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

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

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

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.

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

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.

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

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.

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.

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%

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.)

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)

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.

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

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.

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.

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

Direct determination of cadmium in foods by solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry using a tungsten coil trap

Science.gov (United States)

Zhang, Ying; Mao, Xuefei; Liu, Jixin; Wang, Min; Qian, Yongzhong; Gao, Chengling; Qi, Yuehan

2016-04-01

In this work, a solid sampling device consisting of a tungsten coil trap, porous carbon vaporizer and on-line ashing furnace of a Ni-Cr coil was interfaced with inductively coupled plasma mass spectrometry (ICP-MS). A modified double gas circuit system was employed that was composed of carrier and supplemental gas lines controlled by separate gas mass flow controllers. For Cd determination in food samples using the assembled solid sampling ICP-MS, the optimal ashing and vaporization conditions, flow rate of the argon-hydrogen (Ar/H2) (v:v = 24:1) carrier gas and supplemental gas, and minimum sampling mass were investigated. Under the optimized conditions, the limit of quantification was 0.5 pg and the relative standard deviation was within a 10.0% error range (n = 10). Furthermore, the mean spiked recoveries for various food samples were 99.4%-105.9% (n = 6). The Cd concentrations measured by the proposed method were all within the certified values of the reference materials or were not significantly different (P > 0.05) from those of the microwave digestion ICP-MS method, demonstrating the good accuracy and precision of the solid sampling ICP-MS method for Cd determination in food samples.

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

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.

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.

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}.

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.

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.

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.

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.

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.

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. �

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.

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

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.

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...

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

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.

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.

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.

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

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.

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

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.

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.

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.

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.

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...

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.

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.

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

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

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...

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.

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.

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

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

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

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.

Simulation of two-dimensional interior ballistics model of solid propellant electrothermal-chemical launch with discharge rod plasma generator

Directory of Open Access Journals (Sweden)

Yan-jie Ni

2017-08-01

Full Text Available Instead of the capillary plasma generator (CPG, a discharge rod plasma generator (DRPG is used in the 30 mm electrothermal-chemical (ETC gun to improve the ignition uniformity of the solid propellant. An axisymmetric two-dimensional interior ballistics model of the solid propellant ETC gun (2D-IB-SPETCG is presented to describe the process of the ETC launch. Both calculated pressure and projectile muzzle velocity accord well with the experimental results. The feasibility of the 2D-IB-SPETCG model is proved. Depending on the experimental data and initial parameters, detailed distribution of the ballistics parameters can be simulated. With the distribution of pressure and temperature of the gas phase and the propellant, the influence of plasma during the ignition process can be analyzed. Because of the radial flowing plasma, the propellant in the area of the DRPG is ignited within 0.01 ms, while all propellant in the chamber is ignited within 0.09 ms. The radial ignition delay time is much less than the axial delay time. During the ignition process, the radial pressure difference is less than 5  MPa at the place 0.025 m away from the breech. The radial ignition uniformity is proved. The temperature of the gas increases from several thousand K (conventional ignition to several ten thousand K (plasma ignition. Compare the distribution of the density and temperature of the gas, we know that low density and high temperature gas appears near the exits of the DRPG, while high density and low temperature gas appears at the wall near the breech. The simulation of the 2D-IB-SPETCG model is an effective way to investigate the interior ballistics process of the ETC launch. The 2D-IB-SPETC model can be used for prediction and improvement of experiments.

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.

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.)

Sample Results from MCU Solids Outage

Energy Technology Data Exchange (ETDEWEB)

Peters, T.; Washington, A.; Oji, L.; Coleman, C.; Poirier, M.

2014-09-22

Savannah River National Laboratory (SRNL) has received several solid and liquid samples from MCU in an effort to understand and recover from the system outage starting on April 6, 2014. SRNL concludes that the presence of solids in the Salt Solution Feed Tank (SSFT) is the likely root cause for the outage, based upon the following discoveries: A solids sample from the extraction contactor #1 proved to be mostly sodium oxalate; A solids sample from the scrub contactor#1 proved to be mostly sodium oxalate; A solids sample from the Salt Solution Feed Tank (SSFT) proved to be mostly sodium oxalate; An archived sample from Tank 49H taken last year was shown to contain a fine precipitate of sodium oxalate; A solids sample from ; A liquid sample from the SSFT was shown to have elevated levels of oxalate anion compared to the expected concentration in the feed. Visual inspection of the SSFT indicated the presence of precipitated or transferred solids, which were likely also in the Salt Solution Receipt Tank (SSRT). The presence of the solids coupled with agitation performed to maintain feed temperature resulted in oxalate solids migration through the MCU system and caused hydraulic issues that resulted in unplanned phase carryover from the extraction into the scrub, and ultimately the strip contactors. Not only did this carryover result in the Strip Effluent (SE) being pushed out of waste acceptance specification, but it resulted in the deposition of solids into several of the contactors. At the same time, extensive deposits of aluminosilicates were found in the drain tube in the extraction contactor #1. However it is not known at this time how the aluminosilicate solids are related to the oxalate solids. The solids were successfully cleaned out of the MCU system. However, future consideration must be given to the exclusion of oxalate solids into the MCU system. There were 53 recommendations for improving operations recently identified. Some additional considerations or

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

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

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

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

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

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.

Laser solid sampling for a solid-state-detector ICP emission spectrometer

International Nuclear Information System (INIS)

Noelte, J.; Moenke-Blankenburg, L.; Schumann, T.

1994-01-01

Solid sampling with laser vaporization has been coupled to an ICP emission spectrometer with an Echelle optical system and a solid-state-detector for the analysis of steel and soil samples. Pulsation of the vaporized material flow was compensated by real-time background correction and internal standardization, resulting in good accuracy and precision. (orig.)

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...

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)

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.

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

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

WC-Co coatings deposited by the electro-thermal chemical spray method

Energy Technology Data Exchange (ETDEWEB)

Zhitomirsky, V.N. [Tel Aviv Univ. (Israel). Faculty of Engineering; Wald, S.; Rabani, L.; Zoler, D. [Propulsion Physics Division, SOREQ NRC, 81800, Yavne (Israel); Factor, M.; Roman, I. [School of Applied Sciences, The Hebrew University, 91904, Jerusalem (Israel); Cuperman, S.; Bruma, C. [School of Physics and Astronomy, Tel-Aviv University, 69978, Tel-Aviv (Israel)

2000-10-02

A novel thermal spray technology - an electro-thermal chemical spray (ETCS) for producing hard coatings is presented. The experimental coating apparatus consists of a machine gun barrel, a cartridge containing the coating material in powder form, a solid propellant, and a plasma ignition system. The plasma ignition system produces plasma in pulsed mode to ignite the solid propellant. On ignition, the drag force exerted by the combustion gases accelerates the powder particles towards the substrate. Using the ETCS technique, the process of single-shot WC-Co coating deposition on stainless steel substrate was studied. The influence of process parameters (plasma energy, mass of the solid propellant and the coated powder, distance between the gun muzzle and the substrate) on the coating structure and some of its properties were investigated. It was shown that ECTS technique effectively deposited the WC-Co coating with deposition thicknesses of 100-200 {mu}m per shot, while deposition yield of {proportional_to}70% was attained. The WC-Co coatings consisted of carbide particles distributed in amorphous matrix. The powder particle velocity was found to depend on the solid propellant mass and was weakly dependent on the plasma energy, while the particle processing temperature was strongly dependent on the plasma energy and almost independent of the solid propellant mass. Whilst increasing the solid propellant mass from 5 to 7 g, the deposition rate and yield correspondingly increased. When increasing the plasma energy, the temperature of the powder particles increased, the average carbide particle size decreased and their shape became more rounded. The deposition yield and microhardness at first increased and then achieved saturation by increasing the plasma energy. (orig.)

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).

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.

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.

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

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.

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.

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...

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

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

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

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

Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

Directory of Open Access Journals (Sweden)

Helena Prosen

2014-05-01

Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

Science.gov (United States)

Prosen, Helena

2014-05-23

Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

OpenAIRE

Helena Prosen

2014-01-01

Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several...

Assessing total and volatile solids in municipal solid waste samples.

Science.gov (United States)

Peces, M; Astals, S; Mata-Alvarez, J

2014-01-01

Municipal solid waste is broadly generated in everyday activities and its treatment is a global challenge. Total solids (TS) and volatile solids (VS) are typical control parameters measured in biological treatments. In this study, the TS and VS were determined using the standard methods, as well as introducing some variants: (i) the drying temperature for the TS assays was 105°C, 70°C and 50°C and (ii) the VS were determined using different heating ramps from room tempature to 550°C. TS could be determined at either 105°C or 70°C, but oven residence time was tripled at 70°C, increasing from 48 to 144 h. The VS could be determined by smouldering the sample (where the sample is burnt without a flame), which avoids the release of fumes and odours in the laboratory. However, smouldering can generate undesired pyrolysis products as a consequence of carbonization, which leads to VS being underestimated. Carbonization can be avoided using slow heating ramps to prevent the oxygen limitation. Furthermore, crushing the sample cores decreased the time to reach constant weight and decreased the potential to underestimate VS.

Procedures for sampling and sample-reduction within quality assurance systems for solid biofuels

Energy Technology Data Exchange (ETDEWEB)

NONE

2005-04-15

The bias introduced when sampling solid biofuels from stockpiles or containers instead of from moving streams is assessed as well as the number and size of samples required to represent accurately the bulk sample, variations introduced when reducing bulk samples into samples for testing, and the usefulness of sample reduction methods. Details are given of the experimental work carried out in Sweden and Denmark using sawdust, wood chips, wood pellets, forestry residues and straw. The production of a model European Standard for quality assurance of solid biofuels is examined.

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 ...

Paraffin scintillator for radioassay of solid support samples

International Nuclear Information System (INIS)

Fujii, Haruo; Takiue, Makoto

1989-01-01

A new paraffin scintillator used for solid support sample counting has been proposed, and its composition and various characteristics are described. The solid support sample treated with this scintillator can be easily handled because of rigid sample conditions. This technique provides great advantages such as the elimination of a large volume of scintillator and little radioactive waste material by using an economical polyethylene bag instead of the conventional counting vial. (author)

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.

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.)

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...

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)

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%.

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%.

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

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.

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

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

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%.

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

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.

Cr(VI) generation during sample preparation of solid samples – A ...

African Journals Online (AJOL)

Cr(VI) generation during sample preparation of solid samples – A chromite ore case study. R.I Glastonbury, W van der Merwe, J.P Beukes, P.G van Zyl, G Lachmann, C.J.H Steenkamp, N.F Dawson, M.H Stewart ...

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.)

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

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.

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.

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.

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...

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...

Fast sampling calorimetry with solid argon ionization chambers

International Nuclear Information System (INIS)

Clark, E.; Linn, S.; Piekarz, H.; Wahl, H.; Womersley, J.; Hansen, S.; Hurh, P.; Rivetta, C.; Sanders, R.; Schmitt, R.; Stanek, R.; Stefanik, A.

1992-01-01

A proposal for the fast sampling calorimetry with solid argon as active medium and the preliminary results from the solid argon test cell are presented. The proposed test calorimeter module structure, the signal routing and the mechanical and cryogenic arrangements are also discussed

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.

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.

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.

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

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

Spin imaging in solids using synchronously rotating field gradients and samples

International Nuclear Information System (INIS)

Wind, R.A.; Yannoni, C.S.

1983-01-01

A method for spin-imaging in solids using nuclear magnetic resonance (NMR) spectroscopy is described. With this method, the spin density distribution of a two- or three-dimensional object such as a solid can be constructed resulting in an image of the sample. This method lends itself to computer control to map out an image of the object. This spin-imaging method involves the steps of placing a solid sample in the rf coil field and the external magnetic field of an NMR spectrometer. A magnetic field gradient is superimposed across the sample to provide a field gradient which results in a varying DC field that has different values over different parts of the sample. As a result, nuclei in different parts of the sample have different resonant NMR frequencies. The sample is rotated about an axis which makes a particular angle of 54.7 degrees with the static external magnetic field. The magnetic field gradient which has a spatial distribution related to the sample spinning axis is then rotated synchronously with the sample. Data is then collected while performing a solid state NMR line narrowing procedure. The next step is to change the phase relation between the sample rotation and the field gradient rotation. The data is again collected as before while the sample and field gradient are synchronously rotated. The phase relation is changed a number of times and data collected each time. The spin image of the solid sample is then reconstructed from the collected data

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

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.

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.

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.

Automated, Ultra-Sterile Solid Sample Handling and Analysis on a Chip

Science.gov (United States)

Mora, Maria F.; Stockton, Amanda M.; Willis, Peter A.

2013-01-01

There are no existing ultra-sterile lab-on-a-chip systems that can accept solid samples and perform complete chemical analyses without human intervention. The proposed solution is to demonstrate completely automated lab-on-a-chip manipulation of powdered solid samples, followed by on-chip liquid extraction and chemical analysis. This technology utilizes a newly invented glass micro-device for solid manipulation, which mates with existing lab-on-a-chip instrumentation. Devices are fabricated in a Class 10 cleanroom at the JPL MicroDevices Lab, and are plasma-cleaned before and after assembly. Solid samples enter the device through a drilled hole in the top. Existing micro-pumping technology is used to transfer milligrams of powdered sample into an extraction chamber where it is mixed with liquids to extract organic material. Subsequent chemical analysis is performed using portable microchip capillary electrophoresis systems (CE). These instruments have been used for ultra-highly sensitive (parts-per-trillion, pptr) analysis of organic compounds including amines, amino acids, aldehydes, ketones, carboxylic acids, and thiols. Fully autonomous amino acid analyses in liquids were demonstrated; however, to date there have been no reports of completely automated analysis of solid samples on chip. This approach utilizes an existing portable instrument that houses optics, high-voltage power supplies, and solenoids for fully autonomous microfluidic sample processing and CE analysis with laser-induced fluorescence (LIF) detection. Furthermore, the entire system can be sterilized and placed in a cleanroom environment for analyzing samples returned from extraterrestrial targets, if desired. This is an entirely new capability never demonstrated before. The ability to manipulate solid samples, coupled with lab-on-a-chip analysis technology, will enable ultraclean and ultrasensitive end-to-end analysis of samples that is orders of magnitude more sensitive than the ppb goal given

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

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.

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.

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...

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.

Strontium mono-chloride — A new molecule for the determination of chlorine using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

Energy Technology Data Exchange (ETDEWEB)

Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Lopez, Alfredo H.D.; Gois, Jefferson S. de; Caramori, Giovanni F. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Borges, Daniel L.G.; Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

2014-12-01

A new method has been developed for the determination of chlorine in biological reference materials using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) of the strontium mono-chloride (SrCl) molecule and direct solid sample analysis. The use of the SrCl molecule for high-temperature MAS was not described up to now in the literature. Preliminary time-dependent density functional theory calculations of the SrCl structure were carried out in order to obtain reasonable estimates of the absorption spectrum of the target molecule. The calculations, which were carried out at BHandHLyp/def2-QZVP level of theory, proved a very accurate and inexpensive way to get information about the spectrum of the SrCl molecule, which enabled us to perform the Cl determination with good sensitivity and specificity. The molecular absorption of the SrCl molecule has been measured using the wavelength at 635.862 nm, and zirconium and palladium have been evaluated as the chemical modifiers in order to increase the sensitivity of the gaseous SrCl molecule generated in the graphite furnace. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Accuracy and precision of the method have been evaluated using biological certified reference materials of both animal and plant origins, showing good agreement with the informed and certified values. Limit of detection and characteristic mass were 1.0 and 2.2 ng, respectively. The results found using HR-CS GF MAS were in agreement (95% confidence level) compared to those obtained by electrothermal vaporization-inductively coupled plasma mass spectrometry. - Highlights: • The spectrum of the SrCl molecule was calculated on a theoretical basis and found very close to the predicted wavelength. • It is the first time that the spectrum of the SrCl molecule is described and used analytically for the determination of Cl. • No spectral interferences were observed as the

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...

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)

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.

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

Optimization of cloud point extraction and solid phase extraction methods for speciation of arsenic in natural water using multivariate technique.

Science.gov (United States)

Baig, Jameel A; Kazi, Tasneem G; Shah, Abdul Q; Arain, Mohammad B; Afridi, Hassan I; Kandhro, Ghulam A; Khan, Sumaira

2009-09-28

The simple and rapid pre-concentration techniques viz. cloud point extraction (CPE) and solid phase extraction (SPE) were applied for the determination of As(3+) and total inorganic arsenic (iAs) in surface and ground water samples. The As(3+) was formed complex with ammonium pyrrolidinedithiocarbamate (APDC) and extracted by surfactant-rich phases in the non-ionic surfactant Triton X-114, after centrifugation the surfactant-rich phase was diluted with 0.1 mol L(-1) HNO(3) in methanol. While total iAs in water samples was adsorbed on titanium dioxide (TiO(2)); after centrifugation, the solid phase was prepared to be slurry for determination. The extracted As species were determined by electrothermal atomic absorption spectrometry. The multivariate strategy was applied to estimate the optimum values of experimental factors for the recovery of As(3+) and total iAs by CPE and SPE. The standard addition method was used to validate the optimized methods. The obtained result showed sufficient recoveries for As(3+) and iAs (>98.0%). The concentration factor in both cases was found to be 40.

Solid state characterization of commercial crystalline and amorphous atorvastatin calcium samples.

Science.gov (United States)

Shete, Ganesh; Puri, Vibha; Kumar, Lokesh; Bansal, Arvind K

2010-06-01

Atorvastatin calcium (ATC), an anti-lipid BCS class II drug, is marketed in crystalline and amorphous solid forms. The objective of this study was to perform solid state characterization of commercial crystalline and amorphous ATC drug samples available in the Indian market. Six samples each of crystalline and amorphous ATC were characterized using X-ray powder diffractometry (XRPD), differential scanning calorimetry (DSC), thermogravimetric analysis, Karl Fisher titrimetry, microscopy (hot stage microscopy, scanning electron microscopy), contact angle, and intrinsic dissolution rate (IDR). All crystalline ATC samples were found to be stable form I, however one sample possessed polymorphic impurity, evidenced in XRPD and DSC analysis. Amongst the amorphous ATC samples, XRPD demonstrated five samples to be amorphous 'form 27', while, one matched amorphous 'form 23'. Thermal behavior of amorphous ATC samples was compared to amorphous ATC generated by melt quenching in DSC. ATC was found to be an excellent glass former with T(g)/T(m) of 0.95. Residual crystallinity was detected in two of the amorphous samples by complementary use of conventional and modulated DSC techniques. The wettability and IDR of all amorphous samples was found to be higher than the crystalline samples. In conclusion, commercial ATC samples exhibited diverse solid state behavior that can impact the performance and stability of the dosage forms.

