-30 microg L(-1) Pb levels in wine. Good agreement has been demonstrated between results obtained by CF-HGAFS and direct electrothermal atomic absorption spectrometry in analyses of red and white wines within the concentration range of 9.2-25.8 microg L(-1) Pb.

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

    Science.gov (United States)

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

    1967-01-01

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

  12. Energy-dispersive x-ray fluorescence spectroscopy and inductively coupled plasma emission spectrometry evaluated for multielement analysis in complex biological matrices.

    Science.gov (United States)

    Irons, R D; Schenk, E A; Giauque, R D

    1976-12-01

    Energy-dispersive x-ray spectroscopy and inductively coupled plasma emission spectrometry were evaluated as methods for routine multielement analysis of biological material. Standard samples included Standard Reference Materials (National Bureau of Standards), compounded mixtures, and supplements that provided a wide range of elemental concentrations for analysis. Elements included in this study were Zn, Pb, Ni, Mn, Fe, Mg, Cu, Ca, As, Se, Br, Rb, and Sr. Standards were analyzed as unknowns by participating laboratories. The two methods were evaluated for sensitivity, precision, and accuracy, and the results compared to those obtained for atomic absorption spectrometric analysis of identical standard unknowns. Both methods compared favorably and both were determined to be highly reliable for such an application. Advantages and disadvantages of each method are compared and discussed.

  13. Microwaves spark emission spectroscopy for the analysis of cations: A simple form of atomic emission spectroscopy

    Institute of Scientific and Technical Information of China (English)

    Zahid Hussain; Khalid Mohammed Khan; Khadim Hussain; Sadam Hussain; Shahnaz Perveen

    2011-01-01

    A novel method for the cation analysis was investigated. The analysis is based on the sparking of the salts of metals in a microwave oven after placing in a graphite cell. The graphite cell absorbs microwaves and produces high temperature which converts the salt into light emitting species. The colour of light was found to dependent on the nature of cation, however, the intensity of the emitted light was found to be depending upon the form and shape of the graphite assembly in addition to the concentration of the salt. This communication presents explanation for all these observations and for the systematic and quantitative analysis using microwave spark emission technique.

  14. Controlling spontaneous emission of a two-level atom by hyperbolic metamaterials

    CERN Document Server

    Liu, Zheng; Jiang, Xunya

    2012-01-01

    Within the frame of quantum optics we analyze the properties of spontaneous emission of two-level atom in media with indefinite permittivity tensor where the geometry of the dispersion relation is characterized by an ellipsoid or a hyperboloid(hyperbolic medium). The decay rate is explicitly given with the orientation of the dipole transition matrix element taken into account. It indicates that for the ellipsoid case the intensity of the photons coupled into different modes can be tuned by changing the direction of the matrix element and for the hyperboloid case it is found that spontaneous emission in hyperbolic medium can be dramatically enhanced compared to the dielectric background. Moreover, spontaneous emission exhibit the strong directivity and get the maximum in the asymptote direction.

  15. Atoms

    Institute of Scientific and Technical Information of China (English)

    刘洪毓

    2007-01-01

    Atoms(原子)are all around us.They are something like the bricks (砖块)of which everything is made. The size of an atom is very,very small.In just one grain of salt are held millions of atoms. Atoms are very important.The way one object acts depends on what

  16. Study of atomic oxygen greenline dayglow emission in thermosphere during geomagnetic storm conditions

    Science.gov (United States)

    Bag, T.; Singh, Vir; Sunil Krishna, M. V.

    2017-01-01

    The influence of geomagnetic storms on the atomic oxygen greenline (557.7 nm) dayglow emission in thermosphere is studied during solar active and solar quiet conditions. This study is primarily based on the photochemical model with inputs obtained from experimental observations and empirical models. The updated rate coefficients, quantum yields and related cross-sections have been used from experimental results and theoretical studies. This study is presented for a low latitude station Tirunelveli (8.7°N, 77.8°E), India. The volume emission rate (VER) has been calculated using densities and temperatures from the empirical models. The modeled VER shows a positive correlation with the Dst index. The VER also shows a negative correlation with the number densities of O, O2, and N2. The VER, calculated at peak emission altitude, exhibits depletion during the main phase of the storm. The altitude of peak emission rate is unaffected by the geomagnetic storm activity. The study also reveals that the peak emission altitude depends on the F10.7 solar index. The peak emission altitude moves upward as the value of F10.7 solar index increases.

  17. Optical Emission Spectroscopic Measurement of Hydroxyl Radicals in Air Discharge with Atomized Water%Optical Emission Spectroscopic Measurement of Hydroxyl Radicals in Air Discharge with Atomized Water

    Institute of Scientific and Technical Information of China (English)

    孙明; 陈维刚; 张颖

    2011-01-01

    Effects of discharge mode, voltage applied, size of the nozzle discharge electrode and flow rate of water on the generation of hydroxyl radical were investigated in air discharge with atomized water, by using optical emission spectroscopy (OES). Water was injected into the discharge region through the discharge nozzle electrode, and a large amount of fine water drops, formed and distributed in the discharge region, corona discharge was more effective to generate were observed. It was found that negative DC the hydroxyl radicals in comparison to positive DC corona discharge or negative pulsed discharge. A larger outer diameter of the nozzle electrode or a stronger electric field is beneficial for hydroxyl-radical generation. Moreover, there is a critical value in the flow rate of atomized water against the discharge voltage. Below this critical value, hydroxyl-radical generation increases with the increase in flow rate of the water, while above this value, it decreases. In addition, it is observed that OES from the discharge is mainly in the ultraviolet domain. The results are helpful in the study of the mechanism and application of plasma in pollution-control in either air or water.

  18. 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

  19. Determination of Ultratrace Amounts of Copper(Ⅱ) in Water Samples by Electrothermal Atomic Absorption Spectrometry After Cloud Point Extraction

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction (CPE). 1-( 2-Pyridylazo)-2-naphthol was used as the chelating reagent and Triton X-114 as the micellar-forming surfactant. CPE was conducted in a pH 8.0 medium at 40 ℃ for 10 min. After the separation of the phases by centrifugation, the surfactant-rich phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20 μL of the diluted surfactant-rich phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconcentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0ng/mL, and the relative standard deviation was found to be less than 3.1% for a sample containing 1.0 ng/mL Cu(Ⅱ). This developed method was successfully applied to the determination of ultratrace amounts of Cu in drinking water, tap water, and seawater samples.

  20. Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Liu Qingyang, E-mail: liuqingyang0807@yahoo.com.c [Beijing Center for Physical and Chemical Analysis, Beijing 100089 (China)

    2010-07-15

    This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg{sup 0}, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL{sup -1} for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury (n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).

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

    Science.gov (United States)

    Cvetković, J; Stafilov, T; Mihajlović, D

    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 degrees C and 800 degrees C were chosen for aqueous and organic solutions, respectively; 2700 degrees C and 2100 degrees 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 degrees C and 1600 degrees 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 microg L(-1).

  2. Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

    Science.gov (United States)

    Liu, Qingyang

    2010-07-01

    This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg 0, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL -1 for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury ( n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).

  3. Single and double hydrogen atom migrations in substituted alkyl benzoates: a study on the substituent effect using MIKE spectrometry

    Science.gov (United States)

    Tobita, Seiji; Tajima, Susumu; Ishihara, Yasuko; Kojima, Masahiro; Shigihara, Atsushi

    1994-03-01

    The substituent effect on the single and double hydrogen atom migrations is ionized ortho-, meta-, and para-substituted isobutyl (XC6H4COOC4H9) and isopropyl (XC6H4COOC3H7) benzoates is investigated by mass-analyzed ion kinetic energy spectrometry. The observed product ion ratios [XC6H4COOH]+/[XC6H4COOH2]+ show a general tendency: the compounds with an electron-donating substituent favour the formation of [XC6H4COOH]+ by single hydrogen atom migration (McLafferty rearrangement), while those with an electron-withdrawing substituent produce preferentially [XC6H4COOH2]+ through double hydrogen atom migration (McLaffery + 1 rearrangement). The thermochemical considerations combined with MO calculations show that the substituent effects observed are rationalized by the effects of substituent on the ionization energy (IE) and proton affinity (PA) of XC6H4COOH, i.e. the product ratios are determined by the difference of the product thermochemical stabilities which can be evaluated as IE(XC6H4COOH) + PA(XC6H4COOH).

  4. Graphite furnace atomic absorption spectrometry as a routine method for the quantification of beryllium in blood and serum

    Directory of Open Access Journals (Sweden)

    Brousseau Pauline

    2008-07-01

    Full Text Available Abstract Background A routine method for the quantification of beryllium in biological fluids is essential for the development of a chelation therapy for Chronic Beryllium Disease (CBD. We describe a procedure for the direct determination of beryllium in undigested micro quantities of human blood and serum using graphite furnace atomic absorption spectrometry. Blood and serum samples are prepared respectively by a simple 8-fold and 5-fold dilution with a Nash Reagent. Three experimental setups are compared: using no modifier, using magnesium nitrate and using palladium/citric acid as chemical modifiers. Results In serum, both modifiers did not improve the method sensitivity, the optimal pyrolysis and atomization temperatures are 1000°C and 2900°C, respectively. In blood, 6 μg of magnesium nitrate was found to improve the method sensitivity. The optimal pyrolysis and atomization temperatures were 800°C and 2800°C respectively. Conclusion In serum, the method detection limit was 2 ng l-1, the characteristic mass was 0.22 (± 0.07 pg and the accuracy ranged from 95 to 100%. In blood, the detection limit was 7 ng l-1, the characteristic mass was 0.20 (± 0.02 pg and the accuracy ranged from 99 to 101%.

  5. 原子荧光光谱法测定土壤中的砷含量%Determination of Arsenic in Soil by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘燕芬

    2015-01-01

    通过结合具体的试验对运用原子荧光光谱法测定土壤中的砷含量进行了探讨,以期能为有关方面的需要提供有益的参考和借鉴。%In order to provide a useful reference for the relevant aspects of the arsenic content in soil by atomic fluorescence spectrometry, the method of atomic fluorescence spectrometry was used to determine the arsenic content in soil.

  6. 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.

  7. proEQUIB: IDL/GDL library for atomic level populations and line emissivities in statistical equilibrium

    Science.gov (United States)

    Danehkar, Ashkbiz

    2016-11-01

    The proEQUIB library calculates atomic level populations and line emissivities in statistical equilibrium in multi-level atoms for different physical conditions of stratified layers in a nebula where chemical elements are ionized. It includes an Interactive Data Language (IDL)/GNU Data Language (GDL) implementation of the Fortran code EQUIB (ascl:1603.005).

  8. 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

  9. Absolute isotopic composition and atomic weight of neodymium using thermal ionization mass spectrometry.

    Science.gov (United States)

    Zhao, Motian; Zhou, Tao; Wang, Jun; Lu, Hai; Fang, Xiang; Guo, Chunhua; Li, Qiuli; Li, Chaofeng

    2005-01-01

    Synthetic mixtures prepared gravimetrically from highly enriched isotopes of neodymium in the form of oxides of well-defined purity were used to calibrate a thermal ionization mass spectrometer. A new error analysis was applied to calculate the final uncertainty of the atomic weight value. Measurements on natural neodymium samples yielded an absolute isotopic composition of 27.153(19) atomic percent (at.%) 142Nd, 12.173(18) at.% 143Nd, 23.798(12) at.% 144Nd, 8.293(7) at.% 145Nd, 17.189(17) at.% 146Nd, 5.756(8) at.% 148Nd, and 5.638(9) at.% 150Nd, and the atomic weight of neodymium as 144.2415(13), with uncertainties given on the basis of 95% confidence limits. No isotopic fractionation was found in terrestrial neodymium materials.

  10. Feasibility guidelines for kaonic atom experiments with ultra-high-resolution X-ray spectrometry

    Science.gov (United States)

    Friedman, E.; Okada, S.

    2013-10-01

    Recent studies of strong-interaction effects in kaonic atoms suggest that analysing so-called 'lower' and 'upper' levels in the same atom could separate one-nucleon absorption from multinucleon processes. The present work examines the feasibility of direct measurements of upper level widths in addition to lower level widths in future experiments, using superconducting microcalorimeter detectors. About ten elements are identified as possible candidates for such experiments, all of medium-weight and heavy nuclei. New experiments focused on achieving good accuracy for widths of such pairs of levels could contribute significantly to our knowledge of the K--nucleon interaction in the nuclear medium.

  11. Oxygen bomb combustion of biological samples for inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    Souza, Gilberto B.; Carrilho, Elma Neide V. M.; Oliveira, Camila V.; Nogueira, Ana Rita A.; Nóbrega, Joaquim A.

    2002-12-01

    A rapid sample preparation method is proposed for decomposition of milk powder, corn bran, bovine and fish tissues, containing certified contents of the analytes. The procedure involves sample combustion in a commercial stainless steel oxygen bomb operating at 25 bar. Most of the samples were decomposed within 5 min. Diluted nitric acid or water-soluble tertiary amines 10% v/v were used as absorption solutions. Calcium, Cu, K, Mg, Na, P, S and Zn were recovered with the bomb washings and determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Ethanol mixed with paraffin was used as a combustion aid to allow complete combustion. A cooling step prior releasing of the bomb valve was employed to increase the efficiency of sample combustion. Iodine was also determined in milk samples spiked with potassium iodide to evaluate the volatilization and collection of iodine in amine CFA-C medium and the feasibility of its determination by ICP-OES with axial view configuration. Most of the element recoveries in the samples were between 91 and 105% and the certified and found contents exhibited a fair agreement at a 95% confidence level.

  12. Improving the analytical performance of hydride generation non-dispersive atomic fluorescence spectrometry. Combined effect of additives and optical filters

    Science.gov (United States)

    D'Ulivo, Alessandro; Bramanti, Emilia; Lampugnani, Leonardo; Zamboni, Roberto

    2001-10-01

    The effects of tetrahydroborate and acid concentration and the presence of L-cysteine and thiourea were investigated in the determination of As, Bi and Sn using continuous flow hydride generation atomic fluorescence spectrometry (HG AFS). The aim was to find conditions allowing the control of those effects exerting negative influence on the analytical performance of the HG AFS apparatus. The effects taken into account were: (i) the radiation scattering generated by carryover of solution from the gas-liquid separator to the atomizer; (ii) the introduction of molecular species generated by tetrahydroborate decomposition into the atomizer; and (iii) interference effects arising from other elements in the sample matrix and from different acids. The effects (i) and (ii) could be controlled using mild reaction conditions in the HG stage. The effect of HG conditions on carryover was studied by radiation scattering experiments without hydride atomization. Compromised HG conditions were found by studying the effects of tetrahydroborate (0.1-20 g l -1) and acid (0.01-7 mol l -1) concentration, and the addition of L-cysteine (10 g l -1) and thiourea (0.1 mol l -1) on the HG AFS signals. The effect of optical filters was investigated with the aim of improving the signal-to-noise ratio. Optical filters with peak wavelengths of 190 and 220 nm provided an improvement of detection limits by factors of approximately 4 and 2 for As and Te, respectively. Under optimized conditions the detection limits were 6, 5, 3, 2, 2 and 9 ng l -1 for As, Sb, Bi, Sn, Se and Te, respectively. Good tolerance to various acid compositions and sample matrices was obtained by using L-cysteine or thiourea as masking agents. Determination of arsenic in sediment and copper certified reference materials, and of bismuth in steel, sediment, soil and ore certified reference material is reported.

  13. 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.

  14. 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.

  15. Measurement of visible and UV emission from Energetic Neutral Atom Precipitation (ENAP), on Spacelab

    Science.gov (United States)

    Tinsley, B. A.

    1980-01-01

    The charge exchange of plasmaspheric ions and exospheric H and O and of solar wind ions with exospheric and interplanetary H are sources of precipitating neutrals whose faint emission may be observed by the imaging spectrometric observatory during dark periods of the SL-1 orbit. Measurements of the interactions of these precipitating atoms with the thermosphere are needed to evaluate the heating and ionization effects on the atmosphere as well as the selective loss of i energetic ions from the sources (predominantly the ring current).

  16. Chemical Analysis of Impurity Boron Atoms in Diamond Using Soft X-ray Emission Spectroscopy

    OpenAIRE

    Muramatsu, Yasuji

    2009-01-01

    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 mo...

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

    Science.gov (United States)

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

    2006-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Wu Peng [Analytical and Testing Center, Sichuan University, Chengdu, Sichuan 610064 (China); Zhang Yunchang [College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China); Lv Yi [College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China); Hou Xiandeng [Analytical and Testing Center, Sichuan University, Chengdu, Sichuan 610064 (China) and College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China)]. E-mail: houxd@scu.edu.cn

    2006-12-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Kiran, K. [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India); Kumar, K. Suresh; Prasad, B.; Suvardhan, K. [Department of Chemistry, S. V. University, Tirupati, 517502 A.P. (India); Lekkala, Ramesh Babu [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India); Janardhanam, K. [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India)], E-mail: Kandukurijanardhanam@gmail.com

    2008-02-11

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

  20. 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.

  1. Design and evaluation of a continuous flow, integrated nebulizer-hydride generator for flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Miguel Murillo

    2008-01-01

    Full Text Available An evaluation of the performance of a continuous flow hydride generator-nebulizer for flame atomic absorption spectrometry was carried out. Optimization of nebulizer gas flow rate, sample acid concentration, sample and tetrahydroborate uptake rates and reductant concentration, on the As and Se absorbance signals was carried out. A hydrogen-argon flame was used. An improvement of the analytical sensitivity relative to the conventional bead nebulizer used in flame AA was obtained (2 (As and 4.8 (Se µg L-1. Detection limits (3σb of 1 (As and 1.3 (Se µg L-1 were obtained. Accuracy of the method was checked by analyzing an oyster tissue reference material.

