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Sample records for sampling electrothermal atomic

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-06-15

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

  2. Rare earth analysis in human biological samples by atomic absorption using electrothermal atomization

    International Nuclear Information System (INIS)

    Citron, I.M.; Holtzman, R.B.; Leiman, J.

    1982-01-01

    The determination of Sc and seven rare earth elements, Nd, Sm, Dy, Ho, Eu, Tm, and Yb, in biological samplesby atomic absorption spectrophotometric analysis (AAS) using electrothermal atomization in a pyrolytic graphite tube is shown to be rapid, precise and accurate. The technique utilizes the method of standard additions and linear regression analysis to determine results from peak area data. Inter-elemental interferences are negligible. The elements found sensitive enough for this type of analysis are, in order of decreasing sensitivity, Yb, Eu, Tm, Dy, Sc, Ho, Sm and Nd. The determination in these types of materials of Gd and elements less sensitive to AAS detection than Gd does not appear to be feasible. Results are presented on the concentrations of these elements in 41 samples from human subjects, cows and vegetables with normal environmental exposure to the rare earth elements. The composite percent mean deviation in peak-area readings for all samples and all elements examined was 4%. The mean standard error in the results among samples was about 6.5%

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

    International Nuclear Information System (INIS)

    Sardans, Jordi; Montes, Fernando; Penuelas, Josep

    2010-01-01

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

  4. 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

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

    Czech Academy of Sciences Publication Activity Database

    Vojtková, Blanka; Dočekal, Bohumil

    2005-01-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Science.gov (United States)

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

    2010-04-07

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

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    International Nuclear Information System (INIS)

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

    1993-01-01

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

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

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  11. Use of electrothermal atomization for determining metallic impurities in nuclearly pure uranium compounds

    International Nuclear Information System (INIS)

    Franco, M.B.

    1986-01-01

    Atomic absorption spectrometry with electrothermal atomization was used for the determination of Al, Cd, Cr, Fe, Mn, Mo and Ni as impurities in uranium oxide samples. The determinations were performed in solubilized samples both with and without uranium separation as well as in solid samples. (Author) [pt

  12. Use of electrothermal atomization for determining metallic impurities in nuclearly pure uranium compounds

    International Nuclear Information System (INIS)

    Franco, M.B.

    1985-01-01

    Atomic absorption spectrometry with electrothermal atomization was used for the determination of Al, Cd, Cr, Fe, Mn, Mo and Ni as impurities in uranium oxide samples. The determinations were performed in solubilized samples both with and without uranium separation as well as in solid samples. (Author) [pt

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  14. Discussion of parameters associated with the determination of arsenic by electrothermal atomic absorption spectrometry in slurried environmental samples.

    Science.gov (United States)

    Vassileva, E; Baeten, H; Hoenig, M

    2001-01-02

    A slurry sampling-fast program procedure has been developed for the determination of arsenic in plants, soils and sediments by electrothermal atomic absorption spectrometry. Efficiencies of various single and mixed modifiers for thermal stabilization of arsenic and for a better removal of the matrix during pyrolysis step were compared. The influence of the slurry concentration, amounts of modifier and parameters of the pyrolysis step on the As integrated absorbance signals have been studied and a comparison between fast and conventional furnace programs was also made. The ultrasonic agitation of the slurry followed by a fast electrothermal program using an Ir/Mg modifier provides the most consistent performance in terms of precision and accuracy. The reliability of the whole procedure has been compared with results obtained after application of a wet digestion method with an HF step and validated by analyzing eleven certified reference materials. Arsenic detection and quantitation limits expressed on dry sample matter were about 30 and 100 micrograms kg-1, respectively.

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    Science.gov (United States)

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

    1989-12-01

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  20. Study on the application of electrothermal atomization atomic absorption spectrometry for the determination of metallic Cu, Pb, Zn, Cd traces in sea water samples

    International Nuclear Information System (INIS)

    Nguyen Thi Kim Dung; Doan Thanh Son; Tran Thi Ngoc Diep

    2004-01-01

    The trace amount of some heavy metallic elements (Cu, Zn, Pb, Cd) in sea water samples were determined directly (without separation) and quantitatively by using Electro-Thermal Atomization Atomic Absorption Spectrometry (ETA-AAS). The effect of mainly major constituents such as Na, Mg, Ca, K, and the mutual effect of the trace elements, which were present in the matrix on the absorption intensity of each analyzed element was studied. The adding of a certain chemical modification for each trace element was also investigated in order to eliminate the overall effect of the background during the pyrolysis and atomization. The sea water sample after fitrating through a membrane with 0.45 μm-hole size was injected in to the graphite tube via an autosampler (MPE50). The absorption intensity of each element was then measured on the VARIO-6 under the optimum parameters for spectrometer such as: maximum wavelength, current of hollow cathode lamp, and that for graphite furnace such as dry temperature, pyrolysis temperature, atomization temperature, ect. The analytical procedures were set-up and applied for the determination of these above mentioned elements in the synthesized sea water sample and in the real sea water samples with high precision and accuracy. (author)

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

    Science.gov (United States)

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

    1996-09-15

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

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

    Science.gov (United States)

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

    2011-06-15

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

  3. The use of slurry sampling for the determination of manganese and copper in various samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Tokman, Nilgun

    2007-01-01

    Manganese and copper in multivitamin-mineral supplements and standard reference materials were determined by slurry sampling electrothermal atomic absorption spectrometry. Slurries were prepared in an aqueous solution containing Triton X-100. The effects of different parameters such as ratio of solid to liquid phase volume, total slurry volume and addition of Triton X-100 as a dispersant on the analytical results were investigated. The graphite furnace programs were optimized for slurry sampling depending on the analytes and their concentrations in the samples. The linear calibration method with aqueous standard solutions was used for the quantification. At optimum experimental conditions, R.S.D. values were below 5%. The analytes were determined in the limits of 95% confidence level with respect to certified values in coal and soil standard reference materials and to those found by wet-digestion in multivitamin-mineral supplements. Detection limits (3δ) for Mn and Cu were 0.10 μg L -1 and 1.82 μg L -1 for 10 μL coal standard reference material slurry, respectively

  4. Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples.

    Science.gov (United States)

    Taher, Mohammad Ali; Pourmohammad, Fatemeh; Fazelirad, Hamid

    2015-12-01

    In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra-trace amounts of rhodium after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015-0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

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

    2016-02-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    OpenAIRE

    NUKATSUKA, Isoshi; OHZEKI, Kunio

    2006-01-01

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

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

    International Nuclear Information System (INIS)

    Vilar Farinas, M.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.; Herrero Latorre, C.

    2007-01-01

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO 3 ) 2 and (NH 4 )H 2 PO 4 -Mg(NO 3 ) 2 ] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 μg L -1 ), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged -1

  9. 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.)

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-08-01

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

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

    Science.gov (United States)

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

    1994-12-01

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

  13. Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Nomura, Cassiana S.; Silva, Cintia S.; Nogueira, Ana R.A.; Oliveira, Pedro V.

    2005-01-01

    This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 deg. C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 deg. C and 2300 deg. C for Cu, and 700 deg. C and 1700 deg. C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 μg of W + 200 μg of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg - 1 and 128 mg kg - 1 , respectively. The relative standard deviations were lower than 6% (n = 5). The

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

    International Nuclear Information System (INIS)

    Andrada, Daniel; Pinto, Frederico G.; Magalhaes, Cristina Goncalves; Nunes, Berta R.; Silva, Jose Bento Borba da; Franco, Milton B.

    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 (ETAAS). 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 HNO 3 1% v/v and 0.02% v/v of cetyl trimethyl ammonium chloride (CTAC) were prepared directly in the autosampler cups and placed into the graphite furnace. For modifiers in solutions 10 μL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 μg), the best pyrolysis and atomization temperatures were 900 and 1600 deg C, respectively, with a characteristic mass of 12 pg (recommended of 10 pg), with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence) for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh) and between 93.9 and 105.2% (Zr+Rh). In both recovery studies, the relative standard deviation (n=3) was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r 2 higher than 0.99. The limits of detection were 0.7 μg L -1 for serum samples, with Zr+Rh permanent, and 1.0 μg L -1 for urine with iridium permanent. (author)

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

    Directory of Open Access Journals (Sweden)

    Andrada Daniel

    2006-01-01

    Full Text Available 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 cups and placed into the graphite furnace. For modifiers in solutions 10 µL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 µg, the best pyrolysis and atomization temperatures were 900 and 1600 ºC, respectively, with a characteristic mass of 12 pg (recommended of 10 pg, with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh and between 93.9 and 105.2% (Zr+Rh. In both recovery studies, the relative standard deviation (n=3 was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r² higher than 0.99. The limits of detection were 0.7 µg L-1 for serum samples, with Zr+Rh permanent, and 1.0 µg L-1 for urine with iridium permanent.

  16. 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

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

    Science.gov (United States)

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

    2016-05-01

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

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  20. Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Olmedo, P.; Pla, A.; Hernandez, A.F.; Lopez-Guarnido, O.; Rodrigo, L. [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain); Gil, F., E-mail: fgil@ugr.es [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain)

    2010-02-05

    For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

  1. Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Olmedo, P.; Pla, A.; Hernandez, A.F.; Lopez-Guarnido, O.; Rodrigo, L.; Gil, F.

    2010-01-01

    For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

  2. Determination of Cu, Cd, Pb and Cr in yogurt by slurry sampling electrothermal atomic absorption spectrometry: A case study for Brazilian yogurt.

    Science.gov (United States)

    de Andrade, Camila Kulek; de Brito, Patrícia Micaella Klack; Dos Anjos, Vanessa Egéa; Quináia, Sueli Pércio

    2018-02-01

    A slurry sampling electrothermal atomic absorption spectrometric method is proposed for the determination of trace elements such as Cu, Cr, Cd and Pb in yogurt. The main factors affecting the slurry preparation were optimized: nature and concentration of acid solution and sonication time. The analytical method was validated in-house by calibration, linearity, limits of detection and quantification, precision and accuracy test obtaining satisfactory results in all cases. The proposed method was applied for the determination of Cd, Cr, Cu and Pb in some Brazilian yogurt samples. For these samples, the concentrations ranged from 2.5±0.2 to 12.4±0.2ngg -1 ; 34±3 to 899±7ngg -1 ; <8.3 to 12±1ngg -1 ; and <35.4 to 210±16ngg -1 for Cd, Cu, Cr and Pb, respectively. The daily intake of Cd, Cu, Cr and Pb via consumption of these samples was estimated. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Preconcentration and determination of boron in milk, infant formula, and honey samples by solid phase extraction-electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, I.; Vinas, P.; Romero-Romero, R. [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, M. [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain)], E-mail: hcordoba@um.es

    2009-02-15

    This work presents alternative procedures for the electrothermal atomic absorption spectrometric determination of boron in milk, infant formulas, and honey samples. Honey samples (10% m/v) were diluted in a medium containing 1% v/v HNO{sub 3} and 50% v/v H{sub 2}O{sub 2} and introduced in the atomizer. A mixture of 20 {mu}g Pd and 0.5 {mu}g Mg was used for chemical modification. Calibration was carried out using aqueous solutions prepared in the same medium, in the presence of 10% m/v sucrose. The detection limit was 2 {mu}g g{sup -1}, equivalent to three times the standard error of the estimate (s{sub y/x}) of the regression line. For both infant formulas and milk samples, due to their very low boron content, we used a procedure based on preconcentration by solid phase extraction (Amberlite IRA 743), followed by elution with 2 mol L{sup -1} hydrochloric acid. Detection limits were 0.03 {mu}g g{sup -1} for 4% m/v honey, 0.04 {mu}g g{sup -1} for 5% m/v infant formula and 0.08 {mu}g mL{sup -1} for 15% v/v cow milk. We confirmed the accuracy of the procedure by comparing the obtained results with those found via a comparable independent procedure, as well by the analysis of four certified reference materials.

  4. Wet sample digestion for quantification of vanadium(V) in serum by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Heinemann, G.; Vogt, W.; Jacob, K.

    1999-01-01

    Three types of pressure digestion systems used prior to the determination of the ultratrace element vanadium by electrothermal atomic absorption spectrometry were evaluated: The high-pressure ashing (HPA) system, the DAB III pressure digestion system and the pressurized microwave digestion (PMD) system. Complete sample digestion and no loss of graphite tube sensitivity as well as reliable vanadium values could only be achieved with HPA digests of freeze-dried serum. The mean recovery rate was 98% and no loss of tube sensitivity could be observed. Using non-lyophilized serum the mean recovery rate was 70%. The DAB III digestion system, vicarious for closed pressure digestion in steel bombs with an allowable temperature up to about 200C, cannot be recommended to mineralize human biological material for vanadium determinations, because the remaining not completely decomposed organic compounds extracted together with the vanadium-cupferron complex caused a marked carbon-buildup and formation of carbides in the graphite tube were found to change the shape of the absorption signals distinctly, and to decline the tube sensitivity strongly (about 25%) so that reliable results cannot be achieved. The recovery rate was too low in general (about 50%). In addition, a subsequent treatment of the DAB III digests with perchloric acid was unsuccessful. The PMD system proved to be not suited, because the samples became highly contaminated by vanadium possibly from the titan seal. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  5. Monitoring and Method development of Hg in Istanbul Airborne Particulates by Solid Sampling Continuum Source-High Resolution Electrothermal Atomic Absorption Spectromerty

    Directory of Open Access Journals (Sweden)

    Soydemir E.

    2014-07-01

    Full Text Available In this work, a method has been developed and monitoring for the determination of mercury in PM2.5 airborne particulates by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry. The PM2.5 airborne particulates were collected on quartz filters using high volume samplers (500 L/min in Istanbul (Turkey for 96 hours every month in one year. At first, experimental conditions as well as the validation tests were optimized using collected filter. For this purpose, the effects of atomization temperature, amount of sample intoduced in to the furnace, addition of acids and/or KMnO4 on the sample, covering of graphite tube and platform or using of Ag nanoparticulates, Au nanoparticulates, and Pd solutions on the accuracy and precision were investigated. After optimization of the experimental conditions, the mercury concentrations were determined in the collected filter. The filters with PM2.5 airborne particulates were dried, divided into small fine particles and then Hg concentrations were determined directly. In order to eliminate any error due to the sensitivity difference between aqueous standards and solid samples, the quantification was performed using solid calibrants. The limit of detection, based on three times the standard deviations for ten atomizations of an unused filter, was 30 ng/g. The Hg content was dependent on the sampling site, season etc, ranging from samples, addition of AuNPs, AgNPs and Pd solution for amalgamation effects on the recoveries were investigated. The results were compared using statistical tests.

  6. Electrothermal atomic absorption spectrometry: contribution to the establishment of a rational method for the determination of trace elements in natural media

    International Nuclear Information System (INIS)

    Hoenig, Michel

    1990-01-01

    This research thesis aimed at extending, rationalising, simplifying and accelerating opportunities initially offered by electrothermal atomic absorption spectroscopy (ETAAS), more particularly in the marine, estuarine, rural or urban environment. Thus, this work mainly focused on the various aspects of this technique. The author first addresses the electrothermal atomisation process by presenting the atomiser, the platform, the sample insertion, ETAAS properties and use, the electrothermal program, and a comparison of ETAAS with other spectroscopic methods. She reports the study of spectral, ionisation and chemical perturbations, and of their correction. She introduces matrix and analyte modifiers, and presents refractory elements (effect of carbon surface, problems faced with molybdenum, barium, chromium and vanadium). She presents and discusses aspects related to sample preparation: problems related to trace dosing, methods of preparation of solutions, analyte concentration or separation, examples of applications to plants, to animal tissues, to geological materials, to soils and sediments, to atmospheric particles and matters in suspension in natural waters, and to blood and urine. She finally addresses the analysis of solid samples with a description of the apparatus and of the adopted methodology in the case of slurries [fr

  7. Laser-induced fluorescence of se, as, and sb in an electrothermal atomizer.

    Science.gov (United States)

    Swart, D J; Ezer, M; Pacquette, H L; Simeonsson, J B

    1998-04-01

    Trace detection of Se, As, and Sb atoms has been performed by electrothermal atomization laser-induced fluorescence (ETA-LIF) approaches. Production of far-UV radiation necessary for excitation of As atoms at 193.696 nm and Se atoms at 196.026 nm was accomplished by stimulated Raman shifting (SRS) of the output of a frequency-doubled dye laser operating near 230 nm. Both wavelengths were obtained as second-order anti-Stokes shifts of the dye laser radiation and provided up to 10 μJ/pulse, which was shown through power dependence studies to be sufficient for saturation in the ETA. An excited-state direct line fluorescence approach using excitation at 206.279 nm was also investigated for the LIF detection of Se. High-sensitivity LIF of Sb atoms was accomplished using 206.833-nm excitation and detection at 259.805 nm. The accuracy of the ETA-LIF approaches was demonstrated by determining the As and Se content of aqueous reference samples. The limits of detection (absolute mass) were 200 fg by ground-state LIF and 150 fg by excited-state direct line fluorescence for Se, 200 fg for As, and 10 fg for Sb; these LODs compare favorably with results reported previously in the literature for ETA-LIF, GFAAS, and ICP-MS methods.

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

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

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

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

    International Nuclear Information System (INIS)

    Konecna, Marie; Komarek, Josef

    2007-01-01

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

  10. 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...

  11. The determination, by atomic-absorption spectrophotometry using electrothermal atomization, of platinum, palladium, rhodium, ruthenium, and iridium

    International Nuclear Information System (INIS)

    Haines, J.; Robert, R.V.D.

    1982-01-01

    A method that involves measurement by atomic-absorption spectrophotometry using electrothermal atomization has been developed for the determination of trace quantities of platinum, palladium, rhodium, ruthenium, and iridium in mineralogical samples. The elements are separated and concentrated by fusion, nickel sulphide being used as the collector, and the analyte elements are measured in the resulting acid solution. An organic extraction procedure was found to offer no advantages over the proposed method. Mutual interferences between the five platinum-group metals examined, as well as interferences from gold, silver, and nickel were determined. The accuracy of the measurement was established by the analysis of a platinum-ore reference material. The lower limits of determination of each of the analyte elements in a sample material are as follows: platinum 1,6μg/l, palladium 0,2μg/1, rhodium 0,5μg/l, ruthenium 3μg/l, and iridium 2,5μg/l. The relative standard deviations range from 0,05 for rhodium to 0.08 for iridium. The method, which is described in detail in the Appendix, is applicable to the determination of these elements in ores, tailings, and geological materials in which the total concentration of the noble metals is less than 1g/t

  12. Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R.M.; Herrero Latorre, C., E-mail: carlos.herrero@usc.es

    2015-04-01

    A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3 ng L{sup −1}, respectively, and for Pb these limits were 0.13 and 0.43 μg L{sup −1}. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n = 10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. - Highlights: • Cd and Pb determination based on the combination of DSP, SS and ETAAS • Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes. • Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer.

  13. Application of Plackett-Burman and Doehlert designs for optimization of selenium analysis in plasma with electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    El Ati-Hellal, Myriam; Hellal, Fayçal; Hedhili, Abderrazek

    2014-10-01

    The aim of this study was the optimization of selenium determination in plasma samples with electrothermal atomic absorption spectrometry using experimental design methodology. 11 variables being able to influence selenium analysis in human blood plasma by electrothermal atomic absorption spectrometry (ETAAS) were evaluated with Plackett-Burman experimental design. These factors were selected from sample preparation, furnace program and chemical modification steps. Both absorbance and background signals were chosen as responses in the screening approach. Doehlert design was used for method optimization. Results showed that only ashing temperature has a statistically significant effect on the selected responses. Optimization with Doehlert design allowed the development of a reliable method for selenium analysis with ETAAS. Samples were diluted 1/10 with 0.05% (v/v) TritonX-100+2.5% (v/v) HNO3 solution. Optimized ashing and atomization temperatures for nickel modifier were 1070°C and 2270°C, respectively. A detection limit of 2.1μgL(-1) Se was obtained. Accuracy of the method was checked by the analysis of selenium in Seronorm™ Trace element quality control serum level 1. The developed procedure was applied for the analysis of total selenium in fifteen plasma samples with standard addition method. Concentrations ranged between 24.4 and 64.6μgL(-1), with a mean of 42.6±4.9μgL(-1). The use of experimental designs allowed the development of a cheap and accurate method for selenium analysis in plasma that could be applied routinely in clinical laboratories. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  14. 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...

  15. Hollow fiber based liquid-phase microextraction for the determination of mercury traces in water samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, Ignacio; Rivas, Ricardo E. [Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence ' Campus Mare Nostrum' , University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, Manuel, E-mail: hcordoba@um.es [Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence ' Campus Mare Nostrum' , University of Murcia, E-30071 Murcia (Spain)

    2012-09-19

    Highlight: Black-Right-Pointing-Pointer Hg (II) traces are preconcentrated by means of a three-phase liquid microextraction system. Black-Right-Pointing-Pointer PAN and ammonium iodide are used in the donor and acceptor phase, respectively. Black-Right-Pointing-Pointer Hollow-fiber pores are continuously fed with toluene placed in the lumen. Black-Right-Pointing-Pointer Mercuric ions can be measured in waters below the {mu}g L{sup -1} level. - Abstract: A three-phase liquid microextraction procedure for the determination of mercury at low concentrations is discussed. To the aqueous sample placed at pH 7 by means of a phosphate buffer, 0.002% (m/v) 1-(2-pyridylazo)-2-naphthol (PAN) is incorporated, and the mixture submitted to microextraction with a hollow-fiber impregnated with toluene and whose lumen contains a 0.05 mol L{sup -1} ammonium iodide solution. The final measurement of the extract is carried out by electrothermal atomic absorption spectrometry (300 Degree-Sign C and 1100 Degree-Sign C for the calcination and atomization temperatures, respectively). The pyrolytic graphite atomizer is coated electrolytically with palladium. An enrichment factor of 270, which results in a 0.06 {mu}g L{sup -1} mercury for the detection limit is obtained. The relative standard deviation at the 1 {mu}g L{sup -1} mercury level is 3.2% (n = 5). The reliability of the procedure is verified by analyzing waters as well as six certified reference materials.

  16. Monitoring content of cadmium, calcium, copper, iron, lead, magnesium and manganese in tea leaves by electrothermal and flame atomizer atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Prkić Ante

    2017-08-01

    Full Text Available Due to the simplicity of tea preparation (pouring hot water onto different dried herbs and its high popularity as a beverage, monitoring and developing a screening methodology for detecting the metal content is very important. The concentrations of Cd, Ca, Cu, Fe, Pb, Mg and Mn in 11 different samples of sage (Salvia officinalis L., linden (Tilia L. and chamomile (Matricaria chamomilla L. purchased at local herbal pharmacy were determined using electrothermal atomizer atomic absorption spectrometry (ETAAS and flame atomizer atomic absorption spectrometry (FAAS. The concentrations determined were: Cd (0.012 – 0.470 mg kg−1, Ca (5209 – 16340 mg kg−1, Cu (22.01 – 33.05 mg kg−1, Fe (114.2 – 440.3 mg kg−1, Pb (0.545 – 2.538 mg kg−1, Mg (2649 – 4325 mg kg−1 and Mn (34.00 – 189.6 mg kg−1. Principal Component Analysis (PCA was applied to identify factors (soil and climate influencing the content of the measured elements in herbal samples. The proposed methodology developed in this work was successfully applied to the detection of metals in herbal samples. The analysis showed that the content of toxic metals in herbal teas was below the maximum dose recommended by the World Health Organization (WHO.

  17. Monte Carlo simulation of electrothermal atomization on a desktop personal computer

    Science.gov (United States)

    Histen, Timothy E.; Güell, Oscar A.; Chavez, Iris A.; Holcombea, James A.

    1996-07-01

    Monte Carlo simulations have been applied to electrothermal atomization (ETA) using a tubular atomizer (e.g. graphite furnace) because of the complexity in the geometry, heating, molecular interactions, etc. The intense computational time needed to accurately model ETA often limited its effective implementation to the use of supercomputers. However, with the advent of more powerful desktop processors, this is no longer the case. A C-based program has been developed and can be used under Windows TM or DOS. With this program, basic parameters such as furnace dimensions, sample placement, furnace heating and kinetic parameters such as activation energies for desorption and adsorption can be varied to show the absorbance profile dependence on these parameters. Even data such as time-dependent spatial distribution of analyte inside the furnace can be collected. The DOS version also permits input of external temperaturetime data to permit comparison of simulated profiles with experimentally obtained absorbance data. The run-time versions are provided along with the source code. This article is an electronic publication in Spectrochimica Acta Electronica (SAE), the electronic section of Spectrochimica Acta Part B (SAB). The hardcopy text is accompanied by a diskette with a program (PC format), data files and text files.

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

    Science.gov (United States)

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

    2015-11-01

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

  19. An evaluation of inductively coupled plasma optical emission spectrometry using electrothermal atomisation sample introduction and photographic plate detection

    International Nuclear Information System (INIS)

    Khathing, D.T.; Pickford, C.J.

    1984-05-01

    A photographic radiation measurement approach has been used with an inductively coupled plasma source to evaluate and tabulate the more prominent optical emission lines of 66 elements. Compared with the more common sample introduction technique using nebulisation, increased sensitivity for multielement analysis of small samples was achieved by using a simple graphite electrothermal atomisation system. This was constructed to serve as a dual purpose atomiser ie both for Atomic Absorption and for Inductively Coupled Plasma Emission spectroscopy. The system offers the advantage of a wide multi-elemental coverage, but sensitivities achieved with photographic detection are poorer than those obtained photoelectrically. (author)

  20. Determination of total tin in geological materials by electrothermal atomic-absorption spectrophotometry using a tungsten-impregnated graphite furnace

    Science.gov (United States)

    Zhou, L.; Chao, T.T.; Meier, A.L.

    1984-01-01

    An electrothermal atomic-absorption spectrophotometric method is described for the determination of total tin in geological materials, with use of a tungsten-impregnated graphite furnace. The sample is decomposed by fusion with lithium metaborate and the melt is dissolved in 10% hydrochloric acid. Tin is then extracted into trioctylphosphine oxide-methyl isobutyl ketone prior to atomization. Impregnation of the furnace with a sodium tungstate solution increases the sensitivity of the determination and improves the precision of the results. The limits of determination are 0.5-20 ppm of tin in the sample. Higher tin values can be determined by dilution of the extract. Replicate analyses of eighteen geological reference samples with diverse matrices gave relative standard deviations ranging from 2.0 to 10.8% with an average of 4.6%. Average tin values for reference samples were in general agreement with, but more precise than, those reported by others. Apparent recoveries of tin added to various samples ranged from 95 to 111% with an average of 102%. ?? 1984.

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

    International Nuclear Information System (INIS)

    Blecker, Carlo R.; Hermann, Gerd M.

    2009-01-01

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

  2. Determination of metallic impurities in nuclearly pure uranium compounds by electrothermal spectrophotometry

    International Nuclear Information System (INIS)

    Franco, M.B.

    1986-01-01

    Atomic absorption spectrometry, with electrothermal atomization, has been used for the determination of Al, Cd, Cr, Fe, Mn and Ni in uranium oxide standards. The analysis were performed without sample dissolution and without uranium chemical separation. This technique is adequate for the qualification of nuclearly pure uranium, according to the standard specifications. (Author) [pt

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-04-15

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

  5. Chemical modifiers in electrothermal atomic absorption determination of Platinum and Palladium containing preparations in blood serum

    Directory of Open Access Journals (Sweden)

    Аntonina Alemasova

    2012-11-01

    Full Text Available The biological liquids matrixes influence on the characteristic masses and repeatability of Pt and Pd electrothermal atomic absorption spectroscopy (ETAAS determination was studied. The chemical modifiers dimethylglyoxime and ascorbic acid for matrix interferences elimination and ETAAS results repeatability improvement were proposed while bioliquids ETAAS analysis, and their action mechanism was discussed.

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

    Science.gov (United States)

    Swart, D J; Simeonsson, J B

    1999-11-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

    Katskov, Dmitri

    2015-01-01

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

  9. 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

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

    Science.gov (United States)

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

    2013-11-15

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

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

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

  12. Laser-induced fluorescence with an OPO system. Part II: direct determination of lead content in seawater by electrothermal atomization-laser-excited atomic fluorescence (ETA-LEAF).

    Science.gov (United States)

    Le Bihan, A; Lijour, Y; Giamarchi, P; Burel-Deschamps, L; Stephan, L

    2003-03-01

    Fluorescence was induced by coupling a laser with an optical parametric oscillator (OPO) to develop an analytical method for the direct determination of lead content, at ultra-trace level, in seawater by electrothermal atomization-laser-excited atomic fluorescence (ETA-LEAF). The optimization of atomization conditions, laser pulse energy, and mainly temporal parameters allowed us to reach a 3 fg detection limit (0.3 ng L(-1)) despite the low repetition rate of the device. The expected error on predicted concentrations of lead, at trace levels, in seawater was below 15%.

  13. Determination of cadmium in whole blood and scalp hair samples of Pakistani male lung cancer patients by electrothermal atomic absorption spectrometer

    International Nuclear Information System (INIS)

    Kazi, T.G.; Memon, A.R.; Afridi, H.I.; Jamali, M.K.; Arain, M.B.; Jalbani, N.; Sarfraz, R.A.

    2008-01-01

    A large number of epidemiologic studies have been undertaken to identify potential risk factors for cancer, amongst which the association with cadmium has received considerable attention. There is compelling evidence in support of positive associations between cadmium and risk of lung cancer. In present study we measured the concentration of Cd in whole blood and scalp hair samples of 120 male lung cancer patients (smokers) and 150 controls or referents (smokers and nonsmokers) from different cities of Pakistan. Both referents and patients were of same age group (ranged 40-70 years), socio-economic status, localities and dietary habits. The scalp hair and whole blood samples were oxidized by 65% nitric acid: 30% hydrogen peroxide (2:1) ratio in microwave oven. To check the validity of the proposed method, a conventional wet acid digestion method was used to obtain total Cd concentration in certified samples of human hair BCR 397 and Clincheck control-lyophilized human whole blood. All digests were analyzed for Cd concentration by electrothermal atomic absorption spectrometer (ETAAS). The results of this study showed that the average Cd concentration was higher in the blood and scalp hair of lung cancer patients at different stages as compared to controls (p < 001). The smoker referents have high level of Cd in both biological samples as compared to nonsmoker subjects. These results illustrate that the patients who continued smoking after confirmed diagnosis of lung cancer have 34.2-67.26 and 22.4-57.3% more Cd in blood samples and scalp hair than lung cancer patients who cease smoking. This study is compelling evidence in support of positive associations between cadmium, cigarette smoking and lung cancer risk

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

    Science.gov (United States)

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

    2017-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Cvetkovic, J. [Inst. of Agriculture, Skopje (Yugoslavia); Stafilov, T. [Inst. of Chemistry, Faculty of Science Sts. Cyril and Methodius Univ., Skopje (Yugoslavia); Mihajlovic, D. [RZ Tehnicka Kontrola, Skopje (Yugoslavia)

    2001-08-01

    A mixed matrix modifier of nickel and strontium nitrates was used as a chemical modifier for the determination of selenium in wines by Zeeman electrothermal atomic absorption spectrometry. Wine samples were heated on a boiling water bath with small amounts of nitric acid and hydrogen peroxide. For complete elimination of interference, especially from sulfates and phosphates, selenium is complexed with ammonium pyrolidinedithiocarbamate (APDTC), extracted into methyl isobutyl ketone (MIBK), and measured by ETAAS. The graphite furnace temperature program was optimized for both aqueous and organic solutions. Pyrolysis temperatures of 1300 C and 800 C were chosen for aqueous and organic solutions, respectively; 2700 C and 2100 C were used as optimum atomization temperatures for aqueous and organic solutions, respectively. The optimum modifier mass established is markedly lower than those presented in the literature. The platform atomization ensures pretreatment stabilization up to 1100 C and 1600 C, respectively, for organic and aqueous selenium solutions. The procedure was verified by the method of standard addition. The investigated wine samples originated from the different regions of the Republic of Macedonia. The selenium concentration varied from not detectable to 0.93 {mu}g L{sup -1}. (orig.)

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  17. Determination of arsenic in petroleum refinery streams by electrothermal atomic absorption spectrometry after multivariate optimization based on Doehlert design

    Science.gov (United States)

    Cassella, Ricardo J.; de Sant'Ana, Otoniel D.; Santelli, Ricardo E.

    2002-12-01

    This paper reports the development of a methodology for the determination of arsenic in petroleum refinery aqueous streams containing large amounts of unknown volatile organic compounds, employing electrothermal atomic absorption spectrometry with polarized Zeeman-effect background correction. In order to make the procedure applicable, the influence of chemical modification and the drying step was examined. Also, pyrolysis and atomization temperatures and the amount of nitric acid added to the sample were optimized using a multivariate approach based on Doehlert matrix. Obtained results indicate that, in this kind of sample, arsenic must be determined by standard addition procedure with a careful control of the drying step temperature and ramp pattern. In order to evaluate the accuracy of the procedure, a test was performed in six spiked samples of petroleum refinery aqueous streams and the relative errors verified in the analysis of such samples (added As between 12.5 and 190 μg l -1) ranged from -7.2 to +16.7%. The detection limit and the relative standard deviation were also calculated and the values are 68 pg and 7.5% (at 12.5 μg l -1 level), respectively.

  18. Determination of arsenic in petroleum refinery streams by electrothermal atomic absorption spectrometry after multivariate optimization based on Doehlert design

    International Nuclear Information System (INIS)

    Cassella, Ricardo J.; Sant'Ana, Otoniel D. de; Santelli, Ricardo E.

    2002-01-01

    This paper reports the development of a methodology for the determination of arsenic in petroleum refinery aqueous streams containing large amounts of unknown volatile organic compounds, employing electrothermal atomic absorption spectrometry with polarized Zeeman-effect background correction. In order to make the procedure applicable, the influence of chemical modification and the drying step was examined. Also, pyrolysis and atomization temperatures and the amount of nitric acid added to the sample were optimized using a multivariate approach based on Doehlert matrix. Obtained results indicate that, in this kind of sample, arsenic must be determined by standard addition procedure with a careful control of the drying step temperature and ramp pattern. In order to evaluate the accuracy of the procedure, a test was performed in six spiked samples of petroleum refinery aqueous streams and the relative errors verified in the analysis of such samples (added As between 12.5 and 190 μg l -1 ) ranged from -7.2 to +16.7%. The detection limit and the relative standard deviation were also calculated and the values are 68 pg and 7.5% (at 12.5 μg l -1 level), respectively

  19. Determinação de As em amostras orgânicas de interesse ambiental por espectrometria de absorção atômica com atomização eletrotérmica após combustão em bomba de O2 Determination of As in environmental organic samples by atomic absorption spectrometry with electrothermal atomization after O2 bomb combustion

    Directory of Open Access Journals (Sweden)

    Vera Maria da Costa Dias

    2003-10-01

    Full Text Available The toxicity of the major As species present in the environment justifies the effort for quantifying the element in environmental organic samples, which can vary from animal and vegetal tissues to coal and industrial residues. This paper comments about the applicability of the O2 bomb digestion, as a general procedure for all environmental organic materials. A rapid and straightforward method is suggested, which consists in burning the sample in the bomb at high O2 pressure, dissolving the vapours in diluted HNO3 and determining As in the resulting solution by atomic absorption spectrometry with electrothermal atomization. The method was applied to certified materials and plant samples.

  20. Ultratrace determination of Pb, Se and As in wine samples by electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-10-12

    The determination of Pb, Se and As in wine has a great interest due to health risks and legal requirements. To perform the analysis of wine, two considerations must be taken into account: (i) the low concentration level of the analytes; and (ii) the risk of interferences due to wine matrix components. The goal of this work is to evaluate electrothermal vaporization (ETV) sample introduction for ultratrace determination of Pb, Se and As in wine samples by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained with ETV-ICP-MS were compared to those obtained with conventional liquid sample introduction in ICP-MS and electrothermal atomic absorption spectrometry (ETAAS). Analytical figures of merit of ETV sample introduction strongly depend on the amount of wine sample, on the modifier nature (i.e. Pd, ascorbic acid or citric acid) and concentration and on the temperature program. Wine matrix components exert a great influence on analyte transport efficiency. Due to this fact, the analysis of wine cannot be performed by means of external calibration but the standard addition methodology should be used. The determination of Pb and Se in wine by ETV-ICP-MS provides similar results as conventional liquid sample introduction ICP-MS. For As, the concentration values obtained with ETV sample introduction were between two and four times lower than with the conventional system. These differences are related to the lower intensity of polyatomic interferences (i.e. {sup 40}Ar{sup 35}Cl{sup +} vs. {sup 75}As{sup +}) obtained for ETV sample introduction when compared to the conventional system. Finally, no differences for Pb determination were observed between ETV sample introduction and ETAAS. Unfortunately, the limits of detection for As and Se in ETAAS were not low enough to quantify these elements in the wine samples tested.

  1. Ultratrace determination of Pb, Se and As in wine samples by electrothermal vaporization inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

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

    2009-01-01

    The determination of Pb, Se and As in wine has a great interest due to health risks and legal requirements. To perform the analysis of wine, two considerations must be taken into account: (i) the low concentration level of the analytes; and (ii) the risk of interferences due to wine matrix components. The goal of this work is to evaluate electrothermal vaporization (ETV) sample introduction for ultratrace determination of Pb, Se and As in wine samples by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained with ETV-ICP-MS were compared to those obtained with conventional liquid sample introduction in ICP-MS and electrothermal atomic absorption spectrometry (ETAAS). Analytical figures of merit of ETV sample introduction strongly depend on the amount of wine sample, on the modifier nature (i.e. Pd, ascorbic acid or citric acid) and concentration and on the temperature program. Wine matrix components exert a great influence on analyte transport efficiency. Due to this fact, the analysis of wine cannot be performed by means of external calibration but the standard addition methodology should be used. The determination of Pb and Se in wine by ETV-ICP-MS provides similar results as conventional liquid sample introduction ICP-MS. For As, the concentration values obtained with ETV sample introduction were between two and four times lower than with the conventional system. These differences are related to the lower intensity of polyatomic interferences (i.e. 40 Ar 35 Cl + vs. 75 As + ) obtained for ETV sample introduction when compared to the conventional system. Finally, no differences for Pb determination were observed between ETV sample introduction and ETAAS. Unfortunately, the limits of detection for As and Se in ETAAS were not low enough to quantify these elements in the wine samples tested.

  2. Determination of lead and cadmium in hen eggs by graphite france electrothermal atomic absorption spectrometry and estimation of the daily intake

    International Nuclear Information System (INIS)

    Siddiqui, I.; Nizami, S.S.

    2012-01-01

    A total of 54 hen eggs were procured from nine poultry farms of Sindh, Pakistan in different batches to determine lead and cadmium toxicity. The quantitative analysis of lead (Pb) and cadmium (Cd) in egg samples were performed on electrothermal atomic absorption spectrometer (ETAAS), with Zeeman effects background correction. Lead concentrations in hen egg samples ranged from 0.027 to 1.056 micro g/g with a mean value of 0.283 micro g/g +- 0.86, whereas cadmium concentrations ranged from 0.001 to 0.012 micro g/g with a mean value of 0.003 micro g/g +-0.002. Lead concentrations exceeded the normal levels of 0.020 but cadmium was found lower than the normal levels of 0.005 micro g/g. (author)

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  4. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

  5. Green method for ultrasensitive determination of Hg in natural waters by electrothermal-atomic absorption spectrometry following sono-induced cold vapor generation and 'in-atomizer trapping'

    International Nuclear Information System (INIS)

    Gil, Sandra; Lavilla, Isela; Bendicho, Carlos

    2007-01-01

    Sono-induced cold vapor generation (SI-CVG) has been used for the first time in combination with a graphite furnace atomizer for determination of Hg in natural waters by electrothermal-atomic absorption spectrometry after in situ trapping onto a noble metal-pretreated platform (Pd, Pt or Rh) inserted into a graphite tube. The system allows 'in-atomizer trapping' of Hg without the use of conventional reduction reactions based on sodium borohydride or tin chloride in acid medium for cold vapor generation. The sono-induced reaction is accomplished by applying ultrasound irradiation to the sample solution containing Hg(II) in the presence of an organic compound such as formic acid. As this organic acid is partly degraded upon ultrasound irradiation to yield CO, CO 2 , H 2 and H 2 O, the amount of lab wastes is minimized and a green methodology is achieved. For this purpose, experimental variables influencing the generation/trapping process are fully investigated. The limit of detection for a 10 min trapping time and 10 mL sample volume was 0.03 μg L -1 (Integrated absorbance) and the repeatability expressed as relative standard deviation was about 3%. Carbonates and chlorides at 100 mg L -1 level caused a signal depression by 20-30%. The enhanced trapping efficiency observed with the sono-induced cold vapor generation as compared with 'in-atomizer trapping' methods employing chemical vapor generation is discussed. A reaction pathway for SI-CVG is proposed on the basis of the current knowledge for synthesis of noble metal nanoparticles by ultrasound

  6. Dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous separation/preconcentration of nickel, cobalt and copper prior to determination by electrothermal atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mooud Amirkavei

    2013-01-01

    Full Text Available A dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous extraction of trace amounts of nickel, cobalt and copper followed by their determination with electrothermal atomic absorption spectrometry was developed. 300 µL of acetone and 1-undecanol was injected into an aqueous sample containing diethyldithiocarbamate complexes of metal ions. For a sample volume of 10 mL, enrichment factors of 277, 270 and 300 and detection limits of 1.2, 1.1 and 1 ng L-1 for nickel, cobalt and copper were obtained, respectively. The method was applied to the extraction and determination of these metals in different water samples.

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

    Science.gov (United States)

    Panyabut, Teerawat; Sirirat, Natnicha; Siripinyanond, Atitaya

    2018-02-13

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

  8. Synthesis and application of a nanoporous ion-imprinted polymer for the separation and preconcentration of trace amounts of vanadium from food samples before determination by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Dehghanpoor Frashah, Shahab

    2016-04-01

    A vanadium ion-imprinted polymer was synthesized in the presence of V(V) and N-benzoyl-N-phenyl hydroxyl amine using 4-vinyl pyridine as the monomer, ethylene glycol dimethacrylate as the cross linker and 2,2'-azobis(isobutyronitrile) as the initiator. The imprinted V(V) ions were completely removed by leaching the polymer with 5 mol/L nitric acid, and the polymer structure was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The ion-imprinted polymer was used as the sorbent in the development of the solid-phase extraction method for V(V) prior to its determination by electrothermal atomic absorption spectrometry. The maximum sorption capacity for V(V) ions was 26.7 mg/g at pH 4.0. Under the optimum conditions, for a sample volume of 150.0 mL, an enrichment factor of 289.0 and a detection limit of 6.4 ng/L were obtained. The developed method was successfully applied to the determination of vanadium in parsley, zucchini, black tea, rice, and water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Selenium analysis by an integrated microwave digestion-needle trap device with hydride sorption on carbon nanotubes and electrothermal atomic absorption spectrometry determination

    Science.gov (United States)

    Maratta Martínez, Ariel; Vázquez, Sandra; Lara, Rodolfo; Martínez, Luis Dante; Pacheco, Pablo

    2018-02-01

    An integrated microwave assisted digestion (MW-AD) - needle trap device (NTD) for selenium determination in grape pomace samples is presented. The NTD was filled with oxidized multiwall carbon nanotubes (oxMWCNTS) where Se hydrides were preconcentrated. Determination was carried out by flow injection-electrothermal atomic absorption spectrometry (FI-ETAAS). The variables affecting the system were established by a multivariate design (Plackett Burman), indicating that the following variables significantly affect the system: sample amount, HNO3 digestion solution concentration, NaBH4 volume and elution volume. A Box-Behnken design was implemented to determine the optimized values of these variables. The system improved Se atomization in the graphite furnace, since only trapped hydrides reached the graphite furnace, and the pyrolysis stage was eliminated according to the aqueous matrix of the eluate. Under optimized conditions the system reached a limit of quantification of 0.11 μg kg- 1, a detection limit of 0.032 μg kg- 1, a relative standard deviation of 4% and a preconcentration factor (PF) of 100, reaching a throughput sample of 5 samples per hour. Sample analysis show Se concentrations between 0.34 ± 0.03 μg kg- 1 to 0.48 ± 0.03 μg kg- 1 in grape pomace. This system provides minimal reagents and sample consumption, eliminates discontinuous stages between samples processing reaching a simpler and faster Se analysis.

  10. Preconcentration of lead using solidification of floating organic drop and its determination by electrothermal atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mahmoud Chamsaz

    2013-07-01

    Full Text Available A simple microextraction method based on solidification of a floating organic drop (SFOD was developed for preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry (ETAAS. Ammonium pyrolidinedithiocarbamate (APDC was used as complexing agent, and the formed complex was extracted into a 20 μL of 1-undecanol. The extracted complex was diluted with ethanol and injected into a graphite furnace. An orthogonal array design (OAD with OA16 (45 matrix was employed to study the effects of different parameters such as pH, APDC concentration, stirring rate, sample solution temperature and the exposure time on the extraction efficiency. Under the optimized experimental conditions the limit of detection (based on 3 s and the enhancement factor were 0.058 μg L−1 and 113, respectively. The relative standard deviation (RSD for 8 replicate determinations of 1 μg L−1 of Pb was 8.8%. The developed method was validated by the analysis of certified reference materials and was successfully applied to the determination of lead in water and infant formula base powder samples.

  11. Species selective preconcentration and quantification of gold nanoparticles using cloud point extraction and electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Hartmann, Georg; Schuster, Michael

    2013-01-25

    The determination of metallic nanoparticles in environmental samples requires sample pretreatment that ideally combines pre-concentration and species selectivity. With cloud point extraction (CPE) using the surfactant Triton X-114 we present a simple and cost effective separation technique that meets both criteria. Effective separation of ionic gold species and Au nanoparticles (Au-NPs) is achieved by using sodium thiosulphate as a complexing agent. The extraction efficiency for Au-NP ranged from 1.01 ± 0.06 (particle size 2 nm) to 0.52 ± 0.16 (particle size 150 nm). An enrichment factor of 80 and a low limit of detection of 5 ng L(-1) is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L(-1). The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L(-1) is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry for a sensitive determination of cadmium in water samples

    International Nuclear Information System (INIS)

    Li Shengqing; Cai Shun; Hu Wei; Chen Hao; Liu Hanlan

    2009-01-01

    A new method was developed for the determination of cadmium in water samples using ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (IL-based USA-DLLME) followed by electrothermal atomic absorption spectrometry (ETAAS). The IL-based USA-DLLME procedure is free of volatile organic solvents, and there is no need for a dispersive solvent, in contrast to conventional DLLME. The ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate (HMIMPF 6 ), was quickly disrupted by an ultrasonic probe for 1 min and dispersed in water samples like a cloud. At this stage, a hydrophobic cadmium-DDTC complex was formed and extracted into the fine droplets of HMIMPF 6 . After centrifugation, the concentration of the enriched cadmium in the sedimented phase was determined by ETAAS. Some effective parameters of the complex formation and microextraction, such as the concentration of the chelating agent, the pH, the volume of the extraction solvent, the extraction time, and the salt effect, have been optimized. Under optimal conditions, a high extraction efficiency and selectivity were reached for the extraction of 1.0 ng of cadmium in 10.0 mL of water solution employing 73 μL of HMIMPF 6 as the extraction solvent. The enrichment factor of the method is 67. The detection limit was 7.4 ng L - 1 , and the characteristic mass (m 0 , 0.0044 absorbance) of the proposed method was 0.02 pg for cadmium (Cd). The relative standard deviation (RSD) for 11 replicates of 50 ng L - 1 Cd was 3.3%. The method was applied to the analysis of tap, well, river, and lake water samples and the Environmental Water Reference Material GSBZ 50009-88 (200921). The recoveries of spiked samples were in the range of 87.2-106%.

  13. Liquid-phase microextraction with solidification of the organic floating drop for the preconcentration and determination of mercury traces by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, I.; Rivas, R.E.; Hernandez-Cordoba, M. [Faculty of Chemistry, University of Murcia, Department of Analytical Chemistry, Murcia (Spain)

    2010-04-15

    A procedure for the determination of traces of mercury by liquid-phase microextraction based on solidification of a floating organic droplet for separation and electrothermal atomic absorption spectrometry for final measurement has been developed. For this purpose, 50 {mu}L of pre-heated (50 C) undecanoic acid (UA), are added to 25 mL of aqueous sample solution at pH 5. The mixture, maintained at 50 C, is stirred for 10 min using a high stirring rate in order to fragment the UA drop into droplets, thus favoring the extraction process. Next, the vial is immersed in an ice bath, which results in the solidification of the UA drop that is easily separated. Injection into the atomizer is carried out after gentle heating. The pyrolytic atomizers are coated with electrolytically reduced palladium that acts as an effective chemical modifier for more than 500 firings. Under the optimized conditions, the detection limit was 70 ng L{sup -1} mercury with an enrichment factor of 430. The relative standard deviation of the measurements was in the 2.1-3.5% range. Recovery studies applied to the determination of mercuric ions in bottled and tap water samples were in the 92-104% range. (orig.)

  14. Use of cetyltrimethylammonium bromide as surfactant for the determination of copper and chromium in gasoline emulsions by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Santos, Denilson S.S. dos; Teixeira, Alete P.; Barbosa, Jose T.P.; Ferreira, Sergio L.C.; Korn, Maria das Gracas A; Teixeira, Leonardo S.G.

    2007-01-01

    In this work, the use of cetyltrimethylammonium bromide as surfactant for the preparation of oil-in-water emulsions for the determination of Cu and Cr in gasoline by electrothermal atomic absorption spectrometry (ET AAS) was evaluated. The surfactant amount was tested in the range of 25 to 300 mg, added to 2 ml of gasoline, and completed to 10 mL with 0.1% (v/v) nitric acid solution. 150 mg of surfactant was found optimum, and a sonication time of 10 min sufficient to form an oil-in-water emulsion that was stable for several hours. The ET AAS temperature program was established based on pyrolysis and atomization curves. The pyrolysis temperatures were set at 700 and 1300 deg. C for Cu and Cr, respectively and the selected atomization temperatures were 2400 and 2500 deg. C. The time and temperature of the drying stage and the atomization time were experimentally tested to provide optimum conditions. The limits of detection were found to be 5 μg L -1 and 1.5 μg L -1 for Cu and Cr, respectively in the original gasoline samples. The relative standard deviation (RSD) ranged from 4 to 9% in oil-in-water emulsions spiked with 5 μg L -1 and 15 μg L -1 of each metal, respectively. Recoveries varied from 90 to 98%. The accuracy of the proposed method was tested by an alternate procedure using complete evaporation of the gasoline sample. The method was adequate for the determination of Cu and Cr in gasoline samples collected from different gas stations in Salvador, BA, Brazil

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

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

    International Nuclear Information System (INIS)

    Acar, O.

