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

Energy Technology Data Exchange (ETDEWEB)

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

2013-01-01

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

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

International Nuclear Information System (INIS)

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

1997-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-03-15

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

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

International Nuclear Information System (INIS)

Jiang Xianjuan; Gan Wuer; Han Suping; He Youzhao

2008-01-01

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

Achieving 100% Efficient Postcolumn Hydride Generation for As Speciation Analysis by Atomic Fluorescence Spectrometry.

Science.gov (United States)

Marschner, Karel; Musil, Stanislav; Dědina, Jiří

2016-04-05

An experimental setup consisting of a flow injection hydride generator coupled to an atomic fluorescence spectrometer was optimized in order to generate arsanes from tri- and pentavalent inorganic arsenic species (iAs(III), iAs(V)), monomethylarsonic acid (MAs(V)), and dimethylarsinic acid (DMAs(V)) with 100% efficiency with the use of only HCl and NaBH4 as the reagents. The optimal concentration of HCl was 2 mol L(-1); the optimal concentration of NaBH4 was 2.5% (m/v), and the volume of the reaction coil was 8.9 mL. To prevent excessive signal noise due to fluctuations of hydride supply to an atomizer, a new design of a gas-liquid separator was implemented. The optimized experimental setup was subsequently interfaced to HPLC and employed for speciation analysis of arsenic. Two chromatography columns were tested: (i) ion-pair chromatography and (ii) ion exchange chromatography. The latter offered much better results for human urine samples without a need for sample dilution. Due to the equal hydride generation efficiency (and thus the sensitivities) of all As species, a single species standardization by DMAs(V) standard was feasible. The limits of detection for iAs(III), iAs(V), MAs(V), and DMAs(V) were 40, 97, 57, and 55 pg mL(-1), respectively. Accuracy of the method was tested by the analysis of the standard reference material (human urine NIST 2669), and the method was also verified by the comparative analyses of human urine samples collected from five individuals with an independent reference method.

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

International Nuclear Information System (INIS)

Bye, R.

1986-01-01

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

Arsenic fractionation in agricultural soil using an automated three-step sequential extraction method coupled to hydride generation-atomic fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Rosas-Castor, J.M. [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico); Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Portugal, L.; Ferrer, L. [Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Guzmán-Mar, J.L.; Hernández-Ramírez, A. [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico); Cerdà, V. [Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Hinojosa-Reyes, L., E-mail: laura.hinojosary@uanl.edu.mx [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico)

2015-05-18

Highlights: • A fully automated flow-based modified-BCR extraction method was developed to evaluate the extractable As of soil. • The MSFIA–HG-AFS system included an UV photo-oxidation step for organic species degradation. • The accuracy and precision of the proposed method were found satisfactory. • The time analysis can be reduced up to eight times by using the proposed flow-based BCR method. • The labile As (F1 + F2) was <50% of total As in soil samples from As-contaminated-mining zones. - Abstract: A fully automated modified three-step BCR flow-through sequential extraction method was developed for the fractionation of the arsenic (As) content from agricultural soil based on a multi-syringe flow injection analysis (MSFIA) system coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS). Critical parameters that affect the performance of the automated system were optimized by exploiting a multivariate approach using a Doehlert design. The validation of the flow-based modified-BCR method was carried out by comparison with the conventional BCR method. Thus, the total As content was determined in the following three fractions: fraction 1 (F1), the acid-soluble or interchangeable fraction; fraction 2 (F2), the reducible fraction; and fraction 3 (F3), the oxidizable fraction. The limits of detection (LOD) were 4.0, 3.4, and 23.6 μg L{sup −1} for F1, F2, and F3, respectively. A wide working concentration range was obtained for the analysis of each fraction, i.e., 0.013–0.800, 0.011–0.900 and 0.079–1.400 mg L{sup −1} for F1, F2, and F3, respectively. The precision of the automated MSFIA–HG-AFS system, expressed as the relative standard deviation (RSD), was evaluated for a 200 μg L{sup −1} As standard solution, and RSD values between 5 and 8% were achieved for the three BCR fractions. The new modified three-step BCR flow-based sequential extraction method was satisfactorily applied for arsenic fractionation in real agricultural

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-02-15

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

Automated system for on-line determination of dimethylarsinic and inorganic arsenic by hydride generation-atomic fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Chaparro, L.L.; Leal, L.O. [Renewable Energy and Environmental Protection Department, Advanced Materials Research Center (CIMAV), Chihuahua, Chihuahua (Mexico); Ferrer, L.; Cerda, V. [University of the Balearic Islands, Department of Chemistry, Palma de Mallorca (Spain)

2012-09-15

A multisyringe flow-injection approach has been coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS) with UV photo-oxidation for dimethylarsinic (DMA), inorganic As and total As determination, depending on the pre-treatment given to the sample (extraction or digestion). The implementation of a UV lamp allows on-line photo-oxidation of DMA and the following arsenic detection, whereas a bypass leads the flow directly to the HG-AFS system, performing inorganic arsenic determination. DMA concentration is calculated by the difference of total inorganic arsenic and measurement of the photo-oxidation step. The detection limits for DMA and inorganic arsenic were 0.09 and 0.47 {mu}g L{sup -1}, respectively. The repeatability values accomplished were of 2.4 and 1.8 %, whereas the injection frequencies were 24 and 28 injections per hour for DMA and inorganic arsenic, respectively. This method was validated by means of a solid reference material BCR-627 (muscle of tuna) with good agreement with the certified values. Satisfactory results for DMA and inorganic arsenic determination were obtained in several water matrices. The proposed method offers several advantages, such as increasing the sampling frequency, low detection limits and decreasing reagents and sample consumption, which leads to lower waste generation. (orig.)

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

International Nuclear Information System (INIS)

Marschner, Karel; Musil, Stanislav; Dědina, Jiří

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-07-01

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

Determination of total inorganic arsenic in potable water through spectroscopy of atomic absorption with generation of hydride

International Nuclear Information System (INIS)

Rodriguez Roman, S.

1997-01-01

This study developed a method for the cuantitative analysis of arsenic in potable water , through the spectrophotometric technique of atomic absorption. It used an automatic system of injection of flux for the generation of hydrides. It studied the effect produced by reducer agents, in the prereduction of arsenic in water, obtaining the best result with the use of potasium iodide 1.5% and ascorbic acid 0.25% in hydrochloric acid 3.7%, for the direct determination of total inorganic arsenic. It observed the effect produced by cadmium and selenium to the half of the concentration of arsenic, chromium, lead and silver at the same concentration, and barium at a ten times higher concentration, in the recuperation of total inorganic arsenic. It also used sodium borohydride 0.3% in sodium hydroxide 0.05% (5mL/min), for the formation of the volatile hydrides. It used hydrochloric acid 3.7% (12 mL/min) as disolution of transport; argon as inert gas, and a flame air-acetylene, for the atomization of the hydrides. This method was applied to 19 samples of potable water, and the result was no detectable for all of them. (S. Grainger)

An improved method for the determination of trace levels of arsenic and antimony in geological materials by automated hydride generation-atomic absorption spectroscopy

Science.gov (United States)

Crock, J.G.; Lichte, F.E.

1982-01-01

An improved, automated method for the determination of arsenic and antimony in geological materials is described. After digestion of the material in sulfuric, nitric, hydrofluoric and perchloric acids, a hydrochloric acid solution of the sample is automatically mixed with reducing agents, acidified with additional hydrochloric acid, and treated with a sodium tetrahydroborate solution to form arsine and stibine. The hydrides are decomposed in a heated quartz tube in the optical path of an atomic absorption spectrometer. The absorbance peak height for arsenic or antimony is measured. Interferences that exist are minimized to the point where most geological materials including coals, soils, coal ashes, rocks and sediments can be analyzed directly without use of standard additions. The relative standard deviation of the digestion and the instrumental procedure is less than 2% at the 50 ??g l-1 As or Sb level. The reagent-blank detection limit is 0.2 ??g l-1 As or Sb. ?? 1982.

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

Czech Academy of Sciences Publication Activity Database

D'Ulivo, A.; Dědina, Jiří

2002-01-01

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

Trapping interference effects of arsenic, antimony and bismuth hydrides in collection of selenium hydride within iridium-modified transversally-heated graphite tube atomizer

Energy Technology Data Exchange (ETDEWEB)

Furdikova, Zuzana [Department of Environmental Chemistry and Technology, Faculty of Chemistry, Brno University of Technology, Purkynova 118, CZ-61200 Brno (Czech Republic); Institute of Analytical Chemistry of the Academy of Sciences of the Czech Republic v.v.i., Veveri 97, CZ-60200, Brno (Czech Republic); Docekal, Bohumil [Institute of Analytical Chemistry of the Academy of Sciences of the Czech Republic v.v.i., Veveri 97, CZ-60200, Brno (Czech Republic)], E-mail: docekal@iach.cz

2009-04-15

Interference effects of co-generated hydrides of arsenic, antimony and bismuth on trapping behavior of selenium hydride (analyte) within an iridium-modified, transversely heated graphite tube atomizer (THGA) were investigated. A twin-channel hydride generation system was used for independent separate generation and introduction of analyte and interferent hydrides, i.e. in a simultaneous and/or sequential analyte-interferent and interferent-analyte mode of operation. The influence of the analyte and modifier mass, interferent amount, trapping temperature and composition of the gaseous phase was studied. A simple approach for the elimination of mutual interference effects by modification of the gaseous phase with oxygen in a substoichiometric ratio to chemically generated hydrogen is proposed and the suppression of these interference effects is demonstrated. A hypothesis on the mechanism of trapping and mutual interference effects is drawn.

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

Energy Technology Data Exchange (ETDEWEB)

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

2003-07-01

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

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

International Nuclear Information System (INIS)

D'Ulivo, Alessandro; Dedina, Jiri

2002-01-01

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

Dielectric barrier discharge plasma atomizer for hydride generation atomic absorption spectrometry—Performance evaluation for selenium

Energy Technology Data Exchange (ETDEWEB)

Duben, Ondřej [Institute of Analytical Chemistry of the CAS, v.v.i., Veveří 97, CZ-602 00 Brno (Czech Republic); Faculty of Science, Department of Analytical Chemistry, Charles University in Prague, Hlavova 8, Prague, CZ 128 43 Czech Republic (Czech Republic); Boušek, Jaroslav [Faculty of Electrical Engineering and Communications, Brno University of Technology, Technická 1058/10, 61600 Brno (Czech Republic); Dědina, Jiří [Institute of Analytical Chemistry of the CAS, v.v.i., Veveří 97, CZ-602 00 Brno (Czech Republic); Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz [Institute of Analytical Chemistry of the CAS, v.v.i., Veveří 97, CZ-602 00 Brno (Czech Republic)

2015-09-01

Atomization of selenium hydride in a quartz dielectric barrier discharge (DBD) atomizer was optimized and its performance was compared to that of the externally heated quartz multiatomizer. Argon was found as the best DBD discharge gas employing a flow rate of 75 ml min{sup −1} Ar while the DBD power was optimized at 14 W. The detection limits reached 0.24 ng ml{sup −1} Se in the DBD and 0.15 ng ml{sup −1} Se in the multiatomizer. The tolerance of DBD to interferences is even better than with the multiatomizer. - Highlights: • SeH{sub 2} atomization in a dielectric barrier discharge (DBD) was optimized for AAS. • Atomizer performance was compared for DBD and externally heated quartz atomizer. • Detection limits were quantified and interferences were studied in both atomizers. • Atomization efficiency in the DBD was estimated.

Evaluation of a hydride generation-atomic fluorescence system for the determination of arsenic using a dielectric barrier discharge atomizer

International Nuclear Information System (INIS)

Zhu Zhenli; Liu Jixin; Zhang Sichun; Na Xing; Zhang Xinrong

2008-01-01

A new atomizer based on atmospheric pressure dielectric barrier discharge (DBD) plasma was specially designed for atomic fluorescence spectrometry (AFS) in order to be applied to the measurement of arsenic. The characteristics of the DBD atomizer and the effects of different parameters (power, discharge gas, gas flow rate, and KBH 4 concentration) were discussed in the paper. The DBD atomizer shows the following features: (1) low operation temperature (between 44 and 70 deg. C, depending on the operation conditions); (2) low power consumption; (3) operation at atmospheric pressure. The detection limit of As(III) using hydride generation (HG) with the proposed DBD-AFS was 0.04 μg L -1 . The analytical results obtained by the present method for total arsenic in reference materials, orchard leaves (SRM 1571) and water samples GBW(E) 080390, agree well with the certified values. The present HG-DBD-AFS is more sensitive and reliable for the determination of arsenic. It is a very promising technique allowing for field arsenic analysis based on atomic spectrometry

Mechanism of selenium hydride atomization, fate of free atoms and temperature distribution in an argon shielded, highly fuel-rich, hydrogen-oxygen diffusion micro-flame studied by atomic absorption spectrometry

Czech Academy of Sciences Publication Activity Database

D'Ulivo, A.; Dědina, Jiří; Lampugnani, L.; Matoušek, Tomáš

2002-01-01

Roč. 17, č. 3 (2002), s. 253-257 ISSN 0267-9477 R&D Projects: GA ČR GA203/01/0453; GA ČR GA203/98/0754 Institutional research plan: CEZ:AV0Z4031919 Keywords : hydride atomization * hydride generation * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.250, year: 2002

Electrochemical hydride generation atomic fluorescence spectrometry for detection of tin in canned foods using polyaniline-modified lead cathode

Energy Technology Data Exchange (ETDEWEB)

Jiang Xianjuan [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Gan Wuer, E-mail: wgan@ustc.edu.cn [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Wan Lingzhong; Deng Yun; Yang Qinghua; He Youzhao [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China)

2010-12-15

An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH{sub 4} and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL{sup -1} (3{sigma}) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL{sup -1} Sn(IV) standard solution.