  2. The application of solid sorbents for the purification of aluminum contaminated chemicals used as modifiers in electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Bulska, E; Pyrzyńska, K

    1996-06-01

    Various microcolumns with solid sorbents (ion exchange resins, functionalised cellulose sorbents, chelating resins) have been tested with respect to their ability for the purification of aluminum contaminated chemicals used as modifiers in electrothermal atomic absorption spectrometry. The purification of NaNO(3), Mg(NO(3))(2), K(2)SO(4) and (NH(4))(2)HPO(4) has been the most effective with an almost 100% efficiency, when Spheron-Oxine was used as chelating resin. The sorption of aluminum from KOH solution has been found to be very high (around 90%) for all investigated sorbents. However, the best results have been obtained with anion-exchange resins. It has been difficult to purify concentrated mineral acids (HCl, H(2)SO(4)). A retention of aluminum above 80% has been achieved only when Cellex P, Chelex 100 or Amberlite XAD-2 have been used.

  3. 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.

  4. Correspondence Between Oscillations and Emitted Photon Closed-Orbits in Spontaneous Emission Rate of an Atom Near a Dielectric Slab

    Institute of Scientific and Technical Information of China (English)

    YUN Su-Jun; WANG Fu-He; ZHOU Yun-Song; DU Meng-Li

    2007-01-01

    We study the oscillations in the spontaneous emission rate of an atom near a dielectric slab. The emission rate is calculated as a function of system size using quantum electrodynamics. It exhibits multi-periodic oscillations.Four frequencies of the oscillations are extracted by Fourier transforms. They agree with actions of photon closed-orbits going away and returning to the atom. These oscillations are explained as manifestations of quantum interference effects between the emitted photon wave near the atom and the returning photon waves travelling along various closed-orbits.

  5. Energetic Neutral Atom Emissions From Venus: VEX Observations and Theoretical Modeling

    Science.gov (United States)

    Fok, M.-C.; Galli, A.; Tanaka, T.; Moore, T. E.; Wurz, P.; Holmstrom, M.

    2007-01-01

    Venus has almost no intrinsic magnetic field to shield itself from its surrounding environment. The solar wind thus directly interacts with the planetary ionosphere and atmosphere. One of the by-products of this close encounter is the production of energetic neutral atom (ENA) emissions. Theoretical studies have shown that significant amount of ENAs are emanated from the planet. The launch of the Venus Express (VEX) in 2005 provided the first light ever of the Venus ENA emissions. The observed ENA flux level and structure are in pretty good agreement with the theoretical studies. In this paper, we present VEX ENA data and the comparison with numerical simulations. We seek to understand the solar wind interaction with the planet and the impacts on its atmospheres.

  6. Daily and hourly sourcing of metallic and mineral dust in urban air contaminated by traffic and coal-burning emissions

    NARCIS (Netherlands)

    Moreno, T.; Karanasiou, A.; Amato, F.; Lucarelli, F.; Nava, S.; Calzolai, G.; Chiari, M.; Coz, E.; Artíñano, B.; Lumbreras, J.; Borge, R.; Boldo, E.; Linares, C.; Alastuey, A.; Querol, X.; Gibbons, W.

    2013-01-01

    A multi-analytical approach to chemical analysis of inhalable urban atmospheric particulate matter (PM), integrating particle induced X-ray emission, inductively coupled plasma mass spectrometry/atomic emission spectroscopy, chromatography and thermal-optical transmission methods, allows comparison

  7. Inductively coupled plasma spectrometry: Noise characteristics of aerosols, application of generalized standard additions method, and Mach disk as an emission source

    Energy Technology Data Exchange (ETDEWEB)

    Luan, Shen [Iowa State Univ., Ames, IA (United States)

    1995-10-06

    This dissertation is focused on three problem areas in the performance of inductively coupled plasma (ICP) source. The noise characteristics of aerosols produced by ICP nebulizers are investigated. A laser beam is scattered by aerosol and detected by a photomultiplier tube and the noise amplitude spectrum of the scattered radiation is measured by a spectrum analyzer. Discrete frequency noise in the aerosol generated by a Meinhard nebulizer or a direct injection nebulizer is primarily caused by pulsation in the liquid flow from the pump. A Scott-type spray chamber suppresses white noise, while a conical, straight-pass spray chamber enhances white noise, relative to the noise seen from the primary aerosol. Simultaneous correction for both spectral interferences and matrix effects in ICP atomic emission spectrometry (AES) can be accomplished by using the generalized standard additions method (GSAM). Results obtained with the application of the GSAM to the Perkin-Elmer Optima 3000 ICP atomic emission spectrometer are presented. The echelle-based polychromator with segmented-array charge-coupled device detectors enables the direct, visual examination of the overlapping lines Cd (1) 228.802 nm and As (1) 228.812 nm. The slit translation capability allows a large number of data points to be sampled, therefore, the advantage of noise averaging is gained. An ICP is extracted into a small quartz vacuum chamber through a sampling orifice in a water-cooled copper plate. Optical emission from the Mach disk region is measured with a new type of echelle spectrometer equipped with two segmented-array charge-coupled-device detectors, with an effort to improve the detection limits for simultaneous multielement analysis by ICP-AES.

  8. Straightforward way to enhance robustness in ultrasonic nebulization-axial view inductively coupled plasma optical emission spectrometry via an additional N2 gas stream

    Science.gov (United States)

    Scheffler, Guilherme Luiz; Pozebon, Dirce

    2015-11-01

    In the present study a low flow of N2 is mixed with the aerosol produced by ultrasonic nebulization (USN) prior analysis using inductively coupled plasma optical emission spectrometry (ICP OES). The foreign gas is added for improving plasma characteristics in axially-viewed ICP. By computing the Mg ionic to atomic ratio (plasma robustness) it was concluded that N2 dissociates closer to the load coil when USN is used as sample introduction system. The maximum emission intensity of Mg(II) for pneumatic nebulization (PN) was observed at 11 mm from the load coil while it was 8 mm for USN, indicating earlier aerosol desolvation, atomization and excitation processes in the ICP. Emission profiles of Ar(I) 415.861 nm, Ba(II) 486.601 nm and Ba(II) 233.527 nm indicated that metastable Ar species are overpopulated in the ICP under the N2 flow. Copper and manganese ionic lines with energy close to 16 eV (Ar ionization) were monitored to evaluate spatially dependent charge-transfer reaction along the ICP axis in the presence and absence of the N2 flow. The Cu(II) signal profiles indicated abundance of Ar+ species at low distances from the load coil when N2 was added. On the other hand, differences were not observed at longer distances from the load coil for both plasmas (mixed-gas and pure Ar-ICP). The calculated limits of detection (LODs) for both plasmas had the same order of magnitude. Analysis of certified reference samples demonstrated that the accuracy was preserved by adding the low flow of N2. It was concluded that adding a low flow of N2 to the aerosol produced by USN is a simple way to increase plasma robustness, which is usually lower than that achieved using conventional PN.

  9. Experimental study of conversion from atomic high-order harmonics to x-ray emissions

    Institute of Scientific and Technical Information of China (English)

    王骐; 陈建新; 夏元钦; 陈德应

    2003-01-01

    There are two physical phenomena in a strong laser intensity. One is the high-order harmonic emission; the other is x-ray emission from optical-field ionized plasmas. The experiment of conversion from high-order harmonics to x-ray emissions was given with a 105fs Ti:sapphire laser by adjusting laser intensities. The ingredient in plasma was investigated by the numerical simulations. Our experimental results suggested that the free electrons have detrimental effects on harmonic generation but are favourable for x-ray emission from optical-field ionized plasmas. If we want to obtain more intense harmonic signals as a coherent light source in the soft x-ray region, we must avoid the production of free electrons in plasmas. At the same time, if we want to observe x-rays for the development of high-repetition-rate table-top soft x-ray lasers, we should strip all atoms in the plasmas to a necessary ionized stage by the optical-fieldionization in the field of a high-intensity laser pulse.

  10. Experimental study of conversion from atomic high—order harmonics to x—ray emissions

    Institute of Scientific and Technical Information of China (English)

    WangQi; ChenJian-Xin; XiaYuan-Qin; ChenDe-Ying

    2003-01-01

    There are two physical phenomena in a strong laser intensity. One is the high-order harmonic emission; the other is x-ray emission from optical-field ionized plasmas. The experiment of conversion from high-order harmonics to x-ray emissions was given with a 105fs Ti:sapphire laser by adjusting laser intensities. The ingredient in plasma was investigated by the numerical simulations.Our experimental results suggested that the free electrons have detrimental effects on harmonic generation but are favourable for x-ray emission from optical-field ionized plasmas. If we want to obtain more intense harmonic signals as a coherent light source in the soft x-ray region, we must avoid the production of free electrons in plasmas. At the same time, if we want to observe x-rays for the development of high-repetition-rate table-top soft x-ray lasers, we should strip all atoms in the plasmas to a necessary ionized stage by the optical-field-ionization in the field of a high-intensity laser pulse.

  11. Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carro, A.M.; Neira, I.; Rodil, R.; Lorenzo, R. A. [Univ. Santiago de Compostela (Spain). Dpto. Quimica Analitica, Nutricion y Bromatologia

    2003-06-01

    A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode. Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables: sample volume, NaBPh{sub 4} volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species. (orig.)

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

    Energy Technology Data Exchange (ETDEWEB)

    Queirolo, F. (Universidad Catolica del Norte, Antofagasta (Chile). Dept. of Chemistry Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry); Ostapczuk, P. (Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie); Valenta, P.; Stegen, S. (Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry); Marin, C.; Vinagre, F.; Sanchez, A. (Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry)

    1991-05-01

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

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

    Science.gov (United States)

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

  14. Spontaneous Emission of an Inertial Multi-Level Atom in a Spacetime with a Reflecting Plane Boundary

    Institute of Scientific and Technical Information of China (English)

    ZHU Zhi-Ying; YU Hong-Wei

    2006-01-01

    @@ We calculate the contributions of the vacuum fluctuations and radiation reaction to the rate of change of the mean atomic energy for a multi-level hydrogen atom in the multipolar coupling scheme in a spacetime with a reflecting boundary. Our results show that, due to the presence of the boundary, the polarizations of the atom in the parallel direction and in the normal direction are weighted differently in terms of their contributions to the spontaneous emission rate, which is an oscillating function of the atom distance from the boundary. The possible experimental implications of our result are briefly discussed.

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

    Science.gov (United States)

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

    1999-12-06

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

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

    Science.gov (United States)

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

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-03-15

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

  18. [Determination of trace silver in water samples by solid phase extraction portable tungsten-coil electrothermal atomic absorption spectrometry].

    Science.gov (United States)

    Fan, Guang-yu; Jiang, Xiao-ming; Zheng, Cheng-bin; Hou, Xian-deng; Xu, Kai-lai

    2011-07-01

    A simple method has been developed for the determination of silver in environmental water samples using solid phase extraction with tungsten-coil electrothermal atomic absorption spectrometry. Silica gel was used as an adsorbent and packed into a syringe barrel for solid phase extraction of silver prior to its determination by using a portable tungsten-coil electrothermal atomic absorption spectrometer. Optimum conditions for adsorption and desorption of silver ion, as well as interferences from co-existing ions, were investigated. A sample pH value of 6.0, a sample loading flow rate of 4.0 mL x min(-1), and the mixture of 4% (m/v) thiourea and 2% (phi) nitrate acid with the eluent flow rate of 0.5 mL x min(-1) for desorption were selected for further studies. Under optimal conditions, a linear range of 0.20-4.00 ng x mL(-1), a limit of detection (3sigma) of 0.03 ng x mL(-1) and a preconcentration factor of 94 were achieved. The proposed method was validated by testing three environmental water samples with satisfactory results.

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

    Energy Technology Data Exchange (ETDEWEB)

    Saygi, Kadriye Ozlem; Tuzen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Chemistry Department, 38039 Kayseri (Turkey)], E-mail: msoylak@gmail.com; Elci, Latif [Pamukkale University, Faculty of Science and Arts, Chemistry Department, 20020 Denizli (Turkey)

    2008-05-30

    A solid phase extraction procedure has been established for chromium speciation in natural water samples prior to determination by atomic absorption spectrometry. The procedure is based on the solid phase extraction of the Cr(VI)- Dowex M 4195 chelating resin. After oxidation of Cr(III) to Cr(VI) by using H{sub 2}O{sub 2}, the presented method was applied to the determination of the total chromium. The level of Cr(III) is calculated by difference of total chromium and Cr(VI) levels. The procedure was optimized for some analytical parameters including pH, eluent type, flow rates of sample and eluent, matrix effects, etc. The presented method was applied for the speciation of chromium in natural water samples with satisfactory results (recoveries >95%, RSDs <10%). In the determinations of chromium species, flame atomic absorption spectrometer was used. The results were checked by using NIST SRM 2711 Montana soil and GBW 07603 Bush branched and leaves.

  20. Determination of vanadium in urine by electrothermal atomic absorption spectrometry using hot injection and preconcentration into the graphite tube

    Energy Technology Data Exchange (ETDEWEB)

    Fernandes, Kelly G.; Nobrega, Joaquim A. [Sao Carlos Univ., SP (Brazil). Dept. de Quimica; Nogueira, Ana Rita A. [Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil)]. E-mail: anarita@cppse.embrapa.br; Gomes Neto, Jose A. [UNESP, Araraquara, SP (Brazil). Inst. de Quimica

    2004-10-01

    In this work it was developed a procedure for the determination of vanadium in urine samples by electrothermal atomic absorption spectrometry using successive injections for preconcentration into a preheated graphite tube. Three 60 {mu}L volumes were sequentially injected into the atomizer preheated to a temperature of 110 deg C. Drying and pyrolysis steps were carried out after each injection. A chemical modifier, barium difluoride (100 mg L{sup -1}), and a surfactant, Triton X-100 (0.3% v v{sup -1}), were added to the urine sample. When injecting into a hot graphite tube, the sample flow-rate was 0.5 {mu} s{sup -1}. The limits of detection and quantification were 0.54 and 1.82 without preconcentration, and 0.11 and 0.37 {mu}g L{sup -1} with preconcentration, respectively. The accuracy of the procedure was evaluated by an addition-recovery experiment employing urine samples. Recoveries varied from 96.0 to 103% for additions ranging from 0.8 to 3.5 {mu}g L{sup -1} V. The developed procedure allows the determination of vanadium in urine without any sample pretreatment and with minimal dilution of the sample. (author)

  1. Efficient high-resolution X-ray emission spectrometry using synchrotron radiation; Effiziente hochaufloesende Roentgenemissionssprektrometrie mit Synchrotronstrahlung

    Energy Technology Data Exchange (ETDEWEB)

    Unterumsberger, Rainer

    2015-07-01

    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{sup -7} g/cm{sup 2} to 2.10{sup -7} g/cm{sup 2} or 3

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

    Science.gov (United States)

    Barker, J; Garner, R C

    1999-01-01

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

  3. Consistency of atomic data for the interpretation of beam emission spectra

    Energy Technology Data Exchange (ETDEWEB)

    Delabie, E; Von Hellermann, M G [FOM Institute for Plasma Physics Rijnhuizen, Association EURATOM-FOM, PO Box 1207, 3430 BE Nieuwegein (Netherlands); Brix, M; Giroud, C; Surrey, E; Zastrow, K D [EURATOM/CCFE Association, Culham Science Centre, Abingdon, OX14 3DB (United Kingdom); Jaspers, R J E [Eindhoven University of Technology, Postbus 513, 5600 MB Eindhoven (Netherlands); Marchuk, O [Forschungszentrum Juelich, Association EURATOM-FZJ, 52425, Juelich (Germany); O' Mullane, M G [Department of Physics, University of Strathclyde, 107 Rottenrow, Glasgow G4 0NG (United Kingdom); Ralchenko, Yu, E-mail: e.delabie@fz-juelich.d [Atomic Physics Division, National Institute of Standards and Technology, Gaithersburg, MD 20899-8422 (United States)

    2010-12-15

    Several collisional-radiative (CR) models (Anderson et al 2000 Plasma Phys. Control. Fusion 42 781-806, Hutchinson 2002 Plasma Phys. Control. Fusion 44 71-82, Marchuk et al 2008 Rev. Sci. Instrum. 79 10F532) have been developed to calculate the attenuation and the population of excited states of hydrogen or deuterium beams injected into tokamak plasmas. The datasets generated by these CR models are needed for the modelling of beam ion deposition and (excited) beam densities in current experiments, and the reliability of these data will be crucial to obtain helium ash densities on ITER combining charge exchange and beam emission spectroscopy. Good agreement between the different CR models for the neutral beam (NB) is found, if corrections to the fundamental cross sections are taken into account. First the H{sub {alpha}} and H{sub {beta}} beam emission spectra from JET are compared with the expected intensities. Second, the line ratios within the Stark multiplet are compared with the predictions of a sublevel resolved model. The measured intensity of the full multiplet is {approx}30% lower than expected on the basis of beam attenuation codes and the updated beam emission rates, but apart from the atomic data this could also be due to the characterization of the NB path and line of sight integration and the absolute calibration of the optics. The modelled n = 3 to n = 4 population agrees very well with the ratio of the measured H{sub {alpha}} to H{sub {beta}} beam emission intensities. Good agreement is found as well between the NB power fractions measured with beam emission in plasma and on the JET Neutral Beam Test Bed. The Stark line ratios and {sigma}/{pi} intensity ratio deviate from a statistical distribution, in agreement with the CR model in parabolic states from Marchuk et al (2010 J. Phys. B: At. Mol. Opt. Phys. 43 011002).

  4. Cloud point extraction for the determination of cadmium and lead in biological samples by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Maranhão, Tatiane De A.; Borges, Daniel L. G.; da Veiga, Márcia A. M. S.; Curtius, Adilson J.

    2005-06-01

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 °C for both elements and atomization temperatures of 1400 and 1600 °C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3σB) of 6 and 40 ng g-1, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H2O2 and HNO3. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated.

  5. Cloud point extraction for the determination of cadmium and lead in biological samples by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Maranhao, Tatiane de A. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borges, Daniel L.G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil)]. E-mail: daniel@qmc.ufsc.br; Veiga, Marcia A.M.S. da [Instituto de Quimica, Universidade de Sao Paulo, 05513-970, CP 26077, Sao Paulo, SP (Brazil); Curtius, Adilson J. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil)

    2005-06-30

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 deg. C for both elements and atomization temperatures of 1400 and 1600 deg. C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3{sigma} {sub B}) of 6 and 40 ng g{sup -1}, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H{sub 2}O{sub 2} and HNO{sub 3}. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated.