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

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

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.

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

Solid-phase microextraction for the analysis of biological samples

NARCIS (Netherlands)

Theodoridis, G; Koster, EHM; de Jong, GJ

2000-01-01

Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

Determination of fluorine in herbs and water samples by molecular absorption spectrometry after preconcentration on nano-TiO2 using ultrasound-assisted dispersive micro solid phase extraction.

Science.gov (United States)

Krawczyk-Coda, Magdalena; Stanisz, Ewa

2017-11-01

This work presents ultrasound-assisted dispersive micro solid phase extraction (USA DMSPE) for preconcentration of fluorine (F) in water and herb samples. TiO 2 nanoparticles (NPs) were used as an adsorbent. The determination with slurry sampling was performed via molecular absorption of calcium monofluoride (CaF) at 606.440 nm using a high-resolution continuum source electrothermal absorption spectrometry (HR-CS ET MAS). Several factors influencing the efficiency of the preconcentration technique, such as the amount of TiO 2 , pH of sample solution, ultrasonication and centrifugation time and TiO 2 slurry solution preparation before injection to HR-CS ET MAS, were investigated in detail. The conditions of detection step (wavelength, calcium amount, pyrolysis and molecule-forming temperatures) were also studied. After extraction, adsorbent with the analyte was mixed with 200 μL of H 2 O to prepare a slurry solution. The concentration limit of detection was 0.13 ng mL -1 . The achieved preconcentration factor was 7. The relative standard deviations (RSDs, %) for F in real samples were 3-15%. The accuracy of this method was evaluated by analyses of certified reference materials after spiking: INCT-MPH-2 (Mixed Polish Herbs), INCT-SBF-4 (Soya Bean Flour), ERM-CAO11b (Hard Drinking Water) and TMDA-54.5 (Lake Ontario Water). The measured F contents in reference materials were in satisfactory agreement with the added amounts, and the recoveries were found to be 97-109%. Under the developed extraction conditions, the proposed method has been successfully applied for the determination of F in real water samples (lake, sea, tap water) and herbs.

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.

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

Solid State Characterization of Commercial Crystalline and Amorphous Atorvastatin Calcium Samples

OpenAIRE

Shete, Ganesh; Puri, Vibha; Kumar, Lokesh; Bansal, Arvind K.

2010-01-01

Atorvastatin calcium (ATC), an anti-lipid BCS class II drug, is marketed in crystalline and amorphous solid forms. The objective of this study was to perform solid state characterization of commercial crystalline and amorphous ATC drug samples available in the Indian market. Six samples each of crystalline and amorphous ATC were characterized using X-ray powder diffractometry (XRPD), differential scanning calorimetry (DSC), thermogravimetric analysis, Karl Fisher titrimetry, microscopy (hot s...

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.

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...

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.

An approach for sampling solid heterogeneous waste at the Hanford Site waste receiving and processing and solid waste projects

International Nuclear Information System (INIS)

Sexton, R.A.

1993-03-01

This paper addresses the problem of obtaining meaningful data from samples of solid heterogeneous waste while maintaining sample rates as low as practical. The Waste Receiving and Processing Facility, Module 1, at the Hanford Site in south-central Washington State will process mostly heterogeneous solid wastes. The presence of hazardous materials is documented for some packages and unknown for others. Waste characterization is needed to segregate the waste, meet waste acceptance and shipping requirements, and meet facility permitting requirements. Sampling and analysis are expensive, and no amount of sampling will produce absolute certainty of waste contents. A sampling strategy is proposed that provides acceptable confidence with achievable sampling rates

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%.

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.

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

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.

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.

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

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%

Solid Phase Characterization of Tank 241-C-105 Grab Samples

International Nuclear Information System (INIS)

Ely, T. M.; LaMothe, M. E.; Lachut, J. S.

2016-01-01

The solid phase characterization (SPC) of three grab samples from single-shell Tank 241-C-105 (C-105) that were received at the laboratory the week of October 26, 2015, has been completed. The three samples were received and broken down in the 11A hot cells.

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)

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.

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.

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...

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

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.

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.

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.

Solid Phase Characterization Of Heel Samples From Tank 241-C-110

International Nuclear Information System (INIS)

Page, J.S.; Cooke, G.A.; Pestovich, J.A.; Huber, H.J.

2011-01-01

During sluicing operations of tank 241-C-110, a significant amount of solids were unable to be retrieved. These solids (often referred to as the tank 'heel') were sampled in 2010 and chemically and mineralogically analyzed in the 222-S Laboratory. Additionally, dissolution tests were performed to identify the amount of undissolvable material after using multiple water contacts. This report covers the solid phase characterization of six samples from these tests using scanning electron microscopy, polarized light microscopy, and X-ray diffraction. The chemical analyses, particle size distribution analysis, and dissolution test results are reported separately. Two of the samples were from composites created from as-received material - Composite A and Composite B. The main phase in these samples was sodium-fluoride-phosphate hydrate (natrophosphate) - in the X-ray diffraction spectra, this phase was the only phase identifiable. Polarized light microscopy showed the presence of minor amounts of gibbsite and other phases. These phases were identified by scanning electron microscopy - energy dispersive X-ray spectroscopy as sodium aluminosilicates, sodium diuranate, and sodium strontium phosphate hydrate (nastrophite) crystals. The natrophosphate crystals in the scanning electron microscopy analysis showed a variety of erosive and dissolution features from perfectly shaped octahedral to well-rounded appearance. Two samples were from water-washed Composites A and B, with no change in mineralogy compared to the as-received samples. This is not surprising, since the water wash had only a short period of water contact with the material as opposed to the water dissolution tests. The last two samples were residual solids from the water dissolution tests. These tests included multiple additions of water at 15 C and 45 C. The samples were sieved to separate a coarser fraction of > 710 μm and a finer fraction of < 710 μm. These two fractions were analyzed separately. The coarser

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.

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)

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)

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

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.

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.

Fast acquisition of multidimensional NMR spectra of solids and mesophases using alternative sampling methods.

Science.gov (United States)

Lesot, Philippe; Kazimierczuk, Krzysztof; Trébosc, Julien; Amoureux, Jean-Paul; Lafon, Olivier

2015-11-01

Unique information about the atom-level structure and dynamics of solids and mesophases can be obtained by the use of multidimensional nuclear magnetic resonance (NMR) experiments. Nevertheless, the acquisition of these experiments often requires long acquisition times. We review here alternative sampling methods, which have been proposed to circumvent this issue in the case of solids and mesophases. Compared to the spectra of solutions, those of solids and mesophases present some specificities because they usually display lower signal-to-noise ratios, non-Lorentzian line shapes, lower spectral resolutions and wider spectral widths. We highlight herein the advantages and limitations of these alternative sampling methods. A first route to accelerate the acquisition time of multidimensional NMR spectra consists in the use of sparse sampling schemes, such as truncated, radial or random sampling ones. These sparsely sampled datasets are generally processed by reconstruction methods differing from the Discrete Fourier Transform (DFT). A host of non-DFT methods have been applied for solids and mesophases, including the G-matrix Fourier transform, the linear least-square procedures, the covariance transform, the maximum entropy and the compressed sensing. A second class of alternative sampling consists in departing from the Jeener paradigm for multidimensional NMR experiments. These non-Jeener methods include Hadamard spectroscopy as well as spatial or orientational encoding of the evolution frequencies. The increasing number of high field NMR magnets and the development of techniques to enhance NMR sensitivity will contribute to widen the use of these alternative sampling methods for the study of solids and mesophases in the coming years. Copyright © 2015 John Wiley & Sons, Ltd.

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)

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.

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

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.

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.

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.

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.

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.

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.

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%

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...

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...

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)

Modified emission-transmission method for determining trace elements in solid samples using the XRF techniques

International Nuclear Information System (INIS)

Poblete, V.; Alvarez, M.; Hermosilla, M.

2000-01-01

This is a study of an analysis of trace elements in medium thick solid samples, by the modified transmission emission method, using the energy dispersion X-ray fluorescence technique (EDXRF). The effects of absorption and reinforcement are the main disadvantages of the EDXRF technique for the quantitative analysis of bigger elements and trace elements in solid samples. The implementation of this method and its application to a variety of samples was carried out using an infinitely thick multi-element white sample that calculates the correction factors by absorbing all the analytes in the sample. The discontinuities in the masic absorption coefficients versus energies association for each element, with medium thick and homogenous samples, are analyzed and corrected. A thorough analysis of the different theoretical and test variables are proven by using real samples, including certified material with known concentration. The simplicity of the calculation method and the results obtained show the method's major precision, with possibilities for the non-destructive routine analysis of different solid samples, using the EDXRF technique (author)

Solid Sampling with a Diode Laser for Portable Ambient Mass Spectrometry.

Science.gov (United States)

Yung, Yeni P; Wickramasinghe, Raveendra; Vaikkinen, Anu; Kauppila, Tiina J; Veryovkin, Igor V; Hanley, Luke

2017-07-18

A hand-held diode laser is implemented for solid sampling in portable ambient mass spectrometry (MS). Specifically, a pseudocontinuous wave battery-powered surgical laser diode is employed for portable laser diode thermal desorption (LDTD) at 940 nm and compared with nanosecond pulsed laser ablation at 2940 nm. Postionization is achieved in both cases using atmospheric pressure photoionization (APPI). The laser ablation atmospheric pressure photoionization (LAAPPI) and LDTD-APPI mass spectra of sage leaves (Salvia officinalis) using a field-deployable quadrupole ion trap MS display many similar ion peaks, as do the mass spectra of membrane grown biofilms of Pseudomonas aeruginosa. These results indicate that LDTD-APPI method should be useful for in-field sampling of plant and microbial communities, for example, by portable ambient MS. The feasibility of many portable MS applications is facilitated by the availability of relatively low cost, portable, battery-powered diode lasers. LDTD could also be coupled with plasma- or electrospray-based ionization for the analysis of a variety of solid samples.

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.

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

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.

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

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.

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.

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.

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...

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.

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

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

Air sampling with solid phase microextraction

Science.gov (United States)

Martos, Perry Anthony

There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

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.

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.

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.

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

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.

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

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.

Sample-size effects in fast-neutron gamma-ray production measurements: solid-cylinder samples

International Nuclear Information System (INIS)

Smith, D.L.

1975-09-01

The effects of geometry, absorption and multiple scattering in (n,Xγ) reaction measurements with solid-cylinder samples are investigated. Both analytical and Monte-Carlo methods are employed in the analysis. Geometric effects are shown to be relatively insignificant except in definition of the scattering angles. However, absorption and multiple-scattering effects are quite important; accurate microscopic differential cross sections can be extracted from experimental data only after a careful determination of corrections for these processes. The results of measurements performed using several natural iron samples (covering a wide range of sizes) confirm validity of the correction procedures described herein. It is concluded that these procedures are reliable whenever sufficiently accurate neutron and photon cross section and angular distribution information is available for the analysis. (13 figures, 5 tables) (auth)

Eosinophilia in routine blood samples as a biomarker for solid tumor development

DEFF Research Database (Denmark)

Andersen, Christen Bertel L; Siersma, V.D.; Hasselbalch, H.C.

2014-01-01

eosinophilia in routine blood samples as a potential biomarker of solid tumor development in a prospective design. MATERIAL AND METHODS: From the Copenhagen Primary Care Differential Count (CopDiff) Database, we identified 356 196 individuals with at least one differential cell count (DIFF) encompassing...... was increased with mild eosinophilia [OR 1.93 (CI 1.29-2.89), p = 0.0013]. No associations with eosinophilia were observed for the remaining solid cancers. CONCLUSION: We demonstrate that eosinophilia in routine blood samples associates with an increased risk of bladder cancer. Our data emphasize...... that additional preclinical studies are needed in order to shed further light on the role of eosinophils in carcinogenesis, where it is still unknown whether the cells contribute to tumor immune surveillance or neoplastic evolution....

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...

Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

International Nuclear Information System (INIS)

Pourreza, N.

2004-01-01

Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

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

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.

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.

Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

Science.gov (United States)

Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

2018-04-01

In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of element concentrations in biological reference materials by solid sampling and other analytical methods

International Nuclear Information System (INIS)

Schauenburg, H.; Weigert, P.

1992-01-01

Using solid sampling with graphite furnace atomic absorption spectrometry (GFAAS), values for cadmium, copper, lead and zinc in six biological reference materials were obtained from up to four laboratories participating in three collaborative studies. These results are compared with those obtained with other methods used in routine analysis from laboratories of official food control. Under certain conditions solid sampling with GFAAS seems to be suitable for routine analysis as well as conventional methods. (orig.)

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.

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.

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....

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

Sampling of solid particles in clouds

International Nuclear Information System (INIS)

Feuillebois, F.; Lasek, A.; Scibilia, M.F.

1986-01-01

This paper is concerned with the sampling of small solid particles from clouds by an airborne apparatus to be mounted on an airplane for meteorological investigations. In the airborne experiment the particles entering the test tube should be as representative as possible of the upstream conditions ahead of the plane, in the real cloud. Due to the inertia of the particles, the proportion of the different sizes of particles entering the test tube depends on the location of the tube mouth. We present a method of calculating the real concentration in particles of different sizes, using the results of measurements executed during the flight of an airplane in a cloud. Two geometries are considered: the nose of the airplane, represented schematically by a hemisphere, and a wing represented by a (2D) Joukowski profile which matches well a NACA 0015 profile on its leading edge

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.

Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

Science.gov (United States)

Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

2018-04-01

This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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.

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.

Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

2015-01-01

The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

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.

Using Peltier cells to study solid-liquid-vapour transitions and supercooling

International Nuclear Information System (INIS)

Torzo, Giacomo; Soletta, Isabella; Branca, Mario

2007-01-01

We propose an apparatus for teaching experimental thermodynamics in undergraduate introductory courses, using thermoelectric modules and a real-time data acquisition system. The device may be made at low cost, still providing an easy approach to the investigation of liquid-solid and liquid-vapour phase transitions and of metastable states (supercooling). The thermoelectric module (a technological evolution of the thermocouple) is by itself an interesting subject that offers a clear example of both thermo-electric (Seebeck effect) and electro-thermal (Peltier effect) energy transformation. We report here some cooling/heating measurements for several liquids and mixtures, including water, salt/water, ethanol/water and sodium acetate, showing how to evaluate the phenomena of freezing point depression and elevation, and how to evaluate the water latent heat

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

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.

Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

Science.gov (United States)

Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

2015-01-01

The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6-4.3%), repeatability (4-9%), reproducibility (9-11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as straightforward

Neutron emission from impacted solid LiD samples

International Nuclear Information System (INIS)

Kaushik, T.C.; Shyam, A.; Kulkarni, L.V.; Srinivasan, M.

1993-01-01

Nylon projectiles with 0.1 g to 0.3 g mass, accelerated to velocities of 0.2-1 km/s using a 60 cm long electromagnetic accelerator (railgun), have been impacted upon solid lithium deuteride (LiD) samples of 3 proportional counters. The output from the BF 3 set-up is monitored in several ways to characterize the possible neutron emission from the target. This includes a simple technique of counting the single channel analyser (SCA) output through a dead-time unit to identify bursts of < 100 μs duration. Counting is started after a delay of ∼ 1 ms to avoid the initial interference from the capacitor bank discharge. The signal is also recorded in a storage oscilloscope from the start of projectile acceleration along with a time marker just before the impact. From a number of shots taken with and without the samples, a significant evidence of neutron emission from the LiD samples appears to emerge. The experiments suggest that approximately 100 neutrons might be generated during every such impact in a duration of < 4 ms. (author). 7 refs., 3 figs

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.

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

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

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)

Gastric emptying of solids: When should we sample

International Nuclear Information System (INIS)

Sfakianakis, G.; Spoliansky, G.; Cassady, J.; Barkin, J.; Serafini, A.

1984-01-01

Gastric emptying of solids has been studied for 20 normal volunteers using Tc-99m-sulfur-colloid labeled chicken liver or eggs. Residual gastric activity measured in 15 min intervals for 2 1/2 hrs was used to calculate gastric emptying. The procedure was proposed and is used to examine patients for suspected abnormal emptying. This approach however ties up one gamma camera and one technologist for a period of 2 1/2 - 3 hrs. Furthermore to classify any value more the 1SD below the mean as abnormal includes 16% of normals as abnormally low (false positives). In order to find the pattern of abnormalities and the best time to study patients we analyzed the results of 54 studies performed in patients with a variety of clinical problems. Gastric emptying was measured in 30 min intervals for 2 1/2 hrs after a standard meal of 2 scrambled eggs labeled with 1 mCi of Tc-99m-sulfur-colloid, 2 slices of bread and 300 ml of juice. To choose the point important to observe the authors studied the distribution of values at each time-point to determine when there is the greatest variability from the reported normal. When there is delayed emptying the 2 1/2 hr observation is the best discriminator and when there is accelerated emptying the 60 min observation is the best discriminator. In the group of patients the 150 min observation had no correlation with the age of the patients. It is possible that sampling at a later time could be more discriminatory. The authors propose sampling at 0, 60, and 150 min time as the most informative and cost effective approach to study the solid gastric emptying. The 2SD rather than 1SD below and above the mean should be used as the level to separate normal from abnormal results

Gastric emptying of solids: When should we sample

Energy Technology Data Exchange (ETDEWEB)

Sfakianakis, G.; Spoliansky, G.; Cassady, J.; Barkin, J.; Serafini, A.

1984-01-01

Gastric emptying of solids has been studied for 20 normal volunteers using Tc-99m-sulfur-colloid labeled chicken liver or eggs. Residual gastric activity measured in 15 min intervals for 2 1/2 hrs was used to calculate gastric emptying. The procedure was proposed and is used to examine patients for suspected abnormal emptying. This approach however ties up one gamma camera and one technologist for a period of 2 1/2 - 3 hrs. Furthermore to classify any value more the 1SD below the mean as abnormal includes 16% of normals as abnormally low (false positives). In order to find the pattern of abnormalities and the best time to study patients we analyzed the results of 54 studies performed in patients with a variety of clinical problems. Gastric emptying was measured in 30 min intervals for 2 1/2 hrs after a standard meal of 2 scrambled eggs labeled with 1 mCi of Tc-99m-sulfur-colloid, 2 slices of bread and 300 ml of juice. To choose the point important to observe the authors studied the distribution of values at each time-point to determine when there is the greatest variability from the reported normal. When there is delayed emptying the 2 1/2 hr observation is the best discriminator and when there is accelerated emptying the 60 min observation is the best discriminator. In the group of patients the 150 min observation had no correlation with the age of the patients. It is possible that sampling at a later time could be more discriminatory. The authors propose sampling at 0, 60, and 150 min time as the most informative and cost effective approach to study the solid gastric emptying. The 2SD rather than 1SD below and above the mean should be used as the level to separate normal from abnormal results.