Determination of bismuth by dielectric barrier discharge atomic absorption spectrometry coupled with hydride generation: Method optimization and evaluation of analytical performance

Czech Academy of Sciences Publication Activity Database

Kratzer, Jan; Boušek, J.; Sturgeon, R. E.; Mester, Z.; Dědina, Jiří

2014-01-01

Roč. 86, č. 19 (2014), s. 9620-9625 ISSN 0003-2700 Grant - others:GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

Electrochemical hydride generation atomic fluorescence spectrometry for detection of tin in canned foods using polyaniline-modified lead cathode.

Science.gov (United States)

Jiang, Xianjuan; Gan, Wuer; Wan, Lingzhong; Deng, Yun; Yang, Qinghua; He, Youzhao

2010-12-15

An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH(4) and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL(-1) (3σ) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL(-1) Sn(IV) standard solution. Copyright © 2010 Elsevier B.V. All rights reserved.

Modular L-design of hydride atomizers for atomic absorption spectrometry

International Nuclear Information System (INIS)

Rezacova, Olga; Dedina, Jiri

2009-01-01

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

[Research on optimization of mathematical model of flow injection-hydride generation-atomic fluorescence spectrometry].

Science.gov (United States)

Cui, Jian; Zhao, Xue-Hong; Wang, Yan; Xiao, Ya-Bing; Jiang, Xue-Hui; Dai, Li

2014-01-01

Flow injection-hydride generation-atomic fluorescence spectrometry was a widely used method in the industries of health, environmental, geological and metallurgical fields for the merit of high sensitivity, wide measurement range and fast analytical speed. However, optimization of this method was too difficult as there exist so many parameters affecting the sensitivity and broadening. Generally, the optimal conditions were sought through several experiments. The present paper proposed a mathematical model between the parameters and sensitivity/broadening coefficients using the law of conservation of mass according to the characteristics of hydride chemical reaction and the composition of the system, which was proved to be accurate as comparing the theoretical simulation and experimental results through the test of arsanilic acid standard solution. Finally, this paper has put a relation map between the parameters and sensitivity/broadening coefficients, and summarized that GLS volume, carrier solution flow rate and sample loop volume were the most factors affecting sensitivity and broadening coefficients. Optimizing these three factors with this relation map, the relative sensitivity was advanced by 2.9 times and relative broadening was reduced by 0.76 times. This model can provide a theoretical guidance for the optimization of the experimental conditions.

Localization of volatile isotopes on a cryotrap

International Nuclear Information System (INIS)

Thirolf, P.G.; Gross, M.; Habs, D.; Kohlhund, A.; Nebel, F.; Neumayr, J.B.; Stoepler, R.; Szerypo, J.

2008-01-01

Neutron-induced fission of uranium allows for the production of high-intensity neutron-rich radioactive ion beams. However, also large quantities of unwanted volatile radioactive species are produced that have to be hindered from contaminating the beamline and vacuum system of the facility. In the framework of radioprotection studies within the MAFF project at the FRM II in Garching with 10 14 fission events/s [D. Habs et al., The Munich accelerator for fission fragments MAFF, Nucl. Instr. and Meth. B 204 (2003) 739], the performance of a cryotrap system has been studied, designed to localize gaseous radioactivity close to its origin. These studies provide important radioprotection information for the planned EURISOL facility with 10 15 fission events/s. Design considerations of a compact cryotrap operated with cold helium gas at a saturation temperature around 18 K will be presented. Activity distribution calculations of the fission source, the cryotrap and the subsequent vacuum system result in a prediction of the retention capability of the cryotrap system of 99.98%. These design calculations have been experimentally verified with three cryotrap prototypes differing in cold surface area as well as in their internal helium gas flow characteristics. Retention capabilities have been measured with and without passive shielding of the external thermal load (300 K) using different tracer gases and an inclusive pressure-related diagnostics as well as mass-spectroscopic measurements.

Atom Probe Analysis of Ex Situ Gas-Charged Stable Hydrides.

Science.gov (United States)

Haley, Daniel; Bagot, Paul A J; Moody, Michael P

2017-04-01

In this work, we report on the atom probe tomography analysis of two metallic hydrides formed by pressurized charging using an ex situ hydrogen charging cell, in the pressure range of 200-500 kPa (2-5 bar). Specifically we report on the deuterium charging of Pd/Rh and V systems. Using this ex situ system, we demonstrate the successful loading and subsequent atom probe analysis of deuterium within a Pd/Rh alloy, and demonstrate that deuterium is likely present within the oxide-metal interface of a native oxide formed on vanadium. Through these experiments, we demonstrate the feasibility of ex situ hydrogen analysis for hydrides via atom probe tomography, and thus a practical route to three-dimensional imaging of hydrogen in hydrides at the atomic scale.

Modular L-design of hydride atomizers for atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

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

2009-07-15

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

Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

Energy Technology Data Exchange (ETDEWEB)

Karadjova, Irina B. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria); Lampugnani, Leonardo [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy)]. E-mail: lampugnani@ipcf.cnr.it; Onor, Massimo [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy); D' Ulivo, Alessandro [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy); Tsalev, Dimiter L. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria)

2005-07-15

Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 {mu}g l{sup -1} As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 {mu}g l{sup -1}. Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l{sup -1} acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l{sup -1} HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 {mu}g l{sup -1} for As(III) and 0.3 {mu}g l{sup -1} for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 {mu}g l{sup -1} (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non

Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

International Nuclear Information System (INIS)

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

2005-01-01

Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 μg l -1 As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 μg l -1 . Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l -1 acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l -1 HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 μg l -1 for As(III) and 0.3 μg l -1 for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 μg l -1 (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non-chromatographic and chromatographic procedures and the As

Nanostructured, complex hydride systems for hydrogen generation

Directory of Open Access Journals (Sweden)

Robert A. Varin

2015-02-01

Full Text Available Complex hydride systems for hydrogen (H2 generation for supplying fuel cells are being reviewed. In the first group, the hydride systems that are capable of generating H2 through a mechanical dehydrogenation phenomenon at the ambient temperature are discussed. There are few quite diverse systems in this group such as lithium alanate (LiAlH4 with the following additives: nanoiron (n-Fe, lithium amide (LiNH2 (a hydride/hydride system and manganese chloride MnCl2 (a hydride/halide system. Another hydride/hydride system consists of lithium amide (LiNH2 and magnesium hydride (MgH2, and finally, there is a LiBH4-FeCl2 (hydride/halide system. These hydride systems are capable of releasing from ~4 to 7 wt.% H2 at the ambient temperature during a reasonably short duration of ball milling. The second group encompasses systems that generate H2 at slightly elevated temperature (up to 100 °C. In this group lithium alanate (LiAlH4 ball milled with the nano-Fe and nano-TiN/TiC/ZrC additives is a prominent system that can relatively quickly generate up to 7 wt.% H2 at 100 °C. The other hydride is manganese borohydride (Mn(BH42 obtained by mechano-chemical activation synthesis (MCAS. In a ball milled (2LiBH4 + MnCl2 nanocomposite, Mn(BH42 co-existing with LiCl can desorb ~4.5 wt.% H2 at 100 °C within a reasonable duration of dehydrogenation. Practical application aspects of hydride systems for H2 generation/storage are also briefly discussed.

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

Czech Academy of Sciences Publication Activity Database

Marschner, Karel; Musil, Stanislav; Dědina, Jiří

2015-01-01

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

Analysis of arsenical metabolites in biological samples.

Science.gov (United States)

Hernandez-Zavala, Araceli; Drobna, Zuzana; Styblo, Miroslav; Thomas, David J

2009-11-01

Quantitation of iAs and its methylated metabolites in biological samples provides dosimetric information needed to understand dose-response relations. Here, methods are described for separation of inorganic and mono-, di-, and trimethylated arsenicals by thin layer chromatography. This method has been extensively used to track the metabolism of the radionuclide [(73)As] in a variety of in vitro assay systems. In addition, a hydride generation-cryotrapping-gas chromatography-atomic absorption spectrometric method is described for the quantitation of arsenicals in biological samples. This method uses pH-selective hydride generation to differentiate among arsenicals containing trivalent or pentavalent arsenic.

Ultratrace determination of lead by hydride generation in-atomizer trapping atomic absorption spectrometry: Optimization of plumbane generation and analyte preconcentration in a quartz trap-and-atomizer device

Energy Technology Data Exchange (ETDEWEB)

Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz

2012-05-15

A compact trap-and-atomizer device and a preconcentration procedure based on hydride trapping in excess of oxygen over hydrogen in the collection step, both constructed and developed previously in our laboratory, were employed to optimize plumbane trapping in this device and to develop a routine method for ultratrace lead determination subsequently. The inherent advantage of this preconcentration approach is that 100% preconcentration efficiency for lead is reached in this device which has never been reported before using quartz or metal traps. Plumbane is completely retained in the trap-and-atomizer device at 290 Degree-Sign C in oxygen-rich atmosphere and trapped species are subsequently volatilized at 830 Degree-Sign C in hydrogen-rich atmosphere. Effect of relevant experimental parameters on plumbane trapping and lead volatilization are discussed, and possible trapping mechanisms are hypothesized. Plumbane trapping in the trap-and-atomizer device can be routinely used for lead determination at ultratrace levels reaching a detection limit of 0.21 ng ml{sup -1} Pb (30 s preconcentration, sample volume 2 ml). Further improvement of the detection limit is feasible by reducing the blank signal and increasing the trapping time. - Highlights: Black-Right-Pointing-Pointer In-atomizer trapping HG-AAS was optimized for Pb. Black-Right-Pointing-Pointer A compact quartz trap-and-atomizer device was employed. Black-Right-Pointing-Pointer Generation, preconcentration and atomization steps were investigated in detail. Black-Right-Pointing-Pointer 100% preconcentration efficiency for lead was reached. Black-Right-Pointing-Pointer Routine analytical method was developed for Pb determination (LOD of 0.2 ng ml{sup -1} Pb).

Determination of As(III) and As(V) by Flow Injection-Hydride Generation-Atomic Absorption Spectrometry via On-line Reduction of As(V) by KI

DEFF Research Database (Denmark)

Nielsen, Steffen; Hansen, Elo Harald

1997-01-01

A volume-based flow injection (FI) procedure is described for the determination and speciation of trace inorganic arsenic, As(III) and As(V), via hydride generation-atomic absorption spectrometry (HG-AAS) of As(III). The determination of total arsenic is obtained by on-line reduction of As(V) to As...

Hydride generation atomic fluorescence spectrometric determination of As, Bi, Sb, Se(IV) and Te(IV) in aqua regia extracts from atmospheric particulate matter using multivariate optimization

International Nuclear Information System (INIS)

Moscoso-Perez, Carmen; Moreda-Pineiro, Jorge; Lopez-Mahia, Purificacion; Muniategui-Lorenzo, Soledad; Fernandez-Fernandez, Esther; Prada-Rodriguez, Dario

2004-01-01

A highly sensitive and simple method, based on hydride generation and atomic fluorescence detection, has been developed for the determination of As, Bi, Sb, Se(IV) and Te(IV) in aqua regia extracts from atmospheric particulate matter samples. Atmospheric particulates matter was collected on glass fiber filters using a medium volume sampler (PM1 particulate matter). Two-level factorial designs have been used to optimise the hydride generation atomic fluorescence spectrometry (HG-AFS) procedure. The effects of several parameters affecting the hydride generation efficiency (hydrochloric acid, sodium tetrahydroborate and potassium iodide concentrations and flow rates) have been evaluated using a Plackett-Burman experimental design. In addition, parameters affecting the hydride measurement (delay, analysis and memory times) have been also investigated. The significant parameters obtained (sodium tetrahydroborate concentration, sodium tetrahydroborate flow rate and analysis time for As; hydrochloric acid concentration and sodium tetrahydroborate flow rate for Se(IV); and sodium tetrahydroborate concentration and sodium tetrahydroborate flow rate for Te(IV)) have been optimized by using 2 n + star central composite design. Hydrochloric acid concentration and sodium tetrahydroborate flow rate were the significant parameters obtained for Sb and Bi determination, respectively. Using a univariate approach these parameters were optimized. The accuracy of methods have been verified by using several certified reference materials: SRM 1648 (urban particulate matter) and SRM 1649a (urban dust). Detection limits in the range of 6 x 10 -3 to 0.2 ng m -3 have been achieved. The developed methods were applied to several atmospheric particulate matter samples corresponding to A Coruna city (NW Spain)

Speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Li Xun [Department of Chemistry, Beijing Normal University, Beijing 100875 (China); Department of Chemistry and Life Science, Gannan Teachers College, Ganzhou 341000 (China); Jia Jing [Department of Chemistry, Beijing Normal University, Beijing 100875 (China); Wang Zhenghao [Department of Chemistry, Beijing Normal University, Beijing 100875 (China)]. E-mail: zhwang@bnu.edu.cn

2006-02-23

A simple procedure was developed for the speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS), without pre-reduction of As(V). Glassy carbon was selected as cathode material in the flow cell. An optimum catholyte concentration for simultaneous generation of arsine from As(III) and As(V) was 0.06 mol l{sup -1} H{sub 2}SO{sub 4}. Under the optimized conditions, adequate sensitivity and difference in ratio of slopes of the calibration curves for As(III) and As(V) can be achieved at the electrolytic currents of 0.6 and 1 A. The speciation of inorganic arsenic can be performed by controlling the electrolytic currents, and the concentration of As(III) and As(V) in the sample can be calculated according to the equations of absorbance additivity obtained at two selected electrolytic currents. The calibration curves were linear up to 50 ng ml{sup -1} for both As(III) and As(V) at 0.6 and 1 A. The detection limits of the method were 0.2 and 0.5 ng ml{sup -1} for As(III) and As(V) at 0.6 A, respectively. The relative standard deviations were of 2.1% for 20 ng ml{sup -1} As(III) and 2.5% for 20 ng ml{sup -1} As(V). The method was validated by the analysis of human hair certified reference material and successfully applied to speciation of soluble inorganic arsenic in Chinese medicine.

Speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry

International Nuclear Information System (INIS)

Li Xun; Jia Jing; Wang Zhenghao

2006-01-01

A simple procedure was developed for the speciation of inorganic arsenic by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS), without pre-reduction of As(V). Glassy carbon was selected as cathode material in the flow cell. An optimum catholyte concentration for simultaneous generation of arsine from As(III) and As(V) was 0.06 mol l -1 H 2 SO 4 . Under the optimized conditions, adequate sensitivity and difference in ratio of slopes of the calibration curves for As(III) and As(V) can be achieved at the electrolytic currents of 0.6 and 1 A. The speciation of inorganic arsenic can be performed by controlling the electrolytic currents, and the concentration of As(III) and As(V) in the sample can be calculated according to the equations of absorbance additivity obtained at two selected electrolytic currents. The calibration curves were linear up to 50 ng ml -1 for both As(III) and As(V) at 0.6 and 1 A. The detection limits of the method were 0.2 and 0.5 ng ml -1 for As(III) and As(V) at 0.6 A, respectively. The relative standard deviations were of 2.1% for 20 ng ml -1 As(III) and 2.5% for 20 ng ml -1 As(V). The method was validated by the analysis of human hair certified reference material and successfully applied to speciation of soluble inorganic arsenic in Chinese medicine

Trace determination of antimony by hydride generation atomic absorption spectrometry with analyte preconcentration/atomization in a dielectric barrier discharge atomizer.

Science.gov (United States)

Zurynková, Pavla; Dědina, Jiří; Kratzer, Jan

2018-06-20

Atomization conditions for antimony hydride in the plasma atomizer based on a dielectric barrier discharge (DBD) with atomic absorption spectrometric detection were optimized. Argon was found as the best discharge gas under a flow rate of 50 mL min - 1 while the DBD power was optimum at 30 W. Analytical figures of merit including interference study of As, Se and Bi have been subsequently investigated and the results compared to those found in an externally heated quartz tube atomizer (QTA). The limit of detection (LOD) reached in DBD (0.15 ng mL -1  Sb) is comparable to that observed in QTA (0.14 ng mL -1  Sb). Finally, possibility of Sb preconcentration by stibane in situ trapping in a DBD atomizer was studied. For trapping time of 300 s, the preconcentration efficiency and LOD, respectively, were 103 ± 2% and 0.02 ng mL -1 . Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of antimony by electrochemical hydride generation atomic absorption spectrometry in samples with high iron content using chelating resins as on-line removal system

International Nuclear Information System (INIS)

Bolea, E.; Arroyo, D.; Laborda, F.; Castillo, J.R.

2006-01-01

A method for the removal of the interference caused by iron on electrochemical generation of stibine is proposed. It consists of a chelating resin Chelex 100 column integrated into a flow injection system and coupled to the electrochemical hydride generator quartz tube atomic absorption spectrometer (EcHG-QT-AAS). Iron, as Fe(II), is retained in the column with high efficiency, close to 99.9% under optimal conditions. No significant retention was observed for Sb(III) under same conditions and a 97 ± 5% signal recovery was achieved. An electrochemical hydride generator with a concentric configuration and a reticulated vitreous carbon cathode was employed. The system is able to determine antimony concentrations in the range of ng ml -1 in presence of iron concentrations up to 400 mg l -1 . The procedure was validated by analyzing PACS-2 marine sediments reference material with a 4% (w/w) iron content and a [Fe]:[Sb] ratio of 4000:1, which caused total antimony signal suppression on the electrochemical hydride generation system. A compost sample with high iron content (0.7%, w/w), was also analyzed. A good agreement was found on both samples with the certified value and the antimony concentration determined by ICP-MS, respectively

Antimony speciation analysis in sediment reference materials using high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry

International Nuclear Information System (INIS)

Potin-Gautier, M.; Pannier, F.; Quiroz, W.; Pinochet, H.; Gregori, I. de

2005-01-01

This work presents the development of suitable methodologies for determination of the speciation of antimony in sediment reference samples. Liquid chromatography with a post-column photo-oxidation step and hydride generation atomic fluorescence spectrometry as detection system is applied to the separation and determination of Sb(III), Sb(V) and trimethylantimony species. Post-column decomposition and hydride generation steps were studied for sensitive detection with the AFS detector. This method was applied to investigate the conditions under which speciation analysis of antimony in sediment samples can be carried out. Stability studies of Sb species during the extraction processes of solid matrices, using different reagents solutions, were performed. Results demonstrate that for the extraction yield and the stability of Sb species in different marine sediment extracts, citric acid in ascorbic acid medium was the best extracting solution for antimony speciation analysis in this matrix (between 55% and 65% of total Sb was recovered from CRMs, Sb(III) being the predominant species). The developed method allows the separation of the three compounds within 6 min with detection limits of 30 ng g -1 for Sb(III) and TMSbCl2 and 40 ng g -1 for Sb(V) in sediment samples

Determination of total antimony and inorganic antimony species by hydride generation in situ trapping flame atomic absorption spectrometry: a new way to (ultra)trace speciation analysis

Energy Technology Data Exchange (ETDEWEB)

Henryk Matusiewicz; Magdalena Krawczyk

2008-07-01

The analytical performance of non-chromatographic coupled hydride generation, integrated atom trap (HG-IAT) atomizer flame absorption spectrometry (FAAS) systems were evaluated for the speciation analysis of antimony in environmental samples. Antimony, using formation of stibine (SbH{sub 3}) vapors were atomized in an air-acetylene flame-heated IAT. A new design of HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements was investigated. For the estimation of Sb(III) and Sb(V) concentrations in samples, the difference between the analytical sensitivities of the absorbance signals obtained for antimony hydride without and with previous treatment of samples with L-cysteine can be used. The concentration of Sb(V) was calculated by the difference between total Sb and Sb(III). A dramatic improvement in detection limit was achieved compared with that obtained using either of the atom trapping techniques, presented above, separately. This novel approach decreases the detection limit down to low pg mL{sup -1} levels. The concentration detection limit, defined as 3 times the blank standard deviation was 0.2 ng mL{sup -1}. For a 120 s in situ pre-concentration time , sensitivity enhancement compared to flame AAS, was 550 fold for Sb, using hydride generation-atom trapping technique. The accuracy of the method was verified by the use of certified reference materials (NIST SRM 2704 Buffalo River Sediment, SRM 2710 Montana Soil, SRM 1633a Coal Fly Ash, SRM 1575 Pine Needles, SRM 1643e Trace Elements in Water) and by aqueous standard calibration technique. The measured Sb content, in reference materials, were in satisfactory agreement with the certified values. The hyphenated technique was applied for antimony determinations in soil, sediment, coal fly ash, sewage and river water.

On-line electrochemically controlled in-tube solid phase microextraction of inorganic selenium followed by hydride generation atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of); Shamsayei, Maryam; Safari, Meysam; Rezaei, Fatemeh [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

2016-05-30

In this work, for the first time, a rapid, simple and sensitive microextraction procedure is demonstrated for the matrix separation, preconcentration and determination of inorganic selenium species in water samples using an electrochemically controlled in-tube solid phase microextraction (EC-in-tube SPME) followed by hydride generation atomic absorption spectrometry (HG-AAS). In this approach, in which EC-in-tube SPME and HG-AAS system were combined, the total analysis time, was decreased and the accuracy, repeatability and sensitivity were increased. In addition, to increases extraction efficiency, a novel nanostructured composite coating consisting of polypyrrole (PPy) doped with ethyleneglycol dimethacrylate (EGDMA) was prepared on the inner surface of a stainless-steel tube by a facile electrodeposition method. To evaluate the offered setup and the new PPy-EGDMA coating, it was used to extract inorganic selenium species in water samples. Extraction of inorganic selenium species was carried out by applying a positive potential through the inner surface of coated in-tube under flow conditions. Under the optimized conditions, selenium was detected in amounts as small as 4.0 parts per trillion. The method showed good linearity in the range of 0.012–200 ng mL{sup −1}, with coefficients of determination better than 0.9996. The intra- and inter-assay precisions (RSD%, n = 5) were in the range of 2.0–2.5% and 2.7–3.2%, respectively. The validated method was successfully applied for the analysis of inorganic selenium species in some water samples and satisfactory results were obtained. - Graphical abstract: An electrochemically controlled in-tube solid phase microextraction followed by hydride generation atomic absorption spectrometry was developed for extraction and determination ultra-trace amounts of Se in aqueous solutions. - Highlights: • A nanostructured composite coating consisting of PPy doped with EGDMA was prepared. • The coating was

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

Science.gov (United States)

Çiftçi, Tülin Deniz; Henden, Emur

2016-08-01

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

A new hydride generator for the determination of volatile elements by atomic absorption spectrophotometry

International Nuclear Information System (INIS)

Kersabiec, A.M. de

1979-01-01

The production of hydrides in order to use them for analysis by atomic absorption spectrophotometry depends on many parameters. A new apparatus has been designed for this specific operation. It is characterized by a reaction chamber with variable size and by appliances for regulation and control of the physical conditions of operation. Properties are both methodological studies and utilization in large scale analysis. The entire description of the apparatus is completed by an analytical study [fr

Determination of total Sb,Se Te, and Bi and evaluation of their inorganic species in garlic by hydride-generation-atomic-fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Matos Reyes, M.N.; Cervera, M.L.; Guardia, M. de la [University of Valencia, Department of Analytical Chemistry, Burjassot, Valencia (Spain)

2009-07-15

A sensitive and simple analytical method has been developed for determination of Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), Te(VI), and Bi(III) in garlic samples by using hydride-generation-atomic-fluorescence spectrometry (HG-AFS). The method is based on a single extraction of the inorganic species by sonication at room temperature with 1 mol L{sup -1} H{sub 2}SO{sub 4} and washing of the solid phase with 0.1% (w/v) EDTA, followed by measurement of the corresponding hydrides generated under two different experimental conditions directly and after a pre-reduction step. The limit of detection of the method was 0.7 ng g{sup -1} for Sb(III), 1.0 ng g{sup -1} for Sb(V), 1.3 ng g{sup -1} for Se(IV), 1.0 ng g{sup -1} for Se(VI), 1.1 ng g{sup -1} for Te(IV), 0.5 ng g{sup -1} for Te(VI), and 0.9 ng g{sup -1} for Bi(III), in all cases expressed in terms of sample dry weight. (orig.)

Improved microwave-assisted wet digestion procedures for accurate Se determination in fish and shellfish by flow injection-hydride generation-atomic absorption spectrometry

International Nuclear Information System (INIS)

Lavilla, I.; Gonzalez-Costas, J.M.; Bendicho, C.