  6. Determination of trace elements in heroin by inductively coupled plasma atomic emission spectrometry using ultrasonic nebulization

    Science.gov (United States)

    Budič, Bojan; Klemenc, Sonja

    2000-06-01

    A method for the determination of Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Ni, P, S, Sr and Zn in heroin samples by ICP-AES using ultrasonic nebulization is described. The samples were microwave digested with HNO 3. To improve the detection limits and minimise the matrix interferences the experimental parameters were optimised by variation of the operating power, carrier gas flow rate and observation height above the load coil. Optimum operating conditions for most of the analytes were at operating power 1550 W, carrier gas flow rate between 0.8 and 1.0 l min -1 and observation height between 10 and 12 mm above load coil. The limits of detection were below 0.5 μg g -1 (dry mass) for most of the elements investigated. The analytical recoveries of spiked samples were in the range between 94 and 103% and precision was on average better than 6%. The analysis of heroin samples shows that the method is simple, rapid and capable of providing accurate results for all the analytes investigated with the exception of nickel which was below the limit of detection in the analyzed samples.

  7. Infrared laser ablation study of pressed soil pellets with inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mikolas, J.; Musil, P.; Stuchlikova, V.; Novotny, K.; Otruba, V.; Kanicky, V. [Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University Brno, Kotlarska 2, 61137 Brno (Czech Republic)

    2002-09-01

    Potential of infrared laser ablation (LA) coupled with ICP-AES as a technique suitable for the determination of trace elements (Zn, Cu, Ni, Cr, and V) in agricultural soils was studied. Operating parameters such as laser beam energy, laser beam focusing with respect to the sample surface, and velocity of the sample translation in the plane perpendicular to the laser beam were optimized. Soil samples were mixed with powdered Ag as a binder, and an internal standard (GeO{sub 2}), and pressed into pellets. Calibration samples were prepared by adding known amounts of oxides of elements of interest into soils of known elemental composition and then processed in the same way as the analyzed samples. Calibration curves were found to be linear at least up to several hundreds of mg kg{sup -1} for the elements of interest. The elemental contents obtained by using LA-ICP-AES were compared with those obtained by analysis using wet chemistry followed by ICP-AES with pneumatic nebulization (PN). The results were in good agreement. Accuracy was also tested using certified reference soils with a bias not exceeding 10% relative. (orig.)

  8. Determination of trace elements in plutonium by solvent extraction and ICP-atomic emission spectrometry

    Science.gov (United States)

    Patwardhan, A. B.; Joshi, M. V.; Kulkarni, V. T.; Radhakrishnan; Sumathi, S.; Jacob, Mary

    This report describes the studies carried out for the determination of trace metallic impurities in plutonium solutions. Plutonium is separated from the impurity elements by the selective extraction of plutonium in tri-butyl-phosphate. The aqueous phase containing the impurities is fed to the high temperature source of excitation such as inductively coupled argon plasma and the analysis is carried out employing computer controlled multichannel direct reading spectrometer. Based on the above studies a method has been standardized for the analysis of sixteen elements in plutonium oxide/nitrate samples. The relative standard deviation of the method for various elements is in the range of +/- 1 to 5%. The method offers distinct advantages over the conventional carrier distillation technique in terms of precision, range, and sensitivity.

  9. Separation of gold, palladium and platinum in chromite by anion exchange chromatography for inductively coupled plasma atomic emission spectrometric analysis

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Kwang Soon; Lee, Chang Heon; Park, Yeong Jae; Joe, Kih Soo; Kim, Won Ho [KAERI, Taejon (Korea, Republic of)

    2001-08-01

    A study has been carried out on the separation of gold, iridium, palladium, rhodium, ruthenium and platinum in chromite samples and their quantitative determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution condition of the minerals by fusion with sodium peroxide was optimized and chromatographic elution behavior of the rare metals was investigated by anion exchange chromatography. Spectral interference of chromium, a matrix of the minerals, was investigated on determination of gold. Chromium interfered on determination of gold at the concentration of 500 mg/L and higher. Gold plus trace amounts of iridium, palladium, rhodium and ruthenium, which must be preconcentrated before ICP-AES was separated by anion exchange chromatography after reducing Cr(VI) to Cr(III) by H{sub 2}O{sub 2}. AuCl{sup -}{sub 4} retained on the resin column was selectively eluted with acetone- HNO{sub 3}-H{sub 2}O as an eluent. In addition, iridium, palladium, rhodium and ruthenium remaining on the resin column were eluted as a group with concentrated HCl. However, platinum was eluted with concentrated HNO{sub 3}. The recovery yield of gold with acetone-HNO{sub 3}-H{sub 2}O was 100.7 {+-} 2.0 % , and the yields of palladium and platinum with concentrated HCl and HNO{sub 3} were 96.1 {+-} 1.8% and 96.6 {+-} 1.3%, respectively. The contents of gold and platinum in a Mongolian chromite sample were 32.6 {+-} 2.2 {mu}g/g and 1.6 {+-} 0.14 {mu}g/g, respectively. Palladium was not detected.

  10. Emission of hydrogen energetic neutral atoms from the Martian subsolar magnetosheath

    Science.gov (United States)

    Wang, X.-D.; Alho, M.; Jarvinen, R.; Kallio, E.; Barabash, S.; Futaana, Y.

    2016-01-01

    We have simulated the hydrogen energetic neutral atom (ENA) emissions from the subsolar magnetosheath of Mars using a hybrid model of the proton plasma charge exchanging with the Martian exosphere to study statistical features revealed from the observations of the Neutral Particle Detectors on Mars Express. The simulations reproduce well the observed enhancement of the hydrogen ENA emissions from the dayside magnetosheath in directions perpendicular to the Sun-Mars line. Our results show that the neutralized protons from the shocked solar wind are the dominant ENA population rather than those originating from the pickup planetary ions. The simulation also suggests that the observed stronger ENA emissions in the direction opposite to the solar wind convective electric field result from a stronger proton flux in the same direction at the lower magnetosheath; i.e., the proton fluxes in the magnetosheath are not cylindrically symmetric. We also confirm the observed increasing of the ENA fluxes with the solar wind dynamical pressure in the simulations. This feature is associated with a low altitude of the induced magnetic boundary when the dynamic pressure is high and the magnetosheath protons can reach to a denser exosphere, and thus, the charge exchange rate becomes higher. Overall, the analysis suggests that kinetic effects play an important and pronounced role in the morphology of the hydrogen ENA distribution and the plasma environment at Mars, in general.

  11. Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry.

    Science.gov (United States)

    Zhang, Yanlin; Adeloju, Samuel B

    2012-04-01

    A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH(4) were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe(3+), Cu(2+) and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu(2+) and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe(3+) gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg(2+). Due to similarity of resulting sensitivity, Hg(2+) was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury, respectively. The use of flow injection enabled rapid analysis with a sample throughput of 180 h(-1).

  12. 40 CFR Table 7 to Subpart Uuu of... - Continuous Compliance With Operating Limits for Metal HAP Emissions From Catalytic Cracking Units

    Science.gov (United States)

    2010-07-01

    ... Method 6010B, Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA Method 6020, Inductively Coupled Plasma-Mass Spectrometry, EPA Method 7520, Nickel Atomic Absorption, Direct Aspiration, or EPA Method 7521, Nickel Atomic Absorption, Direct Aspiration; or by an alternative to EPA Method 6010B,...

  13. Optical emission spectroscopy of excited atoms sputtered on a Ti surface under irradiation with multicharged Ar ions

    Energy Technology Data Exchange (ETDEWEB)

    Motohashi, K [Department of Applied Physics, Tokyo University of Agriculture and Technology, 2-24-16 Koganei-shi, Tokyo 184-8588 (Japan); Saitoh, Y [Department of Advanced Radiation Technology, Takasaki Advanced Radiation Research Institute, Japan Atomic Energy Agency (JAEA), Takasaki, Gunma 370-1292 (Japan); Kitazawa, S, E-mail: motohasi@cc.tuat.ac.j [Division of ITER Project, Fusion Research Development, Japan Atomic Energy Agency (JAEA), Naka, Ibaraki 311-0193 (Japan)

    2009-04-01

    Optical emission spectroscopy of excited atoms was carried out in order to investigate the sputtering processes on solid surfaces under irradiation of slow, multicharged ions. Many atomic lines of Ti I (neutral) and Ti II (single-charged ions) were observed in wavelengths from 250 to 750 nm with irradiation by Ar{sup 3+} (30 keV) on a Ti surface which was placed in a low pressure O{sub 2} atmosphere. The emission intensity of Ti I (520 nm) decreased monotonically with an increase of O{sub 2} partial pressure, whereas that of Ti I / II (670 nm, a 2nd order wavelength of 335 nm) slightly increased. From a semi-logarithmic plot of emission intensity for the 670 nm spectrum as a function of distance from the surface, the mean velocity of the excited Ti atoms and ions in a normal direction parallel to the surface, or

  14. Control of Spontaneous Emission via a Single Elliptically Polarized Light in a Five-Level Atomic System

    Institute of Scientific and Technical Information of China (English)

    ZHANG Duo; LI Jia-Hua; DING Chun-Ling; YANG Xiao-Xue

    2013-01-01

    We investigate the features of the spontaneous emission spectra in a cold five-level atomic system coupled by a single elliptically polarized control field.We use wave function approach to derive the explicit and analytical expressions of atomic spontaneous emission spectra.It is shown that some interesting phenomena such as spectralline enhancement,spectral-line suppression,spectral-line narrowing,spectral-line splitting and dark fluorescence can be observed in the spectra by appropriately modulating the phase difference between the right-hand circularly (LHC) and left-hand circularly (RHC) polarized components of the elliptically polarized control field and the intensity of external magnetic field.The number of emission peaks,the positions of fluorescence-quenching points can be also controlled.Eurthermore,we propose an ultracold 87Rb atomic system for experimental observation.These investigations may find applications in high-precision spectroscopy.

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

    Science.gov (United States)

    Kruger, Pamela C.; Parsons, Patrick J.

    2007-03-01

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass ( m0), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 ± 0.6 pg, compared to 16.1 ± 0.7 pg for the Z5100, and 23.3 ± 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection limits (3

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-03-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-01

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

  18. Secondary emission yields for 3-50 keV H[sup 0] atoms striking a copper target

    Energy Technology Data Exchange (ETDEWEB)

    Allen, J.S. (Dept. of Physics and Astronomy, Univ. of Toledo, OH (United States)); Fang, X.D. (Dept. of Physics and Astronomy, Univ. of Toledo, OH (United States)); Kvale, T.J. (Dept. of Physics and Astronomy, Univ. of Toledo, OH (United States))

    1993-06-01

    By measuring the fractions of all three charged particles (H[sup -], H[sup +], and H[sup 0]) emerging from energetic (3-50 keV) collisions of H[sup -] ions with helium atoms, the absolute secondary negative particle emission yields [gamma] have been determined for H[sup 0] atoms striking a copper surface at an angle of incidence of 30 relative to the normal to the copper surface. The measured secondary emission yields monotonically increase from a value of 1.6 negative particles per atom at an incident energy of 3 keV to a value of 4.0 negative particles per atom at an incident energy of 50 keV. The impact energy dependence of the yield [gamma] is found to be similar to the energy dependence of the yield [gamma] exhibited by the data of previous investigators, which were obtained at projectile angles of incidence different from 30 . (orig.)

  19. Determination of Zn-citrate in human milk by CIM monolithic chromatography with atomic and mass spectrometry detection.

    Science.gov (United States)

    Milačič, Radmila; Ajlec, Dejan; Zuliani, Tea; Žigon, Dušan; Ščančar, Janez

    2012-11-15

    In human milk zinc (Zn) is bound to proteins and low molecular mass (LMM) ligands. Numerous investigations demonstrated that Zn bioavailability in human milk is for infant much higher than in cow's milk. It was presumed that in the LMM human milk fraction highly bioavailable Zn-citrate prevails. However, literature data are controversial regarding the amount of Zn-citrate in human milk since analytical procedures reported were not quantitative. So, complex investigation was carried out to develop analytical method for quantitative determination of this biologically important molecule. Studies were performed within the pH range 5-7 by the use of synthetic solutions of Zn-citrate prepared in HEPES, MOPS and MES buffers. Zn-citrate was separated on weak anion-exchange convective interaction media (CIM) diethylaminoethyl (DEAE) monolithic chromatographic column using NH(4)NO(3) as an eluent. Separated Zn species were determined by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass spectrometry (ICP-MS). Quantitative separation of Zn-citrate complexes ([Zn(Cit)](-) and [Zn(Cit)(2)](4-); column recoveries 94-102%) and good repeatability and reproducibility of results with relative standard deviation (RSD±3.0%) were obtained. In fractions under the chromatographic peaks Zn-binding ligand was identified by electrospray ionization tandem mass spectrometry (ESI-MS-MS). Limits of detection (LOD) for determination of Zn-citrate species by CIM DEAE-FAAS and CIM DEAE-ICP-MS were 0.01 μg Zn mL(-1) and 0.0005 μg Zn mL(-1), respectively. Both techniques were sensitive enough for quantification of Zn-citrate in human milk. Results demonstrated that about 23% of total Zn was present in the LMM milk fraction and that LMM-Zn corresponded to Zn-citrate. The developed speciation method represents a reliable analytical tool for investigation of the percentage and the amount of Zn-citrate in human milk.

  20. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part II. Practical considerations.

    Science.gov (United States)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-07-23

    Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review, Electrothermal Vaporization and Laser Ablation will also be shortly described. The second issue is devoted to the analytical strategies for elemental quantification in such matrices, with particular insight into the isotope dilution technique, particularly used in speciation analysis by ICP-coupled separation techniques.

  1. Intra- and intercycle interference of electron emission in laser assisted XUV atomic ionization

    CERN Document Server

    Gramajo, Ana Alicia; Garibotti, Carlos Roberto; Arbó, Diego

    2016-01-01

    We study the ionization of atomic hydrogen in the direction of polarization due to a linearly polarized XUV pulse in the presence a strong field IR. We describe the photoelectron spectra as an interference problem in the time domain. Electron trajectories steming from different optical laser cycles give rise to intercycle interference energy peaks known as sidebands. These sidebands are modulated by a grosser structure coming from the intracycle interference of the two electron trajectories born during the same optical cycle. We make use of a simple semiclassical model which offers the possibility to establish a connection between emission times and the photoelectron kinetic energy. We compare the semiclassical predictions with the continuum-distorted wave strong field approximation and the ab initio solution of the time dependent Schr\\"odinger equation. We analyze such interference pattern as a function of the time delay between the IR and XUV pulse and also as a function of the laser intensity.

  2. Time-resolved measurement of atomic emission enhancement by fs-ns dual-pulsed laser-induced breakdown spectroscopy

    Institute of Scientific and Technical Information of China (English)

    Yan Li-Xin; Zhang Yong-Sheng; Zheng Guo-Xin; Liu Jing-Ru; Cheng Jian-Ping; Lü Min

    2006-01-01

    Time-resolved measurement of atomic emission enhancement is performed by using a 500-fs KrF laser pulse incident upon a high density supersonic O2 gas jet, synchronized with an orthogonal ns frequency-doubled Nd:YAG laser pulse. The ultra-short pulse serves as an igniter of the gas jet, and the subsequent ns-laser pulse significantly enhances the atomic emission. Analysis shows that the contributions to the enhancement effect are made mainly by the bremsstrahlung radiation and cascade ionization.

  3. Determination of total tin in canned food using inductively coupled plasma atomic emission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Perring, Loic; Basic-Dvorzak, Marija [Department of Quality and Safety Assurance, Nestle Research Centre, P.O. Box 44, Vers chez-les-Blanc, 1000, Lausanne (Switzerland)

    2002-09-01

    Tin is considered to be a priority contaminant by the Codex Alimentarius Commission. Tin can enter foods either from natural sources, environmental pollution, packaging material or pesticides. Higher concentrations are found in processed food and canned foods. Dissolution of the tinplate depends on the of food matrix, acidity, presence of oxidising reagents (anthocyanin, nitrate, iron and copper) presence of air (oxygen) in the headspace, time and storage temperature. To reduce corrosion and dissolution of tin, nowadays cans are usually lacquered, which gives a marked reduction of tin migration into the food product. Due to the lack of modern validated published methods for food products, an ICP-AES (Inductively coupled plasma-atomic emission spectroscopy) method has been developed and evaluated. This technique is available in many laboratories in the food industry and is more sensitive than atomic absorption. Conditions of sample preparation and spectroscopic parameters for tin measurement by axial ICP-AES were investigated for their ruggedness. Two methods of preparation involving high-pressure ashing or microwave digestion in volumetric flasks were evaluated. They gave complete recovery of tin with similar accuracy and precision. Recoveries of tin from spiked products with two levels of tin were in the range 99{+-}5%. Robust relative repeatabilities and intermediate reproducibilities were <5% for different food matrices containing >30 mg/kg of tin. Internal standard correction (indium or strontium) did not improve the method performance. Three emission lines for tin were tested (189.927, 283.998 and 235.485 nm) but only 189.927 nm was found to be robust enough with respect to interferences, especially at low tin concentrations. The LOQ (limit of quantification) was around 0.8 mg/kg at 189.927 nm. A survey of tin content in a range of canned foods is given. (orig.)