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%

Measuring Sulfur Isotope Ratios from Solid Samples with the Sample Analysis at Mars Instrument and the Effects of Dead Time Corrections

Science.gov (United States)

Franz, H. B.; Mahaffy, P. R.; Kasprzak, W.; Lyness, E.; Raaen, E.

2011-01-01

The Sample Analysis at Mars (SAM) instrument suite comprises the largest science payload on the Mars Science Laboratory (MSL) "Curiosity" rover. SAM will perform chemical and isotopic analysis of volatile compounds from atmospheric and solid samples to address questions pertaining to habitability and geochemical processes on Mars. Sulfur is a key element of interest in this regard, as sulfur compounds have been detected on the Martian surface by both in situ and remote sensing techniques. Their chemical and isotopic composition can belp constrain environmental conditions and mechanisms at the time of formation. A previous study examined the capability of the SAM quadrupole mass spectrometer (QMS) to determine sulfur isotope ratios of SO2 gas from a statistical perspective. Here we discuss the development of a method for determining sulfur isotope ratios with the QMS by sampling SO2 generated from heating of solid sulfate samples in SAM's pyrolysis oven. This analysis, which was performed with the SAM breadboard system, also required development of a novel treatment of the QMS dead time to accommodate the characteristics of an aging detector.

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

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.

Performance criteria for EM rail launchers with solid or transition armatures and laminated rails

International Nuclear Information System (INIS)

James, T.E.

1991-01-01

Velocity limitations of EM Rail Launchers with solid armatures due to the velocity skin-effect are assessed for a range of homogeneous materials (copper, aluminium, molybdenum and tungsten). Performance criteria as limited by armature melting in the region adjacent to the rail/armature contact surface and by rail surface melting are deduced analytically based on defined electro-thermal reference conditions. The performance criteria predict the reference transition velocity at which the solid contact surface changes to mainly a melted contact surface which is shown to be a fundamental property of the materials. The paper shows that the critical factors in obtaining a high transition velocity are a relatively high resistivity armature material combined with high temperature rail surface coatings. For example a transition velocity of >2.0 km/s for a molybdenum armature and a tungsten rail surface coating on a copper rail are predicted compared with <0.5 km/s for the aluminium/copper combination frequently used

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

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).

A pyrolysis/gas chromatographic method for the determination of hydrogen in solid samples

Science.gov (United States)

Carr, R. H.; Bustin, R.; Gibson, E. K.

1987-01-01

A method is described for the determination of hydrogen in solid samples. The sample is heated under vacuum after which the evolved gases are separated by gas chromatography with a helium ionization detector. The system is calibrated by injecting known amounts of hydrogen, as determined manometrically. The method, which is rapid and reliable, was checked for a variety of lunar soils; the limit of detection is about 10 ng of hydrogen.

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.

Solid phase microextraction headspace sampling of chemical warfare agent contaminated samples : method development for GC-MS analysis

Energy Technology Data Exchange (ETDEWEB)

Jackson Lepage, C.R.; Hancock, J.R. [Defence Research and Development Canada, Medicine Hat, AB (Canada); Wyatt, H.D.M. [Regina Univ., SK (Canada)

2004-07-01

Defence R and D Canada-Suffield (DRDC-Suffield) is responsible for analyzing samples that are suspected to contain chemical warfare agents, either collected by the Canadian Forces or by first-responders in the event of a terrorist attack in Canada. The analytical techniques used to identify the composition of the samples include gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), Fourier-transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy. GC-MS and LC-MS generally require solvent extraction and reconcentration, thereby increasing sample handling. The authors examined analytical techniques which reduce or eliminate sample manipulation. In particular, this paper presented a screening method based on solid phase microextraction (SPME) headspace sampling and GC-MS analysis for chemical warfare agents such as mustard, sarin, soman, and cyclohexyl methylphosphonofluoridate in contaminated soil samples. SPME is a method which uses small adsorbent polymer coated silica fibers that trap vaporous or liquid analytes for GC or LC analysis. Collection efficiency can be increased by adjusting sampling time and temperature. This method was tested on two real-world samples, one from excavated chemical munitions and the second from a caustic decontamination mixture. 7 refs., 2 tabs., 3 figs.

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...

Determination of radiocaesium in agriculture-related water samples containing suspended solids using gelling method

International Nuclear Information System (INIS)

Matsunami, Hisaya; Shin, Moono; Takahashi, Yoshihiko; Shinano, Takuro; Kitajima, Shiori; Tsuchiya, Takashi

2015-01-01

After the TEPCO Fukushima Dai-ichi Nuclear Power Plant accident in 2011, the radiocaesium, which flowed into the paddy fields via irrigation water, have been widely investigated. When the concentration of radiocaesium in the water samples containing suspended solids were directly measured using a high purity germanium detector with a 2 L marinelli beaker, the radiocaesium concentration might be overestimated due to the sedimentation of the suspended solids during the measurement time. In fact, the values obtained by the direct method were higher than those obtained by the filtering method and/or the gelling method in most of the agriculture-related water samples. We concluded that the gelling method using sodium polyacrylate can be widely adapted for the analysis of the total radiocaesium in the agriculture-related water samples because of its many advantage such as simple preparation procedure, accurate analysis values, excellent long-term stability of geometry and low operating cost. (author)

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.

Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 104

International Nuclear Information System (INIS)

Ross, G.A.

1998-01-01

A sample of solids was obtained from tank 104 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprenel tubing (Phthalate free). The sample obtained in a glass jar with Teflon 2 lid, was analyzed for PCBs as Aroclor mixtures. A soxhlet extraction procedure was used to extract the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). The extraction method closely follows SW-846 method 3540C and the analysis follows SW-846 method

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.)

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.

Fundamental limits to the velocity of solid armatures in railguns

International Nuclear Information System (INIS)

Long, G.C. Jr.

1987-01-01

The fundamental limits to the velocity of solid armatures in railguns are dependent upon the increase in temperature which melts the conducting medium or lowers the yield strength of the material. A two-dimensional transient finite-element electrothermal model is developed to determine the magnetic and temperature fields in the rails and armature of a railgun. The solution for the magnetic and temperature fields is based upon the fundamentals of Maxwell's equations and Fourier's law of heat conduction with no a priori assumptions about the current-density distribution in the rails or the armature. The magnetic-field and temperature-field spatial variations are calculated using finite-element techniques, while the time variations are calculated using finite-differencing methods. A thermal-diffusion iteration is performed between each magnetic diffusion iteration. Joule heating information is provided by solving the magnetic diffusion problem and temperature data for calculating material properties such as the electrical resistivity, thermal conductivity, and specific heat is provided by solving the thermal diffusion problem. Various types of rail and armature designs are simulated to include solid armatures consisting of different homogeneous materials, resistive rails, and a graded-resistance armature

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...

Investigation of the suspected presence of solid hydrocarbon in bedded salt samples from the Palo Duro Basin, Texas

International Nuclear Information System (INIS)

1985-10-01

This report contains laboratory test results for two bedded salt samples from the Grabbe No. 1 (PD-2) Well of the Palo Duro Basin, Texas. This study was commissioned to determine whether or not solid hydrocarbons exist in bedded salt samples in the Palo Duro Basin. Laboratory investigations include electron microprobe examinations on polished thin sections and optical examinations and chemical tests on insoluble residues of the salt samples. No direct evidence was found that identifiable solid hydrocarbons are present in either sample of the bedded salt core. The total carbon content of the two salt samples was measured yielding 0.016 and 0.022 weight percent carbon. Detailed microscopic analyses showed that the carbon in the samples was associated with calcite, clays, and the epoxy resin used in sample preparation

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...

Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

DEFF Research Database (Denmark)

Edjabou, Vincent Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona

2015-01-01

Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both...... comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub......-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10-50 waste fractions, organised according to a three-level (tiered approach) facilitating,comparison of the waste data between individual sub-areas with different fractionation (waste...

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...

Localisation and identification of radioactive particles in solid samples by means of a nuclear track technique

International Nuclear Information System (INIS)

Boehnke, Antje; Treutler, Hanns-Christian; Freyer, Klaus; Schubert, Michael; Holger Weiss

2005-01-01

This study is aimed to develop a generally applicable methodology of investigation that can be used for the localisation of single alpha-active particles in solid samples, such as industrial dust or natural soils, sediments and rocks by autoradiography using solid-state nuclear track detectors. The developed technique allows the detection of local enrichments of alpha-emitters in any solid material. The results of such an investigation are of interest from technical, biological and environmental points of view. The idea behind the methodology is to locate the position of alpha-active spots in a sample by attaching the track detector to the sample in a defined manner, thoroughly described in the paper. The located alpha-active particles are subsequently analysed by an electron microscope and an electron microprobe. An example of the application of this methodology is also given. An ultra-fine -grained ore-processing residue, which causes serious environmental pollution in the respective mining district and thus limits possible land use and affects quality of life in the area, was examined using the described technique. The investigation revealed considerable amounts of alpha-active particles in this material

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

Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

Science.gov (United States)

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-10-01

In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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.

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.

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.

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.

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.

Developments of solid materials for UF₆ sampling

Energy Technology Data Exchange (ETDEWEB)

Smith, Nicholas [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Hebden, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Savina, Joseph [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

2017-11-15

This project demonstrated that a device using majority Commercial Off the Shelf (COTS) components could be used to collect uranium hexafluoride samples safely from gaseous or solid sources. The device was based on the successful Cristallini method developed by ABACC over the past 10 years. The system was designed to capture and store the UF₆ as an inert fluoride salt to ease transportation regulations. In addition, the method was considerably faster than traditional cryogenic methods, collected enough material to perform analyses without undue waste, and could be used either inside a facility or in the storage yard.

Permeability and compression characteristics of municipal solid waste samples

Science.gov (United States)

Durmusoglu, Ertan; Sanchez, Itza M.; Corapcioglu, M. Yavuz

2006-08-01

Four series of laboratory tests were conducted to evaluate the permeability and compression characteristics of municipal solid waste (MSW) samples. While the two series of tests were conducted using a conventional small-scale consolidometer, the two others were conducted in a large-scale consolidometer specially constructed for this study. In each consolidometer, the MSW samples were tested at two different moisture contents, i.e., original moisture content and field capacity. A scale effect between the two consolidometers with different sizes was investigated. The tests were carried out on samples reconsolidated to pressures of 123, 246, and 369 kPa. Time settlement data gathered from each load increment were employed to plot strain versus log-time graphs. The data acquired from the compression tests were used to back calculate primary and secondary compression indices. The consolidometers were later adapted for permeability experiments. The values of indices and the coefficient of compressibility for the MSW samples tested were within a relatively narrow range despite the size of the consolidometer and the different moisture contents of the specimens tested. The values of the coefficient of permeability were within a band of two orders of magnitude (10-6-10-4 m/s). The data presented in this paper agreed very well with the data reported by previous researchers. It was concluded that the scale effect in the compression behavior was significant. However, there was usually no linear relationship between the results obtained in the tests.

Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

Science.gov (United States)

Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

2015-05-11

In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

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

Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 101

International Nuclear Information System (INIS)

Diaz, L.A.

1998-01-01

One waste sample that was obtained with solids from tank 101 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprene tubing (Phthalate free) was obtained in a glass jar with teflon lid was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Results are presented

Effects of sample preparation conditions on biomolecular solid-state NMR lineshapes

Energy Technology Data Exchange (ETDEWEB)

Jakeman, David L.; Mitchell, Dan J.; Shuttleworth, Wendy A.; Evans, Jeremy N.S. [Washington State University, Department of Biochemistry and Biophysics (United States)

1998-10-15

Sample preparation conditions with the 46 kDa enzyme complex of 5-enolpyruvyl-shikimate-3-phosphate (EPSP) synthase, shikimate-3-phosphate (S3P) and glyphosate (GLP) have been examined in an attempt to reduce linewidths in solid-state NMR spectra. The linewidths of {sup 13}P resonances associated with enzyme bound S3P and GLP in the lyophilized ternary complex have been reduced to 150 {+-} 12 Hz and 125 {+-} 7 Hz respectively, by a variety of methods involving additives and freezing techniques.

A general assignment method for oriented sample (OS) solid-state NMR of proteins based on the correlation of resonances through heteronuclear dipolar couplings in samples aligned parallel and perpendicular to the magnetic field.

Science.gov (United States)

Lu, George J; Son, Woo Sung; Opella, Stanley J

2011-04-01

A general method for assigning oriented sample (OS) solid-state NMR spectra of proteins is demonstrated. In principle, this method requires only a single sample of a uniformly ¹⁵N-labeled membrane protein in magnetically aligned bilayers, and a previously assigned isotropic chemical shift spectrum obtained either from solution NMR on micelle or isotropic bicelle samples or from magic angle spinning (MAS) solid-state NMR on unoriented proteoliposomes. The sequential isotropic resonance assignments are transferred to the OS solid-state NMR spectra of aligned samples by correlating signals from the same residue observed in protein-containing bilayers aligned with their normals parallel and perpendicular to the magnetic field. The underlying principle is that the resonances from the same residue have heteronuclear dipolar couplings that differ by exactly a factor of two between parallel and perpendicular alignments. The method is demonstrated on the membrane-bound form of Pf1 coat protein in phospholipid bilayers, whose assignments have been previously made using an earlier generation of methods that relied on the preparation of many selectively labeled (by residue type) samples. The new method provides the correct resonance assignments using only a single uniformly ¹⁵N-labeled sample, two solid-state NMR spectra, and a previously assigned isotropic spectrum. Significantly, this approach is equally applicable to residues in alpha helices, beta sheets, loops, and any other elements of tertiary structure. Moreover, the strategy bridges between OS solid-state NMR of aligned samples and solution NMR or MAS solid-state NMR of unoriented samples. In combination with the development of complementary experimental methods, it provides a step towards unifying these apparently different NMR approaches. Copyright © 2011 Elsevier Inc. All rights reserved.

Molecularly imprinted solid-phase extraction of glutathione from urine samples

International Nuclear Information System (INIS)

Song, Renyuan; Hu, Xiaoling; Guan, Ping; Li, Ji; Zhao, Na; Wang, Qiaoli

2014-01-01

Molecularly imprinted polymer (MIP) particles for glutathione were synthesized through iniferter-controlled living radical precipitation polymerization (IRPP) under ultraviolet radiation at ambient temperature. Static adsorption, solid-phase extraction, and high-performance liquid chromatography were carried out to evaluate the adsorption properties and selective recognition characteristics of the polymers for glutathione and its structural analogs. The obtained IRPP-MIP particles exhibited a regularly spherical shape, rapid binding kinetics, high imprinting factor, and high selectivity compared with the MIP particles prepared using traditional free-radical precipitation polymerization. The selective separation and enrichment of glutathione from the mixture of glycyl-glycine and glutathione disulfide could be achieved on the IRPP-MIP cartridge. The recoveries of glutathione, glycyl-glycine, and glutathione disulfide were 95.6% ± 3.65%, 29.5% ± 1.26%, and 49.9% ± 1.71%, respectively. The detection limit (S/N = 3) of glutathione was 0.5 mg·L −1 . The relative standard deviations (RSDs) for 10 replicate detections of 50 mg·L −1 of glutathione were 5.76%, and the linear range of the calibration curve was 0.5 mg·L −1 to 200 mg·L −1 under optimized conditions. The proposed approach was successfully applied to determine glutathione in spiked human urine samples with recoveries of 90.24% to 96.20% and RSDs of 0.48% to 5.67%. - Highlights: • Imprinted polymer particles were prepared by IRPP at ambient temperature. • High imprinting factor, high selectivity, and rapid binding kinetics were achieved. • Selective solid-phase extraction of glutathione from human urine samples

SESAR: Addressing the need for unique sample identification in the Solid Earth Sciences

Science.gov (United States)

Lehnert, K. A.; Goldstein, S. L.; Lenhardt, C.; Vinayagamoorthy, S.

2004-12-01

The study of solid earth samples is key to our knowledge of Earth's dynamical systems and evolution. The data generated provide the basis for models and hypotheses in all disciplines of the Geosciences from tectonics to magmatic processes to mantle dynamics to paleoclimate research. Sample-based data are diverse ranging from major and trace element abundances, radiogenic and stable isotope ratios of rocks, minerals, fluid or melt inclusions, to age determinations and descriptions of lithology, texture, mineral or fossil content, stratigraphic context, physical properties. The usefulness of these data is critically dependent on their integration as a coherent data set for each sample. If different data sets for the same sample cannot be combined because the sample cannot be unambiguously recognized, valuable information is lost. The ambiguous naming of samples has been a major problem in the geosciences. Different samples are often given identical names, and there is a tendency for different people analyzing the same sample to rename it in their publications according to local conventions. This situation has generated significant confusion, with samples often losing their "history", making it difficult or impossible to link available data. This has become most evident through the compilation of geochemical data in relational databases such as PetDB, NAVDAT, and GEOROC. While the relational data structure allows linking of disparate data for samples published in different references, linkages cannot be established due to ambiguous sample names. SESAR is a response to this problem of ambiguous naming of samples. SESAR will create a common clearinghouse that provides a centralized registry of sample identifiers, to avoid ambiguity, to systematize sample designation, and ensure that all information associated with a sample would in fact be unique. The project will build a web-based digital registry for solid earth samples that will provide for the first time a way to

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.

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.

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.

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.

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.

Determination of lead in rice grains by solid sampling HR-CS GFAAS.

Science.gov (United States)

Gunduz, Sema; Akman, Suleyman

2013-12-01

A study was performed for the determination of lead in rice grains directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) without digesting sample. The effects of sample amount, pyrolysis/atomization temperatures on the determination of lead in rice were investigated and optimized using a certificated rice flour. The lead concentrations were determined applying 800 °C of pyrolysis and 1800 °C of atomization temperatures without modifier. LOD (N=10, 3σ) and characteristic mass were 2.3 μg kg(-1) and 8.1 pg, respectively. The certified lead value of a rice flour CRM was found in its uncertainity limits. The lead contents of various rice samples obtained from markets in Turkey were between 0.009 and 0.162 mg kg(-1) which are in acceptable range. The average lead concentrations in various rice grains taken from the same package were significantly different from each other. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

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

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.