2007-01-01

Accurate determination of Se in biological samples, especially fish and shellfish, by hydride generation techniques has generally proven troublesome owing to the presence of organoselenium that cannot readily converted into inorganic selenium under usual oxidising conditions. Further improvements in the oxidation procedures are needed so as to obtain accurate concentration values when this type of samples is analyzed. Microwave-assisted wet digestion (MAWD) procedures of seafood based on HNO 3 or the mixture HNO 3 /H 2 O 2 and further thermal reduction of the Se(VI) formed to Se(IV) were evaluated. These procedures were as follows: (I) without H 2 O 2 and without heating to dryness; (II) without H 2 O 2 and with heating to dryness; (III) with H 2 O 2 and without heating to dryness; (IV) with H 2 O 2 and with heating to dryness. In general, low recoveries of selenium are obtained for several marine species (e.g., crustaceans and cephalopods), which may be ascribed to the presence of Se forms mainly associated with nonpolar proteins and lipids. Post-digestion UV irradiation proved very efficient since not only complete organoselenium decomposition was achieved but also the final step required for prereduction of Se(VI) into Se(IV) (i.e. heating at 90 deg. C for 30 min in 6 M HCl) could be avoided. With the MAWD/UV procedure, the use of strong oxidising agents (persuphate, etc.) or acids (e.g. perchloric acid) which are typically applied prior to Se determination by hydride generation techniques is overcome, and as a result, sample pre-treatment is significantly simplified. The method was successfully validated against CRM DOLT-2 (dogfish liver), CRM DORM-2 (dogfish muscle) and CRM TORT-2 (lobster hepatopancreas). Automated ultrasonic slurry sampling with electrothermal atomic absorption spectrometry was also applied for comparison. Total Se contents in ten seafood samples were established. Se levels ranged from 0.7 to 2.9 μg g -1

Achieving 100% efficient postcolumn hydride generation for As speciation analysis by atomic fluorescence spectrometry

Czech Academy of Sciences Publication Activity Database

Marschner, Karel; Musil, Stanislav; Dědina, Jiří

2016-01-01

Roč. 88, č. 7 (2016), s. 4041-4047 ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * HPLC Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 6.320, year: 2016

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 As in tobacco by using electrochemical hydride generation at a Nafion® solid polymer electrolyte cell hyphenated with atomic fluorescence spectrometry

Science.gov (United States)

Yang, Qinghua; Gan, Wuer; Deng, Yun; Sun, Huihui

2011-11-01

In the present work, a novel solid polymer electrolyte hydride generation (SPE-HG) cell was developed. The home-made SPE-HG cell, mainly composed of three components (Nafion®117 membrane for separating and H + exchanging, a soft graphite felt cathode and a Ti mesh modified by Ir anode), was employed for detecting As by coupling to atomic fluorescence spectrometry (AFS). The H + generated by electrolysis of pure water in anode chamber transferred to cathode chamber through SPE, and immediately reacted with As 3 + to generate AsH 3. The relative mechanisms and operation conditions for hydride generation of As were investigated in detail. The developed cell employed water as an alternative of acid anolyte, with virtues of low-cost, more than 6 months lifetime and environment friendly compared with the conventional cell. Under the optimized conditions, the limit of determination of As 3 + for sample blank solution was 0.12 μg L - 1 , the RSD was 2.9% for 10 consecutive measurements of 5 μg L - 1 As 3 + standard solution. The accuracy of the method was verified by the determination of As in the reference Tea (GBW07605) and the developed method was successfully applied to determine trace amounts of As in tobacco samples with recovery from 97% to 103%.

Sequential determination of arsenic, selenium, antimony, and tellurium in foods via rapid hydride evolution and atomic absorption spectrometry

International Nuclear Information System (INIS)

Fiorino, J.A.; Jones, J.W.; Capar, S.G.

1976-01-01

Analysis of acid digests of foods for As, Se, Sb, and Te was semiautomated. Hydrides generated by controlled addition of base stabilized NaBH 4 solution to acid digests are transported directly into a shielded, hydrogen (nitrogen diluted), entrained-air flame for atomic absorption spectrophotometric determination of the individual elements. The detection limits, based on 1 g of digested sample, are approximately 10 to 20 ng/g for all four elements. Measurement precision is 1 to 2 percent relative standard deviation for each element measured at 0.10 μg. A comparison is made of results of analysis of lyophilized fish tissues for As and Se by instrumental neutron activation (INAA), hydride generation with atomic absorption spectrometry, fluorometry, and spectrophotometry. NBS standard reference materials (orchard leaves and bovine liver) analyzed for As, Se, and Sb by this method show excellent agreement with certified values and with independent NAA values

Determination of arsenic species in seafood samples from the Aegean Sea by liquid chromatography-(photo-oxidation)-hydride generation-atomic fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Schaeffer, Richard [Department of Applied Chemistry, Corvinus University, Villanyi ut 29-35, 1118 Budapest (Hungary); Soeroes, Csilla [Department of Applied Chemistry, Corvinus University, Villanyi ut 29-35, 1118 Budapest (Hungary); Ipolyi, Ildiko [Department of Applied Chemistry, Corvinus University, Villanyi ut 29-35, 1118 Budapest (Hungary); Fodor, Peter [Department of Applied Chemistry, Corvinus University, Villanyi ut 29-35, 1118 Budapest (Hungary); Thomaidis, Nikolaos S. [Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistiomopolis Zografou, 15776 Athens (Greece)]. E-mail: ntho@chem.uoa.gr

2005-08-15

In this study arsenic compounds were determined in mussels (Mytulis galloprovincialis), anchovies (Engraulis encrasicholus), sea-breams (Sparus aurata), sea bass (Dicentrarchus labrax) and sardines (Sardina pilchardus) collected from Aegean Sea using liquid chromatography-photo-oxidation-hydride generation-atomic fluorescence spectrometry [LC-(PO)-HG-AFS] system. Twelve arsenicals were separated and determined on the basis of their difference in two properties: (i) the pK {sub a} values and (ii) hydride generation capacity. The separation was carried out both with an anion- and a cation-exchange column, with and without photo-oxidation. In all the samples arsenobetaine, AB was detected as the major compound (concentrations ranging between 2.7 and 23.1 {mu}g g{sup -1} dry weight), with trace amounts of arsenite, As(III), dimethylarsinic acid, DMA and arsenocholine, AC, also present. Arsenosugars were detected only in the mussel samples (in concentrations of 0.9-3.6 {mu}g g{sup -1} dry weight), along with the presence of an unknown compound, which, based on its retention time on the anion-exchange column Hamilton PRP-X100 and a recent communication [E. Schmeisser, R. Raml, K.A. Francesconi, D. Kuehnelt, A. Lindberg, Cs. Soeroes, W. Goessler, Chem. Commun. 16 (2004) 1824], is supposed to be a thio-arsenic analogue.

Determination of Inorganic Arsenic in a Wide Range of Food Matrices using Hydride Generation - Atomic Absorption Spectrometry.

Science.gov (United States)

de la Calle, Maria B; Devesa, Vicenta; Fiamegos, Yiannis; Vélez, Dinoraz

2017-09-01

The European Food Safety Authority (EFSA) underlined in its Scientific Opinion on Arsenic in Food that in order to support a sound exposure assessment to inorganic arsenic through diet, information about distribution of arsenic species in various food types must be generated. A method, previously validated in a collaborative trial, has been applied to determine inorganic arsenic in a wide variety of food matrices, covering grains, mushrooms and food of marine origin (31 samples in total). The method is based on detection by flow injection-hydride generation-atomic absorption spectrometry of the iAs selectively extracted into chloroform after digestion of the proteins with concentrated HCl. The method is characterized by a limit of quantification of 10 µg/kg dry weight, which allowed quantification of inorganic arsenic in a large amount of food matrices. Information is provided about performance scores given to results obtained with this method and which were reported by different laboratories in several proficiency tests. The percentage of satisfactory results obtained with the discussed method is higher than that of the results obtained with other analytical approaches.

The determination of arsenic, selenium, antimony, and tin in complex environmental samples by hydride generation AAS

International Nuclear Information System (INIS)

Johnson, D.; Beach, C.

1990-01-01

Hydride generation techniques are used routinely for the determination of As, Se, Sb and Sn in water samples. Advantages include high sensitivity, simplicity, and relative freedom from interferences. Continuous-flow designs greatly reduce analysis time as well as improve precision and allow for automation. However the accurate analysis of more complex environmental samples such as industrial sludges, soil samples, river sediments, and fly ash remains difficult. Numerous contributing factors influence the accuracy of the hydride technique. Sample digestion methods and sample preparation procedures are of critical importance. The digestion must adequately solubilize the elements of interest without loss by volatilization. Sample preparation procedures that guarantee the proper analyte oxidation state and eliminate the nitric acid and inter-element interferences are needed. In this study, difficult environmental samples were analyzed for As, Se, Sb, and Sn by continuous flow hydride generation. Sample preparation methods were optimized to eliminate interferences. The results of spike recovery studies will be presented. Data from the analysis of the same samples by graphite furnace AAS will be presented for comparison of accuracy, precision, and analysis time

Determination of total inorganic arsenic in potable water through spectroscopy of atomic absorption with generation of hydride

International Nuclear Information System (INIS)

Rodriguez Roman, Susan; Barquero, M.

2000-01-01

Arsenic is an element that has been studied in the analysis of environmental samples for its toxicity showed in very low concentrations. The objective of this work is the validation of a method for the determination of total inorganic arsenic in drinking water. Through the spectrophotometric technique of atomic absorption an automatic system of flow injection for the generation of hydrides is used. The prereduction of Arsenic was made with potasium iodide 1,5% m/v and ascorbic acid 0.25% m/v dissolved in hydrochloric acid 3,7% m/v. The recuperation percentage of the method was 97 ± 3% in a dynamic range to 30 μg/L. The detection limit was 0,7 μg/L established over 0,5 mL of sample. The samples analyzed were found under the set limits of normative in Costa Rica of 10 μg/L. (author) [es

Determination of total arsenic and arsenic(III) in phosphate fertilizers by hydride generation atomic absorption spectrometry after ultrasound-assisted extraction based on a control acid media.

Science.gov (United States)

Rezende, Helen Cristine; Coelho, Nivia Maria Melo

2014-01-01

An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample flow rate, and concentrations of the acid and reducer. The determination of As(lll) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 23 factorial design and central composite design. LODs for As(lll) and total As were 0.029 and 0.022 microg/L, respectively. The accuracy of the method was confirmed with certified reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples.

Selective reduction of arsenic species by hydride generation - atomic absorption spectrometry. Part 2 - sample storage and arsenic determination in natural waters

Directory of Open Access Journals (Sweden)

Quináia Sueli P.

2001-01-01

Full Text Available Total arsenic, arsenite, arsinate and dimethylarsinic acid (DMA were selectively determined in natural waters by hydride generation - atomic absorption spectrometry, using sodium tetrahydroborate(III as reductant but in different reduction media. River water samples from the north region of Paraná State, Brazil, were analysed and showed arsenate as the principal arsenical form. Detection limits found for As(III (citrate buffer, As(III + DMA (acetic acid and As(III + As(V (hydrochloric acid were 0.6, 1.1 and 0.5 mg As L-1, respectively. Sample storage on the proper reaction media revealed to be a useful way to preserve the water sample.

Development and evaluation of cryosorption pump and cryotrapping pump for CTR applications

International Nuclear Information System (INIS)

Kuribayashi, S.; Ota, H.; Sato, H.

1986-01-01

In order to obtain the engineering data to design compound cryopump for CTR, the authors tested the cryosorption pump and cryotrapping pump. The cryosorption panel was consisted of coconut charcoal metallically bonded to 4.2K cryopanel by brazing. The initial pumping speed of helium of cryosorption pump was found to be ≅2.2 iota/scm/sup 2/. The speed dropped off with loading (about 8 Torr iota/cm/sup 2/) to 1.5 iota/scm/sup 2/. The initial helium pumping speed of the 4.2K cryotrapping pump by argon spray was found to be ≅6 iota/scm/sup 2/. The speed, however, dropped off with loading (≅0.3 Torr iota/cm/sup 2/) to less than 5%. These results indicate that the cryosorption pump by coconut charcoal is superior to the cryotrapping pump, because the capacity of the former is larger than the latter

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

International Nuclear Information System (INIS)

Ataman, O. Yavuz

2008-01-01

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

Determination of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid in cereals by hydride generation atomic fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Matos Reyes, M.N. [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain); Department of Chemistry, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente, 225, 22453-900, Rio de Janeiro, RJ (Brazil); Cervera, M.L. [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain)], E-mail: m.luisa.cervera@uv.es; Campos, R.C. [Department of Chemistry, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente, 225, 22453-900, Rio de Janeiro, RJ (Brazil); Guardia, M. de la [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain)

2007-09-15

A fast, sensitive and simple non-chromatographic analytical method was developed for the speciation analysis of toxic arsenic species in cereal samples, namely rice and wheat semolina. An ultrasound-assisted extraction of the toxic arsenic species was performed with 1 mol L{sup -1} H{sub 3}PO{sub 4} and 0.1% (m/v) Triton XT-114. After extraction, As(III), As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) concentrations were determined by hydride generation atomic fluorescence spectrometry using a series of proportional equations corresponding to four different experimental reduction conditions. The detection limits of the method were 1.3, 0.9, 1.5 and 0.6 ng g{sup -1} for As(III), As(V), DMA and MMA, respectively, expressed in terms of sample dry weight. Recoveries were always greater than 90%, and no species interconversion occurred. The speciation analysis of a rice flour reference material certified for total arsenic led to coherent results, which were also in agreement with other speciation studies made on the same certified reference material.