  4. X-ray photoelectron spectroscopy study of pyrolytically coated graphite platforms submitted to simulated electrothermal atomic absorption spectrometry conditions

    Energy Technology Data Exchange (ETDEWEB)

    Ruiz, Frine [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Benzo, Zully [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Quintal, Manuelita [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Garaboto, Angel [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Albornoz, Alberto [Laboratorio de Fisicoquimica de Superficies, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Brito, Joaquin L. [Laboratorio de Fisicoquimica de Superficies, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela)]. E-mail: joabrito@ivic.ve

    2006-10-15

    The present work is part of an ongoing project aiming to a better understanding of the mechanisms of atomization on graphite furnace platforms used for electrothermal atomic absorption spectrometry (ETAAS). It reports the study of unused pyrolytic graphite coated platforms of commercial origin, as well as platforms thermally or thermo-chemically treated under simulated ETAAS analysis conditions. X-ray photoelectron spectroscopy (XPS) was employed to study the elements present at the surfaces of the platforms. New, unused platforms showed the presence of molybdenum, of unknown origin, in concentrations up to 1 at.%. Species in two different oxidations states (Mo{sup 6+} and Mo{sup 2+}) were detected by analyzing the Mo 3d spectral region with high resolution XPS. The analysis of the C 1s region demonstrated the presence of several signals, one of these at 283.3 eV related to the presence of Mo carbide. The O 1s region showed also various peaks, including a signal that can be attributed to the presence of MoO{sub 3}. Some carbon and oxygen signals were consistent with the presence of C=O and C-O- (probably C-OH) groups on the platforms surfaces. Upon thermal treatment up to 2900 deg. C, the intensity of the Mo signal decreased, but peaks due to Mo oxides (Mo{sup 6+} and Mo{sup 5+}) and carbide (Mo{sup 2+}) were still apparent. Thermo-chemical treatment with 3 vol.% HCl solutions and heating up to 2900 deg. C resulted in further diminution of the Mo signal, with complete disappearance of Mo carbide species. Depth profiling of unused platforms by Ar{sup +} ion etching at increasing time periods demonstrated that, upon removal of several layers of carbonaceous material, the Mo signal disappears suggesting that this contamination is present only at the surface of the pyrolytic graphite platform.

  5. Determination of platinum traces contamination by graphite furnace atomic absorption spectrometry after preconcentration by cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Chappuy, M. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Caudron, E., E-mail: eric.caudron@eps.aphp.fr [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Groupe de Chimie Analytique de Paris-Sud, EA 4041, IFR 141, School of Pharmacy, Univ Paris-Sud, 92296 Chatenay-Malabry (France); Bellanger, A. [Department of Pharmacy, Pitie-Salpetriere Hospital (Paris Public Hospital Authority), 47 boulevard de l' hopital, 75013 Paris (France); Pradeau, D. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France)

    2010-04-15

    A simple and sensitive method is described for the determination of platinum surface contamination originating from cisplatin, carboplatin and oxaliplatin. Following extraction from swabs and preconcentration with the cloud point extraction (CPE) method, detection was by graphite furnace atomic absorption spectrometry (GFAAS). After desorption of platinum compounds from the swab, CPE involved on preconcentration of platinum in aqueous solution with diethyldithiocarbamate (DDTC) as chelating agent and Triton X-114 as extraction medium. DDTC is not only a chelating agent, but may also be a good candidate for the inactivation of platinum compounds. DDTC is recommended by the Word Health Organization (WHO) for the destruction of platinum-based anticancer drugs. The main factors affecting CPE efficiency, pH of the sample solution, concentrations of DDTC and Triton X-114, equilibration temperature and incubation time, were evaluated in order to enhance sensitivity of the method. The desorption of platinum compounds from the swab was investigated in parallel. Since platinum is bound to DDTC, it must exchange with copper in order to enhance platinum atomizing by GFAAS. A preconcentration factor of 29 was obtained for 10 mL of a platinum solution at 10 {mu}g mL{sup -1}. In optimal conditions, the limit of detection was 0.2 ng mL{sup -1}, corresponding to 2.0 ng of platinum metal on the swab. Absorbance was linear between 0.7 and 15 ng mL{sup -1}. The proposed method was applied for the determination of surface contamination by platinum compounds with correct results.

  6. UV-photochemical vapor generation of selenium for atomic absorption spectrometry: Optimization and 75Se radiotracer efficiency study

    Science.gov (United States)

    Rybínová, Marcela; Musil, Stanislav; Červený, Václav; Vobecký, Miloslav; Rychlovský, Petr

    2016-09-01

    Volatile selenium compounds were generated UV-photochemically in the continuous flow mode using four UV-photoreactors differing in the material of the reaction coil; Teflon tubing and quartz tubes with various inner diameters and wall thicknesses were tested. Atomic absorption spectrometry with an externally heated quartz furnace atomizer was employed as the detector. The relevant experimental generation parameters were optimized and the basic analytical characteristics were determined. Using formic acid as the photochemical agent, limits of detection achieved for selenium were in the range 46-102 ng L- 1 in dependence on the type of UV-photoreactor employed. When nitric acid was also added to the photochemical agent, the limits of detection were reduced to 27-44 ng L- 1. The repeatability did not exceed 2.4% (5 μg L- 1 Se(IV), n = 10). Experiments with 75Se radiotracer have been performed for the first time to quantify the efficiency of UV-photochemical vapor generation (UV-PVG) of selenium. The highest efficiency of 67 ± 1% was obtained for a UV-photoreactor containing a quartz reaction coil (2.0 mm i.d., 4.0 mm o.d.). The generation efficiency of 61 ± 1% was obtained for a Teflon reaction coil (1.0 mm i.d., 1.4 mm o.d.). Mapping of the radiotracer distribution in the individual parts of the apparatus did not reveal substantial transport losses of the analyte in the UV-PVG system.

  7. Silicic acid (Si(OH)(4)) is a significant influence upon the atomic absorption signal of aluminium measured by graphite furnace atomic absorption spectrometry (GFAAS).

    Science.gov (United States)

    Schneider, C; Exley, C

    2001-11-01

    We have identified silicic acid (Si(OH)(4)) as an important modifier of the absorbance signal of aluminium measured by graphite furnace atomic absorption spectrometry (GFAAS). The presence of Si(OH)(4) enhanced the signal by as much as 50%. The extent of the enhancement was dependent upon both [Al] and [Si(OH)(4)] and was maximal when [Al] or =0.50 mmol dm(-3). The enhancement of the Al absorbance signal was not linearly related to [Si(OH)(4)] and the effect was, generally, saturated, for all [Al] tested, at [Si(OH)(4)]> or =0.50 mmol dm(-3). Si(OH)(4) was significantly more effective in enhancing the Al absorbance signal than Mg(NO(3))(2). However, the co-occurrence of 10 mmol dm(-3) Mg(NO(3))(2) and 2 mmol dm(-3) Si(OH)(4) in samples abolished the enhancement due to Si(OH)(4). The presence of Si(OH)(4) in samples could result in an overestimation of the Al content of those samples by as much as 50%. Errors in the measurement of Al in samples containing Si(OH)(4) could be prevented using matrix-matched calibration standards. Our observation could have serious implications for the determination of Al in aqueous samples of both geochemical and biological interest. It may also point towards the application of Si(OH)(4) as a novel and effective matrix modifier in the determination of Al by GFAAS since the inclusion of Si(OH)(4) in standards and samples improved the limit of detection of Al from ca 8 nmol dm(-3) to 3 nmol dm(-3).

  8. Determination of Anionic Surfactants Using Atomic Absorption Spectrometry and Anodic Stripping Voltammetry

    Science.gov (United States)

    John, Richard; Lord, Daniel

    1999-09-01

    An experiment has been developed for our undergraduate analytical chemistry course that demonstrates the indirect analysis of anionic surfactants by techniques normally associated with metal ion determination; that is, atomic absorption spectroscopy (AAS) and anodic stripping voltammetry (ASV). The method involves the formation of an extractable complex between the synthetic surfactant anion and the bis(ethylenediamine)diaqua copper(II) cation. This complex is extracted into chloroform and then back-extracted into dilute acid. The resulting Cu(II) ions are determined by AAS and ASV. Students are required to determine the concentration of a pre-prepared "unknown" anionic surfactant solution and to collect and analyze a real sample of their choice. After the two extraction processes, students typically obtain close to 100% analytical recovery. Correlation between student AAS and ASV results is very good, indicating that any errors that occur probably result from their technique (dilutions, extractions, preparation of standards, etc.) rather than from the end analyses. The experiment is a valuable demonstration of the following analytical principles: indirect analysis; compleximetric analysis; liquid-liquid (solvent) extraction; back-extraction (into dilute acid); analytical recovery; and metal ion analysis using flame-AAS and ASV.

  9. Spatially resolved atomic and molecular emission from the very low-mass star IRS54

    CERN Document Server

    Lopez, R Garcia; Weigelt, G; Nisini, B; Antoniucci, S

    2013-01-01

    Molecular outflows from very low-mass stars (VLMSs) and brown dwarfs (BDs) have been studied very little, and only a few objects have been directly imaged. Using VLT SINFONI K-band observations, we spatially resolved, for the first time, the H2 emission around IRS54, a ~0.1-0.2 Msun Class I source. The molecular emission shows a complex structure delineating a large outflow cavity and an asymmetric molecular jet. In addition, new [FeII] VLT ISAAC observations at 1.644um allowed us to discover the atomic jet counterpart which extends down to the central source. The outflow structure is similar to those found in low-mass Class I young stellar objects (YSOs) and Classical TTauri stars (CTTSs). However, its Lacc/Lbol ratio is very high (~80%), and the derived mass accretion rate is about one order of magnitude higher than in objects with similar mass, pointing to the young nature of the investigated source.

  10. Investigation of the levels of some element in edible oil samples produced in Turkey by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mendil, Durali, E-mail: dmendil@gop.edu.tr [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Uluoezlue, Ozguer Dogan; Tuezen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Department of Chemistry, 38039 Kayseri (Turkey)

    2009-06-15

    The element contents (Fe, Mn, Zn, Cu, Pb, Co, Cd, Na, K, Ca and Mg) in edible oils (olive oil, hazelnut oil, sunflower oil, margarine, butter and corn oil) from Turkey were determined using atomic absorption spectrometry after microwave digestion. The concentrations of trace element in the samples were found to be 291.0-52.0, 1.64-0.04, 3.08-1.03, 0.71-0.05, 0.03-0.01, 1.30-0.50, 84.0-0.90, 50.1-1.30, 174.2-20.8 and 20.8-0.60 {mu}g/g for iron, manganese, zinc, copper, lead, cobalt, sodium, potassium, calcium, and magnesium, respectively. Cadmium was found to be 4.57-0.09 {mu}g/kg. The high heavy metal and minerals accumulation levels in the samples were found in olive oil for Cu, Pb, Co, margarine for Fe, K, corn oil for Zn, Mn, butter for Na, Mg, sunflower oil for Ca and hazelnut oil for Cd, respectively.

  11. Determination of trace nickel in hydrogenated cottonseed oil by electrothermal atomic absorption spectrometry after microwave-assisted digestion.

    Science.gov (United States)

    Zhang, Gai

    2012-01-01

    Microwave digestion of hydrogenated cottonseed oil prior to trace nickel determination by electrothermal atomic absorption spectrometry (ETAAS) is proposed here for the first time. Currently, the methods outlined in U.S. Pharmacopeia 28 (USP28) or British Pharmacopeia (BP2003) are recommended as the official methods for analyzing nickel in hydrogenated cottonseed oil. With these methods the samples may be pre-treated by a silica or a platinum crucible. However, the samples were easily tarnished during sample pretreatment when using a silica crucible. In contrast, when using a platinum crucible, hydrogenated cottonseed oil acting as a reducing material may react with the platinum and destroy the crucible. The proposed microwave-assisted digestion avoided tarnishing of sample in the process of sample pretreatment and also reduced the cycle of analysis. The programs of microwave digestion and the parameters of ETAAS were optimized. The accuracy of the proposed method was investigated by analyzing real samples. The results were compared with the ones by pressurized-PTFE-bomb acid digestion and ones obtained by the U.S. Pharmacopeia 28 (USP28) method. The new method involves a relatively rapid matrix destruction technique compared with other present methods for the quantification of metals in oil.

  12. Cloud point extraction for the preconcentration of silver and palladium in real samples and determination by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tavallali, Hossein; Yazdandoust, Saeed; Yazdandoust, Mozhdeh [Department of Chemistry, Payame Noor University (PNU), Shiraz (Iran)

    2010-03-15

    A cloud point extraction procedure is presented for the preconcentration and simultaneous determination of Ag{sup +} and Pd{sup 2+} in various samples. After complexation with 2-((2-((1H-benzo[d]imidazole-2-yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazol (BIMPI), which was used as a new chelating agent, analyte ions were quantitatively extracted to a phase rich in Triton X-114 following centrifugation, and determination was carried out by flame atomic absorption spectrometry (FAAS). Under the optimum experimental conditions (i. e., pH = 7.0, 15.0.10{sup -5} mol/L BIMPI and 0.036% (w/v) Triton X-114), calibration graphs were linear in the range of 28.0-430.0 {mu}g/L and 57.0-720.0 {mu}g/L with detection limits of 10.0 and 25.0 {mu}g/L for Ag{sup +} and Pd{sup 2+}, respectively. The enrichment factors were 35.0 and 28.0 for Ag{sup +} and Pd{sup 2+}, respectively. The method has been successfully applied to evaluate these metals in some real samples, including waste water, soil and hydrogenation catalyst samples. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  13. Preconcentration procedure using cloud point extraction in the presence of electrolyte for cadmium determination by flame atomic absorption spectrometry

    Science.gov (United States)

    Coelho, Luciana Melo; Arruda, Marco Aurélio Zezzi

    2005-06-01

    This paper describes a micelle-mediated phase separation in the presence of electrolyte as a preconcentration method for cadmium determination by flame atomic absorption spectrometry (FAAS). Cadmium was complexed with ammonium O,O-diethyldithiophosphate (DDTP) in an acidic medium (0.32 mol l- 1 HCl) using Triton X-114 as surfactant and quantitatively extracted into a small volume (about 20 μl) of the surfactant-rich phase after centrifugation. The chemical variables that affect the cloud point extraction, such as complexing time (0 20 min), Triton X114 concentration (0.043 0.87% w/v) and complexing agent concentration (0.01 0.1 mol l- 1), were investigated. The cloud point is formed in the presence of NaCl at room temperature (25 °C), and the electrolyte concentration (0.5 5% w/v) was also investigated. Under optimized conditions, only 8 ml of sample was used in the presence of 0.043% w/v Triton X-114 and 1% (w/v) NaCl. This method permitted limits of detection and quantification of 0.9 μg l- 1 and 2.9 μg l- 1 Cd, respectively, and a linear calibration range from 3 to 400 μg l- 1 Cd. The proposed method was applied to Cd determination in physiological solutions (containing 0.9% (w/v) of NaCl), mineral water, lake water and cigarette samples (tobacco).

  14. Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, M. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: m_ghaedi@mail.yu.ac.ir; Shokrollahi, A.; Ahmadi, F.; Rajabi, H.R. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, M. [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2008-02-11

    A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L{sup -1} HNO{sub 3} nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO{sub 3}, bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL{sup -1} for Cu{sup 2+}, Co{sup 2+} and Ni{sup 2+} along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu{sup 2+}, Ni{sup 2+} and Co{sup 2+}, respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-04-15

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

  16. Cloud point extraction and flame atomic absorption spectrometry combination for copper(II) ion in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Shokrollahi, Ardeshir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: ashokrollahi@mail.yu.ac.ir; Ghaedi, Mehrorang [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: m_ghaedi@mail.yu.ac.ir; Hossaini, Omid; Khanjari, Narges [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, Mustafa [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2008-12-30

    A cloud point extraction procedure was presented for the preconcentration of copper(II) ion in various samples. After complexation by 4-(phenyl diazenyl) benzene-1,3-diamine (PDBDM) (chrysoidine), copper(II) ions were quantitatively recovered in Triton X-114 after centrifugation. 0.5 ml of methanol acidified with 1.0 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The influence of analytical parameters including ligand, Triton X-114 and HNO{sub 3} concentrations, bath temperature, heating time, centrifuge rate and time were optimized. The effect of the matrix ions on the recovery of copper(II) ions was investigated. The detection limit (3S.D.{sub b}/m, n = 10) of 0.6 ng mL{sup -1} along with preconcentration factor of 30 and enrichment factor of 41.1 with R.S.D. of 1.0% for Cu was achieved. The proposed procedure was applied to the analysis of various environmental and biological samples.

  17. Cloud point extraction-flame atomic absorption spectrometry method for preconcentration and determination of trace cadmium in water samples.

    Science.gov (United States)

    Ning, Jinyan; Jiao, Yang; Zhao, Jiao; Meng, Lifen; Yang, Yaling

    2014-01-01

    A method based on cloud point extraction (CPE) separation/preconcentration of trace cadmium (Cd) as a prior step to its determination by flame atomic absorption spectrometry has been developed. Cadmium reacted with 8-hydroxyquinoline to form hydrophobic chelates, which were extracted into the micelles of nonionic surfactant oligoethylene glycol monoalkyl ether (Genapol X-080) in an alkaline medium. Octanol was used to depress the cloud point of Genapol X-080 in the extraction process. The chemical variables that affect the CPE, such as pH of complexation reaction, amount of chelating agent, Genapol X-080 and octanol were evaluated and optimized. Under optimized conditions, linearity was obeyed in the range of 10-500 μg/L, with the correlation coefficient of 0.9993. For 5 mL of sample solution, the enhancement factor was about 20. The limit of detection and limit of quantification of the method were 0.21 and 0.63 μg/L, respectively. The relative standard deviations (n = 6) was 3.2% for a solution containing 100 μg/L of Cd. The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. Recoveries of spiked samples varied in the range of 94.1-103.8%.

  18. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    Science.gov (United States)

    Li, Shan; Wang, Mei; Zhong, Yizhou; Zhang, Zehua; Yang, Bingyi

    2015-09-01

    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea-ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries.