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.

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.

Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

International Nuclear Information System (INIS)

Edjabou, Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn; Petersen, Claus; Scheutz, Charlotte; Astrup, Thomas Fruergaard

2015-01-01

Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

Energy Technology Data Exchange (ETDEWEB)

Edjabou, Maklawe Essonanawe, E-mail: vine@env.dtu.dk [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Petersen, Claus [Econet AS, Omøgade 8, 2.sal, 2100 Copenhagen (Denmark); Scheutz, Charlotte; Astrup, Thomas Fruergaard [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark)

2015-02-15

Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

Solid Phase Microextraction (SPME in Determination of Pesticide Residues in Soil Samples

Directory of Open Access Journals (Sweden)

Rada Đurović

2011-01-01

Full Text Available The basic principles and application possibilities of the methods based on solid phase microextraction (SPME in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy inpesticide determination (type and thickness of microextraction fiber, duration of microextraction,temperature at which it is conducted, effect of addition of salts (the effect of efflorescence,temperature and time of desorption, the choice of optimal solvent for pesticide exctraction from the soil and the optimal number of extraction steps, as well as general guidelines for their optimization are also shown. In the end, current applications of SPMEmethods in the analysis of pesticide residues in soil samples are presented.

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

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

Sampling of tar from sewage sludge gasification using solid phase adsorption.

Science.gov (United States)

Ortiz González, Isabel; Pérez Pastor, Rosa Ma; Sánchez Hervás, José Ma

2012-06-01

Sewage sludge is a residue from wastewater treatment plants which is considered to be harmful to the environment and all living organisms. Gasification technology is a potential source of renewable energy that converts the sewage sludge into gases that can be used to generate energy or as raw material in chemical synthesis processes. But tar produced during gasification is one of the problems for the implementation of the gasification technology. Tar can condense on pipes and filters and may cause blockage and corrosion in the engines and turbines. Consequently, to minimize tar content in syngas, the ability to quantify tar levels in process streams is essential. The aim of this work was to develop an accurate tar sampling and analysis methodology using solid phase adsorption (SPA) in order to apply it to tar sampling from sewage sludge gasification gases. Four types of commercial SPA cartridges have been tested to determine the most suitable one for the sampling of individual tar compounds in such streams. Afterwards, the capacity, breakthrough volume and sample stability of the Supelclean™ ENVI-Carb/NH(2), which is identified as the most suitable, have been determined. Basically, no significant influences from water, H(2)S or NH(3) were detected. The cartridge was used in sampling real samples, and comparable results were obtained with the present and traditional methods.

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

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

Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization

Science.gov (United States)

Loge, G.

1994-09-01

Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U3O8. Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF4 were found to be a kinetic bottleneck to the formation of UF6. This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid.

Solid sampling-graphite furnace atomic absorption spectrometry for the direct determination of boron in plant tissues

International Nuclear Information System (INIS)

Resano, M.; Briceno, J.; Aramendia, M.; Belarra, M.A.

2007-01-01

In this work, the potential of graphite furnace atomic absorption spectrometry for the direct determination of B in plant tissues has been investigated. Three certified reference materials (NIST SRM 1570a spinach leaves, NIST SRM 1573a tomato leaves and BCR CRM 679 white cabbage) were selected for this study, the goal always being to develop a fast procedure that could be robust enough to provide a satisfactory performance for all of them, without any modifications in the conditions applied. The use of a suitable chemical modifier was found to be essential for obtaining a reproducible and sufficiently sensitive signal for boron solutions. In this regard, the performance of the combination of citric acid plus W (added as a permanent modifier) was noteworthy, resulting in well-defined signal profiles, a remarkable analyte stabilization during the pyrolysis step (up to 2100 deg. C) and minimal memory effects. This mixture of modifiers provided a good performance for the direct analysis of solid samples as well, but only if a suitable temperature program, favoring the interaction between the analyte and the modifiers, was used. Thus, such a temperature program, with two pyrolysis steps and the addition of NH 4 NO 3 in order to carry out the in situ sample microdigestion, was optimized. Under these conditions, the peak areas obtained for both solid samples and aqueous standards were comparable. Finally, the analysis of the samples was carried out. In all cases, a good agreement with the certified values was obtained, while R.S.D. values ranged between 6 and 10%. It can be concluded that the method proposed shows significant advantages for the determination of this complicated element in solid samples such as the use of aqueous standards for calibration, a high sample throughput (20 min per sample), a suitable limit of detection (0.3 μg g -1 ) and reduced risk of analyte losses and contamination

Simultaneous Effects of Total Solids Content, Milk Base, Heat Treatment Temperature and Sample Temperature on the Rheological Properties of Plain Stirred Yogurt

Directory of Open Access Journals (Sweden)

Attilio Converti

2006-01-01

Full Text Available Response surface methodology was used to establish a relationship between total solids content, milk base, heat treatment temperature, and sample temperature, and consistency index, flow behaviour index, and apparent viscosity of plain stirred yogurts. Statistical treatments resulted in developments of mathematical models. All samples presented shear thinning fluid behaviour. The increase of the content of total solids (9.3–22.7 % and milk base heat treatment temperature (81.6–98.4 °C resulted in a significant increase in consistency index and a decrease in flow behaviour index. Increase in the sample temperature (1.6–18.4 °C caused a decrease in consistency index and increase in flow behaviour index. Apparent viscosity was directly related to the content of total solids. Rheological properties of yogurt were highly dependent on the content of total solids in milk.

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...

High performance preconcentration of inorganic Se species by dispersive micro-solid phase extraction with a nanosilica-ionic liquid hybrid material

Science.gov (United States)

Llaver, Mauricio; Coronado, Eduardo A.; Wuilloud, Rodolfo G.

2017-12-01

A highly sensitive and efficient dispersive micro-solid phase extraction (D-μ-SPE) method was developed for inorganic Se speciation analysis. A novel ionic liquid (IL)-nanomaterial hybrid consisting of 1-dodecyl-3-methylimidazolium bromide-functionalized nanosilica was used for the efficient retention of Se(IV) complexed with ammonium pyrrolidine dithiocarbamate, followed by elution with an ethyl acetate/Triton X-114 mixture and determination by electrothermal atomic absorption spectroscopy. The Se(VI) species was selectively determined by difference between total inorganic Se and Se(IV) after pre-reduction. The IL-nanomaterial hybrid was characterized by Fourier transform infrared spectroscopy and transmission electronic microscopy. Likewise, Se(IV) sorption capacity of the retention material and maximum amount of IL loaded on its surface were determined. Several factors concerning the functionalization, extraction and elution steps were optimized, yielding a 100% extraction efficiency for Se(IV) under optimal conditions. A limit of detection of 1.1 ng L- 1, a relative standard deviation of 5.7% and a 110-fold enhancement factor were obtained. The D-μ-SPE method was successfully applied to several water samples from different origins and compositions, including rain, tap, underground, river and sea.

Modeling, measuring, and mitigating instability growth in liner implosions on Z

Science.gov (United States)

Peterson, Kyle

2015-11-01

Electro-thermal instabilities result from non-uniform heating due to temperature dependence in the conductivity of a material. In this talk, we will discuss the role of electro-thermal instabilities on the dynamics of magnetically accelerated implosion systems. We present simulations that show electro-thermal instabilities form immediately after the surface material of a conductor melts and can act as a significant seed to subsequent magneto-Rayleigh-Taylor (MRT) instability growth. We discuss measurement results from experiments performed on Sandia National Laboratories Z accelerator to investigate signatures of electro-thermal instability growth on well-characterized initially solid aluminum or beryllium rods driven with a 20 MA, 100 ns risetime current pulse. These measurements show good agreement with electro-thermal instability simulations and exhibit larger instability growth than can be explained by MRT theory alone. Recent experiments have confirmed simulation predictions of dramatically reduced instability growth in solid metallic rods when thick dielectric coatings are used to mitigate density perturbations arising from the electro-thermal instability. These results provide further evidence that the inherent surface roughness of the target is not the dominant seed for the MRT instability, in contrast with most inertial confinement fusion approaches. These results suggest a new technique for substantially reducing the integral MRT growth in magnetically driven implosions. Indeed, recent results on the Z facility with 100 km/s Al and Be liner implosions show substantially reduced growth. These new results include axially magnetized, CH-coated beryllium liner radiographs in which the inner liner surface is observed to be remarkably straight and uniform at a radius of about 120 microns (convergence ratio ~20). Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy under

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)

Receiver calibration and the nonlinearity parameter measurement of thick solid samples with diffraction and attenuation corrections.

Science.gov (United States)

Jeong, Hyunjo; Barnard, Daniel; Cho, Sungjong; Zhang, Shuzeng; Li, Xiongbing

2017-11-01

This paper presents analytical and experimental techniques for accurate determination of the nonlinearity parameter (β) in thick solid samples. When piezoelectric transducers are used for β measurements, the receiver calibration is required to determine the transfer function from which the absolute displacement can be calculated. The measured fundamental and second harmonic displacement amplitudes should be modified to account for beam diffraction and material absorption. All these issues are addressed in this study and the proposed technique is validated through the β measurements of thick solid samples. A simplified self-reciprocity calibration procedure for a broadband receiver is described. The diffraction and attenuation corrections for the fundamental and second harmonics are explicitly derived. Aluminum alloy samples in five different thicknesses (4, 6, 8, 10, 12cm) are prepared and β measurements are made using the finite amplitude, through-transmission method. The effects of diffraction and attenuation corrections on β measurements are systematically investigated. When diffraction and attenuation corrections are all properly made, the variation of β between different thickness samples is found to be less than 3.2%. Copyright © 2017 Elsevier B.V. All rights reserved.

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)

Augmentation and Control of Burn Rates in Plasma Devices

National Research Council Canada - National Science Library

Bourham, Mohamed

1999-01-01

Interaction of electrothermal plasmas with solid propellants necessitates thorough understanding of plasma-propellant interface physics, momentum and energy transfer, plasma flow regimes, and mixing processes...

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.

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.

Headspace Solid Phase Microextraction in Pesticide Residues Analysis: 2. Apple Samples

Directory of Open Access Journals (Sweden)

Jelena Milinović

2007-01-01

Full Text Available Headspace solid phase microextraction method (HS/SPME, optimised previously for pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion and bifenthrin in apple samples. One-hour extraction procedure was performed at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS fiber was used. Detection and quantification were carried out by gas chromatography/mass spectrometry (GC/MS. A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-1.25 mg/kg concentration range in order to determine analytical parameters of the method applied. Linearity with regression coefficient (R values higher than 0.99 were obtained over the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection (LOD values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD values obtained for multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%.

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.

Determination of Pu isotopic composition and 241Am by high resolution gamma spectrometry on solid samples

International Nuclear Information System (INIS)

Sarkar, Arnab; Paul, Sumana; Aggarwal, Suresh K.; Tomar, Bhupendra S.

2011-08-01

The present report gives a detailed account of the development of non-destructive assay technique using high resolution gamma-ray spectrometry (HRGS) for determination of plutonium (Pu) isotopic composition and the 241 Am content in solid Pu samples. Energy range 120-420 keV was used in this study. The methodology involves in situ relative efficiency calibration during the measurement process itself, to reduce the errors and increase the reliability of the method. Twenty solid Pu samples of power reactor and research reactor grade were analyzed by this method and the results were compared with those obtained by thermal ionization mass spectrometry. The accuracy of the final results depends strongly upon the accuracy of the available nuclear data (decay constant, gamma abundance etc.). MATLAB based programme was written to perform the analysis. A counting time of 4 hour was chosen for achieving good statistics on the results for samples having 100-200 mg of Pu. The attainable accuracy is found to be 0.5-1% for the fissile isotopes ( 239 Pu + 241 Pu) and 5-10% for 241 Am content. (author)

Inorganic mass spectrometry of solid samples

International Nuclear Information System (INIS)

Adams, F.; Vertes, A.

1990-01-01

In this review some recent developments in the field of inorganic mass spectrometry of solids are described with special emphasis on the actual state of understanding of the ionization processes. It concentrates on the common characteristics of methods such as spark source-, laser-, secondary ion-, inductively coupled plasma- and glow discharge mass spectrometry. (orig.)

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.)

Discrete element method (DEM) simulations of stratified sampling during solid dosage form manufacturing.

Science.gov (United States)

Hancock, Bruno C; Ketterhagen, William R

2011-10-14

Discrete element model (DEM) simulations of the discharge of powders from hoppers under gravity were analyzed to provide estimates of dosage form content uniformity during the manufacture of solid dosage forms (tablets and capsules). For a system that exhibits moderate segregation the effects of sample size, number, and location within the batch were determined. The various sampling approaches were compared to current best-practices for sampling described in the Product Quality Research Institute (PQRI) Blend Uniformity Working Group (BUWG) guidelines. Sampling uniformly across the discharge process gave the most accurate results with respect to identifying segregation trends. Sigmoidal sampling (as recommended in the PQRI BUWG guidelines) tended to overestimate potential segregation issues, whereas truncated sampling (common in industrial practice) tended to underestimate them. The size of the sample had a major effect on the absolute potency RSD. The number of sampling locations (10 vs. 20) had very little effect on the trends in the data, and the number of samples analyzed at each location (1 vs. 3 vs. 7) had only a small effect for the sampling conditions examined. The results of this work provide greater understanding of the effect of different sampling approaches on the measured content uniformity of real dosage forms, and can help to guide the choice of appropriate sampling protocols. Copyright © 2011 Elsevier B.V. All rights reserved.

A new method for determining the uranium and thorium distribution in volcanic rock samples using solid state nuclear track detectors

International Nuclear Information System (INIS)

Misdaq, M.A.; Bakhchi, A.; Ktata, A.; Koutit, A.; Lamine, J.; Ait nouh, F.; Oufni, L.

2000-01-01

A method based on using solid state nuclear track detectors (SSNTD) CR- 39 and LR-115 type II and calculating the probabilities for the alpha particles emitted by the uranium and thorium series to reach and be registered on these films was utilized for uranium and thorium contents determination in various geological samples. The distribution of uranium and thorium in different volcanic rocks has been investigated using the track fission method. In this work, the uranium and thorium contents have been determined in different volcanic rock samples by using CR-39 and LR-115 type II solid state nuclear track detectors (SSNTD). The mean critical angles of etching of the solid state nuclear track detectors utilized have been calculated. A petrographical study of the volcanic rock thin layers studied has been conducted. The uranium and thorium distribution inside different rock thin layers has been studied. The mechanism of inclusion of the uranium and thorium nuclei inside the volcanic rock samples studied has been investigated. (author)

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.

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.

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.

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

Determination of colloidal and dissolved silver in water samples using colorimetric solid-phase extraction.

Science.gov (United States)

Hill, April A; Lipert, Robert J; Porter, Marc D

2010-03-15

The increase in bacterial resistance to antibiotics has led to resurgence in the use of silver as a biocidal agent in applications ranging from washing machine additives to the drinking water treatment system on the International Space Station (ISS). However, growing concerns about the possible toxicity of colloidal silver to bacteria, aquatic organisms and humans have led to recently issued regulations by the US EPA and FDA regarding the usage of silver. As part of an ongoing project, we have developed a rapid, simple method for determining total silver, both ionic (silver(I)) and colloidal, in 0.1-1mg/L aqueous samples, which spans the ISS potable water target of 0.3-0.5mg/L (total silver) and meets the US EPA limit of 0.1mg/L in drinking water. The method is based on colorimetric solid-phase extraction (C-SPE) and involves the extraction of silver(I) from water samples by passage through a solid-phase membrane impregnated with the colorimetric reagent DMABR (5-[4-(dimethylamino)benzylidene]rhodanine). Silver(I) exhaustively reacts with impregnated DMABR to form a colored compound, which is quantified using a handheld diffuse reflectance spectrophotometer. Total silver is determined by first passing the sample through a cartridge containing Oxone, which exhaustively oxidizes colloidal silver to dissolved silver(I). The method, which takes less than 2 min to complete and requires only approximately 1 mL of sample, has been validated through a series of tests, including a comparison with the ICP-MS analysis of a water sample from ISS that contained both silver(I) and colloidal silver. Potential earth-bound applications are also briefly discussed. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Evaluation of the readsorption of plutonium and americium in dynamic fractionations of environmental solid samples

DEFF Research Database (Denmark)

Petersen, Roongrat; Hou, Xiaolin; Hansen, Elo Harald

2008-01-01

A dynamic extraction system exploiting sequential injection (SI) for sequential extractions incorporating a specially designed extraction column is developed to fractionate radionuclides in environmental solid samples such as soils and sediments. The extraction column can contain a large amount...... of soil sample (up to 5 g), and under optimal operational conditions it does not give rise to creation of back pressure. Attention has been placed on studies of the readsorption problems during sequential extraction using a modified Standards, Measurements and Testing (SM&T) scheme with 4-step sequential...

Assessment of the content of arsenic in solid by-products from coal combustion

Directory of Open Access Journals (Sweden)

Wierońska Faustyna

2017-01-01

Full Text Available The coal combustion processes constitute one of the major sources of heavy metals emission into the atmosphere. From the point of view of the reduction of the emission of heavy metals and the selection of the correct exhaust gas treatment system, it is important to monitor the amount of trace elements in the solid fuels and in the solid by-products from coal combustion. One of these highly toxic elements is arsenic. The average content of arsenic in Polish hard coals and lignites is 0 ÷ 40 mg/kg [1] and 5 ÷ 15 mg/kg [2], respectively. The world average content of arsenic in hard coals and lignites, is equal to 9.0 ± 0.8 and 7.4 ± 1.4 mg/kg [3], respectively. During coal combustion processes, a significant amount of arsenic enters the atmosphere through gases and fly ashes. The proportions in which those two forms of arsenic occur in exhaust gases depend on the conditions of combustion processes [4]. The aim of the research was to determine the content of arsenic in coal blends and by-products of their combustion (slag, fly ash, gypsum, filter cakes. The determination of the arsenic quantity was performed using the Atomic Absorption Spectrometry with the electrothermal atomization.

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.

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.

Automated sample preparation station for studying self-diffusion in porous solids with NMR spectroscopy

Science.gov (United States)

Hedin, Niklas; DeMartin, Gregory J.; Reyes, Sebastián C.