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-08-15

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

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

Directory of Open Access Journals (Sweden)

Sanda Rončević

2012-01-01

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

Determination of mercury and selenium in herbal medicines and hair by using a nanometer TiO2-coated quartz tube atomizer and hydride generation atomic absorption spectrometry

International Nuclear Information System (INIS)

Li, Shun-Xing; Zheng, Feng-Ying; Cai, Shu-Jie; Cai, Tian-Shou

2011-01-01

The nanometer TiO 2 particle was coated onto the inner wall of a T-shaped quartz tube atomizer (QTA) and then was used as a new atomizer (NT-QTA) for the determination of Hg and Se by hydride generation atomic absorption spectrometry (HGAAS). After coating 67.4 mg TiO 2 on a quartz tube, the analytical performance of NT-QTA-HGAAS was compared to conventional QTA-HGAAS and it was improved as follows: (a) the linear range of the calibration curves was expanded from 10.0-80.0 ng mL -1 to 5.0-150.0 ng mL -1 for Hg, and from 10.0-70.0 ng mL -1 to 5.0-100.0 ng mL -1 for Se; (b) the characteristic concentration of was decreased from 2.8 ng mL -1 /1% to 1.1 ng mL -1 /1% for Hg and from 1.2 ng mL -1 /1% to 0.8 ng mL -1 /1% for Se; and (c) the interference from the coexistence of As on the determination of Hg and Se could be eliminated. The achieved technique was applied for the determination of Hg and Se in herbal medicines and hair.

Determination of tellurium in lead and lead alloy using flow injection-hydride generation atomic absorption spectrometry

International Nuclear Information System (INIS)

Mesko, Marcia F.; Pozebon, Dirce; Flores, Erico M.M.; Dressler, Valderi L.

2004-01-01

A method based on flow injection-hydride generation atomic absorption spectrometry (FI-HG AAS) for the determination of trace amount of Te in lead and lead alloy is described. A flow injection system (FI) and related analytical parameters as well as Te determination and interference caused by Pb, Bi and Ag on Te were investigated. The Pb interference could be overcome by using a small sample volume, while the Bi interference could be overcome by thiourea. However, it was not possible to minimise the interference caused by Ag on Te. The optimised conditions for Te determination in the analysed samples were: 6 mol l -1 HCl as sample carrier solution, 0.75% (m/v) sodium tetrahydroborate as Te reductant, 40 μl of sample solution, and 200 ml min -1 Ar flow rate as carrier gas. The limit of quantification (LOQ) was 1.0 μg g -1 Te (using 250 mg of sample in 50 ml final solution), the limit of detection (LOD) was 2.5 μg l -1 and the relative standard deviation (RSD) was 6% for five consecutive measurements of sample solution. The standard addition calibration method was used. Relatively high sample throughput (ca. 45 sample runs can be performed in a working hour), reduced sample manipulation since matrix separation is not necessary, and minor waste generation are the main advantages of the proposed method for Te determination by FI-HG AAS

Simultaneous detection of selenium by atomic fluorescence and sulfur by molecular emission by flow-injection hydride generation with on-line reduction for the determination of selenate, sulfate and sulfite

Energy Technology Data Exchange (ETDEWEB)

Tyson, J.F., E-mail: tyson@chem.umass.edu [Department of Chemistry, University of Massachusetts, 710 North Pleasant Street, Amherst, MA 01003 (United States); Palmer, C.D. [Lead Poisoning Trace Elements Laboratory, Wadsworth Center, New York State Department of Health, P.O. Box 509, Empire State Plaza, Albany, NY 12201-0509 (United States)

2009-10-12

An inductively coupled plasma atomic fluorescence spectrometry (ICP-AFS) instrument, was modified so that it was capable of monitoring transient chromatographic or flow-injection profiles and that sulfur molecular emission and selenium atomic fluorescence could be monitored simultaneously in an argon-hydrogen diffusion flame on a glass burner. The analytes were introduced as hydrogen selenide and hydrogen sulfide, generated on a flow-injection manifold. Selenate was reduced to hydride-forming selenite by microwave-assisted on-line reaction with hydrochloric acid, and sulfate, or sulfite, was reduced to hydride-forming sulfide by a mixture of hydriodic acid, acetic acid and sodium hypophosphite. The effects of the nature of reducing agent, flow rate, microwave power and coil length were studied. The limit of detection (3 s) for selenium was 10 {mu}g L{sup -1}, and for sulfide was 70 {mu}g L{sup -1} (200-{mu}L injection volume). The calibration was linear for selenium up to 2 mg L{sup -1} and to 10 mg L{sup -1} for sulfide. The throughput was 180 h{sup -1}. The three sulfur species could be differentiated on the basis of reactivity at various microwave powers.

A New Class of Atomically Precise, Hydride-Rich Silver Nanoclusters Co-Protected by Phosphines

KAUST Repository

Bootharaju, Megalamane Siddaramappa

2016-10-10

Thiols and phosphines are the most widely used organic ligands to attain atomically precise metal nanoclusters (NCs). Here, we used simple hydrides (e.g., H–) as ligands along with phosphines, such as triphenylphosphine (TPP), 1,2-bis(diphenylphosphino)ethane [DPPE], and tris(4-fluorophenyl)phosphine [TFPP] to design and synthesize a new class of hydride-rich silver NCs. This class includes [Ag18H16(TPP)10]2+, [Ag25H22(DPPE)8]3+, and [Ag26H22(TFPP)13]2+. Our work reveals a new family of atomically precise NCs protected by H– ligands and labile phosphines, with potentially more accessible active metal sites for functionalization and provides a new set of stable NC sizes with simpler ligand–metal bonding for researchers to explore both experimentally and computationally.

Speciation of arsenic in water samples by high-performance liquid chromatography-hydride generation-atomic absorption spectrometry at trace levels using a post-column reaction system

Energy Technology Data Exchange (ETDEWEB)

Stummeyer, J. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany); Harazim, B. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany); Wippermann, T. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany)

1996-02-01

Anion-exchange HPLC has been combined with hydride generation - atomic absorption spectrometry (HG-AAS) for the routine speciation of arsenite, arsenate, monomethylarsenic acid and dimethylarsinic acid. The sensitivity of the AAS-detection was increased by a post-column reaction system to achieve complete formation of volatile arsines from the methylated species and arsenate. The system allows the quantitative determination of 0.5 {mu}g/l of each arsenic compound in water samples. The stability of synthetical and natural water containing arsenic at trace levels was investigated. To preserve stored water samples, a method for quantitative separation of arsenate at high pH-values with the basic anion-exchange resin Dowex 1 x 8 was developed. (orig.)

Determination of mercury and selenium in herbal medicines and hair by using a nanometer TiO{sub 2}-coated quartz tube atomizer and hydride generation atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Li, Shun-Xing, E-mail: lishunxing@fjzs.edu.cn [Department of Chemistry and Environmental Science, Zhangzhou Normal University, Zhangzhou 363000 (China); Fujian Province University Key Laboratory of Analytical Science (Zhangzhou Normal University), Zhangzhou 363000 (China); Zheng, Feng-Ying [Department of Chemistry and Environmental Science, Zhangzhou Normal University, Zhangzhou 363000 (China); Fujian Province University Key Laboratory of Analytical Science (Zhangzhou Normal University), Zhangzhou 363000 (China); Cai, Shu-Jie; Cai, Tian-Shou [Department of Chemistry and Environmental Science, Zhangzhou Normal University, Zhangzhou 363000 (China)

2011-05-15

The nanometer TiO{sub 2} particle was coated onto the inner wall of a T-shaped quartz tube atomizer (QTA) and then was used as a new atomizer (NT-QTA) for the determination of Hg and Se by hydride generation atomic absorption spectrometry (HGAAS). After coating 67.4 mg TiO{sub 2} on a quartz tube, the analytical performance of NT-QTA-HGAAS was compared to conventional QTA-HGAAS and it was improved as follows: (a) the linear range of the calibration curves was expanded from 10.0-80.0 ng mL{sup -1} to 5.0-150.0 ng mL{sup -1} for Hg, and from 10.0-70.0 ng mL{sup -1} to 5.0-100.0 ng mL{sup -1} for Se; (b) the characteristic concentration of was decreased from 2.8 ng mL{sup -1}/1% to 1.1 ng mL{sup -1}/1% for Hg and from 1.2 ng mL{sup -1}/1% to 0.8 ng mL{sup -1}/1% for Se; and (c) the interference from the coexistence of As on the determination of Hg and Se could be eliminated. The achieved technique was applied for the determination of Hg and Se in herbal medicines and hair.

Characterization and mutual comparison of new electrolytic cell designs for hydride generation-atomic absorption spectrometry with a quartz tube atomizer using Se as a model analyte and Se-75 as a radioactive indicator

Czech Academy of Sciences Publication Activity Database

Hraníček, J.; Červený, V.; Kratzer, Jan; Vobecký, Miloslav; Rychlovský, P.

2012-01-01

Roč. 27, č. 10 (2012), s. 1761-1771 ISSN 0267-9477 R&D Projects: GA ČR GA203/09/1783 Institutional support: RVO:68081715 Keywords : electrochemical hydride generation AAS * selenium hydride * radiotracer study Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.155, year: 2012

Hydrogen generation using silicon nanoparticles and their mixtures with alkali metal hydrides

Science.gov (United States)

Patki, Gauri Dilip

Hydrogen is a promising energy carrier, for use in fuel cells, engines, and turbines for transportation or mobile applications. Hydrogen is desirable as an energy carrier, because its oxidation by air releases substantial energy (thermally or electrochemically) and produces only water as a product. In contrast, hydrocarbon energy carriers inevitably produce CO2, contributing to global warming. While CO2 capture may prove feasible in large stationary applications, implementing it in transportation and mobile applications is a daunting challenge. Thus a zero-emission energy carrier like hydrogen is especially needed in these cases. Use of H2 as an energy carrier also brings new challenges such as safe handling of compressed hydrogen and implementation of new transport, storage, and delivery processes and infrastructure. With current storage technologies, hydrogen's energy per volume is very low compared to other automobile fuels. High density storage of compressed hydrogen requires combinations of high pressure and/or low temperature that are not very practical. An alternative for storage is use of solid light weight hydrogenous material systems which have long durability, good adsorption properties and high activity. Substantial research has been conducted on carbon materials like activated carbon, carbon nanofibers, and carbon nanotubes due to their high theoretical hydrogen capacities. However, the theoretical values have not been achieved, and hydrogen uptake capacities in these materials are below 10 wt. %. In this thesis we investigated the use of silicon for hydrogen generation. Hydrogen generation via water oxidation of silicon had been ignored due to slow reaction kinetics. We hypothesized that the hydrogen generation rate could be improved by using high surface area silicon nanoparticles. Our laser-pyrolysis-produced nanoparticles showed surprisingly rapid hydrogen generation and high hydrogen yield, exceeding the theoretical maximum of two moles of H2 per

Determination of arsenic concentration in tiger tooth croaker (Otolithes ruber and indian halibut (Psettodes erumei using hydride generation atomic absorption spectrophotometer

Directory of Open Access Journals (Sweden)

E Rahimi

2011-11-01

Full Text Available Heavy metal contaminants in fish are of particular interest because of their potential risk to human. This study was undertaken to determine the levels of arsenic in two fish type including tiger tooth croaker and Indian halibut  in Esfahan. A total of 42 fish samples including 28 tiger tooth croaker (Otolithes ruber and 14 Indian halibut (Psettodes erumei were collected from retails of Esfahan from May 2010 to January 2011. For detection of arsenic contamination, the edible muscles of  fish samples were analyzed by hydride generation atomic absorption spectrophotometer. The arsenic contamination in fish samples were found to be in the range of 11 to 98 µg/kg. Concentration of arsenic in tiger tooth croaker and Indian halibut was 11-56 and 32-98 µg/kg, respectively. Arsenic concentrations were below the limit was acceptable to the World Health Organization. According to the results, the concentration of arsenic did not exceed the maximum acceptable intake limit.

Determination of arsenic speciation in sulfidic waters by Ion Chromatography Hydride-Generation Atomic Fluorescence Spectrometry (IC-HG-AFS).

Science.gov (United States)

Keller, Nicole S; Stefánsson, Andri; Sigfússon, Bergur

2014-10-01

A method for the analysis of arsenic species in aqueous sulfide samples is presented. The method uses an ion chromatography system connected with a Hydride-Generation Atomic Fluorescence Spectrometer (IC-HG-AFS). With this method inorganic As(III) and As(V) species in water samples can be analyzed, including arsenite (HnAs(III)O3(n-3)), thioarsenite (HnAs(III)S3(n-3)), arsenate (HnAs(V)O4(n-3)), monothioarsenate (HnAs(V)SO3(n-3)), dithioarsenate (HnAs(V)S2O2(n-3)), trithioarsenate (HnAs(V)S3O(n-3)) and tetrathioarsenate (HnAs(V)S4(n-3)). The peak identification and retention times were determined based on standard analysis of the various arsenic compounds. The analytical detection limit was ~1-3 µg L(-1) (LOD), depending on the quality of the baseline. This low detection limit makes this method also applicable to discriminate between waters meeting the drinking water standard of max. 10 µg L(-1) As, and waters that do not meet this standard. The new method was successfully applied for on-site determination of arsenic species in natural sulfidic waters, in which seven species were unambiguously identified. Copyright © 2014 Elsevier B.V. All rights reserved.

A modified routine analysis of arsenic content in drinking-water in Bangladesh by hydride generation-atomic absorption spectrophotometry.