  19. Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun Zhimei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Department of Chemistry and Biology, Huainan Normal University, Huainan 232001 (China); Liang Pei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)]. E-mail: liangpei@mail.ccnu.edu.cn; Ding Qiong [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Cao Jing [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)

    2006-09-21

    A new method based on the cloud point extraction (CPE) preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of trace nickel in water samples. When the micelle solution temperature is higher than the cloud point of surfactant p-octylpolyethyleneglycolphenyether (Triton X-100), the complex of Ni{sup 2+} with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) could enter surfactant-rich phase and be concentrated, then determined by GFAAS. The main factors affecting the cloud point extraction were investigated in detail. An enrichment factor of 27 was obtained for the preconcentration of Ni{sup 2+} with 10 mL solution. Under the optimal conditions, the detection limit of Ni{sup 2+} is 0.12 ng mL{sup -1} with R.S.D. of 4.3% (n = 10, c = 100 ng mL{sup -1}). The proposed method was applied to determination of trace nickel in water samples with satisfactory results.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-04-15

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

  1. The determination of wear metals in used lubricating oils by flame atomic absorption spectrometry using sulphanilic acid as ashing agent.

    Science.gov (United States)

    Ekanem, E J; Lori, J A; Thomas, S A

    1997-11-01

    A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of calcium, magnesium, zinc, iron, chromium and nickel by flame atomic absorption spectrometry. Sulphanilic acid was added to oil samples and the mixture coked and the coke ashed at 550 degrees C. The solutions of the ash were analysed by flame AAS for the metals. The release of calcium, zinc, iron and chromium was improved by the addition of sulphanilic acid to samples. The relative standard deviations of metal concentration results in the initial oil samples were 1.5% for Ca (1500 mg l(-1) level), 0.3% for Mg (100 mg l(-1) level), 3.1% for Zn (1500 mg l(-1) level), 0.7% for Fe (500 mg l(-1) level), 0.02% for Cr (50 mg l(-1) level) and 0.002% for Ni (10 mg l(-1) level). The optimum sample size for efficient metal release was 20 g while the optimum sulphanilic acid to oil ratio was 0.05 g per gram of oil for Zn and Cr and 0.10 g for Ca and Fe. Results obtained by this procedure were highly reproducible and comparable with those obtained for the same samples using standard procedures.

  2. Determination of total arsenic in coal and wood using oxygen flask combustion method followed by hydride generation atomic absorption spectrometry.

    Science.gov (United States)

    Geng, Wenhua; Furuzono, Takuya; Nakajima, Tsunenori; Takanashi, Hirokazu; Ohki, Akira

    2010-04-15

    A simple and sensitive procedure for the determination of total arsenic in coal and wood was conducted by use of oxygen flask combustion (OFC) followed by hydride generation atomic absorption spectrometry (HGAAS). The effect of various items (composition of absorbent, standing time between the combustion and filtration, particle size and mass of sample) was investigated. Under the optimized conditions of the OFC method, nine certified reference materials were analyzed, and the values of arsenic concentration obtained by this method were in good accordance with the certified values. The limit of detection (LOD) and relative standard deviation (RSD) of the method were 0.29 microg g(-1) and less than 8%, respectively. In addition, eight kinds of coals and four chromated copper arsenate (CCA)-treated wood wastes were analyzed by the present method, and the data were compared to those from the microwave-acid digestion (MW-AD) method. The determination of arsenic in solid samples was discussed in terms of applicable scope and concentration range of arsenic.

  3. Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Ghaedi, M; Shokrollahi, A; Ahmadi, F; Rajabi, H R; Soylak, M

    2008-02-11

    A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L(-1) HNO(3) nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO(3), bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL(-1) for Cu(2+), Co(2+) and Ni(2+) along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu(2+), Ni(2+) and Co(2+), respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

  4. Evaluation of arsenic, cobalt, copper and manganese in biological Samples of Steel mill workers by electrothermal atomic absorption Spectrometry.

    Science.gov (United States)

    Afridi, H I; Kazi, T G; Kazi, N G; Jamali, M K; Arain, M B; Sirajuddin; Kandhro, G A; Shah, A Q; Baig, J A

    2009-02-01

    The determination of trace and toxic elements in biological samples (blood, urine and scalp hair samples) of human beings is an important clinical test. The aim of our present study was to determine the concentration of arsenic (As), copper (Cu), cobalt (Co) and manganese (Mn), in biological samples of male production workers (PW) and quality control workers (QW) of steel mill, with aged 25-55 years, to assess the possible influence of environmental exposure. For comparison purpose, the same biological samples of unexposed healthy males of same age group were collected as control subjects. The determination of all elements in biological samples was carried out by electrothermal atomic absorption spectrometry, prior to microwave assisted acid digestion. The accuracy of the As, Cu, Co and Mn measurements was tested by simultaneously analyzing certified reference materials (CRMs) and for comparative purposes conventional wet acid digestion method was used on the same CRMs. No significant differences were observed between the analytical results and the certified values, using both methods (paired t-test at P > 0.05). The results indicate that concentrations of As, Cu, Co and Mn in all three biological samples of the exposed workers (QW and PW) were significantly higher than those of the controls. The possible correlation of these elements with the etiology of different physiological disorders is discussed. The results were also demonstrated the need of attention for improvements in workplace, ventilation and industrial hygiene practices.

  5. Comparison of selenium determination in liver samples by atomic absorption spectroscopy and inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Miksa, Irina Rudik; Buckley, Carol L; Carpenter, Nancy P; Poppenga, Robert H

    2005-07-01

    Selenium (Se) is an essential trace element that is often deficient in the natural diets of domestic animal species. The measurement of Se in whole blood or liver is the most accurate way to assess Se status for diagnostic purposes. This study was conducted to compare hydride generation atomic absorption spectroscopy (HG-AAS) with inductively coupled plasma-mass spectrometry (ICP-MS) for the detection and quantification of Se in liver samples. Sample digestion was accomplished with magnesium nitrate and nitric acid for HG-AAS and ICP-MS, respectively. The ICP-MS detection was optimized for 82Se with yttrium used as the internal standard and resulted in a method detection limit of 0.12 microg/g. Selenium was quantified by both methods in 310 samples from a variety of species that were submitted to the Toxicology Laboratory at New Bolton Center (Kennett Square, PA) for routine diagnostic testing. Paired measurements for each sample were evaluated by a mean difference plot method. Limits of agreement were used to describe the maximum differences likely to occur between the 2 methods. Results suggest that under the specified conditions ICP-MS can be reliably used in place of AAS for quantitation of tissue Se at or below 2 microg/g to differentiate between adequate and deficient liver Se concentrations.

  6. Determination of Trace Amounts of Nickel (Ⅱ) by Graphite Furnace Atomic Absorption Spectrometry Coupled with Cloud Point Extraction

    Institute of Scientific and Technical Information of China (English)

    SHAH Syed Mazhar; WANG Hao-nan; SU Xing-guang

    2011-01-01

    A new method based on the cloud point extraction(CPE) for separation and preconcentration of nickel(Ⅱ)and its subsequent determination by graphite furnace atomic absorption spectrometry(GFAAS) was proposed,8-hydroxyquinoline and Triton X-100 were usedl as the ligand and surfactant respectively. Nickel(Ⅱ) can form a hydrophobic complex with 8-hydroxyquinoline, the complex can be extracted into the small volume surfactant rich phase at the cloud point temperature(CPT) for GFAAS determination. The factors affecting the cloud point extraction,such as pH, ligand concentration, surfactant concentration, and the incubation time were optimized. Under the optimal conditions, a detection limit of 12 ng/L and a relative standard deviation(RSD) of 2.9% were obtained for Ni(Ⅱ) determination. The enrichment factor was found to be 25. The proposed method was successfully applied to the determination of nickel(Ⅱ) in certified reference material and different types of water samples and the recovery was in a range of 95% 103%.

  7. Sensitive determination of cadmium in water samples by room temperature ionic liquid-based preconcentration and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-10-17

    A sensitive preconcentration methodology for Cd determination at trace levels in water samples was developed in this work. 1-Butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]) room temperature ionic liquid (RTIL) was successfully used for Cd preconcentration, as cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex [Cd-5-Br-PADAP]. Subsequently, Cd was back-extracted from the RTIL phase with 500 {mu}L of 0.5 mol L{sup -1} nitric acid and determined by electrothermal atomic absorption spectrometry (ETAAS). A preconcentration factor of 40 was achieved with 20 mL of sample. The limit of detection (LOD) obtained under optimum conditions was 3 ng L{sup -1} and the relative standard deviation (R.S.D.) for 10 replicates at 1 {mu}g L{sup -1} Cd{sup 2+} concentration level was 3.5%, calculated at peak heights. The calibration graph was linear from concentration levels near the detection limits up to at least 5 {mu}g L{sup -1}. A correlation coefficient of 0.9997 was achieved. Validation of the methodology was performed by standard addition method and analysis of certified reference material (CRM). The method was successfully applied to the determination of Cd in river and tap water samples.

  8. Determination of platinum and palladium in road dust after their separation on immobilized fungus by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Woinska, Sylwia; Godlewska-Zylkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2011-07-15

    A flow solid phase extraction procedure based on biosorption of Pt(IV) and Pd(II) on Aspergillus sp. immobilized on cellulose resin Cellex-T was proposed for the separation and preconcentration of Pt and Pd before their determination by electrothermal atomic absorption spectrometry (ETAAS). The analytical conditions including sample pH, eluent type, flow rates of sample and eluent solutions were examined. The analytes were selectively retained on the biosorbent in acidic medium (pH 1) and subsequently eluted from the column with 1 mL of thiourea solution (0.25 mol L{sup -1} thiourea in 0.3 mol L{sup -1} HCl). The reproducibility of the procedure was below 5%. The limit of detection of the method was 0.020 ng mL{sup -1} for Pt and 0.012 ng mL{sup -1} for Pd. The method validation was performed by analysis of certified reference materials BCR-723 (tunnel dust) and SARM-76 (platinum ore). The developed separation procedure was applied to the determination of Pt and Pd in road dust samples by ETAAS. The applied biosorbent is characterized by high sorption capacity: 0.47 mg g{sup -1} for Pt and 1.24 mg g{sup -1} for Pd.

  9. Metabolism of cycloate in radish leaf: metabolite identification by packed capillary flow fast atom bombardment tandem mass spectrometry.

    Science.gov (United States)

    Onisko, B C; Barnes, J P; Staub, R E; Walker, F H; Kerlinger, N

    1994-10-01

    The metabolism of cycloate, a thiocarbamate herbicide, was investigated in mature radish leaf. Twelve new metabolites were identified by liquid chromatographic/mass spectrometric analysis using fast atom bombardment and packed capillary liquid chromatography columns. Full-scan and tandem mass spectrometric methods were employed. Application of the on-column focusing technique resulted in identifications with injections of as little as 15 ng of metabolite (20 ppb in radish). This injection technique allows the practical use of packed capillary liquid chromatography/mass spectrometry in sample-limited applications. Cycloate is oxidized to several ring-hydroxylated isomers that are subsequently glucosylated and esterified with malonic acid. Cycloate is also conjugated with glutathione. Metabolic hydrolysis of the glutathione conjugate formed a cysteine conjugate that is further metabolized by amidation with either malonic or acetic acid. Transamination of the cysteine conjugate gave a thiolactic acid derivative. Metabolites were also identified that were the result of both ring-hydroxylation and conjugation with glutathione. One of these, an N-acetylcysteine conjugate, is the first report of a mercapturic acid in plants. The structures of two of the new metabolites were confirmed by chemical synthesis.

  10. Unusual calibration curves observed for iron using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Welz, Bernhard, E-mail: w.bernardo@terra.com.b [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis-SC (Brazil); Instituto Nacional de Ciencia e Tecnologia do CMPq-INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador-BA (Brazil); Santos, Lisia M.G. dos [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis-SC (Brazil); Instituto Nacional de Controle de Qualidade em Saude-INCQS-Fiocruz, 21040-900 Rio de Janeiro-RJ (Brazil); Araujo, Rennan G.O. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis-SC (Brazil); Departamento de Quimica, Universidade Federal de Sergipe, 49100-000 Sao Cristovao-SE (Brazil); Jacob, Silvana do C. [Instituto Nacional de Controle de Qualidade em Saude-INCQS-Fiocruz, 21040-900 Rio de Janeiro-RJ (Brazil); Vale, Maria Goreti R. [Instituto Nacional de Ciencia e Tecnologia do CMPq-INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador-BA (Brazil); Instituto de Quimica, Universidade Federal do Rio Grande do Sul, 91501-970 Porto Alegre-RS (Brazil); Okruss, Michael; Becker-Ross, Helmut [Leibniz-Institut fuer Analytische Wissenschaften-ISAS-Department Berlin, 12489 Berlin (Germany)

    2010-03-15

    The simultaneous determination of cadmium and iron in plant and soil samples has been investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry. The primary cadmium resonance line at 228.802 nm and an adjacent secondary iron line at 228.726 nm, which is within the spectral interval covered by the charge-coupled device (CCD) array detector, have been used for the investigations. Due to the very high iron content in most of the soil samples the possibility has been investigated to reduce the sensitivity and extend the working range by using side pixels for measurement at the line wings instead of the line core. It has been found that the calibration curves measured at all the analytically useful pixels of this line consisted of two linear parts with distinctly different slopes. This effect has been independent of the positioning of the wavelength, i.e., if the Cd line or the Fe line was in the center of the CCD array. The most likely explanation for this unusual behavior is a significant difference between the instrument width DELTAlambda{sub Instr} and the absorption line width DELTAlambda{sub Abs}, which is quite pronounced in the case of Fe. Using both parts of the calibration curves and simultaneous measurement at the line center and at the wings made it possible to extend the working range for the iron determination to more than three orders of magnitude.

  11. Determination of lead in environmental waters with dispersive liquid-liquid microextraction prior to atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Qingxiang, E-mail: zhouqx@cup.edu.cn [School of Chemistry and Environmental Sciences, Henan Normal University, Henan Key Laboratory for Environmental Pollution Control, Key Laboratory for Yellow River and Huaihe River Water Environment and Pollution Control, Ministry of Education, Xinxiang 453007 (China); State Laboratory of Petroleum Resource and Prospecting, College of Geosciences, China University of Petroleum Beijing, Beijing 102249 (China); Zhao, Na [State Laboratory of Petroleum Resource and Prospecting, College of Geosciences, China University of Petroleum Beijing, Beijing 102249 (China); Xie, Guohong [College of Resources and Environment, Henan Institute of Science and Technology, Xinxiang 453003 (China)

    2011-05-15

    This paper established a new, rapid and sensitive method for the determination of lead in water samples preconcentrated by dispersive liquid-liquid microextraction (DLLME) prior to atomic fluorescence spectrometry. Dithizone was used as the chelating agent. In the DLLME procedure, lead formed lead-dithizone complex and migrated into the carbon tetrachloride micro-droplets. Important factors that would affect the extraction efficiency had been investigated including the kind and volume of extraction solvent and dispersive solvent, sample pH, the amount of chelating agent, extraction time and centrifugation time. The results showed that the coexisting ions containing in water samples had no obvious negative effect on the determination of lead. The experimental results indicated that the proposed method had a good linear range of 0.01-100 ng mL{sup -1} (r{sup 2} = 0.9990). The precision was 2.12% (RSD, n = 7) and the detection limit was 0.95 ng L{sup -1}. Proposed method was validated with four real environmental samples and the results indicated that the proposed method was excellent for the future use and satisfied spiked recoveries were in the range of 92.9-97.4%.

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

    Science.gov (United States)

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

    2012-01-01

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

  13. Analysis of trace element in intervertebral disc by Atomic Absorption Spectrometry techniques in degenerative disc disease in the Polish population

    Directory of Open Access Journals (Sweden)

    Andrzej Nowakowski

    2015-05-01

    Full Text Available Objective. Although trace elements are regarded crucial and their content has been determined in number of tissue there are only few papers addressing this problem in intervertebral disc in humans. Most of the trace elements are important substrates of enzymes influencing metabolism and senescence process. Others are markers of environmental pollution. Therefore the aim of the research was to analyzed of the trace element content in the intervertebral disc, which may be a vital argument recognizing the background of degenerative changes to be the effect of the environment or metabolic factors. Materials and methods. Material consist of 18 intervertebral disc from 15 patients, acquired in surgical procedure of due to the degenerative disease with Atomic Absorption Spectrometry content of Al, Cd, Co, Pb, Cu, Ni, Mo, Mg, Zn was evaluated. Results. Only 4 of the trace elements were detected in all samples. The correlation analysis showed significant positive age correlation with Al and negative in case of Co. Among elements significant positive correlation was observed between Al/Pb, Co/Mo, Al/Mg, Al/Zn Pb/Zn and Mg/Zn. Negative correlation was observed in Al/Co, Cd/Mg, Co/Mg, Mo/Mg, Co/Zn and Mo/Zn. Conclusions. This study is the first to our knowledge that profiles the elements in intervertebral disc in patients with degenerative changes. We have confirmed significant differences between the trace element contents in intervertebral disc and other tissue. It can be ground for further investigation.

  14. The use of a sequential extraction procedure for heavy metal analysis of house dusts by atomic absorption spectrometry.

    Science.gov (United States)

    Altundag, Huseyin; Dundar, Mustafa Sahin; Doganci, Secil; Celik, Muhammed; Tuzen, Mustafa

    2013-01-01

    In general, dust is considered as house or street dust. Indoor dust, as a contamination source, has been studied for many years. In this work, the original Community Bureau of Reference of the European Commission (BCR) three-stage sequential extraction procedure was applied to the fractionation of Cr, Cu, Fe, Mn, Pb, and Zn in 20 house dust samples from five different areas of Sakarya, Turkey. Acetic acid, hydroxylammonium chloride, and hydrogen peroxide plus ammonium acetate were used for the first, second, and third steps of the BCR method, respectively. The extracts were analyzed for the studied heavy metals using flame atomic absorption spectrometry. Validation of the results was performed by using a standard reference material (BCR 701 Sediment) to certify the experimental results obtained and to evaluate the reliability of the method used. The elemental loadings typically increased in magnitude according to the area order: Izmit Caddesi>Ankara Caddesi >Erenler>Karaman>Korucuk. The results were in agreement with values reported in the literature.