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Acar, O.

    2012-07-01

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

  18. Slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for steelmaking flue dust analysis

    Science.gov (United States)

    Coedo, A. G.; Dorado, T.; Padilla, I.; Maibusch, R.; Kuss, H.-M.

    2000-02-01

    A commercial atomic absorption graphite furnace (AAGF), with a self-made adapter and valve system, was used as a slurry sampling cell for electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). The system was applied to the determination of As, Sn, Sb, Se, Te, Bi, Cd, V, Ti and Mo in steelmaking flue dusts. Experimental conditions with respect to ETV and ICP-MS operating parameters were optimized. Compared to aqueous solutions, slurry samples were found to present better analyte transport. Microgram amounts of Rh were used to reduce the difference in analyte response in sensitivity for aqueous solutions of the tested analytes. No such increasing effect was observed for slurry samples and aqueous standards. An added quantity of Rh acting as modifier/carrier resulted in an increase for the same analytes in matrix-slurry solutions, even the addition of an extra Rh quantity has resulted in a decrease in the signals. The effect of Triton X-100 (used as a dispersant agent) on analyte intensity and precision was also studied. External calibration from aqueous standards spiked with 100 μg ml -1 Rh was performed to quantified 0.010 g/100 ml slurry samples. Results are presented for a certified reference electrical arc furnace flue dust (EAF): CRM-876-1 (Bureau of Analysis Samples Ltd., Cleveland, UK), a reference sample of coke ashes X-3705 (from AG der Dillinger Hüttenwerke, Germany), and a representative sample of EAF flue dust from a Spanish steelmaking company (CENIM-1). For the two reference materials an acceptable agreement with certificate values was achieved, and the results for the CENIM sample matched with those obtained from conventional nebulization solution.

  19. 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).

  20. Interfase y software de control para operar en sincronismo un automuestreador y un atomizador electrotérmico por filamento de tungsteno en espectrofotometría de absorción atómica Development of interface and software for synchronous operation of an autosampler and a tungsten coil electrothermal atomizer coupled to an atomic absorption spectophotometer

    Directory of Open Access Journals (Sweden)

    J. Neira

    1998-07-01

    Full Text Available The interface and software for synchronous control of an autosampler and an electrothermal tungsten coil atomizer in atomic absorption spectrophotometry were developed. The control of the power supply, the trigger of the Read function of the spectrophotometer and the automatic operation of the autosampler was performed by software written in "TurboBasic". The system was evaluated by comparison of the repeatability of peak-height absorbances obtained in the atomization of lead by consecutive 10-µl injections of solutions (prepared in 0.2% v/v HNO3 using autosampler and manual sample introduction, and also by long term operation.

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

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    A sequential injection (SI) on-line matrix removal and trace metal preconcentration procedure by using a novel microcolumn packed with PTFE beads is described, and demonstrated for trace cadmium analysis with detection by electrothermal atomic absorption spectrometry (ETAAS). The analyte...

  2. Direct determination of trace rare earth elements in ancient porcelain samples with slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Xiang Guoqiang; Jiang Zucheng; He Man; Hu Bin

    2005-01-01

    A method for the direct determination of trace rare earth elements in ancient porcelain samples by slurry sampling fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry was developed with the use of polytetrafluoroethylene as fluorinating reagent. It was found that Si, as a main matrix element in ancient porcelain sample, could be mostly removed at the ashing temperature of 1200 deg. C without considerable losses of the analytes. However, the chemical composition of ancient porcelain sample is very complicated, which makes the influences resulting from other matrix elements not be ignored. Therefore, the matrix effect of ancient porcelain sample was also investigated, and it was found that the matrix effect is obvious when the matrix concentration was larger than 0.8 g l -1 . The study results of particle size effect indicated that when the sample particle size was less than 0.057 mm, the particle size effect is negligible. Under the optimized operation conditions, the detection limits for rare earth elements by fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry were 0.7 ng g -1 (Eu)-33.3 ng g -1 (Nd) with the precisions of 4.1% (Yb)-10% (La) (c = 1 μg l -1 , n = 9). The proposed method was used to directly determine the trace rare earth elements in ancient porcelain samples produced in different dynasty (Sui, Ming and Qing), and the analytical results are satisfactory

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  4. Toxic metals distribution in different components of Pakistani and imported cigarettes by electrothermal atomic absorption spectrometer

    International Nuclear Information System (INIS)

    Kazi, T.G.; Jalbani, N.; Arain, M.B.; Jamali, M.K.; Afridi, H.I.; Sarfraz, R.A.; Shah, A.Q.

    2009-01-01

    It was extensively investigated that a significant flux of toxic metals, along with other toxins, reaches the lungs through smoking. In present study toxic metals (TMs) (Al, Cd, Ni and Pb) were determined in different components of Pakistani local branded and imported cigarettes, including filler tobacco (FT), filter (before and after normal smoking by a single volunteer) and ash by electrothermal atomic absorption spectrometer (ETAAS). Microwave-assisted digestion method was employed. The validity and accuracy of methodology were checked by using certified sample of Virginia tobacco leaves (ICHTJ-cta-VTL-2). The percentages (%) of TMs in different components of cigarette were calculated with respect to their total contents in FT of all branded cigarettes before smoking, while smoke concentration has been calculated by subtracting the filter and ash contents from the filler tobacco content of each branded cigarette. The highest percentage (%) of Al was observed in ash of all cigarettes, with range 97.3-99.0%, while in the case of Cd, a reverse behaviour was observed, as a range of 15.0-31.3% of total contents were left in the ash of all branded cigarettes understudy

  5. 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)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-11-15

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

  7. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L{sup −1} and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L{sup −1} of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic.

  8. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-01-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L −1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L −1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic

  9. Spectral and non-spectral interferences in the determination of thallium in environmental materials using electrothermal atomization and vaporization techniques--a case study

    International Nuclear Information System (INIS)

    Vale, Maria Goreti R.; Welz, Bernhard

    2002-01-01

    The literature on the determination of Tl in environmental samples using electrothermal atomization (ETA) and vaporization (ETV) techniques has been reviewed with special attention devoted to potential interferences and their control. Chloride interference, which is due to the formation of the volatile monochloride in the condensed phase, is the most frequently observed problem. Due to its high dissociation energy (88 kcal/mol), TlCl is difficult to dissociate in the gas phase and is easily lost. The best means of controlling this interference in ETA is atomization under isothermal conditions according to the stabilized temperature platform furnace concept, and the use of reduced palladium as a modifier. An alternative approach appears to be the 'fast furnace' concept, wherein both the use of a modifier and the pyrolysis stage are omitted. This concept requires an efficient background correction system, and high-resolution continuum-source atomic absorption spectrometry (HR-CS AAS) appears to offer the best results. This chloride interference can also cause significant problems when ETV techniques are used. Among the spectral interferences found in the determination of thallium are those due to Pd, the most efficient modifier, and Fe, which is frequently found at high concentrations in environmental samples. Both interferences are due to nearby atomic lines, and are observed only when deuterium background correction and relatively high atomization temperatures are used. A more serious spectral interference is that due to the molecular absorption spectrum of SO 2 , which has a maximum around the Tl line and exhibits a pronounced rotational fine structure. HR-CS AAS again showed the best performance in coping with this interference

  10. Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Pena, Francisco; Lavilla, Isela; Bendicho, Carlos

    2008-01-01

    Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

  11. Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pena, Francisco; Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain)], E-mail: bendicho@uvigo.es

    2008-04-15

    Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 {mu}g/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters.

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

    Science.gov (United States)

    Horlick, Gary

    1984-01-01

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

  13. Determination of sub-microgram amounts of selenium in geological materials by atomic-absorption spectrophotometry with electrothermal atomisation after solvent extraction

    Science.gov (United States)

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

    1981-01-01

    An atomic-absorption spectrophotometric method with electrothermal atomisation has been developed for the determination of selenium in geological materials. The sample is decomposed with a mixture of nitric, perchloric and hydrofluoric acids and heated with hydrochloric acid to reduce selenium to selenium (IV). Selenium is then extracted into toluene from a hydrochloric acid - hydrobromic acid medium containing iron. A few microlitres of the toluene extract are injected into a carbon rod atomiser, using a nickel solution as a matrix modifier. The limits of determination are 0.2-200 p.p.m. of selenium in a geological sample. For concentrations between 0.05 and 0.2 p.p.m., back-extraction of the selenium into dilute hydrochloric acid is employed before atomisation. Selenium values for reference samples obtained by replicate analysis are in general agreement with those reported by other workers, with relative standard deviations ranging from 4.1 to 8.8%. Recoveries of selenium spiked at two levels were 98-108%. Major and trace elements commonly encountered in geological materials do not interfere. Arsenic has a suppressing effect on the selenium signals, but only when its concentration is greater than 1000 p.p.m. Nitric acid interferes seriously with the extraction of selenium and must be removed by evaporation in the sample-digestion step.

  14. Selective and sensitive speciation analysis of Cr(VI) and Cr(III), at sub-μgL-1 levels in water samples by electrothermal atomic absorption spectrometry after electromembrane extraction.

    Science.gov (United States)

    Tahmasebi, Zeinab; Davarani, Saied Saeed Hosseiny

    2016-12-01

    In this work, electromembrane extraction in combination with electrothermal atomic absorption spectrometry (ET-AAS) was investigated for speciation, preconcentration and quantification of Cr(VI) and Cr(III) in water samples through the selective complexation of Cr(VI) with 1,5-diphenylcarbazide (DPC) as a complexing agent. DPC reduces Cr(VI) to Cr(III) ions and then Cr(III) species are extracted based on electrokinetic migration of their cationic complex (Cr(III)-DPC) toward the negative electrode placed in the hollow fiber. Also, once oxidized to Cr(VI), Cr(III) ions in initial sample were determined by this procedure. The influence of extraction parameters such as pH, type of organic solvent, chelating agent concentration, stirring rate, extraction time and applied voltage were evaluated following a one-at-a-time optimization approach. Under optimized conditions, the extracted analyte was quantified by ETAAS, with an acceptable linearity in the range of 0.05-5ngmL -1 (R 2 value=0.996), and a repeatability (%RSD) between 3.7% and 12.2% (n=4) for 5.0 and 1.0ngmL -1 of Cr(VI), respectively. Also, we obtained an enrichment factor of 110 that corresponded to the recovery of 66%. The detection limit (S/N ratio of 3:1) was 0.02ngmL -1 . Finally, this new method was successfully employed to determine Cr(III) and Cr(VI) species in real water samples. Copyright © 2016. Published by Elsevier B.V.

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

    International Nuclear Information System (INIS)

    Mandiwana, Khakhathi L.; Panichev, Nikolay

    2010-01-01

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

  16. Electrothermal frequency reference

    NARCIS (Netherlands)

    Makinwa, K.A.A.; Kashmiri, S.M.

    2011-01-01

    An electrothermal frequency-locked loop (EFLL) circuit is described. This EFLL circuit includes an oscillator in a feedback loop. A drive circuit in the EFLL circuit generates a first signal having a fundamental frequency, and an electrothermal filter (ETF) in the EFLL circuit provides a second

  17. Magnetic ferrite particles combined with electrothermal atomic absorption spectrometry for the speciation of low concentrations of arsenic.

    Science.gov (United States)

    López-García, Ignacio; Marín-Hernández, Juan José; Hernández-Córdoba, Manuel

    2018-05-01

    Freshly in situ prepared ferrite particles were used for the micro-solid phase extraction of arsenic species. When the separation was carried out at pH 8, inorganic arsenic (As(III) + As(V)) and monomethylarsonic acid (MMA) were retained in the magnetic material. A second aliquot was treated with 2,3 dimercapto propanol, leading to the retention of As(V)+MMA, while a third aliquot was first treated with sodium thiosulphate, in which case only inorganic arsenic passed to the solid phase. In all cases, the solid residue collected by a magnet was suspended in a dilute nitric acid solution containing Triton X-100 and introduced into the electrothermal atomizer to obtain the analytical signal of arsenic. The use of palladium as a chemical modifier allowed calibration to be carried out with aqueous standards. The detection limit was 0.02µgL -1 arsenic for a 10mL sample volume. The procedure was applied to waters and herbal infusions, and its reliability was evaluated by analyzing eleven certified reference materials for which speciation data are provided. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Working towards accreditation by the International Standards Organization 15189 Standard: how to validate an in-house developed method an example of lead determination in whole blood by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Garcia Hejl, Carine; Ramirez, Jose Manuel; Vest, Philippe; Chianea, Denis; Renard, Christophe

    2014-09-01

    Laboratories working towards accreditation by the International Standards Organization (ISO) 15189 standard are required to demonstrate the validity of their analytical methods. The different guidelines set by various accreditation organizations make it difficult to provide objective evidence that an in-house method is fit for the intended purpose. Besides, the required performance characteristics tests and acceptance criteria are not always detailed. The laboratory must choose the most suitable validation protocol and set the acceptance criteria. Therefore, we propose a validation protocol to evaluate the performance of an in-house method. As an example, we validated the process for the detection and quantification of lead in whole blood by electrothermal absorption spectrometry. The fundamental parameters tested were, selectivity, calibration model, precision, accuracy (and uncertainty of measurement), contamination, stability of the sample, reference interval, and analytical interference. We have developed a protocol that has been applied successfully to quantify lead in whole blood by electrothermal atomic absorption spectrometry (ETAAS). In particular, our method is selective, linear, accurate, and precise, making it suitable for use in routine diagnostics.

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-08-05

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

  1. Species selective preconcentration and quantification of gold nanoparticles using cloud point extraction and electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Hartmann, Georg; Schuster, Michael

    2013-01-01

    Highlights: ► We optimized cloud point extraction and ET-AAS parameters for Au-NPs measurement. ► A selective ligand (sodium thiosulphate) is introduced for species separation. ► A limit of detection of 5 ng Au-NP per L is achieved for aqueous samples. ► Measurement of samples with high natural organic mater content is possible. ► 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 −1 is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L −1 . The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L −1 is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples.

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

    International Nuclear Information System (INIS)

    Kowalewska, Zofia

    2007-01-01

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

  3. A new supramolecular based liquid solid microextraction method for preconcentration and determination of trace bismuth in human blood serum and hair samples by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Kahe, Hadi; Chamsaz, Mahmoud

    2016-11-01

    A simple and reliable supramolecule-aggregated liquid solid microextraction method is described for preconcentration and determination of trace amounts of bismuth in water as well as human blood serum and hair samples. Catanionic microstructures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) surfactants, dissolved in deionized water/propanol, are used as a green solvent to extract bismuth (III)-diethyldithiocarbamate complexes by dispersive microextraction methodology. The extracted solid phase is easily removed and dissolved in 50 μL propanol for subsequent measurement by electrothermal atomic absorption spectrometry (ET-AAS). The procedure benefits the merits of supramolecule aggregates' properties and dispersive microextraction technique using water as the main component of disperser solvent, leading to direct interaction with analyte. Phase separation behavior of extraction solvent and different parameters influencing the extraction efficiency of bismuth ion such as salt concentration, pH, centrifugation time, amount of chelating agent, SDS:CTAB mole ratio, and solvent amounts were thoroughly optimized. Under the optimal experimental conditions, the calibration curve was linear in the range of 0.3-6 μg L -1 Bi (III) with a limit of detection (LOD) of 0.16 μg L -1 (S/N = 3). The relative standard deviations (RSD) of determination were obtained to be 5.1 and 6.2 % for 1 and 3 μg L -1 of Bi (III), respectively. The developed method was successfully applied as a sensitive and accurate technique for determination of bismuth ion in human blood serum, hair samples, and a certified reference material.

  4. Flow injection on-line dilution for zinc determination in human saliva with electrothermal atomic absorption spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Burguera-Pascu, Margarita [Department of Oral Medicine, School of Dentistry, University of Granada, Granada (Spain)], E-mail: margaburpas@hotmail.com; Rodriguez-Archilla, Alberto [Department of Oral Medicine, School of Dentistry, University of Granada, Granada (Spain); Burguera, Jose Luis; Burguera, Marcela; Rondon, Carlos; Carrero, Pablo [Department of Chemistry, Faculty of Sciences, University of Los Andes, Merida (Venezuela)

    2007-09-26

    An automated method is described for the determination of zinc in human saliva by electrothermal atomic absorption spectrometry (ET AAS) after on-line dilution of samples with a significant reduction of sample consumption per analysis (<0.4 mL including the dead volume of the system). In order to fulfill this aim without changing the sample transport conduits during the experiments, a flow injection (FI) dilution system was constructed. Its principal parts are: one propulsion device (peristaltic pump, PP) for either samples, standards or washing solution all located in an autosampler tray and for the surfactant solution (Triton X-100) used as diluent, and a two-position time based solenoid injector (TBSI{sub 1}) which allowed the introduction of 10 {mu}L of either solution in the diluent stream. To avoid unnecessary waste of samples, the TBSI{sub 1} also permitted the recirculation of the solutions to their respective autosampler cups. The downstream diluted solution fills a home made sampling arm assembly. The sequential deposition of 20 {mu}L aliquots of samples or standards on the graphite tube platform was carried out by air displacement with a similar time based solenoid injector (TBSI{sub 2}). The dilution procedure and the injection of solutions into the atomizer are computer controlled and synchronized with the operation of the temperature program. Samples or standards solutions were submitted to two drying steps (at 90 and 130 deg. C), followed by pyrolysis and atomization at 700 and 1700 deg. C, respectively. The aqueous calibration was linear up to 120.0 {mu}g L{sup -1} for diluted standard solutions/samples and its slope was similar (p > 0.05) to the standard addition curve, indicating lack of matrix effect. The precision tested by repeated analysis of real saliva samples was less than 3% and the detection limit (3{sigma}) was of 0.35 {mu}g L{sup -1}. To test the accuracy of the proposed procedure, recovery tests were performed, obtaining mean recovery

  5. Determination of gold, indium, tellurium and thallium in the same sample digest of geological materials by atomic-absorption spectroscopy and two-step solvent extraction

    Science.gov (United States)

    Hubert, A.E.; Chao, T.T.

    1985-01-01

    A rock, soil, or stream-sediment sample is decomposed with hydrofluoric acid, aqua regia, and hydrobromic acid-bromine solution. Gold, thallium, indium and tellurium are separated and concentrated from the sample digest by a two-step MIBK extraction at two concentrations of hydrobromic add. Gold and thallium are first extracted from 0.1M hydrobromic acid medium, then indium and tellurium are extracted from 3M hydrobromic acid in the presence of ascorbic acid to eliminate iron interference. The elements are then determined by flame atomic-absorption spectrophotometry. The two-step solvent extraction can also be used in conjunction with electrothermal atomic-absorption methods to lower the detection limits for all four metals in geological materials. ?? 1985.

  6. A highly selective and sensitive ultrasonic assisted dispersive liquid phase microextraction based on deep eutectic solvent for determination of cadmium in food and water samples prior to electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Zounr, Rizwan Ali; Tuzen, Mustafa; Deligonul, Nihal; Khuhawar, Muhammad Yar

    2018-07-01

    A simple, fast, green, sensitive and selective ultrasonic assisted deep eutectic solvent liquid-phase microextraction technique was used for preconcentration and extraction of cadmium (Cd) in water and food samples by electrothermal atomic absorption spectrometry (ETAAS). In this technique, a synthesized reagent (Z)-N-(3,5-diphenyl-1H-pyrrol-2-yl)-3,5-diphenyl-2H-pyrrol-2-imine (Azo) was used as a complexing agent for Cd. The main factors effecting the pre-concentration and extraction of Cd such as effect of pH, type and composition of deep eutectic solvent (DES), volume of DES, volume of complexing agent, volume of tetrahydrofuran (THF) and ultrasonication time have been examined in detail. At optimum conditions the value of pH and molar ratio of DES were found to be 6.0 and 1:4 (ChCl:Ph), respectively. The detection limit (LOD), limit of quantification (LOQ), relative standard deviation (RSD) and preconcentration factor (PF) were observed as 0.023 ng L -1 , 0.161 ng L -1 , 3.1% and 100, correspondingly. Validation of the developed technique was observed by extraction of Cd in certified reference materials (CRMs) and observed results were successfully compared with certified values. The developed procedure was practiced to various food, beverage and water samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

  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. Survey of content of cadmium, calcium, chromium, copper, iron, lead, magnesium, manganese, mercury, sodium and zinc in chamomile and green tea leaves by electrothermal or flame atomizer atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Prkić Ante

    2018-03-01

    Full Text Available Due to the simplicity of tea preparation (pouring hot water onto different dried herbs and its high popularity as a beverage, monitoring and developing a screening methodology for detecting the metal content is very important. The concentrations of Cd, Ca, Cr, Cu, Fe, Pb, Mg, Mn, Hg, Na and Zn in 8 samples of green tea (Camellia sinesis and in 11 samples chamomile (Matricaria chamomilla L. purchased both at local herbal pharmacies and supermarkets were determined using electrothermal atomizer atomic absorption spectrometry (ETAAS and flame atomizer atomic absorption spectrometry (FAAS. The found concentrations in chamomile were: Cd (0.008 – 284 mg kg−1, Ca (2.42 – 6.29%, Cr (0.91 – 6.92 mg kg−1, Cu (6.27 – 11.39 mg kg−1, Fe (133.5 – 534 mg kg−1, Pb (0.561 – 1.277 mg kg−1, Mg (2.27 – 3.73%, Mn (62.2 – 165.6 mg kg−1, Hg (0.660 – 1.346 μg kg−1, Na (0.91 – 1.28% and Zn (63.37 – 108.5 mg kg−1, in green tea Cd (36.29 – 202.1 mg kg−1, Ca (2.77 – 6.40%, Cr (1.520 – 5.278 mg kg−1, Cu (9.354 – 22.56 mg kg−1, Fe (162.6 – 513.3 mg kg−1, Pb (1.808 – 4.770 mg kg−1, Mg (1.41 – 2.62 %, Mn (1.147 – 1.729 g kg−1, Hg (1.045 – 2.802 μg kg−1, Na (0.44 – 0.98% and Zn (30.65 – 115.6 mg kg−1, respectively. Principal Component Analysis (PCA was applied to identify factors (soil, climate and country of origin influencing the content of the measured elements in herbal samples. The proposed methodology developed in this work was successfully applied to the detection of metals in herbal samples. The analysis showed that the content of toxic metals in green tea samples was significantly higher and very close to the maximum dose recommended by the World Health Organization (WHO.

  9. Method development for the determination of fluorine in water samples via the molecular absorption of strontium monofluoride formed in an electrothermal atomizer

    Energy Technology Data Exchange (ETDEWEB)

    Ozbek, Nil, E-mail: nil.ozbek@itu.edu.tr; Akman, Suleyman, E-mail: akmans@itu.edu.tr

    2012-03-15

    The presence of fluorine (F) was detected via the rotational molecular absorption line of diatomic strontium-monofluoride (SrF) generated in the gas phase at 651.187 nm using high-resolution continuum source electrothermal atomic absorption spectrometry. Upon the addition of excess strontium (Sr) as the nitrate, the fluorine in the sample was converted to SrF in the gas phase of a graphite furnace. The effects on the accuracy, precision and sensitivity of variables such as the SrF wavelength, graphite furnace program, amount of Sr, coating of the graphite tube and platform with Zr and Ir and the use of a modifier were investigated and optimized. It was determined that there was no need to use a modifier or to cover the platform/tubes with Zr or Ir. Fluorine concentrations in various water samples (certified waste water, tap water, drinking water and mineral water) were determined using 20 {mu}g of Sr as the molecule-forming reagent and applying a maximum pyrolysis temperature of 800 Degree-Sign C and a molecule-forming temperature of 2200 Degree-Sign C with a heating rate of 2000 Degree-Sign C s{sup -1}. Good linearity was maintained up to 0.1 {mu}g of F. The accuracy and precision of the method were tested by analyzing certified reference wastewater. The results were in good agreement with certified values, and the precision was satisfactory (RSD < 10%). The limit of detection and the characteristic mass for the method were 0.36 ng and 0.55 ng, respectively. Finally, the fluorine concentrations in several drinking water and mineral water samples taken from the market were determined. The results were in good agreement with the values supplied by the producers. No significant differences were found between the results from the linear calibration and standard addition techniques. The method was determined to be simple, fast, accurate and sensitive. - Highlights: Black-Right-Pointing-Pointer F is determined via MAS of SrF at 651.187 nm using HR-CS-ET AAS. Black

  10. Advances in atomic spectroscopy

    CERN Document Server

    Sneddon, J

    1998-01-01

    This volume continues the series'' cutting-edge reviews on developments in this field. Since its invention in the 1920s, electrostatic precipitation has been extensively used in industrial hygiene to remove dust and particulate matter from gases before entering the atmosphere. This combination of electrostatic precipitation is reported upon in the first chapter. Following this, chapter two reviews recent advances in the area of chemical modification in electrothermal atomization. Chapter three consists of a review which deal with advances and uses of electrothermal atomization atomic absorption spectrometry. Flow injection atomic spectroscopy has developed rapidly in recent years and after a general introduction, various aspects of this technique are looked at in chapter four. Finally, in chapter five the use of various spectrometric techniques for the determination of mercury are described.

  11. Highly sensitive and interference-free determination of bismuth in environmental samples by electrothermal vaporization atomic fluorescence spectrometry after hydride trapping on iridium-coated tungsten coil

    International Nuclear Information System (INIS)

    Liu Rui; Wu Peng; Xu Kailai; Lv Yi; Hou Xiandeng

    2008-01-01

    Bismuthine was on-line trapped on tungsten coil and subsequently electrothermally vaporized for the determination by atomic fluorescence spectrometry (AFS). Several noble metals, including Pd, Rh, Pt, and Ir, were explored as permanent chemical modifier for tungsten coil on-line trapping. Investigation showed that Ir gave the best performance, in which bismuthine was on-line trapped on Ir-coated tungsten coil at 560 o C, and then released at 1550 o C for subsequent transfer to AFS by a mixture of Ar and H 2 . Under optimum instrumental conditions, the trapping efficiency was found to be 73 ± 3%. With 120 s (12 mL sample volume) trapping time, a limit of detection (LOD) of 4 ng L -1 was obtained, compared to conventional hydride generation AFS (0.09 μg L -1 ); the LOD can be lowered down to 1 ng L -1 by increasing the trapping time to 480 s. The LOD was found to be better or at least comparable to literature levels involving on-line trapping and some other sophisticated instrumental methods such as ICP-MS and GF-AAS. A comprehensive interference study involving conventional hydride-forming elements and some transition metals was carried out, and the result showed that the gas phase interference from other hydride-forming elements was largely reduced, thanks to the use of on-line tungsten coil trapping. Finally, the proposed method was applied to the determination of bismuth in several biological and environmental standard reference materials, and a t-test shows that the analytical results by the proposed method have no significant difference from the certified values at the confidence level of 95%

  12. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    Energy Technology Data Exchange (ETDEWEB)

    Gil, Sandra [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Fragueiro, Sandra [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain)]. E-mail: bendicho@uvigo.es

    2005-01-10

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-{mu}l volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium.

  13. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    International Nuclear Information System (INIS)

    Gil, Sandra; Fragueiro, Sandra; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-μl volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium

  14. Electrothermally Tunable Arch Resonator

    KAUST Repository

    Hajjaj, Amal Z.

    2017-03-18

    This paper demonstrates experimentally, theoretically, and numerically a wide-range tunability of electrothermally actuated microelectromechanical arch beams. The beams are made of silicon and are intentionally fabricated with some curvature as in-plane shallow arches. An electrothermal voltage is applied between the anchors of the beam generating a current that controls the axial stress caused by thermal expansion. When the electrothermal voltage increases, the compressive stress increases inside the arch beam. This leads to an increase in its curvature, thereby increasing its resonance frequencies. We show here that the first resonance frequency can increase monotonically up to twice its initial value. We show also that after some electrothermal voltage load, the third resonance frequency starts to become more sensitive to the axial thermal stress, while the first resonance frequency becomes less sensitive. These results can be used as guidelines to utilize arches as wide-range tunable resonators. Analytical results based on the nonlinear Euler Bernoulli beam theory are generated and compared with the experimental data and the results of a multi-physics finite-element model. A good agreement is found among all the results. [2016-0291

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

    DEFF Research Database (Denmark)

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

    2005-01-01

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

  16. Electrothermal atomisation atomic absorption conditions and matrix modifications for determining antimony, arsenic, bismuth, cadmium, gallium, gold, indium, lead, molybdenum, palladium, platinum, selenium, silver, tellurium, thallium and tin following back-extraction of organic aminohalide extracts

    Science.gov (United States)

    Clark, J.R.

    1986-01-01

    A multi-element organic-extraction and back-extraction procedure, that had been developed previously to eliminate matrix interferences in the determination of a large number of trace elements in complex materials such as geological samples, produced organic and aqueous solutions that were complex. Electrothermal atomisation atomic absorption conditions and matrix modifications have been developed for 13 of the extracted elements (Ag, As, Au, Bi, Cd, Ga, In, Pb, Sb, Se, Sn, Te and Tl) that enhance sensitivity, alleviate problems resulting from the complex solutions and produce acceptable precision. Platinum, Pd and Mo can be determined without matrix modification directly on the original unstripped extracts.

  17. Selenium determination in biological material by atomic absorption spectrophotometry in graphite furnace and using vapor generation

    International Nuclear Information System (INIS)

    Carvalho Vidal, M. de F. de.

    1984-01-01

    The applicability of the atomic absorption spectrophotometry to the determination of selenium in biological material using vapor generation and electrothermal atomization in the graphite furnace was investigated. Instrumental parameters and the analytical conditions of the methods were studied. Decomposition methods for the samples were tested, and the combustion in the Wickbold apparatus was chosen. (author) [pt

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

    International Nuclear Information System (INIS)

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

    2008-01-01

    The artifacts created in the measurement of phosphorus at the 213.6-nm non-resonance line by electrothermal atomic absorption spectrometry using line source atomic absorption spectrometry (LS AAS) and deuterium lamp background correction (D 2 BC) have been investigated using high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). The absorbance signals and the analytical curves obtained by LS AAS without and with D 2 BC, and with HR-CS AAS without and with automatic correction for continuous background absorption, and also with least-squares background correction for molecular absorption with rotational fine structure were compared. The molecular absorption due to the suboxide PO that exhibits pronounced fine structure could not be corrected by the D 2 BC system, causing significant overcorrection. Among the investigated chemical modifiers, NaF, La, Pd and Pd + Ca, the Pd modifier resulted in the best agreement of the results obtained with LS AAS and HR-CS AAS. However, a 15% to 100% higher sensitivity, expressed as slope of the analytical curve, was obtained for LS AAS compared to HR-CS AAS, depending on the modifier. Although no final proof could be found, the most likely explanation is that this artifact is caused by a yet unidentified phosphorus species that causes a spectrally continuous absorption, which is corrected without problems by HR-CS AAS, but which is not recognized and corrected by the D 2 BC system of LS AAS

  19. Magnetic-field dependence of electrothermal conductivity in YBCO

    Energy Technology Data Exchange (ETDEWEB)

    Marino, A.; Uribe, R. [Universidad del Tolima, Ibague (Colombia); Grupo de Superconductividad y Nuevos Materiales, Universidad Nacional de Colombia, Bogota (Colombia)

    2008-11-15

    Experimental measurements of the electrothermal conductivity (P) near T{sub c}, as a function of external magnetic field were carried out in undoped YBCO (123) superconducting samples. The electrothermal conductivity which relates electrical and thermal currents, depends on the applied magnetic field in high T{sub c} materials, contrary to conventional low T{sub c} superconductors where P is nearly independent of the magnetic field. The experimental P(B,T) data determined from resistivity and thermopower measurements were analyzed in terms of theoretical models and showed a behavior consistent with an order-parameter symmetry (OPS) of d{sub x{sup 2}-y{sup 2}}-wave type. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  20. Interfase y software de control para operar en sincronismo un automuestreador y un atomizador electrotérmico por filamento de tungsteno en espectrofotometría de absorción atómica Development of interface and software for synchronous operation of an autosampler and a tungsten coil electrothermal atomizer coupled to an atomic absorption spectophotometer

    OpenAIRE

    J. Neira; G. Valenzuela; J. Vega; J. Moya; C. G. Bruhn; J. A. Nóbrega

    1998-01-01

    The interface and software for synchronous control of an autosampler and an electrothermal tungsten coil atomizer in atomic absorption spectrophotometry were developed. The control of the power supply, the trigger of the Read function of the spectrophotometer and the automatic operation of the autosampler was performed by software written in "TurboBasic". The system was evaluated by comparison of the repeatability of peak-height absorbances obtained in the atomization of lead by consecutive 1...

  1. Electrothermal atomic absorption spectrometric determination of copper in nickel-base alloys with various chemical modifiers*1

    Science.gov (United States)

    Tsai, Suh-Jen Jane; Shiue, Chia-Chann; Chang, Shiow-Ing

    1997-07-01

    The analytical characteristics of copper in nickel-base alloys have been investigated with electrothermal atomic absorption spectrometry. Deuterium background correction was employed. The effects of various chemical modifiers on the analysis of copper were investigated. Organic modifiers which included 2-(5-bromo-2-pyridylazo)-5-(diethylamino-phenol) (Br-PADAP), ammonium citrate, 1-(2-pyridylazo)-naphthol, 4-(2-pyridylazo)resorcinol, ethylenediaminetetraacetic acid and Triton X-100 were studied. Inorganic modifiers palladium nitrate, magnesium nitrate, aluminum chloride, ammonium dihydrogen phosphate, hydrogen peroxide and potassium nitrate were also applied in this work. In addition, zirconium hydroxide and ammonium hydroxide precipitation methods have also been studied. Interference effects were effectively reduced with Br-PADAP modifier. Aqueous standards were used to construct the calibration curves. The detection limit was 1.9 pg. Standard reference materials of nickel-base alloys were used to evaluate the accuracy of the proposed method. The copper contents determined with the proposed method agreed closely with the certified values of the reference materials. The recoveries were within the range 90-100% with relative standard deviation of less than 10%. Good precision was obtained.

  2. Preconcentration and speciation of chromium in a sequential injection system incorporating dual mini-columns coupled with electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zou Aimei; Tang Xiaoyan; Chen Mingli [Research Center for Analytical Sciences, Northeastern University, Box 332, Shenyang 110004 (China); Wang Jianhua [Research Center for Analytical Sciences, Northeastern University, Box 332, Shenyang 110004 (China)], E-mail: jianhuajrz@mail.neu.edu.cn

    2008-05-15

    A procedure for chromium preconcentration and speciation with a dual mini-column sequential injection system coupled with electrothermal atomic absorption spectrometry (ETAAS) was developed. At pH 6, the sample solution was firstly aspirated to flow through a Chlorella vulgaris cell mini-column on which the Cr(III) was retained. The effluent was afterwards directed to flow through a 717 anion exchange resin mini-column accompanied by the retention of Cr(VI). Thereafter, Cr(III) and Cr(VI) were eluted by 0.04 mol L{sup -1} and 1.0 mol L{sup -1} nitric acid, respectively, and the eluates were quantified with ETAAS. Chemical and flow variables governing the performance of the system were investigated. By using a sampling volume of 600 {mu}L, sorption efficiencies of 99.7% for Cr(III) and 99% for Cr(VI) were achieved along with enrichment factors of 10.5 for Cr(III) and 11.6 for Cr(VI), within linear ranges of 0.1-2.5 {mu}g L{sup -1} for Cr(III) and 0.12-2.0 {mu}g L{sup -1} for Cr(VI). Detection limits of 0.02 {mu}g L{sup -1} for Cr(III) and 0.03 {mu}g L{sup -1} for Cr(VI) along with RSD values of 1.9% for Cr(III) and 2.5% for Cr(VI) (1.0 {mu}g L{sup -1}, n = 11) were obtained. The procedure was validated by analyzing a certified reference material of GBW08608 and further demonstrated by chromium speciation in river and tap water samples.

  3. Electrothermally Tunable Bridge Resonator

    KAUST Repository

    Hajjaj, Amal Z.; Alcheikh, Nouha; Ramini, Abdallah; Hafiz, Md Abdullah Al; Younis, Mohammad I.

    2016-01-01

    This paper demonstrates experimentally, theoretically, and numerically a wide-range tunability of an in-plane clamped-clamped microbeam, bridge, and resonator compressed by a force due to electrothermal actuation. We demonstrate that a single resonator can be operated at a wide range of frequencies. The microbeam is actuated electrothermally, by passing a DC current through it. We show that when increasing the electrothermal voltage, the compressive stress inside the microbeam increases, which leads eventually to its buckling. Before buckling, the fundamental frequency decreases until it drops to very low values, almost to zero. After buckling, the fundamental frequency increases, which is shown to be as high as twice the original resonance frequency. Analytical results based on the Galerkin discretization of the Euler Bernoulli beam theory are generated and compared to the experimental data and to simulation results of a multi-physics finite-element model. A good agreement is found among all the results.

  4. Electrothermally Tunable Bridge Resonator

    KAUST Repository

    Hajjaj, Amal Z.

    2016-12-05

    This paper demonstrates experimentally, theoretically, and numerically a wide-range tunability of an in-plane clamped-clamped microbeam, bridge, and resonator compressed by a force due to electrothermal actuation. We demonstrate that a single resonator can be operated at a wide range of frequencies. The microbeam is actuated electrothermally, by passing a DC current through it. We show that when increasing the electrothermal voltage, the compressive stress inside the microbeam increases, which leads eventually to its buckling. Before buckling, the fundamental frequency decreases until it drops to very low values, almost to zero. After buckling, the fundamental frequency increases, which is shown to be as high as twice the original resonance frequency. Analytical results based on the Galerkin discretization of the Euler Bernoulli beam theory are generated and compared to the experimental data and to simulation results of a multi-physics finite-element model. A good agreement is found among all the results.

  5. Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

    Science.gov (United States)

    de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

    2017-08-15

    Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl -1 , respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. 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.

  7. Comparison of colorimetry and electrothermal atomic absorption spectroscopy for the quantification of non-transferrin bound iron in human sera.

    Science.gov (United States)

    Jittangprasert, Piyada; Wilairat, Prapin; Pootrakul, Pensri

    2004-12-01

    This paper describes a comparison of two analytical techniques, one employing bathophenanthrolinedisulfonate (BPT), a most commonly-used reagent for Fe (II) determination, as chromogen and an electrothermal atomic absorption spectroscopy (ETAAS) for the quantification of non-transferrin bound iron (NTBI) in sera from thalassemic patients. Nitrilotriacetic acid (NTA) was employed as the ligand for binding iron from low molecular weight iron complexes present in the serum but without removing iron from the transferrin protein. After ultrafiltration the Fe (III)-NTA complex was then quantified by both methods. Kinetic study of the rate of the Fe (II)-BPT complex formation for various excess amounts of NTA ligand was also carried out. The kinetic data show that a minimum time duration (> 60 minutes) is necessary for complete complex formation when large excess of NTA is used. Calibration curves given by colorimetric and ETAAS methods were linear over the range of 0.15-20 microM iron (III). The colorimetric and ETAAS methods exhibited detection limit (3sigma) of 0.13 and 0.14 microM, respectively. The NTBI concentrations from 55 thalassemic serum samples measured employing BPT as chromogen were statistically compared with the results determined by ETAAS. No significant disagreement at 95% confidence level was observed. It is, therefore, possible to select any one of these two techniques for determination of NTBI in serum samples of thalassemic patients. However, the colorimetric procedure requires a longer analysis time because of a slow rate of exchange of NTA ligand with BPT, leading to the slow rate of formation of the colored complex.

  8. Speciation and determination of inorganic mercury and methylmercury by headspace single drop microextraction and electrothermal atomic absorption spectrometry in water and fish

    Energy Technology Data Exchange (ETDEWEB)

    Sarica, Deniz Yurtsever [Scientific and Technological Research Council of Turkey, Ankara Test and Analysis Laboratory, TUeBITAK/ATAL, Besevler, Ankara (Turkey); Tuerker, Ali Rehber [Science Faculty, Department of Chemistry, Gazi University, Ankara (Turkey)

    2012-05-15

    In this study, headspace single drop microextraction (HS-SDME) method in combination with electrothermal atomic absorption spectrometry (ETAAS) method was developed and validated for the speciation and determination of inorganic mercury (iHg) and methylmercury (MeHg). MeHg and iHg species were reduced to volatile methylmercury hydride (CH{sub 3}HgH) and elemental mercury, respectively, in the presence of NaBH{sub 4} and trapped onto a drop of acceptor phase in the tip of a microsyringe. Thiourea and ammonium pyrrolydinedithiocarbamate (APDC) were tested as the acceptor phase. The experimental parameters of the method such as microextraction time, temperature, NaBH{sub 4} concentration, acceptor phase concentration, and pH of the medium were investigated to obtain distinctive conditions for mercury species. Possible interference effects have also been investigated. In order to validation of the method, analytical figures of merits such as accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), and linear working range have been evaluated. Accuracy of the method has been verified by analyzing certified reference materials (BCR 453 Tuna fish) and spiked samples. The proposed method was applied for the speciation and determination of mercury species in water and fish samples. Mercury species (MeHg and iHg) have been determined in the real samples with a relative error less than 10%. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  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. Speciation of silver nanoparticles and Ag(I) species using cloud point extraction followed by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

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

    2014-01-01

    Silver nanoparticles in the presence of Triton-X114 were extracted into a micellar phase obtained after incubation at 40 °C for 10 min followed by centrifugation. After injection of an aliquot (30 μL) of the surfactant-rich phase into the electrothermal atomizer, the enrichment effect due to cloud point extraction allowed a detection limit of 2 ng L −1 silver to be achieved. The preconcentration factor was 242, and the repeatability for ten measurements at a 50 ng L −1 silver level was 4.6%. Ag(I) species were adsorbed onto the silver nanoparticles and were also extracted in the micellar phase. The incorporation of 0.01 mol L −1 ammonium thiocyanate to the sample solution prevented the extraction of Ag(I) species. Speciation was carried out using two extractions, one in the absence and the other in the presence of thiocyanate, the concentration of Ag(I) species being obtained by difference. The procedure was applied to the determination of silver nanoparticles and Ag(I) species in waters and in lixiviates obtained from sticking plasters and cleaning cloths. - Highlights: • Silver nanoparticles and Ag(I) species are separated into a surfactant-rich phase. • The Ag(I) species are not extracted in the presence of thiocyanate. • The cloud point extraction of two aliquots allows speciation to be carried out. • Extreme sensitivity (detection limit 2 ng L −1 ) is achieved

  11. Speciation of silver nanoparticles and Ag(I) species using cloud point extraction followed by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    López-García, Ignacio; Vicente-Martínez, Yesica; Hernández-Córdoba, Manuel, E-mail: hcordoba@um.es

    2014-11-01

    Silver nanoparticles in the presence of Triton-X114 were extracted into a micellar phase obtained after incubation at 40 °C for 10 min followed by centrifugation. After injection of an aliquot (30 μL) of the surfactant-rich phase into the electrothermal atomizer, the enrichment effect due to cloud point extraction allowed a detection limit of 2 ng L{sup −1} silver to be achieved. The preconcentration factor was 242, and the repeatability for ten measurements at a 50 ng L{sup −1} silver level was 4.6%. Ag(I) species were adsorbed onto the silver nanoparticles and were also extracted in the micellar phase. The incorporation of 0.01 mol L{sup −1} ammonium thiocyanate to the sample solution prevented the extraction of Ag(I) species. Speciation was carried out using two extractions, one in the absence and the other in the presence of thiocyanate, the concentration of Ag(I) species being obtained by difference. The procedure was applied to the determination of silver nanoparticles and Ag(I) species in waters and in lixiviates obtained from sticking plasters and cleaning cloths. - Highlights: • Silver nanoparticles and Ag(I) species are separated into a surfactant-rich phase. • The Ag(I) species are not extracted in the presence of thiocyanate. • The cloud point extraction of two aliquots allows speciation to be carried out. • Extreme sensitivity (detection limit 2 ng L{sup −1}) is achieved.

  12. Separation/preconcentration and determination of vanadium with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) and electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Asadollahi, Tahereh; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

    2010-06-30

    A novel dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for separation/preconcentration of ultra trace amount of vanadium and its determination with the electrothermal atomic absorption spectrometry (ETAAS) was developed. The DLLME-SFO behavior of vanadium (V) using N-benzoyl-N-phenylhydroxylamine (BPHA) as complexing agent was systematically investigated. The factors influencing the complex formation and extraction by DLLME-SFO method were optimized. Under the optimized conditions: 100 microL, 200 microL and 25 mL of extraction solvent (1-undecanol), disperser solvent (acetone) and sample volume, respectively, an enrichment factor of 184, a detection limit (based on 3S(b)/m) of 7 ng L(-1) and a relative standard deviation of 4.6% (at 500 ng L(-1)) were obtained. The calibration graph using the preconcentration system for vanadium was linear from 20 to 1000 ng L(-1) with a correlation coefficient of 0.9996. The method was successfully applied for the determination of vanadium in water and parsley. Copyright 2010 Elsevier B.V. All rights reserved.

  13. Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero, E-mail: carlos.herrero@usc.es

    2014-11-01

    The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption–elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L{sup −1}, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64–22.9 μg Pb L{sup −1}). - Highlights: • Lead determination in urine using a solid phase extraction procedure followed by ETAAS • Carbon nanotubes as SPE adsorbent for Pb in urine • Matrix elimination for the Pb determination in urine by using SPE based on carbon nanotubes • The detection limit was 0.08 μg Pb L{sup −1}.

  14. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.; Teixeira, Leonardo S. G.

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box-Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L- 1 HNO3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg- 1. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method.

  15. Speciation analysis of thallium using electrothermal AAS following on-line pre-concentration in a microcolumn filled with multiwalled carbon nanotubes

    International Nuclear Information System (INIS)

    Gil, R.A.; Pacheco, P.H.; Olsina, R.A.; Martinez, L.D.; Smichowski, P.

    2009-01-01

    The enrichment ability of carbon nanotubes (CNTs) was investigated and a new method established for the determination of trace thallium species in environmental samples using electrothermal atomization-atomic absorption spectrometry (ETAAS). The CNTs were employed as sorbent substrate in a continuous flow system coupled to ETAAS. Parameters influencing the recoveries of thallium were optimized. Under optimal conditions, the detection limit and precision of the method were 0.009 μg L -1 and 3.9 %, respectively. The method was applied to the determination of thallium in real environmental samples and the recoveries were in the range from 96 to 100 %. This system was able to separate thallium (I) from the matrix, which allowed its selective determination. The total thallium content was then determined by reducing Tl(III) with hydroxylamine. All these experimental results indicated that this new procedure can be applied to the determination of trace thallium in drinking water samples. (author)

  16. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.

    2015-01-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO 3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L −1 HNO 3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg −1 . Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and samples

  17. Electrothermal Frequency Modulated Resonator for Mechanical Memory

    KAUST Repository

    Hafiz, Md Abdullah Al

    2016-08-18

    In this paper, we experimentally demonstrate a mechanical memory device based on the nonlinear dynamics of an electrostatically actuated microelectromechanical resonator utilizing an electrothermal frequency modulation scheme. The microstructure is deliberately fabricated as an in-plane shallow arch to achieve geometric quadratic nonlinearity. We exploit this inherent nonlinearity of the arch and drive it at resonance with minimal actuation voltage into the nonlinear regime, thereby creating softening behavior, hysteresis, and coexistence of states. The hysteretic frequency band is controlled by the electrothermal actuation voltage. Binary values are assigned to the two allowed dynamical states on the hysteretic response curve of the arch resonator with respect to the electrothermal actuation voltage. Set-and-reset operations of the memory states are performed by applying controlled dc pulses provided through the electrothermal actuation scheme, while the read-out operation is performed simultaneously by measuring the motional current through a capacitive detection technique. This novel memory device has the advantages of operating at low voltages and under room temperature. [2016-0043

  18. Flame emission, atomic absorption and fluorescence spectrometry

    International Nuclear Information System (INIS)

    Horlick, G.

    1980-01-01

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

  19. Separation and preconcentration of ultratrace levels of cadmium(II) in a sequential injection (SI) system with a PTFE packed column as a mimic sequential injection lab-on-valve (SI-LOV) system with renewable column employing detection by electrothermal atomic absorption spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Gała, Piotr

    of cadmium(II) by detection with electrothermal atomic absorption spectrometry (ETAAS). The non-charged complex formed between the analyste and the chelating reagent diethyldithiophosphate (DDPA) was selectively adsorbed on the surface of the PTFE beads and eluted by ethanol before being directed...

  20. Highly Tunable Electrothermally Actuated Arch Resonator

    KAUST Repository

    Hajjaj, Amal Z.

    2016-12-05

    This paper demonstrates experimentally, theoretically, and numerically a wide-range tunability of electrothermally actuated MEMS arch beams. The beams are made of silicon and are intentionally fabricated with some curvature as in-plane shallow arches. Analytical results based on the Galerkin discretization of the Euler Bernoulli beam theory are generated and compared to the experimental data and results of a multi-physics finite-element model. A good agreement is found among all the results. The electrothermal voltage is applied between the anchors of the clamped-clamped MEMS arch beam, generating a current that passes through the MEMS arch beam and controls its axial stress caused by thermal expansion. When the electrothermal voltage increases, the compressive stress increases inside the arch beam. This leads to increase in its curvature, thereby increases the resonance frequencies of the structure. We show here that the first resonance frequency can increase up to twice its initial value. We show also that after some electro-thermal voltage load, the third resonance frequency starts to become more sensitive to the axial thermal stress, while the first resonance frequency becomes less sensitive. These results can be used as guidelines to utilize arches as wide-range tunable resonators.