2006-03-01

In studies of gas diffusion in porous solids with nuclear magnetic resonance (NMR) spectroscopy the sample preparation procedure becomes very important. An apparatus is presented here that pretreats the sample ex situ and accurately sets the desired pressure and temperature within the NMR tube prior to its introduction in the spectrometer. The gas manifold that supplies the NMR tube is also connected to a microbalance containing another portion of the same sample, which is kept at the same temperature as the sample in the NMR tube. This arrangement permits the simultaneous measurement of the adsorption loading on the sample, which is required for the interpretation of the NMR diffusion experiments. Furthermore, to ensure a good seal of the NMR tube, a hybrid valve design composed of titanium, a Teflon® seat, and Kalrez® O-rings is utilized. A computer controlled algorithm ensures the accuracy and reproducibility of all the procedures, enabling the NMR diffusion experiments to be performed at well controlled conditions of pressure, temperature, and amount of gas adsorbed on the porous sample.

Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization. Final report

International Nuclear Information System (INIS)

Loge, G.

1994-01-01

Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U 3 O 8 . Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF 4 were found to be a kinetic bottleneck to the formation of UF 6 . This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid

Detection of fission fragments using thick samples in contact with solid state nuclear track detectors

International Nuclear Information System (INIS)

Lima, D.A. de; Martins, J.B.; Tavares, O.A.P.

1987-01-01

Whenever use is made of thick samples in contact with solid state nuclear track detectors for determining fission yields, one of the fundamental problems is the evaluation of the effective number of target nuclei which contributes to the fraction of the number of fission events that will be recorded. The evaluation of the effective number of target nuclei which contributes to recorded events is based on the effective thickness of the sample. A method for evaluating effective thickness of thick samples for binary fission modes, is presented. A cross section equation which takes into account all the necessary corrections due to fragment attenuation effects by a thick target for calculation induced fission yields, was obtained. (Author) [pt

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.

Reimiep 87. An interlaboratory U-235 enrichment determination by gamma measurement on solid UF6 sample

International Nuclear Information System (INIS)

Aparo, M.; Cresti, P.

1988-01-01

Gamma spectroscopy technique, based on the measurement of U 235 186 KeV flux, is now currently used for the determination of Uranium enrichment in different material of nuclear fuel cycle, namely: Uranium metallic, UO 2 pellets, UF 6 liquid or solid. The present paper describes the use of such a technique and the obtained results in determining the U 235 /U atomic isotopic abundance on a certified UF 6 solid sample. The measurements have been carried out in the frame work of the partecipation to the ''UF 6 Interlaboratory Measurements Evaluation Programme'' organized by CBNM/Geel with the support of the ESARDA (European Safeguards Research and Development Association)

The indicating FTA elute cartridge a solid sample carrier to detect high-risk HPV and high-grade cervical lesions

NARCIS (Netherlands)

Bie, R.P. de; Schmeink, C.E.; Bakkers, J.M.J.E.; Snijders, P.J.L.M.; Quint, W.G.V.; Massuger, L.F.A.G.; Bekkers, R.L.M.; Melchers, W.J.G.

2011-01-01

The clinically validated high-risk human papillomavirus (hrHPV) Hybrid Capture 2 (HC2) and GP5+/6+-PCR assays were analyzed on an Indicating FTA Elute cartridge (FTA cartridge). The FTA cartridge is a solid dry carrier that allows safe transport of cervical samples. FTA cartridge samples were

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)

Calibration of track detectors and measurement of radon exhalation rate from solid samples

International Nuclear Information System (INIS)

Singh, Ajay Kumar; Jojo, P.J.; Prasad, Rajendra; Khan, A.J.; Ramachandran, T.V.

1997-01-01

CR-39 and LR-115 type II track detectors to be used for radon exhalation measurements have been calibrated. The configurations fitted with detectors in Can technique in the open cup mode are cylindrical plastic cup (PC) and conical plastic cup (CPC). The experiment was performed in radon exposure chamber having monodisperse aerosols of 0.2 μm size, to find the relationship between track density and the radon concentration. The calibration factors for PC and CPC type dosimeters with LR-115 type II detector were found to be 0.056 and 0.083 tracks cm -2 d -1 (Bqm -3 ) -1 respectively, while with CR-39 detector the values were 0.149 and 0.150 tracks cm -2 d -1 (Bq m -3 ) -1 . Employing the Can technique, measurements of exhalation rates from solid samples used as construction materials, are undertaken. Radon exhalation rate is found to be minimum in cement samples while in fly ash it is not enhanced as compared to coal samples. (author)

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.

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.

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

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.)

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.

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)

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.

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.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

Science.gov (United States)

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

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%.

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.

Dynamic Flow-through Methods for Metal Fractionation in Environmental Solid Samples

DEFF Research Database (Denmark)

Miró, Manuel; Hansen, Elo Harald; Petersen, Roongrat

occurring processes always take place under dynamic conditions, recent trends have been focused on the development of alternative flow-through dynamic methods aimed at mimicking environmental events more correctly than their classical extraction counterparts. In this lecture particular emphasis is paid......Accummulation of metal ions in different compartments of the biosphere and their possible mobilization under changing environmental conditions induce a pertubation of the ecosystem and may cause adverse health effects. Nowadays, it is widely recognized that the information on total content...... the ecotoxicological significance of metal ions in solid environmental samples. The background of end-over-end fractionation for releasing metal species bound to particular soil phases is initially discussed, its relevant features and limitations being thoroughly described. However, taking into account that naturally...

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.

EPA Method 3135.2I: Cyanide, Total and Amenable in Aqueous and Solid Samples Automated Colorimetric With Manual Digestion

Science.gov (United States)

This method describes procedures for preparation and analysis of solid, water and wipe samples for detection and measurement of cyanide amendable to chlorination using acid digestion and spectrophotometry.

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.

Solvent-assisted dispersive solid-phase extraction: A sample preparation method for trace detection of diazinon in urine and environmental water samples.

Science.gov (United States)

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-09-02

In this research, a sample preparation method termed solvent-assisted dispersive solid-phase extraction (SA-DSPE) was applied. The used sample preparation method was based on the dispersion of the sorbent into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was received by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the diazinon, the cloudy solution was centrifuged and diazinon in the sediment phase dissolved in ethanol and determined by gas chromatography-flame ionization detector. Under the optimized conditions (pH of solution=7.0, Sorbent: benzophenone, 2%, Disperser solvent: ethanol, 500μL, Centrifuge: centrifuged at 4000rpm for 3min), the method detection limit for diazinon was 0.2, 0.3, 0.3 and 0.3μgL(-1) for distilled water, lake water, waste water and urine sample, respectively. Furthermore, the pre-concentration factor was 363.8, 356.1, 360.7 and 353.38 in distilled water, waste water, lake water and urine sample, respectively. SA-DSPE was successfully used for trace monitoring of diazinon in urine, lake and waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Stir-bar supported micro-solid-phase extraction for the determination of polychlorinated biphenyl congeners in serum samples.

Science.gov (United States)

Sajid, Muhammad; Basheer, Chanbasha

2016-07-15

In present work, a new configuration of micro-solid phase extraction was introduced and termed as stir-bar supported micro-solid-phase extraction (SB-μ-SPE). A tiny stir-bar was packed inside the porous polypropylene membrane along with sorbent material and the edges of membrane sheet were heat sealed to secure the contents. The packing of stir-bar inside the μ-SPE device does not allow the device to stick with the wall or any corner of the sample vial during extraction, which is, however, a frequent observation in routine μ-SPE. Moreover, it enhances effective surface area of the sorbent exposed to sample solution through continuous agitation (motion and rotation). It also completely immerses the SB-μ-SPE device in the sample solution even for non-polar sorbents. Polychlorinated biphenyls (PCBs) were selected as model compounds and the method performance was evaluated in human serum samples. After extraction, samples were analyzed by gas chromatography mass spectrometry (GC-MS). The factors that affect extraction efficiency of SB-μ-SPE were optimized. Under optimum conditions, a good linearity (0.1-100ngmL(-1)) with coefficients of determinations ranging from 0.9868 to 0.9992 was obtained. Limits of detections were ranged between 0.003 and 0.047ngmL(-1). Acceptable values for inter-day (3.2-9.1%) and intra-day (3.1-7.2%) relative standard deviations were obtained. The optimized method was successfully applied to determine the concentration of PCB congeners in human serum samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of Sr-90 in environmental samples using solid phase extraction disk

International Nuclear Information System (INIS)

Zal U'yun Wan Mahmood

2002-01-01

A method is described for determination of Sr-90 in environmental samples using solid phase extraction disk (Empore TM Strontium Rad Disk) and GM counter. To determine the optimum condition for capacity of Empore TM Strontium Rad Disk, its characterization studies such as the effects Sr content, acidity (molarity) of acids, presence of Ca 2+ and other major ions (Na + , Mg 2+ etc), influence of interference (Pb and Bi) and others were carried out. An optimized the using of Empore TM Strontium Rad Disk for determination of Sr-90 was validated by application to environmental samples. Quantitative recoveries above 95%for Sr (stable) were recorded in 6M HCl condition. Typical environmental samples may contain an assortment of anionic and cationic species, but in general, Empore TM Strontium Rad Disk has enough capacity to effectively separate Sr for wide variety of aqueous solutions. Sr recovery in a matrix-free or the content of matrix less than 300 mg/sample is typically greater than 99% is reported in this research work. In particular, sample, which may contain interference such as Pb and Bi would require an addition separation step before processing to ensure an accurate measurement of Sr. In this research work, radiotracer 85 Sr was used to monitor the behavior of Sr and calculation its recovery. For analytical methods that can count Y-90, the Sr-90 activity/concentration in environmental sample was calculated. The concentration of Sr-90 in ash sample (Quality Controled Sample) of 276 ± 18 Bq/kg ash was determined from Y-90 activity. The relative percent difference of 1.1% was achievable for Empore TM Sr-Rad Disk methods when compared to the conventional method (fumed-HNO 3 method) - 279 ± 11 Bq/kg ash. (Author)

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.

Chromium speciation in environmental samples using a solid phase spectrophotometric method

Science.gov (United States)

Amin, Alaa S.; Kassem, Mohammed A.

2012-10-01

A solid phase extraction technique is proposed for preconcentration and speciation of chromium in natural waters using spectrophotometric analysis. The procedure is based on sorption of chromium(III) as 4-(2-benzothiazolylazo)2,2'-biphenyldiol complex on dextran-type anion-exchange gel (Sephadex DEAE A-25). After reduction of Cr(VI) by 0.5 ml of 96% concentrated H2SO4 and ethanol, the system was applied to the total chromium. The concentration of Cr(VI) was calculated as the difference between the total Cr and the Cr(III) content. The influences of some analytical parameters such as: pH of the aqueous solution, amounts of 4-(2-benzothiazolylazo)2,2'-biphenyldiol (BTABD), and sample volumes were investigated. The absorbance of the gel, at 628 and 750 nm, packed in a 1.0 mm cell, is measured directly. The molar absorptivities were found to be 2.11 × 107 and 3.90 × 107 L mol-1 cm-1 for 500 and 1000 ml, respectively. Calibration is linear over the range 0.05-1.45 μg L-1 with RSD of <1.85% (n = 8.0). Using 35 mg exchanger, the detection and quantification limits were 13 and 44 ng L-1 for 500 ml sample, whereas for 1000 ml sample were 8.0 and 27 ng L-1, respectively. Increasing the sample volume can enhance the sensitivity. No considerable interferences have been observed from other investigated anions and cations on the chromium speciation. The proposed method was applied to the speciation of chromium in natural waters and total chromium preconcentration in microwave digested tobacco, coffee, tea, and soil samples. The results were simultaneously compared with those obtained using an ET AAS method, whereby the validity of the method has been tested.

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.

Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review.

Science.gov (United States)

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

2013-12-04

Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

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.

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)

Sampling, characterisation and processing of solid recovered fuel production from municipal solid waste: An Italian plant case study.

Science.gov (United States)

Ranieri, Ezio; Ionescu, Gabriela; Fedele, Arcangela; Palmieri, Eleonora; Ranieri, Ada Cristina; Campanaro, Vincenzo

2017-08-01

This article presents the classification of solid recovered fuel from the Massafra municipal solid waste treatment plant in Southern Italy in compliancy with the EN 15359 standard. In order to ensure the reproducibility of this study, the characterisation methods of waste input and output flow, the mechanical biological treatment line scheme and its main parameters for each stage of the processing chain are presented in details, together with the research results in terms of mass balance and derived fuel properties. Under this study, only 31% of refused municipal solid waste input stream from mechanical biological line was recovered as solid recovered fuel with a net heating value (NC=HV) average of 15.77 MJ kg -1 ; chlorine content average of 0.06% on a dry basis; median of mercury solid recovered fuel produced meets the European Union standard requirements and can be classified with the class code: Net heating value (3); chlorine (1); mercury (1).

Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Amberger, Martin A.; Hoeltig, Michael; Broekaert, Jose A.C.

2010-01-01

The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL -1 . As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL -1 of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 μg g -1 for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al 2 O 3 , powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a

Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Amberger, Martin A.; Hoeltig, Michael [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Broekaert, Jose A.C., E-mail: jose.broekaert@chemie.uni-hamburg.d [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

2010-02-15

The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL{sup -1}. As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL{sup -1} of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 mug g{sup -1} for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al{sub 2}O{sub 3}, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective

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

Determination of the Basis for Temperature Compensation in ETC Ignited Solid Propellant Guns

National Research Council Canada - National Science Library

Pesce-Rodriguez, R. A; Beyer, R. A

2004-01-01

A series of experiments and reanalysis of previously published results has led to the discovery of the key interaction between the plasma of an electrothermal igniter and the gun propellant in large caliber cannon...

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.

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.

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.

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

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.

Are Flow Injection-based Approaches Suitable for Automated Handling of Solid Samples?

DEFF Research Database (Denmark)

Miró, Manuel; Hansen, Elo Harald; Cerdà, Victor

Flow-based approaches were originally conceived for liquid-phase analysis, implying that constituents in solid samples generally had to be transferred into the liquid state, via appropriate batch pretreatment procedures, prior to analysis. Yet, in recent years, much effort has been focused...... electrolytic or aqueous leaching, on-line dialysis/microdialysis, in-line filtration, and pervaporation-based procedures have been successfully implemented in continuous flow/flow injection systems. In this communication, the new generation of flow analysis, including sequential injection, multicommutated flow.......g., soils, sediments, sludges), and thus, ascertaining the potential mobility, bioavailability and eventual impact of anthropogenic elements on biota [2]. In this context, the principles of sequential injection-microcolumn extraction (SI-MCE) for dynamic fractionation are explained in detail along...

Preparation of solid-state samples of a transition metal coordination compound for synchrotron radiation photoemission studies

CERN Document Server

Crotti, C; Celestino, T; Fontana, S

2003-01-01

The aim of this research was to identify a sample preparation method suitable for the study of transition metal complexes by photoemission spectroscopy with synchrotron radiation as the X-ray source, even in the case where the compound is not evaporable. Solid-phase samples of W(CO) sub 4 (dppe) [dppe=1,2-bis(diphenylphosphino)ethane] were prepared according to different methods and their synchrotron radiation XPS spectra measured. The spectra acquired from samples prepared by spin coating show core level peaks only slightly broader than the spectrum recorded from UHV evaporated samples. Moreover, for these samples the reproducibility of the binding energy values is excellent. The dependence of the spin coating technique on parameters such as solvent and solution concentration, spinning speed and support material was studied. The same preparation method also allowed the acquisition of valence band spectra, the main peaks of which were clearly resolved. The results suggest that use of the spin coating techniqu...

Liquid-solid extraction of uranium (VI) with TOPO - molten naphthalene and determination by laser fluorimetry in geological samples

International Nuclear Information System (INIS)

Kumar, Sanjay; Krishnakumar, M.; Patwardhan, A.A.

2007-01-01

A simple, rapid, sensitive, cost-effective and efficient method for separation of uranium using tri-n-octylphosphine oxide (TOPO)-molten naphthalene as solid phase extractant and its determination by laser fluorimetry in geological samples (rock, soil, sediment) was developed. Under optimum conditions, using 50 mg TOPO and 100 mg naphthalene, 50 - 5000 ng of uranium in 10 ml sample solution (3% (v/v) HNO 3 ) could be extracted quantitatively. The extracted uranium was stripped using tetra sodium pyrophosphate (5% (v/v) solution, pH adjusted to 7.0 with H 3 PO 4 ) and determined by laser fluorimetry. The influence of different acid concentrations, the amount of solid phase extractant, sample volumes, different stripping reagents, their volumes and effect of foreign ions on the extraction and determination of uranium (VI) were investigated. Synthetic samples of varying concentration as regards uranium were prepared and analysed. Recoveries ranging from 90% to 105% were obtained. The method was validated by analyzing four certified reference materials namely, BL-5, DH-1a, SY-2, SY-3 and the values obtained for uranium agreed well with the certified values. The method was also applied to the determination of uranium in geological samples (rock, soil and sediment) by laser fluorimetry and the results obtained compared favorably with those obtained from the pellet fluorimetry method. Following the proposed method, determination limit for uranium was found to be 1 μg/g with RSD ± 10%. (author)

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.

A long-term validation of the modernised DC-ARC-OES solid-sample method.

Science.gov (United States)

Flórián, K; Hassler, J; Förster, O

2001-12-01

The validation procedure based on ISO 17025 standard has been used to study and illustrate both the longterm stability of the calibration process of the DC-ARC solid sample spectrometric method and the main validation criteria of the method. In the calculation of the validation characteristics depending on the linearity(calibration), also the fulfilment of predetermining criteria such as normality and homoscedasticity was checked. In order to decide whether there are any trends in the time-variation of the analytical signal or not, also the Neumann test of trend was applied and evaluated. Finally, a comparison with similar validation data of the ETV-ICP-OES method was carried out.

Multielement trace determination in SiC powders: assessment of interlaboratory comparisons aimed at the validation and standardization of analytical procedures with direct solid sampling based on ETV ICP OES and DC arc OES.

Science.gov (United States)

Matschat, Ralf; Hassler, Jürgen; Traub, Heike; Dette, Angelika

2005-12-01

The members of the committee NMP 264 "Chemical analysis of non-oxidic raw and basic materials" of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to "the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials" by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and

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

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.

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

Innovative separation and preconcentration technique of coagulating homogenous dispersive micro solid phase extraction exploiting graphene oxide nanosheets.