  15. Determination of platinum and palladium in road dust after their separation on immobilized fungus by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Woińska, Sylwia; Godlewska-Żyłkiewicz, Beata

    2011-07-01

    A flow solid phase extraction procedure based on biosorption of Pt(IV) and Pd(II) on Aspergillus sp. immobilized on cellulose resin Cellex-T was proposed for the separation and preconcentration of Pt and Pd before their determination by electrothermal atomic absorption spectrometry (ETAAS). The analytical conditions including sample pH, eluent type, flow rates of sample and eluent solutions were examined. The analytes were selectively retained on the biosorbent in acidic medium (pH 1) and subsequently eluted from the column with 1 mL of thiourea solution (0.25 mol L - 1 thiourea in 0.3 mol L - 1 HCl). The reproducibility of the procedure was below 5%. The limit of detection of the method was 0.020 ng mL - 1 for Pt and 0.012 ng mL - 1 for Pd. The method validation was performed by analysis of certified reference materials BCR-723 (tunnel dust) and SARM-76 (platinum ore). The developed separation procedure was applied to the determination of Pt and Pd in road dust samples by ETAAS. The applied biosorbent is characterized by high sorption capacity: 0.47 mg g - 1 for Pt and 1.24 mg g - 1 for Pd.

  16. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A., E-mail: djan@terra.com.br

    2013-08-01

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v{sup −1} of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L{sup −1} with a limit of detection of 4.9 μg L{sup −1} and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L{sup −1} Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials. - Highlights: ► Molybdenum was determined in plants by flame AAS. ► Flame AAS sensitivity was improved using microextraction and discrete nebulization. ► The developed procedure can be easily implemented in routine analysis. ► Green chemistry principles are followed.

  17. Sequential injection ionic liquid dispersive liquid-liquid microextraction for thallium preconcentration and determination with flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Anthemidis, Aristidis N.; Ioannou, Kallirroy-Ioanna G. [Aristotle University, Laboratory of Analytical Chemistry, Department of Chemistry, Thessaloniki (Greece)

    2012-08-15

    A novel, automatic on-line sequential injection dispersive liquid-liquid microextraction (SI-DLLME) method, based on 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF{sub 6}]) ionic liquid as an extractant solvent was developed and demonstrated for trace thallium determination by flame atomic absorption spectrometry. The ionic liquid was on-line fully dispersed into the aqueous solution in a continuous flow format while the TlBr{sub 4} {sup -} complex was easily migrated into the fine droplets of the extractant due to the huge contact area of them with the aqueous phase. Furthermore, the extractant was simply retained onto the surface of polyurethane foam packed into a microcolumn. No specific conditions like low temperature are required for extractant isolation. All analytical parameters of the proposed method were investigated and optimized. For 15 mL of sample solution, an enhancement factor of 290, a detection limit of 0.86 {mu}g L{sup -1} and a precision (RSD) of 2.7% at 20.0 {mu}g L{sup -1} Tl(I) concentration level, was obtained. The developed method was evaluated by analyzing certified reference materials while good recoveries from environmental and biological samples proved that present method was competitive in practical applications. (orig.)

  18. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Teslima Daşbaşı

    2016-01-01

    Full Text Available A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4- complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1 with detection limit of 4.0 μg L−1 (n=13. The precision as relative standard deviation was 3% (n=11, 0.20 mg L−1 and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water.

  19. Antimony speciation analysis in sediment reference materials using high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Potin-Gautier, M. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Pannier, F. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France)]. E-mail: Florence.pannier@univ-pau.fr; Quiroz, W. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Pinochet, H. [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Gregori, I. de [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile)

    2005-11-30

    This work presents the development of suitable methodologies for determination of the speciation of antimony in sediment reference samples. Liquid chromatography with a post-column photo-oxidation step and hydride generation atomic fluorescence spectrometry as detection system is applied to the separation and determination of Sb(III), Sb(V) and trimethylantimony species. Post-column decomposition and hydride generation steps were studied for sensitive detection with the AFS detector. This method was applied to investigate the conditions under which speciation analysis of antimony in sediment samples can be carried out. Stability studies of Sb species during the extraction processes of solid matrices, using different reagents solutions, were performed. Results demonstrate that for the extraction yield and the stability of Sb species in different marine sediment extracts, citric acid in ascorbic acid medium was the best extracting solution for antimony speciation analysis in this matrix (between 55% and 65% of total Sb was recovered from CRMs, Sb(III) being the predominant species). The developed method allows the separation of the three compounds within 6 min with detection limits of 30 ng g{sup -1} for Sb(III) and TMSbCl2 and 40 ng g{sup -1} for Sb(V) in sediment samples.

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

    Directory of Open Access Journals (Sweden)

    Yukun Wang

    2016-09-01

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

  1. Determination of copper in powdered chocolate samples by slurry-sampling flame atomic-absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Walter N.L. dos; Silva, Erik G.P. da; Fernandes, Marcelo S.; Araujo, Rennan G.O.; Costa, Anto' ' enio C.S.; Ferreira, Sergio L.C. [Nucleo de Excelencia em Quimica Analitica da Bahia, Universidade Federal da Bahia, Instituto de Quimica, Salvador, Bahia (Brazil); Vale, M.G.R. [Instituto de Quimica, Universidade Federal da Bahia do Rio Grande do Sul, Porto Alegre, Rio Grande do Sul (Brazil)

    2005-06-01

    Chocolate is a complex sample with a high content of organic compounds and its analysis generally involves digestion procedures that might include the risk of losses and/or contamination. The determination of copper in chocolate is important because copper compounds are extensively used as fungicides in the farming of cocoa. In this paper, a slurry-sampling flame atomic-absorption spectrometric method is proposed for determination of copper in powdered chocolate samples. Optimization was carried out using univariate methodology involving the variables nature and concentration of the acid solution for slurry preparation, sonication time, and sample mass. The recommended conditions include a sample mass of 0.2 g, 2.0 mol L{sup -1} hydrochloric acid solution, and a sonication time of 15 min. The calibration curve was prepared using aqueous copper standards in 2.0 mol L{sup -1} hydrochloric acid. This method allowed determination of copper in chocolate with a detection limit of 0.4 {mu}g g{sup -1} and precision, expressed as relative standard deviation (RSD), of 2.5% (n=10) for a copper content of approximately 30 {mu}g g{sup -1}, using a chocolate mass of 0.2 g. The accuracy was confirmed by analyzing the certified reference materials NIST SRM 1568a rice flour and NIES CRM 10-b rice flour. The proposed method was used for determination of copper in three powdered chocolate samples, the copper content of which varied between 26.6 and 31.5 {mu}g g{sup -1}. The results showed no significant differences with those obtained after complete digestion, using a t-test for comparison. (orig.)

  2. Chemical modifiers in arsenic determination in biological materials by tungsten coil electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bruhn, C.G.; Huerta, V.N.; Neira, J.Y. [Departamento de Analisis Instrumental, Facultad de Farmacia, Universidad de Concepcion, P.O. Box 237, Concepcion (Chile)

    2004-01-01

    Palladium, iridium, and rhodium are evaluated as possible chemical modifiers in the determination of As in digest solutions of biological materials (human hair and clam) by tungsten coil electrothermal atomic absorption spectrophotometry (TCA-AAS). The modifier in solution was applied onto the coil and thermally pre-reduced; the pre-reduction conditions, the amount of modifier, and the thermal program were optimized. Palladium was not satisfactory, whereas Ir and Rh were effective modifiers and rendered better relative sensitivity for As by a factor of 1.4 and 1.9, respectively compared to the case without modifier. Upon optimization of thermal conditions for As in pre-reduced Ir (2.0 {mu}g) and Rh (2.0 {mu}g) modifiers and in the digest solutions of the study matrices, Rh (2.0 {mu}g) was more effective modifier and was selected as such. The mean within-day repeatability was 2.8% in consecutive measurements (25-100 {mu}g L{sup -1}) (3 cycles, each of n=6) and confirmed good short-term stability of the absorbance measurements. The mean reproducibility was 4.4% (n=20 in a 3-day period) and the detection limit (3{sigma}{sub blank}/slope) was 29 pg (n=15). The useful coil lifetime in Rh modifier was extended to 300-400 firings. Validation was by determination of As in the certified reference material (CRM) of ''Oyster tissue'' solution with a percentage relative error (E{sub rel}%) of 2% and percentage relative standard deviation (RSD%) of 3% (n=4), and by analytical recovery of As spiked in CRM of human hair [94{+-}8% (n=4)]. The methodology is simple, fast (sample readout frequency 21 h{sup -1}), reliable, of low cost, and was applied to the determination of As in hair samples of exposed and unexposed workers. (orig.)

  3. Position Dependent Spontaneous Emission Spectra of a A-Type Atomic System Embedded in a Defective Photonic Crystal

    Institute of Scientific and Technical Information of China (English)

    S. Roshan Entezar

    2012-01-01

    We investigate the position dependent spontaneous emission spectra of a A-type three-level atom with one transition coupled to the free vacuum reservoir and the other one coupled to a double-band photonic band gap reservoir with a defect mode in the band gap. It is shown that, for the atom at the defect location, we have a two-peak spectrum with a wide dark line due to the strong coupling between the atom and the defect mode. While, when the atom is far from the defect location (or in the absence of the defect mode), the spectrum has three peaks with two dark lines due to the coupling between the atom and the photonic band gap reservoir with the largest density of states near the band edges. On the other hand, we have a four-peak spectrum for the atom at the space in between. Moreover, the average spontaneous emission spectra of the atoms uniformly embedded in high dielectric or low dielectric regions are described. It is shown that the atoms embedded in high (low) dielectric regions far from the defect location, effectively couple to the modes of the lower (upper) photonic band. However, the atoms embedded in high dielectric or low dielectric regions at the defect location, are coupled mainly to the defect modes. While, the atoms uniformly embedded in high (low) dielectric regions with a normal distance from the defect location, are coupled to both of defect and lower (upper) photonic band modes.

  4. Uncertainty Estimation of Metals and Semimetals Determination in Wastewater by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)

    Science.gov (United States)

    Marques, J. R.; Villa-Soares, S. M.; Stellato, T. B.; Silva, T. B. S. C.; Faustino, M. G.; Monteiro, L. R.; Pires, M. A. F.; Cotrim, M. E. B.

    2016-07-01

    The measurement uncertainty is a parameter that represents the dispersion of the results obtained by a method of analysis. The estimation of measurement uncertainty in the determination of metals and semimetals is important to compare the results with limits defined by environmental legislation and conclude if the analytes are meeting the requirements. Therefore, the aim of this paper is present all the steps followed to estimate the uncertainty of the determination of amount of metals and semimetals in wastewater by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). Measurement uncertainty obtained was between 4.6 and 12.2% in the concentration range of mg.L-1.

  5. Nanometer-scale isotope analysis of bulk diamond by atom probe tomography

    NARCIS (Netherlands)

    Schirhagl, R.; Raatz, N.; Meijer, J.; Markham, M.; Gerstl, S. S. A.; Degen, C. L.

    2015-01-01

    Atom-probe tomography (APT) combines field emission of atoms with mass spectrometry to reconstruct three-dimensional tomograms of materials with atomic resolution and isotope specificity. Despite significant recent progress in APT technology, application to wide-bandgap materials with strong covalen

  6. Study on Determination of copper ores by atomic absorption spectrometry%原子吸收光谱分析测定铜矿石成分探讨

    Institute of Scientific and Technical Information of China (English)

    廖淑珍

    2016-01-01

    In 1950s,China began to use atomic spectroscopy to analyze various elements,such as metallurgy, geology and machinery and other industries.With the development of the atomic spectrum analysis technology,a lot of new analytical techniques are derived. At present,the combination of atomic absorption spectrometry and atomic fluorescence spectrometry has become the main means of atomic spectrum analysis in China. In this paper,we study the chemical analysis of silver,copper,zinc and other elements in the samples of the mine.%20世纪50年代,我国开始应用原子光谱对各种元素进行分析,诸如,冶金、地质和机械等行业.随着原子光谱分析技术的不断发展,衍生出很多新的分析技术,使样品元素的研究更加清晰.目前,原子吸收和原子荧光光谱分析的结合,成为我国原子光谱分析的主要手段.本文以此为切入点,研究矿山样品中的银、铜、锌等元素的化学分析.

  7. Determination of Pb(Ⅱ) and Cu(Ⅱ) by Electrothermal Atomic Absorption Spectrometry after Preconcentration by a Schiff Base Adsorbed on Surfactant Coated Alumina

    Institute of Scientific and Technical Information of China (English)

    SABER TEHRANI Mohammad; RASTEGAR Faramarz; PARCHEHBAF Ayob; KHATAMIAN Masoomeh

    2006-01-01

    1,2-Bis(salicylidenamino)ethane loaded onto sodium dodecyl sulfate-coated alumina was used as a new chelating sorbent for the preconcentration of traces of Pb(Ⅱ) and Cu(Ⅱ) prior to atomic absorption spectrometric determination. The influence of pH, flow rates of sample and eluent solutions, and foreign ions on the recovery of Pb(Ⅱ)by electrothermal atomic absorption spectrometry (ETAAS). The data of limit of detection (3σ) for Pb(Ⅱ) and Cu(Ⅱ)posed method was successfully applied to determination of lead and copper in different water samples.

  8. Determination of trace selenium in high purity tellurium by hydride generation atomic fluorescence spectrometry after solid phase extraction of a diaminobenzidine-selenium chelate

    Science.gov (United States)

    Tong, Wang; Ying, Zeng; Jinyong, Xu

    2016-09-01

    Macroporous adsorption resin was used as the sorbent for solid phase extraction and determination of the trace Se content in high purity tellurium prior to hydride generation atomic fluorescence spectrometry analysis. Selenium was converted into an organic Se chelate using 3,3‧-diaminobenzidine and was separated from the tellurium matrix by solid phase extraction. The resin was packed as a column for solid phase extraction. Under optimum conditions, trace Se can be quantitatively extracted and the tellurium matrix can be removed. The Se in the eluate was determined by hydride generation atomic fluorescence spectrometry. The limit of detection (3σ) of this method was 0.22 ng g- 1 and the relative standard deviation (RSD, n = 5) ranged from 2.0 to 2.5% for the three investigated tellurium samples. The proposed method was successfully applied for the determination of the trace Se content in high purity tellurium samples.

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

    Science.gov (United States)

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

    2016-01-01

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

  10. Preconcentration of Copper Using 1,5-Diphenyl Carbazide as the Complexing Agent via Dispersive Liquid-Liquid Microextraction and Determination by Flame Atomic Absorption Spectrometry

    OpenAIRE

    Reyhaneh Rahnama; Elaheh Shafiei; Mohammad Reza Jamali

    2013-01-01

    We report a simple and sensitive microextraction system for the preconcentration and determination of Cu (II) by flame atomic absorption spectrometry (FAAS). Dispersive liquid-liquid microextraction is a modified solvent extraction method and its acceptor-to-donor phase ratio is greatly reduced compared with other methods. In the proposed approach, 1,5-diphenyl carbazide (DPC) was used as a copper ion selective complexing agent. Several variables such as the extraction and dispersive solvent ...

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

    OpenAIRE

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

    2014-01-01

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

  12. Application of atomic absorption spectrometry with continuous light source to analyze selected metals important for human health in different parts of oranges

    Directory of Open Access Journals (Sweden)

    Szwerc Wojciech

    2014-09-01

    Full Text Available The publication describes the application of high-resolution continuum source atomic absorption spectrometry (H-R CS AAS to determine some physiologically essential and toxic elements occurring in citrus fruits of different origins. Before analysis, the samples were mineralized using a mixture of deionized water and 69% nitric acid 3:1 (v/v in high pressure microwave digestion at 188°C during one hour.

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

    Directory of Open Access Journals (Sweden)

    Man Xiao

    2017-01-01

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

  14. Characterization of direct current He-N{sub 2} mixture plasma using optical emission spectroscopy and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Flores, O.; Castillo, F.; Martinez, H. [Laboratorio de Espectroscopia, Instituto de Ciencias Físicas, Universidad Nacional Autónoma de México, Apartado Postal 48-3, 62251, Cuernavaca, Morelos (Mexico); Villa, M.; Reyes, P. G. [Facultad de Ciencias, Universidad Autónoma del Estado de México, Estado de México (Mexico); Villalobos, S. [Laboratorio de Espectroscopia, Instituto de Ciencias Físicas, Universidad Nacional Autónoma de México, Apartado Postal 48-3, 62251, Cuernavaca, Morelos (Mexico); Facultad de Ingeniería, Universidad Nacional Autónoma de México, México D.F. (Mexico)

    2014-05-15

    This study analyses the glow discharge of He and N{sub 2} mixture at the pressure of 2.0 Torr, power of 10 W, and flow rate of 16.5 l/min, by using optical emission spectroscopy and mass spectrometry. The emission bands were measured in the wavelength range of 200–1100 nm. The principal species observed were N{sub 2}{sup +} (B{sup 2}Σ{sup +}{sub u}→X{sup 2}Σ{sup +}{sub g}), N{sub 2} (C{sup 3}Π{sub u}→B{sup 3}Π{sub g}), and He, which are in good agreement with the results of mass spectrometry. Besides, the electron temperature and ion density were determined by using a double Langmuir probe. Results indicate that the electron temperature is in the range of 1.55–2.93 eV, and the electron concentration is of the order of 10{sup 10} cm{sup −3}. The experimental results of electron temperature and ion density for pure N{sub 2} and pure He are in good agreement with the values reported in the literature.