Science.gov (United States)

Wahed, M A; Chowdhury, Dulaly; Nermell, Barbro; Khan, Shafiqul Islam; Ilias, Mohammad; Rahman, Mahfuzar; Persson, Lars Ake; Vahter, Marie

2006-03-01

The high prevalence of elevated levels of arsenic in drinking-water in many countries, including Bangladesh, has necessitated the development of reliable and rapid methods for the determination of a wide range of arsenic concentrations in water. A simple hydride generation-atomic absorption spectrometry (HG-AAS) method for the determination of arsenic in the range of microg/L to mg/L concentrations in water is reported here. The method showed linearity over concentrations ranging from 1 to 30 microg/L, but requires dilution of samples with higher concentrations. The detection limit ranged from 0.3 to 0.5 microg/L. Evaluation of the method, using internal quality-control (QC) samples (pooled water samples) and spiked internal QC samples throughout the study, and Standard Reference Material in certain lots, showed good accuracy and precision. Analysis of duplicate water samples at another laboratory also showed good agreement. In total, 13,286 tubewell water samples from Matlab, a rural area in Bangladesh, were analyzed. Thirty-seven percent of the water samples had concentrations below 50 microg/L, 29% below the WHO guideline value of 10 microg/L, and 17% below 1 microg/L. The HG-AAS was found to be a precise, sensitive, and reasonably fast and simple method for analysis of arsenic concentrations in water samples.

Determination and Uncertainty Analysis of Inorganic Arsenic in Husked Rice by Solid Phase Extraction and Atomic Absorption Spectrometry with Hydride Generation.

Science.gov (United States)

Saxena, Sushil Kumar; Karipalli, Agnes Raju; Krishnan, Anoop A; Rangasamy, Rajesh; Malekadi, Praveen; Singh, Dhirendra P; Vasu, Vimesh; Singh, Vijay K

2017-05-01

This study enables the selective determination of inorganic arsenic (iAs) with a low detection limit using an economical instrument [atomic absorption spectrometer with hydride generation (HG)] to meet the regulatory requirements as per European Commission (EC) and Codex guidelines. Dry rice samples (0.5 g) were diluted using 0.1 M HNO3-3% H2O2 and heated in a water bath (90 ± 2°C) for 60 min. Through this process, all the iAs is solubilized and oxidized to arsenate [As(V)]. The centrifuged extract was loaded onto a preconditioned and equilibrated strong anion-exchange SPE column (silica-based Strata SAX 500 mg/6 mL), followed by selective and sequential elution of As(V), enabling the selective quantification of iAs using atomic absorption spectrometry with HG. In-house validation showed a mean recovery of 94% and an LOQ of 0.025 mg/kg. The repeatability (HorRatr) and reproducibility (HorRatR) values were <2, meeting the performance criteria mandated by the EC. The combined standard measurement uncertainty by this method was less than the maximum standard measurement uncertainty; thus, the method can be considered for official control purposes. The method was applied for the determination of iAs in husked rice samples and has potential applications in other food commodities.

Selective determination of four arsenic species in rice and water samples by modified graphite electrode-based electrolytic hydride generation coupled with atomic fluorescence spectrometry.

Science.gov (United States)

Yang, Xin-An; Lu, Xiao-Ping; Liu, Lin; Chi, Miao-Bin; Hu, Hui-Hui; Zhang, Wang-Bing

2016-10-01

This work describes a novel non-chromatographic approach for the accurate and selective determining As species by modified graphite electrode-based electrolytic hydride generation (EHG) for sample introduction coupled with atomic fluorescence spectrometry (AFS) detection. Two kinds of sulfydryl-containing modifiers, l-cysteine (Cys) and glutathione (GSH), are used to modify cathode. The EHG performance of As has been changed greatly at the modified cathode, which has never been reported. Arsenite [As(III)] on the GSH modified graphite electrode (GSH/GE)-based EHG can be selectively and quantitatively converted to AsH3 at applied current of 0.4A. As(III) and arsenate [As(V)] on the Cys modified graphite electrode (Cys/GE) EHG can be selectively and efficiently converted to arsine at applied current of 0.6A, whereas monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA) do not form any or only less volatile hydrides under this condition. By changing the analytical conditions, we also have achieved the analysis of total As (tAs) and DMA. Under the optimal condition, the detection limits (3s) of As(III), iAs and tAs in aqueous solutions are 0.25μgL(-1), 0.22μgL(-1) and 0.10μgL(-1), respectively. The accuracy of the method is verified through the analysis of standard reference materials (SRM 1568a). Copyright © 2016 Elsevier B.V. All rights reserved.

Validation of a hydride generation atomic absorption spectrometry methodology for determination of mercury in fish designed for application in the Brazilian national residue control plan.

Science.gov (United States)

Damin, Isabel C F; Santo, Maria A E; Hennigen, Rosmari; Vargas, Denise M

2013-01-01

In the present study, a method for the determination of mercury (Hg) in fish was validated according to ISO/IEC 17025, INMETRO (Brazil), and more recent European recommendations (Commission Decision 2007/333/EC and 2002/657/EC) for implementation in the Brazilian Residue Control Plan (NRCP) in routine applications. The parameters evaluated in the validation were investigated in detail. The results obtained for limit of detection and quantification were respectively, 2.36 and 7.88 μg kg(-1) of Hg. While the recovery varies between 90-96%. The coefficient of variation was of 4.06-8.94% for the repeatability. Furthermore, a comparison using an external proficiency testing scheme was realized. The results of method validated for the determination of the mercury in fish by Hydride generation atomic absorption spectrometry were considered suitable for implementation in routine analysis.

Mechanisms of chemical generation of volatile hydrides for trace element determination (IUPAC Technical Report)

Czech Academy of Sciences Publication Activity Database

D'Ulivo, A.; Dědina, Jiří; Mester, Z.; Sturgeon, R. E.; Wang, Q.; Welz, B.

2011-01-01

Roč. 83, č. 6 (2011), s. 1283-1340 ISSN 0033-4545 Institutional research plan: CEZ:AV0Z40310501 Keywords : borane complexes * chemical generation of volatile hydrides (CHG) * volatile hydrides Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.789, year: 2011

NMR study of hydride systems

International Nuclear Information System (INIS)

Peretz, M.

1980-02-01

The hydrides of thorium (ThH 2 , Th 4 H 15 and Th 4 D 15 ) and the intermetallic compound system (Zr(Vsub(1-x)Cosub(x)) 2 and its hydrides were investigated using the nuclear magnetic resonance (NMR) technique. From the results for the thorium hydride samples it was concluded that the density of states at the Fermi level n(Esub(f)) is higher in Th 4 H 15 than in ThH 2 ; there is an indirect reaction between the protons and the d electrons belonging to the Th atoms in Th 4 H 15 ; n(E) has a sharp structure near Esub(f). It was also found that the hydrogen diffusion mechanism changes with temperature. From the results for the intermetallic compound system conclusions were drawn concerning variations in the electronic structure, which explain the behavior of the system. In hydrogen diffusion studies in several samples it was found that Co atoms slow the diffusion rate. Quadrupole spectra obtained at low temperatures show that the H atoms preferably occupy tetrahedral sites formed by three V atoms and one Z atom. (H.K.)

Determination of total arsenic in fish by hydride-generation atomic absorption spectrometry: method validation, traceability and uncertainty evaluation

Science.gov (United States)

Nugraha, W. C.; Elishian, C.; Ketrin, R.

2017-03-01

Fish containing arsenic compound is one of the important indicators of arsenic contamination in water monitoring. The high level of arsenic in fish is due to absorption through food chain and accumulated in their habitat. Hydride generation (HG) coupled with atomic absorption spectrometric (AAS) detection is one of the most popular techniques employed for arsenic determination in a variety of matrices including fish. This study aimed to develop a method for the determination of total arsenic in fish by HG-AAS. The method for sample preparation from American of Analytical Chemistry (AOAC) Method 999.10-2005 was adopted for acid digestion using microwave digestion system and AOAC Method 986.15 - 2005 for dry ashing. The method was developed and validated using Certified Reference Material DORM 3 Fish Protein for trace metals for ensuring the accuracy and the traceability of the results. The sources of uncertainty of the method were also evaluated. By using the method, it was found that the total arsenic concentration in the fish was 45.6 ± 1.22 mg.Kg-1 with a coverage factor of equal to 2 at 95% of confidence level. Evaluation of uncertainty was highly influenced by the calibration curve. This result was also traceable to International Standard System through analysis of Certified Reference Material DORM 3 with 97.5% of recovery. In summary, it showed that method of preparation and HG-AAS technique for total arsenic determination in fish were valid and reliable.

Development of a direct hydride generation nebulizer for the determination of selenium by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Carrion, Nereida; Murillo, Miguel; Montiel, Edie; Diaz, Dorfe

2003-01-01

A study was conducted to evaluate the performance of a new direct hydride generation nebulizer system for determination of hydride forming elements by inductively coupled plasma optical emission spectroscopy. This system was designed and optimized to obtain the highest sensitivity. Several experimental designs were used for these purposes. To optimize the individual parameters of the system, and to study the interaction between these parameters for both direct hydride generation nebulizers, a central composite orthogonal design with eight factors was set up. Significant behavioral differences were observed in the two direct hydride generation nebulizers studied. Finally, a 70 μm gas orifice nebulizer exhibits a better detection limit than the 120 μm nebulizer. Generally, for determination of selenium, this new direct hydride generation nebulizer system exhibits a linear dynamic range and detection limit (3σb) of 3 orders of magnitude and 0.2 μg l -1 for selenium, respectively. This new hydride generator is much simpler system that conventional hydride generation systems, which does not need to be changed to work in normal mode with the inductively coupled plasma, since this system may be used for hydride forming elements and those that do not form them. It produces a rapid response with low memory effect. It reduces the interference level of Ni, Co and Cu to 600, 500 and 5 mg l -1 , respectively. The accuracy of the system was verified by the determination of selenium in several standard reference materials of ambient, food and clinical sample matrices. No statistically significant differences (95 confidence level) were obtained between our method and the reference values

Gas atomization processing of tin and silicon modified LaNi₅ for nickel-metal hydride battery applications

Energy Technology Data Exchange (ETDEWEB)

Ting, Jason [Iowa State Univ., Ames, IA (United States)

1999-02-12

Numerous researchers have studied the relevant material properties of so-called AB₅ alloys for battery applications. These studies involved LaNi₅ substituted alloys which were prepared using conventional cast and crush alloying techniques. While valuable to the understanding of metal hydride effects, the previous work nearly ignored the potential for alternative direct powder production methods, like high pressure gas atomization (HPGA). Thus, there is a need to understand the relationship between gas atomization processes, powder particle solidification phases, and hydrogen absorption properties of ultra fine (< 25 μm) atomized powders with high surface area for enhanced battery performance. Concurrently, development of a gas atomization nozzle that is more efficient than all current designs is needed to increase the yield of ultrafine AB₅ alloy powder for further processing advantage. Gas atomization processing of the AB₅ alloys was demonstrated to be effective in producing ultrafine spherical powders that were resilient to hydrogen cycling for the benefit of improving corrosion resistance in battery application. These ultrafine powders benefited from the rapid solidification process by having refined solute segregation in the microstructure of the gas atomized powders which enabled a rapid anneal treatment of the powders. The author has demonstrated the ability to produce high yields of ultrafine powder efficiently and cost effectively, using the new HPGA-III technology. Thus, the potential benefits of processing AB₅ alloys using the new HPGA technology could reduce manufacturing cost of nickel-metal hydride powder. In the near future, the manufacture of AB₅ alloy powders could become a continuous and rapid production process. The economic benefit of an improved AB₅ production process may thereby encourage the use of nickel-metal hydride rechargeable batteries in electrical vehicle

Atomic hydrogen storage. [cryotrapping and magnetic field strength

Science.gov (United States)

Woollam, J. A. (Inventor)

1980-01-01

Atomic hydrogen, for use as a fuel or as an explosive, is stored in the presence of a strong magnetic field in exfoliated layered compounds such as molybdenum disulfide or an elemental layer material such as graphite. The compound is maintained at liquid temperatures and the atomic hydrogen is collected on the surfaces of the layered compound which are exposed during delamination (exfoliation). The strong magnetic field and the low temperature combine to prevent the atoms of hydrogen from recombining to form molecules.

Flow analysis-hydride generation-gas phase derivative molecular absorption spectrophotometric determination of antimony in antileishmanial drugs

Directory of Open Access Journals (Sweden)

Máximo Gallignani

2009-01-01

Full Text Available In the present work, the development of a method based on the coupling of flow analysis (FA, hydride generation (HG, and derivative molecular absorption spectrophotometry (D-EAM in gas phase (GP, is described in order to determine total antimony in antileishmanial products. Second derivative order (D²224nm of the absorption spectrum (190 - 300 nm is utilized as measurement criterion. Each one of the parameters involved in the development of the proposed method was examined and optimized. The utilization of the EAM in GP as detection system in a continuous mode instead of atomic absorption spectrometry represents the great potential of the analytic proposal.

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

Energy Technology Data Exchange (ETDEWEB)

Li, Shan, E-mail: ls_tuzi@163.com; Wang, Mei, E-mail: wmei02@163.com; Zhong, Yizhou, E-mail: yizhz@21cn.com; Zhang, Zehua, E-mail: kazuki.0101@aliyun.com; Yang, Bingyi, E-mail: e_yby@163.com

2015-09-01

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

On the Chemistry of Hydrides of N Atoms and O+ Ions

Science.gov (United States)

Awad, Zainab; Viti, Serena; Williams, David A.