  1. Electrothermal instability growth in magnetically driven pulsed power liners

    International Nuclear Information System (INIS)

    Peterson, Kyle J.; Sinars, Daniel B.; Yu, Edmund P.; Herrmann, Mark C.; Cuneo, Michael E.; Slutz, Stephen A.; Smith, Ian C.; Atherton, Briggs W.; Knudson, Marcus D.; Nakhleh, Charles

    2012-01-01

    This paper explores the role of electro-thermal instabilities on the dynamics of magnetically accelerated implosion systems. Electro-thermal instabilities result from non-uniform heating due to temperature dependence in the conductivity of a material. Comparatively little is known about these types of instabilities compared to the well known Magneto-Rayleigh-Taylor (MRT) instability. We present simulations that show electrothermal instabilities form immediately after the surface material of a conductor melts and can act as a significant seed to subsequent MRT instability growth. We also present the results of several experiments performed on Sandia National Laboratories Z accelerator to investigate signatures of electrothermal instability growth on well characterized initially solid aluminum and copper rods driven with a 20 MA, 100 ns risetime current pulse. These experiments show excellent agreement with electrothermal instability simulations and exhibit larger instability growth than can be explained by MRT theory alone.

  2. Determination of chromium in treated crayfish, Procambarus clarkii, by electrothermal ASS: study of chromium accumulation in different tissues

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez, F.; Diaz, J.; Medina, J.; Del Ramo, J.; Pastor, A.

    1986-06-01

    In the present study, the authors investigated the accumulation of chromium in muscle, hepatopancreas, antennal glands, and gills of Procambarus clarkii (Girard) from Lake Albufera following Cr(VI)-exposure. Determinations of chromium were made by using Electrothermal Atomic Absorption Spectroscopy and the standard additions method.

  3. 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

  4. Cloud point extraction combined with electrothermal atomic absorption spectrometry for the speciation of antimony(III) and antimony(V) in food packaging materials

    International Nuclear Information System (INIS)

    Jiang Xiuming; Wen Shengping; Xiang Guoqiang

    2010-01-01

    A simple, sensitive method for the speciation of inorganic antimony by cloud point extraction combined with electrothermal atomic absorption spectrometry (ETAAS) is presented and evaluated. The method based on the fact that formation of a hydrophobic complex of antimony(III) with ammonium pyrrolidine dithiocarbamate (APDC) at pH 5.0 and subsequently the hydrophobic complex enter into surfactant-rich phase, whereas antimony(V) remained in aqueous solutions. Antimony(III) in surfactant-rich phase was analyzed by ETAAS after dilution by 0.2 mL nitric acid in methanol (0.1 M), and antimony(V) was calculated by subtracting antimony(III) from the total antimony after reducing antimony(V) to antimony(III) by L-cysteine. The main factors affecting the cloud point extraction, such as pH, concentration of APDC and Triton X-114, equilibrium temperature and incubation time, sample volume were investigated in detail. Under the optimum conditions, the detection limit (3σ) of the proposed method was 0.02 ng mL -1 for antimony(III), and the relative standard deviation was 7.8% (c = 1.0 ng mL -1 , n = 7). The proposed method was successfully applied to speciation of inorganic antimony in the leaching solutions of different food packaging materials with satisfactory results.

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

    International Nuclear Information System (INIS)

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

    1980-01-01

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

  6. Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

    2016-02-01

    An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be < 5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L- 1 and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples.

  7. Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

    2016-02-05

    An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be <5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L(-1) and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Evaluation of a novel PTFE material for use as a means for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems. Determination of cadmium (II) with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Hansen, Elo Harald

    2004-01-01

    with an external packed column and in a sequential injection lab-on-valve (SI-LOV) system. Employed for the determination of cadmium(II), complexed with diethyldithiophosphate (DDPA), and detection by electrothermal atomic absorption spectrometry (ETAAS), its performance was compared to that of a previously used...

  9. Scalable Pressure Sensor Based on Electrothermally Operated Resonator

    KAUST Repository

    Hajjaj, Amal Z.; Hafiz, Md Abdullah Al; Alcheikh, Nouha; Younis, Mohammad I.

    2017-01-01

    We experimentally demonstrate a new pressure sensor that offers the flexibility of being scalable to small sizes up to the nano regime. Unlike conventional pressure sensors that rely on large diaphragms and big-surface structures, the principle of operation here relies on convective cooling of the air surrounding an electrothermally heated resonant structure, which can be a beam or a bridge. This concept is demonstrated using an electrothermally tuned and electrostatically driven MEMS resonator, which is designed to be deliberately curved. We show that the variation of pressure can be tracked accurately by monitoring the change in the resonance frequency of the resonator at a constant electrothermal voltage. We show that the range of the sensed pressure and the sensitivity of detection are controllable by the amount of the applied electrothermal voltage. Theoretically, we verify the device concept using a multi-physics nonlinear finite element model. The proposed pressure sensor is simple in principle and design and offers the possibility of further miniaturization to the nanoscale.

  10. Scalable Pressure Sensor Based on Electrothermally Operated Resonator

    KAUST Repository

    Hajjaj, Amal Z.

    2017-11-03

    We experimentally demonstrate a new pressure sensor that offers the flexibility of being scalable to small sizes up to the nano regime. Unlike conventional pressure sensors that rely on large diaphragms and big-surface structures, the principle of operation here relies on convective cooling of the air surrounding an electrothermally heated resonant structure, which can be a beam or a bridge. This concept is demonstrated using an electrothermally tuned and electrostatically driven MEMS resonator, which is designed to be deliberately curved. We show that the variation of pressure can be tracked accurately by monitoring the change in the resonance frequency of the resonator at a constant electrothermal voltage. We show that the range of the sensed pressure and the sensitivity of detection are controllable by the amount of the applied electrothermal voltage. Theoretically, we verify the device concept using a multi-physics nonlinear finite element model. The proposed pressure sensor is simple in principle and design and offers the possibility of further miniaturization to the nanoscale.

  11. In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

    2018-03-01

    In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

  12. Spatial discrimination against background with different optical systems for collection of fluorescence in laser-excited atomic fluorescence spectrometry with a graphite tube electrothermal atomizer.

    Science.gov (United States)

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

    1995-07-01

    A single 90 degrees off-axis ellipsoidal mirror fragment was used in a dispersive detection system for electrothermal atomization laser-excited atomic fluorescence spectrometry. The performance of the new optical arrangement was compared with those of optical arrangements that employed a plane mirror in combination with biconvex or plano-convex lenses. All the optical arrangements collected fluorescence in a scheme called front surface illustration. BEAM-4, an optical ray tracing program, was used for calculations of spatial ray distributions and optical collection efficiency for the various optical configurations. Experimentally, the best collection efficiency was obtained by use of the ellipsoidal mirror, in qualitative agreement with simulations done by use of the BEAM-4 software. The best detection limit for cobalt with the new optical arrangement was 20 fg, which was a factor of 5 better than that obtained with conventional optical arrangements with otherwise the same instrumentation. The signal-to-background ratio and the fluorescence collection efficiency were also studied as a function of position of the optical components for the various optical arrangements. For both cobalt and phosphorus, the signal-to-background ratio with the new optical arrangement remained stable within 10-20% during +/- 8 mm shifts in the position of the detection system from the focal plane of the optics. Overall, the new optical arrangement offered high collection efficiency, excellent sensitivity, and facile optical alignment due to efficient spatial separation between the fluorescence signal and the background radiation. The advantages of the new optical arrangement were particularly important during measurements in the presence of high levels of blackbody radiation.

  13. Coupling sequential injection on-line preconcentration by means of a renewable microcolumn with ion-exchange beads with detection by electrothermal atomic absorption spectrometry. Comparing the performance of eluting the loaded beads with transporting them directly into the graphite tube

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2001-01-01

    The design of a flow injection/sequential injection (FIA/SIA) on-line preconcentration system incorporating a renewable microcolumn with ion-exchange beads and interfaced with an electrothermal atomic absorption spectrometry (ETAAS) detector is described, and its practical applicability.......4% for the procedure in which the loaded beads are transported directly to the graphite furnace for pyrolysis and atomization, and even improved in comparison to the traditional unidirectional and bidirectional repetitive elution procedures which under comparable conditions yield R.S.D.-values of 5.8 and 4...

  14. Sample Preprocessing For Atomic Spectrometry

    International Nuclear Information System (INIS)

    Kim, Sun Tae

    2004-08-01

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

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

    Science.gov (United States)

    Giakisikli, Georgia; Anthemidis, Aristidis N

    2013-06-15

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

  16. Electrothermal atomic absorption spectrometric determination of cobalt, copper, lead and nickel traces in aragonite following flotation and extraction separation.

    Science.gov (United States)

    Zendelovska, D; Pavlovska, G; Cundeva, K; Stafilov, T

    2001-03-30

    A method of determination of Co, Cu, Pb and Ni in nanogram quantities from aragonite is presented. Flotation and extraction of Co, Cu, Pb and Ni is suggested as methods for elimination matrix interferences of calcium. The method of flotation is performed by iron(III) hexamethylenedithiocarbamate, Fe(HMDTC)(3), as a colloid precipitate collector. The liquid-liquid extraction of Co, Cu, Pb and Ni is carried out by sodium diethyldithiocarbamate, NaDDTC, as complexing reagent into methylisobutyl ketone, MIBK. The electrothermal atomic absorption spectrometry (ETAAS) is used for determination of analytes. The detection limits of ETAAS followed by flotation are: 7.8 ng.g(-1) for Co, 17.1 ng.g(-1) for Cu, 7.2 ng.g(-1) for Pb and 9.0 mug.g(-1) for Ni. The detection limits of ETAAS followed by extraction are found to be: 12.0 ng.g(-1) for Co, 51.0 ng.g(-1) for Cu, 24.0 ng.g(-1) for Pb and 21.0 ng.g(-1) for Ni.

  17. 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.

  18. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Jorge S.; Anunciação, Taiana A. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Brandão, Geovani C. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); INCT de Energia e Ambiente, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Dantas, Alailson F. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Lemos, Valfredo A. [Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, Jequié, Bahia 45506-191 (Brazil); and others

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO{sub 3} gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L{sup −1} HNO{sub 3} as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg{sup −1}. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and

  19. Compliant electro-thermal microactuators

    DEFF Research Database (Denmark)

    Jonsmann, Jacques; Sigmund, Ole; Bouwstra, Siebe

    1999-01-01

    This paper describes design, microfabrication and characterisation of topology optimised compliant electro-thermal microactuators. The actuators are fabricated by a fast prototyping process using laser micromachining and electroplating. Actuators are characterised with respect to displacement...

  20. Electrothermal plasma gun as a pellet injector

    International Nuclear Information System (INIS)

    Kincaid, R.W.; Bourham, M.A.

    1994-01-01

    The NCSU electrothermal plasma gun SIRENS has been used to accelerate plastic (Lexan polycarbonate) pellets, to determine the feasibility of the use of electrothermal guns as pellet injectors. The use of an electrothermal gun to inject frozen hydrogenic pellets requires a mechanism to provide protective shells (sabots) for shielding the pellet from ablation during acceleration into and through the barrel of the gun. The gun has been modified to accommodate acceleration of the plastic pellets using special acceleration barrels equipped with diagnostics for velocity and position of the pellet, and targets to absorb the pellet's energy on impact. The length of the acceleration path could be varied between 15 and 45 cm. The discharge energy of the electrothermal gun ranged from 2 to 6 kJ. The pellet velocities have been measured via a set of break wires. Pellet masses were varied between 0.5 and 1.0 grams. Preliminary results on 0.5 and 1.0 g pellets show that the exit velocity reaches 0.9 km/s at 6 kJ input energy to the source. Higher velocities of 1.5 and 2.7 km/s have been achieved using 0.5 and 1.0 gm pellets in 30 cm long barrel, without cleaning the barrel between the shots

  1. Dynamic response modelling and characterization of a vertical electrothermal actuator

    International Nuclear Information System (INIS)

    Li, Lijie; Uttamchandani, Deepak

    2009-01-01

    Mathematical modelling and characterization of the dynamic response of a microelectromechanical system (MEMS) electrothermal actuator are presented in this paper. The mathematical model is based on a second-order partial differential equation (one-dimensional heat transfer) and a second-order ordinary differential equation (mechanical dynamic equation). The simulations are implemented using the piecewise finite difference method and the Runge–Kutta algorithm. The electrothermal modelling includes thermal conduction, convective thermal loss and radiation effects. The temperature dependence of resistivity and thermal conductivity of single crystal silicon have also been taken into consideration in the electrothermal modelling. It is calculated from the simulation results that the 'cold' beam of the electrothermal actuator is not only a mechanical constraint but also a thermal response compensation structure. The 0–90% electrothermal rise times for the individual 'hot' and 'cold' beams are calculated to be 32.9 ms and 42.8 ms, respectively, while the 0–90% electrothermal rise time for the whole actuator is calculated to be 17.3 ms. Nonlinear cubic stiffness has been considered in the thermal-mechanical modelling. Dynamic performances of the device have been characterized using a laser vibrometer, and the 0–90% thermal response time of the whole structure has been measured to be 16.8 ms, which matches well with the modelling results. The displacements of the device under different driving conditions and at resonant frequency have been modelled and measured, and the results from both modelling and experiment agree reasonably well. This work provides a comprehensive understanding of the dynamic behaviour of the electrothermal actuation mechanism. The model will be useful for designing control systems for microelectrothermal actuated devices

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

    Science.gov (United States)

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

    1996-02-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  4. Electrothermally actuated tunable clamped-guided resonant microbeams

    Science.gov (United States)

    Alcheikh, N.; Hajjaj, A. Z.; Jaber, N.; Younis, M. I.

    2018-01-01

    We present simulation and experimental investigation demonstrating active alteration of the resonant and frequency response behavior of resonators by controlling the electrothermal actuation method on their anchors. In-plane clamped-guided arch and straight microbeams resonators are designed and fabricated with V-shaped electrothermal actuators on their anchors. These anchors not only offer various electrothermal actuation options, but also serve as various mechanical stiffness elements that affect the operating resonance frequency of the structures. We have shown that for an arch, the first mode resonance frequency can be increased up to 50% of its initial value. For a straight beam, we have shown that before buckling, the resonance frequency decreases to very low values and after buckling, it increases up to twice of its initial value. These results can be promising for the realization of different wide-range tunable microresonator. The experimental results have been compared to multi-physics finite-element simulations showing good agreement among them.

  5. Electrothermally actuated tunable clamped-guided resonant microbeams

    KAUST Repository

    Alcheikh, Nouha

    2017-06-11

    We present simulation and experimental investigation demonstrating active alteration of the resonant and frequency response behavior of resonators by controlling the electrothermal actuation method on their anchors. In-plane clamped-guided arch and straight microbeams resonators are designed and fabricated with V-shaped electrothermal actuators on their anchors. These anchors not only offer various electrothermal actuation options, but also serve as various mechanical stiffness elements that affect the operating resonance frequency of the structures. We have shown that for an arch, the first mode resonance frequency can be increased up to 50% of its initial value. For a straight beam, we have shown that before buckling, the resonance frequency decreases to very low values and after buckling, it increases up to twice of its initial value. These results can be promising for the realization of different wide–range tunable microresonator. The experimental results have been compared to multi-physics finite-element simulations showing good agreement among them.

  6. Uranium determination using atomic spectrometric techniques: An overview

    International Nuclear Information System (INIS)

    Santos, Juracir S.; Teixeira, Leonardo S.G.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Godoy, Jose M.; Ferreira, Sergio L.C.

    2010-01-01

    This review focuses on the determination of uranium using spectroanalytical techniques that are aimed at total determination such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), inductively coupled plasma optical emission spectrometry (ICP-OES); and inductively coupled plasma mass spectrometry (ICP-MS) that also enables the determination of uranium isotopes. The advantages and shortcomings related to interferences, precision, accuracy, sample type and equipment employed in the analysis are taken into account, as well as the complexity and costs (i.e., acquisition, operation and maintenance) associated with each of the techniques. Strategies to improve their performance that employ separation and/or preconcentration steps are considered, with an emphasis given to solid-phase extraction because of its advantages compared to other preconcentration procedures.

  7. L-tyrosine immobilized on multiwalled carbon nanotubes: a new substrate for thallium separation and speciation using stabilized temperature platform furnace-electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Pacheco, Pablo H; Gil, Raúl A; Smichowski, Patricia; Polla, Griselda; Martinez, Luis D

    2009-12-10

    An approach for the separation and determination of inorganic thallium species is described. A new sorbent, L-tyrosine-carbon nanotubes (L-tyr-CNTs), was used and applied to the analysis of tap water samples. At pH 5.0, L-tyr was selective only towards Tl(III), while total thallium was determined directly by stabilized temperature platform furnace-electrothermal atomic absorption spectrometry (STPF-ETAAS). The Tl(III) specie, which was retained by L-tyrosine, was quantitatively eluted from the column with 10% of nitric acid. An on-line breakthrough curve was used to determine the column capacity, which resulted to be 9.00 micromol of Tl(III) g(-1) of L-tyr-CNTs with a molar ratio of 0.14 (moles of Tl bound to moles of L-tyr at pH 5). Transient peak areas revealed that Tl stripping from the column occurred instantaneously. Effects of sample flow rate, concentration and flow rate of the eluent, and interfering ions on the recovery of the analyte were systematically investigated. The detection limit for the determination of total thallium (3sigma) by STPF-ETAAS was 150 ng L(-1). The detection limit (3sigma) for Tl(III) employing the separation system was 3 ng L(-1), with an enrichment factor of 40. The precision of the method expressed as the relative standard deviation (RSD) resulted to be 3.4%. The proposed method was applied to the speciation and determination of inorganic thallium in tap water samples. The found concentrations were in the range of 0.88-0.91 microg L(-1) of Tl(III), and 3.69-3.91 microg L(-1) of total thallium.

  8. L-Tyrosine immobilized on multiwalled carbon nanotubes: A new substrate for thallium separation and speciation using stabilized temperature platform furnace-electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Pacheco, Pablo H.; Gil, Raul A.; Smichowski, Patricia; Polla, Griselda; Martinez, Luis D.

    2009-01-01

    An approach for the separation and determination of inorganic thallium species is described. A new sorbent, L-tyrosine-carbon nanotubes (L-tyr-CNTs), was used and applied to the analysis of tap water samples. At pH 5.0, L-tyr was selective only towards Tl(III), while total thallium was determined directly by stabilized temperature platform furnace-electrothermal atomic absorption spectrometry (STPF-ETAAS). The Tl(III) specie, which was retained by L-tyrosine, was quantitatively eluted from the column with 10% of nitric acid. An on-line breakthrough curve was used to determine the column capacity, which resulted to be 9.00 μmol of Tl(III) g -1 of L-tyr-CNTs with a molar ratio of 0.14 (moles of Tl bound to moles of L-tyr at pH 5). Transient peak areas revealed that Tl stripping from the column occurred instantaneously. Effects of sample flow rate, concentration and flow rate of the eluent, and interfering ions on the recovery of the analyte were systematically investigated. The detection limit for the determination of total thallium (3σ) by STPF-ETAAS was 150 ng L -1 . The detection limit (3σ) for Tl(III) employing the separation system was 3 ng L -1 , with an enrichment factor of 40. The precision of the method expressed as the relative standard deviation (RSD) resulted to be 3.4%. The proposed method was applied to the speciation and determination of inorganic thallium in tap water samples. The found concentrations were in the range of 0.88-0.91 μg L -1 of Tl(III), and 3.69-3.91 μg L -1 of total thallium.

  9. Simultaneous Multi-Element Electrothermal Atomic Absorption ...

    African Journals Online (AJOL)

    width of transmittance profile 120 pm, a linear CCD array attached to a PC and a tube atomizer furnished with a carbon fibre collector. In the experiments simultaneous determination of 18 elements was performed in the mixed solutions at the mg ...

  10. Evaluation of pyrolysis curves for volatile elements in aqueous standards and carbon-containing matrices in electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, A.F. [Delft University of Technology, Faculty of Applied Sciences, DelftChemTech, Julianalaan 136, 2628 BL Delft (Netherlands); Universidade Federal de Santa Catarina, Departamento de Quimica, 88040-900 Florianopolis, SC (Brazil); Welz, B. [Universidade Federal de Santa Catarina, Departamento de Quimica, 88040-900 Florianopolis, SC (Brazil); Loos-Vollebregt, M.T.C. de [Delft University of Technology, Faculty of Applied Sciences, DelftChemTech, Julianalaan 136, 2628 BL Delft (Netherlands)], E-mail: m.t.c.deloos-vollebregt@tudelft.nl

    2008-07-15

    Pyrolysis curves in electrothermal atomic absorption spectrometry (ET AAS) and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) have been compared for As, Se and Pb in lobster hepatopancreas certified reference material using Pd/Mg as the modifier. The ET AAS pyrolysis curves confirm that the analytes are not lost from the graphite furnace up to a pyrolysis temperature of 800 deg. C. Nevertheless, a downward slope of the pyrolysis curve was observed for these elements in the biological material using ETV-ICP-MS. This could be related to a gain of sensitivity at low pyrolysis temperatures due to the matrix, which can act as carrier and/or promote changes in the plasma ionization equilibrium. Experiments with the addition of ascorbic acid to the aqueous standards confirmed that the higher intensities obtained in ETV-ICP-MS are related to the presence of organic compounds in the slurry. Pyrolysis curves for As, Se and Pb in coal and coal fly ash were also investigated using the same Pd/Mg modifier. Carbon intensities were measured in all samples using different pyrolysis temperatures. It was observed that pyrolysis curves for the three analytes in all slurry samples were similar to the corresponding graphs that show the carbon intensity for the same slurries for pyrolysis temperatures from 200 deg. C up to 1000 deg. C.

  11. Simultaneous Multi-Element Electrothermal Atomic Absorption ...

    African Journals Online (AJOL)

    NICO

    and chemical interferences are associated with optimization of the light source and atomization programme and modification ... The following excerpts from the theory should help to estimate .... applicability of Equation (11) in practice depends on the spectral ..... The authors would like to acknowledge the National Research.

  12. Topology optimized electrothermal polysilicon microgrippers

    DEFF Research Database (Denmark)

    Sardan Sukas, Özlem; Petersen, Dirch Hjorth; Mølhave, Kristian

    2008-01-01

    This paper presents the topology optimized design procedure and fabrication of electrothermal polysilicon microgrippers for nanomanipulation purposes. Performance of the optimized microactuators is compared with a conventional three-beam microactuator design through finite element analysis...

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

    International Nuclear Information System (INIS)

    Ruiz, Frine; Benzo, Zully; Quintal, Manuelita; Garaboto, Angel; Albornoz, Alberto; Brito, Joaquin L.

    2006-01-01

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

  14. A carbon nanofibre scanning probe assembled using an electrothermal microgripper

    DEFF Research Database (Denmark)

    Carlson, Kenneth; Dyvelkov, Karin Nordström; Eicchorn, V.

    2007-01-01

    Functional devices can be directly assembled using microgrippers with an in situ electron microscope. Two simple and compact silicon microgripper designs are investigated here. These are operated by electrothermal actuation, and are used to transfer a catalytically grown multi-walled carbon...... nanofibre from a fixed position on a substrate to the tip of an atomic force microscope cantilever, inside a scanning electron microscope. Scanning of high aspect ratio trenches using the nanofibre supertip shows a significantly better performance than that with standard pyramidal silicon tips. Based...... on manipulation experiments as well as a simple analysis, we show that shear pulling (lateral movement of the gripper) is far more effective than tensile pulling (vertical movement of gripper) for the mechanical removal of carbon nanotubes from a substrate....

  15. A carbon nanofibre scanning probe assembled using an electrothermal microgripper

    International Nuclear Information System (INIS)

    Carlson, K; Andersen, K N; Eichorn, V; Petersen, D H; Moelhave, K; Bu, I Y Y; Teo, K B K; Milne, W I; Fatikow, S; Boeggild, P

    2007-01-01

    Functional devices can be directly assembled using microgrippers with an in situ electron microscope. Two simple and compact silicon microgripper designs are investigated here. These are operated by electrothermal actuation, and are used to transfer a catalytically grown multi-walled carbon nanofibre from a fixed position on a substrate to the tip of an atomic force microscope cantilever, inside a scanning electron microscope. Scanning of high aspect ratio trenches using the nanofibre supertip shows a significantly better performance than that with standard pyramidal silicon tips. Based on manipulation experiments as well as a simple analysis, we show that shear pulling (lateral movement of the gripper) is far more effective than tensile pulling (vertical movement of gripper) for the mechanical removal of carbon nanotubes from a substrate

  16. A low-power-consumption out-of-Plane electrothermal actuator

    OpenAIRE

    Girbau Sala, David; Llamas Morote, Marco Antonio; Casals Terré, Jasmina; Simó Selvas, Francisco Javier; Pradell i Cara, Lluís; Lázaro Guillén, Antoni

    2007-01-01

    This paper proposes a new vertical electrothermal actuator. It can be considered as a hybrid between the traditional in-plane buckle-beam actuator and the vertical hot-cold actuator. It is here referred to as vertical buckle beam. At identical dimensional and bias conditions, it features a displacement larger than that of other vertical electrothermal actuators proposed so far in the literature. The actuator performance is demonstrated by means of an analytical model along with finite-element...

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  18. Analytical techniques for measurement of 99Tc in environmental samples

    International Nuclear Information System (INIS)

    Anon.

    1979-01-01

    Three new methods have been developed for measuring 99 Tc in environmental samples. The most sensitive method is isotope dilution mass spectrometry, which allows measurement of about 1 x 10 -12 grams of 99 Tc. Results on analysis of five samples by this method compare very well with values obtained by a second independent method, which involves counting of beta particles from 99 Tc and internal conversion electrons from /sup 97m/Tc. A third method involving electrothermal atomic absorption has also been developed. Although this method is not as sensitive as the first two techniques, the cost per analysis is expected to be considerably less for certain types of samples

  19. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    International Nuclear Information System (INIS)

    Grijalba, Alexander Castro; Martinis, Estefanía M.; Lascalea, Gustavo E.; Wuilloud, Rodolfo G.

    2015-01-01

    A flow injection system based on a modified polytetrafluoroethylene (PTFE) knotted reactor (KR) was developed for arsenite [As(III)] and arsenate [As(V)] species preconcentration and determination by electrothermal atomic absorption spectrometry (ETAAS). Activated carbon (AC) was immobilized on the inner walls of a PTFE KR by a thermal treatment. A significant increase in analyte retention was obtained with the AC-modified KR (100%) as compared to the regular PTFE KR (25%). The preconcentration method involved the on-line formation of As(III)-ammonium pyrrolidinedithiocarbamate (As-APDC) complex, followed by its adsorption onto the inner walls of the AC-modified KR. After analyte retention, the complex was eluted with acetone directly into the graphite furnace of ETAAS. The parameters affecting the flow injection system were evaluated with a full central composite face centered design with three center points. Under optimum conditions, a preconcentration factor of 200 was obtained with 10 ml of sample. The detection limit was 4 ng L −1 and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L −1 of As were 4.3% and 4.7% for As(III) and As(V), respectively. The developed methodology was highly selective towards As(III), while As(V), monomethylarsonic acid [MMA(V)] and dimethylarsinic [DMA(V)] were not retained in the AC-modified KR. The proposed method was successfully applied for As speciation analysis in infusions originated from medicinal herbs and tea. - Highlights: • We report an efficient method for As speciation. • We have modified a knotted reactor with activated carbon for high sorption capacity. • We provide a simple procedure for surface modification of a PTFE knotted reactor. • We have selectively separated inorganic As species from complex matrix samples. • We have implemented a modified KR in a flow injection system coupled to ETAAS

  20. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Martinis, Estefanía M. [Laboratory of Analytical Chemistry for Research and Development (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo, Padre J. Contreras 1300, (5500) Mendoza (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina); Lascalea, Gustavo E. [Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Laboratory of Analytical Chemistry for Research and Development (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo, Padre J. Contreras 1300, (5500) Mendoza (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina)

    2015-01-01

    A flow injection system based on a modified polytetrafluoroethylene (PTFE) knotted reactor (KR) was developed for arsenite [As(III)] and arsenate [As(V)] species preconcentration and determination by electrothermal atomic absorption spectrometry (ETAAS). Activated carbon (AC) was immobilized on the inner walls of a PTFE KR by a thermal treatment. A significant increase in analyte retention was obtained with the AC-modified KR (100%) as compared to the regular PTFE KR (25%). The preconcentration method involved the on-line formation of As(III)-ammonium pyrrolidinedithiocarbamate (As-APDC) complex, followed by its adsorption onto the inner walls of the AC-modified KR. After analyte retention, the complex was eluted with acetone directly into the graphite furnace of ETAAS. The parameters affecting the flow injection system were evaluated with a full central composite face centered design with three center points. Under optimum conditions, a preconcentration factor of 200 was obtained with 10 ml of sample. The detection limit was 4 ng L{sup −1} and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L{sup −1} of As were 4.3% and 4.7% for As(III) and As(V), respectively. The developed methodology was highly selective towards As(III), while As(V), monomethylarsonic acid [MMA(V)] and dimethylarsinic [DMA(V)] were not retained in the AC-modified KR. The proposed method was successfully applied for As speciation analysis in infusions originated from medicinal herbs and tea. - Highlights: • We report an efficient method for As speciation. • We have modified a knotted reactor with activated carbon for high sorption capacity. • We provide a simple procedure for surface modification of a PTFE knotted reactor. • We have selectively separated inorganic As species from complex matrix samples. • We have implemented a modified KR in a flow injection system coupled to ETAAS.

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

    International Nuclear Information System (INIS)

    Ataman, O. Yavuz

    2008-01-01

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

  2. Reexamination of basal plane thermal conductivity of suspended graphene samples measured by electro-thermal micro-bridge methods

    Directory of Open Access Journals (Sweden)

    Insun Jo

    2015-05-01

    Full Text Available Thermal transport in suspended graphene samples has been measured in prior works and this work with the use of a suspended electro-thermal micro-bridge method. These measurement results are analyzed here to evaluate and eliminate the errors caused by the extrinsic thermal contact resistance. It is noted that the room-temperature thermal resistance measured in a recent work increases linearly with the suspended length of the single-layer graphene samples synthesized by chemical vapor deposition (CVD, and that such a feature does not reveal the failure of Fourier’s law despite the increase in the reported apparent thermal conductivity with length. The re-analyzed apparent thermal conductivity of a single-layer CVD graphene sample reaches about 1680 ± 180 W m−1 K−1 at room temperature, which is close to the highest value reported for highly oriented pyrolytic graphite. In comparison, the apparent thermal conductivity values measured for two suspended exfoliated bi-layer graphene samples are about 880 ± 60 and 730 ± 60 Wm−1K−1 at room temperature, and approach that of the natural graphite source above room temperature. However, the low-temperature thermal conductivities of these suspended graphene samples are still considerably lower than the graphite values, with the peak thermal conductivities shifted to much higher temperatures. Analysis of the thermal conductivity data reveals that the low temperature behavior is dominated by phonon scattering by polymer residue instead of by the lateral boundary.

  3. Development of electrothermal actuation based planar variable optical attenuators (VOAs)

    International Nuclear Information System (INIS)

    Lee, Chengkuo; Yeh, J Andrew

    2006-01-01

    Several sorts of MEMS (Microelectromechanical Systems) based have been demonstrated by using electrostatic actuation scheme up to date. The comb drive and parallel plate are the two most common electrostatic actuators that have been well studied in variable optical attenuator (VOA) applications. In addition to the known retro-reflection type of optical attenuation being realized by our new devices driven by electrothermal actuators in present study, a novel planar tilted mirror with rotational and translation moving capability is proposed by using electrothermal actuators as well. Using electrothermal actuators to provide said planar tilted mirror with rotational and translational displacement has granted us a more efficient way to perform the light attenuation for in-plane structure. The static and transient characteristics of devices operated at ambient room temperature environment show good repeatability and stability

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

    Science.gov (United States)

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

    1979-01-01

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

  5. Trends in tungsten coil atomic spectrometry

    Science.gov (United States)

    Donati, George L.

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

  6. Highly Tunable Electrothermally Actuated Arch Resonator

    KAUST Repository

    Hajjaj, Amal Z.; Ramini, Abdallah; Alcheikh, Nouha; Younis, Mohammad I.

    2016-01-01

    that after some electro-thermal voltage load, the third resonance frequency starts to become more sensitive to the axial thermal stress, while the first resonance frequency becomes less sensitive. These results can be used as guidelines to utilize arches

  7. Electrothermal Frequency Modulated Resonator for Mechanical Memory

    KAUST Repository

    Hafiz, Md Abdullah Al; Kosuru, Lakshmoji; Younis, Mohammad I.

    2016-01-01

    In this paper, we experimentally demonstrate a mechanical memory device based on the nonlinear dynamics of an electrostatically actuated microelectromechanical resonator utilizing an electrothermal frequency modulation scheme. The microstructure

  8. A Novel Electro-Thermal Laminated Ceramic with Carbon-Based Layer

    Directory of Open Access Journals (Sweden)

    Yi Ji

    2017-06-01

    Full Text Available A novel electro-thermal laminated ceramic composed of ceramic tile, carbon-based layer, dielectric layer, and foaming ceramic layer was designed and prepared by tape casting. The surface temperature achieved at an applied voltage of 10 V by the laminated ceramics was 40.3 °C when the thickness of carbon-based suspension was 1.0 mm and the adhesive strength between ceramic tile and carbon-based layer was 1.02 ± 0.06 MPa. In addition, the thermal aging results at 100 °C up to 192 h confirmed the high thermal stability and reliability of the electro-thermal laminated ceramics. The development of this laminated ceramic with excellent electro-thermal properties and safety provides a new individual heating device which is highly expected to be widely applied in the field of indoor heat supply.

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

    OpenAIRE

    2011-01-01

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

  10. Selective determination of inorganic cobalt in nutritional supplements by ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction and electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Berton, Paula; Martinis, Estefanía M.; Martinez, Luis D.; Wuilloud, Rodolfo G.

    2012-01-01

    Highlights: ► Synergy of ultrasound energy and TILDLME technique for improved metal extraction. ► Highly selective determination of inorganic Co species at trace levels. ► Speciation analysis of Co in several nutritional supplements with highly complex matrices. ► Development of an environmentally friendly microextraction technique with minimal waste production and sample consumption. - Abstract: In the present work, a simple and rapid analytical method based on application of ionic liquids (ILs) for inorganic Co(II) species (iCo) microextraction in a variety of nutrient supplements was developed. Inorganic Co was initially chelated with 1-nitroso-2-naphtol (1N2N) reagent followed by a modern technique named ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction (USA-TILDLME). The extraction was performed with 1-hexyl-3-methylimidazolium hexafluorophosphate [C 6 mim][PF 6 ] with the aid of ultrasound to improve iCo recovery. Finally, the iCo-enriched IL phase was solubilized in methanol and directly injected into an electrothermal atomic absorption spectrometer (ETAAS). Several parameters that could influence iCo microextraction and detection were carefully studied. Since the main difficulty in these samples is caused by high concentrations of potential interfering ions, different approaches were evaluated to eliminate interferences. The limit of detection (LOD) was 5.4 ng L −1 , while the relative standard deviation (RSD) was 4.7% (at 0.5 μg L −1 Co level and n = 10), calculated from the peak height of absorbance signals. Selective microextraction of iCo species was achieved only by controlling the pH value during the procedure. The method was thus successfully applied for determination of iCo species in nutritional supplements.

  11. Selective determination of inorganic cobalt in nutritional supplements by ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Berton, Paula; Martinis, Estefania M. [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Martinez, Luis D. [INQUISAL-CONICET, Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, San Luis (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

    2012-02-03

    Highlights: Black-Right-Pointing-Pointer Synergy of ultrasound energy and TILDLME technique for improved metal extraction. Black-Right-Pointing-Pointer Highly selective determination of inorganic Co species at trace levels. Black-Right-Pointing-Pointer Speciation analysis of Co in several nutritional supplements with highly complex matrices. Black-Right-Pointing-Pointer Development of an environmentally friendly microextraction technique with minimal waste production and sample consumption. - Abstract: In the present work, a simple and rapid analytical method based on application of ionic liquids (ILs) for inorganic Co(II) species (iCo) microextraction in a variety of nutrient supplements was developed. Inorganic Co was initially chelated with 1-nitroso-2-naphtol (1N2N) reagent followed by a modern technique named ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction (USA-TILDLME). The extraction was performed with 1-hexyl-3-methylimidazolium hexafluorophosphate [C{sub 6}mim][PF{sub 6}] with the aid of ultrasound to improve iCo recovery. Finally, the iCo-enriched IL phase was solubilized in methanol and directly injected into an electrothermal atomic absorption spectrometer (ETAAS). Several parameters that could influence iCo microextraction and detection were carefully studied. Since the main difficulty in these samples is caused by high concentrations of potential interfering ions, different approaches were evaluated to eliminate interferences. The limit of detection (LOD) was 5.4 ng L{sup -1}, while the relative standard deviation (RSD) was 4.7% (at 0.5 {mu}g L{sup -1} Co level and n = 10), calculated from the peak height of absorbance signals. Selective microextraction of iCo species was achieved only by controlling the pH value during the procedure. The method was thus successfully applied for determination of iCo species in nutritional supplements.

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

    International Nuclear Information System (INIS)

    Acar, Orhan

    2005-01-01

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

  13. 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

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

    Directory of Open Access Journals (Sweden)

    Oliveira Pedro V. de

    2000-01-01

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

  15. Highly Tunable Electrothermally and Electrostatically Actuated Resonators

    KAUST Repository

    Hajjaj, Amal Z.

    2016-03-30

    This paper demonstrates experimentally, theoretically, and numerically for the first time, a wide-range tunability of an in-plane clamped-clamped microbeam, bridge, and resonator actuated electrothermally and electrostatically. Using both actuation methods, we demonstrate that a single resonator can be operated at a wide range of frequencies. The microbeam is actuated electrothermally by passing a dc current through it, and electrostatically by applying a dc polarization voltage between the microbeam and the stationary electrode. We show that when increasing the electrothermal voltage, the compressive stress inside the microbeam increases, which leads eventually to its buckling. Before buckling, the fundamental frequency decreases until it drops to very low values, almost to zero. After buckling, the fundamental frequency increases, which is shown to be as high as twice the original resonance frequency. Adding a dc bias changes the qualitative nature of the tunability both before and after buckling, which adds another independent way of tuning. This reduces the dip before buckling, and can eliminate it if desired, and further increases the fundamental frequency after buckling. Analytical results based on the Galerkin discretization of the Euler Bernoulli beam theory are generated and compared with the experimental data and simulation results of a multi-physics finite-element model. A good agreement is found among all the results. [2015-0341

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-08-15

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

  17. Evaluation of some toxic metals in blood samples of smokers in ...

    African Journals Online (AJOL)

    Methods: The study setting was Riyadh, the capital city of Saudi Arabia, Riyadh City. Male volunteers, ... optical emission spectrometry [10] or ICP - mass ... The validation parameters including .... patients by electrothermal atomic absorption.

  18. Determination of Cu, Mn, Ni and Sn in gasoline by electrothermal vaporization inductively coupled plasma mass spectrometry, and emulsion sample introduction

    International Nuclear Information System (INIS)

    Saint'Pierre, Tatiana D.; Dias, Lucia Felicidade; Pozebon, Dirce; Aucelio, Ricardo Q.; Curtius, Adilson J.; Welz, Bernhard

    2002-01-01

    Trace metals in fuels, except in the case of additives, are usually undesirable and normally they occur in very low concentrations in gasoline, requiring sensitive techniques for their determination. Coupling of electrothermal vaporization with inductively coupled plasma mass spectrometry minimizes the problems related to the introduction of organic solvents into the plasma. Furthermore, sample preparation as oil-in-water emulsions reduces problems related to gasoline analysis. In this work, a method for determination of Cu, Mn, Ni and Sn in gasoline is proposed. Samples were prepared by forming a 10-fold diluted emulsion with a surfactant (Triton X-100), after treatment with concentrated HNO 3 . The sample emulsion was pre-concentrated in the graphite tube by repeated pipetting and drying. External calibration was used with aqueous standards in a purified gasoline emulsion. Six samples from different gas stations were analyzed, and the analyte concentrations were found to be in the μg l -1 range or below. The limits of detection were 0.22, 0.02, 0.38 and 0.03 μg l -1 for Cu, Mn, Ni and Sn, respectively. The accuracy of the method was estimated using a recovery test

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-02-01

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

  20. Highly Tunable Electrothermally and Electrostatically Actuated Resonators

    KAUST Repository

    Hajjaj, Amal Z.; Alcheikh, Nouha; Ramini, Abdallah; Hafiz, Md Abdullah Al; Younis, Mohammad I.

    2016-01-01

    methods, we demonstrate that a single resonator can be operated at a wide range of frequencies. The microbeam is actuated electrothermally by passing a dc current through it, and electrostatically by applying a dc polarization voltage between the microbeam

  1. An electro-thermal model and its application on a spiral-wound lithium ion battery with porous current collectors

    International Nuclear Information System (INIS)

    Ye, Yonghuang; Shi, Yixiang; Saw, Lip Huat; Tay, Andrew A.O.

    2014-01-01

    Highlights: • A local electro-thermal model is developed to verify the validity of a lump electro-thermal model. • Comparisons on edge effect of batteries with porous current collectors and batteries normal current collector foil. • Investigation on thermal performance of novel battery with porous current collector sheets. - Abstract: A local electro-thermal model for a spiral-wound lithium ion battery is developed to provide detailed and local insights of electrochemistry, transport phenomenon and heat transfer processes in spiral-wound geometries. The discharging potential, bulk heat generation rate, battery surface temperature and the temperature distribution within battery predicted by the model are used to verify a lumped electro-thermal model. The results show good agreement between the lumped electro-thermal model and the local electro-thermal model. The edge effect is investigated using the local electro-thermal model. And the results indicate that a novel battery with porous current collector sheets has a higher utilization rate of porous electrode materials than a commercial battery with normal current collector foils. The novel battery with porous current collector sheets is also investigated using the local electro-thermal model, simulation results show smaller liquid phase potential gradient and smaller liquid concentration gradient in the novel battery. The increased electrical resistance has minor effect on the overall heat generation within the battery when the porous current collector is employed, while it reduces the discharging potential of the battery

  2. Laser-Excited Atomic Fluorescence and Ionization in a Graphite Furnace for the Determination of Metals and Nonmetals

    Science.gov (United States)

    Butcher, David James

    1990-01-01

    Here is reported novel instrumentation for atomic spectrometry that combined the use of a pulsed laser system as the light source and an electrothermal atomizer as the atom cell. The main goal of the research was to develop instrumentation that was more sensitive for elemental analysis than commercially available instruments and could be used to determine elements in real sample matrices. Laser excited atomic fluorescence spectrometry (LEAFS) in an electrothermal atomizer (ETA) was compared to ETA atomic absorption spectrometry (AAS) for the determination of thallium, manganese, and lead in food and agricultural standard reference materials (SRMs). Compared to ETA AAS, ETA LEAFS has a longer linear dynamic range (LDR) (5-7 orders of magnitude compared to 2-3 orders of magnitude) and higher sensitivity (10 ^{-16} to 10^{ -14} g as compared to 10^{ -13} to 10^{-11} g). Consequently, ETA LEAFS allows elemental analysis to be done over a wider range of concentrations with less dilution steps. Thallium was accurately determined in biological samples by ETA LEAFS at amounts five to one hundred times below the ETA AAS detection limit. ETA AAS and ETA LEAFS were compared for the determination of lead and manganese, and in general, the accuracies and precisions of ETA AAS were the same, with typical precisions between 3% and 6%. Fluorine was determined using laser excited molecular fluorescence spectrometry (LEMOFS) in an ETA. Molecular fluorescence from magnesium fluoride was collected, and the detection limit of 0.3 pg fluorine was two to six orders of magnitude more sensitive than other methods commonly used for the determination of fluorine. Significant interferences from ions were observed, but the sensitivity was high enough that fluorine could be determined in freeze dried urine SRMs by diluting the samples by a factor of one hundred to remove the interferences. Laser enhanced ionization (LEI) in an ETA was used for the determination of metals. For thallium, indium

  3. An electrothermal chemical technology for thermal spray coatings

    International Nuclear Information System (INIS)

    Wald, S.; Appelbaum, G.; Alimi, R.; Rabani, L.; Zoler, D.; Zhitomirsky, V.; Factor, M.; Roman, I.

    1998-01-01

    A new spray technology for producing hard-coatings, has been developed at the SOREQ Nuclear Research Center. The concept is based on the extensive experience accumulated at SOREQ in the course of the development of Electrothermal (ET), Electrothermal-Chemical (ETC) and Solid-Propellant Electrothermal-Chemical (SPETC) guns(r). High quality coatings may be obtained by thermal spraying powder particles onto a variety of substrates. Mature state-of-the-art technologies such as plasma spray, high velocity oxy fuel (HVOF) and detonation gun (D-Gun) are widely used for many applications. As each method has its own drawbacks there is a need for a combination of several parameters which cannot be achieved by any existing individual commercial technology. The method presented is oriented toward a high-quality, multi-step, high-throughput, easily programmable continuous coating process and relatively inexpensive technology. The combustion products of a solid or liquid propellant accelerate the powder particles of the coating material. A pulsed-plasma jet, provided by a confined capillary discharge, ignites the propellant and controls the combustion process. The powder particles are accelerated to velocities over 1000 m/s. Due to the very high carrier gas density, high velocity, high throughput and high powder consumption efficiency are obtained. The plasma jet enables control of the gas temperature and consequently influences the powder temperature

  4. Multimodal Electrothermal Silicon Microgrippers for Nanotube Manipulation

    DEFF Research Database (Denmark)

    Nordström Andersen, Karin; Petersen, Dirch Hjorth; Carlson, Kenneth

    2009-01-01

    Microgrippers that are able to manipulate nanoobjects reproducibly are key components in 3-D nanomanipulation systems. We present here a monolithic electrothermal microgripper prepared by silicon microfabrication, and demonstrate pick-and-place of an as-grown carbon nanotube from a 2-D array onto...

  5. Electrothermally-Actuated Micromirrors with Bimorph Actuators—Bending-Type and Torsion-Type

    Directory of Open Access Journals (Sweden)

    Cheng-Hua Tsai

    2015-06-01

    Full Text Available Three different electrothermally-actuated MEMS micromirrors with Cr/Au-Si bimorph actuators are proposed. The devices are fabricated with the SOIMUMPs process developed by MEMSCAP, Inc. (Durham, NC, USA. A silicon-on-insulator MEMS process has been employed for the fabrication of these micromirrors. Electrothermal actuation has achieved a large angular movement in the micromirrors. Application of an external electric current 0.04 A to the bending-type, restricted-torsion-type, and free-torsion-type mirrors achieved rotation angles of 1.69°, 3.28°, and 3.64°, respectively.

  6. In-situ water vaporization improves bitumen production during electrothermal processes

    Energy Technology Data Exchange (ETDEWEB)

    Wang, J. [Calgary Univ., AB (Canada); McGee, B. [E-T Energy, Calgary, AB (Canada); Kantzas, A. [Calgary Univ., AB (Canada). Tomographic Imaging and Porous Media Laboratory

    2008-10-15

    Electro-thermal processes are now being considered as an alternative or complementary process to steam injection processes. This study used an in situ vaporized water process to optimize electrothermal processes for steam injection enhanced oil recovery (EOR). A simulation tool was used to model electro-thermal processes in an Athabasca oil sands reservoir. Incremental oil recovery was estimated based on a 3-block conceptual model. A field scale model was then used to investigate the effects of electrode spacing, water injection rates, and electrical heating rates on bitumen recovery. Results of the simulation studies were then analyzed using a statistical tool in order to determine optimal conditions for maximizing bitumen production. Results of the study showed that incremental recovery using the water vaporization technique resulted in oil recovery rates of 25 per cent original oil in place (OOIP). Sensitivity analyses showed that medium electrical heating rates, low water injection rates, and small spacings between electrodes maximized bitumen production rates. It was concluded that the technique can be used alone or combined with other methods to economically produce bitumens. 2 refs., 7 tabs., 9 figs.

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

    Directory of Open Access Journals (Sweden)

    Acar, Orhan

    2012-10-01

    Full Text Available The Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS using an Sc + Ir + NH4H2PO4 chemical modifier mixture and flame atomic absorption spectrometer (FAAS after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 μg L–1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH4H2PO4 mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compared with international and national food quality guidelines as well as with literature values.

    Se han determinado los metales Cd, Cu, Pb, Fe y Zn en aceites vegetales comestibles (soja, girasol, flores, nueces, maíz y aceite de oliva y aceitunas (aceitunas-1, negra, verde, negra machacadas con semillas y verde machacadas con semillas mediante espectrometría de absorción atómica electrotérmica (ETAAS utilizando como modificador químico la mezcla Sc + Ir + NH4H2PO4 y mediante espectrometría de absorción atómica de llama (FAAS tras digestión con microondas. Se estudiaron las temperaturas de pirólisis y atomización para Cd

  8. Highly selective micro-sequential injection lab-on-valve (muSI-LOV) method for the determination of ultra-trace concentrations of nickel in saline matrices using detection by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

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

    2006-10-01

    A highly selective procedure is proposed for the determination of ultra-trace level concentrations of nickel in saline aqueous matrices exploiting a micro-sequential injection Lab-On-Valve (muSI-LOV) sample pretreatment protocol comprising bead injection separation/pre-concentration and detection by electrothermal atomic absorption spectrometry (ETAAS). Based on the dimethylglyoxime (DMG) reaction used for nickel analysis, the sample, as contained in a pH 9.0 buffer, is, after on-line merging with the chelating reagent, transported to a reaction coil attached to one of the external ports of the LOV to assure sufficient reaction time for the formation of Ni(DMG)(2) chelate. The non-ionic coordination compound is then collected in a renewable micro-column packed with a reversed-phase copolymeric sorbent [namely, poly(divinylbenzene-co-N-vinylpyrrolidone)] containing a balanced ratio of hydrophilic and lipophilic monomers. Following elution by a 50-muL methanol plug in an air-segmented modality, the nickel is finally quantified by ETAAS. Under the optimized conditions and for a sample volume of 1.8 mL, a retention efficiency of 70 % and an enrichment factor of 25 were obtained. The proposed methodology showed a high tolerance to the commonly encountered alkaline earth matrix elements in environmental waters, that is, calcium and magnesium, and was successfully applied for the determination of nickel in an NIST standard reference material (NIST 1640-Trace elements in natural water), household tap water of high hardness and local seawater. Satisfying recoveries were achieved for all spiked environmental water samples with maximum deviations of 6 %. The experimental results for the standard reference material were not statistically different to the certified value at a significance level of 0.05.