  15. Atom-specific look at the surface chemical bond using x-ray emission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Nilsson, A.; Wassdahl, N.; Weinelt, M. [Uppsala Univ. (Sweden)] [and others

    1997-04-01

    CO and N{sub 2} adsorbed on the late transition metals have become prototype systems regarding the general understanding of molecular adsorption. It is in general assumed that the bonding of molecules to transition metals can be explained in terms of the interaction of the frontier HOMO and LUMO molecular orbitals with the d-orbitals. In such a picture the other molecular orbitals should remain essentially the same as in the free molecule. For the adsorption of the isoelectronic molecules CO and N{sub 2} this has led to the so called Blyholder model i.e., a synergetic {sigma} (HOMO) donor and {pi} (LUMO) backdonation bond. The authors results at the ALS show that such a picture is oversimplified. The direct observation and identification of the states related to the surface chemical bond is an experimental challenge. For noble and transition metal surfaces, the adsorption induced states overlap with the metal d valence band. Their signature is therefore often obscured by bulk substrate states. This complication has made it difficult for techniques such as photoemission and inverse photoemission to provide reliable information on the energy of chemisorption induced states and has left questions unanswered regarding the validity of the frontier orbitals concept. Here the authors show how x-ray emission spectroscopy (XES), in spite of its inherent bulk sensitivity, can be used to investigate adsorbed molecules. Due to the localization of the core-excited intermediate state, XE spectroscopy allows an atomic specific separation of the valence electronic states. Thus the molecular contributions to the surface measurements make it possible to determine the symmetry of the molecular states, i.e., the separation of {pi} and {sigma} type states. In all the authors can obtain an atomic view of the electronic states involved in the formation of the chemical bond to the surface.

  16. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen–argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, E. H.; Pritzl, G.

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting...... the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs......-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...

  17. Separation of seven arsenic compounds by high performance liquid chromatography with on-line detection by hydrogen-argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, Erik Huusfeldt; Pritzl, G.

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting...... the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs......-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...

  18. Trace element determination-I Use of 2,9-dimethyl-1,10-phenanthroline in determination of copper in heavy matrices by carbon furnace atomic-absorption spectrometry.

    Science.gov (United States)

    Battistoni, P; Bruni, P; Cardellini, L; Fava, G; Gobbi, G

    1980-08-01

    A method for the determination of copper in complex matrices by electrothermal atomic-absorption spectrometry has been developed. It uses neocuproine as complexing agent. The detection limit is 0.2 ng/ml, and interferences are minimized.

  19. Preconcentration procedure using cloud point extraction in the presence of electrolyte for cadmium determination by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Melo Coelho, Luciana [Departamento de Quimica Analitica, Universidade Estadual de Campinas (Unicamp), Cidade Universitaria ' Zeferino Vaz' , 13084-971, Campinas, Sao Paulo (Brazil); Arruda, Marco Aurelio Zezzi [Departamento de Quimica Analitica, Universidade Estadual de Campinas (Unicamp), Cidade Universitaria ' Zeferino Vaz' , 13084-971, Campinas, Sao Paulo (Brazil)]. E-mail: zezzi@iqm.unicamp.br

    2005-06-30

    This paper describes a micelle-mediated phase separation in the presence of electrolyte as a preconcentration method for cadmium determination by flame atomic absorption spectrometry (FAAS). Cadmium was complexed with ammonium O,O-diethyldithiophosphate (DDTP) in an acidic medium (0.32 mol l{sup -} {sup 1} HCl) using Triton X-114 as surfactant and quantitatively extracted into a small volume (about 20 {mu}l) of the surfactant-rich phase after centrifugation. The chemical variables that affect the cloud point extraction, such as complexing time (0-20 min), Triton X114 concentration (0.043-0.87% w/v) and complexing agent concentration (0.01-0.1 mol l{sup -} {sup 1}), were investigated. The cloud point is formed in the presence of NaCl at room temperature (25 deg. C), and the electrolyte concentration (0.5-5% w/v) was also investigated. Under optimized conditions, only 8 ml of sample was used in the presence of 0.043% w/v Triton X-114 and 1% (w/v) NaCl. This method permitted limits of detection and quantification of 0.9 {mu}g l{sup -} {sup 1} and 2.9 {mu}g l{sup -} {sup 1} Cd, respectively, and a linear calibration range from 3 to 400 {mu}g l{sup -} {sup 1} Cd. The proposed method was applied to Cd determination in physiological solutions (containing 0.9% (w/v) of NaCl), mineral water, lake water and cigarette samples (tobacco)

  20. Simultaneous flow injection preconcentration of lead and cadmium using cloud point extraction and determination by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Edson Luiz [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario, 303, CP 96, 13416-000 Piracicaba, SP (Brazil)], E-mail: edsonqmc@hotmail.com; Santos Roldan, Paulo dos [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario, 303, CP 96, 13416-000 Piracicaba, SP (Brazil)

    2009-01-15

    A flow injection (FI) micelle-mediated separation/preconcentration procedure for the determination of lead and cadmium by flame atomic absorption spectrometry (FAAS) has been proposed. The analytes reacted with 1-(2-thiazolylazo)-2-naphthol (TAN) to form hydrophobic chelates, which were extracted into the micelles of 0.05% (w/v) Triton X-114 in a solution buffered at pH 8.4. In the preconcentration stage, the micellar solution was continuously injected into a flow system with four mini-columns packed with cotton, glass wool, or TNT compresses for phase separation. The analytes-containing micelles were eluted from the mini-columns by a stream of 3 mol L{sup -1} HCl solution and the analytes were determined by FAAS. Chemical and flow variables affecting the preconcentration of the analytes were studied. For 15 mL of preconcentrated solution, the enhancement factors varied between 15.1 and 20.3, the limits of detection were approximately 4.5 and 0.75 {mu}g L{sup -1} for lead and cadmium, respectively. For a solution containing 100 and 10 {mu}g L{sup -1} of lead and cadmium, respectively, the R.S.D. values varied from 1.6 to 3.2% (n = 7). The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. The method was susceptible to matrix effects, but these interferences were minimized by adding barium ions as masking agent in the sample solutions, and recoveries from spiked sample varied in the range of 95.1-107.3%.

  1. Determination of ultra trace arsenic species in water samples by hydride generation atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Ulusoy, Halil Ibrahim, E-mail: hiulusoy@yahoo.com [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey); Akcay, Mehmet; Ulusoy, Songuel; Guerkan, Ramazan [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey)

    2011-10-10

    Graphical abstract: The possible complex formation mechanism for ultra-trace As determination. Highlights: {yields} CPE/HGAAS system for arsenic determination and speciation in real samples has been applied first time until now. {yields} The proposed method has the lowest detection limit when compared with those of similar CPE studies present in literature. {yields} The linear range of the method is highly wide and suitable for its application to real samples. - Abstract: Cloud point extraction (CPE) methodology has successfully been employed for the preconcentration of ultra-trace arsenic species in aqueous samples prior to hydride generation atomic absorption spectrometry (HGAAS). As(III) has formed an ion-pairing complex with Pyronine B in presence of sodium dodecyl sulfate (SDS) at pH 10.0 and extracted into the non-ionic surfactant, polyethylene glycol tert-octylphenyl ether (Triton X-114). After phase separation, the surfactant-rich phase was diluted with 2 mL of 1 M HCl and 0.5 mL of 3.0% (w/v) Antifoam A. Under the optimized conditions, a preconcentration factor of 60 and a detection limit of 0.008 {mu}g L{sup -1} with a correlation coefficient of 0.9918 was obtained with a calibration curve in the range of 0.03-4.00 {mu}g L{sup -1}. The proposed preconcentration procedure was successfully applied to the determination of As(III) ions in certified standard water samples (TMDA-53.3 and NIST 1643e, a low level fortified standard for trace elements) and some real samples including natural drinking water and tap water samples.

  2. Determination of calcium, magnesium and zinc in lubricating oils by flame atomic absorption spectrometry using a three-component solution.

    Science.gov (United States)

    Zmozinski, Ariane V; de Jesus, Alexandre; Vale, Maria G R; Silva, Márcia M

    2010-12-15

    Lubricating oils are used to decrease wear and friction of movable parts of engines and turbines, being in that way essential for the performance and the increase of that equipment lifespan. The presence of some metals shows the addition of specific additives such as detergents, dispersals and antioxidants that improve the performance of these lubricants. In this work, a method for determination of calcium, magnesium and zinc in lubricating oil by flame atomic absorption spectrometry (F AAS) was developed. The samples were diluted with a small quantity of aviation kerosene (AVK), n-propanol and water to form a three-component solution before its introduction in the F AAS. Aqueous inorganic standards diluted in the same way have been used for calibration. To assess the accuracy of the new method, it was compared with ABNT NBR 14066 standard method, which consists in diluting the sample with AVK and in quantification by F AAS. Two other validating methods have also been used: the acid digestion and the certified reference material NIST (SRM 1084a). The proposed method provides the following advantages in relation to the standard method: significant reduction of the use of AVK, higher stability of the analytes in the medium and application of aqueous inorganic standards for calibration. The limits of detection for calcium, magnesium and zinc were 1.3 μg g(-1), 0.052 μg g(-1) and 0.41 μg g(-1), respectively. Concentrations of calcium, magnesium and zinc in six different samples obtained by the developed method did not differ significantly from the results obtained by the reference methods at the 95% confidence level (Student's t-test and ANOVA). Therefore, the proposed method becomes an efficient alternative for determination of metals in lubricating oil.

  3. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shan, E-mail: ls_tuzi@163.com; Wang, Mei, E-mail: wmei02@163.com; Zhong, Yizhou, E-mail: yizhz@21cn.com; Zhang, Zehua, E-mail: kazuki.0101@aliyun.com; Yang, Bingyi, E-mail: e_yby@163.com

    2015-09-01

    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea–ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries. - Highlights: • Cloud point extraction was firstly established to determine trace inorganic arsenic(As) species combining with HGAFS. • Separate As(III) and As(V) determinations improve the accuracy. • Ultrasonic release of complexed As(V) enables complete As(V) reduction to As(III). • Direct HGAFS analysis can be performed.

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

    Directory of Open Access Journals (Sweden)

    SIMONA MURKO

    2010-01-01

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

  5. Evidence for aluminum-binding erythropoietin by size-exclusion chromatography coupled to electrothermal absorption atomic spectrometry.

    Science.gov (United States)

    Veiga, Marlei; Bohrer, Denise; Noremberg, Simone; do Nascimento, Paulo C; de Carvalho, Leandro M

    2011-11-01

    Erythropoietin (EPO) is a glycoprotein that stimulates erythropoiesis and is clinically used for treating anemia during chronic renal failure and for anemia in preterm infants. EPO formulations usually have elevated rates of contamination due to aluminum (Al), which is toxic to both types of patients. Size-exclusion chromatography (SEC) coupled with graphite furnace atomic absorption spectrometry (GF AAS) was employed to separate proteins and to quantify the amount of aluminum present in the elution volume corresponding to EPO and, therefore, to evaluate possible binding. Because EPO formulations contain human serum albumin (HSA), a chromatographic method was optimized for the separation of these proteins. Subsequent to the chromatographic separation, 1-mL fractions of the column effluent were collected, and the Al content in these aliquots was measured by GF AAS. EPO and HSA samples were incubated with Al for 4h at 4°C and 37°C as well as for 16 h at 4°C and 37°C. Afterwards, they were injected into the chromatographic system. These samples were also submitted to ultrafiltration (10 and 50 kDa membranes), and Al was measured in the ultrafiltrates. The results showed that Al was present in the eluent volume corresponding to the EPO peak but not in the HSA peak in the chromatograms. Temperature strengthened the interaction because the Al present in the EPO fraction was 3 times higher at 37°C compared to 4°C. Thirty-eight percent of the Al present in a 2.4 μg/mL EPO standard solution, and approximately 50% of the Al in formulation samples containing approximately 11 μg/mL EPO and either citrate or phosphate, were non-ultrafiltrable, which suggests that EPO is an effective Al acceptor in vitro.

  6. Preconcentration of gold ions from water samples by modified organo-nanoclay sorbent prior to flame atomic absorption spectrometry determination

    Energy Technology Data Exchange (ETDEWEB)

    Afzali, Daryoush, E-mail: daryoush_afzali@yahoo.com [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Mostafavi, Ali [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mirzaei, Mohammad [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2010-09-15

    In this work, the applicability of modified organo nanoclay as a new and easy prepared solid sorbent for the preconcentration of trace amounts of Au(III) ion from water samples is studied. The organo nanoclay was modified with 5-(4'-dimethylamino benzyliden)-rhodanine and used as a sorbent for separation of Au(III) ions. The sorption of gold ions was quantitative in the pH range of 2.0-6.0. Quantitative desorption occurred with 6.0 mL of 1.0 mol L{sup -1} Na{sub 2}S{sub 2}O{sub 3}. The amount of eluted Au(III) was measured using flame atomic absorption spectrometry. In the initial solution the linear dynamic range was in the range of 0.45 ng mL{sup -1} to 10.0 {mu}g mL{sup -1}, the detection limit was 0.1 ng mL{sup -1} and the preconcentration factor was 105. Also, the relative standard deviation was {+-}2.3% (n = 8 and C = 2.0 {mu}g mL{sup -1}) and the maximum capacity of the sorbent was 3.9 mg of Au(III) per gram of modified organo nanoclay. The influences of the experimental parameters including sample pH, eluent volume and eluent type, sample volume, and interference of some ions on the recoveries of the gold ion were investigated. The proposed method was applied for preconcentration and determination of gold in different samples.

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

    Energy Technology Data Exchange (ETDEWEB)

    Hartmann, Georg, E-mail: georg.hartmann@tum.de [Department of Chemistry, Technische Universitaet Muenchen, 85748 Garching (Germany); Schuster, Michael, E-mail: michael.schuster@tum.de [Department of Chemistry, Technische Universitaet Muenchen, 85748 Garching (Germany)

    2013-01-25

    Highlights: Black-Right-Pointing-Pointer We optimized cloud point extraction and ET-AAS parameters for Au-NPs measurement. Black-Right-Pointing-Pointer A selective ligand (sodium thiosulphate) is introduced for species separation. Black-Right-Pointing-Pointer A limit of detection of 5 ng Au-NP per L is achieved for aqueous samples. Black-Right-Pointing-Pointer Measurement of samples with high natural organic mater content is possible. Black-Right-Pointing-Pointer Real water samples including wastewater treatment plant effluent were analyzed. - Abstract: The determination of metallic nanoparticles in environmental samples requires sample pretreatment that ideally combines pre-concentration and species selectivity. With cloud point extraction (CPE) using the surfactant Triton X-114 we present a simple and cost effective separation technique that meets both criteria. Effective separation of ionic gold species and Au nanoparticles (Au-NPs) is achieved by using sodium thiosulphate as a complexing agent. The extraction efficiency for Au-NP ranged from 1.01 {+-} 0.06 (particle size 2 nm) to 0.52 {+-} 0.16 (particle size 150 nm). An enrichment factor of 80 and a low limit of detection of 5 ng L{sup -1} is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L{sup -1}. The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L{sup -1} is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples.

  8. The determination of low lead levels in the bone of lead-depleted mice by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Iavicoli, I.; Carelli, G.; Castellino, N. [Univ. Cattolica del Sacro Cuore, Roma (Italy). Inst. of Occupational Health; Schlemmer, G. [Bodenseewerk Perkin-Elmer und Co. GmbH, Ueberlingen (Germany)

    2001-08-01

    Low lead levels in the femurs of mice fed with a lead-depleted diet have been determined by use of electrothermal atomic absorption spectrometry with Zeeman-effect background correction. The method is based on the use of Mg(NO{sub 3}){sub 2}/Pd as matrix modifier which enables significant reduction of the spectral interferences prevalent if chemical modifiers based on NH{sub 4}H{sub 2}PO{sub 4} with either Ca or Mg are used for samples rich in Ca{sub 3}(PO{sub 4}){sub 2} matrix. The method was developed and validated by use of the NIST standard reference material 1486 bone. Bones were decomposed in a pressurized microwave-heated system using 70% nitric acid. Forty-three mice femurs, with a mass of 74.62 {+-} 12.54 mg, were dissolved in concentrated nitric acid. The lead results found in SRM 1486 (1.25 {+-} 0.15 {mu}g g{sup -1}, n = 9) were in good agreement with the certificate (1.335 {+-} 0.014 {mu}g g{sup -1}). Recoveries of 200 ng lead added to the SRM before or after digestion were 99.0 {+-} 1.4% and 98.5 {+-} 1.6%, respectively. The lead detection limit in bone samples is 0.06 {mu}g g{sup -1} dry mass. This method is, therefore, suitable for the determination of very low lead levels (0.06-0.20 {mu}g Pb kg{sup -1} bone) in the femurs of mice fed a diet with lead level of < 20 {mu}g kg{sup -1}. (orig.)

  9. Coacervative extraction of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hagarová, Ingrid, E-mail: hagarova@fns.uniba.sk; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb–dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l{sup −1} HNO{sub 3}. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l{sup −1}, quantification limit of 0.38 μg l{sup −1}, relative standard deviation of 4.2% (for 2 μg l{sup −1} of Pb; n = 26), linearity of the calibration graph in the range of 0.5–4.0 μg l{sup −1} (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91–96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters. - Highlights: • The potential of coacervates for the extraction of metal ions is examined. • No difficulties in coupling of ETAAS with the proposed CAE are observed. • Achieved preconcentration factor results in enhanced sensitivity. • Analytical performance is confirmed by the reliable determination of trace Pb. • The proposed CAE is ecofriendly and efficient.

  10. Coacervative extraction of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Hagarová, Ingrid; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb-dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l- 1 HNO3. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l- 1, quantification limit of 0.38 μg l- 1, relative standard deviation of 4.2% (for 2 μg l- 1 of Pb; n = 26), linearity of the calibration graph in the range of 0.5-4.0 μg l- 1 (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91-96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters.

  11. Determination of some heavy metal levels in soft drinks on the Ghanaian market using atomic absorption spectrometry method.