2016-08-01

Previous work by various authors has suggested that the detection by Herschel/HIFI of nitrogen hydrides along the low-density lines of sight toward G10.6-0.4 (W31C) cannot be accounted for by gas-phase chemical models. In this paper we investigate the role of surface reactions on dust grains in diffuse regions, and we find that formation of the hydrides by surface reactions on dust grains with efficiency comparable to that for H2 formation reconciles models with observations of nitrogen hydrides. However, similar surface reactions do not contribute significantly to the hydrides of O+ ions detected by Herschel/HIFI that are present along many sight lines in the Galaxy. The O+ hydrides can be accounted for by conventional gas-phase chemistry either in diffuse clouds of very low density with normal cosmic-ray fluxes or in somewhat denser diffuse clouds with high cosmic-ray fluxes. Hydride chemistry in dense dark clouds appears to be dominated by gas-phase ion-molecule reactions.

Gas atomization of Cu-modified AB5 metal hydride alloys

International Nuclear Information System (INIS)

Young, K.; Ouchi, T.; Banik, A.; Koch, J.; Fetcenko, M.A.; Bendersky, L.A.; Wang, K.; Vaudin, M.

2011-01-01

Research highlights: → The gas atomization process together with a hydrogen annealing process was demonstrated on AB5 alloys. → The method was found to be effective in restoring the original cycle life sacrificed by the incorporation of copper in the alloy formula as a means of improving the low temperature performance of AB 5 alloys. → The new process also improves high rate, low temperature, and charge retention performances for both Cu-free and Cu-containing AB 5 alloys. - Abstract: Gas atomization together with a hydrogen annealing process has been proposed as a method to achieve improved low-temperature performance of AB 5 alloy electrodes in Ni/MH batteries and restore the original cycle life which was sacrificed by the incorporation of copper in the alloy formula. While the gas atomization process reduces the lattice constant aspect ratio c/a of the Cu-containing alloys, the addition of a hydrogen annealing step recovers this property, although it is still inferior to the conventionally prepared annealed Cu-free alloy. This observation correlates very well with the cycle life performance. In addition to extending the cycle life of the Cu-containing metal hydride electrode, processing by gas atomization with additional hydrogen annealing improves high-rate, low-temperature, and charge retention performances for both Cu-free and Cu-containing AB 5 alloys. The degradation mechanisms of alloys made by different processes through cycling are also discussed.

Rapid hydrogen gas generation using reactive thermal decomposition of uranium hydride.

Energy Technology Data Exchange (ETDEWEB)

Kanouff, Michael P.; Van Blarigan, Peter; Robinson, David B.; Shugard, Andrew D.; Gharagozloo, Patricia E.; Buffleben, George M.; James, Scott Carlton; Mills, Bernice E.

2011-09-01

Oxygen gas injection has been studied as one method for rapidly generating hydrogen gas from a uranium hydride storage system. Small scale reactors, 2.9 g UH{sub 3}, were used to study the process experimentally. Complimentary numerical simulations were used to better characterize and understand the strongly coupled chemical and thermal transport processes controlling hydrogen gas liberation. The results indicate that UH{sub 3} and O{sub 2} are sufficiently reactive to enable a well designed system to release gram quantities of hydrogen in {approx} 2 seconds over a broad temperature range. The major system-design challenge appears to be heat management. In addition to the oxidation tests, H/D isotope exchange experiments were performed. The rate limiting step in the overall gas-to-particle exchange process was found to be hydrogen diffusion in the {approx}0.5 {mu}m hydride particles. The experiments generated a set of high quality experimental data; from which effective intra-particle diffusion coefficients can be inferred.

Evaluation of Neutron shielding efficiency of Metal hydrides

Energy Technology Data Exchange (ETDEWEB)

Jeon, Sang Hwan; Chae, San; Kim, Yong Soo [Hanyang University, Seoul (Korea, Republic of)

2012-05-15

Neutron shielding is achieved of interaction with material by moderation and absorption. Material that contains large amounts hydrogen atoms which are almost same neutron atomic weight is suited for fast neutron shielding material. Therefore, polymers containing high density hydrogen atom are being used for fast neutron shielding. On the other hand, composite materials containing high thermal neutron absorption cross section atom (Li, B, etc) are being used for thermal neutron shielding. However, these materials have low fast neutron absorption cross section. Therefore, these materials are not suited for fast neutron shielding. Hydrogen which has outstanding neutron energy reduction ability has very low thermal neutron absorption cross section, almost cannot be used for thermal neutron shielding. In this case, a large atomic number material (Pb, U, etc.) has been used. Thus, metal hydrides are considered as complement to concrete shielding material. Because metal hydrides contain high hydrogen density and elements with high atomic number. In this research neutron shielding performance and characteristic of nuclear about metal hydrides ((TiH{sub 2}, ZrH{sub 2}, HfH{sub 2}) is evaluated by experiment and MCNPX using {sup 252}Cf neutron source as purpose development shielding material to developed shielding material

Quantifying uncertainty in measurement of mercury in suspended particulate matter by cold vapor technique using atomic absorption spectrometry with hydride generator.

Science.gov (United States)

Singh, Nahar; Ahuja, Tarushee; Ojha, Vijay Narain; Soni, Daya; Tripathy, S Swarupa; Leito, Ivo

2013-01-01

As a result of rapid industrialization several chemical forms of organic and inorganic mercury are constantly introduced to the environment and affect humans and animals directly. All forms of mercury have toxic effects; therefore accurate measurement of mercury is of prime importance especially in suspended particulate matter (SPM) collected through high volume sampler (HVS). In the quantification of mercury in SPM samples several steps are involved from sampling to final result. The quality, reliability and confidence level of the analyzed data depends upon the measurement uncertainty of the whole process. Evaluation of measurement uncertainty of results is one of the requirements of the standard ISO/IEC 17025:2005 (European Standard EN IS/ISO/IEC 17025:2005, issue1:1-28, 2006). In the presented study the uncertainty estimation in mercury determination in suspended particulate matter (SPM) has been carried out using cold vapor Atomic Absorption Spectrometer-Hydride Generator (AAS-HG) technique followed by wet chemical digestion process. For the calculation of uncertainty, we have considered many general potential sources of uncertainty. After the analysis of data of seven diverse sites of Delhi, it has been concluded that the mercury concentration varies from 1.59 ± 0.37 to 14.5 ± 2.9 ng/m(3) with 95% confidence level (k = 2).

Determination of ultra trace arsenic species in water samples by hydride generation atomic absorption spectrometry after cloud point extraction

Energy Technology Data Exchange (ETDEWEB)

Ulusoy, Halil Ibrahim, E-mail: hiulusoy@yahoo.com [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey); Akcay, Mehmet; Ulusoy, Songuel; Guerkan, Ramazan [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey)

2011-10-10

Graphical abstract: The possible complex formation mechanism for ultra-trace As determination. Highlights: {yields} CPE/HGAAS system for arsenic determination and speciation in real samples has been applied first time until now. {yields} The proposed method has the lowest detection limit when compared with those of similar CPE studies present in literature. {yields} The linear range of the method is highly wide and suitable for its application to real samples. - Abstract: Cloud point extraction (CPE) methodology has successfully been employed for the preconcentration of ultra-trace arsenic species in aqueous samples prior to hydride generation atomic absorption spectrometry (HGAAS). As(III) has formed an ion-pairing complex with Pyronine B in presence of sodium dodecyl sulfate (SDS) at pH 10.0 and extracted into the non-ionic surfactant, polyethylene glycol tert-octylphenyl ether (Triton X-114). After phase separation, the surfactant-rich phase was diluted with 2 mL of 1 M HCl and 0.5 mL of 3.0% (w/v) Antifoam A. Under the optimized conditions, a preconcentration factor of 60 and a detection limit of 0.008 {mu}g L{sup -1} with a correlation coefficient of 0.9918 was obtained with a calibration curve in the range of 0.03-4.00 {mu}g L{sup -1}. The proposed preconcentration procedure was successfully applied to the determination of As(III) ions in certified standard water samples (TMDA-53.3 and NIST 1643e, a low level fortified standard for trace elements) and some real samples including natural drinking water and tap water samples.

Simultaneous analysis of arsenic, antimony, selenium and tellurium in environmental samples using hydride generation ICPMS

International Nuclear Information System (INIS)

Jankowski, L.M.; Breidenbach, R.; Bakker, I.J.I.; Epema, O.J.

2009-01-01

Full text: A quantitative method for simultaneous analysis of arsenic, antimony, selenium and tellurium in environmental samples is being developed using hydride generation ICPMS. These elements must be first transformed into hydride-forming oxidation states. This is particularly challenging for selenium and antimony because selenium is susceptible to reduction to the non-hydride-forming elemental state and antimony requires strong reducing conditions. The effectiveness of three reducing agents (KI, thiourea, cysteine) is studied. A comparison is made between addition of reducing agent to the sample and addition of KI to the NaBH 4 solution. Best results were obtained with the latter approach. (author)

Thermodynamics of various F420 coenzyme models as sources of electrons, hydride ions, hydrogen atoms and protons in acetonitrile.

Science.gov (United States)

Xia, Ke; Shen, Guang-Bin; Zhu, Xiao-Qing

2015-06-14

32 F420 coenzyme models with alkylation of the three different N atoms (N1, N3 and N10) in the core structure (XFH(-)) were designed and synthesized and the thermodynamic driving forces (defined in terms of the molar enthalpy changes or the standard redox potentials in this work) of the 32 XFH(-) releasing hydride ions, hydrogen atoms and electrons, the thermodynamic driving forces of the 32 XFH˙ releasing protons and hydrogen atoms and the thermodynamic driving forces of XF(-)˙ releasing electrons in acetonitrile were determined using titration calorimetry and electrochemical methods. The effects of the methyl group at N1, N3 and N10 and a negative charge on N1 and N10 atoms on the six thermodynamic driving forces of the F420 coenzyme models and their related reaction intermediates were examined; the results show that seating arrangements of the methyl group and the negative charge have remarkably different effects on the thermodynamic properties of the F420 coenzyme models and their related reaction intermediates. The effects of the substituents at C7 and C8 on the six thermodynamic driving forces of the F420 coenzyme models and their related reaction intermediates were also examined; the results show that the substituents at C7 and C8 have good Hammett linear free energy relationships with the six thermodynamic parameters. Meanwhile, a reasonable determination of possible reactions between members of the F420 family and NADH family in vivo was given according to a thermodynamic analysis platform constructed using the elementary step thermodynamic parameter of F420 coenzyme model 2FH(-) and NADH model MNAH releasing hydride ions in acetonitrile. The information disclosed in this work can not only fill a gap in the chemical thermodynamics of F420 coenzyme models as a class of very important organic sources of electrons, hydride ions, hydrogen atoms and protons, but also strongly promote the fast development of the chemistry and applications of F420 coenzyme.

Flame emission, atomic absorption and fluorescence spectrometry

International Nuclear Information System (INIS)

Horlick, G.

1980-01-01

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

Reliability of graphite furnace atomic absorption spectrometry as ...

African Journals Online (AJOL)

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

Preparation of beryllium hydride

International Nuclear Information System (INIS)

Lowrance, B.R.

1975-01-01

A process is described for the preparation of beryllium hydride which comprises pyrolyzing, while in solution in a solvent inert under the reaction conditions, with respect to reactants and products and at a temperature in the range of about 100 0 to about 200 0 C, sufficient to result in the formation of beryllium hydride, a di-t-alkyl beryllium etherate wherein each tertiary alkyl radical contains from 4 to 20 carbon atoms. The pyrolysis is carried out under an atmosphere inert under the reaction conditions, with respect to reactants and products. (U.S.)

ON THE CHEMISTRY OF HYDRIDES OF N ATOMS AND O{sup +} IONS

Energy Technology Data Exchange (ETDEWEB)

Awad, Zainab [Astronomy, Space Science, and Meteorology Department, Faculty of Science, Cairo University, Giza (Egypt); Viti, Serena; Williams, David A., E-mail: zma@sci.cu.edu.eg [Physics and Astronomy Department, University College London, Gower Street, London WC1E 6BT (United Kingdom)

2016-08-01

Previous work by various authors has suggested that the detection by Herschel /HIFI of nitrogen hydrides along the low-density lines of sight toward G10.6-0.4 (W31C) cannot be accounted for by gas-phase chemical models. In this paper we investigate the role of surface reactions on dust grains in diffuse regions, and we find that formation of the hydrides by surface reactions on dust grains with efficiency comparable to that for H{sub 2} formation reconciles models with observations of nitrogen hydrides. However, similar surface reactions do not contribute significantly to the hydrides of O{sup +} ions detected by Herschel /HIFI that are present along many sight lines in the Galaxy. The O{sup +} hydrides can be accounted for by conventional gas-phase chemistry either in diffuse clouds of very low density with normal cosmic-ray fluxes or in somewhat denser diffuse clouds with high cosmic-ray fluxes. Hydride chemistry in dense dark clouds appears to be dominated by gas-phase ion–molecule reactions.