  9. Impurity effects in the electrothermal instability

    International Nuclear Information System (INIS)

    Tomimura, A.; Azevedo, M.T. de

    1982-01-01

    A 'impure' plasma model is proposed based on the homogeneous hydrogen plasma used in the theory formulated by Tomimura and Haines to explain the electrothermal instable mode growth with the wave vector perpendicular to the applied magnetic field. The impurities are introduced implicitly in the transport coefficients of the two-fluid model through a effective charge number Z sub(eff). (Author) [pt

  10. Selenium speciation using capillary electrophoresis coupled with modified electrothermal atomic absorption spectrometry after selective extraction with 5-sulfosalicylic acid functionalized magnetic nanoparticles.

    Science.gov (United States)

    Yan, Lizhen; Deng, Biyang; Shen, Caiying; Long, Chanjuan; Deng, Qiufen; Tao, Chunyao

    2015-05-22

    A new method for selenium speciation in fermented bean curd wastewater and juice was described. This method involved sample extraction with 5-sulfosalicylic acid (SSA)-functionalized silica-coated magnetic nanoparticles (SMNPs), capillary electrophoresis (CE) separation, and online detection with a modified electrothermal atomic absorption spectrometry (ETAAS) system. The modified interface for ETAAS allowed for the introduction of CE effluent directly through the end of the graphite tube. Elimination of the upper injection hole of the graphite tube reduced the loss of the anlayte and enhanced the detection sensitivity. The SSA-SMNPs were synthesized and used to extract trace amounts of selenite [Se(IV)], selenite [Se(VI)], selenomethionine (SeMet), and selenocystine (SeCys2) from dilute samples. The concentration enrichment factors for Se(VI), Se(IV), SeMet, and SeCys2 were 21, 29, 18, and 12, respectively, using the SSA-SMNPs extraction. The limits of detection for Se(VI), Se(IV), SeMet, and SeCys2 were 0.18, 0.17, 0.54, 0.49ngmL(-1), respectively. The RSD values (n=6) of method for intraday were observed between 0.7% and 2.9%. The RSD values of method for interday were less than 3.5%. The linear range of Se(VI) and Se(IV) were in the range of 0.5-200ngmL(-1), and the linear ranges of SeMet and SeCys2 were 2-500 and 2-1000ngmL(-1), respectively. The detection limits of this method were improved by 10 times due to the enrichment by the SSA-SMNP extraction. The contents of Se(VI) and Se(IV) in fermented bean curd wastewater were measured as 3.83 and 2.62ngmL(-1), respectively. The contents of Se(VI), Se(IV), SeMet, and SeCys2 in fermented bean curd juice were determined as 6.39, 4.08, 2.77, and 4.00ngmL(-1), respectively. The recoveries were in the range of 99.14-104.5% and the RSDs (n=6) of recoveries between 0.82% and 3.5%. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. A Combined Electro-Thermal Breakdown Model for Oil-Impregnated Paper

    Directory of Open Access Journals (Sweden)

    Meng Huang

    2017-12-01

    Full Text Available The breakdown property of oil-impregnated paper is a key factor for converter transformer design and operation, but it is not well understood. In this paper, breakdown voltages of oil-impregnated paper were measured at different temperatures. The results showed that with the increase of temperature, electrical, electro-thermal and thermal breakdown occurred successively. An electro-thermal breakdown model was proposed based on the heat equilibrium and space charge transport, and negative differential mobility was introduced to the model. It was shown that carrier mobility determined whether it was electrical or thermal breakdown, and the model can effectively explain the temperature-dependent breakdown.

  12. Arsenic speciation in environmental samples by hydride generation and electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Anawar, Hossain Md

    2012-01-15

    For the past few years many studies have been performed to determine arsenic (As) speciation in drinking water, food chain and other environmental samples due to its well-recognized carcinogenic and toxic effects relating to its chemical forms and oxidation states. This review provides an overview of analytical methods, preconcentration and separation techniques, developed up to now, using HGAAS and ETAAS for the determination of inorganic As and organoarsenic species in environmental samples. Specific advantages, disadvantages, selectivity, sensitivity, efficiency, rapidity, detection limit (DL), and some aspects of recent improvements and modifications for different analytical and separation techniques, that can define their application for a particular sample analysis, are highlighted. HG-AAS has high sensitivity, selectivity and low DL using suitable separation techniques; and it is a more suitable, affordable and much less expensive technique than other detectors. The concentrations of HCl and NaBH(4) have a critical effect on the HG response of As species. Use of l-cysteine as pre-reductant is advantageous over KI to obtain the same signal response for different As species under the same, optimum and mild acid concentration, and to reduce the interference of transition metals on the arsine generation. Use of different pretreatment, digestion, separation techniques and surfactants can determine As species with DL from ngL(-1) to μgL(-1). Out of all the chromatographic techniques coupled with HGAAS/ETAAS, ion-pair reversed-phase chromatography (IP-RP) is the most popular due to its higher separation efficiency, resolution selectivity, simplicity, and ability to separate up to seven As species for both non-ionic and ionic compounds in a signal run using the same column and short time. However, a combination of anion- and cation-exchange chromatography seems the most promising for complete resolution up to eight As species. The ETAAS method using different

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  14. Experimental Studies of Electrothermal Plasma Gun

    International Nuclear Information System (INIS)

    Diab, F.B.A.

    2013-01-01

    The aim of the present work is to study the capillary plasma discharge dynamics and characteristics. The capillary plasma device is a new technology for producing high density plasma after ablating the capillary wall using a pulsed electric power. An Electrothermal Plasma Gun (ETG) is composed of a capillary discharge tube made of Teflon operated with simple RLC circuit. The device called Electrothermal Gun (ETG) which is composed of 4 capacitors (70 μF, 10 kV, 1.28 μH) connected in parallel to a plasma source by means of one high power supply. The gun was operated in open air at discharge energies between 35 J - 3.5 kJ according to charging voltage. The work presented in this thesis covers the following items, 1- Measurements of the basic parameters and characterizations of the pretest results of the electrical circuits and capillary plasma discharge using Rogowski coil, voltage probe and Photomultiplier. 2- Material processing including (physics of the surface modifications, the morphology of the surface by using Scanning Electron Microscope (SEM) at different conditions, compositions of the materials by using X-ray Fluorescence (XRF), Micro hardness test and material particle deposition.

  15. Electrothermal Desorption of CWA Simulants from Activated Carbon Cloth

    National Research Council Canada - National Science Library

    Sullivan, Patrick D; Wander, Joseph D; Newsome, Kolin C

    2006-01-01

    The use of activated carbon fabrics (ACFs) that are desorbed electrothermally, also known as the Joule effect, is explored as a potential method to create a regenerating chemical warfare agent (CWA) filter...

  16. Experimental electro-thermal method for nondestructively testing welds in stainless steel pipes

    International Nuclear Information System (INIS)

    Green, D.R.

    1979-01-01

    Welds in austenitic stainless steel pipes are notoriously difficult to nondestructively examine using conventional ultrasonic and eddy current methods. Survace irregularities and microscopic variations in magnetic permeability cause false eddy current signal variations. Ultrasonic methods have been developed which use computer processing of the data to overcome some of the problems. Electro-thermal nondestructive testing shows promise for detecting flaws that are difficult to detect using other NDT methods. Results of a project completed to develop and demonstrate the potential of an electro-thermal method for nondestructively testing stainless steel pipe welds are presented. Electro-thermal NDT uses a brief pulse of electrical current injected into the pipe. Defects at any depth within the weld cause small differences in surface electrical current distribution. These cause short-lived transient temperature differences on the pipe's surface that are mapped using an infrared scanning camera. Localized microstructural differences and normal surface roughness in the welds have little effect on the surface temperatures

  17. Multielement methods of atomic fluorescence analysis of enviromental samples

    International Nuclear Information System (INIS)

    Rigin, V.I.

    1985-01-01

    A multielement method of atomic fluorescence analysis of environmental samples based on sample decomposition by autoclave fluorination and gas-phase atomization of volatile compounds in inductive araon plasma using a nondispersive polychromator is suggested. Detection limits of some elements (Be, Sr, Cd, V, Mo, Te, Ru etc.) for different sample forms introduced in to an analyzer are given

  18. A simple optimized microwave digestion method for multielement monitoring in mussel samples

    International Nuclear Information System (INIS)

    Saavedra, Y.; Gonzalez, A.; Fernandez, P.; Blanco, J.

    2004-01-01

    With the aim of obtaining a set of common decomposition conditions allowing the determination of several metals in mussel tissue (Hg by cold vapour atomic absorption spectrometry; Cu and Zn by flame atomic absorption spectrometry; and Cd, PbCr, Ni, As and Ag by electrothermal atomic absorption spectrometry), a factorial experiment was carried out using as factors the sample weight, digestion time and acid addition. It was found that the optimal conditions were 0.5 g of freeze-dried and triturated samples with 6 ml of nitric acid and subjected to microwave heating for 20 min at 180 psi. This pre-treatment, using only one step and one oxidative reagent, was suitable to determine the nine metals studied with no subsequent handling of the digest. It was possible to carry out the determination of atomic absorption using calibrations with aqueous standards and matrix modifiers for cadmium, lead, chromium, arsenic and silver. The accuracy of the procedure was checked using oyster tissue (SRM 1566b) and mussel tissue (CRM 278R) certified reference materials. The method is now used routinely to monitor these metals in wild and cultivated mussels, and found to be good

  19. Parallel-beams/lever electrothermal out-of-plane actuator

    NARCIS (Netherlands)

    Deladi, S.; Krijnen, Gijsbertus J.M.; Elwenspoek, Michael Curt

    2004-01-01

    We report on the design, modeling, fabrication and testing of a powerful electrothermal actuator allowing for various modes of movement and exhibiting forces large enough to be usable in a micro-tribotester. The performance of the actuator has been simulated combining numerical and analytical

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

    International Nuclear Information System (INIS)

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

    1981-01-01

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

  1. Effect of nitric acid for equal stabilization and sensitivity of different selenium species in electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-08-15

    Determination of selenium by electrothermal atomic absorption spectrometry (ETAAS) is complicated by the presence of different species of this analyte. The presence of different oxidation states (-II, IV and VI) may result in different sensitivities obtained for each species rendering impossible the use of a single species for calibration. These species also exhibit different behaviours regarding thermal stabilities; the temperature program must be provided to conform to this problem. Chemical modifiers are commonly used for thermal stabilization of selenium species. In this study, experiments were carried out to demonstrate the effect of nitric acid in the presence of chemical modifiers. Nickel and palladium + magnesium were selected as the most commonly used chemical modifiers. Using both aqueous and human serum solutions it has been demonstrated that although chemical modifiers provide thermal stabilization of species so that higher ashing temperatures can be used, equal sensitivities cannot be achieved unless nitric acid is also present. Selenite, selenate, selenomethionine and selenocystine were used in experiments. When equal sensitivities for all these species are achieved, determination of total selenium by ETAAS can be performed by using a single species as the standard; selenite was used in this study. Precision was 5.0% or better using peak height signals. There was no significant difference in detection limits (3s) when Ni or Pd + Mg(NO{sub 3}){sub 2} was used as chemical modifier; 37 and 35 pg of selenium were found to be the detection limits for Ni and Pd + Mg(NO{sub 3}){sub 2} chemical modifiers, respectively. For chemical modifications, either 5 {mu}g of Ni or 0.5 {mu}g of Pd and 5 {mu}g of Mg(NO{sub 3}){sub 2} were used; final solutions contained 2.5% HNO{sub 3}. In serum analyses, 10 {mu}g of Ni was used in presence of 2.5% HNO{sub 3}.

  2. Analytical characteristics of a continuum-source tungsten coil atomic absorption spectrometer.

    Science.gov (United States)

    Rust, Jennifer A; Nóbrega, Joaquim A; Calloway, Clifton P; Jones, Bradley T

    2005-08-01

    A continuum-source tungsten coil electrothermal atomic absorption spectrometer has been assembled, evaluated, and employed in four different applications. The instrument consists of a xenon arc lamp light source, a tungsten coil atomizer, a Czerny-Turner high resolution monochromator, and a linear photodiode array detector. This instrument provides simultaneous multi-element analyses across a 4 nm spectral window with a resolution of 0.024 nm. Such a device might be useful in many different types of analyses. To demonstrate this broad appeal, four very different applications have been evaluated. First of all, the temperature of the gas phase was measured during the atomization cycle of the tungsten coil, using tin as a thermometric element. Secondly, a summation approach for two absorption lines for aluminum falling within the same spectral window (305.5-309.5 nm) was evaluated. This approach improves the sensitivity without requiring any additional preconcentration steps. The third application describes a background subtraction technique, as it is applied to the analysis of an oil emulsion sample. Finally, interference effects caused by Na on the atomization of Pb were studied. The simultaneous measurements of Pb and Na suggests that negative interference arises at least partially from competition between Pb and Na atoms for H2 in the gas phase.

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

    Science.gov (United States)

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

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-01-01

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

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

    Science.gov (United States)

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

    2000-12-01

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

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

    Czech Academy of Sciences Publication Activity Database

    Šíma, Jan; Rychlovský, P.

    2003-01-01

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

  7. Electrothermal efficiency, temperature and thermal conductivity

    Indian Academy of Sciences (India)

    A study was made to evaluate the electrothermal efficiency of a DC arc plasma torch and temperature and thermal conductivity of plasma jet in the torch. The torch was operated at power levels from 4 to 20 kW in non-transferred arc mode. The effect of nitrogen in combination with argon as plasma gas on the above ...

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  9. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    Science.gov (United States)

    Huang, Shih-Yi; Jiang, Shiuh-Jen; Sahayam, A. C.

    2014-11-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min- 1 methane (CH4) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g- 1 for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g- 1 (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions.

  10. Matrix modification with silver for the electrothermal atomization of arsenic and selenium

    Science.gov (United States)

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

    1981-01-01

    Silver as a matrix modifier is shown to improve the carbon-rod atomization of both arsenic and selenium for atomic absorption spectrometry. Compared to nickel, the efficiency of silver is greater for arsenic and about the same for selenium. Silver fulfils two functions in its reaction, namely stabilization during the ashing stage and enhancement of absorbance in the final atomization. ?? 1981.

  11. Electrothermal Behavior of High-Frequency Silicon-On-Glass Transistors

    NARCIS (Netherlands)

    Nenadovic, N.

    2004-01-01

    In this thesis, research is focused on the investigation of electrothermal effects in high-speed silicon transistors. At high current levels the power dissipation in these devices can lead to heating of both the device itself and the adjacent devices. In advanced transistors these effects are

  12. Exploiting the bead-injection approach in the integrated sequential injection Lab-on-Valve format using hydrophobic packing materials for on-line matrix removal and preconcentration of trace levels of cadmium in environmental and biological samples via formation of non-charged chelates prior

    DEFF Research Database (Denmark)

    Miró, Manuel; Jonczyk, Sylwia; Wang, Jianhua

    2003-01-01

    The concept of renewable microcolumns within the conduits of an automated single injection lab-on-valve system was exploited in a sorption/elution fashion using sorbents of hydrophobic nature. The scheme's practical applicability was demonstrated for the electrothermal atomic absorption spectrome......The concept of renewable microcolumns within the conduits of an automated single injection lab-on-valve system was exploited in a sorption/elution fashion using sorbents of hydrophobic nature. The scheme's practical applicability was demonstrated for the electrothermal atomic absorption...

  13. The electrical Discharge Characteristics of the 3.5 KJ Electrothermal Plasma Gun Experiment

    International Nuclear Information System (INIS)

    Diab, F.; El-Aragi, G.M.; El-Kashef, G.M.; Saudy, A.H.

    2013-01-01

    In order to better understand the operating characteristics of an electrothermal plasma gun and its design, a variety of operation characteristics including ( the length of the capillary, applied voltage, diameter of the capillary tube, circuit inductance) were investigated to determine performance effects and viability in a real system. An Electrothermal Plasma Gun (ETG) is composed of a capillary discharge tube made of Teflon operated with simple RLC circuit. The device called Electrothermal Gun (ETG) which is composed of 4 capacitors (70 μF, 10 kV, 1.3 μH) connected in parallel to a plasma source by means of one high power plane transmission line by mean of a switch triggered by negative pulse 360/385 V. For the present studies a simple RLC was chosen, which allowed the circuit parameters to be easily measure d. The electrothermal discharge characteristics of the plasma gun operated in open air, So that at atmospheric pressure the main parameters were measured. The gun voltage and discharge current are measured with voltage divider and Rogowiski coil respectively. From the results recorded we found that, the current lagged the voltage i-e the plasma source has an inductive reactivity. Moreover, the current value was changed by changing the circuit parameters, including the discharge voltage and circuit inductance, and the wire properties such as the length and diameter. The maximum gun current ranged between (5 - 50 KA) according to the charging voltage of capacitors between (1-7 KV), a typical discharge times are on the order r of 125 μS.

  14. Nanostructured carbon materials based electrothermal air pump actuators

    Science.gov (United States)

    Liu, Qing; Liu, Luqi; Kuang, Jun; Dai, Zhaohe; Han, Jinhua; Zhang, Zhong

    2014-05-01

    Actuator materials can directly convert different types of energy into mechanical energy. In this work, we designed and fabricated electrothermal air pump-type actuators by utilization of various nanostructured carbon materials, including single wall carbon nanotubes (SWCNTs), reduced graphene oxide (r-GO), and graphene oxide (GO)/SWCNT hybrid films as heating elements to transfer electrical stimulus into thermal energy, and finally convert it into mechanical energy. Both the actuation displacement and working temperature of the actuator films show the monotonically increasing trend with increasing driving voltage within the actuation process. Compared with common polymer nanocomposites based electrothermal actuators, our actuators exhibited better actuation performances with a low driving voltage (film actuator due to the intrinsic gas-impermeability nature of graphene platelets. In addition, the high modulus of the r-GO and GO/SWCNT films also guaranteed the large generated stress and high work density. Specifically, the generated stress and gravimetric work density of the GO/SWCNT hybrid film actuator could reach up to more than 50 MPa and 30 J kg-1, respectively, under a driving voltage of 10 V. The resulting stress value is at least two orders of magnitude higher than that of natural muscles (~0.4 MPa).Actuator materials can directly convert different types of energy into mechanical energy. In this work, we designed and fabricated electrothermal air pump-type actuators by utilization of various nanostructured carbon materials, including single wall carbon nanotubes (SWCNTs), reduced graphene oxide (r-GO), and graphene oxide (GO)/SWCNT hybrid films as heating elements to transfer electrical stimulus into thermal energy, and finally convert it into mechanical energy. Both the actuation displacement and working temperature of the actuator films show the monotonically increasing trend with increasing driving voltage within the actuation process. Compared with

  15. Application of direct solid sample analysis for the determination of chlorine in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos de Gois, Jefferson; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); Welz, Bernhard [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil); Borges, Daniel L.G., E-mail: daniel.borges@ufsc.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil)

    2015-03-01

    This work describes a methodology developed to carry out Cl determination in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry and direct solid sample analysis. The solid samples were directly weighed into graphite ‘cups’ and inserted into the graphite furnace. The RF power and the carrier gas flow rate were optimized at 1300 W and 0.7 L min{sup −1}, respectively. Calibration could be carried out using aqueous standard solutions with pre-dried modifiers (Pd + Nd or Pd + Ca) or using solid certified reference materials with the same pre-dried modifiers or without the use of modifiers. The limit of quantification was determined as 5 μg g{sup −1} under optimized conditions and the Cl concentration was determined in five certified reference materials with certified concentrations for Cl, in addition to three certified reference materials, for which certified values for Cl were unavailable; in the latter case, the results were compared with those obtained using high-resolution continuum source molecular absorption spectrometry. Good agreement at a 95% statistical confidence level was achieved between determined and certified or reference values. - Highlights: • Direct determination of chlorine in solid biological materials is described for the first time using ICP-MS. • Calibration against aqueous standards is feasible. • The method is accurate and sensitive, regardless of the composition of the solid sample.

  16. FEM assisted design and simulation of novel electrothermal actuators

    NARCIS (Netherlands)

    Deladi, S.; Krijnen, Gijsbertus J.M.; Elwenspoek, Michael Curt

    2003-01-01

    In this work the authors present the design, simulation, and experimental results of novel electrothermal actuators, such as the trimorph actuator for out-of-plane motion, the coupled in-plane actuator for in-plane motion and an actuator providing combined in- and out-of-plane motion that have been

  17. Quantitative Determination of Arsenic in Bottled Drinking Water Using Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    Maria Guţu Claudia

    2013-10-01

    Full Text Available Background: Many studies have been performed in the past few years, to determine arsenic speciation in drinking water, food chain and environment, arsenic being a well-recognized carcinogenic and toxic agent mainly in its inorganic species. The instrumental techniques used for arsenic determination, such as hydride generation atomic absorption spectrometry (HGAAS, graphite furnace atomic absorption spectrometry (GFAAS and inductively coupled plasma mass spectrometry (ICP-MS, can provide a great sensitivity only on the total amount. Objective: The aim of this study was to develop a simple and rapid method and to analyze the concentration of total inorganic arsenic in bottled drinking water. Methods: Total arsenic was determined in samples from six different types of commercially available bottled drinking water using atomic absorption spectrometry with electrothermal or hydride generation vaporisation. All drinking water samples were acidified with 0.1M nitric acid to match the acidity of the standards. Results: The method was linear within the studied range (1-5 μg/L, R = 0.9943. The quantification limits for arsenic determination were 0.48 μg/L (HGAAS and 0.03 μg/L (GFAAS. The evaluated arsenic content in drinking water was within the accepted limits provided by law. Conclusions: A simple and sensitive method for the quantification of arsenic in drinking water using atomic absorbtion spectroscopy was described, which can be further used in toxicological studies. As an additional advantage, the system is very fast, efficient and environmental friendly

  18. Dynamic behavior of ultra large graphene-based membranes using electrothermal transduction

    Science.gov (United States)

    Al-mashaal, A. K.; Wood, G. S.; Torin, A.; Mastropaolo, E.; Newton, M. J.; Cheung, R.

    2017-12-01

    This letter reports an experimental study of an electrothermal actuator made from an ultra-large graphene-based bilayer thin film with a diameter to thickness aspect ratio of ˜10 000. Suspended thin films consisting of multilayer graphene and 350-500 nm-thick Poly(methyl methacrylate) have been transferred over circular cavities with a diameter of 3.5 mm. The use of bilayer materials with different mechanical and thermal properties results in thin film structures that can be induced to vibrate mechanically under the electrothermal transduction mechanism. The dynamic response of the bilayer has been investigated electrothermally by driving the structures with a combination of alternating current and direct current actuation voltages ( Va c and Vd c) and characterizing their resonant frequencies. It has been found that the bilayer thin film structure behaves as a membrane. In addition, the actuation configurations affect not only the amplitude of vibration but also the tuning of the resonant frequency of the vibrating membranes. The existence of Joule heating-induced tension lowers the mechanical stiffness of the membrane and hence shifts the resonant frequency downwards by -108187 ppm. A resonant frequency of 3.26 kHz with a vibration amplitude of 4.34 nm has been achieved for 350 nm-thick membranes under actuation voltages of 1 V of Va c and 8 V of Vd c.

  19. Electrothermal model of choking-coils for the analysis of dc-dc converters

    Energy Technology Data Exchange (ETDEWEB)

    Gorecki, Krzysztof, E-mail: gorecki@am.gdynia.pl [Gdynia Maritime University, Department of Marine Electronics, Morska 83, Gdynia (Poland); Detka, Kalina [Pomeranian Higher School in Gdynia, Opata Hackiego 8-10, Gdynia (Poland)

    2012-09-01

    The paper concerns modelling the choking-coil for the needs of the electrothermal analysis of dc-dc converters. A new electrothermal model of the choking-coil is proposed. This model is dedicated for SPICE software and it takes into account nonlinearity of the dependences of the inductance on the current, selfheating and mutual thermal interactions between the core and the winding. The structure of this model is described in detail and its correctness is experimentally verified for the choking-coils with the ferrite and powder cores. Both the characteristics of the choking-coils and the buck converter with these choking-coils were considered. The satisfying agreement between the results of calculations and measurements is obtained.

  20. Electrothermal model of choking-coils for the analysis of dc–dc converters

    International Nuclear Information System (INIS)

    Górecki, Krzysztof; Detka, Kalina

    2012-01-01

    The paper concerns modelling the choking-coil for the needs of the electrothermal analysis of dc–dc converters. A new electrothermal model of the choking-coil is proposed. This model is dedicated for SPICE software and it takes into account nonlinearity of the dependences of the inductance on the current, selfheating and mutual thermal interactions between the core and the winding. The structure of this model is described in detail and its correctness is experimentally verified for the choking-coils with the ferrite and powder cores. Both the characteristics of the choking-coils and the buck converter with these choking-coils were considered. The satisfying agreement between the results of calculations and measurements is obtained.

  1. Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

    International Nuclear Information System (INIS)

    Cortez Diaz, Mirella del Carmen

    2002-01-01

    Heavy metals are a big source of environmental contamination and are also highly toxic to humans. Since shellfish are bio-accumulators of these metals, proper techniques for quantifying them should be available. This work aims to develop an analytical method for the quantitative determination of heavy metals in biological materials (shellfish), specifically arsenic and cadmium at the trace level, using graphite furnace atomic absorption spectrometry, for which nickel and phosphate solutions were used to modify the modifiers. Prior to the analysis, the sample was diluted with nitric acid in a DAB II pressure digestion system order to destroy the organic matter. The instrument conditions were initially set (wavelength, slit, integration peaks, graphite tube, etc.), then the work range was defined for each element and the most appropriate operational parameters were studied, such as: temperature, ramp times, hold times and internal gas flow, in the different stage of the electrothermal treatment (drying, calcination, atomization) for the furnace program. Once the above mentioned conditions were set and since this was a biological sample, a matrix chemical modifier had to be used, in order to make the elements that accompany the element being studied more volatile. In this way the chemical and spectral interferences decrease together with the high background absorption of the matrix. Therefore, different matrix modifiers were studied for the definition of each analyte. The method validation was done using Certified Oyster Tissue Reference Material N o 1566a from the National Institute of Standards and Technology applying different tests in order to eliminate outliers. Repeatability, uncertainty, sensitivity, lineal range, working range, detection limit and quantification limit were evaluated for each element, and the results were compared with the values for the certified material. The Fisher and Student tests were the statistical tools used. The experimental values

  2. Developments in the application of atomic spectroscopy to trace metal analysis

    International Nuclear Information System (INIS)

    Fuavao, V.A.

    1983-01-01

    A method is described for the determination of selenium in horse blood by generation, atomization and analysis of the selenium hydride. A pooled horse blood sample which contained 8.8 μg 1 -1 of selenium exhibited a precision of analysis of 4.32% for ten replicate analyses. A study of the sensitivity of nonresonance and resonance lines of ytterbium utilizing microboat and platform atomization was investigated. Increases of at least twofold for all nonresonance lines were observed. Microboat sensitivity fell between that of the wall and the platform. Alternative surfaces of electrothermal atomization atomic absorption spectrophotometry (ETAAS) and the thermodynamic process for atom formation in ETAAS were investigated. Sensitivities for carbide-formation elements such as ytterbium and molybdenum and other noncarbide formation elements were determined by precoating graphite tubes and inserting collars. An improvement in analytical sensitivity and reduction in memory effect compared to commercially available pyrolytic graphite tubes were observed for all except the molybdenum analyte where a depression in analytical sensitivity resulted. The useful lifetime (analysis cycles) of all surfaces (except metal collars) were recorded at 250 to 400 cycles with acceptable and comparable precisions. A method is described for proposing the thermodynamic process in IL655 ETAAS. Appearance temperatures of analytes and free energy were studied and two major pathways were found operative: 1) thermal dissociation of the analyte oxide; 2) carbon reduction of the oxide followed by atomization of the free metal

  3. The determination, by atomic-absorption spectrophotometry, of impurities in manganese dioxide

    International Nuclear Information System (INIS)

    Balaes, G.E.E.; Robert, R.V.D.

    1981-01-01

    This report describes various methods for the determination of impurities in electrolytic manganese dioxide by atomic-absorption spectrophotometry (AAS). The sample is dissolved in a mixture of acids, any residue being ignited and retreated with acid. Several AAS methods were applied so that the analysis required to meet the specifications could be attained. These involved conventional flame AAS, AAS with electrothermal atomization (ETA), hydride generation coupled with AAS, and cold-vapour AAS. Of the elements examined, copper, iron, zinc, and lead can be determined direct with confidence with or without corrections based on recoveries obtained from spiked solutions. Nickel can be determined direct by use of the method of standard additions, and copper, nickel, and lead by ETA with the method of standard additions. Arsenic and antimony are determined by hydride generation coupled with AAS, and mercury by cold-vapour AAS. The precision of analysis (relative standard deviation) is generally less than 0,050. Values were obtained for aluminium, molybdenum, magnesium, sodium, copper, chromium, and cadmium, but the accuracy of these determinations has not been fully established

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

    International Nuclear Information System (INIS)

    Li Yan; Yin Xuebo; Yan Xiuping

    2008-01-01

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

  5. New approaches to nanoparticle sample fabrication for atom probe tomography

    International Nuclear Information System (INIS)

    Felfer, P.; Li, T.; Eder, K.; Galinski, H.; Magyar, A.P.; Bell, D.C.; Smith, G.D.W.; Kruse, N.; Ringer, S.P.; Cairney, J.M.

    2015-01-01

    Due to their unique properties, nano-sized materials such as nanoparticles and nanowires are receiving considerable attention. However, little data is available about their chemical makeup at the atomic scale, especially in three dimensions (3D). Atom probe tomography is able to answer many important questions about these materials if the challenge of producing a suitable sample can be overcome. In order to achieve this, the nanomaterial needs to be positioned within the end of a tip and fixed there so the sample possesses sufficient structural integrity for analysis. Here we provide a detailed description of various techniques that have been used to position nanoparticles on substrates for atom probe analysis. In some of the approaches, this is combined with deposition techniques to incorporate the particles into a solid matrix, and focused ion beam processing is then used to fabricate atom probe samples from this composite. Using these approaches, data has been achieved from 10–20 nm core–shell nanoparticles that were extracted directly from suspension (i.e. with no chemical modification) with a resolution of better than ±1 nm. - Highlights: • Samples for APT of nanoparticles were fabricated from particle powders and dispersions. • Electrophoresis was suitable for producing samples from dispersions. • Powder lift-out was successfully producing samples from particle agglomerates. • Dispersion application/coating delivered the highest quality results.

  6. New approaches to nanoparticle sample fabrication for atom probe tomography

    Energy Technology Data Exchange (ETDEWEB)

    Felfer, P., E-mail: peter.felfer@sydney.edu.au [School for Aerospace, Mechanical and Mechatronic Engineering/Australian Centre for Microscopy and Microanalysis, The University of Sydney, NSW 2006 (Australia); Li, T. [School for Aerospace, Mechanical and Mechatronic Engineering/Australian Centre for Microscopy and Microanalysis, The University of Sydney, NSW 2006 (Australia); Materials Department, The University of Oxford, Oxford (United Kingdom); Eder, K. [School for Aerospace, Mechanical and Mechatronic Engineering/Australian Centre for Microscopy and Microanalysis, The University of Sydney, NSW 2006 (Australia); Galinski, H. [School of Engineering and Applied Sciences, Harvard University, Cambridge, MA 02138 (United States); Magyar, A.P.; Bell, D.C. [School of Engineering and Applied Sciences, Harvard University, Cambridge, MA 02138 (United States); Center for Nanoscale Systems, Harvard University, Cambridge, MA 02138 (United States); Smith, G.D.W. [Materials Department, The University of Oxford, Oxford (United Kingdom); Kruse, N. [Chemical Physics of Materials (Catalysis-Tribology), Université Libre de Bruxelles, Campus Plaine, CP 243, 1050 Brussels (Belgium); Ringer, S.P.; Cairney, J.M. [School for Aerospace, Mechanical and Mechatronic Engineering/Australian Centre for Microscopy and Microanalysis, The University of Sydney, NSW 2006 (Australia)

    2015-12-15

    Due to their unique properties, nano-sized materials such as nanoparticles and nanowires are receiving considerable attention. However, little data is available about their chemical makeup at the atomic scale, especially in three dimensions (3D). Atom probe tomography is able to answer many important questions about these materials if the challenge of producing a suitable sample can be overcome. In order to achieve this, the nanomaterial needs to be positioned within the end of a tip and fixed there so the sample possesses sufficient structural integrity for analysis. Here we provide a detailed description of various techniques that have been used to position nanoparticles on substrates for atom probe analysis. In some of the approaches, this is combined with deposition techniques to incorporate the particles into a solid matrix, and focused ion beam processing is then used to fabricate atom probe samples from this composite. Using these approaches, data has been achieved from 10–20 nm core–shell nanoparticles that were extracted directly from suspension (i.e. with no chemical modification) with a resolution of better than ±1 nm. - Highlights: • Samples for APT of nanoparticles were fabricated from particle powders and dispersions. • Electrophoresis was suitable for producing samples from dispersions. • Powder lift-out was successfully producing samples from particle agglomerates. • Dispersion application/coating delivered the highest quality results.

  7. A Fast Electro-Thermal Co-Simulation Modeling Approach for SiC Power MOSFETs

    DEFF Research Database (Denmark)

    Ceccarelli, Lorenzo; Bahman, Amir Sajjad; Iannuzzo, Francesco

    2017-01-01

    The purpose of this work is to propose a novel electro-thermal co-simulation approach for the new generation of SiC MOSFETs, by development of a PSpice-based compact and physical SiC MOSFET model including temperature dependency of several parameters and a Simulink-based thermal network. The PSpice...... the FEM simulation of the DUT’s structure, performed in ANSYS Icepack. A MATLAB script is used to process the simulation data and feed the needed settings and parameters back into the simulation. The parameters for a CREE 1.2 kV/30 A SiC MOSFET have been identified and the electro-thermal model has been...

  8. Device to investigate samples by means of flameless atomic absorption measurement

    International Nuclear Information System (INIS)

    Sperling, K.R.

    1977-01-01

    An improvement on a device to investigate samples by means of flameless atomic absorption measurement is suggested in which one aims to produce a most complete possible atomic clond from the sample to be investigated within the sample space defined by the beam bundle, through which the measuring beam bundle is passed. According to the invention, the tubular sample space should be closed by an optically penetrable window on one side. (RW) [de

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

    Science.gov (United States)

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

    2012-12-01

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

  10. Lithium-ion Battery Electrothermal Model, Parameter Estimation, and Simulation Environment

    Directory of Open Access Journals (Sweden)

    Simone Orcioni

    2017-03-01

    Full Text Available The market for lithium-ion batteries is growing exponentially. The performance of battery cells is growing due to improving production technology, but market request is growing even more rapidly. Modeling and characterization of single cells and an efficient simulation environment is fundamental for the development of an efficient battery management system. The present work is devoted to defining a novel lumped electrothermal circuit of a single battery cell, the extraction procedure of the parameters of the single cell from experiments, and a simulation environment in SystemC-WMS for the simulation of a battery pack. The electrothermal model of the cell was validated against experimental measurements obtained in a climatic chamber. The model is then used to simulate a 48-cell battery, allowing statistical variations among parameters. The different behaviors of the cells in terms of state of charge, current, voltage, or heat flow rate can be observed in the results of the simulation environment.

  11. Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Nischkauer, Winfried; Herincs, Esther; Puschenreiter, Markus; Wenzel, Walter; Limbeck, Andreas

    2013-01-01

    Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g −1 , 0.14 μg g −1 and 0.13 μg g −1 were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was investigated

  12. Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nischkauer, Winfried [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); Herincs, Esther [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Puschenreiter, Markus; Wenzel, Walter [University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Limbeck, Andreas, E-mail: A.Limbeck@tuwien.ac.at [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria)

    2013-11-01

    Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g{sup −1}, 0.14 μg g{sup −1} and 0.13 μg g{sup −1} were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was

  13. Determination of lead in water by electrothermal atomic absorption spectrometry with a nickel(II)-ammonium tartrate modifier

    International Nuclear Information System (INIS)

    Sekerka, I.; Lechner, J.F.

    1991-01-01

    A method is described for the determination of low concentrations of lead in water samples. Atomic absorption spectrometry is used with a tungsten ribbon furnace and Zeeman background correction. Interferences are eliminated by the addition of ammonium tartrate and nickel(II) nitrate to the samples to act as a matrix modifier and adjust the pH. The results show the superior performance of this modifier over other types used conventionally. The detection limit is 1 μg l -1 relative standard deviation of -1 can be obtained. The instrumentation is simple and the method is efficient for the determination of lead in various water samples. 25 refs.; 7 figs.; 6 tabs

  14. Electrode Cooling Effect on Out-Of-Phase Electrothermal Streaming in Rotating Electric Fields

    Directory of Open Access Journals (Sweden)

    Weiyu Liu

    2017-11-01

    Full Text Available In this work, we focus on investigating electrothermal flow in rotating electric fields (ROT-ETF, with primary attention paid to the horizontal traveling-wave electrothermal (TWET vortex induced at the center of the electric field. The frequency-dependent flow profiles in the microdevice are analyzed using different heat transfer models. Accordingly, we address in particular the importance of electrode cooling in ROT-ETF as metal electrodes of high thermal conductivity, while substrate material of low heat dissipation capability is employed to develop such microfluidic chips. Under this circumstance, cooling of electrode array due to external natural convection on millimeter-scale electrode pads for external wire connection occurs and makes the internal temperature maxima shift from the electrode plane to a bit of distance right above the cross-shaped interelectrode gaps, giving rise to reversal of flow rotation from a typical repulsion-type to attraction-type induction vortex, which is in good accordance with our experimental observations of co-field TWET streaming at frequencies in the order of reciprocal charge relaxation time of the bulk fluid. These results point out a way to make a correct interpretation of out-of-phase electrothermal streaming behavior, which holds great potential for handing high-conductivity analytes in modern microfluidic systems.

  15. Electrothermally Driven Fluorescence Switching by Liquid Crystal Elastomers Based On Dimensional Photonic Crystals.

    Science.gov (United States)

    Lin, Changxu; Jiang, Yin; Tao, Cheng-An; Yin, Xianpeng; Lan, Yue; Wang, Chen; Wang, Shiqiang; Liu, Xiangyang; Li, Guangtao

    2017-04-05

    In this article, the fabrication of an active organic-inorganic one-dimensional photonic crystal structure to offer electrothermal fluorescence switching is described. The film is obtained by spin-coating of liquid crystal elastomers (LCEs) and TiO 2 nanoparticles alternatively. By utilizing the property of LCEs that can change their size and shape reversibly under external thermal stimulations, the λ max of the photonic band gap of these films is tuned by voltage through electrothermal conversion. The shifted photonic band gap further changes the matching degree between the photonic band gap of the film and the emission spectrum of organic dye mounting on the film. With rhodamine B as an example, the enhancement factor of its fluorescence emission is controlled by varying the matching degree. Thus, the fluorescence intensity is actively switched by voltage applied on the system, in a fast, adjustable, and reversible manner. The control chain of using the electrothermal stimulus to adjust fluorescence intensity via controlling the photonic band gap is proved by a scanning electron microscope (SEM) and UV-vis reflectance. This mechanism also corresponded to the results from the finite-difference time-domain (FDTD) simulation. The comprehensive usage of photonic crystals and liquid crystal elastomers opened a new possibility for active optical devices.

  16. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Shih-Yi [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Jiang, Shiuh-Jen, E-mail: sjjiang@faculty.nsysu.edu.tw [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Department of Medical Laboratory Science and Biotechnology, Kaohsiung Medical University, Kaohsiung 80708, Taiwan (China); Sahayam, A.C. [National Centre for Compositional Characterisation of Materials (CCCM), Hyderabad (India)

    2014-11-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min{sup −1} methane (CH{sub 4}) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g{sup −1} for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g{sup −1} (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions. - Highlights: • Determination of Cr, Fe, Cu, Zn and Se in cereal samples • Ultrasonic slurry sampling in combination with DRC-ICP-MS • Better sensitivity with thioacetamide modifier in ETV • Decreased sample preparation time with solid sampling • Validation with NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour.

  17. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    International Nuclear Information System (INIS)

    Huang, Shih-Yi; Jiang, Shiuh-Jen; Sahayam, A.C.

    2014-01-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min −1 methane (CH 4 ) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g −1 for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g −1 (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions. - Highlights: • Determination of Cr, Fe, Cu, Zn and Se in cereal samples • Ultrasonic slurry sampling in combination with DRC-ICP-MS • Better sensitivity with thioacetamide modifier in ETV • Decreased sample preparation time with solid sampling • Validation with NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour

  18. A scalable pressure sensor based on an electrothermally and electrostatically operated resonator

    KAUST Repository

    Hajjaj, Amal Z.; Alcheikh, Nouha; Hafiz, Md Abdullah Al; Ilyas, Saad; Younis, Mohammad I.

    2017-01-01

    We present a pressure sensor based on the convective cooling of the air surrounding an electrothermally heated resonant bridge. Unlike conventional pressure sensors that rely on diaphragm deformation in response to pressure, the sensor does

  19. 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

    International Nuclear Information System (INIS)

    Queirolo, F.; Forschungszentrum Juelich GmbH; Universidad de Extremadura, Badajoz; Ostapczuk, P.; Valenta, P.; Stegen, S.; Universidad de Extremadura, Badajoz; Marin, C.; Vinagre, F.; Sanchez, A.

    1991-01-01

    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)

  20. Evaluation of sample preparation methods and optimization of nickel determination in vegetable tissues

    Directory of Open Access Journals (Sweden)

    Rodrigo Fernando dos Santos Salazar

    2011-02-01

    Full Text Available Nickel, although essential to plants, may be toxic to plants and animals. It is mainly assimilated by food ingestion. However, information about the average levels of elements (including Ni in edible vegetables from different regions is still scarce in Brazil. The objectives of this study were to: (a evaluate and optimize a method for preparation of vegetable tissue samples for Ni determination; (b optimize the analytical procedures for determination by Flame Atomic Absorption Spectrometry (FAAS and by Electrothermal Atomic Absorption (ETAAS in vegetable samples and (c determine the Ni concentration in vegetables consumed in the cities of Lorena and Taubaté in the Vale do Paraíba, State of São Paulo, Brazil. By means of the analytical technique for determination by ETAAS or FAAS, the results were validated by the test of analyte addition and recovery. The most viable method tested for quantification of this element was HClO4-HNO3 wet digestion. All samples but carrot tissue collected in Lorena contained Ni levels above the permitted by the Brazilian Ministry of Health. The most disturbing results, requiring more detailed studies, were the Ni concentrations measured in carrot samples from Taubaté, where levels were five times higher than permitted by Brazilian regulations.

  1. Nonlinear Dynamics of Cantilever-Sample Interactions in Atomic Force Microscopy

    Science.gov (United States)

    Cantrell, John H.; Cantrell, Sean A.

    2010-01-01

    The interaction of the cantilever tip of an atomic force microscope (AFM) with the sample surface is obtained by treating the cantilever and sample as independent systems coupled by a nonlinear force acting between the cantilever tip and a volume element of the sample surface. The volume element is subjected to a restoring force from the remainder of the sample that provides dynamical equilibrium for the combined systems. The model accounts for the positions on the cantilever of the cantilever tip, laser probe, and excitation force (if any) via a basis set of set of orthogonal functions that may be generalized to account for arbitrary cantilever shapes. The basis set is extended to include nonlinear cantilever modes. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a matrix iteration procedure. The effects of oscillatory excitation forces applied either to the cantilever or to the sample surface (or to both) are obtained from the solution set and applied to the to the assessment of phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) modalities. The influence of bistable cantilever modes of on AFM signal generation is discussed. The effects on the cantilever-sample surface dynamics of subsurface features embedded in the sample that are perturbed by surface-generated oscillatory excitation forces and carried to the cantilever via wave propagation are accounted by the Bolef-Miller propagating wave model. Expressions pertaining to signal generation and image contrast in A-AFM are obtained and applied to amplitude modulation (intermittent contact) atomic force microscopy and resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM). The influence of phase accumulation in A-AFM on image contrast is discussed, as is the effect of hard contact and maximum nonlinearity regimes of A-AFM operation.

  2. A Temperature-to-Digital Converter Based on an Optimized Electrothermal Filter

    NARCIS (Netherlands)

    Kashmiri, S.M.; Xia, S.; Makinwa, K.A.A.

    2009-01-01

    This paper describes the design of a CMOS temperature-to-digital converter (TDC). It operates by measuring the temperature-dependent phase shift of an electrothermal filter (ETF). Compared to previous work, this TDC employs an ETF whose layout has been optimized to minimize the thermal phase spread

  3. Dynamics of entanglement between two atomic samples with spontaneous scattering

    International Nuclear Information System (INIS)

    Di Lisi, Antonio; De Siena, Silvio; Illuminati, Fabrizio

    2004-01-01

    We investigate the effects of spontaneous scattering on the evolution of entanglement of two atomic samples, probed by phase-shift measurements on optical beams interacting with both samples. We develop a formalism of conditional quantum evolutions and present a wave function analysis implemented in numerical simulations of the state vector dynamics. This method allows us to track the evolution of entanglement and to compare it with the predictions obtained when spontaneous scattering is neglected. We provide numerical evidence that the interferometric scheme to entangle atomic samples is only marginally affected by the presence of spontaneous scattering and should thus be robust even in more realistic situations

  4. A zero-dimensional model for electrothermal-chemical launchers

    International Nuclear Information System (INIS)

    Song Shengyi; Chen Li; Sun Chengwei

    2002-01-01

    In this paper a zero-dimensional (0-D) model for the electrothermal-chemical (ETC) launchers has been established, where the propellant is an energetic work liquid. The model consists of three parts to correspond to three steps of the process in ETC launching. The results calculated with the model are well compared to the measured ones. Additionally, the dependence of chamber pressure, mass fraction of burnt propellant and muzzle velocity of projectile on capillary current has been investigated

  5. Electrothermal adsorption and desorption of volatile organic compounds on activated carbon fiber cloth

    Energy Technology Data Exchange (ETDEWEB)

    Son, H.K. [Department of Health and Environment, Kosin University, Dong Sam Dong, Young Do Gu, Busan (Korea, Republic of); Sivakumar, S., E-mail: ssivaphd@yahoo.com [Department of Bioenvironmental Energy, College of Natural Resource and Life Science, Pusan National University, Miryang-si, Gyeongsangnam-do 627-706 (Korea, Republic of); Rood, M.J. [Department of Civil and Environmental Engineering, University of Illinois, Urbana, IL (United States); Kim, B.J. [Construction Engineering Research Laboratory, U.S. Army Engineer Research and Development Center (ERDC-CERL), Champaign, IL (United States)

    2016-01-15

    Highlights: • We study the adsorption and desorption of VOCs by an activated carbon fiber cloth. • Desorption concentration was controlled via electrothermal heating. • The desorption rate was successfully equalized and controlled by this system. - Abstract: Adsorption is an effective means to selectively remove volatile organic compounds (VOCs) from industrial gas streams and is particularly of use for gas streams that exhibit highly variable daily concentrations of VOCs. Adsorption of such gas streams by activated carbon fiber cloths (ACFCs) and subsequent controlled desorption can provide gas streams of well-defined concentration that can then be more efficiently treated by biofiltration than streams exhibiting large variability in concentration. In this study, we passed VOC-containing gas through an ACFC vessel for adsorption and then desorption in a concentration-controlled manner via electrothermal heating. Set-point concentrations (40–900 ppm{sub v}) and superficial gas velocity (6.3–9.9 m/s) were controlled by a data acquisition and control system. The results of the average VOC desorption, desorption factor and VOC in-and-out ratio were calculated and compared for various gas set-point concentrations and superficial gas velocities. Our results reveal that desorption is strongly dependent on the set-point concentration and that the VOC desorption rate can be successfully equalized and controlled via an electrothermal adsorption system.

  6. A variance-reduced electrothermal Monte Carlo method for semiconductor device simulation

    Energy Technology Data Exchange (ETDEWEB)

    Muscato, Orazio; Di Stefano, Vincenza [Univ. degli Studi di Catania (Italy). Dipt. di Matematica e Informatica; Wagner, Wolfgang [Weierstrass-Institut fuer Angewandte Analysis und Stochastik (WIAS) Leibniz-Institut im Forschungsverbund Berlin e.V., Berlin (Germany)

    2012-11-01

    This paper is concerned with electron transport and heat generation in semiconductor devices. An improved version of the electrothermal Monte Carlo method is presented. This modification has better approximation properties due to reduced statistical fluctuations. The corresponding transport equations are provided and results of numerical experiments are presented.

  7. Electrothermal Feedback and Absorption-Induced Open-Circuit-Voltage Turnover in Solar Cells

    Science.gov (United States)

    Ullbrich, Sascha; Fischer, Axel; Tang, Zheng; Ávila, Jorge; Bolink, Henk J.; Reineke, Sebastian; Vandewal, Koen

    2018-05-01

    Solar panels easily heat up upon intense solar radiation due to excess energy dissipation of the absorbed photons or by nonradiative recombination of charge carriers. Still, photoinduced self-heating is often ignored when characterizing lab-sized samples. For light-intensity-dependent measurements of the open-circuit voltage (Suns-VO C ), allowing us to characterize the recombination mechanism, sample heating is often not considered, although almost 100% of the absorbed energy is converted into heat. Here, we show that the frequently observed stagnation or even decrease in VOC at increasingly high light intensities can be explained by considering an effective electrothermal feedback between the recombination current and the open-circuit voltage. Our analytical model fully explains the experimental data for various solar-cell technologies, comprising conventional inorganic semiconductors as well as organic and perovskite materials. Furthermore, the model can be exploited to determine the ideality factor, the effective gap, and the temperature rise from a single Suns-VOC measurement at ambient conditions.