Science.gov (United States)

Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Rashidi, Ali Morad; Shirkhanloo, Hamid; Rahighi, Reza

2016-01-01

A uniquely novel, fast, and facile technique is introduced for the first time in which a scant amount of graphene oxide (GO), without modification, has been utilized in dispersive mode of solid phase extraction (SPE) for an efficient yet simple separation. The proposed method of coagulating homogenous dispersive micro solid phase extraction (CHD-µSPE) is based on coagulation of homogeneous GO solution with the aid of polyetheneimine (PEI). CHD-µSPE use full adsorption capacity of GO because in this method was used GO solution obtained from synthesis process without drying step and stacking nanosheets. In optimized condition, 30 µL GO solution (7 mg mL(-1)), obtained in synthesis process, was injected into 1.5 mL the sample solution followed by immediate injection of 53 µL PEI solution (1 mg mL(-1)). After inserting PEI, GO sheets aggregate and can be readily separated by centrifugation. PEI not only cause aggregation of GO, but also form three-dimensional network of GO with easy handling in following separation steps. Lead, cadmium, and chromium were selected as model analytes and the effecting parameters including the amount of GO, concentration of PEI, sample pH, extraction time, and type of desorption solvent were investigated and optimized. The results indicate that the proposed CHD-µSPE method can be successfully applied GO in dispersive mode of SPE without effecting on good capability adsorption of GO. The novel method was applied in determination of lead, cadmium, and chromium in water, human saliva, and urine samples by electrothermal atomic absorption spectrometry. The detection limits are as low as 0.035, 0.005, and 0.012 µg L(-1) for Pb, Cd, and Cr respectively. The intra-day precisions (RSDs) were lower than 3.8%. CHD-µSPE method showed a good linear ranges of 0.24-15.6, 0.015-0.95 and 0.039-2.33 µg L(-1) for Pb, Cd and Cr respectively. Method performance was investigated by determination of mentioned metal ions in river water, human urine and

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

Assessment of Metaborate Fusion for the Rapid Dissolution of Solid Samples: Suitability with the Northstar ARSIIe

Science.gov (United States)

2016-07-01

5 Table 3. Residual Silicates avec Flocculation in Glass Beaker or Polyethylene Cone ................ 8 Table 4...is formed. Since the concentration of silicates in soil or sediment is high (up to 70-75% in silicon dioxide ( SiO2 ) in some cases), the condensation...flux, for the fusion of acidic samples such as solids containing a significant portion of SiO2 . Conversely, lithium tetraborate, an acidic flux, will

System and process for dissolution of solids

Science.gov (United States)

Liezers, Martin; Farmer, III, Orville T.

2017-10-10

A system and process are disclosed for dissolution of solids and "difficult-to-dissolve" solids. A solid sample may be ablated in an ablation device to generate nanoscale particles. Nanoparticles may then swept into a coupled plasma device operating at atmospheric pressure where the solid nanoparticles are atomized. The plasma exhaust may be delivered directly into an aqueous fluid to form a solution containing the atomized and dissolved solids. The composition of the resulting solution reflects the composition of the original solid sample.

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.

Interfering removal in samples with high amounts of dissolved solids for the determination of arsenic and selenium by TXRF

International Nuclear Information System (INIS)

Menegario, Amauri A.; Gomes, Ana Carla F.; Pellegrinotti, Daniel C.; Gine, Maria F.; Krug, Francisco J.; Nascimento Filho, Virgilio F.

2002-01-01

A matrix separation flow system coupled with total reflection X-ray fluorescence (TXRF) is proposed to remove Ca ++ , Mg ++ , Na + and K + major cations from samples containing high amounts of totally dissolved solids, using solid-liquid phases in flow system. This system is assembled with a 1.25 mL column of AG50W-X8 resin (in protonated form) and manual commutator, allowed the separation, addition of internal standard and subsequently a 40 μL aliquot of the eluate was deposited in the reflector support, dried in a furnace for 12 hours at 60 ± 5 deg C and analysed by TXRF. All the procedure is carried out in about 90 s and 0.5 mL of sample are required. The proposed approach was applied for determination of As and Se in plant material and sea water samples. When comparing with direct analysis (without separation), a reduction of 2 to 6 times on the limits of detection for these elements was attained. The accuracy of this methodology was satisfactory for As and Se in sea water and Se in rice certified samples. This procedure could be also used for Pb interference removal in the determination of As by X-ray fluorescence. (author)

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...

Direct observation of electrothermal instability structures on intensely Ohmically heated aluminum with current flowing in a surface skin layer

Science.gov (United States)

Awe, Thomas

2017-10-01

Implosions on the Z Facility assemble high-energy-density plasmas for radiation effects and ICF experiments, but achievable stagnation pressures and temperatures are degraded by the Magneto-Rayleigh-Taylor (MRT) instability. While the beryllium liners (tubes) used in Magnetized Liner Inertial Fusion (MagLIF) experiments are astonishingly smooth (10 to 50 nm RMS roughness), they also contain distributed micron-scale resistive inclusions, and large MRT amplitudes are observed. Early in the implosion, an electrothermal instability (ETI) may provide a perturbation which greatly exceeds the initial surface roughness of the liner. Resistive inhomogeneities drive nonuniform current density and Joule heating, resulting in locally higher temperature, and thus still higher resistivity. Such unstable temperature and pressure growth produce density perturbations which seed MRT. For MagLIF liners, ETI seeding of MRT has been inferred by evaluating late-time MRT, but a direct observation of ETI is not made. ETI is directly observed on the surface of 1.0-mm-diameter solid Al rods pulsed to 1 MA in 100 ns via high resolution gated optical imaging (2 ns temporal and 3 micron spatial resolution). Aluminum 6061 alloy rods, with micron-scale resistive inclusions, consistently first demonstrate overheating from distinct, 10-micron-scale, sub-eV spots, which 5-10 ns later merge into azimuthally stretched elliptical spots and discrete strata (40-100 microns wide by 10 microns tall). Axial plasma filaments form shortly thereafter. Surface plasma can be suppressed for rods coated with dielectric, enabling extended study of the evolution of stratified ETI structures, and experimental inference of ETI growth rates. This fundamentally new and highly 3-dimensional dataset informs ETI physics, including when the ETI seed of MRT may be initiated.

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.

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.

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

Science.gov (United States)

Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

2018-01-01

Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

Selective solid-phase extraction of Ni(II) by an ion-imprinted polymer from water samples

International Nuclear Information System (INIS)

Saraji, Mohammad; Yousefi, Hamideh

2009-01-01

A new ion-imprinted polymer (IIP) material was synthesized by copolymerization of 4-vinylpyridine as monomer, ethyleneglycoldimethacrylate as crosslinking agent and 2,2'-azobis-sobutyronitrile as initiator in the presence of Ni-dithizone complex. The IIP was used as sorbent in a solid-phase extraction column. The effects of sampling volume, elution conditions, sample pH and sample flow rate on the extraction of Ni ions form water samples were studied. The maximum adsorption capacity and the relative selectivity coefficients of imprinted polymer for Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were calculated. Compared with non-imprinted polymer particles, the IIP had higher selectivity for Ni(II). The relative selectivity factor (α r ) values of Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were 21.6, 54.3, and 22.7, respectively, which are greater than 1. The relative standard deviation of the five replicate determinations of Ni(II) was 3.4%. The detection limit for 150 mL of sample was 1.6 μg L -1 using flame atomic absorption spectrometry. The developed method was successfully applied to the determination of trace nickel in water samples with satisfactory results.

Solid phase extraction for sample preparation in trace analysis of ionogenic compounds by capillary isotachophoresis

International Nuclear Information System (INIS)

Hutta, M.; Kaniansky, D.; Simunicova, E.; Zelenska, V.; Madajova, V.; Siskova, A.

1992-01-01

Various sorbents recommended for solid phase extraction (SPE) in sample preparation procedures were studied for use in combination with capillary isotachophoresis (ITP). They were very efficient in achieving trace concentration levels (low ppb, i.e., low parts per 10 9 ) for different types of ITP analytes present in environmental and biological matrices. A macroporous carbon sorbent was convenient for sample preparation in ITP analysis of short chain fatty acids (C 4 -C 9 ) in drinking water. Chelating sorbents based on hydroxyalkyl methacrylate matrix with salicylate, thioglycolate and 8-hydroxyquinolinate functionalities were found to be very suitable for preconcentration of heavy metals with an inherent sample clean-up. An octadecyl-bonded silica sorbent enabled in ITP a photometric detection of γ-aminobutyrate (labeled with a 2,4,6-trinitrophenyl group) at concentrations considerably lower than required for the determination of this amino acid in cerebrospinal fluid (∼5*10 -8 mol/l). (author) 34 refs.; 3 figs.; 1 tab

Hexagonal boron nitride nanosheets as adsorbents for solid-phase extraction of polychlorinated biphenyls from water samples

Energy Technology Data Exchange (ETDEWEB)

Jia, Shiliang; Wang, Zhenhua; Ding, Ning [Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Academy of Sciences, Jinan, Shandong (China); Elaine Wong, Y.-L. [Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Chen, Xiangfeng, E-mail: xiangfchensdas@163.com [Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Academy of Sciences, Jinan, Shandong (China); Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Qiu, Guangyu [Department of Physics and Materials Science, City University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Dominic Chan, T.-W., E-mail: twdchan@cuhk.edu.hk [Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong)

2016-09-14

The adsorptive potential of hexagonal boron nitride nanosheets (h-BNNSs) for solid-phase extraction (SPE) of pollutants was investigated for the first time. Seven indicators of polychlorinated biphenyls (PCBs) were selected as target analytes. The adsorption of PCBs on the surface of the h-BNNSs in water was simulated by the density functional theory and molecular dynamics. The simulation results indicated that the PCBs are adsorbed on the surface by π–π, hydrophobic, and electrostatic interactions. The PCBs were extracted with an h-BNNS-packed SPE cartridge, and eluted by dichloromethane. Gas chromatography–tandem mass spectrometry working in the multiple reaction monitor mode was used for the sample quantification. The effect of extraction parameters, including the flow rate, pH value, breakthrough volume, and the ionic strength, were investigated. Under the optimal working conditions, the developed method showed low limits of detection (0.24–0.50 ng L{sup −1}; signal-to-noise ratio = 3:1), low limits of quantification (0.79–1.56 ng L{sup −1}; signal-to-noise ratio = 10:1), satisfactory linearity (r > 0.99) within the concentration range of 2–1000 ng L{sup −1}, and good precision (relative standard deviation < 12%). The PCBs concentration in environmental water samples was determined by the developed method. This results demonstrate that h-BNNSs have high analytical potential in the enrichment of pollutants. - Highlights: • The hexagonal boron nitride nanosheets were synthesized. • The nanosheets were used as adsorbent for solid-phase extraction. • The h-BN demonstrates remarkable adsorption of PCBs from water samples. • The method was successfully applied in determination of PCBs in water samples.

Development of Solid Ceramic Dosimeters for the Time-Integrative Passive Sampling of Volatile Organic Compounds in Waters.

Science.gov (United States)

Bonifacio, Riza Gabriela; Nam, Go-Un; Eom, In-Yong; Hong, Yong-Seok

2017-11-07

Time-integrative passive sampling of volatile organic compounds (VOCs) in water can now be accomplished using a solid ceramic dosimeter. A nonporous ceramic, which excludes the permeation of water, allowing only gas-phase diffusion of VOCs into the resin inside the dosimeter, effectively captured the VOCs. The mass accumulation of 11 VOCs linearly increased with time over a wide range of aqueous-phase concentrations (16.9 to 1100 μg L -1 ), and the linearity was dependent upon the Henry's constant (H). The average diffusivity of the VOCs in the solid ceramic was 1.46 × 10 -10 m 2 s -1 at 25 °C, which was 4 orders of magnitude lower than that in air (8.09 × 10 -6 m 2 s -1 ). This value was 60% greater than that in the water-permeable porous ceramic (0.92 × 10 -10 m 2 s -1 ), suggesting that its mass accumulation could be more effective than that of porous ceramic dosimeters. The mass accumulation of the VOCs in the solid ceramic dosimeter increased in the presence of salt (≥0.1 M) and with increasing temperature (4 to 40 °C) but varied only slightly with dissolved organic matter concentration. The solid ceramic dosimeter was suitable for the field testing and measurement of time-weighted average concentrations of VOC-contaminated waters.

Innovative separation and preconcentration technique of coagulating homogenous dispersive micro solid phase extraction exploiting graphene oxide nanosheets

Energy Technology Data Exchange (ETDEWEB)

Ghazaghi, Mehri [Department of Chemistry, College of Science, Semnan University, P.O. Box: 35131-19111, Semnan (Iran, Islamic Republic of); Mousavi, Hassan Zavvar, E-mail: hzmousavi@semnan.ac.ir [Department of Chemistry, College of Science, Semnan University, P.O. Box: 35131-19111, Semnan (Iran, Islamic Republic of); Rashidi, Ali Morad [Nanotechnology Research Center, Research Institute of Petroleum Industry (RIPI), West Entrance Blvd., Olympic Village, P.O. Box: 14857-33111, Tehran (Iran, Islamic Republic of); Shirkhanloo, Hamid [Occupational and Environmental Health Research Center (OEHRC), Iranian Petroleum Industry Health Research Institute (IPIHRI), Tehran (Iran, Islamic Republic of); Rahighi, Reza [Nanotechnology Research Center, Research Institute of Petroleum Industry (RIPI), West Entrance Blvd., Olympic Village, P.O. Box: 14857-33111, Tehran (Iran, Islamic Republic of); Department of Research and Development, Sharif Ultrahigh Nanotechnologists (SUN) Company, P.O. Box: 13488-96394, Tehran (Iran, Islamic Republic of)

2016-01-01

A uniquely novel, fast, and facile technique is introduced for the first time in which a scant amount of graphene oxide (GO), without modification, has been utilized in dispersive mode of solid phase extraction (SPE) for an efficient yet simple separation. The proposed method of coagulating homogenous dispersive micro solid phase extraction (CHD-µSPE) is based on coagulation of homogeneous GO solution with the aid of polyetheneimine (PEI). CHD-µSPE use full adsorption capacity of GO because in this method was used GO solution obtained from synthesis process without drying step and stacking nanosheets. In optimized condition, 30 µL GO solution (7 mg mL{sup −1}), obtained in synthesis process, was injected into 1.5 mL the sample solution followed by immediate injection of 53 µL PEI solution (1 mg mL{sup −1}). After inserting PEI, GO sheets aggregate and can be readily separated by centrifugation. PEI not only cause aggregation of GO, but also form three-dimensional network of GO with easy handling in following separation steps. Lead, cadmium, and chromium were selected as model analytes and the effecting parameters including the amount of GO, concentration of PEI, sample pH, extraction time, and type of desorption solvent were investigated and optimized. The results indicate that the proposed CHD-µSPE method can be successfully applied GO in dispersive mode of SPE without effecting on good capability adsorption of GO. The novel method was applied in determination of lead, cadmium, and chromium in water, human saliva, and urine samples by electrothermal atomic absorption spectrometry. The detection limits are as low as 0.035, 0.005, and 0.012 µg L{sup −1} for Pb, Cd, and Cr respectively. The intra-day precisions (RSDs) were lower than 3.8%. CHD-µSPE method showed a good linear ranges of 0.24–15.6, 0.015–0.95 and 0.039–2.33 µg L{sup −1} for Pb, Cd and Cr respectively. Method performance was investigated by determination of mentioned

Electrothermal modeling, fabrication and analysis of low-power consumption thermal actuator with buckling arm

KAUST Repository

So, Hongyun

2013-10-31

© 2013, Springer-Verlag Berlin Heidelberg. This paper reports on a novel thermal actuator with sub-micron metallic structures and a buckling arm to operate with low voltages and to generate very large deflections, respectively. A lumped electrothermal model and analysis were also developed to validate the mechanical design and easily predict the temperature distribution along arms of the sub-micron actuator. The actuator was fabricated via the combination of electron beam lithography to form actuator arms with a minimum feature size of 200 nm and lift-off process to deposit a high aspect ratio nickel structure. Reproducible displacements of up to 1.9 μm at the tip were observed up to 250 mV under confocal microscope. The experimentally measured deflection values and theoretically calculated temperature distribution by the developed model were compared with finite element analysis results and they were in good agreement. This study shows a promising approach to develop more sophisticated nano actuators required larger deflections for manipulation of sub-micron scale objects with low-power consumption.

Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples

International Nuclear Information System (INIS)

Ghaedi, M.; Ahmadi, F.; Soylak, M.

2007-01-01

A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni 2+ , Cu 2+ and Co 2+ ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 μg L -1 for copper, 0.75 μg L -1 for nickel and 0.80 μg L -1 for cobalt. The loading capacity was 0.56 mg g -1 for Ni 2+ , 0.50 mg g -1 for Cu 2+ and 0.47 mg g -1 for Co 2+ . The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n = 3)

Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples

Energy Technology Data Exchange (ETDEWEB)

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

2007-08-17

A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni{sup 2+}, Cu{sup 2+} and Co{sup 2+} ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 {mu}g L{sup -1} for copper, 0.75 {mu}g L{sup -1} for nickel and 0.80 {mu}g L{sup -1} for cobalt. The loading capacity was 0.56 mg g{sup -1} for Ni{sup 2+}, 0.50 mg g{sup -1} for Cu{sup 2+} and 0.47 mg g{sup -1} for Co{sup 2+}. The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n = 3)

Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples.

Science.gov (United States)

Ghaedi, M; Ahmadi, F; Soylak, M

2007-08-17

A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni2+, Cu2+ and Co2+ ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 microg L(-1) for copper, 0.75 microg L(-1) for nickel and 0.80 microg L(-1) for cobalt. The loading capacity was 0.56 mg g(-1) for Ni2+, 0.50 mg g(-1) for Cu2+ and 0.47 mg g(-1) for Co2+. The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n=3).

Solid-Phase Extraction Strategies to Surmount Body Fluid Sample Complexity in High-Throughput Mass Spectrometry-Based Proteomics

Science.gov (United States)

Bladergroen, Marco R.; van der Burgt, Yuri E. M.

2015-01-01

For large-scale and standardized applications in mass spectrometry- (MS-) based proteomics automation of each step is essential. Here we present high-throughput sample preparation solutions for balancing the speed of current MS-acquisitions and the time needed for analytical workup of body fluids. The discussed workflows reduce body fluid sample complexity and apply for both bottom-up proteomics experiments and top-down protein characterization approaches. Various sample preparation methods that involve solid-phase extraction (SPE) including affinity enrichment strategies have been automated. Obtained peptide and protein fractions can be mass analyzed by direct infusion into an electrospray ionization (ESI) source or by means of matrix-assisted laser desorption ionization (MALDI) without further need of time-consuming liquid chromatography (LC) separations. PMID:25692071

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

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.

Analysis of microcontaminants in aqueous samples by fully automated on-line solid-phase extraction-gas chromatography-mass selective detection.