    Science.gov (United States)

    Ackah, Michael; Anim, Alfred Kwablah; Zakaria, Nafisatu; Osei, Juliet; Saah-Nyarko, Esther; Gyamfi, Eva Tabuaa; Tulasi, Delali; Enti-Brown, Sheriff; Hanson, John; Bentil, Nash Owusu

    2014-12-01

    Twenty-three soft drink samples (i.e., four pineapple-based fruit drinks, eight citrus-based fruit juices, one soya-based drink, three cola carbonated drinks, one apple-based fruit drink, and six cocktail fruit drinks) were randomly purchased from retail outlets in an urban market in Accra and analyzed for the concentrations of iron, cobalt, cadmium, zinc, lead, and copper using flame atomic absorption spectrometry. The mean concentration of iron and cadmium were 0.723 ± 0.448 mg/L and 0.032 ± 0.012 mg/L, respectively. The mean cobalt concentration was 0.071 ± 0.049 mg/L, while the mean Zn concentration in the samples was 0.060 ± 0.097 mg/L. The mean concentrations of Pb and Cu in the fruit juice samples were 0.178 ± 0.091 mg/L and 0.053 ± 0.063 mg/L respectively. About 78 % of the samples exceeded the United States Environmental Protection Agency (USEPA) maximum contaminant level of 0.3 mg/L prescribed for iron, whereas all the samples exceeded the USEPA maximum contaminant level of 0.005 mg/L prescribed for cadmium. About 91 % of the samples exceeded the EU maximum contaminant level prescribed for lead insoft drinks.

  12. Determination of lead in blood by chelation with ammonium pyrrolidine dithio-carbamate followed by tungsten-coil atomic absorption spectrometry

    Science.gov (United States)

    Salido, Arthur; Sanford, Caryn L.; Jones, Bradley T.

    1999-08-01

    An inexpensive, bench-top blood Pb analyzer has been developed. The system is based on tungsten-coil atomic absorption spectrometry. Pb atomization occurs on W-coils extracted from commercially available slide projector bulbs. The system has minimal power requirements: 120 ACV and 15 A. A small, computer-controlled CCD spectrometer is used as the detector. A Pb hollow cathode lamp is used as the source. Blood Pb is chelated with ammonium pyrrolidine dithio-carbamate and extracted into methyl iso-butyl ketone (4-methyl 2-pentanone). Twenty-microliter volumes of the organic phase are deposited on the W-coil, dried at 1.4 A, charred at 2.3 A and atomized at 6.0 A. Graphite furnace atomic absorption spectrometry is used as a comparison for W-coil results. Levels 1-4 of a NIST standard reference material 955b ‘lead in bovine blood’ are used to test accuracy and precision. The analytical figures of merit for the system are: 12-pg instrument detection limit, 24-pg blood detection limit and a characteristic mass of 28 pg.

  13. Determination of methane emission rates on a biogas plant using data from laser absorption spectrometry.

    Science.gov (United States)

    Groth, Angela; Maurer, Claudia; Reiser, Martin; Kranert, Martin

    2015-02-01

    The aim of the work was to establish a method for emission control of biogas plants especially the observation of fugitive methane emissions. The used method is in a developmental stage but the topic is crucial to environmental and economic issues. A remote sensing measurement method was adopted to determine methane emission rates of a biogas plant in Rhineland-Palatinate, Germany. An inverse dispersion model was used to deduce emission rates. This technique required one concentration measurement with an open path tunable diode laser absorption spectrometer (TDLAS) downwind and upwind the source and basic wind information, like wind speed and direction. Different operating conditions of the biogas plant occurring on the measuring day (December 2013) could be represented roughly in the results. During undisturbed operational modes the methane emission rate averaged 2.8 g/s, which corresponds to 4% of the methane gas production rate of the biogas plant.

  14. Comparative mass spectrometric analyses of Photofrin oligomers by fast atom bombardment mass spectrometry, UV and IR matrix-assisted laser desorption/ionization mass spectrometry, electrospray ionization mass spectrometry and laser desorption/jet-cooling photoionization mass spectrometry.

    Science.gov (United States)

    Siegel, M M; Tabei, K; Tsao, R; Pastel, M J; Pandey, R K; Berkenkamp, S; Hillenkamp, F; de Vries, M S

    1999-06-01

    Photofrin (porfimer sodium) is a porphyrin derivative used in the treatment of a variety of cancers by photodynamic therapy. This oligomer complex and a variety of porphyrin monomers, dimers and trimers were analyzed with five different mass spectral ionization techniques: fast atom bombardment, UV and IR matrix-assisted laser desorption/ionization, electrospray ionization, and laser desorption/jet-cooling photoionization. All five approaches resulted in very similar oligomer distributions with an average oligomer length of 2.7 +/- 0.1 porphyrin units. In addition to the Photofrin analysis, this study provides a side-by-side comparison of the spectra for the five different mass spectrometric techniques.

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

    Science.gov (United States)

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

    2009-06-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Duarte, Fabio Andrei; Bizzi, Cezar Augusto; Goldschmidt Antes, Fabiane; Dressler, Valderi Luiz [Departamento de Quimica, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Flores, Erico Marlon de Moraes [Departamento de Quimica, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil)], E-mail: flores@quimica.ufsm.br

    2009-06-15

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

  17. Glow Discharge Emission Spectrometry (GDOES): Theoretical Introduction, General Aspects, and its Applications within the Framework of the Technofusion Programs; Glow Discharge Emission Spectrometry (GDOES): Introduccion Teorica, Aspectos Generales y Aplicabilidad en el Marco del Programa Technofusion

    Energy Technology Data Exchange (ETDEWEB)

    Martin-Rojo, A. B.; Gonzalez, M.; Tabares, F. L.

    2013-02-01

    The demand by material research groups for the direct composition analysis of solids is increasing as a solution to the time-consuming problems and errors inherent to classical chemical analysis, where the attack and solubilisation of the starting material is mandatory, often producing the introduction of impurities and component loss of the initial matrix. From the existing solid analysis techniques the present work is focused on the Glow Discharge Emission Spectrometry (GDOES), a fast, simply-executed technique, for which quantitative, high resolution depth profile determination of any element in the periodic table can be performed with a high sensibility and detection limit. The theoretical concepts, the required instrumentation and the basic analytic applications are revised, giving especial attention to the issues related to the analysis of materials for fusion applications. Finally, a comparative study with a more advanced spectroscopic technique (Secondary Ion Mass Spectrometry (SIMS)) is performed and the concomitance of both techniques to correct limitations such as the spatial resolution and the quantification of the analysis, important factors that are required in the chemical analysis of the complex materials used in Fusion, is addressed. (Author) 41 refs.

  18. Topographical and Chemical Imaging of a Phase Separated Polymer Using a Combined Atomic Force Microscopy/Infrared Spectroscopy/Mass Spectrometry Platform.

    Science.gov (United States)

    Tai, Tamin; Karácsony, Orsolya; Bocharova, Vera; Van Berkel, Gary J; Kertesz, Vilmos

    2016-03-01

    In this paper, the use of a hybrid atomic force microscopy/infrared spectroscopy/mass spectrometry imaging platform was demonstrated for the acquisition and correlation of nanoscale sample surface topography and chemical images based on infrared spectroscopy and mass spectrometry. The infrared chemical imaging component of the system utilized photothermal expansion of the sample at the tip of the atomic force microscopy probe recorded at infrared wave numbers specific to the different surface constituents. The mass spectrometry-based chemical imaging component of the system utilized nanothermal analysis probes for thermolytic surface sampling followed by atmospheric pressure chemical ionization of the gas phase species produced with subsequent mass analysis. The basic instrumental setup, operation, and image correlation procedures are discussed, and the multimodal imaging capability and utility are demonstrated using a phase separated poly(2-vinylpyridine)/poly(methyl methacrylate) polymer thin film. The topography and both the infrared and mass spectral chemical images showed that the valley regions of the thin film surface were comprised primarily of poly(2-vinylpyridine) and hill or plateau regions were primarily poly(methyl methacrylate). The spatial resolution of the mass spectral chemical images was estimated to be 1.6 μm based on the ability to distinguish surface features in those images that were also observed in the topography and infrared images of the same surface.

  19. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part II. Practical 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

    Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

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

    Science.gov (United States)

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

    2016-06-01

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

  1. Metastable argon atom density in complex argon/acetylene plasmas determined by means of optical absorption and emission spectroscopy

    Science.gov (United States)

    Sushkov, Vladimir; Herrendorf, Ann-Pierra; Hippler, Rainer

    2016-10-01

    Optical emission and absorption spectroscopy has been utilized to investigate the instability of acetylene-containing dusty plasmas induced by growing nano-particles. The density of Ar(1s5) metastable atoms was derived by two methods: tunable diode laser absorption spectroscopy and with the help of the branching ratio method of emitted spectral lines. Results of the two techniques agree well with each other. The density of Ar(1s3) metastable atoms was also measured by means of optical emission spectroscopy. The observed growth instability leads to pronounced temporal variations of the metastable and other excited state densities. An analysis of optical line ratios provides evidence for a depletion of free electrons during the growth cycle but no indication for electron temperature variations.

  2. Online Determination of Sm, Eu and Yb in Environmental Samples by Inductively Coupled Plasma – Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    J. Dilip Kumar

    2007-01-01

    Full Text Available A procedure was developed for the determination of Sm, Eu and Yb in water samples by inductively coupled plasma-optical emission spectrometry (ICP-OES after preconcentration on synthesized 5-(4-pyridyl azo-8-quinolinol supported by Borassus flabellifer inflorescence (BFI. The sorbed element was subsequently eluted with 0.4 M HNO3 and the acid eluates were analyzed by ICP-OES. Under the optimal conditions, Sm, Eu and Yb in aqueous samples were concentrated 100-fold. Recoveries were obtained by the proposed method in the range of 98.6 -99.8%. This method was also applied for the analysis of spiked and natural water samples. The results provide strong evidence to support the hypothesis of an adsorption mechanism.

  3. Effect of magnesium acetylacetonate on the signal of organic forms of vanadium in graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Kowalewska, Zofia; Welz, Bernhard; Castilho, Ivan N B; Carasek, Eduardo

    2013-01-15

    The aim of this work was to investigate the influence of magnesium acetylacetonate (MgA) on the signal of organic forms of vanadium in xylene solution by graphite furnace atomic absorption spectrometry. MgA alone or mixed with palladium acetylacetonate (PdA) was considered as a chemical modifier. It has been found that MgA does not improve, but decreases significantly the integrated absorbance of V in the form of alkyl-aryl sulfonates, acetylacetonates, porphyrins and in lubricating oils, while its effect is negligible in the case of "dark products" from petroleum distillation, i.e., heavy oil fractions and residues. The decrease is also observed in the presence of Pd. The MgA (or MgA+PdA) effect on the integrated absorbance of V has been studied using the following variants: different ways of modifier application, various pyrolysis temperature, additional application of air ashing, preliminary pretreatment with iodine and methyltrioctylammonium chloride, application of various graphite furnace heating systems (longitudinal or transverse) and various optical and background correction systems (medium-resolution line source spectrometer with deuterium background correction or high-resolution continuum source spectrometer). The experiments indicate formation of more refractory compounds as a possible reason for the decrease of the integrated absorbance for some forms of V in the presence of MgA. The application of MgA as a chemical modifier in V determination is not recommended. Results of this work have general importance as, apart from the intentional use of MgA as a modifier, organic Mg compounds, present in petroleum products for other reason (e.g. as an additive), can influence the signal of V compounds and hence the accuracy in V determination. Generally, petroleum products with known amount of V are recommended as standards; however, lubricating oils can be inadequate for "dark products" from petroleum distillation. In the case of unknown samples it is

  4. Lead and cadmium in human teeth from Jordan by atomic absorption spectrometry: Some factors influencing their concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Alomary, A. [Department of Chemistry, Yarmouk University, Irbid (Jordan)]. E-mail: ahmedalomary1000@hotmail.com; Al-Momani, I.F. [Department of Chemistry, Yarmouk University, Irbid (Jordan); Massadeh, A.M. [Department of Medicinal Chemistry and Pharmacognosy, Faculty of Pharmacy, Jordan University of Science and Technology, Irbid (Jordan)

    2006-10-01

    The aim of this study was to measure the concentrations of lead (Pb) and cadmium (Cd) in human teeth and to investigate the affecting factors. Teeth samples (n = 268) were collected from people living in different cities in Jordan including Amman, Zarqa, Al-Mafraq and Irbid and analyzed for Pb and Cd using atomic absorption spectrometry (AAS). A questionnaire was used to gather information on each person, such as age, sex, place where the patient lives, smoking, presence of amalgam fillings inside the mouth, and whether the patient uses toothpaste or not. The mean concentrations of Pb and Cd were 28.91 {mu}g/g and 0.44 {mu}g/g, respectively. The results indicate that there is a clear relation between Pb and Cd concentrations and the presence of amalgam fillings, smoking, and place of living. Pb was sex-dependent, whereas Cd was not. Our results show that Pb and Cd concentrations in samples obtained from Al-Mafraq and Irbid are higher than those obtained from Amman and Zarqa. Pb was highest in Mafraq, whereas Cd was highest in Irbid. The Pb and Cd concentrations in teeth from smokers (means: Pb = 31.89 {mu}g/g, Cd = 0.49 {mu}g/g) were significantly higher than those from nonsmokers (means: Pb = 24.07 {mu}g/g, Cd = 0.37 {mu}g/g). Pb and Cd concentrations in teeth of patients with amalgam fillings (means: Pb = 31.02 {mu}g/g and Cd = 0.52 {mu}g/g) were significantly higher than those from patients without amalgam fillings (means: Pb = 26.87 {mu}g/g and Cd = 0.41 {mu}g/g). Our results show that brushing the teeth daily with toothpaste does not significantly decrease the concentration of both Pb and Cd. The mean concentrations of Pb and Cd do not vary significantly between the ages 20-30, 31-40, and 41-50, but both increased rapidly at age 51-60.

  5. Oxygen dayglow emissions as proxies for atomic oxygen and ozone in the mesosphere and lower thermosphere

    Science.gov (United States)

    Yankovsky, Valentine A.; Martyshenko, Kseniia V.; Manuilova, Rada O.; Feofilov, Artem G.

    2016-09-01

    The main goal of this study is to propose and then to justify a set of methods for retrieving the [O] and [O3] altitude distributions from the observation of emissions of the excited oxygen molecules and O(1D) atom at daytime in the mesosphere and lower thermosphere (MLT) region. In other words, we propose retrieving the [O] and [O3] using the proxies. One of the main requirements for the proxy is that the measured value should be directly related to a variable of our interest while, at the same time, the influence of the proxies on [O3] and [O(3P)] should be minimal. For a comprehensive analysis of different O3 and O(3P) proxies, we use a full model of electronic vibrational kinetics of excited products of O3 and O2 photolysis in the MLT of the Earth. Based on this model, we have tested five excited components; namely, O2(b1Σg+, v = 0, 1, 2), O2(a1Δg , v = 0) and O(1D) as the [O3] and [O(3P)] proxies in the MLT region. Using an analytical approach to sensitivity studies and uncertainty analysis, we have therefore developed the following methods of [O(3P)] and [O3] retrieval, which utilise electronic-vibrational transitions from the oxygen molecule second singlet level (O2(b1 Σg+, v = 0, 1, 2). We conclude that O2(b1 Σg+, v = 2) and O2(b1 Σg+, v = 0) are preferable proxies for [O(3P)] retrieval in the altitude range of 90-140 km, while O2(b1 Σg+, v = 1) is the best proxy for [O3] retrieval in the altitude range of 50-98 km.

  6. Observation of Atomic Emission Enhancement by fs-ns Dual-Pulse Laser-Induced Breakdown Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    YAN Li-Xin; ZHANG Yong-Sheng; ZHANG Li-Rong; LIU Jing-Ru; CHENG Jian-Ping; L(U) Min

    2006-01-01

    An experiment of a 500-fs KrF laser pulse incident upon a high density supersonic O2 gas jet synchronously with an ns frequency-doubled Nd:YAG laser pulse is performed in orthogonal configuration.Significant atomic emission enhancement of over forty-fold is observed with an optical multi-channel analyser.The enhancement effect is probably attributed to the different ionization mechanisms between fs and ns laser pulses.

  7. Projectile X-ray emission in relativistic ion-atom collisions

    Energy Technology Data Exchange (ETDEWEB)

    Salem, Shadi Mohammad Ibrahim

    2010-03-16

    This work reports on the study of the projectile X-ray emission in relativistic ion-atom collisions. Excitation of K-shell in He-like uranium ions, electron capture into H-like uranium ions and Simultaneous ionization and excitation of initially He-like uranium ions have been studied using the experimental storage ring at GSI. For the K{sub {alpha}}{sub 1} and K{sub {alpha}}{sub 2} transitions originating from the excitation of the He-like uranium ions, no alignment was observed. In contrast, the Ly{sub {alpha}}{sub 1} radiation from the simultaneous ionization-excitation process of the He-like uranium ions shows a clear alignment. The experimental value leads to the inclusion of a magnetic term in the interaction potential. The capture process of target electrons into the highly-charged heavy ions was studied using H-like uranium ions at an incident energy of 220 MeV/u, impinging on N{sub 2} gas-target. It was shown that, the strongly aligned electrons captured in 2p{sub 3/2} level couple with the available 1s{sub 1/2} electron which shows no initial directional preference. The magnetic sub-state population of the 2p{sub 3/2} electron is redistributed according to the coupling rules to the magnetic sub-states of the relevant two-electron states. This leads to the large anisotropy in the corresponding individual ground state transitions contributing to the K{sub {alpha}}{sub 1} emission. From the K{sub {alpha}}{sub 1}/K{sub {alpha}}{sub 2} ratio, the current results show that the incoherent addition of the E1 and M2 transition components yield to an almost isotropic emission of the total K{sub {alpha}}{sub 1}. In contrast to the radiative electron capture, the experimental results for the K-shell single excitation of He-like uranium ions indicate that only the {sup 1}P{sub 1} level contributes to the K{sub {alpha}}{sub 1} transition. For this case, the anisotropy parameter {beta}{sub 20} was found to be -0.20{+-}0.03. This work also reports on the study of a two

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-01-30

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

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

    DEFF Research Database (Denmark)

    Fiamegkos, I.; Cordeiro, F.; Robouch, P.;

    2016-01-01

    the release of all arsenic species into solution, and (ii) subsequent extraction of the inorganic arsenic present in the acid medium using chloroform followed by back-extraction to acidic medium. The final detection and quantification is done by flow injection hydride generation atomic absorption spectrometry......A collaborative trial was con