  8. Rigorous Mathematical Modeling of an Adsorption System With Electrothermal Regeneration of the Used Adsorbent

    National Research Council Canada - National Science Library

    Petkovska, Menka; Antov-Bozalo, Danijela; Nikacevic, Nikola

    2006-01-01

    The general objective of the project is fundamental mathematical modeling of a complex TSA system with electrothermal desorption step, with absorbers assembled of one or more cartridge-type, radial...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-07-01

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

  10. A reduced low-temperature electro-thermal coupled model for lithium-ion batteries

    International Nuclear Information System (INIS)

    Jiang, Jiuchun; Ruan, Haijun; Sun, Bingxiang; Zhang, Weige; Gao, Wenzhong; Wang, Le Yi; Zhang, Linjing

    2016-01-01

    Highlights: • A reduced low-temperature electro-thermal coupled model is proposed. • A novel frequency-dependent equation for polarization parameters is presented. • The model is validated under different frequency and low-temperature conditions. • The reduced model exhibits a high accuracy with a low computational effort. • The adaptability of the proposed methodology for model reduction is verified. - Abstract: A low-temperature electro-thermal coupled model, which is based on the electrochemical mechanism, is developed to accurately capture both electrical and thermal behaviors of batteries. Activation energies reveal that temperature dependence of resistances is greater than that of capacitances. The influence of frequency on polarization voltage and irreversible heat is discussed, and frequency dependence of polarization resistance and capacitance is obtained. Based on the frequency-dependent equation, a reduced low-temperature electro-thermal coupled model is proposed and experimentally validated under different temperature, frequency and amplitude conditions. Simulation results exhibit good agreement with experimental data, where the maximum relative voltage error and temperature error are below 2.65% and 1.79 °C, respectively. The reduced model is demonstrated to have almost the same accuracy as the original model and require a lower computational effort. The effectiveness and adaptability of the proposed methodology for model reduction is verified using batteries with three different cathode materials from different manufacturers. The reduced model, thanks to its high accuracy and simplicity, provides a promising candidate for development of rapid internal heating and optimal charging strategies at low temperature, and for evaluation of the state of battery health in on-board battery management system.

  11. Fringe-tunable electrothermal Fresnel mirror for use in compact and high-speed diffusion sensor.

    Science.gov (United States)

    Kiuchi, Yuki; Taguchi, Yoshihiro; Nagasaka, Yuji

    2017-01-23

    This paper reports the development of an electrothermal microelectromechanical systems (MEMS) mirror with serpentine shape actuators. A micro Fresnel mirror with fringe-spacing tunability is required to realize a compact and high-speed diffusion sensor for biological samples whose diffusion coefficient changes significantly because of a conformational change. In this case, the measurement time-constant is dependent on the fringe-spacing and diffusion coefficient of the sample. In this study, a fringe-tunable MEMS mirror with an actuation voltage less than 10 V was developed. The characteristics of the fabricated mirror were investigated experimentally. A high-visibility optical interference fringe was successfully demonstrated using both an ultranarrow-linewidth solid-state laser and a low-cost compact laser diode. The experimental results demonstrated a distinct possibility of developing a measurement device using only simple and low-voltage optical components.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  13. Rigorous Mathematical Modeling of an Adsorption System With Electrothermal Regeneration of the Used Adsorbent

    National Research Council Canada - National Science Library

    Petkovska, Menka; Antov-Bozalo, Danijela; Markovic, Ana

    2005-01-01

    The general objective of the project is fundamental mathematical modeling of a complex TSA system with electrothermal desorption step, with adsorbers assembled of one or more activated carbon fiber clot (ACFC...

  14. Influence of the measurement medium and matrix modifiers on the ...

    African Journals Online (AJOL)

    An electrothermal atomic absorption (ETAAS) method has been developed for the direct determination of Si in natural waters. Measurements were carried out on previously alkalinized samples and using a mixture of Pd and Mg(NO3)2 as matrix modifier, with an ashing temperature of 1400 oC and an atomization ...

  15. Effect of electrothermal annealing on the transformation behavior of TiNi shape memory alloy and two-way shape memory spring actuated by direct electrical current

    International Nuclear Information System (INIS)

    Wang, Z.G.; Zu, X.T.; Feng, X.D.; Zhu, S.; Deng, J.; Wang, L.M.

    2004-01-01

    In this work, the effect of electrothermal annealing on the transformation characterization of TiNi shape memory alloy and the electrothermal actuating characteristics of a two-way shape memory effect (TWSME) extension spring were investigated with direct electrical current. The results showed that with increasing direct electrical current density, the B2→R-phase transformation shifts to a lower temperature and R-phase→B19' shifts to a higher temperature in the cooling process. When annealing electrical current density reached 12.2 A/mm 2 , the R-phase disappeared and austenite transformed into martensite directly. The electrothermal annealing was an effective method of heat treatment in a selected part of shape memory alloy device. The electrothermal actuating characteristics of a TWSME spring showed that the time response and the maximum elongation greatly depended on the magnitude of the electrical current

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  17. Review of research and development on the microwave-plasma electrothermal rocket

    Energy Technology Data Exchange (ETDEWEB)

    Hawley, M.C.; Asmussen, J.; Filpus, J.W.; Frasch, L.L.; Whitehair, S.

    1987-01-01

    The microwave-plasma electrothermal rocket (MWPETR) shows promise for spacecraft propulsion and maneuvering, without some of the drawbacks of competitive electric propulsion systems. In the MWPETR, the electric power is first converted to microwave-frequency radiation. In a specially-designed microwave cavity system, the electromagnetic energy of the radiation is transferred to the electrons in a plasma sustained in the working fluid. The resulting high-energy electrons transfer their energy to the atoms and molecules of the working fluid by collisions. The working fluid, thus heated, expands through a nozzle to generate thrust. In the MWPETR, no electrodes are in contact with the working fluid, the energy is transferred into the working fluid by nonthermal mechanisms, and the main requirement for the materials of construction is that the walls of the plasma chamber be insulating and transparent to microwave radiation at operating conditions. In this survey of work on the MWPETR, several experimental configurations are described and compared. Diagnostic methods used in the study are described and compared, including titration, spectroscopy, calorimetry, electric field measurements, gas-dynamic methods, and thrust measurements. Measured and estimated performance efficiencies are reported. Results of computer modeling of the plasma and of the gas flowing from the plasma are summarized. 32 references.

  18. Study of cadmium, lead and tin distribution in surface marine sediment samples from Ria de Arousa (NW of Spain)

    Energy Technology Data Exchange (ETDEWEB)

    Barciela-Alonso, M.C.; Pazos-Capeans, P.; Regueira-Miguens, M.E.; Bermejo-Barrera, A.; Bermejo-Barrera, P

    2004-10-25

    In this work a study of the Cd, Pb and Sn content in marine surface sediment from the Ria de Arousa has been realised. For this, 21 sediment samples were taken in triplicate, lyophilised and sieved, and the fraction <63 {mu}m was taken for analysis. The samples were prepared in a form of slurries and analysed by electrothermal atomic absorption spectrometry. The concentration ranges obtained were 90-990 {mu}g kg{sup -1} Cd, 26.5-91.3 {mu}g g{sup -1} Pb and 5.0-20.8 {mu}g g{sup -1} Sn. The highest concentrations of these metals are in the inner part of the Ria, near to the port and urban nucleus such as Vilagarcia or Rianxo, and decrease toward the mouth of the Ria.

  19. The role of total-reflection x-ray fluorescence in atomic spectroscopy

    International Nuclear Information System (INIS)

    Toelg, G.; Klockenkaemper, R.

    1993-01-01

    Total-reflection X-ray fluorescence (TXRF) is a universal and economic method for the simultaneous determination of elements with atomic numbers > 11 down to the lower pg-level. It is a microanalytical tool for the analysis of small sample amounts placed on flat carriers and for contaminations on flat sample surfaces. Analyses of stratified near-surface layers are made possible by varying the incident angle of the primary beam in the region of total-reflection. This non-destructive method is especially suitable for thin layers of a few nanometres, deposited on wafer material although not usable as a microprobe method with a high lateral resolution. Furthermore, depth profiles of biological samples can be recorded by means of microtome sectioning of only a few micrometres, as, for example in the gradient analysis of human organs. In addition to micro- and surface-layer analysis, TXRF is effectively applied to element trace analysis. Homogeneous solutions, for example aqueous solutions, high-purity acids or body fluids, are pipetted onto carriers and, after evaporation, the dry residues are analyzed directly down to the pg/ml region. Particularly advantageous is the absence of matrix effects, so that an easy calibration can be carried out by adding a single internal standard element. A digestion or separation step preceding the actual determination becomes necessary if a more complex matrix is to be analysed or especially low detection limits have to be reached. A critical evaluation of the recent developments in atomic spectroscopy places TXRF in a leading position. Its outstanding features compete with those of e.g. electrothermal atomic absorption spectrometry (ETAAS), microwave induced plasma optical emission spectroscopy (MIP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) in the field of micro- and trace analysis and with Rutherford backscattering (RBS) and secondary ion mass spectrometry (SIMS) in the surface-layer analysis. (author)

  20. Infrared electro-thermal NDE of stainless steel

    International Nuclear Information System (INIS)

    Green, D.R.; Hassberger, J.A.

    1975-01-01

    Electro-thermal examination, a branch of thermal testing, is a promising method being developed for nondestructive examination of stainless steel welds. This paper describes the first phase of development; i.e., preliminary demonstration and laboratory evaluation of the method's sensitivity to notches in Type 304 stainless steel plate specimens. It also includes a description of the basic principles, together with a description of the hardware and experimental results showing that electrical discharge machined notches down to 0.16 cm long x 0.08 cm deep were detected. A qualitative technique for interpreting the test results to determine whether defects are at the surface or deeper within the material is demonstrated

  1. Experimental investigation and characterization of micro resistance welding with an electro-thermal actuator

    International Nuclear Information System (INIS)

    Chang, Chun-Wei; Yeh, Cheng-Chi; Hsu Wensyang

    2009-01-01

    Resistance welding is a common scheme of assembly on the macro scale by pressing together two workpieces with current passing through them to generate joule heating at the contact region due to high contact resistance. However, micro assembly by resistance welding is seldom reported. Here, resistance welding with an electro-thermal microactuator to assemble micro Ni structures is experimentally investigated and characterized. The bent-beam electro-thermal microactuator is designed to provide the necessary displacements and pressing forces. The two-mask metal-based surface micromachining process is adopted to fabricate the micro Ni structures. The calibrated initial contact resistance is shown to decrease with increasing contact pressure. Furthermore, stronger welding strength is achieved at a smaller initial contact resistance, which indicates that a larger clamping force would enhance the welding strength as large as 3.09 MPa (74.4 µN) at a contact resistance of 2.7 Ω here. The input welding energy is also found to be a critical factor. In our tests, when welding energy is below the threshold limit of 0.05 J, the welding trials all fail. For the energy between 0.05 J and 1 J, there is a transition from a lower yield of 33.3% to a higher yield of 58.3%. At high welding energy, between 1 and 10 J, 100% yield is achieved. With the demonstration and characterization of micro resistance welding by the electro-thermal microactuator, the scheme proposed here would be helpful in the automation of micro assembly

  2. Distribution of heavy metals (Cu, Zn and Cr in groundwater from the area of a future radioactive waste repository Saligny – Romania

    Directory of Open Access Journals (Sweden)

    Tudorache A.

    2013-04-01

    Full Text Available A study of some heavy metals (Cu, Zn and Cr concentrations in natural groundwater has been conducted, by considering samples collected from the area located in the neighbourhood of Saligny village (Cernavodă, Romania. Atomic absorption spectrometry methods with thermal and electrothermal atomization has been developed, tested and used for some heavy metals content determination. The results show various concentrations of Cu, Zn and Cr in groundwater samples.

  3. Dynamic electro-thermal modeling of all-vanadium redox flow battery with forced cooling strategies

    International Nuclear Information System (INIS)

    Wei, Zhongbao; Zhao, Jiyun; Xiong, Binyu

    2014-01-01

    Highlights: • A dynamic electro-thermal model is proposed for VRB with forced cooling. • The Foster network is adopted to model the battery cooling process. • Both the electrolyte temperature and terminal voltage can be accurately predicted. • The flow rate of electrolyte and coolant significantly impact battery performance. - Abstract: The present study focuses on the dynamic electro-thermal modeling for the all-vanadium redox flow battery (VRB) with forced cooling strategies. The Foster network is adopted to dynamically model the heat dissipation of VRB with heat exchangers. The parameters of Foster network are extracted by fitting the step response of it to the results of linearized CFD model. Then a complete electro-thermal model is proposed by coupling the heat generation model, Foster network and electrical model. Results show that the established model has nearly the same accuracy with the nonlinear CFD model in electrolyte temperature prediction but drastically improves the computational efficiency. The modeled terminal voltage is also benchmarked with the experimental data under different current densities. The electrolyte temperature is found to be significantly influenced by the flow rate of coolant. As compared, although the electrolyte flow rate has unremarkable impact on electrolyte temperature, its effect on system pressure drop and battery efficiency is significant. Increasing the electrolyte flow rate improves the coulombic efficiency, voltage efficiency and energy efficiency simultaneously but at the expense of higher pump power demanded. An optimal flow rate exists for each operating condition to maximize the system efficiency

  4. Heavy metals in moss samples exposed to tHe atmospHeric dust after eruption of eyjafjallajökull volcano

    Directory of Open Access Journals (Sweden)

    Patryk Ochota

    2012-03-01

    Full Text Available Background: Volcanic ash, which is ejected during volcanic eruptions, flies in the air and spreads by the wind over large distances. It is a magmatic source and as such may contain heavy metals. The aim of the study was to carry out investigation on heavy metal content: Pb, Cd, Zn, Fe, Mn, Cu and Cr in samples of moss bags exposed to atmospheric dust containing volcanic ash in Sosnowiec (Poland after eruption of Eyjafjallajökull volcano in Iceland. Materials and methods: Samples have been exposed to atmospheric dust after volcanic eruption for 2 months, and were mineralised in 70% HNO3 and 30% H2O2. The content of Pb and Cd was analysed by atomic absorption spectrometry with electrothermal atomization (ETAAS and Zn, Fe, Mn, Cu, Cr by atomic absorption spectrometry with flame atomization (FAAS. Results: During the experiment the content of lead in samples of moss increased by 54,9 μg/g, cadmium by 3,41 μg/g, manganese by 150 μg/g, iron by 6,09 mg/g, zinc by 514 μg/g, copper by 20,77 μg/g and chromium by 6,99 μg/g. Conclusions: In Sosnowiec the comparable increase of metal content was from several to 41 times higher than in the areas not exposed to volcanic ash. It indicates that volcanic ash can be a potential source of heavy metals in the environment and, consequently, affect our health.

  5. A scalable pressure sensor based on an electrothermally and electrostatically operated resonator

    KAUST Repository

    Hajjaj, Amal Z.

    2017-11-29

    We present a pressure sensor based on the convective cooling of the air surrounding an electrothermally heated resonant bridge. Unlike conventional pressure sensors that rely on diaphragm deformation in response to pressure, the sensor does not require diaphragms of the large surface area, and hence is scalable and can be realized even at the nanoscale. The concept is demonstrated using both straight and arch microbeam resonators driven and sensed electrostatically. The change in the surrounding pressure is shown to be accurately tracked by monitoring the change in the resonance frequency of the structure. The sensitivity of the sensor, which is controllable by the applied electrothermal load, is shown near 57 811 ppm/mbar for a pressure range from 1 to 10 Torr. We show that a straight beam operated near the buckling threshold leads to the maximum sensitivity of the device. The experimental data and simulation results, based on a multi-physics finite element model, demonstrate the feasibility and simplicity of the pressure sensor. Published by AIP Publishing.

  6. Comparative study of injection into a pneumatic nebuliser and tungsten coil electrothermal vaporisation for the determination of rare earth elements by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Dittrich, K.

    1988-01-01

    Injection into a pneumatic nebuliser and vaporisation using a tungsten coil electrothermal vaporisation system, with a 3-kW argon-nitrogen inductively coupled plasma (ICP), are compared for the determination of the rare earth elements. The sampling efficiency and thus also the absolute power of detection of the tungsten coil ICP optical emission spectrometric (ICP-OES) technique are better by two orders of magnitude, than the injection technique. The absolute detection limits for the rare earth elements are at the pg level; for the refractory rare earth elements (Er, La, Lu and Y), they are lower than those obtained by graphite furnace atomic absorption spectrometry, whereas for the other rare earth elements (Eu, Sc, Tm and Yb), the detection limits are comparable. With injection of samples into a pneumatic nebuliser and ICP-OES, matrix effects are low and absolute amounts of the order of mg of the rare earth matrix can be tolerated, giving relative detection limits down to 1 μg g -1 . The amount of rare earth matrix that can be tolerated with the tungsten-coil atomiser is two orders of magnitude lower. Thus the relatively detection limits of the two methods are of the same order, although the matrix effects are considerably higher with the tungsten coil. (author)

  7. Transient electro-thermal modeling of bipolar power semiconductor devices

    CERN Document Server

    Gachovska, Tanya Kirilova; Du, Bin

    2013-01-01

    This book presents physics-based electro-thermal models of bipolar power semiconductor devices including their packages, and describes their implementation in MATLAB and Simulink. It is a continuation of our first book Modeling of Bipolar Power Semiconductor Devices. The device electrical models are developed by subdividing the devices into different regions and the operations in each region, along with the interactions at the interfaces, are analyzed using the basic semiconductor physics equations that govern device behavior. The Fourier series solution is used to solve the ambipolar diffusio

  8. Electrothermally Actuated Microbeams With Varying Stiffness

    KAUST Repository

    Tella, Sherif Adekunle

    2017-11-03

    We present axially loaded clamped-guided microbeams that can be used as resonators and actuators of variable stiffness, actuation, and anchor conditions. The applied axial load is implemented by U-shaped electrothermal actuators stacked at one of the beams edges. These can be configured and wired in various ways, which serve as mechanical stiffness elements that control the operating resonance frequency of the structures and their static displacement. The experimental results have shown considerable increase in the resonance frequency and mid-point deflection of the microbeam upon changing the end conditions of the beam. These results can be promising for applications requiring large deflection and high frequency tunability, such as filters, memory devices, and switches. The experimental results are compared to multi-physics finite-element simulations showing good agreement among them.

  9. Electro-thermal modeling of high power IGBT module short-circuits with experimental validation

    DEFF Research Database (Denmark)

    Wu, Rui; Iannuzzo, Francesco; Wang, Huai

    2015-01-01

    A novel Insulated Gate Bipolar Transistor (IGBT) electro-thermal modeling approach involving PSpice and ANSYS/Icepak with both high accuracy and simulation speed has been presented to study short-circuit of a 1.7 kV/1 kA commercial IGBT module. The approach successfully predicts the current...

  10. Solid phase extraction for analysis of biogenic carbonates by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS): an investigation of rare earth element signatures in otolith microchemistry

    International Nuclear Information System (INIS)

    Arslan, Zikri; Paulson, Anthony J.

    2003-01-01

    Uptake of trace elements into fish otoliths is governed by several factors such as life histories and environment in addition to stock and species differences. In an attempt to elucidate the elemental signatures of rare earth elements (REEs) in otoliths, a solid phase extraction (SPE) protocol was used in combination with electrothermal vaporization (ETV) as a sample introduction procedure for the determinations by inductively coupled plasma quadrupole mass spectrometry (ICP-MS). Effects of various parameters, such as carrier gas flow rate, atomization temperature and chemical modification, were examined for optimization of the conditions by ETV-ICP-MS. Atomization was achieved at 2800 deg. C. Lower temperatures (i.e. 2600 deg. C) resulted in severe memory problems due to incomplete atomization. Palladium was used as a chemical modifier. It was found that an increase in Pd concentration up to 0.5 μg in the injection volume (70 μl) led up to four-fold enhancement in the integrated signals. This phenomenon is attributed to the carrier effect of Pd rather than the stabilization since no significant losses were observed for high temperature drying around 700 deg. C even in the absence of Pd. Preconcentration was performed on-line at pH 5 by using a mini-column of Toyopearl AF-Chelate 650M chelating resin, which also eliminated the calcium matrix of otolith solutions. After preconcentration of 6.4 ml of solution, the concentrate was collected in 0.65 ml of 0.5% (v/v) HNO 3 in autosampler cups, and then analyzed by ETV-ICP-MS. The method was validated with the analysis of a fish otolith certified reference material (CRM) of emperor snapper, and then applied to samples. Results obtained from otoliths of fish captured in the same habitat indicated that otolith rare earth element concentrations are more dependent on environmental conditions of the habitat than on species differences

  11. Simultaneous electrothermal vaporization and nebulizer sample introduction system for inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Arnquist, Isaac J.; Kreschollek, Thomas E.; Holcombe, James A.

    2011-01-01

    The novel analytical application of the combination of an inline electrothermal vaporization (ETV) and nebulization source for inductively coupled plasma mass spectrometry (ICP-MS) has been studied. Wet plasma conditions are sustained during ETV introduction by 200 mL/min gas flow through the nebulizer, which is merged with the ETV transport line at the torch. The use of a wet plasma with ETV introduction avoided the need to change power settings and torch positions that normally accompany a change from wet to dry plasma operating conditions. This inline-ETV source is shown to have good detection limits for a variety of elements in both HNO 3 and HCl matrices. Using the inline-ETV source, improved limits of detection (LOD) were obtained for elements typically suppressed by polyatomic interferences using a nebulizer. Specifically, improved LODs for 51 V and 53 Cr suffering from Cl interferences ( 51 ClO + and 53 ClO + respectively) in a 1% HCl matrix were obtained using the inline-ETV source. LODs were improved by factors of 65 and 22 for 51 V and 53 Cr, respectively, using the inline-ETV source compared to a conventional concentric glass nebulizer. For elements without polyatomic interferences, LODs from the inline-ETV were comparable to conventional dry plasma ETV-ICP time-of-flight mass spectrometry results. Lastly, the inline-ETV source offers a simple means of changing from nebulizer introduction to inline-ETV introduction without extinguishing the plasma. This permits, for example, the use of the time-resolved ETV-ICP-MS signals to distinguish between an analyte ion and polyatomic isobar.

  12. Minimizing tip-sample forces in jumping mode atomic force microscopy in liquid

    Energy Technology Data Exchange (ETDEWEB)

    Ortega-Esteban, A. [Departamento de Fisica de la Materia Condensada, C-3, Universidad Autonoma de Madrid, Cantoblanco, 28049 Madrid (Spain); Horcas, I. [Nanotec Electronica S.L., Centro Empresarial Euronova 3, Ronda de Poniente 12, 28760 Tres Cantos, Madrid (Spain); Hernando-Perez, M. [Departamento de Fisica de la Materia Condensada, C-3, Universidad Autonoma de Madrid, Cantoblanco, 28049 Madrid (Spain); Ares, P. [Nanotec Electronica S.L., Centro Empresarial Euronova 3, Ronda de Poniente 12, 28760 Tres Cantos, Madrid (Spain); Perez-Berna, A.J.; San Martin, C.; Carrascosa, J.L. [Centro Nacional de Biotecnologia (CNB-CSIC), Darwin 3, 28049 Madrid (Spain); Pablo, P.J. de [Departamento de Fisica de la Materia Condensada, C-3, Universidad Autonoma de Madrid, Cantoblanco, 28049 Madrid (Spain); Gomez-Herrero, J., E-mail: julio.gomez@uam.es [Departamento de Fisica de la Materia Condensada, C-3, Universidad Autonoma de Madrid, Cantoblanco, 28049 Madrid (Spain)

    2012-03-15

    Control and minimization of tip-sample interaction forces are imperative tasks to maximize the performance of atomic force microscopy. In particular, when imaging soft biological matter in liquids, the cantilever dragging force prevents identification of the tip-sample mechanical contact, resulting in deleterious interaction with the specimen. In this work we present an improved jumping mode procedure that allows detecting the tip-sample contact with high accuracy, thus minimizing the scanning forces ({approx}100 pN) during the approach cycles. To illustrate this method we report images of human adenovirus and T7 bacteriophage particles which are prone to uncontrolled modifications when using conventional jumping mode. -- Highlights: Black-Right-Pointing-Pointer Improvement in atomic force microscopy in buffer solution. Black-Right-Pointing-Pointer Peak force detection. Black-Right-Pointing-Pointer Subtracting the cantilever dragging force. Black-Right-Pointing-Pointer Forces in the 100 pN range. Black-Right-Pointing-Pointer Imaging of delicate viruses with atomic force microscopy.

  13. Determination of rare earth elements in natural water samples – A review of sample separation, preconcentration and direct methodologies

    Energy Technology Data Exchange (ETDEWEB)

    Fisher, Andrew, E-mail: afisher@plymouth.ac.uk [School of Geography, Earth and Environmental Sciences, Plymouth University, Drake Circus, Plymouth, Devon, PL4 8AA (United Kingdom); Kara, Derya [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100, Balikesir (Turkey)

    2016-09-07

    This review discusses and compares the methods given for the determination of rare earth elements (REE) in natural water samples, including sea, river, lake, tap, ground and waste waters as well as Antarctic ice. Since REE are at very low concentrations in natural waters, numerous different preconcentration methods have been proposed to enable their measurement. These include liquid liquid extraction, dispersive liquid-liquid micro-extraction and solidified floating drop micro-extraction. In addition to liquid-liquid extraction methods, solid phase extraction using commercial resins, resins made in-house, silica-based exchange materials and other solid media is also discussed. These and other techniques such as precipitation/co-precipitation and flotation are compared in terms of speed, preconcentration factors achieved, precision, accuracy and limits of detection (LOD). Some papers have discussed the direct determination of REE in these sample types. Some have used specialised sample introduction systems such as ultrasonic nebulization whereas others have used a standard sample introduction system coupled with inductively coupled plasma mass spectrometry (ICP-MS) detection. These direct methods have also been discussed and compared. - Highlights: • The determination of rare earth elements in waters is reviewed. • Assorted preconcentration techniques are discussed and evaluated. • Detection techniques include atomic spectrometry, potentiometry and spectrophotometry. • Special nebulisers and electrothermal vaporization approaches are reviewed.

  14. Flow injection on-line preconcentration of low levels of Cr(VI) with detection by ETAAS

    DEFF Research Database (Denmark)

    Som-aum, Waraporn; Liawruangrath, Saisunee; Hansen, Elo Harald

    2002-01-01

    A flow injection (FI) on-line sorption preconcentration procedure utilizing a packed column reactor and combined with electrothermal atomic absorption spectrometry (ETAAS) is proposed for the determination of low levels of Cr(VI) in water samples. Polytetrafluoroethylene (PTFE) beads packed in a ...

  15. Chromium in marine sediment samples from the Ria de Arousa (Galicia, NW of Spain): analysis of the total content in slurries by ETAAS

    International Nuclear Information System (INIS)

    Pazos-Capeans, P.; Barciela-Alonso, M.C.; Bermejo-Barrera, A.; Bermejo-Barrera, P.

    2004-01-01

    The study attempts to measure the total chromium content in sediments of all the Ria de Arousa (Galicia, NW Spain). The method was developed by analysing slurries by electrothermal atomic absorption spectrometry. The metal determination was carried out optimising the electrothermal programme and the concentration of magnesium nitrate as a chemical modifier. What was aimed to be achieved is a general explanation of the chromium content along the estuary because there could be a chromium sink in this marine environment. Results obtained were between 43.4±1.7 μg g -1 and 184.6±26.9 μg g -1 from the end of the Ulla river to the Atlantic Ocean, most of them higher than the background reference levels

  16. Chromium in marine sediment samples from the Ria de Arousa (Galicia, NW of Spain): analysis of the total content in slurries by ETAAS

    Energy Technology Data Exchange (ETDEWEB)

    Pazos-Capeans, P.; Barciela-Alonso, M.C.; Bermejo-Barrera, A.; Bermejo-Barrera, P

    2004-10-25

    The study attempts to measure the total chromium content in sediments of all the Ria de Arousa (Galicia, NW Spain). The method was developed by analysing slurries by electrothermal atomic absorption spectrometry. The metal determination was carried out optimising the electrothermal programme and the concentration of magnesium nitrate as a chemical modifier. What was aimed to be achieved is a general explanation of the chromium content along the estuary because there could be a chromium sink in this marine environment. Results obtained were between 43.4{+-}1.7 {mu}g g{sup -1} and 184.6{+-}26.9 {mu}g g{sup -1} from the end of the Ulla river to the Atlantic Ocean, most of them higher than the background reference levels.

  17. Statics and dynamics of electrothermal micromirrors

    Science.gov (United States)

    Morrison, Jessica A.

    Adaptive and smart systems are growing in popularity as we shift toward personalization as a culture. With progressive demands on energy efficiency, it is increasingly important to focus on the utilization of energy in a novel way. This thesis investigates a microelectromechanical system (MEMS) mirror with the express intent to provide flexibility in solid state lighting (SSL). By coupling the micromirror to an optical source, the reflected light may be reshaped and directed so as to optimize the overall illumination profile. In addition, the light may be redirected in order to provide improved signal strength in visible light communications (VLC) with negligible impact on energy demands. With flexibility and full analog control in mind, the design of a fully integrated tip-tilt-piston micromirror with an additional variable focus degree of freedom is outlined. Electrothermal actuators are used to both steer the light and tune the focal length. A detailed discussion of the underlying physics behind composite beams and thermal actuators is addressed. This leads directly into an overview of the two main mirror components, namely the segmented mirror and the deflection actuators. An in-depth characterization of the dynamics of the mirror is discussed including the linearity of the thermal response. Frequency domain analysis of such a system provides insight into tunable mechanical properties such as the resonant frequency and quality factor. The degenerate resonant modes can be separated significantly. It is shown that the frequency response may be tuned by straining specific actuators and that it follows a predictable pattern. As a result, the system can be scanned at increasingly large angles. In other words, coupled mechanical modes allow variable damping and amplification. A means to determine the level of coupling is examined and the mode shape variations are tracked as a function of the tuning parameters. Finally, the applications of such a device are explored

  18. An electro-thermally activated rotary micro-positioner for slider-level dual-stage positioning in hard disk drives

    International Nuclear Information System (INIS)

    Lau, Gih Keong; Chong, Nyok Boon; Yang, Jiaping; Tan, Cheng Peng

    2016-01-01

    Slider-level micro-positioners are useful to assist a voice coil motor to perform fine head positioning over a Tb/in 2 magnetic disk. Recently, a new kind of slider-level micro-positioner was developed using the thermal unimorph of the Si/SU8 composite. It has the advantages of a very small footprint and high mechanical resonant frequency, but its stroke generation is inadequate, with a 50 nm dynamic stroke at 1 kHz. There is a need for a larger thermally induced stroke. This paper presents a rotary design of an electrothermal micro-positioner to address the stroke requirements without consuming more power or decreasing the mechanical resonant frequency. Experimental studies show the present rotary design can produce a six-fold larger displacement, as compared to the previous lateral design, while possessing a 35 kHz resonant frequency. In addition, simple analytical models were developed to estimate: (i) the rotational stiffness and system’s natural frequency, (ii) thermal unimorph bending and stage rotation, and (iii) the system’s thermal time constant for this rotary electro-thermal micro-positioner. This study found that this rotary electro-thermal micro-positioner can meet the basic stroke requirement and high mechanical resonant frequency for a moving slider, but its thermal cut-off frequency needs to be increased further. (paper)

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  20. Characterising thermal resistances and capacitances of GaN high-electron-mobility transistors through dynamic electrothermal measurements

    DEFF Research Database (Denmark)

    Wei, Wei; Mikkelsen, Jan H.; Jensen, Ole Kiel

    2014-01-01

    This study presents a method to characterise thermal resistances and capacitances of GaN high-electron-mobility transistors (HEMTs) through dynamic electrothermal measurements. A measured relation between RF gain and the channel temperature (Tc) is formed and used for indirect measurements...

  1. A low aspect ratio electrothermal gun for metal plasma vapor discharge and ceramic nanopowder production

    International Nuclear Information System (INIS)

    Kim, Kyoung Jin; Peterson, Dennis R.

    2008-01-01

    Traditionally, the electrothermal gun design has the bore of a large aspect ratio: however, a low aspect ratio design with a shorter bore length has been employed for efficient production of metal plasma vapors and synthesis of nanomaterials. In a comparison of the arc resistance-current relationship, a low aspect ratio design is found to exhibit distinctively different characteristics compared to a high aspect ratio design, and this trend is explained by the scaling law of plasma properties including theory of plasma electrical conductivity. A one-dimensional isothermal model has been applied to the present experiments to confirm the scaling laws, and it was found that the present modification of the electrothermal gun is able to produce fully ionized metal plasma vapor, while the plasma vapor produced in a conventional design is partially ionized. Also, by reacting metal plasma vapors with the controlled gases in the reaction chamber, nanoscale materials such as aluminum oxide, aluminum nitride, and titanium oxide were synthesized successfully

  2. Fabrication of 3D electro-thermal micro actuators in silica glass by femtosecond laser wet etch and microsolidics

    Science.gov (United States)

    Li, Qichao; Shan, Chao; Yang, Qing; Chen, Feng; Bian, Hao; Hou, Xun

    2017-02-01

    This paper demonstrates a novel electro-thermal micro actuator's design, fabrication and device tests which combine microfluidic technology and microsolidics process. A three-dimensional solenoid microchannel with high aspect ratio is fabricated inside the silica glass by an improved femtosecond laser wet etch (FLWE) technology, and the diameter of the spiral coil is only 200 μm. Molten alloy (Bi/In/Sn/Pb) with high melting point is injected into the three-dimensional solenoid microchannel inside the silica glass , then it solidifys and forms an electro-thermal micro actuator. The device is capable of achieving precise temperature control and quick response, and can also be easily integrated into MEMS, sensors and `lab on a chip' (LOC) platform inside the fused silica substrate.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-10-24

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

  5. Material impacts and heat flux characterization of an electrothermal plasma source with an applied magnetic field

    Science.gov (United States)

    Gebhart, T. E.; Martinez-Rodriguez, R. A.; Baylor, L. R.; Rapp, J.; Winfrey, A. L.

    2017-08-01

    To produce a realistic tokamak-like plasma environment in linear plasma device, a transient source is needed to deliver heat and particle fluxes similar to those seen in an edge localized mode (ELM). ELMs in future large tokamaks will deliver heat fluxes of ˜1 GW/m2 to the divertor plasma facing components at a few Hz. An electrothermal plasma source can deliver heat fluxes of this magnitude. These sources operate in an ablative arc regime which is driven by a DC capacitive discharge. An electrothermal source was configured with two pulse lengths and tested under a solenoidal magnetic field to determine the resulting impact on liner ablation, plasma parameters, and delivered heat flux. The arc travels through and ablates a boron nitride liner and strikes a tungsten plate. The tungsten target plate is analyzed for surface damage using a scanning electron microscope.

  6. Experimental evidences of electro-thermal ablation acceleration of water

    International Nuclear Information System (INIS)

    Ikuta, Kazunari.

    1987-07-01

    We report the first demonstrations of driving water of about 1000 grams by electro-thermally ablated gas pressure in a cavity with a single exhauster. A blob of water was shot into the air with a shooting angle of about 45 deg, and the flight velocity observed was about 13 meters per second with the capacitor (28μF) charged up to 10 KV. The discharge sound was almost suppressed by the water blob loaded in the chamber possilbly because the energy of sound was dissipated into the water blob. The application of this ablation water driver to ship propulsion is also discussed. (author)

  7. Assessment of lead in blood samples of children residing in the vicinity of industries

    International Nuclear Information System (INIS)

    Shah, F.; Kazi, T.G.; Afridi, H.I.; Brahaman, K.D.; Arain, S.S.; Panhwar, A.H.

    2013-01-01

    The aim of present study was to determine the lead (Pb) distributions in blood and prevalence of elevated Pb exposure among children, age ranged (5-10 years), residing near industrialized region of Hyderabad city, Pakistan. For comparison, biological samples of children of same age group from non-industrial area were also analyzed. The Pb concentration in blood samples was determined by electrothermal atomic absorption spectrometry, prior to microwave assisted acid digestion. The results showed that significantly higher proportion of children living in the vicinity of industrial area, had blood Pb levels (BLL) in the range of 15.4-35.6 micro g/dL, and 8.51-16.7 micro g/dL for those of non-industrial area. The blood Pb level was higher in boys of both groups as compared to girls of same age group, but the difference was not significant (p=0.178). Negative correlation was observed between BLL and hemoglobin levels (p<0.001), while positive correlation was observed between BLL and age. (author)

  8. Construção de espectrômetro de emissão atômica com atomização eletrotérmica em filamento de tungstênio (WCAES Construction of a tungsten coil atomic emission spectrometer (WCAES

    Directory of Open Access Journals (Sweden)

    Mário H. Gonzalez

    2010-01-01

    Full Text Available It is here discussed the development of a low cost analytical instrument with capacity for metals determination using atomic emission measurements in an electrothermal atomization system with a tungsten coil atomizer. The main goal was to show a new frontier for using this atomizer and to demonstrate that the simple instrumental arrangement here proposed has potential for portability and for solving analytical tasks related to metals determination. Atomic emission of calcium was selected for the adjustment of instrumental parameters and to evaluate the main characteristics of the lab-built instrument. Cobalt was determined in medicines and one alloy to demonstrate its feasibility.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  10. Coupling on-line preconcentration by ion-exchange with ETAAS. A novel flow injection approach based on the use of a renewable microcolumn as demonstrated for the determination of nickel in environmental and biological samples

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2000-01-01

    microcolumn incorporated within an integrated micro FI-system, the column is loaded with a defined volume of small beads of an SP Sephadex C-25 cation-exchange resin and subsequently exposed to a metered amount of sample solution. However, instead of eluting the retained analyte from the organic ion-exchange......A novel way of exploiting flow injection/sequential injection (FIA/SIA) on-line ion-exchange preconcentration with detection by electrothermal atomic absorption spectrometry (ETAAS) is described and demonstrated for the determination of trace-levels of nickel. Based on the use of a renewable...... resin, the beads are along with 30 mul of carrier (buffer) solution transported via air segmentation directly into the graphite tube, where they are ashed during the pyrolysis and atomization process. The ETAAS determination is performed in parallel with the preconcentration process of the ensuing...

  11. Lumped-Element Dynamic Electro-Thermal model of a superconducting magnet

    Science.gov (United States)

    Ravaioli, E.; Auchmann, B.; Maciejewski, M.; ten Kate, H. H. J.; Verweij, A. P.

    2016-12-01

    Modeling accurately electro-thermal transients occurring in a superconducting magnet is challenging. The behavior of the magnet is the result of complex phenomena occurring in distinct physical domains (electrical, magnetic and thermal) at very different spatial and time scales. Combined multi-domain effects significantly affect the dynamic behavior of the system and are to be taken into account in a coherent and consistent model. A new methodology for developing a Lumped-Element Dynamic Electro-Thermal (LEDET) model of a superconducting magnet is presented. This model includes non-linear dynamic effects such as the dependence of the magnet's differential self-inductance on the presence of inter-filament and inter-strand coupling currents in the conductor. These effects are usually not taken into account because superconducting magnets are primarily operated in stationary conditions. However, they often have significant impact on magnet performance, particularly when the magnet is subject to high ramp rates. Following the LEDET method, the complex interdependence between the electro-magnetic and thermal domains can be modeled with three sub-networks of lumped-elements, reproducing the electrical transient in the main magnet circuit, the thermal transient in the coil cross-section, and the electro-magnetic transient of the inter-filament and inter-strand coupling currents in the superconductor. The same simulation environment can simultaneously model macroscopic electrical transients and phenomena at the level of superconducting strands. The model developed is a very useful tool for reproducing and predicting the performance of conventional quench protection systems based on energy extraction and quench heaters, and of the innovative CLIQ protection system as well.

  12. Speciation of Cr(VI) in environmental samples in the vicinity of the ferrochrome smelter.

    Science.gov (United States)

    Sedumedi, Hilda N; Mandiwana, Khakhathi L; Ngobeni, Prince; Panichev, Nikolay

    2009-12-30

    The impact of ferrochrome smelter on the contamination of its environment with toxic hexavalent chromium, Cr(VI), was assessed by analyzing smelter dusts, soil, grass and tree barks. For the separation of Cr(VI) from Cr(III), solid samples were treated with 0.1M Na(2)CO(3) and filtered through hydrophilic PDVF 0.45 microm filter prior to the determination of Cr(VI) by electrothermal atomic absorption spectrometry (ET-AAS). Ferrochrome smelter dust was found to contain significant levels of Cr(VI), viz. 43.5 microg g(-1) (cyclone dust), 2710 microg g(-1) (fine dust), and 7800 microg g(-1) (slimes dust) which exceeded the maximum acceptable risk concentration (20 microg g(-1)). The concentration of Cr(VI) in environmental samples of grass (3.4+/-0.2), soil (7.7+/-0.2), and tree bark (11.8+/-1.2) collected in the vicinity of the chrome smelter were higher as compared with the same kind of samples collected from uncontaminated area. The results of the investigation show that ferrochrome smelter is a source of environmental pollution with contamination factors of Cr(VI) ranging between 10 and 50.

  13. Speciation of Cr(VI) in environmental samples in the vicinity of the ferrochrome smelter

    International Nuclear Information System (INIS)

    Sedumedi, Hilda N.; Mandiwana, Khakhathi L.; Ngobeni, Prince; Panichev, Nikolay

    2009-01-01

    The impact of ferrochrome smelter on the contamination of its environment with toxic hexavalent chromium, Cr(VI), was assessed by analyzing smelter dusts, soil, grass and tree barks. For the separation of Cr(VI) from Cr(III), solid samples were treated with 0.1 M Na 2 CO 3 and filtered through hydrophilic PDVF 0.45 μm filter prior to the determination of Cr(VI) by electrothermal atomic absorption spectrometry (ET-AAS). Ferrochrome smelter dust was found to contain significant levels of Cr(VI), viz. 43.5 μg g -1 (cyclone dust), 2710 μg g -1 (fine dust), and 7800 μg g -1 (slimes dust) which exceeded the maximum acceptable risk concentration (20 μg g -1 ). The concentration of Cr(VI) in environmental samples of grass (3.4 ± 0.2), soil (7.7 ± 0.2), and tree bark (11.8 ± 1.2) collected in the vicinity of the chrome smelter were higher as compared with the same kind of samples collected from uncontaminated area. The results of the investigation show that ferrochrome smelter is a source of environmental pollution with contamination factors of Cr(VI) ranging between 10 and 50.

  14. Determination of arsenic species in rice samples using CPE and ETAAS.

    Science.gov (United States)

    Costa, Bruno Elias Dos Santos; Coelho, Nívia Maria Melo; Coelho, Luciana Melo

    2015-07-01

    A highly sensitive and selective procedure for the determination of arsenate and total arsenic in food by electrothermal atomic absorption spectrometry after cloud point extraction (ETAAS/CPE) was developed. The procedure is based on the formation of a complex of As(V) ions with molybdate in the presence of 50.0 mmol L(-1) sulfuric acid. The complex was extracted into the surfactant-rich phase of 0.06% (w/v) Triton X-114. The variables affecting the complex formation, extraction and phase separation were optimized using factorial designs. Under the optimal conditions, the calibration graph was linear in the range of 0.05-10.0 μg L(-1). The detection and quantification limits were 10 and 33 ng L(-1), respectively and the corresponding value for the relative standard deviation for 10 replicates was below 5%. Recovery values of between 90.8% and 113.1% were obtained for spiked samples. The accuracy of the method was evaluated by comparison with the results obtained for the analysis of a rice flour sample (certified material IRMM-804) and no significant difference at the 95% confidence level was observed. The method was successfully applied to the determination of As(V) and total arsenic in rice samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Electrothermal Equivalent Three-Dimensional Finite-Element Model of a Single Neuron.

    Science.gov (United States)

    Cinelli, Ilaria; Destrade, Michel; Duffy, Maeve; McHugh, Peter

    2018-06-01

    We propose a novel approach for modelling the interdependence of electrical and mechanical phenomena in nervous cells, by using electrothermal equivalences in finite element (FE) analysis so that existing thermomechanical tools can be applied. First, the equivalence between electrical and thermal properties of the nerve materials is established, and results of a pure heat conduction analysis performed in Abaqus CAE Software 6.13-3 are validated with analytical solutions for a range of steady and transient conditions. This validation includes the definition of equivalent active membrane properties that enable prediction of the action potential. Then, as a step toward fully coupled models, electromechanical coupling is implemented through the definition of equivalent piezoelectric properties of the nerve membrane using the thermal expansion coefficient, enabling prediction of the mechanical response of the nerve to the action potential. Results of the coupled electromechanical model are validated with previously published experimental results of deformation for squid giant axon, crab nerve fibre, and garfish olfactory nerve fibre. A simplified coupled electromechanical modelling approach is established through an electrothermal equivalent FE model of a nervous cell for biomedical applications. One of the key findings is the mechanical characterization of the neural activity in a coupled electromechanical domain, which provides insights into the electromechanical behaviour of nervous cells, such as thinning of the membrane. This is a first step toward modelling three-dimensional electromechanical alteration induced by trauma at nerve bundle, tissue, and organ levels.

  16. Numerical simulation of travelling wave induced electrothermal fluid flow

    International Nuclear Information System (INIS)

    Perch-Nielsen, Ivan R; Green, Nicolas G; Wolff, Anders

    2004-01-01

    Many microdevices for manipulating particles and cells use electric fields to produce a motive force on the particles. The movement of particles in non-uniform electric fields is called dielectrophoresis, and the usual method of applying this effect is to pass the particle suspension over a microelectrode structure. If the suspension has a noticeable conductivity, one important side effect is that the electric field drives a substantial conduction current through the fluid, causing localized Joule-heating. The resulting thermal gradient produces local conductivity and permittivity changes in the fluid. Dielectrophoretic forces acting upon these pockets of fluid will then produce motion of both the fluid and the particles. This paper presents a numerical solution of the electrical force and the resulting electrothermal driven fluid flow on a travelling wave structure. This common electrode geometry consists of interdigitated electrodes laid down in a long array, with the phase of the applied potential shifted by 90 0 on each subsequent electrode. The resulting travelling electric field was simulated and the thermal field and electrical body force on the fluid calculated, for devices constructed from two typical materials: silicon and glass. The electrothermal fluid flow in the electrolyte over the electrode array was then numerically simulated. The model predicts that the thermal field depends on the conductivity and applied voltage, but more importantly on the geometry of the system and the material used in the construction of the device. The velocity of the fluid flow depends critically on the same parameters, with slight differences in the thermal field for glass and silicon leading to diametrically opposite flow direction with respect to the travelling field for the two materials. In addition, the imposition of slight external temperature gradients is shown to have a large effect on the fluid flow in the device, under certain conditions leading to a reversal of

  17. Design and Modeling of Polysilicon Electrothermal Actuators for a MEMS Mirror with Low Power Consumption

    Directory of Open Access Journals (Sweden)

    Miguel Lara-Castro

    2017-06-01

    Full Text Available Endoscopic optical-coherence tomography (OCT systems require low cost mirrors with small footprint size, out-of-plane deflections and low bias voltage. These requirements can be achieved with electrothermal actuators based on microelectromechanical systems (MEMS. We present the design and modeling of polysilicon electrothermal actuators for a MEMS mirror (100 μm × 100 μm × 2.25 μm. These actuators are composed by two beam types (2.25 μm thickness with different cross-section area, which are separated by 2 μm gap. The mirror and actuators are designed through the Sandia Ultra-planar Multi-level MEMS Technology V (SUMMiT V® process, obtaining a small footprint size (1028 μm × 1028 µm for actuators of 550 µm length. The actuators have out-of-plane displacements caused by low dc voltages and without use material layers with distinct thermal expansion coefficients. The temperature behavior along the actuators is calculated through analytical models that include terms of heat energy generation, heat conduction and heat energy loss. The force method is used to predict the maximum out-of-plane displacements in the actuator tip as function of supplied voltage. Both analytical models, under steady-state conditions, employ the polysilicon resistivity as function of the temperature. The electrothermal-and structural behavior of the actuators is studied considering different beams dimensions (length and width and dc bias voltages from 0.5 to 2.5 V. For 2.5 V, the actuator of 550 µm length reaches a maximum temperature, displacement and electrical power of 115 °C, 10.3 µm and 6.3 mW, respectively. The designed actuation mechanism can be useful for MEMS mirrors of different sizes with potential application in endoscopic OCT systems that require low power consumption.

  18. Design and characterization of a microelectromechanical system electro-thermal linear motor with interlock mechanism for micro manipulators.

    Science.gov (United States)

    Hu, Tengjiang; Zhao, Yulong; Li, Xiuyuan; Zhao, You; Bai, Yingwei

    2016-03-01

    The design, fabrication, and testing of a novel electro-thermal linear motor for micro manipulators is presented in this paper. The V-shape electro-thermal actuator arrays, micro lever, micro spring, and slider are introduced. In moving operation, the linear motor can move nearly 1 mm displacement with 100 μm each step while keeping the applied voltage as low as 17 V. In holding operation, the motor can stay in one particular position without consuming energy and no creep deformation is found. Actuation force of 12.7 mN indicates the high force generation capability of the device. Experiments of lifetime show that the device can wear over two million cycles of operation. A silicon-on-insulator wafer is introduced to fabricate a high aspect ratio structure and the chip size is 8.5 mm × 8.5 mm × 0.5 mm.

  19. 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)

  20. A multilayer electro-thermal model of pouch battery during normal discharge and internal short circuit process

    International Nuclear Information System (INIS)

    Chen, Mingbiao; Bai, Fanfei; Song, Wenji; Lv, Jie; Lin, Shili

    2017-01-01

    Highlights: • 2D network equivalent circuit considers the interplay of cell units. • The temperature non-uniformity Φ of multilayer model is bigger than that of lumped model. • The temperature non-uniformity is quantified and the reason of non-uniformity is analyzed. • Increasing the thermal conductivity of the separator can effectively relieve the heat spot effect of ISC. - Abstract: As the electrical and thermal characteristic will affect the batteries’ safety, performance, calendar life and capacity fading, an electro-thermal coupled model for pouch battery LiFePO_4/C is developed in normal discharge and internal short circuit process. The battery is discretized into many cell elements which are united as a 2D network equivalent circuit. The electro-thermal model is solved with finite difference method. Non-uniformity of current distribution and temperature distribution is simulated and the result is validated with experiment data at various discharge rates. Comparison of the lumped model and the multilayer structure model shows that the temperature non-uniformity Φ of multilayer model is bigger than that of lumped model and shows more precise. The temperature non-uniformity is quantified and the reason of non-uniformity is analyzed. The electro-thermal model can also be used to guide the safety design of battery. The temperature of the ISC element near tabs is the highest because the equivalent resistance of the external circuit (not including the ISC element) is the smallest when the resistance of cell units is small. It is found that increasing the thermal conductivity of integrated layer can effectively relieve the heat spot effect of ISC.