NARCIS (Netherlands)

Louter, A.J.H.; van Beekvelt, C.A.; Cid Montanes, P.; Slobodník, J.; Vreuls, J.J.; Brinkman, U.A.T.

1996-01-01

The trace-level analysis of unknown organic pollutants in water requires the use of fast and sensitive methods which also provide structural information. In the present study, an on-line technique was used which combines sample preparation by means of solid-phase extraction (SPE) on a small

Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Orani, Anna Maria; Han, Eunmi; Mandjukov, Petko; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

2015-01-01

Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine sediment samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS AAS) and direct solid sample analysis has been developed. The application of fast programs in combination with direct solid sampling allows to eliminate the drying and pretreatment steps, however makes impossible the use of liquid standards for calibration. Iridium treated platforms were applied throughout the present study. Calibration technique based on the use of solid certified reference materials (marine sediments) similar to the nature of the analyzed sample and statistics of regression analysis were applied to the real sediment samples. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signals. The ISO-17025 requirements and Eurachem guidelines were followed in the validation of the proposed analytical procedure. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability reproducibility, limits of detection and quantification and expanded uncertainty (k = 2) for all investigated elements were assessed. Two different approaches for the estimation of measurement uncertainty were applied and obtained results compared. The major contributors to the combined uncertainty of the analyte mass fraction were found to be the homogeneity of the samples and the microbalance precision. The influence of sample particle sizes on the total combined uncertainty was also evaluated. Traceability to SI system of units of the obtained by the proposed analytical procedure results was demonstrated. Additionally, validation of the methodology developed was effectuated by the comparison of the obtained results with independent method e.g. ICP-MS with external calibration. The use of solid sampling HR CS AAS for the determination of trace elements in marine sediment matrix gives significant advantages

Preliminary evaluation of new polymer matrix for solid-phase extraction of nonylphenol from water samples.

Science.gov (United States)

Guerreiro, António; Soares, Ana; Piletska, Elena; Mattiasson, Bo; Piletsky, Sergey

2008-03-31

Molecularly imprinted (MIP) and blank polymers with affinity for nonylphenol were designed using computational modelling. Chromatographic tests demonstrated higher affinity of imprinted polymers towards the template nonylphenol as compared with blank polymers. The performance of both polymers in solid-phase extraction was however very similar. Both blank and imprinted polymers appeared to be suitable for the removal and pre-concentration of nonylphenol from contaminated water samples with 99% efficiency of the recovery. The commercial resins PH(EC) (Biotage) and C18 (Varian) tested in the same conditions used for comparative purposes had recovery rate <84%. The polymer capacity for nonylphenol was 231 mg g(-1) for blank and 228 mg g(-1) for MIP. The synthesised materials can have significance for sample pre-concentration and environmental analysis of this class of compounds.

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)

Major- and minor-metal composition of three distinct solid material fractions associated with Juan de Fuca hydrothermal fluids (northeast Pacific), and calculation of dilution fluid samples

Science.gov (United States)

Hinkley, T.K.; Seeley, J.L.; Tatsumoto, M.

1988-01-01

Three distinct types of solid material are associated with each sample of the hydrothermal fluid that was collected from the vents of the Southern Juan de Fuca Ridge. The solid materials appear to be representative of deposits on ocean floors near mid-ocean ridges, and interpretation of the chemistry of the hydrothermal solutions requires understanding of them. Sr isotopic evidence indicates that at least two and probably all three of these solid materials were removed from the solution with which they are associated, by precipitation or adsorption. This occurred after the "pure" hydrothermal fluid was diluted and thoroughly mixed with ambient seawater. The three types of solid materials, are, respectively, a coarse Zn- and Fe-rich material with small amounts of Na and Ca; a finer material also rich in Zn and Fe, but with alkali and alkaline-earth metals; and a scum composed of Ba or Zn, with either considerable Fe or Si, and Sr. Mineral identification is uncertain because of uncertain anion composition. Only in the cases of Ba and Zn were metal masses greater in solid materials than in the associated fluids. For all other metals measured, masses in fluids dwarf those in solids. The fluids themselves contain greater concentrations of all metals measured, except Mg, than seawater. We discuss in detail the relative merits of two methods of determining the mixing proportions of "pure" hydrothermal solution and seawater in the fluids, one based on Sr isotopes, and another previously used method based on Mg concentrations. Comparison of solute concentrations in the several samples shows that degree of dilution of "pure" hydrothermal solutions by seawater, and amounts of original solutes that were removed from it as solid materials, are not related. There is no clear evidence that appreciable amounts of solid materials were not conserved (lost) either during or prior to sample collection. ?? 1988.

Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

Energy Technology Data Exchange (ETDEWEB)

Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

2015-03-01

The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration.

Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

International Nuclear Information System (INIS)

Hu, Qiufen; Yang, Guangyu; Huang, Zhangjie; Yin, Jiayuan

2004-01-01

A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with C 18 membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with C 18 membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was 1.32 x 10 5 L mol -1 cm -1 at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 μg/mL. This method was applied to the determination of nickel in water and biological samples with good results

Solid phase assays

International Nuclear Information System (INIS)

Reese, M.G.; Johnson, L.R.; Ransom, D.K.

1980-01-01

In a solid phase assay for quantitative determination of biological and other analytes, a sample such as serum is contacted with a receptor for the analyte being assayed, the receptor being supported on a solid support. No tracer for the analyte is added to the sample before contacting with the receptor; instead the tracer is contacted with the receptor after unbound analyte has been removed from the receptor. The assay can be otherwise performed in a conventional manner but can give greater sensitivity. (author)

Comparison of 22G reverse-beveled versus standard needle for endoscopic ultrasound-guided sampling of solid pancreatic lesions

Science.gov (United States)

Alatawi, Abdullah; Beuvon, Frédéric; Grabar, Sophie; Leblanc, Sarah; Chaussade, Stanislas; Terris, Benoit; Barret, Maximilien

2015-01-01

Objectives Endoscopic ultrasound-guided fine-needle aspiration (EUS-FNA) using standard needles has a high diagnostic value in the evaluation of solid pancreatic masses. Fenestrated needles have been developed to improve the quality of EUS-guided tissue sampling by providing core biopsies (FNB). Methods Patients with solid pancreatic masses of >2 cm were prospectively included in our study and randomized to receive EUS sampling, using either a standard 22G FNA or a 22G Procore® FNB needle. The main study endpoint was the number of needle passes required to obtain a diagnosis in more than 90% of cases. Results We included 100 patients (male = 63, female = 37; mean age = 68.4 years) in our study. We found that 88% of the lesions were malignant, with a mean size of 32 mm. A sample adequate for diagnosis was obtained in more than 90% of cases after the second needle pass in the FNB group, versus the third needle pass in the FNA group. Slide cellularity and presence of tissue microfragments were significantly higher in the FNB group. Sensitivity for the diagnosis of malignancy was 88.4% versus 97.8% for the EUS-FNA and EUS-FNB group, respectively, while specificity for both techniques was 100%. No complications were recorded. Conclusions Although the accuracy of both needle types for proving malignancy was similar, a lower number of passes was required with the FNB needles to achieve the same contributive sample rate as with the FNA needles. FNB also improved the histopathological quality of specimens, suggesting an overall superiority of FNB sampling. PMID:26279842

Perspectives of an acoustic–electrostatic/electrodynamic hybrid levitator for small fluid and solid samples

International Nuclear Information System (INIS)

Lierke, E G; Holitzner, L

2008-01-01

The feasibility of an acoustic–electrostatic hybrid levitator for small fluid and solid samples is evaluated. A proposed design and its theoretical assessment are based on the optional implementation of simple hardware components (ring electrodes) and standard laboratory equipment into typical commercial ultrasonic standing wave levitators. These levitators allow precise electrical charging of drops during syringe- or ink-jet-type deployment. The homogeneous electric 'Millikan field' between the grounded ultrasonic transducer and the electrically charged reflector provide an axial compensation of the sample weight in an indifferent equilibrium, which can be balanced by using commercial optical position sensors in combination with standard electronic PID position control. Radial electrostatic repulsion forces between the charged sample and concentric ring electrodes of the same polarity provide stable positioning at the centre of the levitator. The levitator can be used in a pure acoustic or electrostatic mode or in a hybrid combination of both subsystems. Analytical evaluations of the radial–axial force profiles are verified with detailed numerical finite element calculations under consideration of alternative boundary conditions. The simple hardware modification with implemented double-ring electrodes in ac/dc operation is also feasible for an electrodynamic/acoustic hybrid levitator

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.

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

Rapid determination of trace level copper in tea infusion samples by solid contact ion selective electrode

Directory of Open Access Journals (Sweden)

Aysenur Birinci

2016-07-01

Full Text Available A new solid contact copper selective electrode with a poly (vinyl chloride (PVC membrane consisting of o-xylylenebis(N,N-diisobutyldithiocarbamate as ionophore has been prepared. The main novelties of constructed ion selective electrode concept are the enhanced robustness, cheapness, and fastness due to the use of solid contacts. The electrode exhibits a rapid (< 10 seconds and near-Nernstian response to Cu2+ activity from 10−1 to 10−6 mol/L at the pH range of 4.0–6.0. No serious interference from common ions was found. The electrode characterizes by high potential stability, reproducibility, and full repeatability. The electrode was used as an indicator electrode in potentiometric titration of Cu(II ions with EDTA and for the direct assay of tea infusion samples by means of the calibration graph technique. The results compared favorably with those obtained by the atomic absorption spectroscopy (AAS.

Characterization of an electrothermal plasma source for fusion transient simulations

Science.gov (United States)

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

2018-01-01

The realization of fusion energy requires materials that can withstand high heat and particle fluxes at the plasma material interface. In this work, an electrothermal (ET) plasma source has been designed as a transient heat flux source for a linear plasma material interaction device. An ET plasma source operates in the ablative arc regime driven by a DC capacitive discharge. The current channel width is defined by the 4 mm bore of a boron nitride liner. At large plasma currents, the arc impacts the liner wall, leading to high particle and heat fluxes to the liner material, which subsequently ablates and ionizes. This results in a high density plasma with a large unidirectional bulk flow out of the source exit. The pulse length for the ET source has been optimized using a pulse forming network to have durations of 1 and 2 ms. The peak currents and maximum source energies seen in this system are 1.9 kA and 1.2 kJ for the 2 ms pulse and 3.2 kA and 2.1 kJ for the 1 ms pulse, respectively. This work is a proof of the principal project to show that an ET source produces electron densities and heat fluxes comparable to those anticipated in transient events in large future magnetic confinement fusion devices. Heat flux, plasma temperature, and plasma density were determined for each shot using infrared imaging and optical spectroscopy techniques. This paper will discuss the assumptions, methods, and results of the experiments.

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD and Dispersive Solid Phase Extraction (d-SPE of Plant Samples

Directory of Open Access Journals (Sweden)

Ireneusz Sowa

2018-03-01

Full Text Available Polyaniline (PANI is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME. In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI was used for dispersive solid phase extraction (d-SPE and matrix solid–phase extraction (MSPD. The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples.

STEALTH: a Lagrange explicit finite difference code for solids, structural, and thermohydraulic analysis. Volume 2: sample and verification problems. Computer code manual

International Nuclear Information System (INIS)

Hofmann, R.

1982-08-01

STEALTH sample and verification problems are presented to help users become familiar with STEALTH capabilities, input, and output. Problems are grouped into articles which are completely self-contained. The pagination in each article is A.n, where A is a unique alphabetic-character article identifier and n is a sequential page number which starts from 1 on the first page of text for each article. Articles concerning new capabilities will be added as they become available. STEALTH sample and verification calculations are divided into the following general categories: transient mechanical calculations dealing with solids; transient mechanical calculations dealing with fluids; transient thermal calculations dealing with solids; transient thermal calculations dealing with fluids; static and quasi-static calculations; and complex boundary interaction calculations

A sensitive method for determining total vanadium in water samples using colorimetric-solid-phase extraction-fiber optic reflectance spectroscopy

International Nuclear Information System (INIS)

Filik, Hayati; Yanaz, Zeynep

2009-01-01

A selective colorimetric-solid-phase extraction (C-SPE) method for the determination of total vanadium in water samples was developed. This method introduced a new variation of C-SPE. The colour reaction is based on the reaction of vanadium(V) ternary complex formed with 1-(2-Pyridylazo)-2-naphtol (PAN) in the presence hydrogen peroxide (H 2 O 2 ). In this technique, the target analytes in samples are extracted onto solid matrix loaded with a colorimetric reagent and then quantified directly on the adsorbent surface by using a miniature fiber optic reflectance spectrometer. The measurements were carried out at a wavelength of 589.4 nm since it yielded the largest divergence different in reflectance spectra before and after reaction with the vanadium. The overall time required for the C-SPE procedure was ∼20 min. The amount of concentrated V is then determined in a few seconds by using miniature reflectance spectrometer. At the optimal conditions, a calibration curve was constructed, revealing a linear range of 0.05-0.52 mg L -1 and a detection limit as low as 0.01 mg L -1 while the RSD lower than 2.8%. In order to verify the accuracy of the method, a certified reference water samples (TMDA) were analysed and the results obtained were in good agreement with the certified values. The proposed method was applied to the determination of vanadium in tap water, seawater samples with a recovery for the spiked samples in the range of 98-102%.

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.

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.

Box-Behnken design in modeling of solid-phase tea waste extraction for the removal of uranium from water samples

Energy Technology Data Exchange (ETDEWEB)

Khajeh, Mostafa; Jahanbin, Elham; Ghaffari-Moghaddam, Mansour; Moghaddam, Zahra Safaei [Zabol Univ. (Iran, Islamic Republic of). Dept. of Chemistry; Bohlooli, Mousa [Zabol Univ. (Iran, Islamic Republic of). Dept. of Biology

2015-07-01

In this study, the solid-phase tea waste procedure was used for separation, preconcentration and determination of uranium from water samples by UV-Vis spectrophotometer. In addition, Box-Behnken experimental design was employed to investigated the influence of six variables including pH, mass of adsorbent, eluent volume, amount of 1-(2-pyridylazo)-2-naphthol (PAN); and sample and eluent flow rates on the extraction of analyte. High determination coefficient (R{sup 2}) of 0.972 and adjusted-R{sup 2} of 0.943 showed the satisfactory adjustment of the polynomial regression model. This method was used for the extraction of uranium from real water samples.

Box-Behnken design in modeling of solid-phase tea waste extraction for the removal of uranium from water samples

International Nuclear Information System (INIS)

Khajeh, Mostafa; Jahanbin, Elham; Ghaffari-Moghaddam, Mansour; Moghaddam, Zahra Safaei; Bohlooli, Mousa

2015-01-01

In this study, the solid-phase tea waste procedure was used for separation, preconcentration and determination of uranium from water samples by UV-Vis spectrophotometer. In addition, Box-Behnken experimental design was employed to investigated the influence of six variables including pH, mass of adsorbent, eluent volume, amount of 1-(2-pyridylazo)-2-naphthol (PAN); and sample and eluent flow rates on the extraction of analyte. High determination coefficient (R 2 ) of 0.972 and adjusted-R 2 of 0.943 showed the satisfactory adjustment of the polynomial regression model. This method was used for the extraction of uranium from real water samples.

A large-strain, fast-response, and easy-to-manufacture electrothermal actuator based on laser-reduced graphene oxide

Science.gov (United States)

Zhang, Tian-Yu; Wang, Qian; Deng, Ning-Qin; Zhao, Hai-Ming; Wang, Dan-Yang; Yang, Zhen; Liu, Ying; Yang, Yi; Ren, Tian-Ling

2017-09-01

In this paper, we have developed a high-performance graphene electrothermal actuator (ETA). The fabrication method is easy, fast, environmentally friendly, and suitable for preparing both large-size and miniature graphene ETAs. When applied with the driving voltage of 65 V, the graphene ETA achieves a large bending angle of 270° with a fast response of 8 s and the recovery process costs 19 s. The large bending deformation is reversible and can be precisely controlled by the driving voltage. A simple robotic hand prepared by using a single graphene ETA can hold the object, which is more than ten times the weight of itself. By virtue of its large-strain, fast response, and easy-to-manufacture, we believe that the graphene ETA has tremendous potential in extensive applications involving biomimetic robotics, artificial muscles, switches, and microsensors in both macroscopic and microscopic fields.

Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

International Nuclear Information System (INIS)

He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

2010-01-01

A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L -1 . The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

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%.

Design and Characterisation of Solid Electrolytes for All-Solid-State Lithium Batteries

DEFF Research Database (Denmark)

Sveinbjörnsson, Dadi Þorsteinn

The development of all-solid-state lithium batteries, in which the currently used liquid electrolytes are substituted for solid electrolyte materials, could lead to safer batteries offering higher energy densities and longer cycle lifetimes. Designing suitable solid electrolytes with sufficient...... chemical and electrochemical stability, high lithium ion conduction and negligible electronic conduction remains a challenge. The highly lithium ion conducting LiBH4-LiI solid solution is a promising solid electrolyte material. Solid solutions with a LiI content of 6.25%-50% were synthesised by planetary......-rich microstructures during ball milling is found to significantly influence the conductivity of the samples. The long-range diffusion of lithium ions was measured using quasi-elastic neutron scattering. The solid solutions are found to exhibit two-dimensional conduction in the hexagonal plane of the crystal structure...

A method of estimating hydrogen in solid and liquid samples by means of neutron thermalisation

International Nuclear Information System (INIS)

Carter, D.H.; Sanders, J.E.

1967-06-01

The count-rate of a cadmium-covered Pu239 fission chamber placed in a reactor neutron flux increases when a hydrogen-containing material is inserted due to the thermalisation of epicadmium neutrons. This effect forms the basis of a non-destructive method of estimating hydrogen in solid or liquid samples, and trial experiments to demonstrate the principles have been made. The sensitivity is such that hydrogen down to 10 p.p.m. in a typical metal should be detected. A useful feature of the method is its very low response to elements other than hydrogen. (author)

Microporous Carbon Spheres Solid Phase Membrane Tip Extraction for the Analysis of Nitrosamines in Water Samples

International Nuclear Information System (INIS)

Mohammed Salisu Musa; Wan Aini Wan Ibrahim

2015-01-01

A simple solid phase membrane tip extraction (SPMTE) utilizing microporous carbon spheres (MCS) was developed for the analysis of nitrosamines in aqueous samples. The method termed MCS-SPMTE was optimized for various important extraction parameters namely conditioning organic solvent, extraction time, effects of salt addition and pH change, desorption time, desorption solvent and sample volume. Under the optimized conditions, the method indicated good linearity in the range of 10-100 μg/ L with coefficients of determination, r 2 ≥0.9984. The method also demonstrated good reproducibility with % RSDs values ranging from 2.2 - 8.9 (n = 3). Limit of detection (LOD) and limit of quantification (LOQ) for the method ranged from 3.2 - 4.8 μg/ L and 10.9 - 15.9 μg/L respectively. Recoveries for both tap-water and lake water samples spiked at 10 μg/L were in the range of 83.2 - 107.5 %. (author)

Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

Science.gov (United States)

Krawczyk-Coda, Magdalena

2017-03-01

In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

Investigation of ceramic materials using ICP-AES with external electrothermal vaporization

International Nuclear Information System (INIS)

Reisch, M.; Gartz, R.; Mazurkiewicz, M.; Nickel, H.