  1. Wear-out Failure Analysis of an Impedance-Source PV Microinverter Based on System-Level Electro-Thermal Modeling

    DEFF Research Database (Denmark)

    Shen, Yanfeng; Chub, Andrii; Wang, Huai

    2018-01-01

    and system-level finite element method (FEM) simulations, the electro-thermal models are built for the most reliability-critical components, i.e., power semi-conductor devices and capacitors. The dependence of the power loss on the junction/hotspot temperature is considered, the enclosure temperature...

  2. Electrothermal frequency references in standard CMOS

    CERN Document Server

    Kashmiri, S Mahdi

    2013-01-01

    This book describes an alternative method of accurate on-chip frequency generation in standard CMOS IC processes. This method exploits the thermal-diffusivity of silicon, the rate at which heat diffuses through a silicon substrate.  This is the first book describing thermal-diffusivity-based frequency references, including the complete theoretical methodology supported by practical realizations that prove the feasibility of the method.  Coverage also includes several circuit and system-level solutions for the analog electronic circuit design challenges faced.   ·         Surveys the state-of-the-art in all-silicon frequency references; ·         Examines the thermal properties of silicon as a solution for the challenge of on-chip accurate frequency generation; ·         Uses simplified modeling approaches that allow an electronics engineer easily to simulate the electrothermal elements; ·         Follows a top-down methodology in circuit design, in which system-level des...

  3. Atomic absorption determination of ultratrace tellurium in rocks utilizing high sensitivity sampling systems

    International Nuclear Information System (INIS)

    Beaty, R.D.

    1973-01-01

    The sampling boat and the graphite furnace were shown to possess the required sensitivity to detect tellurium at ultratrace levels, in a variety of sample types, by atomic absorption. In the sampling boat approach, tellurium in sample solutions is chemically separated and concentrated by extraction into methyl isobutyl ketone before measurement. For samples exhibiting extraction interferences or excessively high background absorption, a preliminary separation of tellurium by coprecipitation with selenium is described. Using this technique, tellurium can be quantitatively detected down to 5 nanograms and linear response is observed to 100 nanograms. Relative standard deviations of better than 7 percent are achieved for 50 nanograms of tellurium. For samples that have a tellurium content below the detection limits of the sampling boat, the graphite furnace is used for atomization. By this method, as little as 0.07 nanograms of tellurium can be detected, and a precision of 1 percent relative standard deviation is achievable at the 5 nanogram level. A routinely applicable procedure was developed for determining tellurium in rocks, using the graphite furnace, after a hydrofluoric acid decomposition of the sample. Using this procedure, tellurium data were obtained on 20 different rocks, and the significance of this new information is discussed. (Diss. Abstr. Int., B)

  4. Determination of the neutral oxygen atom density in a plasma reactor loaded with metal samples

    Science.gov (United States)

    Mozetic, Miran; Cvelbar, Uros

    2009-08-01

    The density of neutral oxygen atoms was determined during processing of metal samples in a plasma reactor. The reactor was a Pyrex tube with an inner diameter of 11 cm and a length of 30 cm. Plasma was created by an inductively coupled radiofrequency generator operating at a frequency of 27.12 MHz and output power up to 500 W. The O density was measured at the edge of the glass tube with a copper fiber optics catalytic probe. The O atom density in the empty tube depended on pressure and was between 4 and 7 × 1021 m-3. The maximum O density was at a pressure of about 150 Pa, while the dissociation fraction of O2 molecules was maximal at the lowest pressure and decreased with increasing pressure. At about 300 Pa it dropped below 10%. The measurements were repeated in the chamber loaded with different metallic samples. In these cases, the density of oxygen atoms was lower than that in the empty chamber. The results were explained by a drain of O atoms caused by heterogeneous recombination on the samples.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-08-01

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

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

  7. Development, validation and accreditation of a method for the determination of Pb, Cd, Cu and As in seafood and fish feed samples.

    Science.gov (United States)

    Psoma, A K; Pasias, I N; Rousis, N I; Barkonikos, K A; Thomaidis, N S

    2014-05-15

    A rapid, sensitive, accurate and precise method for the determination of Pb, Cd, As and Cu in seafood and fish feed samples by Simultaneous Electrothermal Atomic Absorption Spectrometry was developed in regard to Council Directive 333/2007EC and ISO/IEC 17025 (2005). Different approaches were investigated in order to shorten the analysis time, always taking into account the sensitivity. For method validation, precision (repeatability and reproducibility) and accuracy by addition recovery tests have been assessed as performance criteria. The expanded uncertainties based on the Eurachem/Citac Guidelines were calculated. The method was accredited by the Hellenic Accreditation System and it was applied for an 8 years study in seafood (n=202) and fish feeds (n=275) from the Greek market. The annual and seasonal variation of the elemental content and correlation among the elemental content in fish feeds and the respective fish samples were also accomplished. Copyright © 2013 Elsevier Ltd. All rights reserved.

  8. Electrothermal Simulation of Large-Area Semiconductor Devices

    Directory of Open Access Journals (Sweden)

    C Kirsch

    2017-06-01

    Full Text Available The lateral charge transport in thin-film semiconductor devices is affected by the sheet resistance of the various layers. This may lead to a non-uniform current distribution across a large-area device resulting in inhomogeneous luminance, for example, as observed in organic light-emitting diodes (Neyts et al., 2006. The resistive loss in electrical energy is converted into thermal energy via Joule heating, which results in a temperature increase inside the device. On the other hand, the charge transport properties of the device materials are also temperature-dependent, such that we are facing a two-way coupled electrothermal problem. It has been demonstrated that adding thermal effects to an electrical model significantly changes the results (Slawinski et al., 2011. We present a mathematical model for the steady-state distribution of the electric potential and of the temperature across one electrode of a large-area semiconductor device, as well as numerical solutions obtained using the finite element method.

  9. Electric and electrothermal conductivity of planetary ionospheres

    International Nuclear Information System (INIS)

    Pavlov, A.V.

    1984-01-01

    In the first, second and third approximations of expansion of the Chapman-Enskog method in Sonin polynomials, an explicit form is found of coefficients of electrical and electrothermal electron condituctjvity in a magnetic field in a multicomponent ionosphere with allowance for the electron temperature difference from the heavy component temperature. The generic expressions for the electron transport coefficients are reduced to the form suitable for practical applications. In the first approximation of expansion in Sonin polynomials, the equations are derived for determining the ion diffusion velocities in a magnetic field in a multicomponent gas mixtures. +he approximating expressions for frequencies of electron collisions with main neutral components of planet upper atmospheres are refined. In the first, second and third approximations the equations are derived for determining velocities of ambipolar ion diffusion in a multicomponent ionosphere without a magnetic field (or parallel to it). The explicit form of the electron thermodiffusion factor, being a part of these equations, has been found

  10. Label-free quantification of Tacrolimus in biological samples by atomic force microscopy

    International Nuclear Information System (INIS)

    Menotta, Michele; Biagiotti, Sara; Streppa, Laura; Rossi, Luigia; Magnani, Mauro

    2015-01-01

    Highlights: • Tacrolimus is a potent immunosuppressant drug that has to be continually monitored. • We present an atomic force microscope approach for quantification of Tacrolimus in blood samples. • Detection and quantification have been successfully achieved. - Abstract: In the present paper we describe an atomic force microscopy (AFM)-based method for the quantitative analysis of FK506 (Tacrolimus) in whole blood (WB) samples. Current reference methods used to quantify this immunosuppressive drug are based on mass spectrometry. In addition, an immunoenzymatic assay (ELISA) has been developed and is widely used in clinic, even though it shows a small but consistent overestimation of the actual drug concentration when compared with the mass spectrometry method. The AFM biosensor presented herein utilises the endogen drug receptor, FKBP12, to quantify Tacrolimus levels. The biosensor was first assayed to detect the free drug in solution, and subsequently used for the detection of Tacrolimus in blood samples. The sensor was suitable to generate a dose–response curve in the full range of clinical drug monitoring. A comparison with the clinically tested ELISA assay is also reported

  11. Label-free quantification of Tacrolimus in biological samples by atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Menotta, Michele, E-mail: michele.menotta@uniurb.it [Department of Biomolecular Sciences, University of Urbino “Carlo Bo” via Saffi 2, Urbino (Italy); Biagiotti, Sara [Department of Biomolecular Sciences, University of Urbino “Carlo Bo” via Saffi 2, Urbino (Italy); Streppa, Laura [Physics Laboratory, CNRS-ENS, UMR 5672, Lyon (France); Cell and Molecular Biology Laboratory, CNRS-ENS Lyon, UMR 5239, IFR128, Lyon (France); Rossi, Luigia; Magnani, Mauro [Department of Biomolecular Sciences, University of Urbino “Carlo Bo” via Saffi 2, Urbino (Italy)

    2015-07-16

    Highlights: • Tacrolimus is a potent immunosuppressant drug that has to be continually monitored. • We present an atomic force microscope approach for quantification of Tacrolimus in blood samples. • Detection and quantification have been successfully achieved. - Abstract: In the present paper we describe an atomic force microscopy (AFM)-based method for the quantitative analysis of FK506 (Tacrolimus) in whole blood (WB) samples. Current reference methods used to quantify this immunosuppressive drug are based on mass spectrometry. In addition, an immunoenzymatic assay (ELISA) has been developed and is widely used in clinic, even though it shows a small but consistent overestimation of the actual drug concentration when compared with the mass spectrometry method. The AFM biosensor presented herein utilises the endogen drug receptor, FKBP12, to quantify Tacrolimus levels. The biosensor was first assayed to detect the free drug in solution, and subsequently used for the detection of Tacrolimus in blood samples. The sensor was suitable to generate a dose–response curve in the full range of clinical drug monitoring. A comparison with the clinically tested ELISA assay is also reported.

  12. Trace elements in bottom sediments of the Barents Sea on the standard section "Kola Meridian"

    OpenAIRE

    Lapteva A. M.; Plotitsyna N. F.

    2017-01-01

    The levels of trace metals (Cu, Zn, Ni, Cr, Mn, Co, Pb, Cd, Hg) and arsenic (As) in samples of bottom sediments from the Barents Sea on eight stations of the standard section "Kola Meridian" have been investigated. Trace elements have been determined on atomic absorption spectrophotometer AA-6800 with mercury-hydride attachment HVG-1 of the company Shimadzu (Japan) by the methods of flaming (acetylene – air) and electrothermal atomization. Common and very toxic trace elements incl...

  13. Atomic energy

    International Nuclear Information System (INIS)

    Ramanna, R.

    1978-01-01

    Development of nuclear science in India, particularly the research and development work at the Bhabha Atomic Research Centre (BARC), Bombay, is described. Among the wide range of materials developed for specific functions under rigorous conditions are nuclear pure grade uranium, zirconium and beryllium, and conventional materials like aluminium, carbon steel and stainless steels. Radioisotopes are produced and used for tracer studies in various fields. Various types of nuclear gauges and nuclear instruments are produced. Radiations have been used to develop new high yielding groundnut mutants with large kernals. The sterile male technique for pest control and radiosterilization technique to process potatoes, onions and marine foods for storage are ready for exploitation. Processes and equipment have been developed for production of electrolytic hydrogen, electrothermal phosphorus and desalinated water. Indigenously manufactured components and materials are now being used for the nuclear energy programme. Indian nuclear power programme strategy is to build heavy water reactors and to utilise their byproduct plutonium and depleted uranium to feed fast breeder reactors which will produce more fissile material than burnt. Finally a special mention has been made of the manpower development programme of the BARC. BARC has established a training school in 1957 giving advanced training in physics, chemistry and various branches of engineering and metallurgy

  14. Electro-thermal Modeling of Modern Power Devices for Studying Abnormal Operating Conditions

    DEFF Research Database (Denmark)

    Wu, Rui

    in industrial power electronic systems in the range above 10 kW. The failure of IGBTs can be generally classified as catastrophic failures and wear out failures. A wear out failure is mainly induced by accumulated degradation with time, while a catastrophic failure is triggered by a single-event abnormal....... The objective of this project has been to model and predict the electro-thermal behavior of IGBT power modules under abnormal conditions, especially short circuits. A thorough investigation on catastrophic failure modes and mechanisms of modern power semiconductor devices, including IGBTs and power diodes, has...

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

    Science.gov (United States)

    Kowalewska, Zofia; Ruszczyńska, Anna; Bulska, Ewa

    2005-03-01

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

  16. Comparison of four-probe thermal and thermoelectric transport measurements of thin films and nanostructures with microfabricated electro-thermal transducers

    Science.gov (United States)

    Kim, Jaehyun; Fleming, Evan; Zhou, Yuanyuan; Shi, Li

    2018-03-01

    Two different four-probe thermal and thermoelectric measurement methods have been reported for measuring the thermal conductivity, Seebeck coefficient, and electrical conductivity of suspended thin films and nanostructures with microfabricated electro-thermal transducers. The thermal contact resistance was extracted from the measured thermoelectric voltage drop at the contacts in the earlier four-probe method based on the assumption of constant thermal and thermoelectric properties along the sample. In comparison, the latter four-probe method can directly obtain the contact thermal resistance together with the intrinsic sample thermal resistance without making this assumption. Here, the measurement theory and data reduction processes of the latter four-probe measurement method are re-examined and improved. The measured thermal conductivity result of this improved method on representative thin film samples are found to agree with those obtained from the earlier four-probe method, which has obtained similar Seebeck coefficient and electrical conductivity as those measured with a different method for a supported thin film. The agreement provides further validation of the latest four-probe thermal transport measurement method of thin films and nanostructures.

  17. Note: A silicon-on-insulator microelectromechanical systems probe scanner for on-chip atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fowler, Anthony G.; Maroufi, Mohammad; Moheimani, S. O. Reza, E-mail: Reza.Moheimani@newcastle.edu.au [School of Electrical Engineering and Computer Science, University of Newcastle, Callaghan, NSW 2308 (Australia)

    2015-04-15

    A new microelectromechanical systems-based 2-degree-of-freedom (DoF) scanner with an integrated cantilever for on-chip atomic force microscopy (AFM) is presented. The silicon cantilever features a layer of piezoelectric material to facilitate its use for tapping mode AFM and enable simultaneous deflection sensing. Electrostatic actuators and electrothermal sensors are used to accurately position the cantilever within the x-y plane. Experimental testing shows that the cantilever is able to be scanned over a 10 μm × 10 μm window and that the cantilever achieves a peak-to-peak deflection greater than 400 nm when excited at its resonance frequency of approximately 62 kHz.

  18. Estimation of the thermal characteristics of a bridgewire environment by an electrothermal response test

    International Nuclear Information System (INIS)

    Donaldson, A.B.; Strasburg, A.C.

    1976-01-01

    The electrothermal response of an electroexplosive device is determined by applying a subcritical square wave current pulse to the bridgewire and monitoring the resultant temperature excursion. The temperature profile, thus obtained, can be utilized with a mathematical model called the ''Probe Method'' for approximating thermal properties. It is possible to estimate the thermal conductivity and specific heat of the pyrotechnic and the thermal contact conductance at the bridgewire/pyrotechnic interface by this technique

  19. Feasibility study on infrared electro-thermal NDE of stainless steel

    International Nuclear Information System (INIS)

    Green, D.R.; Hassberger, J.A.

    1975-11-01

    Electro-thermal examination, a branch of thermal testing (TT), is a promising method being developed for NDE of stainless steel welds. This report describes the first phase of development; i.e., preliminary demonstration and laboratory evaluation of the method's sensitivity to notches in Type 304 stainless steel plate specimens. It also includes a description of the basic principles, together with a description of the hardware and experimental results showing that electrical discharge machined notches down to 0.16 cm (0.06 in.) long x 0.08 cm (0.03 in.) deep were detected. A qualitative technique for interpreting the test results to determine whether defects are at the surface or deeper within the material is demonstrated

  20. Speciation of Cr(VI) in environmental samples in the vicinity of the ferrochrome smelter

    Energy Technology Data Exchange (ETDEWEB)

    Sedumedi, Hilda N. [Department of Chemistry, Tshwane University of Technology, P.O. Box 56208, Arcadia, 0007, Pretoria (South Africa); Mandiwana, Khakhathi L., E-mail: MandiwanaKL@tut.ac.za [Department of Chemistry, Tshwane University of Technology, P.O. Box 56208, Arcadia, 0007, Pretoria (South Africa); Ngobeni, Prince; Panichev, Nikolay [Department of Chemistry, Tshwane University of Technology, P.O. Box 56208, Arcadia, 0007, Pretoria (South Africa)

    2009-12-30

    The impact of ferrochrome smelter on the contamination of its environment with toxic hexavalent chromium, Cr(VI), was assessed by analyzing smelter dusts, soil, grass and tree barks. For the separation of Cr(VI) from Cr(III), solid samples were treated with 0.1 M Na{sub 2}CO{sub 3} and filtered through hydrophilic PDVF 0.45 {mu}m filter prior to the determination of Cr(VI) by electrothermal atomic absorption spectrometry (ET-AAS). Ferrochrome smelter dust was found to contain significant levels of Cr(VI), viz. 43.5 {mu}g g{sup -1} (cyclone dust), 2710 {mu}g g{sup -1} (fine dust), and 7800 {mu}g g{sup -1} (slimes dust) which exceeded the maximum acceptable risk concentration (20 {mu}g g{sup -1}). The concentration of Cr(VI) in environmental samples of grass (3.4 {+-} 0.2), soil (7.7 {+-} 0.2), and tree bark (11.8 {+-} 1.2) collected in the vicinity of the chrome smelter were higher as compared with the same kind of samples collected from uncontaminated area. The results of the investigation show that ferrochrome smelter is a source of environmental pollution with contamination factors of Cr(VI) ranging between 10 and 50.

  1. Imaging of elements in leaves of tobacco by solid sampling–electrothermal vaporization–inductively coupled plasma-optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Masson, Pierre, E-mail: masson@bordeaux.inra.fr

    2014-12-01

    Plants take up and store elements according to the environment in which they are growing. Because plants are at the base of the food chain, the determination of essential elements or toxic elements in plant materials is of importance. However, it is assumed that the element content determined on selected tissues may provide more specific information than that derived from the whole plant analysis. In this work, we assessed the feasibility of solid sampling–electrothermal vaporization–inductively coupled plasma-optical emission spectrometry analyses for quantitative imaging of Cd and Mg in plant leaves. Leaves of tobacco (Nicotiana tabacum) were selected to be used as samples. To produce a two dimensional image, sections cut from leaf samples were analyzed. Cellulose doped with multi-element solution standards was used as calibration samples. Two certified reference materials (NIST SRM 1547 Peach Leaves and NIST SRM 1573a Tomato leaves) were used to verify the accuracy of measurements with good agreement between the measured concentrations and the certified values. Quantitative imaging revealed the inhomogeneous distribution of the selected elements. Excess of Cd and Mg tended to be focused on peripheral regions and the tip of the leaf.

  2. Reversible and Precisely Controllable p/n-Type Doping of MoTe2 Transistors through Electrothermal Doping.

    Science.gov (United States)

    Chang, Yuan-Ming; Yang, Shih-Hsien; Lin, Che-Yi; Chen, Chang-Hung; Lien, Chen-Hsin; Jian, Wen-Bin; Ueno, Keiji; Suen, Yuen-Wuu; Tsukagoshi, Kazuhito; Lin, Yen-Fu

    2018-03-01

    Precisely controllable and reversible p/n-type electronic doping of molybdenum ditelluride (MoTe 2 ) transistors is achieved by electrothermal doping (E-doping) processes. E-doping includes electrothermal annealing induced by an electric field in a vacuum chamber, which results in electron (n-type) doping and exposure to air, which induces hole (p-type) doping. The doping arises from the interaction between oxygen molecules or water vapor and defects of tellurium at the MoTe 2 surface, and allows the accurate manipulation of p/n-type electrical doping of MoTe 2 transistors. Because no dopant or special gas is used in the E-doping processes of MoTe 2 , E-doping is a simple and efficient method. Moreover, through exact manipulation of p/n-type doping of MoTe 2 transistors, quasi-complementary metal oxide semiconductor adaptive logic circuits, such as an inverter, not or gate, and not and gate, are successfully fabricated. The simple method, E-doping, adopted in obtaining p/n-type doping of MoTe 2 transistors undoubtedly has provided an approach to create the electronic devices with desired performance. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Adjustable static and dynamic actuation of clamped-guided beams using electrothermal axial loads

    KAUST Repository

    Alcheikh, Nouha

    2018-02-14

    The paper presents adjustable static and dynamic actuations of in-plane clamped-guided beams. The structures, of variable stiffness, can be used as highly tunable resonators and actuators. Axial loads are applied through electrothermal U-shaped and flexure beams actuators stacked near the edges of curved (arch) beams. The electrothermal actuators can be configurred in various ways to adjust as desired the mechanical stiffness of the structures; thereby controlling their deformation stroke as actuators and their operating resonance frequency as resonators. The experimental and finite element results demonstrate the flexibility of the designs in terms of static displacements and resonance frequencies of the first and second symmetric modes of the arches. The results show considerable increase in the resonance frequency and deflection of the microbeam upon changing end actuation conditions, which can be promising for low voltage actuation and tunable resonators applications, such as filters and memory devices. As case studies of potential device configurations of the proposed design, we demonstrate eight possibilities of achieving new static and dynamic behaviors, which produce various resonance frequencies and static displacement curves. The ability to actively shift the entire frequency response curve of a device is desirable for several applications to compensate for in-use anchor degradations and deformations. As an example, we experimentally demonstrate using the device as a resonant logic gate, with active resonance tuning, showing fundamental 2-bit logic functions, such as AND,XOR, and NOR.

  4. Adjustable static and dynamic actuation of clamped-guided beams using electrothermal axial loads

    KAUST Repository

    Alcheikh, Nouha; Tella, Sherif Adekunle; Younis, Mohammad I.

    2018-01-01

    The paper presents adjustable static and dynamic actuations of in-plane clamped-guided beams. The structures, of variable stiffness, can be used as highly tunable resonators and actuators. Axial loads are applied through electrothermal U-shaped and flexure beams actuators stacked near the edges of curved (arch) beams. The electrothermal actuators can be configurred in various ways to adjust as desired the mechanical stiffness of the structures; thereby controlling their deformation stroke as actuators and their operating resonance frequency as resonators. The experimental and finite element results demonstrate the flexibility of the designs in terms of static displacements and resonance frequencies of the first and second symmetric modes of the arches. The results show considerable increase in the resonance frequency and deflection of the microbeam upon changing end actuation conditions, which can be promising for low voltage actuation and tunable resonators applications, such as filters and memory devices. As case studies of potential device configurations of the proposed design, we demonstrate eight possibilities of achieving new static and dynamic behaviors, which produce various resonance frequencies and static displacement curves. The ability to actively shift the entire frequency response curve of a device is desirable for several applications to compensate for in-use anchor degradations and deformations. As an example, we experimentally demonstrate using the device as a resonant logic gate, with active resonance tuning, showing fundamental 2-bit logic functions, such as AND,XOR, and NOR.

  5. Method development for the determination of cadmium, copper, lead, selenium and thallium in sediments by slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry and isotopic dilution calibration

    International Nuclear Information System (INIS)

    Dias, Lucia Felicidade; Miranda, Gilson R.; Saint'Pierre, Tatiana D.; Maia, Sandra M.; Frescura, Vera L.A.; Curtius, Adilson J.

    2005-01-01

    A procedure for the determination of Cd, Cu, Pb, Se and Tl by slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) with calibration by isotopic dilution is proposed. The slurry is prepared by mixing the sample with diluted nitric and hydrofluoric acids in an ultrasonic bath and then in a water bath at 60 deg C for 120 min. The slurries were let to stand at least for 12 h, manually shaken before poured into the autosampler cups and homogenized by passing through an argon flow, just before pipetting it into the furnace. The analytes were determined in two groups, according to their thermal behaviors. The furnace temperature program was optimized and the selected compromised pyrolysis temperatures were: 400 deg C for Cd, Se and Tl and 700 deg C for Cu and Pb. The vaporization temperature was 2300 deg C. The analyses were carried out without modifier as no significant effect was observed for different tested modifiers. Different sample particle sizes did not affect the sensitivity significantly, then a particle size ≤50 μm was adopted. The accuracy was checked by analyzing five certified reference sediments, with analytes concentrations from sub-μg g -1 to a few hundreds μg g -1 . The great majority of the obtained concentrations were in agreement with the certified values. The detection limits, determined for the MESS-2 certified sediment, were, in μg g -1 : 0.01 for Cd; 0.8 for Cu; 0.4 for Pb; 0.4 for Se and 0.06 for Tl. The precision was adequate with relative standard deviations lower than 12%. Isotopic dilution showed to be an efficient calibration technique for slurry, as the extraction of the analyte to the liquid phase of the slurry and the reactions in the vaporizer must help the equilibration between the added isotope and the isotope in the sample

  6. Energy landscape of all-atom protein-protein interactions revealed by multiscale enhanced sampling.

    Directory of Open Access Journals (Sweden)

    Kei Moritsugu

    2014-10-01

    Full Text Available Protein-protein interactions are regulated by a subtle balance of complicated atomic interactions and solvation at the interface. To understand such an elusive phenomenon, it is necessary to thoroughly survey the large configurational space from the stable complex structure to the dissociated states using the all-atom model in explicit solvent and to delineate the energy landscape of protein-protein interactions. In this study, we carried out a multiscale enhanced sampling (MSES simulation of the formation of a barnase-barstar complex, which is a protein complex characterized by an extraordinary tight and fast binding, to determine the energy landscape of atomistic protein-protein interactions. The MSES adopts a multicopy and multiscale scheme to enable for the enhanced sampling of the all-atom model of large proteins including explicit solvent. During the 100-ns MSES simulation of the barnase-barstar system, we observed the association-dissociation processes of the atomistic protein complex in solution several times, which contained not only the native complex structure but also fully non-native configurations. The sampled distributions suggest that a large variety of non-native states went downhill to the stable complex structure, like a fast folding on a funnel-like potential. This funnel landscape is attributed to dominant configurations in the early stage of the association process characterized by near-native orientations, which will accelerate the native inter-molecular interactions. These configurations are guided mostly by the shape complementarity between barnase and barstar, and lead to the fast formation of the final complex structure along the downhill energy landscape.

  7. Directional emission of single photons from small atomic samples

    DEFF Research Database (Denmark)

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

    2013-01-01

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

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

    International Nuclear Information System (INIS)

    Kowalewska, Zofia; Ruszczynska, Anna; Bulska, Ewa

    2005-01-01

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

  9. Ultrasound-assisted extraction technique for establishing selenium contents in breast cancer biopsies by Zeeman-electrothermal atomic absorption spectrometry using multi-injection

    International Nuclear Information System (INIS)

    Lavilla, I.; Mosquera, A.; Millos, J.; Cameselle, J.; Bendicho, C.

    2006-01-01

    A solid-liquid extraction method is developed to establish the contents of selenium in breast cancer biopsies. The method is based on the ultrasound-assisted extraction of selenium from pretreated biopsies prior to Se determination by atomic absorption spectrometry with longitudinal-Zeeman background correction. Fifty-one breast biopsies were collected from the Cies Hospital (Vigo, Spain), 32 of which correspond to tumor tissue and 19 to normal tissue (parenchyma). Difficulties arising from the samples analyzed, i.e. small samples mass (50-100 mg), extremely low Se contents and sample texture modification including tissue hardening due to formaldehyde preservation are addressed and overcome. High intensity sonication using a probe together with addition of hydrogen peroxide succeeded in completely extracting Se from biopsies. The multiple injection technique was useful to tackle the low Se contents present in some biopsies. The detection limit was 25 ng g -1 of Se and the precision, expressed as relative standard deviation, was less than 10%. Se contents ranged from 0.08 to 0.4 μg g -1 for parenchyma samples and from 0.09 to 0.8 μg g -1 for tumor samples. In general, Se levels in tumor biopsies were higher as compared with the adjacent normal tissue in 19 patients by a factor of up to 6. Analytical data confirmed Se accumulation in the breast tumors

  10. Electrothermal vaporisation ICP-mass spectrometry (ETV-ICP-MS) for the determination and speciation of trace elements in solid samples - A review of real-life applications from the author's lab

    Energy Technology Data Exchange (ETDEWEB)

    Vanhaecke, Frank; Resano, Martin; Moens, Luc [Laboratory of Analytical Chemistry, Ghent University, Institute for Nuclear Sciences, Proeftuinstraat 86, 9000 Ghent (Belgium)

    2002-09-01

    The use of electrothermal vaporisation (ETV) from a graphite furnace as a means of sample introduction in inductively coupled plasma mass spectrometry (ICP-MS) permits the direct analysis of solid samples. A multi-step furnace temperature programme is used to separate the vaporisation of the target element(s) and of the matrix components from one another. Sometimes, a chemical modifier is used to enable a higher thermal pre-treatment temperature, by avoiding premature analyte losses (stabilisation) or promoting the selective volatilisation of matrix components. In almost all instances, accurate results can be obtained via external calibration or single standard addition using an aqueous standard solution. Absolute limits of detection are typically 1 pg, which corresponds to 1 ng/g for a typical sample mass of 1 mg. Real-life applications carried out in the author's lab are used to illustrate the utility of this approach. These applications aim at trace element determination in industrial and environmental materials. The industrial materials analysed include different types of plastics - Carilon, polyethylene, poly(ethyleneterephtalate) and polyamide - and photo- and thermographic materials. As samples from environmental origin, plant material, animal tissue and sediments were investigated. Some applications aimed at a multi-element determination, while in other, the content of a single, but often challenging, element (e.g., Si or S) had to be measured. ETV-ICP-MS was also used in elemental speciation studies. Separation of Se-containing proteins was accomplished using polyacrylamide gel electrophoresis (PAGE). Subsequent quantification of the Se content in the protein spots was carried out using ETV-ICP-MS. As the volatilisation of methylmercury and inorganic mercury could be separated from one another with respect to time, no chromatographic or electrophoretic separation procedure was required, but ETV-ICP-MS as such sufficed for Hg speciation in fish tissue

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

    Directory of Open Access Journals (Sweden)

    Ion V. POPESCU

    2011-05-01

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

  12. Distribución de metales en el acíbar de hojas de zábila (Aloe vera (L. Burm.f.

    Directory of Open Access Journals (Sweden)

    Carlos E. Rondón

    Full Text Available This work presents the distribution of Na, Ca, Mg, K, Cu, Zn, Mn and Fe in Aloe vera leaves exudate by flame atomic absorption spectrometry (FAAS and Cr by electrothermal atomic absorption spectrometry (ETAAS. The plants were cultivated in the city of Coro, Falcón state. The samples were collected from internal, medium and external leaves. The accuracy of the method was evaluated using a certified reference material NBS 1572. The average precision was 1.39%. The applied method was accurate, precise and free from interferences.

  13. 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.)

  14. A non-destructive technique for assigning effective atomic number to scientific samples by scattering of 59.54 keV gamma photons

    International Nuclear Information System (INIS)

    Singh, M.P.; Sharma, Amandeep; Singh, Bhajan; Sandhu, B.S.

    2010-01-01

    The objective of present experiment, employing a scattering of 59.54 keV gamma photons, is to assign effective atomic number (Z eff ) to scientific samples (rare earths) of known composition. An HPGe semiconductor detector, placed at 90 o to the incident beam, detects gamma photons scattered from the sample under investigation. The experiment is performed on various elements with atomic number satisfying, 6≤Z≤82, for 59.54 keV incident photons. The intensity ratio of Rayleigh to Compton scattered peaks, corrected for photo-peak efficiency of gamma detector and absorption of photons in the sample and air, is plotted as a function of atomic number and constituted a best fit-curve. From this fit-curve, the respective effective atomic numbers to samples of rare earths are determined. The agreement of measured values of Z eff with theoretical calculations is quite satisfactory.

  15. Determination of arsenic, lead, selenium and tin in sediments by slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry using Ru as permanent modifier and NaCl as a carrier

    International Nuclear Information System (INIS)

    Dias, Lucia Felicidade; Saint'Pierre, Tatiana D.; Maia, Sandra M.; Mesquita da Silva, Marcia A.; Frescura, Vera L.A.; Welz, Bernhard; Curtius, Adilson J.

    2002-01-01

    A procedure for the determination of As, Pb, Se and Sn in sediment slurries by electrothermal vaporization inductively coupled plasma mass spectrometry is proposed. The slurry, 1 mg ml -1 , is prepared by mixing the sample ground to a particle size ≤50 μm with 5% v/v nitric and 1% v/v hydrofluoric acids in an ultrasonic bath. The slurry was homogenized with a constant flow of argon in the autosampler cup, just before transferring an aliquot to the graphite furnace. The tube was treated with Ru as a permanent modifier, and an optimized mass of 1 μg of NaCl was added as a physical carrier. The pyrolysis temperature was optimized through pyrolysis curves, and a compromised temperature of 800 deg. C was used; the vaporization temperature was 2300 deg. C. The effect of different acid concentrations in the slurry on the analyte signal intensities was also evaluated. The accuracy of the method was assured by the analysis of certified reference sediments MESS-2, PACS-2 and HISS-1 from the National Research Council Canada, SRM 2704 and SRM 1646a from the National Institute of Standards and Technology and RS-4 from a round robin test, using external calibration with aqueous standards prepared in the same medium as the slurries. The obtained concentrations were in agreement with the certified values according to the Student's t-test for a confidence level of 95%. The detection limits in the samples were: 0.17 μg g -1 for As; 0.3 μg g -1 for Pb; 0.05 μg g -1 for Se and 0.28 μg g -1 for Sn. The precision found for the different sediment samples, expressed as R.S.D. was 1-8% for As, 2-9% for Pb, 6-12% for Se and 3-8% for Sn (n=5)

  16. A radiotracer study on the volatilization and transport effects of thermochemical reagents used in the analysis of alumina powders by slurry electrothermal vaporization inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Peschel, Birgit U.; Herdering, Wilhelm; Broekaert, Jose A.C.

    2007-01-01

    A neutron-activated Al 2 O 3 powder SRM 699 (NIST) containing the γ-radiation emitting radionuclides 51 Cr, 59 Fe, 60 Co and 65 Zn has been used to study the influence of thermochemical reagents on the volatilization and transport efficiency for these trace elements in electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) of Al 2 O 3 powders. From the signals in the γ-spectra for the radiotracers it has been found that less than 2% of the elements Cr, Fe, Co and Zn is left back in a graphite furnace from Al 2 O 3 powders at 2200 deg. C even without addition of a thermochemical reagent and the latter even was found to decrease the volatilization efficiencies. The recovery for the radiotracers on filters at the end of the transport tube as measured from the signals in the γ-spectra, however, was found to increase in most cases (i.e. from about 10% to more than 20%) when Pd(NO 3 ) 2 , Pd(NO 3 ) 2 + Mg(NO 3 ) 2 , PdCl 2 , IrCl 3 , SnCl 2 , AgCl, NaF, NH 4 Cl and NH 4 F were added at amounts generally used in electrothermal vaporization inductively coupled plasma mass spectrometry. However, when adding higher amounts as stoichiometrically required for a complete halogenation of the sample matrix in the case of AgCl, C 8 F 15 O 2 Na, IrCl 3 or PdCl 2 the transport efficiencies considerably decrease again. As shown in the case of NH 4 Cl the amount of thermochemical reagent used has to be optimized so as to obtain maximum analyte transport efficiencies. A comparison of the influence of NH 4 Cl on the transport efficiencies with its influence on the ETV-ICP-MS signals for Fe demonstrates the importance of transport efficiency changes for the effects of thermochemical reagents in electrothermal vaporization inductively coupled plasma mass spectrometry

  17. Photovoltaic optimizer boost converters: Temperature influence and electro-thermal design

    International Nuclear Information System (INIS)

    Graditi, G.; Adinolfi, G.; Tina, G.M.

    2014-01-01

    Highlights: • The influence of temperature on DC–DC converter devices properties is considered. • An electro-thermal design method for PV power optimizer converters is proposed. • The electro-thermal design method proposed is applied to DR boost and SR boost. • Efficiency results of the designed SR converter and DR converters are presented. - Abstract: Objective: Photovoltaic (PV) systems can operate in presence of not uniform working conditions caused by continuously changing temperature and irradiance values and mismatching and shadowing phenomena. The more the PV system works in these conditions, the more its energy performances are negatively affected. Distributed Maximum Power Point Tracking (DMPPT) converters are now increasingly used to overcome this problem and to improve PV applications efficiency. A DMPPT system consists in a DC–DC converters equipped with a suitable controller dedicated to the Maximum Power Point Tracking (MPPT) of a single PV module. It is arranged either inside the junction-box or in a separate box close to the PV generator. Many power optimizers are now commercially available. In spite of different adopted DC–DC converter topologies, the shared interests of DMPPT systems designers are the high efficiency and reliability values. It is worth noting that to obtain so high performances converters, electronic components have to be carefully selected between the whole commercial availability and appropriately matched together. In this scenario, an electro-thermal design methodology is proposed and a reliability study by means of the Military Handbook 217F is carried out. Method: The developed DMPPT converters design method is constituted by many steps. In fact, beginning from installation site, PV generators and load data, this process selects power optimizers commercially available devices and it verifies their electro-thermal behavior to the aim to identify a set of suitable components for DMPPT applications. Repeating this

  18. Single-drop microextraction for the determination of manganese in seafood and water samples

    International Nuclear Information System (INIS)

    Lemos, V.A.; Vieira, U.S.

    2013-01-01

    We describe a method for single drop microextraction of manganese from fish, mollusk, and from natural waters using the reagent 1-(2-pyridylazo)-2-naphthol as the complexing agent and chloroform as the fluid extractor. After extraction, the analyte was directly submitted to graphite furnace electrothermal atomic absorption spectrometry. Once optimized, the method has a detection limit of 30 ng L -1 , a limit of quantification of 100 ng L -1 , and an enrichment factor of 16. Its accuracy was verified by applying the procedure to the following certified reference materials: apple leaves, spinach leaves, bovine liver, and mussel tissue. The procedure was also successfully applied to the determination of manganese in seafood and natural waters. (author)

  19. MEMS-based silicon cantilevers with integrated electrothermal heaters for airborne ultrafine particle sensing

    Science.gov (United States)

    Wasisto, Hutomo Suryo; Merzsch, Stephan; Waag, Andreas; Peiner, Erwin

    2013-05-01

    The development of low-cost and low-power MEMS-based cantilever sensors for possible application in hand-held airborne ultrafine particle monitors is described in this work. The proposed resonant sensors are realized by silicon bulk micromachining technology with electrothermal excitation, piezoresistive frequency readout, and electrostatic particle collection elements integrated and constructed in the same sensor fabrication process step of boron diffusion. Built-in heating resistor and full Wheatstone bridge are set close to the cantilever clamp end for effective excitation and sensing, respectively, of beam deflection. Meanwhile, the particle collection electrode is located at the cantilever free end. A 300 μm-thick, phosphorus-doped silicon bulk wafer is used instead of silicon-on-insulator (SOI) as the starting material for the sensors to reduce the fabrication costs. To etch and release the cantilevers from the substrate, inductively coupled plasma (ICP) cryogenic dry etching is utilized. By controlling the etching parameters (e.g., temperature, oxygen content, and duration), cantilever structures with thicknesses down to 10 - 20 μm are yielded. In the sensor characterization, the heating resistor is heated and generating thermal waves which induce thermal expansion and further cause mechanical bending strain in the out-of-plane direction. A resonant frequency of 114.08 +/- 0.04 kHz and a quality factor of 1302 +/- 267 are measured in air for a fabricated rectangular cantilever (500x100x13.5 μm3). Owing to its low power consumption of a few milliwatts, this electrothermal cantilever is suitable for replacing the current external piezoelectric stack actuator in the next generation of the miniaturized cantilever-based nanoparticle detector (CANTOR).

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

    International Nuclear Information System (INIS)

    Montaser, A.

    1993-01-01

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

  1. Radionuclide determination in environmental samples by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Lariviere, Dominic; Taylor, Vivien F.; Evans, R. Douglas; Cornett, R. Jack

    2006-01-01

    The determination of naturally occurring and anthropogenic radionuclides in the environment by inductively coupled plasma mass spectrometry has gained recognition over the last fifteen years, relative to radiometric techniques, as the result of improvement in instrumental performance, sample introduction equipment, and sample preparation. With the increase in instrumental sensitivity, it is now possible to measure ultratrace levels (fg range) of many radioisotopes, including those with half-lives between 1 and 1000 years, without requiring very complex sample pre-concentration schemes. However, the identification and quantification of radioisotopes in environmental matrices is still hampered by a variety of analytical issues such as spectral (both atomic and molecular ions) and non-spectral (matrix effect) interferences and instrumental limitations (e.g., abundance sensitivity). The scope of this review is to highlight recent analytical progress and issues associated with the determination of radionuclides by inductively coupled plasma mass spectrometry. The impact of interferences, instrumental limitations (e.g., degree of ionization, abundance sensitivity, detection limits) and low sample-to-plasma transfer efficiency on the measurement of radionuclides by inductively coupled plasma mass spectrometry will be described. Solutions that overcome these issues will be discussed, highlighting their pros and cons and assessing their impact on the measurement of environmental radioactivity. Among the solutions proposed, mass and chemical resolution through the use of sector-field instruments and chemical reactions/collisions in a pressurized cell, respectively, will be described. Other methods, such as unique sample introduction equipment (e.g., laser ablation, electrothermal vaporisation, high efficiency nebulization) and instrumental modifications/optimizations (e.g., instrumental vacuum, radiofrequency power, guard electrode) that improve sensitivity and performance

  2. Influence of atomic force microscope tip-sample interaction on the study of scaling behavior

    NARCIS (Netherlands)

    Aue, J.; de Hosson, J.T.M.

    1997-01-01

    Images acquired with atomic force microscopy are based on tip-sample interaction. It is shown that using scanning probe techniques for determining scaling parameters of a surface leads to an underestimate of the actual scaling dimension, due to the dilation of tip and surface. How much we

  3. Determination of indium in geological materials by electrothermal-atomization atomic absorption spectrometry with a tungsten-impregnated graphite furance

    Science.gov (United States)

    Zhou, L.; Chao, T.T.; Meier, A.L.

    1984-01-01

    The sample is fused with lithium metaborate and the melt is dissolved in 15% (v/v) hydrobromic acid. Iron(III) is reduced with ascorbic acid to avoid its coextraction with indium as the bromide into methyl isobutyl ketone. Impregnation of the graphite furnace with sodium tungstate, and the presence of lithium metaborate and ascorbic acid in the reaction medium improve the sensitivity and precision. The limits of determination are 0.025-16 mg kg-1 indium in the sample. For 22 geological reference samples containing more than 0.1 mg kg-1 indium, relative standard deviations ranged from 3.0 to 8.5% (average 5.7%). Recoveries of indium added to various samples ranged from 96.7 to 105.6% (average 100.2%). ?? 1984.

  4. Determination of sulfur in coal and ash slurry by high-resolution continuum source electrothermal molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nakadi, Flávio V.; Rosa, Lilian R.; Veiga, Márcia A.M.S. da, E-mail: mamsveiga@ffclrp.usp.br

    2013-10-01

    We propose a procedure for the determination of sulfur in coal slurries by high resolution continuum source electrothermal molecular absorption spectrometry. The slurry, whose concentration is 1 mg mL{sup −1}, was prepared by mixing 50 mg of the sample with 5% v/v nitric acid and 0.04% m/v Triton X-100 and was homogenized manually. It sustained good stability. The determination was performed via CS molecular absorption at 257.592 nm, and the optimized vaporization temperature was 2500 °C. The accuracy of the method was ensured by analysis of certified reference materials SRM 1632b (trace elements in coal) and SRM 1633b (coal fly ash) from the National Institute of Standards and Technology, using external calibration with aqueous standards prepared in the same medium and used as slurry. We achieved good agreement with the certified reference materials within 95% confidence interval, LOD of 0.01% w/w, and RSD of 6%, which confirms the potential of the proposed method. - Highlights: • HR-CS ET MAS as a technique to determine sulfur in coal and ash • Utilization of (coal and coal fly ash) slurry as a sample preparation • Simple and fast method, which uses external calibration with aqueous standards without chemical modifier.

  5. Compact electro-thermal modeling of a SiC MOSFET power module under short-circuit conditions

    DEFF Research Database (Denmark)

    Ceccarelli, Lorenzo; Reigosa, Paula Diaz; Bahman, Amir Sajjad

    2017-01-01

    A novel physics-based, electro-thermal model which is capable of estimating accurately the short-circuit behavior and thermal instabilities of silicon carbide MOSFET multi-chip power modules is proposed in this paper. The model has been implemented in PSpice and describes the internal structure.......2 kV breakdown voltage and about 300 A rated current. The short-circuit behavior of the module is investigated experimentally through a non-destructive test setup and the model is validated. The estimation of overcurrent and temperature distribution among the chips can provide useful information...

  6. On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yebra, M.C.; Moreno-Cid, A.

    2003-01-01

    Manganese is extracted on-line from solid seafood samples by a simple continuous ultrasound-assisted extraction system (CUES). This system is connected to an on-line manifold, which permits the flow-injection flame atomic absorption spectrometric determination of manganese. Optimisation of the continuous leaching procedure is performed by an experimental design. The proposed method allows the determination of manganese with a relative standard deviation of 0.9% for a sample containing 23.4 μg g -1 manganese (dry mass). The detection limit is 0.4 μg g -1 (dry mass) for 30 mg of sample and the sample throughput is ca. 60 samples per hour. Accurate results are obtained by measuring TORT-1 certified reference material. The procedure is finally applied to mussel, tuna, sardine and clams samples

  7. Automated Sampling and Extraction of Krypton from Small Air Samples for Kr-85 Measurement Using Atom Trap Trace Analysis

    International Nuclear Information System (INIS)

    Hebel, S.; Hands, J.; Goering, F.; Kirchner, G.; Purtschert, R.

    2015-01-01

    Atom-Trap-Trace-Analysis (ATTA) provides the capability of measuring the Krypton-85 concentration in microlitre amounts of krypton extracted from air samples of about 1 litre. This sample size is sufficiently small to allow for a range of applications, including on-site spot sampling and continuous sampling over periods of several hours. All samples can be easily handled and transported to an off-site laboratory for ATTA measurement, or stored and analyzed on demand. Bayesian sampling methodologies can be applied by blending samples for bulk measurement and performing in-depth analysis as required. Prerequisite for measurement is the extraction of a pure krypton fraction from the sample. This paper introduces an extraction unit able to isolate the krypton in small ambient air samples with high speed, high efficiency and in a fully automated manner using a combination of cryogenic distillation and gas chromatography. Air samples are collected using an automated smart sampler developed in-house to achieve a constant sampling rate over adjustable time periods ranging from 5 minutes to 3 hours per sample. The smart sampler can be deployed in the field and operate on battery for one week to take up to 60 air samples. This high flexibility of sampling and the fast, robust sample preparation are a valuable tool for research and the application of Kr-85 measurements to novel Safeguards procedures. (author)

  8. Electrothermal impedance spectroscopy measurement on high power LiMO2/Li4Ti5O12 battery cell with low bandwidth test setup

    DEFF Research Database (Denmark)

    Swierczynski, Maciej Jozef; Stroe, Daniel Loan; Stanciu, Tiberiu

    2015-01-01

    be executed on-line (e.g. in the electric vehicle Battery Management System). The Electrothermal Impedance Spectroscopy (ETIS) can be used as a relatively simple and fast method for non-destructive parametrization of the battery thermal models. However, the ETIS requires expensive galvanostat with high...

  9. Introduction of Flame Atomic Absorption Spectrometry (FAAS) For River Water Samples Analysis

    International Nuclear Information System (INIS)

    Shakirah Abd Shukor; Mohd Suhaimi Hamzah; Shamsiah Abdul Rahman

    2015-01-01

    Metal contamination in water is a major component in the determination of water quality monitoring. In spite of the viability of several other metal ion analysis techniques for river water, atomic absorption spectroscopy (AAS) method is most commonly used due to the reproducibility results, short analysis time, cost effective, lower level detection and robust. Therefore, this article gives an overview on the principles, instrumentation techniques, sample preparations, instrument calibration and data analysis in a simple manner for beginner. (author)

  10. Flow analysis by using solenoid valves for As(III determination in natural waters by an on-line separation and pre-concentration system coupled to a tungsten coil atomizer

    Directory of Open Access Journals (Sweden)

    José Y. Neira

    2005-03-01

    Full Text Available A flow system coupled to a tungsten coil atomizer in an atomic absorption spectrometer (TCA-AAS was developed for As(III determination in waters, by extraction with sodium diethyldithiocarbamate (NaDDTC as complexing agent, and by sorption of the As(III-DDTC complex in a micro-column filled with 5 mg C18 reversed phase (10 µL dry sorbent, followed by elution with ethanol. A complete pre-concentration/elution cycle took 208 s, with 30 s sample load time (1.7 mL and 4 s elution time (71 µL. The interface and software for the synchronous control of two peristaltic pumps (RUN/ STOP, an autosampler arm, seven solenoid valves, one injection valve, the electrothermal atomizer and the spectrometer Read function were constructed. The system was characterized and validated by analytical recovery studies performed both in synthetic solutions and in natural waters. Using a 30 s pre-concentration period, the working curve was linear between 0.25 and 6.0 µg L-1 (r = 0.9976, the retention efficiency was 94±1% (6.0 µg L-1, and the pre-concentration coefficient was 28.9. The characteristic mass was 58 pg, the mean repeatability (expressed as the variation coefficient was 3.4% (n=5, the detection limit was 0.058 µg L-1 (4.1 pg in 71 µL of eluate injected into the coil, and the mean analytical recovery in natural waters was 92.6 ± 9.5 % (n=15. The procedure is simple, economic, less prone to sample loss and contamination and the useful lifetime of the micro-column was between 200-300 pre-concentration cycles.

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

    Science.gov (United States)

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

    2011-01-01

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

  12. Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

    Energy Technology Data Exchange (ETDEWEB)

    Karadjova, Irina B. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria); Lampugnani, Leonardo [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy)]. E-mail: lampugnani@ipcf.cnr.it; Onor, Massimo [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy); D' Ulivo, Alessandro [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy); Tsalev, Dimiter L. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria)

    2005-07-15

    Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 {mu}g l{sup -1} As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 {mu}g l{sup -1}. Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l{sup -1} acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l{sup -1} HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 {mu}g l{sup -1} for As(III) and 0.3 {mu}g l{sup -1} for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 {mu}g l{sup -1} (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non

  13. Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

    International Nuclear Information System (INIS)

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

    2005-01-01

    Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 μg l -1 As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 μg l -1 . Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l -1 acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l -1 HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 μg l -1 for As(III) and 0.3 μg l -1 for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 μg l -1 (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non-chromatographic and chromatographic procedures and the As

  14. A novel electro-thermal model for wide bandgap semiconductor based devices

    DEFF Research Database (Denmark)

    Sintamarean, Nicolae Christian; Blaabjerg, Frede; Wang, Huai

    2013-01-01

    This paper propose a novel Electro-Thermal Model for the new generation of power electronics WBG-devices (by considering the SiC MOSFET-CMF20120D from CREE), which is able to estimate the device junction and case temperature. The Device-Model estimates the voltage drop and the switching energies...... by considering the device current, the off-state blocking voltage and junction temperature variation. Moreover, the proposed Thermal-Model is able to consider the thermal coupling within the MOSFET and its freewheeling diode, integrated into the same package, and the influence of the ambient temperature...... variation. The importance of temperature loop feedback in the estimation accuracy of device junction and case temperature is studied. Furthermore, the Safe Operating Area (SOA) of the SiC MOSFET is determined for 2L-VSI applications which are using sinusoidal PWM. Thus, by considering the heatsink thermal...

  15. Current role of ICP-MS in clinical toxicology and forensic toxicology: a metallic profile.

    Science.gov (United States)

    Goullé, Jean-Pierre; Saussereau, Elodie; Mahieu, Loïc; Guerbet, Michel

    2014-08-01

    As metal/metalloid exposure is inevitable owing to its omnipresence, it may exert toxicity in humans. Recent advances in metal/metalloid analysis have been made moving from flame atomic absorption spectrometry and electrothermal atomic absorption spectrometry to the multi-elemental inductively coupled plasma (ICP) techniques as ICP atomic emission spectrometry and ICP-MS. ICP-MS has now emerged as a major technique in inorganic analytical chemistry owing to its flexibility, high sensitivity and good reproducibility. This in depth review explores the ICP-MS metallic profile in human toxicology. It is now routinely used and of great importance, in clinical toxicology and forensic toxicology to explore biological matrices, specifically whole blood, plasma, urine, hair, nail, biopsy samples and tissues.

  16. Atomic absorption determination of metals in soils using ultrasonic sample preparation

    International Nuclear Information System (INIS)

    Chmilenko, F.A.; Smityuk, N.M.; Baklanov, A.N.

    2002-01-01

    It was shown that ultrasonic treatment accelerates sample preparation of soil extracts from chernozem into different solvents by a factor of 6 to 60. These extracts are used for the atomic absorption determination of soluble species of Cd, Co, Cr, Cu, Ni, Pb, and Zn. The optimum ultrasound parameters (frequency, intensity, and treatment time) were found for preparing soil extracts containing analytes in concentrations required in agrochemical procedures. Different extractants used to extract soluble heavy metals from soils of an ordinary chernozem type in agrochemical procedures using ultrasonic treatment were classified in accordance with the element nature [ru

  17. Determination of lead in whole blood: Comparison of the LeadCare blood lead testing system with zeeman longitudinal electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Pineau, A.; Viallefont, A.; Fauconneau, B.; Rafael, M.; Guillard, O.

    2002-01-01

    This study compares the efficiency of blood lead level analysis by graphite furnace atomic absorption spectrometry (GFAAS) and the portable LeadCare Blood lead testing system (LCS). Recoveries of two added lead concentrations of 22 and 42 μg/dL ranged from 102.4 to 105.5% for LCS and from 96.3 to 97.2% for GFAAS. Measurement of a certified sample (Certified Danish Whole Blood) at a blood lead concentration of 26.2 μg/dL gave within- and between-run coefficients of variation which were both approximately 8% by LCS and 2% by GFAAS. Comparison of the tested method (LCS) versus GFAAS from analysis of 76 samples of blood lead collected from workers in different industrial sectors showed imperfect overall correlation (r = 0.95). The LCS is quite suitable for screening purposes, but requires the use of non-frozen blood collected less than 24 h before. Conservative threshold values should be applied when using the LCS for initial screening in the field. (orig.)

  18. Mass transport in Ti0.5Sb2Te3 phase-change nanobridge

    International Nuclear Information System (INIS)

    Ji, Xinglong; Wu, Liangcai; Lv, Shilong; Rao, Feng; Zhu, Min; Song, Zhitang; Zhou, Xilin; Feng, Songlin

    2014-01-01

    Investigation of atomic migration behavior in nanoscale phase-change material is very valuable for phase-change memory applications. In this work, Ti 0.5 Sb 2 Te 3 -based phase-change nanobridges were fabricated and mass transport by atomic migration was studied. A 3-D finite-element simulation on the electrothermal field was introduced to describe the electrothermal environment in the phase-change region. During the nanosecond operation, an obvious compositional distribution resulting from atomic migration was observed in the Ti 0.5 Sb 2 Te 3 phase-change nanobridge. Based on the mass continuity equation, a physical model for mass transport is proposed to illustrate that the density variation during the amorphous-to-crystalline structural transformation is the main reason for the atomic migration in nanoscale Ti 0.5 Sb 2 Te 3 phase-change material

  19. Neutron-induced {sup 63}Ni activity and microscopic observation of copper samples exposed to the Hiroshima atomic bomb

    Energy Technology Data Exchange (ETDEWEB)

    Shizuma, Kiyoshi, E-mail: shizuma@hiroshima-u.ac.jp [Quantum Energy Applications, Department of Mechanical Science and Engineering, Graduate School of Engineering, Hiroshima University, Higashi-Hiroshima 739-8527 (Japan); Endo, Satoru [Quantum Energy Applications, Department of Mechanical Science and Engineering, Graduate School of Engineering, Hiroshima University, Higashi-Hiroshima 739-8527 (Japan); Shinozaki, Kenji [Materials Joining Science and Engineering, Department of Mechanical Science and Engineering, Graduate School of Engineering, Hiroshima University, Higashi-Hiroshima 739-8527 (Japan); Fukushima, Hiroshi [Materials Physics, Department of Mechanical Science and Engineering, Graduate School of Engineering, Hiroshima University, Higashi-Hiroshima 739-8527 (Japan)

    2013-05-01

    Fast neutron activation data for {sup 63}Ni in copper samples exposed to the Hiroshima atomic bomb are important in evaluating neutron doses to the survivors. Up to until now, accelerator mass spectrometry and liquid scintillation counting methods have been applied in {sup 63}Ni measurements and data were accumulated within 1500 m from the hypocenter. The slope of the activation curve versus distance shows reasonable agreement with the calculation result, however, data near the hypocenter are scarce. In the present work, two copper samples obtained from the Atomic bomb dome (155 m from the hypocenter) and the Bank of Japan building (392 m) were utilized in {sup 63}Ni beta-ray measurement with a Si surface barrier detector. Additionally, microscopic observation of the metal surfaces was performed for the first time. Only upper limit of {sup 63}Ni production was obtained for copper sample of the Atomic bomb dome. The result of the {sup 63}Ni measurement for Bank of Japan building show reasonable agreement with the AMS measurement and to fast neutron activation calculations based on the Dosimetry System 2002 (DS02) neutrons.

  20. Visualization and automatic detection of defect distribution in GaN atomic structure from sampling Moiré phase.

    Science.gov (United States)

    Wang, Qinghua; Ri, Shien; Tsuda, Hiroshi; Kodera, Masako; Suguro, Kyoichi; Miyashita, Naoto

    2017-09-19

    Quantitative detection of defects in atomic structures is of great significance to evaluating product quality and exploring quality improvement process. In this study, a Fourier transform filtered sampling Moire technique was proposed to visualize and detect defects in atomic arrays in a large field of view. Defect distributions, defect numbers and defect densities could be visually and quantitatively determined from a single atomic structure image at low cost. The effectiveness of the proposed technique was verified from numerical simulations. As an application, the dislocation distributions in a GaN/AlGaN atomic structure in two directions were magnified and displayed in Moire phase maps, and defect locations and densities were detected automatically. The proposed technique is able to provide valuable references to material scientists and engineers by checking the effect of various treatments for defect reduction. © 2017 IOP Publishing Ltd.

  1. Effect of impurities in the electrothermic instability

    International Nuclear Information System (INIS)

    Azevedo, M.T. de.

    1982-04-01

    It is proposed a model for a ''impure'' plasma based on the homogenous hydrogen plasma used in the theory formulated by Tomimura and Haines to explain the increasing of instable electrothermal modes with wave vector perpendicular to the applyed magnetic field. The impurities are implicity introduced in the transport coeficients of the model of two fluids through the effective charge number Z eff as suggested by Duechs et al., Furth etc... The results obtained are: (i) the greatest increasing ratio for the absolute mode (non-convective) decreases with the increasing of Z eff going to zero for a given value of these parameter which is denominated Z crit ; (ii) the wavelenght associated with that greatest ratio of increasing decreases with the increasing of Z eff ; (iii) Z crit x T eo /T io curves, where T eo and T io are the electronic and ionic temperatures of equilibri um show that, for each value of T eo (used as a parameter) there is a limiting value Z crit from which the plasma is stable, independently of the temperature ratio. The correlation of these results with that of a difuse pinch model, which shows the tendency in assume in the stationary state a filamental current structure is inconclusive with respect to the Z eff dependence. (M.W.O.) [pt

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

    Science.gov (United States)

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

    2008-01-01

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

  3. Computer model for the recombination zone of a microwave-plasma electrothermal rocket

    Energy Technology Data Exchange (ETDEWEB)

    Filpus, J.W.; Hawley, M.C.

    1987-01-01

    As part of a study of the microwave-plasma electrothermal rocket, a computer model of the flow regime below the plasma has been developed. A second-order model, including axial dispersion of energy and material and boundary conditions at infinite length, was developed to partially reproduce the absence of mass-flow rate dependence that was seen in experimental temperature profiles. To solve the equations of the model, a search technique was developed to find the initial derivatives. On integrating with a trial set of initial derivatives, the values and their derivatives were checked to judge whether the values were likely to attain values outside the practical regime, and hence, the boundary conditions at infinity were likely to be violated. Results are presented and directions for further development are suggested. 17 references.

  4. Imaging contrast and tip-sample interaction of non-contact amplitude modulation atomic force microscopy with Q -control

    International Nuclear Information System (INIS)

    Shi, Shuai; Guo, Dan; Luo, Jianbin

    2017-01-01

    Active quality factor ( Q ) exhibits many promising properties in dynamic atomic force microscopy. Energy dissipation and image contrasts are investigated in the non-contact amplitude modulation atomic force microscopy (AM-AFM) with an active Q -control circuit in the ambient air environment. Dissipated power and virial were calculated to compare the highly nonlinear interaction of tip-sample and image contrasts with different Q gain values. Greater free amplitudes and lower effective Q values show better contrasts for the same setpoint ratio. Active quality factor also can be employed to change tip-sample interaction force in non-contact regime. It is meaningful that non-destructive and better contrast images can be realized in non-contact AM-AFM by applying an active Q -control to the dynamic system. (paper)

  5. Non-linear Calibration Leads to Improved Correspondence between Uncertainties

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    2007-01-01

    limit theorem, an excellent correspondence was obtained between predicted uncertainties and measured uncertainties. In order to validate the method, experiments were applied of flame atomic absorption spectrometry (FAAS) for the analysis of Co and Pt, and experiments of electrothermal atomic absorption...

  6. Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Jian [State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, Xiamen 361102 (China); Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States); Sengupta, Mrinal K. [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States); Thermo Fisher Scientific, Dionex Products, 445 Lakeside Drive, Sunnyvale, CA, 94085 (United States); Yuan, Dongxing [State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, Xiamen 361102 (China); Dasgupta, Purnendu K., E-mail: Dasgupta@uta.edu [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States)

    2014-06-01

    Highlights: • Compilation of principal official documents and major review articles, including the toxicology and chemistry of As. • Review of non-atomic spectrometric methods for speciation and detection of arsenic in aqueous samples (2005–2013) of the performance of field-usable methods. - Abstract: Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been

  7. Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

    International Nuclear Information System (INIS)

    Ma, Jian; Sengupta, Mrinal K.; Yuan, Dongxing; Dasgupta, Purnendu K.

    2014-01-01

    Highlights: • Compilation of principal official documents and major review articles, including the toxicology and chemistry of As. • Review of non-atomic spectrometric methods for speciation and detection of arsenic in aqueous samples (2005–2013) of the performance of field-usable methods. - Abstract: Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been

  8. The use of atomic absorption spectroscopy to measure arsenic, selenium, molybdenum, and vanadium in water and soil samples from uranium mill tailings sites

    International Nuclear Information System (INIS)

    Hollenbach, M.H.

    1988-01-01

    The Technical Measurements Center (TMC) was established to support the environmental measurement needs of the various DOE remedial action programs. A laboratory intercomparison study conducted by the TMC, using soil and water samples from sites contaminated by uranium mill tailings, indicated large discrepancies in analytical results reported by participating laboratories for arsenic, selenium, molybdenum, and vanadium. The present study was undertaken to investigate the most commonly used analytical techniques for measuring these four elements, ascertain routine and reliable quantification, and assess problems and successes of analysts. Based on a survey of the technical literature, the analytical technique of atomic absorption spectroscopy was selected for detailed study. The application of flame atomic absorption, graphite furnace atomic absorption, and hydride generation atomic absorption to the analysis of tailings-contaminated samples is discussed. Additionally, laboratory sample preparation methods for atomic absorption spectroscopy are presented. The conclusion of this report is that atomic absorption can be used effectively for the determination of arsenic, selenium, molybdenum, and vanadium in water and soil samples if the analyst understands the measurement process and is aware of potential problems. The problem of accurate quantification of arsenic, selenium, molybdenum, and vanadium in water and soil contaminated by waste products from uranium milling operations affects all DOE remedial action programs [Surplus Facilities Management Program (SFMP), Formerly Utilized Site Remedial Action Program (FUSRAP), and Uranium Mill Tailings Remedial Action Program (UMTRAP)], since all include sites where uranium was processed. 96 refs., 9 figs

  9. Microstructural evolution and mechanical properties of differently heat-treated binder jet printed samples from gas- and water-atomized alloy 625 powders

    International Nuclear Information System (INIS)

    Mostafaei, Amir; Toman, Jakub; Stevens, Erica L.; Hughes, Eamonn T.; Krimer, Yuval L.; Chmielus, Markus

    2017-01-01

    In this study, we investigate the effect of powders resulting from different atomization methods on properties of binder jet printed and heat-treated samples. Air-melted gas atomized (GA) and water atomized (WA) nickel-based alloy 625 powders were used to binder jet print samples for a detailed comparative study on microstructural evolution and mechanical properties. GA printed samples achieved higher sintering density (99.2%) than WA samples (95.0%) due to differences in powder morphology and chemistry. Grain sizes of GA and WA samples at their highest density were 89 ± 21 μm and 88 ± 26 μm, respectively. Mechanical tests were conducted on optimally sintered samples and sintered plus aged samples; aging further improved microstructure and mechanical properties. This study shows that microstructural evolution (densification, and carbide, oxide and intermetallic phase formation) is very different for GA and WA binder jet printed and heat-treated samples. This difference in microstructural evolution results in different mechanical properties with the superior sintered and aged GA specimen reaching a hardness of 327 ± 7 HV_0_._1, yield strength of 394 ± 15 MPa, and ultimate tensile strength of 718 ± 14 MPa which are higher than cast alloy 625 values.

  10. Determinação de baixas concentrações de cobre em águas naturais por espectrofotometria de absorção atômica em chama usando um sistema SIA com uma coluna de poli(etilenimina

    Directory of Open Access Journals (Sweden)

    Costa Rui Cerdeira de Campos

    2001-01-01

    Full Text Available This paper describes a sequential injection analysis (SIA set-up coupled to a flame atomic absorption spectrometer (FAAS to accomplish the determination of low concentrations of copper in drinking waters. Copper is first retained under neutral media in an on-line 29x1.6 mm column filled with poly(ethylenimine immobilised on silica gel. The retained analyte is then eluted by flowing through the column 250 mL of a nitric acid solution. The selection of 3.85 ml of sample enabled to obtain a detection limit of 0.27 mug/L and a sampling rate of about 24 samples/h. There was a good agrement between the results of 12 samples furnished by the proposed procedure and by electrothermal atomic absorption spectrometry. Repeatability assessment gave a relative standard deviation of 1.3 % after ten replicate analysis of a sample containing about 70 mug/L in copper..

  11. Experimental observation of the stratified electrothermal instability on aluminum with thickness greater than a skin depth

    Science.gov (United States)

    Hutchinson, T. M.; Awe, T. J.; Bauer, B. S.; Yates, K. C.; Yu, E. P.; Yelton, W. G.; Fuelling, S.

    2018-05-01

    A direct observation of the stratified electrothermal instability on the surface of thick metal is reported. Aluminum rods coated with 70 μ m Parylene-N were driven to 1 MA in 100 ns , with the metal thicker than the skin depth. The dielectric coating suppressed plasma formation, enabling persistent observation of discrete azimuthally correlated stratified thermal perturbations perpendicular to the current whose wave numbers, k , grew exponentially with rate γ (k ) =0.06 n s-1-(0.4 n s-1μ m2ra d-2 ) k2 in ˜1 g /c m3 , ˜7000 K aluminum.

  12. Experimental Observation of the Stratified Electrothermal Instability on Aluminum with Thickness Greater than a Skin Depth

    Energy Technology Data Exchange (ETDEWEB)

    Hutchinson, Trevor M. [Univ. of Nevada, Reno, NV (United States); Hutchinson, Trevor M. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Awe, Thomas James [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Bauer, Bruno S. [Univ. of Nevada, Reno, NV (United States); Yates, Kevin [Univ. of New Mexico, Albuquerque, NM (United States); Yu, Edmund p. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Yelton, William G. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Fuelling, Stephan [Univ. of Nevada, Reno, NV (United States)

    2017-07-01

    The first direct observation of the stratified electrothermal instability on the surface of thick metal is reported. Aluminum rods coated with 70 μm Parylene-N were driven to 1 MA in approximately 100 ns, with the metal thicker than the skin depth. The dielectric coating suppressed plasma formation, enabling persistent observation of discrete azimuthally-correlated stratified structures perpendicular to the current. Strata amplitudes grow rapidly, while their Fourier spectrum shifts toward longer wavelength. Assuming blackbody emission, radiometric calculations indicate strata are temperature perturbations that grow exponentially with rate γ = 0.04 ns -1 in 3000- 10,000 K aluminum.

  13. An analytical model for pulse shape and electrothermal stability in two-body transition-edge sensor microcalorimeters

    International Nuclear Information System (INIS)

    Bennett, D. A.; Horansky, R. D.; Schmidt, D. R.; Swetz, D. S.; Vale, L. R.; Ullom, J. N.; Hoover, A. S.; Hoteling, N. J.; Rabin, M. W.

    2010-01-01

    High-resolution superconducting gamma-ray sensors show potential for the more accurate analysis of nuclear material. These devices are part of a larger class of microcalorimeters and bolometers based on transition edge sensors (TESs) that have two distinct thermal bodies. We derive the time domain behavior of the current and temperature for compound TES devices in the small signal limit and demonstrate the utility of these equations for device design and characterization. In particular, we use the model to fit pulses from our gamma-ray microcalorimeters and demonstrate how critical damping and electrothermal stability can be predicted.

  14. Modeling the capillary discharge of an electrothermal (ET) launcher

    Science.gov (United States)

    Least, Travis

    Over the past few decades, different branches of the US Department of Defense (DoD) have invested at improving the field ability of electromagnetic launchers. One such focus has been on achieving hypervelocity launch velocities in excess of 7 km/s for direct launch to space applications [1]. It has been shown that pre-injection is required for this to be achieved. One method of pre-injection which has promise involves using an electro-thermal (ET) due to its ability to achieve the desired velocities with a minimal amount of hot plasma injected into the launcher behind the projectile. Despite the demonstration of pre-injection using this method, polymer ablation is not very well known and this makes it challenging to predict how the system will behave for a given input of electrical power. In this work, the rate of ablation has been studied and predicted using different models to generate the best possible characteristic curve. [1] - Wetz, David A., Francis Stefani, Jerald V. Parker, and Ian R. McNab. "Advancements in the Development of a Plasma-Driven Electromagnetic Launcher." IEEE TRANSACTIONS ON MAGNETICS 45.1 (2009): 495--500. IEEE Xplore. Web. 18 Aug. 2012.

  15. Organic palladium and palladium-magnesium chemical modifiers in direct determination of lead in fractions from distillation of crude oil by electrothermal atomic absorption analysis

    Science.gov (United States)

    Kowalewska, Zofia; Bulska, Ewa; Hulanicki, Adam

    1999-05-01

    Platinum reforming catalysts are easily poisoned by increased levels of lead, therefore a sensitive atomic absorption spectrometric procedure for lead determination in fractions from crude oil distillation was developed. Lead was present in organic form in the samples analysed therefore the behaviour of various lead compounds (Pb-alkylarylsulphonate, Pb-4-cyclohexanobutyrate, tetraethyllead, Pb in fuel oil) was studied. The best procedure for the determination of lead in different petroleum products, including those containing asphaltenes includes a pretreatment with iodine and methyltrioctylammonium chloride, followed by the use of an organic Pd-Mg modifier. Under these conditions an effective matrix removal is possible at a pyrolysis temperature up to approximately 1100°C and the behaviour of lead present in different forms is unified. The characteristic mass is 11-12 pg Pb, corresponding to a detection limit of 0.25 ng g -1 for 20 μl sample solution. This can be lowered by multiple injection.

  16. Electro-thermal modelling of anode and cathode in micro-EDM

    International Nuclear Information System (INIS)

    Yeo, S H; Kurnia, W; Tan, P C

    2007-01-01

    Micro-electrical discharge machining is an evolution of conventional EDM used for fabricating three-dimensional complex micro-components and microstructure with high precision capabilities. However, due to the stochastic nature of the process, it has not been fully understood. This paper proposes an analytical model based on electro-thermal theory to estimate the geometrical dimensions of micro-crater. The model incorporates voltage, current and pulse-on-time during material removal to predict the temperature distribution on the workpiece as a result of single discharges in micro-EDM. It is assumed that the entire superheated area is ejected from the workpiece surface while only a small fraction of the molten area is expelled. For verification purposes, single discharge experiments using RC pulse generator are performed with pure tungsten as the electrode and AISI 4140 alloy steel as the workpiece. For the pulse-on-time range up to 1000 ns, the experimental and theoretical results are found to be in close agreement with average volume approximation errors of 2.7% and 6.6% for the anode and cathode, respectively

  17. Electro-thermal modelling of anode and cathode in micro-EDM

    Energy Technology Data Exchange (ETDEWEB)

    Yeo, S H; Kurnia, W; Tan, P C [School of Mechanical and Aerospace Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 (Singapore)

    2007-04-21

    Micro-electrical discharge machining is an evolution of conventional EDM used for fabricating three-dimensional complex micro-components and microstructure with high precision capabilities. However, due to the stochastic nature of the process, it has not been fully understood. This paper proposes an analytical model based on electro-thermal theory to estimate the geometrical dimensions of micro-crater. The model incorporates voltage, current and pulse-on-time during material removal to predict the temperature distribution on the workpiece as a result of single discharges in micro-EDM. It is assumed that the entire superheated area is ejected from the workpiece surface while only a small fraction of the molten area is expelled. For verification purposes, single discharge experiments using RC pulse generator are performed with pure tungsten as the electrode and AISI 4140 alloy steel as the workpiece. For the pulse-on-time range up to 1000 ns, the experimental and theoretical results are found to be in close agreement with average volume approximation errors of 2.7% and 6.6% for the anode and cathode, respectively.

  18. Electro-thermal modelling of anode and cathode in micro-EDM

    Science.gov (United States)

    Yeo, S. H.; Kurnia, W.; Tan, P. C.

    2007-04-01

    Micro-electrical discharge machining is an evolution of conventional EDM used for fabricating three-dimensional complex micro-components and microstructure with high precision capabilities. However, due to the stochastic nature of the process, it has not been fully understood. This paper proposes an analytical model based on electro-thermal theory to estimate the geometrical dimensions of micro-crater. The model incorporates voltage, current and pulse-on-time during material removal to predict the temperature distribution on the workpiece as a result of single discharges in micro-EDM. It is assumed that the entire superheated area is ejected from the workpiece surface while only a small fraction of the molten area is expelled. For verification purposes, single discharge experiments using RC pulse generator are performed with pure tungsten as the electrode and AISI 4140 alloy steel as the workpiece. For the pulse-on-time range up to 1000 ns, the experimental and theoretical results are found to be in close agreement with average volume approximation errors of 2.7% and 6.6% for the anode and cathode, respectively.

  19. Design and Simulation of an Electrothermal Actuator Based Rotational Drive

    Science.gov (United States)

    Beeson, Sterling; Dallas, Tim

    2008-10-01

    As a participant in the Micro and Nano Device Engineering (MANDE) Research Experience for Undergraduates program at Texas Tech University, I learned how MEMS devices operate and the limits of their operation. Using specialized AutoCAD-based design software and the ANSYS simulation program, I learned the MEMS fabrication process used at Sandia National Labs, the design limitations of this process, the abilities and drawbacks of micro devices, and finally, I redesigned a MEMS device called the Chevron Torsional Ratcheting Actuator (CTRA). Motion is achieved through electrothermal actuation. The chevron (bent-beam) actuators cause a ratcheting motion on top of a hub-less gear so that as voltage is applied the CTRA spins. The voltage applied needs to be pulsed and the frequency of the pulses determine the angular frequency of the device. The main objective was to design electromechanical structures capable of transforming the electrical signals into mechanical motion without overheating. The design was optimized using finite element analysis in ANSYS allowing multi-physics simulations of our model system.

  20. Micro-sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry for calcium determination in blood and mitochondrial suspensions.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Satrústegui, Jorgina; Procopio, Jesús R

    2017-08-01

    A micro-sampling and straightforward method based on high resolution continuum source atomic absorption spectrometry (HR-CS AAS) was developed to determine extracellular and intracellular Ca in samples of interest in clinical and biomedical analysis. Solid sampling platforms were used to introduce the micro-samples into the graphite furnace atomizer. The secondary absorption line for Ca, located at 239.856nm, was selected to carry out the measurements. Experimental parameters such as pyrolysis and atomization temperatures and the amount of sample introduced for the measurements were optimized. Calibration was performed using aqueous standards and the approach to measure at the wings of the absorption lines was employed for the expansion of the linear response range. The limit of detection was of 0.02mgL -1 Ca (0.39ng Ca) and the upper limit of linear range was increased up to 8.0mgL -1 Ca (160ng Ca). The proposed method was used to determine Ca in mitochondrial suspensions and whole blood samples with successful results. Adequate recoveries (within 91-107%) were obtained in the tests performed for validation purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. All-atom simulation study of protein PTH(1-34) by using the Wang-Landau sampling method

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seung-Yeon [Korea National University of Transportation, Chungju (Korea, Republic of); Kwak, Woo-Seop [Chosun University, Gwangju (Korea, Republic of)

    2014-12-15

    We perform simulations of the N-terminal 34-residue protein fragment PTH(1-34), consisting of 581 atoms, of the 84-residue human parathyroid hormone by using the all-atom ECEPP/3 force field and the Wang-Landau sampling method. Through a massive high-performance computation, the density of states and the partition function Z(T), as a continuous function of T, are obtained for PTH(1-34). From the continuous partition function Z(T), the partition function zeros of PTH(1-34) are evaluated for the first time. From both the specific heat and the partition function zeros, two characteristic transition temperatures are obtained for the all-atom protein PTH(1-34). The higher transition temperature T{sub 1} and the lower transition temperature T{sub 2} of PTH(1-34) can be interpreted as the collapse temperature T{sub θ} and the folding temperature T{sub f} , respectively.

  2. Design and construction of a heat stage for investigations of samples by atomic force microscopy above ambient temperatures

    DEFF Research Database (Denmark)

    Bækmark, Thomas Rosleff; Bjørnholm, Thomas; Mouritsen, Ole G.

    1997-01-01

    The construction from simple and cheap commercially available parts of a miniature heat stage for the direct heating of samples studied with a commercially available optical-lever-detection atomic force microscope is reported. We demonstrate that by using this heat stage, atomic resolution can...... be obtained on highly oriented pyrolytic graphite at 52 °C. The heat stage is of potential use for the investigation of biological material at physiological temperatures. ©1997 American Institute of Physics....

  3. Electrothermal vaporization inductively coupled plasma-mass spectrometry for the determination of Cr, Cu, Cd, Hg and Pb in rice flour

    International Nuclear Information System (INIS)

    Li, P.-C.; Jiang, S.-J.

    2003-01-01

    Ultrasonic slurry sampling (USS)-electrothermal vaporization (ETV) dynamic reaction cell TM (DRC) inductively coupled plasma-mass spectrometry (ICP-MS) has been applied to determine Cr, Cu, Cd, Hg and Pb in rice samples. The influences of instrument operating conditions and slurry preparation on the ion signals were reported. Ascorbic acid was used as a modifier to enhance the ion signals. The background ions at the chromium masses were reduced in intensity significantly by using 0.4 ml min -1 NH 3 as reaction cell gas in the dynamic reaction cell while a q value of 0.6 was used. Since the sensitivities of Cr, Cu, Cd, Hg and Pb in rice flour slurry and aqueous solution were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Cu, Cd, Hg and Pb in these rice samples. This method has been applied to the determination of Cr, Cu, Cd, Hg and Pb in NIST SRM 1568a rice flour reference material and two rice samples purchased from the market. The analytical results for the reference material agreed with the certified values. The results for the rice samples for which no reference values were available were also found to be in good agreement between the isotope dilution and standard addition methods. The method's detection limits estimated from the standard addition plots were about 0.44, 1.7, 0.4, 0.53 and 0.69 ng g -1 for Cr, Cu, Cd, Hg and Pb, respectively, in the original rice flour

  4. Heavy metals burden of Keenjhar Lake, District Thatta, Sindh, Pakistan

    African Journals Online (AJOL)

    Detection of heavy metals (HMs) content from Keenjhar Lake water was carried out monthly from January to December, 2003. Zinc, chromium, copper, iron, manganese, nickel and cadmium were analyzed by dual mode of analytical methods flame atomic absorption spectrometry and electrothermal atomic absorption ...

  5. Contribution to the electrothermal simulation in power electronics. Development of a simulation methodology applied to switching circuits under variable operating conditions; Contribution a la simulation electrothermique en electronique de puissance. Developpement d`une methode de simulation pour circuits de commutation soumis a des commandes variables

    Energy Technology Data Exchange (ETDEWEB)

    Vales, P.

    1997-03-19

    In modern hybrid or monolithic integrated power circuits, electrothermal effects can no longer be ignored. A methodology is proposed in order to simulate electrothermal effects in power circuits, with a significant reduction of the computation time while taking into account electrical and thermal time constants which are usually widely different. A supervising program, written in Fortran, uses system call sequences and manages an interactive dialog between a fast thermal simulator and a general electrical simulator. This explicit coupling process between two specific simulators requires a multi-task operating system. The developed software allows for the prediction of the electrothermal power dissipation drift in the active areas of components, and the prediction of thermally-induced coupling effects between adjacent components. An application to the study of hard switching circuits working under variable operating conditions is presented

  6. Mercury speciation in environmental solid samples using thermal release technique with atomic absorption detection

    Energy Technology Data Exchange (ETDEWEB)

    Shuvaeva, Olga V. [Institute of Inorganic Chemistry, Academician Lavrent' ev Prospect 3, 630090 Novosbirsk (Russian Federation)], E-mail: olga@che.nsk.su; Gustaytis, Maria A.; Anoshin, Gennadii N. [Institute of Geology and Mineralogy, Siberian Branch of Russian Academy of Sciences, Koptyug Prospect 3, 630090 Novosibirsk (Russian Federation)

    2008-07-28

    A sensitive and very simple method for determination of mercury species in solid samples has been developed involving thermal release analysis in combination with atomic absorption (AAS) detection. The method allows determination of mercury(II) chloride, methylmercury and mercury sulfide at the level of 0.70, 0.35 and 0.20 ng with a reproducibility of the results of 14, 25 and 18%, respectively. The accuracy of the developed assay has been estimated using certified reference materials and by comparison of the results with those of an independent method. The method has been applied for Hg species determination in original samples of lake sediments and plankton.

  7. 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,…

  8. Lead ultra-trace on-line preconcentration and determination using selective solid phase extraction and electrothermal atomic absorption spectrometry: applications in seawaters and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Vereda Alonso, E.; Siles Cordero, M.T.; Garcia de Torres, A.; Cano Pavon, J.M. [University of Malaga, Department of Analytical Chemistry Faculty of Sciences, Malaga (Spain)

    2006-08-15

    In this work, a new chelating resin [1,5-bis (2-pyridyl)-3-sulphophenyl methylene] thiocarbonohydrazide immobilised on aminopropyl-controlled pore glass (550 Aa; PSTH-cpg) was synthesised and packed in a microcolumn which replaced the sample tip of the autosampler arm. The system was applied to the preconcentration of lead. When microliters of 10% HNO{sub 3}, which acts as elution agent, pass through the microcolumn, the preconcentrated Pb(II) is eluted and directly deposited in a tungsten-rhodium coated graphite tube. With the use of the separation and preconcentration step and the permanent modifiers, the analytical characteristics of the technique were improved. The proposed method has a linear calibration range from 0.012 to 10 ng ml{sup -1} of lead. At a sample frequency of 36 h{sup -1} with a 90 s preconcentration time, the enrichment factor was 20.5, the detection and determination limits were 0.012 and 0.14 ng ml{sup -1}, respectively and the precision, expressed as relative standard deviation, was 3.2% (at 1 ng ml{sup -1}). Results from the determination of Pb in biological certified reference materials were in agreement with the certified values. Seawaters and other biological samples were analysed too. (orig.)

  9. Highly selective ionic liquid-based microextraction method for sensitive trace cobalt determination in environmental and biological samples

    International Nuclear Information System (INIS)

    Berton, Paula; Wuilloud, Rodolfo G.

    2010-01-01

    A simple and rapid dispersive liquid-liquid microextraction procedure based on an ionic liquid (IL-DLLME) was developed for selective determination of cobalt (Co) with electrothermal atomic absorption spectrometry (ETAAS) detection. Cobalt was initially complexed with 1-nitroso-2-naphtol (1N2N) reagent at pH 4.0. The IL-DLLME procedure was then performed by using a few microliters of the room temperature ionic liquid (RTIL) 1-hexyl-3-methylimidazolium hexafluorophosphate [C 6 mim][PF 6 ] as extractant while methanol was the dispersant solvent. After microextraction procedure, the Co-enriched RTIL phase was solubilized in methanol and directly injected into the graphite furnace. The effect of several variables on Co-1N2N complex formation, extraction with the dispersed RTIL phase, and analyte detection with ETAAS, was carefully studied in this work. An enrichment factor of 120 was obtained with only 6 mL of sample solution and under optimal experimental conditions. The resultant limit of detection (LOD) was 3.8 ng L -1 , while the relative standard deviation (RSD) was 3.4% (at 1 μg L -1 Co level and n = 10), calculated from the peak height of absorbance signals. The accuracy of the proposed methodology was tested by analysis of a certified reference material. The method was successfully applied for the determination of Co in environmental and biological samples.

  10. On-line ion exchange preconcentration in a sequential injection lab-on-valve microsystem incorporating a renewable column with ETAAS for the trace-level determination of bismuth in urine and river sediment

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2001-01-01

    A sequential injection system for on-line ion-exchange separation and preconcentration of trace-level amounts of metal ions with ensuing detection by electrothermal atomic absorption spectrometry (ETAAS) is described. Based on the use of a renewable microcolumn incorporated within an integrated l.......3% for the determination of 2.0 mug/l Bi (n = 7). The procedure was validated by determination of bismuth in a certified reference material CRM 320 (river sediment), and by bismuth spike recoveries in two human urine samples....

  11. Directed Atom-by-Atom Assembly of Dopants in Silicon.

    Science.gov (United States)

    Hudak, Bethany M; Song, Jiaming; Sims, Hunter; Troparevsky, M Claudia; Humble, Travis S; Pantelides, Sokrates T; Snijders, Paul C; Lupini, Andrew R

    2018-05-17

    The ability to controllably position single atoms inside materials is key for the ultimate fabrication of devices with functionalities governed by atomic-scale properties. Single bismuth dopant atoms in silicon provide an ideal case study in view of proposals for single-dopant quantum bits. However, bismuth is the least soluble pnictogen in silicon, meaning that the dopant atoms tend to migrate out of position during sample growth. Here, we demonstrate epitaxial growth of thin silicon films doped with bismuth. We use atomic-resolution aberration-corrected imaging to view the as-grown dopant distribution and then to controllably position single dopants inside the film. Atomic-scale quantum-mechanical calculations corroborate the experimental findings. These results indicate that the scanning transmission electron microscope is of particular interest for assembling functional materials atom-by-atom because it offers both real-time monitoring and atom manipulation. We envision electron-beam manipulation of atoms inside materials as an achievable route to controllable assembly of structures of individual dopants.

  12. Nursing care for patients receiving percutaneous lumbar discectomy and intradiscal electrothermal treatment for lumbar disc herniation

    International Nuclear Information System (INIS)

    Mou Ling

    2009-01-01

    Objective: To summarize the nursing experience in caring patients with lumbar intervertebral disc herniation who received percutaneous lumbar discectomy (PLD) together with intradiscal electrothermal treatment (IDET) under DSA guidance. Methods: The perioperative nursing care measures carried out in 126 patients with lumbar intervertebral disc herniation who underwent PLD and IDET were retrospectively analyzed. Results: Successful treatment of PLD and IDET was accomplished in 112 cases. Under comprehensive and scientific nursing care and observation, no serious complications occurred. Conclusion: Scientific and proper nursing care is a strong guarantee for a successful surgery and a better recovery in treating lumbar intervertebral disc herniation with PLD and IDET under DSA guidance. (authors)

  13. Solid-phase extraction with slurry injection of the resin into ETAAS for trace determination of thallium in natural water

    International Nuclear Information System (INIS)

    Isoshi, Nukatsuka; Hiroyuki, Seitoh; Kunio, Ohzeki

    2004-01-01

    Thallium in natural water samples was determined by electrothermal atomic absorption spectrometry after 1000-fold enrichment by mini solid-phase extraction from a 100-mL sample solution. A TI-pyrrolidine-1-carbodithioate complex formed in a sample solution of pH 1.6 was extracted on fine particles of a cellulose nitrate resin dispersed in the sample solution. The cellulose nitrate resin was then collected on a membrane filter (25 mm ) by filtration under suction using a glass funnel with an effective filtration area of 0.64 cm 2 . As a result, a circular thin layer of the resin phase with a diameter of 9 mm was obtained. Then the resin phase was carved out by an acrylate resin puncher with a 10-mm hole to put it into a sample cup containing 100 μL of 10 mM HNO 3 containing 0.5 mM NaCl. The resin phase was suspended in the solution by ultrasonication. 1000-fold enrichment was thus attained within 15 min, and the suspension was delivered to electrothermal atomic absorption spectrometry. The linear calibration graph was obtained in the range of 0-4 ng of TI in 100 mL of a sample solution. The detection limit obtained by 3 σ method was 0.19 ng. The proposed method was applied to the determination of TI in natural water samples. The results showed the concentration of TI in seawater was 12.1 ± 1.8 pg mL -1 for the calibration graph method and 12.6 ± 1.4 pg mL -1 for the standard addition method. A snowmelt sample contained 20.7 ± 1.0 pg mL -1 of TI. (author)

  14. Highly Enhanced Electromechanical Stability of Large-Area Graphene with Increased Interfacial Adhesion Energy by Electrothermal-Direct Transfer for Transparent Electrodes.

    Science.gov (United States)

    Kim, Jangheon; Kim, Gi Gyu; Kim, Soohyun; Jung, Wonsuk

    2016-09-07

    Graphene, a two-dimensional sheet of carbon atoms in a hexagonal lattice structure, has been extensively investigated for research and industrial applications as a promising material with outstanding electrical, mechanical, and chemical properties. To fabricate graphene-based devices, graphene transfer to the target substrate with a clean and minimally defective surface is the first step. However, graphene transfer technologies require improvement in terms of uniform transfer with a clean, nonfolded and nontorn area, amount of defects, and electromechanical reliability of the transferred graphene. More specifically, uniform transfer of a large area is a key challenge when graphene is repetitively transferred onto pretransferred layers because the adhesion energy between graphene layers is too low to ensure uniform transfer, although uniform multilayers of graphene have exhibited enhanced electrical and optical properties. In this work, we developed a newly suggested electrothermal-direct (ETD) transfer method for large-area high quality monolayer graphene with less defects and an absence of folding or tearing of the area at the surface. This method delivers uniform multilayer transfer of graphene by repetitive monolayer transfer steps based on high adhesion energy between graphene layers and the target substrate. To investigate the highly enhanced electromechanical stability, we conducted mechanical elastic bending experiments and reliability tests in a highly humid environment. This ETD-transferred graphene is expected to replace commercial transparent electrodes with ETD graphene-based transparent electrodes and devices such as a touch panels with outstanding electromechanical stability.

  15. Direct measurement of axial momentum imparted by an electrothermal radiofrequency plasma micro-thruster

    Science.gov (United States)

    Charles, Christine; Boswell, Roderick; Bish, Andrew; Khayms, Vadim; Scholz, Edwin

    2016-05-01

    Gas flow heating using radio frequency plasmas offers the possibility of depositing power in the centre of the flow rather than on the outside, as is the case with electro-thermal systems where thermal wall losses lower efficiency. Improved systems for space propulsion are one possible application and we have tested a prototype micro-thruster on a thrust balance in vacuum. For these initial tests, a fixed component radio frequency matching network weighing 90 grams was closely attached to the thruster in vacuum with the frequency agile radio frequency generator power being delivered via a 50 Ohm cable. Without accounting for system losses (estimated at around 50%), for a few 10s of Watts from the radio frequency generator the specific impulse was tripled to ˜48 seconds and the thrust tripled from 0.8 to 2.4 milli-Newtons.

  16. Direct measurement of axial momentum imparted by an electrothermal radiofrequency plasma micro-thruster

    Directory of Open Access Journals (Sweden)

    Christine eCharles

    2016-05-01

    Full Text Available Gas flow heating using radio frequency plasmas offers the possibility of depositing power in the centre of the flow rather than on the outside, as is the case with electro-thermal systems where thermal wall losses lower efficiency. Improved systems for space propulsion are one possible application and we have tested a prototype micro-thruster on a thrust balance in vacuum. For these initial tests, a fixed component radio frequency matching network weighing 90 grams was closely attached to the thruster in vacuum with the frequency agile radio frequency generator power being delivered via a 50 Ohm cable. Without accounting for system losses (estimated at around 50~$%$, for a few 10s of Watts from the radio frequency generator the specific impulse was tripled to $sim$48 seconds and the thrust tripled from 0.8 to 2.4 milli-Newtons.

  17. Electro-thermal modelling of polymer lithium batteries for starting period and pulse power

    Energy Technology Data Exchange (ETDEWEB)

    Baudry, P. [Electricite de France DER, Site des Renardieres, Moret-sur-Loing (France); Neri, M. [Electricite de France DER, Site des Renardieres, Moret-sur-Loing (France); Gueguen, M. [Bollore Technologies, Odet, 29 Quimper (France); Lonchampt, G. [CEA/CEREM, CENG-85X, 38 Grenoble (France)

    1995-04-01

    Since power capabilities of solid polymer lithium batteries can only be delivered above 60 C, the thermal management in electric-vehicle applications has to be carefully considered. Electro-thermal modelling of a thermally insulated 200 kg battery was performed, and electrochemical data were obtained from laboratory cell impedance measurements at 20 and 80 C. Starting at 20 C as initial working temperature, the battery reaches 40 C after 150 s of discharge in a 0.5 {Omega} resistance. At 40 C, the useful peak power is 20 kW. The energy expense for heating the battery from 20 to 40 C is 1.4 kWh, corresponding to 6% of the energy available in the battery. After a stand-by period of 24 h, the temperature decreases from 80 to 50 C, allowing efficient starting conditions. (orig.)

  18. Sampling and analysis plan for the former Atomic Energy Commission bus lot property

    International Nuclear Information System (INIS)

    Nielson, R.R.

    1998-07-01

    This sampling and analysis plan (SAP) presents the rationale and strategy for the sampling and analysis activities proposed in support of an initial investigation of the former Atomic Energy Commission (AEC) bus lot property currently owned by Battelle Memorial Institute. The purpose of the proposed sampling and analysis activity is to investigate the potential for contamination above established action levels. The SAP will provide defensible data of sufficient quality and quantity to support recommendations of whether any further action within the study area is warranted. To assist in preparing sampling plans and reports, the Washington State Department of Ecology (Ecology) has published Guidance on Sampling and Data Analysis Methods. To specifically address sampling plans for petroleum-contaminated sites, Ecology has also published Guidance for Remediation of Petroleum Contaminated Sites. Both documents were used as guidance in preparing this plan. In 1992, a soil sample was taken within the current study area as part of a project to remove two underground storage tanks (USTs) at Battelle's Sixth Street Warehouse Petroleum Dispensing Station (Section 1.3). The results showed that the sample contained elevated levels of total petroleum hydrocarbons (TPH) in the heavy distillate range. This current study was initiated in part as a result of that discovery. The following topics are considered: the historical background of the site, current site conditions, previous investigations performed at the site, an evaluation based on the available data, and the contaminants of potential concern (COPC)

  19. Sampling and analysis plan for the former Atomic Energy Commission bus lot property

    Energy Technology Data Exchange (ETDEWEB)

    Nielson, R.R.

    1998-07-01

    This sampling and analysis plan (SAP) presents the rationale and strategy for the sampling and analysis activities proposed in support of an initial investigation of the former Atomic Energy Commission (AEC) bus lot property currently owned by Battelle Memorial Institute. The purpose of the proposed sampling and analysis activity is to investigate the potential for contamination above established action levels. The SAP will provide defensible data of sufficient quality and quantity to support recommendations of whether any further action within the study area is warranted. To assist in preparing sampling plans and reports, the Washington State Department of Ecology (Ecology) has published Guidance on Sampling and Data Analysis Methods. To specifically address sampling plans for petroleum-contaminated sites, Ecology has also published Guidance for Remediation of Petroleum Contaminated Sites. Both documents were used as guidance in preparing this plan. In 1992, a soil sample was taken within the current study area as part of a project to remove two underground storage tanks (USTs) at Battelle`s Sixth Street Warehouse Petroleum Dispensing Station (Section 1.3). The results showed that the sample contained elevated levels of total petroleum hydrocarbons (TPH) in the heavy distillate range. This current study was initiated in part as a result of that discovery. The following topics are considered: the historical background of the site, current site conditions, previous investigations performed at the site, an evaluation based on the available data, and the contaminants of potential concern (COPC).

  20. Evaluation of ultrasound-assisted in situ sorbent formation solid-phase extraction method for determination of arsenic in water, food and biological samples.

    Science.gov (United States)

    Ezoddin, Maryam; Majidi, Behrooz; Abdi, Khosrou

    2015-01-01

    A simple and rapid ultrasound-assisted in situ sorbent formation solid-phase extraction (UAISFSPE) coupled with electrothermal atomic absorption spectrometry detection (ET-AAS) was developed for preconcentration and determination of arsenic (As) in various samples. A small amount of cationic surfactant is dissolved in the aqueous sample containing As ions, which were complexed by ammonium pyrrolidinedithiocarbamate After shaking, a little volume of hexafluorophosphate (NaPF6) as an ion-pairing agent was added into the solution by a microsyringe. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed. The alkyl groups of the surfactant in the solid particles strongly interact with the hydrophobic groups of analytes and become bound. Sonication aids the dispersion of the sorbent into the sample solution and mass transfer of the analyte into the sorbent, thus reducing the extraction time. The solid particles are centrifuged, and the sedimented particles can be dissolved in an appropriate solvent to recover the absorbed analyte. After separation, total arsenic (As(III) and As(V)) was determined by ET-AAS. Several experimental parameters were investigated and optimized. A detection limit of 7 ng L(-1) with preconcentration factor of 100 and relative standard deviation for 10 replicate determinations of 0.1 µg L(-1) As(III) were 4.5% achieved. Consequently, the method was applied to the determination of arsenic in certified reference materials, water, food and biological samples with satisfactory results.

  1. Theoretical Analysis for Heat Transfer Optimization in Subcritical Electrothermal Energy Storage Systems

    Directory of Open Access Journals (Sweden)

    Peng Hu

    2017-02-01

    Full Text Available Electrothermal energy storage (ETES provides bulk electricity storage based on heat pump and heat engine technologies. A subcritical ETES is described in this paper. Based on the extremum principle of entransy dissipation, a geometry model is developed for heat transfer optimization for subcritical ETES. The exergy during the heat transfer process is deduced in terms of entropy production. The geometry model is validated by the extremum principle of entropy production. The theoretical analysis results show that the extremum principle of entransy dissipation is an effective criterion for the optimization, and the optimum heat transfer for different cases with the same mass flux or pressure has been discussed. The optimum heat transfer can be achieved by adjusting the mass flux and pressure of the working fluid. It also reveals that with the increase of mass flux, there is a minimum exergy in the range under consideration, and the exergy decreases with the increase of the pressure.

  2. New Electro-Thermal Battery Pack Model of an Electric Vehicle

    Directory of Open Access Journals (Sweden)

    Muhammed Alhanouti

    2016-07-01

    Full Text Available Since the evolution of the electric and hybrid vehicle, the analysis of batteries’ characteristics and influence on driving range has become essential. This fact advocates the necessity of accurate simulation modeling for batteries. Different models for the Li-ion battery cell are reviewed in this paper and a group of the highly dynamic models is selected for comparison. A new open circuit voltage (OCV model is proposed. The new model can simulate the OCV curves of lithium iron magnesium phosphate (LiFeMgPO4 battery type at different temperatures. It also considers both charging and discharging cases. The most remarkable features from different models, in addition to the proposed OCV model, are integrated in a single hybrid electrical model. A lumped thermal model is implemented to simulate the temperature development in the battery cell. The synthesized electro-thermal battery cell model is extended to model a battery pack of an actual electric vehicle. Experimental tests on the battery, as well as drive tests on the vehicle are performed. The proposed model demonstrates a higher modeling accuracy, for the battery pack voltage, than the constituent models under extreme maneuver drive tests.