1989-01-01

The evaporation and excitation processes for several trace elements in ceramic powders are studied. The advantages of an electrothermal vaporization are the easier preparation, no dilution and a shorter experiment duration. The investigated ceramic powders consist of synthetic mixtures including the systems Al 2 O 3 -SiO 2 and Al 2 O 3 -MgO. The trace elements are bound as oxides. The evaporation is monitored by 59 Fe and 115 Cd. Since the evaporation rates are measured in addition to line intensities, the influence of various parameters on evaporation as well as on excitation processes can be individually examined. The influence of matrix composition is determined. It is found that melting and sintering processes of the matrix are of great importance for the evaporation of trace elements. Thus the best results are obtained when trace elements evaporate below the melting temperature of the matrix. Therefore the addition of thermochemical substances is necessary for several elements of low volatility. In the case of highly volatile elements, for example Cd, additives seemed to have only a small influence on the volatilization rate. Accordingly, only the excitation is affected. For example, the evaporation rate of Cd is constant through the whole Al 2 O 3 -MgO system. The measured line intensity of Cd is also constant within a large range of MgO content. The evaporation rate and line intensity of Fe decrease linearly with MgO concentration. (author)

Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction

Energy Technology Data Exchange (ETDEWEB)

Jochmann, Maik A.; Schmidt, Torsten C. [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany); Chair of Instrumental Analysis, University Duisburg-Essen, Duisburg (Germany); Yuan, Xue [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany)

2007-03-15

In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-{mu}m film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons. (orig.)

Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction.

Science.gov (United States)

Jochmann, Maik A; Yuan, Xue; Schmidt, Torsten C

2007-03-01

In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-microm film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons.

Sampling and analytical procedures for the determination of VOCs released into air from natural and anthropogenic sources: A comparison between SPME (Solid Phase Micro Extraction) and ST (Solid Trap) methods

International Nuclear Information System (INIS)

Tassi, F.; Capecchiacci, F.; Buccianti, A.; Vaselli, O.

2012-01-01

In the present study, two sampling and analytical methods for VOC determination in fumarolic exhalations related to hydrothermal-magmatic reservoirs in volcanic and geothermal areas and biogas released from waste landfills were compared: (a) Solid Traps (STs), consisting of three phase (Carboxen B, Carboxen C and Carbosieve S111) absorbent stainless steel tubes and (b) Solid Phase Micro Extraction (SPME) fibers, composed of DiVinylBenzene (DVB), Carboxen and PolyDimethylSiloxane. These techniques were applied to pre-concentrate VOCs discharged from: (i) low-to-high temperature fumaroles collected at Vulcano Island, Phlegrean Fields (Italy), and Nisyros Island (Greece), (ii) recovery wells in a solid waste disposal site located near Florence (Italy). A glass condensing system cooled with water was used to collect the dry fraction of the fumarolic gases, in order to allow more efficient VOC absorption avoiding any interference by water vapor and acidic gases, such as SO 2 , H 2 S, HF and HCl, typically present at relatively high concentrations in these fluids. Up to 37 organic species, in the range of 40–400 m/z, were determined by coupling gas chromatography to mass spectrometry (GC–MS). This study shows that the VOC compositions of fumaroles and biogas determined via SPME and ST are largely consistent and can be applied to the analysis of VOCs in gases released from different natural and anthropogenic environments. The SPME method is rapid and simple and more appropriate for volcanic and geothermal emissions, where VOCs are present at relatively high concentrations and prolonged gas sampling may be hazardous for the operator. The ST method, allowing the collection of large quantities of sample, is to be preferred to analyze the VOC composition of fluids from diffuse emissions and air, where these compounds are present at relatively low concentrations.

Rapid and sensitive determination of radiocesium (Cs-135, Cs-137) in the presence of excess barium by electrothermal vaporization-inductively coupled plasma-mass spectrometry (ETV-ICP-MS) with potassium thiocyanate as modifier

International Nuclear Information System (INIS)

Song, M.; Probst, T.U.; Berryman, N.G.

2001-01-01

An electrothermal vaporization-inductively coupled plasma-mass spectrometric (ETV-ICP-MS) method based on selective volatilization of cesium with KSCN as modifier has been developed for determination of radiocesium, i.e. 135 Cs and 137 Cs, in the presence of isobaric barium. A 10000 times excess of barium, which was volatilized at a temperature of 1100 C, resulted only in a 1% signal increase in the signal of mass 135 amu. The recommended concentration of KSCN is 0.3 mM, and pretreatment and volatilization temperatures are 400 C and 1100 C, respectively. A ramp time of 1 s is recommended for the volatilization step. The achieved limit of detection for 135 Cs is 0.2 pg/mL (10 μBq/mL) and 4 fg (0.2 μBq) absolute for a sample volume of 20 μL. This means a limit of detection for 137 Cs of 0.2 pg/mL (0.6 Bq/mL) and of 4 fg (0.01 Bq) absolute. Signal variations of 135 Cs and 137 Cs, respectively, in spiked samples with various matrices were investigated. (orig.)

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Cabalin, L.M.; Gonzalez, A. [Department of Analytical Chemistry, University of Malaga, E-29071 Malaga (Spain); Ruiz, J. [Department of Applied Physics I, University of Malaga, E-29071 Malaga (Spain); Laserna, J.J., E-mail: laserna@uma.e [Department of Analytical Chemistry, University of Malaga, E-29071 Malaga (Spain)

2010-08-15

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s{sup -1}. Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

Science.gov (United States)

Cabalín, L. M.; González, A.; Ruiz, J.; Laserna, J. J.

2010-08-01

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s - 1 . Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Cabalin, L.M.; Gonzalez, A.; Ruiz, J.; Laserna, J.J.

2010-01-01

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s -1 . Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

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.

Study on an alternating current electrothermal micropump for microneedle-based fluid delivery systems

Science.gov (United States)

Zhang, Rumi; Jullien, Graham A.; Dalton, Colin

2013-07-01

In this paper, we report on a modeling study of an AC electrothermal (ACET) micropump with high operating pressures as well as fast flow rates. One specific application area is for fluid delivery using microneedle arrays which require higher pressures and faster flow rates than have been previously reported with ACET devices. ACET is very suitable for accurate actuation and control of fluid flow, since the technique has been shown to be very effective in high conductivity fluids and has the ability to create a pulsation free flow. However, AC electrokinetic pumps usually can only generate low operating pressures of 1 to 100 Pa, where flow reversal is likely to occur with an external load. In order to realize a high performance ACET micropump for continuous fluid delivery, applying relatively high AC operating voltages (20 to 36 Vrms) to silicon substrate ACET actuators and using long serpentine channel allows the boosting of operating pressure as well as increasing the flow rates. Fast pumping flow rates (102-103 nl/s) and high operating pressures (1-12 kPa) can be achieved by applying both methods, making them of significant importance for continuous fluid delivery applications using microneedle arrays and other such biomedical devices.

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.

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.

[Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

Science.gov (United States)

Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

2014-05-01

To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

Chemonucleolysis and intradiscal electrothermal therapy: What is the current evidence?

International Nuclear Information System (INIS)

Relder-Puig, Rosemarie; Gyimesi, M.; Mittermayr, T.; Geiger-Gritsch, S.

2009-01-01

We evaluated the efficacy and safety of chemonucleolysis and intradiscal electrothermal therapy (IDET) on the basis of the data presented in recently published papers with respect to pain relief, function, and complication rates. Detailed searches for English and German articles published between 2003 and 2008 were performed in a number of electronic databases. Further publications were identified by manual search. For summarizing the evidence, we considered only systematic reviews and controlled studies. The internal validity of reviews and studies was judged by two authors independently. Data extraction was performed by one author, and the extracted data was checked for completeness and correctness by a second author. The evidence of the efficacy of chemonucleolysis using chymopapain or collagenase is summarized in two recent, high-quality systematic reviews. We found 5 controlled studies evaluating nucleolysis using an oxygen-ozone mixture (O 2 O 3 -nucleolysis). Some of those studies were of limited methodological quality, but all showed the efficacy of O 2 O 3 -nucleolysis in comparison to microdiscectomy or the use of alternative substances. There is hardly any data regarding O 2 O 3 -nucleolysis complications. Regarding IDET, the authors of the 6 identified systematic reviews come to different conclusions about the efficacy of the procedure. The results of the 3 included controlled IDET studies, of which 2 are of high methodological quality, are also conflicting. The complication rates range from 0 to 15%. In summary, the evidence of efficacy is presently more compelling for chemonucleolysis than for IDET. This may also be because indications for chemonucleolysis are more firmly established. However, safety aspects should be better evaluated and presented in the literature. (orig.)

Simultaneous Determination of TetracyclinesResidues in Bovine Milk Samples by Solid Phase Extraction and HPLC-FL Method

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Mehra Mesgari Abbasi

2011-06-01

Full Text Available Introduction:Tetracyclines (TCs are widely used in animal husbandry and their residues in milk may resultinharmful effects on human. The aim of this study was to investigate the presence of TCs residues in various bovine milk samples from local markets of Ardabil, Iran. Methods:One hundred and fourteen pasteurized, sterilized and raw milk samples were collected from markets of Ardabil. Tetracycline, Oxytetracycline and Chlortetracycline (TCs residues extraction carried out by Solid Phase Extraction method. Determination of TCs residues were performed by high performance liquid chromatography (HPLC method using Fluorescence detector.Results: The mean of total TCs residues in all samples (114 samples was 97.6 ±16.9ng/g and that of pasteurized, sterilized and raw milk samples were 87.1 ± 17.7, 112.0 ± 57.3 and 154.0 ± 66.3ng/g respectively. Twenty five point four percent of the all samples, and24.4%, 30% and 28.6% of the pasteurized, sterilized and raw milk samples, respectively had higher TCs residues than the recommended maximum levels (100ng/g. Conclusion:This study indicates the presence of tetracycline residues more than allowed amount. Regulatory authorities should ensure proper withdrawal period before milking the animals and definite supervisions are necessary on application of these drugs.

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

WIPP Sampling and Analysis Plan for Solid Waste Management Units and Areas of Concern

International Nuclear Information System (INIS)

2000-01-01

This Sampling and Analysis Plan (SAP) has been prepared to fulfill requirements of Module VII, Section VII.M.2 and Table VII.1, requirement 4 of the Waste Isolation Pilot Plant (WIPP) Hazardous Waste Permit, NM4890139088-TSDF (the Permit); (NMED [New Mexico Environment Department], 1999a). This SAP describes the approach for investigation of the Solid Waste Management Units (SWMU) and Areas of Concern (AOC) specified in the Permit. This SAP addresses the current Permit requirements for a RCRA Facility Investigation(RFI) investigation of SWMUs and AOCs. It uses the results of previous investigations performed at WIPP and expands the investigations as required by the Permit. As an alternative to the RFI specified in Module VII of the Permit, current NMED guidance identifies an Accelerated Corrective Action Approach (ACAA) that may be used for any SWMU or AOC (NMED, 1998). This accelerated approach is used to replace the standard RFI work plan and report sequence with a more flexible decision-making approach. The ACAA process allows a facility to exit the schedule of compliance contained in the facility's Hazardous and Solid Waste Amendments (HSWA) permit module and proceed on an accelerated time frame. Thus, the ACAA process can beentered either before or after a RFI work plan. According to NMED's guidance, a facility can prepare a RFI work plan or SAP for any SWMU or AOC (NMED, 1998).

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.

Solid-Phase Extraction and Large-Volume Sample Stacking-Capillary Electrophoresis for Determination of Tetracycline Residues in Milk

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Gabriela Islas

2018-01-01

Full Text Available Solid-phase extraction in combination with large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE was applied to measure chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples. Under optimal conditions, the proposed method had a linear range of 29 to 200 µg·L−1, with limits of detection ranging from 18.6 to 23.8 µg·L−1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation in all cases. The enrichment factors obtained were from 50.33 to 70.85 for all the TCs compared with a conventional capillary zone electrophoresis (CZE. This method is adequate to analyze tetracyclines below the most restrictive established maximum residue limits. The proposed method was employed in the analysis of 15 milk samples from different brands. Two of the tested samples were positive for the presence of oxytetracycline with concentrations of 95 and 126 µg·L−1. SPE-LVSS-CE is a robust, easy, and efficient strategy for online preconcentration of tetracycline residues in complex matrices.

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.

Multiplexed Colorimetric Solid-Phase Extraction

Science.gov (United States)

Gazda, Daniel B.; Fritz, James S.; Porter, Marc D.

2009-01-01

Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

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

A solid phase extraction-ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples.

Science.gov (United States)

Olkowska, Ewa; Polkowska, Żaneta; Namieśnik, Jacek

2013-11-15

A new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE-for sample preparation) coupled with ion chromatography-conductivity detection (IC-CD-for the final determination). Mean recoveries of analytes between 79% and 93%, and overall method quantification limits in the range from 0.0018 to 0.038 μg/mL for surface water and CRM samples were achieved. The methodology was applied to the determination of individual alkyl benzyl quaternary ammonium compounds in environmental samples (reservoir water) and enables their presence in such types of waters to be confirmed. In addition, it is a simpler, less time-consuming, labour-intensive, avoiding use of toxic chloroform and significantly less expensive methodology than previously described approaches (liquid-liquid extraction coupled with liquid chromatography-mass spectrometry). Copyright © 2013 Elsevier B.V. All rights reserved.

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...

Micelle assisted thin-film solid phase microextraction: a new approach for determination of quaternary ammonium compounds in environmental samples.

Science.gov (United States)

Boyacı, Ezel; Pawliszyn, Janusz

2014-09-16

Determination of quaternary ammonium compounds (QACs) often is considered to be a challenging undertaking owing to secondary interactions of the analytes' permanently charged quaternary ammonium head or hydrophobic tail with the utilized labware. Here, for the first time, a micelle assisted thin-film solid phase microextraction (TF-SPME) using a zwitterionic detergent 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate (CHAPS) as a matrix modifier is introduced as a novel approach for in-laboratory sample preparation of the challenging compounds. The proposed micelle assisted TF-SPME method offers suppression/enhancement free electrospray ionization of analytes in mass spectrometric detection, minimal interaction of the micelles with the TF-SPME coating, and chromatographic stationary phase and analysis free of secondary interactions. Moreover, it was found that the matrix modifier has multiple functions; when its concentration is found below the critical micelle concentration (CMC), the matrix modifier primarily acts as a surface deactivator; above its CMC, it acts as a stabilizer for QACs. Additionally, shorter equilibrium extraction times in the presence of the modifier demonstrated that micelles also assist in the transfer of analytes from the bulk of the sample to the surface of the coating. The developed micelle assisted TF-SPME protocol using the 96-blade system requires only 30 min of extraction and 15 min of desorption. Together with a conditioning step (15 min), the entire method is 60 min; considering the advantage of using the 96-blade system, if all the blades in the brush are used, the sample preparation time per sample is 0.63 min. Moreover, the recoveries for all analytes with the developed method were found to range within 80.2-97.3%; as such, this method can be considered an open bed solid phase extraction. The proposed method was successfully validated using real samples.

Pocket rocket: An electrothermal plasma micro-thruster

Science.gov (United States)

Greig, Amelia Diane

Recently, an increase in use of micro-satellites constructed from commercial off the shelf (COTS) components has developed, to address the large costs associated with designing, testing and launching satellites. One particular type of micro-satellite of interest are CubeSats, which are modular 10 cm cubic satellites with total weight less than 1.33 kg. To assist with orbit boosting and attitude control of CubeSats, micro-propulsion systems are required, but are currently limited. A potential electrothermal plasma micro-thruster for use with CubeSats or other micro-satellites is under development at The Australian National University and forms the basis for this work. The thruster, known as ‘Pocket Rocket’, utilises neutral gas heating from ion-neutral collisions within a weakly ionised asymmetric plasma discharge, increasing the exhaust thermal velocity of the propellant gas, thereby producing higher thrust than if the propellant was emitted cold. In this work, neutral gas temperature of the Pocket Rocket discharge is studied in depth using rovibrational spectroscopy of the nitrogen (N2) second positive system (C3Πu → B3Πg), using both pure N2 and argon/N2 mixtures as the operating gas. Volume averaged steady state gas temperatures are measured for a range of operating conditions, with an analytical collisional model developed to verify experimental results. Results show that neutral gas heating is occurring with volume averaged steady state temperatures reaching 430 K in N2 and 1060 K for argon with 1% N2 at standard operating conditions of 1.5 Torr pressure and 10 W power input, demonstrating proof of concept for the Pocket Rocket thruster. Spatiotemporal profiles of gas temperature identify that the dominant heating mechanisms are ion-neutral collisions within the discharge and wall heating from ion bombardment of the thruster walls. To complement the experimental results, computational fluid dynamics (CFD) simulations using the commercial CFD

AW-101 entrained solids - Solubility versus temperature

International Nuclear Information System (INIS)

GJ Lumetta; RC Lettau; GF Piepel

2000-01-01

This report describes the results of a test conducted by Battelle to assess the solubility of the solids entrained in the diluted AW-101 low-activity waste (LAW) sample. BNFL requested Battelle to dilute the AW-1-1 sample using de-ionized water to mimic expected plant operating conditions. BNFL further requested Battelle to assess the solubility of the solids present in the diluted AW-101 sample versus temperature conditions of 30, 40, and 50 C. BNFL requested these tests to assess the composition of the LAW supernatant and solids versus expected plant-operating conditions. The work was conducted according to test plan BNFL-TP-29953-7, Rev. 0, Determination of the Solubility of LAW Entrained Solids. The test went according to plan, with no deviations from the test plan

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

A Headspace Solid Phase Microextraction (HS-SPME method for the chromatographic determination of alkylpyrazines in cocoa samples