  3. The correlation of arsenic levels in drinking water with the biological samples of skin disorders

    Energy Technology Data Exchange (ETDEWEB)

    Kazi, Tasneem Gul [Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)], E-mail: tgkazi@yahoo.com; Arain, Muhammad Balal [Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)], E-mail: bilal_ku2004@yahoo.com; Baig, Jameel Ahmed [Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)], E-mail: jab_mughal@yahoo.com; Jamali, Muhammad Khan [Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)], E-mail: mkhanjamali@yahoo.com; Afridi, Hassan Imran [Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)], E-mail: hassanimranafridi@yahoo.com; Jalbani, Nusrat [Pakistan Council for Scientific and Industrial Research, University Road Karachi-75280 (Pakistan)], E-mail: nusratjalbani_21@yahoo.com; Sarfraz, Raja Adil [Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)], E-mail: rajaadilsarfraz@gmail.com; Shah, Abdul Qadir [Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)], E-mail: aqshah07@yahoo.com; Niaz, Abdul [Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)], E-mail: niazchemist2k6@yahoo.com

    2009-01-15

    Arsenic (As) poisoning has become a worldwide public health concern. The skin is quite sensitive to As and skin lesions are the most common and earliest nonmalignant effects associated to chronic As exposure. In 2005-2007, a survey was carried out on surface and groundwater arsenic contamination and relationships between As exposure via the drinking water and related adverse health effects (melanosis and keratosis) on villagers resides on the banks of Manchar lake, southern part of Sindh, Pakistan. We screened the population from arsenic-affected villages, 61 to 73% population were identified patients suffering from chronic arsenic toxicity. The effects of As toxicity via drinking water were estimated by biological samples (scalp hair and blood) of adults (males and females), have or have not skin problem (n = 187). The referent samples of both genders were also collected from the areas having low level of As (< 10 {mu}g/L) in drinking water (n = 121). Arsenic concentration in drinking water and biological samples were analyzed using electrothermal atomic absorption spectrometry. The range of arsenic concentrations in lake surface water was 35.2-158 {mu}g/L, which is 3-15 folds higher than World Health Organization [WHO, 2004. Guidelines for drinking-water quality third ed., WHO Geneva Switzerland.]. It was observed that As concentration in the scalp hair and blood samples were above the range of permissible values 0.034-0.319 {mu}g As/g for hair and < 0.5-4.2 {mu}g/L for blood. The linear regressions showed good correlations between arsenic concentrations in water versus hair and blood samples of exposed skin diseased subjects (R{sup 2} = 0.852 and 0.718) as compared to non-diseased subjects (R{sup 2} = 0.573 and 0.351), respectively.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  5. Superconducting microtraps for ultracold atoms

    International Nuclear Information System (INIS)

    Hufnagel, C.

    2011-01-01

    Atom chips are integrated devices in which atoms and atomic clouds are stored and manipulated in miniaturized magnetic traps. State of the art fabrication technologies allow for a flexible design of the trapping potentials and consequently provide extraordinary control over atomic samples, which leads to a promising role of atom chips in the engineering and investigation of quantum mechanical systems. Naturally, for quantum mechanical applications, the atomic coherence has to be preserved. Using room temperature circuits, the coherence time of atoms close to the surface was found to be drastically limited by thermal current fluctuations in the conductors. Superconductors offer an elegant way to circumvent thermal noise and therefore present a promising option for the coherent manipulation of atomic quantum states. In this thesis trapping and manipulation of ultracold Rubidium atoms in superconducting microtraps is demonstrated. In this connection the unique properties of superconductors are used to build traps based on persistent currents, the Meissner effect and remanent magnetization. In experiment it is shown, that in superconducting atom chips, thermal magnetic field noise is significantly reduced. Furthermore it is demonstrated, that atomic samples can be employed to probe the properties of superconducting materials. (author) [de

  6. Characterizing fallout material using Cs and Pu atom ratios in environmental samples from the FDNPP fallout zone

    Science.gov (United States)

    Richards, David; Dunne, James; Martin, Peter; Scott, Tom; Yamashiki, Yosuke; Coath, Chris; Chen, Hart

    2017-04-01

    Here we report the use of combined of Cs and Pu isotope measurements to investigate the extensive plumes of radioactive fallout from the disaster at Fukishima Daiichi nuclear power plant (FNDPP) in March 2011. Among the aims of our study are improved assessment of the physico-chemical nature and changing distribution of land-based fallout. 135Cs/137Cs and 134Cs/137Cs atom ratios are indicative of conditions that relate to the nuclear fission reactions responsible for producing the respective radiocaesium isotopes, and offer much more in terms of forensic and chronological analysis than monitoring 137Cs alone. We briefly present methods to quantify the atom ratios of Cs and Pu isotopes in soil, lichen and moss samples from FDNPP catchment using mass spectrometry (ThermoTRITON for Cs and ThermoNEPTUNE for Pu). High precision data from Fukushima are presented (e.g decay corrected 135Cs/137Cs atom ratio = 0.384 ± 0.001 (n = 5) for roadside dust from Iitate region), and these are in agreement with prelimary estimates by others. We also confirm results for IAEA-330, a spinach sample collected from Polesskoe, Ukraine and subject to contamination from the Chernobyl accident. In addition to Cs isotopes, we adopt Pu isotopes to add a further dimension to the forensic analysis. We discuss the corrections required for background levels prior to the disaster, possibility for multiple components of fallout and complicating factors associated with remobilisation during the clean-up operation. In parallel with this work on digests and leaches from bulk environmental samples, we are refining methods for particle identification, isolation and characterisation using a complementary sequence of cutting-edge materials and manipulation techniques, including combined electron microscopy, focused ion beam techniques (Dualbeam), nano/micro manipulators and nano-scale imaging x-ray photoelectron spectroscopy (NanoESCA) and microCT.

  7. [Detecting Thallium in Water Samples using Dispersive Liquid Phase Microextraction-Graphite Furnace Atomic Absorption Spectroscopy].

    Science.gov (United States)

    Zhu, Jing; Li, Yan; Zheng, Bo; Tang, Wei; Chen, Xiao; Zou, Xiao-li

    2015-11-01

    To develope a method of solvent demulsification dispersive liquid phase microextraction (SD-DLPME) based on ion association reaction coupled with graphite furnace atomic absorption spectroscopy (GFAAS) for detecting thallium in water samples. Methods Thallium ion in water samples was oxidized to Tl(III) with bromine water, which reacted with Cl- to form TlCl4-. The ionic associated compound with trioctylamine was obtained and extracted. DLPME was completed with ethanol as dispersive solvent. The separation of aqueous and organic phase was achieved by injecting into demulsification solvent without centrifugation. The extractant was collected and injected into GFAAS for analysis. With palladium colloid as matrix modifier, a two step drying and ashing temperature programming process was applied for high precision and sensitivity. The linear range was 0.05-2.0 microg/L, with a detection limit of 0.011 microg/L. The relative standard derivation (RSD) for detecting Tl in spiked water sample was 9.9%. The spiked recoveries of water samples ranged from 94.0% to 103.0%. The method is simple, sensitive and suitable for batch analysis of Tl in water samples.

  8. Electro-thermal analysis and optimisation of edge termination of power diode supported by 2-D/3-D numerical modelling and simulation

    International Nuclear Information System (INIS)

    Príbytný, P; Donoval, D; Chvála, A; Marek, J; Molnár, M

    2014-01-01

    Numerical modelling and simulation provide an efficient tool for analysis and optimization of device structure design. In this paper we present the analysis and the geometry optimization of the power module with high power pin diode structure supported by the advanced 2-D/3-D mixed-mode electro-thermal device simulation. The structure under investigation is P + NN + power diode device designed for high reverse voltages and very high forward currents, with a maximum forward surge current up to 2.7 kA.

  9. Atomic force microscopy. A new method for atom identification and manipulation

    International Nuclear Information System (INIS)

    Abe, Masayuki; Sugimoto, Yoshiaki; Morita, Seizo

    2007-01-01

    Frequency modulation atomic force microscopy (FM-AFM) is a scanning probe technique that detects the interaction forces between the outermost atom of a sharp tip and the atoms at a surface to image the sample surface. It is expected that the FM-AFM can cover the research field which scanning tunneling microscopy does not provide. In this article, we would introduce FM-AFM experiments applied to site-specific force measurements and atom manipulation, including how to solve the problems to achieve precise FM-AFM measurements. (author)

  10. Creating large out-of-plane displacement electrothermal motion stage by incorporating beams with step features

    International Nuclear Information System (INIS)

    Kim, Yong-Sik; Dagalakis, Nicholas G; Gupta, Satyandra K

    2013-01-01

    Realizing out-of-plane actuation in micro-electro-mechanical systems (MEMS) is still a challenging task. In this paper, the design, fabrication methods and experimental results for a MEMS-based out-of-plane motion stage are presented based on bulk micromachining technologies. This stage is electrothermally actuated for out-of-plane motion by incorporating beams with step features. The fabricated motion stage has demonstrated displacements of 85 µm with 0.4 µm (mA) −1 rates and generated up to 11.8 mN forces with stiffness of 138.8 N m −1 . These properties obtained from the presented stage are comparable to those for in-plane motion stages, therefore making this out-of-plane stage useful when used in combination with in-plane motion stages. (paper)

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  12. Electrothermal debracketing: patient acceptance and effects on the dental pulp.

    Science.gov (United States)

    Dovgan, J S; Walton, R E; Bishara, S E

    1995-09-01

    Adhesives bond ceramic brackets so effectively that their removal by mechanical forces can fracture the brackets and may damage the tooth surface. Electrothermal debracketers have been developed to facilitate removal; whether the heat generated will damage the underlying pulp is unclear. In our experiment, a prototype device with a high heat tip was used to remove brackets from premolars in patients. The following parameters were evaluated: (1) time required for removal, (2) patient acceptance, and (3) histologic effect on the pulp. Forty-eight experimental teeth planned for orthodontic extraction were bonded by a filled Bis-GMA composite resin and a monocrystalline sapphire bracket. After the chemically cured composite set, debracketing was performed according to the manufacturer's recommendations. Seventeen premolars were not etched or bracketed and served as controls. The interval between heat application and removal of the bracket was timed. Patients were questioned as to sensations during debracketing. Teeth were extracted at 5 to 7 or 28 to 32 days and histologically prepared. Pulps were evaluated for alterations. Brackets were removed in an average of 2.1 seconds, usually at the bracket/composite interface. Patient acceptance was generally positive. Pulpal necrosis was not observed but, in a number of specimens, slight inflammation and odontoblastic disruption occurred at both observation periods.

  13. Electro-thermal dynamic stripping process : integrating environmentalism with bitumen production

    Energy Technology Data Exchange (ETDEWEB)

    McGee, B.C.W.; McDonald, C.W. [Society of Petroleum Engineers, Canadian Section, Calgary, AB (Canada)]|[E-T Energy, Calgary, AB (Canada); Little, L. [Society of Petroleum Engineers, Canadian Section, Calgary, AB (Canada)]|[Alberta Energy Research Inst., Edmonton, AB (Canada)

    2008-10-15

    This paper presented a new method of in situ oil sands extraction developed by Calgary-based E-T Energy. The Electro-Thermal Dynamic Stripping Process (ET-DSP) uses electricity to melt oil sands deposits that are too deep for open pit mining. The energy intensity of production compares favourably with alternative thermal bitumen extraction techniques and water consumption for the process is comparatively low, with all produced water being re-injected into the producing formation without any treatment. With ET-DSP, electrodes are drilled and completed next to the oil sands formation which ensures that the electrical currents are forced to flow to the oil sands formation. The viscosity of the bitumen is lowered by the heat from the current, thereby making the fluid flow more readily into vertical extraction wells. ET-DSP uses electricity directly from the power grid, and does not produce any greenhouse gas (GHG) emissions of its own. The process has the potential to allow operators to focus on areas of oil sands reservoirs that have remained inaccessible. Field studies confirmed that the production of bitumen using this method was achieved with reduced greenhouse gas emissions as compared to other thermal recovery process. The bitumen had trace amount of sand and no emulsions. 5 refs., 5 figs.

  14. Study on laser atomic spectroscopy

    International Nuclear Information System (INIS)

    Lee, Jong Min; Song, Kyu Seok; Jeong, Do Young; Kim, Chul Joong; Han, Phil Soon

    1992-01-01

    Electric discharge type atomic vaporizer is developed for the spectroscopic study on actinide elements. Laser induced fluorescence study on actinide elements is performed by using this high temperature type atomizer. For the effective photoionization of elements, copper vapor laser pumped dye laser and electron beam heating type atomic vaporizer are built and their characteristics are measured. In addition, resonance ionization mass spectroscopic analysis for lead sample as well as laser induced fluorescence study on uranium sample in solution phase is made. (Author)

  15. Low-voltage, large-strain soft electrothermal actuators based on laser-reduced graphene oxide/Ag particle composites

    Science.gov (United States)

    Wang, Qian; Li, Yu-Tao; Zhang, Tian-Yu; Wang, Dan-Yang; Tian, Ye; Yan, Jun-Chao; Tian, He; Yang, Yi; Yang, Fan; Ren, Tian-Ling

    2018-03-01

    In this paper, low-voltage, large-strain flexible electrothermal actuators (ETAs) based on laser-reduced graphene oxide (LRGO)/Ag particle composites were fabricated in a simple and cost-efficient process. By adding Ag particles to the LRGO, the sheet resistance decreased effectively. Under a driving voltage of 28 V, the actuator obtained a bending angle of 192° within 6 s. Besides, the bending deformation could be precisely controlled by the driving voltage ranging from 10° to 192°. Finally, a gripper composed of two actuators was demonstrated to manipulate a piece of polydimethylsiloxane block. With the advantages of low-voltage, fast-response, and easy-to-manufacture, the graphene based ETAs have a promising application in soft robotics and soft machines.

  16. Electrothermal piezoresistive cantilever resonators for personal measurements of nanoparticles in workplace exposure

    Science.gov (United States)

    Wasisto, Hutomo Suryo; Wu, Wenze; Uhde, Erik; Waag, Andreas; Peiner, Erwin

    2015-05-01

    Low-cost and low-power piezoresistive cantilever resonators with integrated electrothermal heaters are developed to support the sensing module enhancement of the second generation of handheld cantilever-based airborne nanoparticle (NP) detector (CANTOR-2). These sensors are used for direct-reading of exposure to carbon engineered nanoparticles (ENPs) at indoor workplaces. The cantilever structures having various shapes of free ends are created using silicon bulk micromachining technologies (i.e, rectangular, hammer-head, triangular, and U-shaped cantilevers). For a complete wearable CANTOR-2, all components of the proposed detector can be grouped into two main units depending on their packaging placements (i.e., the NP sampler head and the electronics mounted in a handy-format housing). In the NP sampler head, a miniaturized electrophoretic aerosol sampler and a resonant silicon cantilever mass sensor are employed to collect the ENPs from the air stream to the cantilever surfaces and measuring their mass concentration, respectively. After calibration, the detected ENP mass concentrations of CANTOR-2 show a standard deviation from fast mobility particle sizer (FMPS, TSI 3091) of 8-14%.

  17. A Fast, Large-Stroke Electrothermal MEMS Mirror Based on Cu/W Bimorph

    Directory of Open Access Journals (Sweden)

    Xiaoyang Zhang

    2015-12-01

    Full Text Available This paper reports a large-range electrothermal bimorph microelectromechanical systems (MEMS mirror with fast thermal response. The actuator of the MEMS mirror is made of three segments of Cu/W bimorphs for lateral shift cancelation and two segments of multimorph beams for obtaining large vertical displacement from the angular motion of the bimorphs. The W layer is also used as the embedded heater. The silicon underneath the entire actuator is completely removed using a unique backside deep-reactive-ion-etching DRIE release process, leading to improved thermal response speed and front-side mirror surface protection. This MEMS mirror can perform both piston and tip-tilt motion. The mirror generates large pure vertical displacement up to 320 μm at only 3 V with a power consumption of 56 mW for each actuator. The maximum optical scan angle achieved is ±18° at 3 V. The measured thermal response time is 15.4 ms and the mechanical resonances of piston and tip-tilt modes are 550 Hz and 832 Hz, respectively.

  18. Programmable and functional electrothermal bimorph actuators based on large-area anisotropic carbon nanotube paper

    Science.gov (United States)

    Li, Qingwei; Liu, Changhong; Fan, Shoushan

    2018-04-01

    Electro-active polymer (EAP) actuators, such as electronic, ionic and electrothermal (ET) actuators, have become an important branch of next-generation soft actuators in bionic robotics. However, most reported EAP actuators could realize only simple movements, being restricted by the small area of flexible electrodes and simple designs. We prepared large-area flexible electrodes of high anisotropy, made of oriented carbon nanotube (CNT) paper, and carried out artful graphic designs and processing on the electrodes to make functional ET bimorph actuators which can realize large bending deformations (over 220°, curvature > 1.5 cm-1) and bionic movements driven by electricity. The anisotropy of CNT paper benefits electrode designs and multiform actuations for complex actuators. Based on the large-area CNT paper, more interesting and functional actuators can be designed and prepared which will have practical applications in the fields of artificial muscles, complicated actuations, and soft and bionic robotics.

  19. Spectrochemical determination of lead in wines

    Directory of Open Access Journals (Sweden)

    DRAGAN MARKOVIC

    2000-06-01

    Full Text Available The determination of lead in wines of different origin was performed by means of atomic emission spectroscopy with argon stabilized DC. U-shaped arc and electrothermal atomic absorption spectrometry. The comparison of the results obtained by the direct and standard addition method has indicated the presence of a depressive effect of the complex organic matrix. The effect is avoided successfully by mineralization, as well as by dissolution of the samples. Thus, a relative simple but precise and sensitive method involving the application of a stabilized arc and photoelectric detection with time integration of the emission signals is recommended for the determination of low concentrations of lead in wines. The complex organic matrix was investigated by recording the IR spectra of different wine fractions.

  20. Note: A scanning electron microscope sample holder for bidirectional characterization of atomic force microscope probe tips

    Energy Technology Data Exchange (ETDEWEB)

    Eisenstein, Alon; Goh, M. Cynthia [Department of Chemistry and Institute for Optical Sciences, University of Toronto, 80 St. George Street, Toronto M5S 3H6 (Canada)

    2012-03-15

    A novel sample holder that enables atomic force microscopy (AFM) tips to be mounted inside a scanning electron microscopy (SEM) for the purpose of characterizing the AFM tips is described. The holder provides quick and easy handling of tips by using a spring clip to hold them in place. The holder can accommodate two tips simultaneously in two perpendicular orientations, allowing both top and side view imaging of the tips by the SEM.

  1. Problems in Determination of Skeletal Lead Burden in Archaeological Samples: An Example From the First African Baptist Church Population

    International Nuclear Information System (INIS)

    Whittmers, L.E. Jr.; Aufderheide, A.C.; Pounds, Joel G.; Jones, Keith; Angel, J.L.

    2008-01-01

    Human bone lead content has been demonstrated to be related to socioeconomic status, occupation and other social and environmental correlates. Skeletal tissue samples from 135 individuals from an early nineteenth century Philadelphia cemetery (First African Baptist Church) were studied by electrothermal atomic absorption spectrometry and x-ray fluorescence for lead content. High bone lead levels led to investigation of possible diagenetic effects. These were investigated by several different approaches including distribution of lead within bone by x-ray fluorescence, histological preservation, soil lead concentration and acidity as well as location and depth of burial. Bone lead levels were very high in children, exceeding those of the adult population that were buried in the cemetery, and also those of present day adults. The antemortem age-related increase in bone lead, reported in other studies, was not evidenced in this population. Lead was even deposited in areas of taphonomic bone destruction. Synchrotron x-ray fluorescence studies revealed no consistent pattern of lead microdistribution within the bone. Our conclusions are that postmortem diagenesis of lead ion has penetrated these archaeological bones to a degree that makes their original bone lead content irretrievable by any known method. Increased bone porosity is most likely responsible for the very high levels of lead found in bones of newborns and children

  2. Observation of atomic arrangement by using photoelectron holography and atomic stereo-photograph

    International Nuclear Information System (INIS)

    Matsushita, Tomohiro; Guo, Fang Zhun; Agui, Akane; Matsui, Fumihiko; Daimon, Hiroshi

    2006-01-01

    Both a photoelectron holography and atomic stereo-photograph are the atomic structure analysis methods on the basis of photoelectron diffraction. They have six special features such as 1) direct determination of atomic structure, 2) measurement of three dimensional atomic arrangements surrounding of specific element in the sample, 3) determination of position of atom in spite of electron cloud, 4) unnecessary of perfect periodic structure, 5) good sensitivity of structure in the neighborhood of surface and 6) information of electron structure. Photoelectron diffraction, the principle and measurement system of photoelectron holography and atomic stereo-photograph is explained. As application examples of atomic stereo-photograph, the single crystal of cupper and graphite are indicated. For examples of photoelectron holography, Si(001)2p and Ge(001)3s are explained. (S.Y.)

  3. An analysis of lead (Pb) from human hair samples (20-40 years of age) by atomic absorption spectrophotometry

    International Nuclear Information System (INIS)

    Gelsano, Flordeliza K.; Timing, Laurie D.

    2003-01-01

    This analysis of lead from human hair samples in five different groups namely scavengers from Payatas Quezon City, tricycle drivers, car shop workers, paint factory workers, and students from Polytechnic University of the Philippines. The people from Nagcarlan, Laguna represented as a ''base-line value'' or as a control group. The method applied was acid digestion using HNO 3 and HClO 4 then the samples were subjected to atomic absorption spectrophotometer. In terms of lead found from hair, the scavengers from Payatas Q.C. obtained high exposure of lead among the samples that were tested. The result of the analysis of concentration of lead was expressed in mg/L. (Authors)

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

    International Nuclear Information System (INIS)

    Zhang Yanlin; Adeloju, Samuel B.

    2012-01-01

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

  5. Application of atomic absorption spectrophotometry to determine Cd, Cu, Pb, Zn,...in vegetable samples in Dalat

    Energy Technology Data Exchange (ETDEWEB)

    Giang, Nguyen; Tam, Nguyen Thanh; Ngoc Trinh, Le Thi; Mai, Truong Phuong; Minh, Nguyen Van [Nuclear Research Institute, Dalat (Viet Nam)

    2004-08-01

    Nowadays atomic absorption spectrometry has become valuable method for trace element analysis because high specificity; low detection litmus, easy to use; easy sample preparation, low investment and running costs... atomic absorption spectrometry is generally accepted as one the most suitable method for single - element analysis of trace elements in various kinds of materiel. In 2003, we applied flame - atomic absorption spectrometry for analyzing Ca, Cd, Cu, Pb, Zn...in vegetables and their extracted juices were collected form 11 locations of Dalat, including two kinds of vegetables (goods and safety) in both the summer and winter. Average concentration of Ca = 240 mg/kg wet, Cd = 0.035 mg/kg wet, Cu = 0.67 mg/kg wet, Mg = 131 mg/kg wet, Fe = 8.1/kg wet, Mn = 3.1/kg wet, Na = 3266 mg/kg wet, Pb = 0.345 mg/kg wet and Zn = 3.3 mg wet. In their extracted juices: Ca = 89 mg/kg wet, Cd = 0.008 mg/kg wet, Cu = 0.19 mg/kg wet, Mg = 43 mg/kg wet, Fe = 2.3 mg/kg wet, Mn = 0.61 mg/kg wet, Na = 971 mg/kg wet, Pb = 0.107 mg/kg wet and Zn = 0.65 mg/kg wet. (author)

  6. Application of atomic absorption spectrophotometry to determine Cd, Cu, Pb, Zn,...in vegetable samples in Dalat

    International Nuclear Information System (INIS)

    Nguyen Giang; Nguyen Thanh Tam; Le Thi Ngoc Trinh; Truong Phuong Mai; Nguyen Van Minh

    2004-01-01

    Nowadays atomic absorption spectrometry has become valuable method for trace element analysis because high specificity; low detection litmus, easy to use; easy sample preparation, low investment and running costs... atomic absorption spectrometry is generally accepted as one the most suitable method for single - element analysis of trace elements in various kinds of materiel. In 2003, we applied flame - atomic absorption spectrometry for analyzing Ca, Cd, Cu, Pb, Zn...in vegetables and their extracted juices were collected form 11 locations of Dalat, including two kinds of vegetables (goods and safety) in both the summer and winter. Average concentration of Ca = 240 mg/kg wet, Cd = 0.035 mg/kg wet, Cu = 0.67 mg/kg wet, Mg = 131 mg/kg wet, Fe = 8.1/kg wet, Mn = 3.1/kg wet, Na = 3266 mg/kg wet, Pb = 0.345 mg/kg wet and Zn = 3.3 mg wet. In their extracted juices: Ca = 89 mg/kg wet, Cd = 0.008 mg/kg wet, Cu = 0.19 mg/kg wet, Mg = 43 mg/kg wet, Fe = 2.3 mg/kg wet, Mn = 0.61 mg/kg wet, Na = 971 mg/kg wet, Pb = 0.107 mg/kg wet and Zn = 0.65 mg/kg wet. (author)

  7. An Electro-thermal MEMS Gripper with Large Tip Opening and Holding Force: Design and Characterization

    Directory of Open Access Journals (Sweden)

    Jay J. KHAZAAI

    2011-12-01

    Full Text Available This paper presents the design, fabrication, and characterization of a novel MEMS gripper that is driven electro-thermally by a new V-shape actuator (VSA and a set of modified Guckel U-shape actuators (mUSA. The modification of the angle between the hot and cold arms in the mUSA facilitates unidirectional in-plane displacement causing the opening of the gripper. This configuration distinguishes the MEMS gripper from others in its ability to generate larger tip displacement and greater holding force. The metallic structures allow for a low operating voltage and low overall power consumption. A tip opening of 173.4 μm has been measured at the operating voltage of 1 V with consuming power of 0.85 W. MetalMUMPs is employed to fabricate the device, in which electroplated nickel is used as the structural material.

  8. Assessment of crystalline disorder in cryo-milled samples of indomethacin using atomic pair-wise distribution functions

    DEFF Research Database (Denmark)

    Bøtker, Johan P; Karmwar, Pranav; Strachan, Clare J

    2011-01-01

    to analyse the cryo-milled samples. The high similarity between the ¿-indomethacin cryogenic ball milled samples and the crude ¿-indomethacin indicated that milled samples retained residual order of the ¿-form. The PDF analysis encompassed the capability of achieving a correlation with the physical......The aim of this study was to investigate the usefulness of the atomic pair-wise distribution function (PDF) to detect the extension of disorder/amorphousness induced into a crystalline drug using a cryo-milling technique, and to determine the optimal milling times to achieve amorphisation. The PDF...... properties determined from DSC, ss-NMR and stability experiments. Multivariate data analysis (MVDA) was used to visualize the differences in the PDF and XRPD data. The MVDA approach revealed that PDF is more efficient in assessing the introduced degree of disorder in ¿-indomethacin after cryo-milling than...

  9. Design of a scanning probe microscope with advanced sample treatment capabilities: An atomic force microscope combined with a miniaturized inductively coupled plasma source

    International Nuclear Information System (INIS)

    Hund, Markus; Herold, Hans

    2007-01-01

    We describe the design and performance of an atomic force microscope (AFM) combined with a miniaturized inductively coupled plasma source working at a radio frequency of 27.12 MHz. State-of-the-art scanning probe microscopes (SPMs) have limited in situ sample treatment capabilities. Aggressive treatments such as plasma etching or harsh treatments such as etching in aggressive liquids typically require the removal of the sample from the microscope. Consequently, time consuming procedures are required if the same sample spot has to be imaged after successive processing steps. We have developed a first prototype of a SPM which features a quasi in situ sample treatment using a modified commercial atomic force microscope. A sample holder is positioned in a special reactor chamber; the AFM tip can be retracted by several millimeters so that the chamber can be closed for a treatment procedure. Most importantly, after the treatment, the tip is moved back to the sample with a lateral drift per process step in the 20 nm regime. The performance of the prototype is characterized by consecutive plasma etching of a nanostructured polymer film

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-06-15

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    Science.gov (United States)

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

    2006-06-30

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

  13. Measurement of trace cadmium and elements in bone by epithermal neutron activation analysis

    International Nuclear Information System (INIS)

    Dowlati, R.; Jervis, R.E.

    1991-01-01

    Epithermal neutron activation analysis (ENAA) was applied to measure quantitatively Cd and other elements in bone samples from control and Cd-fed rats. This method was found to be non-destructive to the bone samples, with no sign of 'radiolytic charring' and was sensitive enough to detect and quantify Cd in bone samples at normal levels for mammals (viz. 0.5-1.0 μg/g) and higher. Two different thermal neutron shield materials were utilized, namely cadmium and boron. The boron shield resulted in a 27% improvement in the detection limit of Cd in bone. The accuracy of ENAA for Cd was assessed by intercomparison with electrothermal atomic absorption spectrophotometry (ETAAS), and the results in fair agreement (±23%) with those from ENAA

  14. Spatiotemporal study of gas heating mechanisms in a radio-frequency electrothermal plasma micro-thruster

    Directory of Open Access Journals (Sweden)

    Amelia eGreig

    2015-10-01

    Full Text Available A spatiotemporal study of neutral gas temperature during the first 100 s of operation for a radio-frequency electrothermal plasma micro-thruster operating on nitrogen at 60 W and 1.5 Torr is performed to identify the heating mechanisms involved. Neutral gas temperature is estimated from rovibrational band fitting of the nitrogen second positive system. A set of baffles are used to restrict the optical image and separate the heating mechanisms occurring in the central bulk discharge region and near the thruster walls.For each spatial region there are three distinct gas heating mechanisms being fast heating from ion-neutral collisions with timescales of tens of milliseconds, intermediate heating with timescales of 10 s from ion bombardment on the inner thruster tube surface creating wall heating, and slow heating with timescales of 100 s from gradual warming of the entire thruster housing. The results are discussed in relation to optimising the thermal properties of future thruster designs.

  15. An analysis of lead (Pb) from human hair samples (20-40 years of age) by atomic absorption spectrophotometry

    Energy Technology Data Exchange (ETDEWEB)

    Gelsano, Flordeliza K; Timing, Laurie D

    2003-02-17

    This analysis of lead from human hair samples in five different groups namely scavengers from Payatas Quezon City, tricycle drivers, car shop workers, paint factory workers, and students from Polytechnic University of the Philippines. The people from Nagcarlan, Laguna represented as a ''base-line value'' or as a control group. The method applied was acid digestion using HNO{sub 3} and HClO{sub 4} then the samples were subjected to atomic absorption spectrophotometer. In terms of lead found from hair, the scavengers from Payatas Q.C. obtained high exposure of lead among the samples that were tested. The result of the analysis of concentration of lead was expressed in mg/L. (Authors)

  16. Determination of ultratrace amounts of uranium and thorium in aluminium and aluminium alloys by electrothermal vaporization/ICP-MS

    International Nuclear Information System (INIS)

    Nakamura, Yasushi; Kobayashi, Yoshio; Kakurai, Yousuke

    1993-01-01

    A method has been developed for determining the 0.01 ng g -1 level of uranium and thorium in aluminium and aluminium alloys by electrothermal vaporization (ETV)/ICP-MS. This method was found to be significantly interfered with any matrices or other elements contained. An ion-exchange technique was therefore applied to separate uranium and thorium from aluminium and other elements. It was known that uranium are adsorbed on an anion-exchange resin and thorium are adsorbed on cation-exchange resin. However, aluminium and copper were eluted with 6 M hydrochloric acid. Dissolve the sample with hydrochloric acid containing copper which was added for analysis of pure aluminium, and oxidize with hydrogen peroxide. Concentration of hydrochloric acid in the solution was adjusted to 6 M, and then passed the solution through the mixed ion-exchange resin column. After the uranium and thorium were eluted with 1 M hydrofluoric acid-0.1 M hydrochloric acid, the solution was evaporated to dryness. It was then dissolved with 1 M hydrochloric acid. Uranium and thorium were analyzed by ETV/ICP-MS using tungsten and molybdenum boats, respectively, since the tungsten boat contained high-level thorium and the molybdenum boat contained uranium. The determination limit of uranium and thorium were 0.003 and 0.005 ng g -1 , respectively. (author)

  17. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    International Nuclear Information System (INIS)

    Virgilio, Alex; Nóbrega, Joaquim A.; Rêgo, Jardes F.; Neto, José A. Gomes

    2012-01-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 °C and 2400 °C, respectively. Slopes of calibration curves (50–750 pg Cr, R 2 > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3–17.7 μg g −1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g −1 Cr. The limit of detection was 3.3 ng g −1 Cr. - Highlights: ► Direct solid sampling is first time employed for Cr in plant materials. ► Calibration curves with liquids and solids are coincident. ► Microanalysis of plants for Cr is validated by reference materials. ► The proposed HR-CS GF AAS method is environmental friendly.

  18. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    Energy Technology Data Exchange (ETDEWEB)

    Virgilio, Alex; Nobrega, Joaquim A. [Department of Chemistry, Federal University of Sao Carlos, Post Office Box 676, 13560-970, Sao Carlos-SP (Brazil); Rego, Jardes F. [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil); Neto, Jose A. Gomes, E-mail: anchieta@iq.unesp.br [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil)

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 Degree-Sign C and 2400 Degree-Sign C, respectively. Slopes of calibration curves (50-750 pg Cr, R{sup 2} > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 {mu}g g{sup -1} Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 {+-} 2.1 {mu}g g{sup -1} Cr. The limit of detection was 3.3 ng g{sup -1} Cr. - Highlights: Black-Right-Pointing-Pointer Direct solid sampling is first time employed for Cr in plant materials. Black-Right-Pointing-Pointer Calibration curves with liquids and solids are coincident. Black-Right-Pointing-Pointer Microanalysis of plants for Cr is validated by reference materials. Black-Right-Pointing-Pointer The proposed HR-CS GF AAS method is environmental friendly.

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  20. Detection of silver nanoparticles in parsley by solid sampling high-resolution-continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Feichtmeier, Nadine S; Leopold, Kerstin

    2014-06-01

    In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples.

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

    Czech Academy of Sciences Publication Activity Database

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

    2017-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2017-01-01

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

  3. Advances in atomic spectroscopy

    CERN Document Server

    Sneddon, J

    1997-01-01

    This series describes selected advances in the area of atomic spectroscopy. It is primarily intended for the reader who has a background in atmoic spectroscopy; suitable to the novice and expert. Although a widely used and accepted method for metal and non-metal analysis in a variety of complex samples, Advances in Atomic Spectroscopy covers a wide range of materials. Each Chapter will completely cover an area of atomic spectroscopy where rapid development has occurred.

  4. Development of the striation and filament form of the electrothermal instability

    Science.gov (United States)

    Yu, Edmund; Awe, T. J.; Yelton, W. G.; McKenzie, B. B.; Peterson, K. J.; Bauer, B. S.; Hutchinson, T. M.; Fuelling, S.; Yates, K. C.; Shipley, G.

    2017-10-01

    Magnetically imploded liners have broad application to ICF, dynamic material property studies, and flux compression. An important consideration in liner performance is the electrothermal instability (ETI), an Ohmic heating instability that manifests in 2 ways: assuming vertical current flow, ETI forms hot, horizontal bands (striations) in metals, and vertical filaments in plasmas. Striations are especially relevant in that they can develop into density perturbations, which then couple to the dangerous magneto Rayleigh-Taylor (MRT) instability during liner acceleration. Recent visible emission images of Ohmically heated rods show evidence of both the striation and filament form of ETI, suggesting several questions: (1) can simulation qualitatively reproduce the data? (2) If so, what seeds the striation ETI, and how does it transition to filaments? (3) Does the striation develop into a strong density perturbation, important for MRT? In this work, we use analytic theory and 3D MHD simulation to study how isolated resistive inclusions, embedded in a perfectly smooth rod and communicating through current redistribution, can be used to address the above questions. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology and Engineering Solutions of Sandia LLC, a wholly owned subsidiary of Honeywell International Inc. for the U.S. DOE NNSA under contract DE-NA0003525.

  5. Control of electrothermal heating during regeneration of activated carbon fiber cloth.

    Science.gov (United States)

    Johnsen, David L; Mallouk, Kaitlin E; Rood, Mark J

    2011-01-15

    Electrothermal swing adsorption (ESA) of organic gases generated by industrial processes can reduce atmospheric emissions and allow for reuse of recovered product. Desorption energy efficiency can be improved through control of adsorbent heating, allowing for cost-effective separation and concentration of these gases for reuse. ESA experiments with an air stream containing 2000 ppm(v) isobutane and activated carbon fiber cloth (ACFC) were performed to evaluate regeneration energy consumption. Control logic based on temperature feedback achieved select temperature and power profiles during regeneration cycles while maintaining the ACFC's mean regeneration temperature (200 °C). Energy requirements for regeneration were independent of differences in temperature/power oscillations (1186-1237 kJ/mol of isobutane). ACFC was also heated to a ramped set-point, and the average absolute error between the actual and set-point temperatures was small (0.73%), demonstrating stable control as set-point temperatures vary, which is necessary for practical applications (e.g., higher temperatures for higher boiling point gases). Additional logic that increased the maximum power application at lower ACFC temperatures resulted in a 36% decrease in energy consumption. Implementing such control logic improves energy efficiency for separating and concentrating organic gases for post-desorption liquefaction of the organic gas for reuse.

  6. Multistable Microactuators Functioning on the Basis of Electromagnetic Lorentz Force: Nonlinear Structural and Electrothermal Analyses

    International Nuclear Information System (INIS)

    Han, Jeong Sam

    2010-01-01

    In this paper, the design and nonlinear simulation of a multistable electromagnetic microactuator, which provides four stable equilibrium positions within its operating range, have been discussed. Quadstable actuator motion has been made possible by using both X- and Y-directional bistable structures with snapping curved beams. Two pairs of the curved beams are attached to an inner frame in both X- and Y-directions to realize independent bistable behavior in each direction. For the actuation of the actuator at the micrometer scale, an electromagnetic actuation method in which Lorentz force is taken into consideration was used. By using this method, micrometer-stroke quadstability in a plane parallel to a substrate was possible. The feasibility of designing an actuator that can realize quadstable motion by using the electromagnetic actuation method has been thoroughly clarified by performing nonlinear static and dynamic analyses and electrothermal coupled-field analysis of the multistable microactuator

  7. Buffer choice and effects of sample composition examined by experiment planning methods for determination of molybdenum by atomic absorption with a flame atomizer

    International Nuclear Information System (INIS)

    Zav'yalkov, P.I.; Danishehvskii, A.L.; Rakita, R.A.; Yakshinskii, A.I.

    1986-01-01

    The authors use orthogonal experiment planning to define the optimum form of buffer and to establish the effects of sample composition since there are high levels of cation and anion interference in the atomic-absorption determination of molybdenum. A spectroscopic buffer has been identified (HCLO 4 + NH 4 Cl mixture), which eliminates the interference from the elements tested and improves the analytical characteristics in determining molybdenum. A model has been formulated enabling one to estimate the buffer performance and the effects of the components on the determination of molybdenum. The model enables one to forecast the expected order of the effect without performing additional experiments

  8. An improved $\\pi$K atom lifetime measurement

    CERN Document Server

    Yazkov, V

    2016-01-01

    This note describes details of analysis of data samples collected by DIRAC experiment on a Pt target in 2007 and Ni targets in 2008–2010 in order to estimate the lifetime of πK atoms. Experimental results consist of eight distinct data samples: both charge combinations ( π + K − and K + π − atoms) obtained in different experimental conditions corresponding to each year of data taking. Estimations of systematic errors are presented. Taking into account both statistical and systematic uncertainties, the lifetime of πK atoms is estimated by the maximum likelihood method. The above sample comprises the total statistics, available for the analysis, thus the improvement over the previous estimation [1,3] of the πK atom lifetime is achieved.

  9. Large-area self-assembled reduced graphene oxide/electrochemically exfoliated graphene hybrid films for transparent electrothermal heaters

    Science.gov (United States)

    Sun, Hongyan; Chen, Ding; Ye, Chen; Li, Xinming; Dai, Dan; Yuan, Qilong; Chee, Kuan W. A.; Zhao, Pei; Jiang, Nan; Lin, Cheng-Te

    2018-03-01

    Graphene shows great promise as a high-efficiency electrothermal film for flexible transparent defoggers/defrosters. However, it remains a great challenge to achieve a good balance between the production cost and the properties of graphene films. Here, we proposed a cost-effective self-assembly method to fabricate high-performance, large-area graphene oxide/electrochemically exfoliated graphene hybrid films for heater applications. The self-assembled graphene hybrid films with the area of 20 × 20 cm2 could be transferred onto arbitrary substrates with nonplanar surfaces and simply patterned with the hard mask. After reduction by hydrogen iodide vapor followed by 800 °C thermal treatment, the hybrid films with the transmittance of 76.2% exhibit good heating characteristics and defogging performance, which reach a saturation temperature of up to 127.5 °C when 40 V was applied for 60 s.

  10. Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    Senturk, Hasan Basri; Gundogdu, Ali; Bulut, Volkan Numan; Duran, Celal; Soylak, Mustafa; Elci, Latif; Tufekci, Mehmet

    2007-01-01

    A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 mol L -1 HNO 3 in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 μg L -1 , respectively. The preconcentration factor was 200. The relative standard deviation of the method was -1 . The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Yanlin [NanoScience and Sensor Technology Research Group, School of Applied Sciences and Engineering, Monash University, Churchill, Victoria 3842 (Australia); Adeloju, Samuel B., E-mail: Sam.Adeloju@monash.edu [NanoScience and Sensor Technology Research Group, School of Applied Sciences and Engineering, Monash University, Churchill, Victoria 3842 (Australia)

    2012-04-06

    Highlights: Black-Right-Pointing-Pointer Successful speciation of inorganic and organic Hg with Fe{sup 3+}, Cu{sup 2+} and thiourea as catalysts. Black-Right-Pointing-Pointer Best sensitivity enhancement and similar sensitivity for MeHg and Hg{sup 2+} with Fe{sup 3+}. Black-Right-Pointing-Pointer Successful use of Hg{sup 2+} as the primary standard for quantification of inorganic and total-Hg. Black-Right-Pointing-Pointer Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. Black-Right-Pointing-Pointer Integration with FIA for rapid analysis with a sample throughput of 180 h{sup -1}. - Abstract: A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH{sub 4} were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe{sup 3+}, Cu{sup 2+} and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu{sup 2+} and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe{sup 3+} gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg{sup 2+}. Due to similarity of resulting sensitivity, Hg{sup 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

  12. Laser trapping of radioactive francium atoms

    International Nuclear Information System (INIS)

    Sprouse, G.D.; Orozco, L.A.; Simsarian, J.E.; Shi, W.; Zhao, W.Z.

    1997-01-01

    The difficult problem of quickly slowing and cooling nuclear reaction products so that they can be injected into a laser trap has been solved by several groups and there are now strong efforts to work with the trapped atoms. The atoms are confined in the trap to a small spatial volume of the order of 1 mm 3 , but more importantly, they are also confined in velocity, which makes them an ideal sample for spectroscopic measurements with other lasers. We have recently trapped radioactive francium and have embarked on a program to further study the francium atom as a prelude to a test of the Standard Model analogous to previous work with Cs. Our sample of 3 min 210 Fr now contains over 20 000 atoms, and is readily visible with an ordinary TV camera. We work on-line with the accelerator, and continuously load the trap to replace losses due to decay and collisions with background gas. We have maintained a sample of Fr atoms in the trap for over 10 hours, with occasional adjustment of the trapping laser frequency to account for drifts. The proposed test of the Standard Model will require accurate calculation of its atomic properties. We are currently testing these calculations by measuring other predicted quantities. (orig.)

  13. Cancer in atomic bomb survivors

    International Nuclear Information System (INIS)

    Shigematsu, I.; Kagan, A.

    1986-01-01

    This book presents information on the following topics: sampling of atomic bomb survivors and method of cancer detection in Hiroshima and Nagasaki; atomic bomb dosimetry for epidemiological studies of survivors in Hiroshima and Nagasaki; tumor and tissue registries in Hiroshima and Nagasaki; the cancer registry in Nagasaki, with atomic bomb survivor data, 1973-1977; cancer mortality; methods for study of delayed health effects of a-bomb radiation; experimental radiation carcinogenesis in rodents; leukemia, multiple myeloma, and malignant lymphoma; cancer of the thyroid and salivary glands; malignant tumors in atomic bomb survivors with special reference to the pathology of stomach and lung cancer; colorectal cancer among atomic bomb survivors; breast cancer in atomic bomb survivors; and ovarian neoplasms in atomic bomb survirors

  14. 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.

  15. Ultra-trace determination of gold nanoparticles in environmental water by surfactant assisted dispersive liquid liquid microextraction coupled with electrothermal vaporization-inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Liu, Ying; He, Man; Chen, Beibei; Hu, Bin

    2016-08-01

    A new method by coupling surfactant assisted dispersive liquid liquid microextraction (SA-DLLME) with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) was proposed for the analysis of gold nanoparticles (AuNPs) in environmental water samples. Effective separation of AuNPs from ionic gold species was achieved by using sodium thiosulphate as a complexing agent. Various experimental parameters affecting SA-DLLME of AuNPs, such as the organic solvent, organic solvent volume, pH of the sample, the kind of surfactant, surfactant concentration, vortex time, speed of centrifugation, centrifugation time, and different coating as well as sizes of AuNPs were investigated carefully. Furthermore, the interference of coexisting ions, dissolved organic matter (DOM) and other metal nanoparticles (NPs) were studied. Under the optimal conditions, a detection limit of 2.2 ng L- 1 and an enrichment factor of 152-fold was achieved for AuNPs, and the original morphology of the AuNPs could be maintained during the extraction process. The developed method was successfully applied for the analysis of AuNPs in environmental water samples, including tap water, the East Lake water, and the Yangtze River water, with recoveries in the range of 89.6-102%. Compared with the established methods for metal NPs analysis, the proposed method has the merits of simple and fast operation, low detection limit, high selectivity, good tolerance to the sample matrix and no digestion or dilution required. It provides an efficient quantification methodology for monitoring AuNPs' pollution in the environmental water and evaluating its toxicity.

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

    International Nuclear Information System (INIS)

    Arruda, Marco Aurelio Zezzi; Figueiredo, Eduardo Costa

    2009-01-01

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

  17. Environmental samples analysis by Atomic Absorption Spectrophotometry and Inductively Coupled Plasma-Optical Emission Spectroscopy

    International Nuclear Information System (INIS)

    Popescu, I.V.; Iordan, M.; Stihi, C.; Bancuta, A.; Busuioc, G.; Dima, G.; Ciupina, V.; Belc, M.; Vlaicu, Gh.; Marian, R.

    2002-01-01

    Biological samples are interesting from many aspects of environmental monitoring. By analyzing tree leaves conclusions can be drown regarding the metal loading in the growth medium. So that, starting from assumption that the pollution factors from environmental medium can modify the normal concentration of elements, we decided to control the presence of toxic elements and the deviation from normal state of elements in leaves of different trees from areas situated at different distances of pollution source. The aim of this work is to determine the elemental composition of tree leaves using Atomic Absorption Spectrophotometry (AAS) method and Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) method. Using AAS spectrophotometer SHIMADZU we identified and determined the concentration of: Cd, Co, Cu, Zn, Mn, Cr, Fe, Se, Pb with an instrumental error less than 1% for most of the elements analyzed. The same samples were analyzed by ICP-OES spectrometer, BAIRD ICP2070-Sequential Plasma spectrometer. We identified and determined in leaves of different trees the concentration of Mg, Ca, and Sr with a precision less than 6%. (authors)

  18. A Fourier Transform Spectrometer Based on an Electrothermal MEMS Mirror with Improved Linear Scan Range

    Directory of Open Access Journals (Sweden)

    Wei Wang

    2016-09-01

    Full Text Available A Fourier transform spectrometer (FTS that incorporates a closed-loop controlled, electrothermally actuated microelectromechanical systems (MEMS micromirror is proposed and experimentally verified. The scan range and the tilting angle of the mirror plate are the two critical parameters for MEMS-based FTS. In this work, the MEMS mirror with a footprint of 4.3 mm × 3.1 mm is based on a modified lateral-shift-free (LSF bimorph actuator design with large piston and reduced tilting. Combined with a position-sensitive device (PSD for tilt angle sensing, the feedback controlled MEMS mirror generates a 430 µm stable linear piston scan with the mirror plate tilting angle less than ±0.002°. The usable piston scan range is increased to 78% of the MEMS mirror’s full scan capability, and a spectral resolution of 0.55 nm at 531.9 nm wavelength, has been achieved. It is a significant improvement compared to the prior work.

  19. A multi-axis electrothermal micromirror for a miniaturized OCT system

    KAUST Repository

    Izhar, U.

    2011-06-01

    We report on the development of a low power thermally actuated bi-axis SOI micromirror that is capable of performing angular and vertical scans for optical coherence tomography (OCT) applications. The device consists of a mirror with an aluminum coating over a 3 μm thick single crystal silicon base, aluminum/polysilicon electrothermal actuators with embedded heaters and polysilicon flexural connectors. In scanning mode, this mirror can satisfy our target specification of 5° angle at the low power of 1.7 mW with a temperature increase of 16.5 °C ± 7 °C from ambient in the actuator. Furthermore, a maximum angle of 32° has been achieved at 12 mW. In piston mode, it can reach vertical displacements of up to 131 μm at 12 mW with the temperature increase of 16.5 °C ± 7 °C from ambient in the actuator. The scanning speed for the mirror has been measured and the time response of the mirror is found to be 100 ms. The curvature of the mirror is found to be 2.4 mm ± 0.26 mm with a roughness of 100 nm ± 20 nm. Due to low driving power and moderate temperatures developed during its operation, this device can potentially be integrated with broadband light source, photodetector and interferometery system, to form a fully integrated OCT system on GaAs substrate. © 2011 Elsevier B.V. All rights reserved.

  20. TRACE ANALYSIS BY LASER-EXCITED ATOMIC FLUORESCENCE WITH ATOMIZATION IN A PULSED PLASMA

    OpenAIRE

    Lunyov , O.; Oshemkov , S.; Petrov , A.

    1991-01-01

    The possibilities of plasma atomization for laser fluorescence trace analysis are discussed. Pulsed hot hollow cathode discharge was used for analysis of solutions and powdered samples. The high voltage spark and laser-induced breakdown (laser spark) were used as atomizers of metal-containing atmospheric aerosols. Detection limits were improved by means of temporal background selection.