ATOM - an OMERO add-on for automated import of image data

Directory of Open Access Journals (Sweden)

Lipp Peter

2011-10-01

Full Text Available Abstract Background Modern microscope platforms are able to generate multiple gigabytes of image data in a single experimental session. In a routine research laboratory workflow, these data are initially stored on the local acquisition computer from which files need to be transferred to the experimenter's (remote image repository (e.g., DVDs, portable hard discs or server-based storage because of limited local data storage. Although manual solutions for this migration, such as OMERO - a client-server software for visualising and managing large amounts of image data - exist, this import process may be a time-consuming and tedious task. Findings We have developed ATOM, a Java-based and thus platform-independent add-on for OMERO enabling automated transfer of image data from a wide variety of acquisition software packages into OMERO. ATOM provides a graphical user interface and allows pre-organisation of experimental data for the transfer. Conclusions ATOM is a convenient extension of the OMERO software system. An automated interface to OMERO will be a useful tool for scientists working with file formats supported by the Bio-Formats file format library, a platform-independent library for reading the most common file formats of microscope images.

Minimum Entropy Generation Theorem Investigation and Optimization of Metal Hydride Alloy Hydrogen Storage

Directory of Open Access Journals (Sweden)

Chi-Chang Wang

2014-05-01

Full Text Available The main purpose of this paper is to carry out numerical simulation of the hydrogen storage on exothermic reaction of metal hydride LaNi5 alloy container. In addition to accelerating the reaction speed of the internal metal hydride by internal control tube water-cooled mode, analyze via the application of second law of thermodynamics the principle of entropy generation. Use COMSOL Mutilphysics 4.3 a to engage in finite element method value simulation on two-dimensional axisymmetric model. Also on the premise that the internal control tube parameters the radius ri, the flow rate U meet the metal hydride saturation time, observe the reaction process of two parameters on the tank, entropy distribution and the results of the accumulated entropy. And try to find the internal tube parameter values of the minimum entropy, whose purpose is to be able to identify the reaction process and the reaction results of internal tank’s optimum energy conservation.

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

Science.gov (United States)

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

1979-01-01

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

Cyclopentadiene-mediated hydride transfer from rhodium complexes.

Science.gov (United States)

Pitman, C L; Finster, O N L; Miller, A J M

2016-07-12

Attempts to generate a proposed rhodium hydride catalytic intermediate instead resulted in isolation of (Cp*H)Rh(bpy)Cl (1), a pentamethylcyclopentadiene complex, formed by C-H bond-forming reductive elimination from the fleeting rhodium hydride. The hydride transfer ability of diene 1 was explored through thermochemistry and hydride transfer reactions, including the reduction of NAD(+).

On-line pre-reduction of Se(VI) by thiourea for selenium speciation by hydride generation

International Nuclear Information System (INIS)

Qiu Jianhua; Wang Qiuquan; Ma Yuning; Yang Limin; Huang Benli

2006-01-01

In this study, thiourea (TU) was novelly developed as a reduction reagent for on-line pre-reduction of selenium(VI) before conventional hydride generation (HG) by KBH 4 /NaOH-HCl. After TU on-line pre-reduction, the HG efficiency of Se(VI) has been greatly improved and because even higher than that of the same amount of Se(IV) obtained in the conventional HG system. The possible pre-reduction mechanism is discussed. The detection limit (DL) of selenate reaches 10 pg mL -1 when using on-line TU pre-reduction followed by HG atomic fluorescence detection. When TU pre-reduction followed by HG is used as an interface between ion-pair high performance liquid chromatography and atomic fluorescence spectrometry, selenocystine, selenomethionine, selenite and selenate can be measured simultaneously and quantitatively. The DLs of these are 0.06, 0.08, 0.05 and 0.04 ng mL -1 , respectively, and the relative standard deviations of 9 duplicate runs for all the 4 species are less than 5%. Furthermore, it was successfully applied to Se speciation analysis of cultured garlic samples, and validated by determination of total selenium and selenium species in certified reference material NIST 1946

Determination of the population of octahedral and tetrahedral interstitials in zirconium hydrides

International Nuclear Information System (INIS)

Fedorov, V.M.; Gogava, V.V.; Shilo, S.I.; Biryukova, E.A.

1983-01-01

Results of neutron investigations of ZrHsub(1.66), ZrHsub(1.75) and ZrHsub(1.98) zirconium hydrides are presented. Investigations were conducted using plane polycrystal samples by multidetector system of scattered neutron detection. Neutron diffraction method was used to determine the number of interstitial hydrogen atoms in interstitials of the lattice cell in the case of statistic atom distribution. The numbers of interstitial atoms in octahedral interstitials for zirconium hydrides were determined experimentally; the difference of potential energies of hydrogen atoms in octa- and tetrahedral interstitials was determined as well. It is shown that experimentally determined difference of potential energies of hydrogen atoms, occupying octa- and tetrahedral positions in investigated zirconium hydrides results at room temperature in the pretailing occupation of tetrahedral interstitials by hydrogen atoms (85-90%); the occupation number grows with temperature decrease and the ordering of interstitial vacancies with formation of hydrogen superstructure takes place at low temperatures

Hydride heat pump. Volume I. Users manual for HYCSOS system design program. [HYCSOS code

Energy Technology Data Exchange (ETDEWEB)

Gorman, R.; Moritz, P.

1978-05-01

A method for the design and costing of a metal hydride heat pump for residential use and a computer program, HYCSOS, which automates that method are described. The system analyzed is one in which a metal hydride heat pump can provide space heating and space cooling powered by energy from solar collectors and electric power generated from solar energy. The principles and basic design of the system are presented, and the computer program is described giving detailed design and performance equations used in the program. The operation of the program is explained, and a sample run is presented. This computer program is part of an effort to design, cost, and evaluate a hydride heat pump for residential use. The computer program is written in standard Fortran IV and was run on a CDC Cyber 74 and Cyber 174 computer. A listing of the program is included as an appendix. This report is Volume 1 of a two-volume document.

A NOVEL METHOD OF THE HYDRIDE SEPARATION FOR THE DETERMINATION OF ARSENIC AND ANTIMONY BY AAS

Directory of Open Access Journals (Sweden)

Ganden Supriyanto

2010-06-01

Full Text Available A novel method is proposed for the hydride separation when determinining of arsenic and antimony by AAS. A chromatomembrane cell was used as preconcentration-, extraction- and separation-manifold instead of the U-tube phase separator, which is normally fitted in continuous flow vapour systems generating conventionaly the hydrides. The absorbances of the hydrides produced were measured by an atomic absorption spectrophotometer at 193.7 nm and 217.6 nm. Under optimized analytical conditions, the calibration plot for arsenic was linear from 50 to 500 ng.mL-1 (r2 = 0.9982. The precision for three subsequent measurements of 500 ng.mL-1 arsenic gave rise to a relative standard deviation of 0.4%. The detection limit was 15 ng.mL-1, which is much lower compared with that of the conventional hydride system (2000 ng.mL-1. A similar result was observed in case of antimony: the detection limit was 8 ng.mL-1 when the proposed method was applied. Consequently, the sensitivity of the novel method surpasses systems with conventional hydride generation, i.e. the precision and the acuracy increase whereas the standard deviation and the detection limit decrease. The proposed method was applied in pharmacheutial analysis and the certified As-content of a commercial product was very sufficiently confirmed.   Keywords: Chromatomembrane Cell, Hydride separation, Arsenic detection, Antimony detection, AAS

Investigation of hydride generation from arsenosugars - Is it feasible for speciation analysis?

Czech Academy of Sciences Publication Activity Database

Marschner, Karel; Musil, Stanislav; Mikšík, Ivan; Dědina, Jiří

2018-01-01

Roč. 1008, MAY (2018), s. 8-17 ISSN 0003-2670 R&D Projects: GA MŠk(CZ) LH15174 Institutional support: RVO:68081715 ; RVO:67985823 Keywords : arsenosugars * hydride generation * speciation analysis Subject RIV: CB - Analytical Chemistry, Separation; CB - Analytical Chemistry, Separation (FGU-C) OBOR OECD: Analytical chemistry; Analytical chemistry (FGU-C) Impact factor: 4.950, year: 2016

Automated atomic absorption spectrophotometer, utilizing a programmable desk calculator

International Nuclear Information System (INIS)

Futrell, T.L.; Morrow, R.W.

1977-01-01

A commercial, double-beam atomic absorption spectrophotometer has been interfaced with a sample changer and a Hewlett-Packard 9810A calculator to yield a completely automated analysis system. The interface electronics can be easily constructed and should be adaptable to any double-beam atomic absorption instrument. The calculator is easily programmed and can be used for general laboratory purposes when not operating the instrument. The automated system has been shown to perform very satisfactorily when operated unattended to analyze a large number of samples. Performance statistics agree well with a manually operated instrument

A novel magnesium-vanadium hydride synthesized by a gigapascal-high-pressure technique

Energy Technology Data Exchange (ETDEWEB)

Kyoi, Daisuke; Sato, Toyoto; Roennebro, Ewa; Tsuji, Yasufumi; Kitamura, Naoyuki; Ueda, Atsushi; Ito, Mikio; Katsuyama, Shigeru; Hara, Shigeta; Noreus, Dag; Sakai, Tetsuo

2004-07-28

A magnesium-based vanadium-doped hydride was prepared in a high-pressure anvil cell by reacting a MgH{sub 2}-25%V molar mixture at 8 GPa and 873 K. The new magnesium-vanadium hydride has a cubic F-centred substructure (a=4.721(1) Angst), with an additional superstructure, which could be described by a doubling of the cubic cell axis and a magnesium atom framework, including an ordered arrangement of both vanadium atoms and vacancies (a=9.437(3) Angst, space group Fm3-bar m (no. 225), Z=4, V=840.55 Angst{sup 3}). The metal atom structure is related to the Ca{sub 7}Ge type structure but the refined metal atom composition with vacancies on one of the magnesium sites corresponding to Mg{sub 6}V nearly in line with EDX analysis. The thermal properties of the new compound were also studied by TPD analysis and TG-DTA. The onset of the hydrogen desorption for the new Mg{sub 6}V hydride occurred at a 160 K lower temperature when compared to magnesium hydride at a heating rate of 10 K/min.

Hydrides of Alkaline Earth–Tetrel (AeTt) Zintl Phases: Covalent Tt–H Bonds from Silicon to Tin

Energy Technology Data Exchange (ETDEWEB)

Auer, Henry; Guehne, Robin; Bertmer, Marko; Weber, Sebastian; Wenderoth, Patrick; Hansen, Thomas Christian; Haase, Jürgen; Kohlmann, Holger (Leipzig); (Saarland-MED); (ILL)

2017-01-18

Zintl phases form hydrides either by incorporating hydride anions (interstitial hydrides) or by covalent bonding of H to the polyanion (polyanionic hydrides), which yields a variety of different compositions and bonding situations. Hydrides (deuterides) of SrGe, BaSi, and BaSn were prepared by hydrogenation (deuteration) of the CrB-type Zintl phases AeTt and characterized by laboratory X-ray, synchrotron, and neutron diffraction, NMR spectroscopy, and quantum-chemical calculations. SrGeD4/3–x and BaSnD4/3–x show condensed boatlike six-membered rings of Tt atoms, formed by joining three of the zigzag chains contained in the Zintl phase. These new polyanionic motifs are terminated by covalently bound H atoms with d(Ge–D) = 1.521(9) Å and d(Sn–D) = 1.858(8) Å. Additional hydride anions are located in Ae4 tetrahedra; thus, the features of both interstitial hydrides and polyanionic hydrides are represented. BaSiD2–x retains the zigzag Si chain as in the parent Zintl phase, but in the hydride (deuteride), it is terminated by H (D) atoms, thus forming a linear (SiD) chain with d(Si–D) = 1.641(5) Å.

Quantifying uncertainty in the measurement of arsenic in suspended particulate matter by Atomic Absorption Spectrometry with hydride generator

Directory of Open Access Journals (Sweden)

Ahuja Tarushee

2011-04-01

Full Text Available Abstract Arsenic is the toxic element, which creates several problems in human being specially when inhaled through air. So the accurate and precise measurement of arsenic in suspended particulate matter (SPM is of prime importance as it gives information about the level of toxicity in the environment, and preventive measures could be taken in the effective areas. Quality assurance is equally important in the measurement of arsenic in SPM samples before making any decision. The quality and reliability of the data of such volatile elements depends upon the measurement of uncertainty of each step involved from sampling to analysis. The analytical results quantifying uncertainty gives a measure of the confidence level of the concerned laboratory. So the main objective of this study was to determine arsenic content in SPM samples with uncertainty budget and to find out various potential sources of uncertainty, which affects the results. Keeping these facts, we have selected seven diverse sites of Delhi (National Capital of India for quantification of arsenic content in SPM samples with uncertainty budget following sampling by HVS to analysis by Atomic Absorption Spectrometer-Hydride Generator (AAS-HG. In the measurement of arsenic in SPM samples so many steps are involved from sampling to final result and we have considered various potential sources of uncertainties. The calculation of uncertainty is based on ISO/IEC17025: 2005 document and EURACHEM guideline. It has been found that the final results mostly depend on the uncertainty in measurement mainly due to repeatability, final volume prepared for analysis, weighing balance and sampling by HVS. After the analysis of data of seven diverse sites of Delhi, it has been concluded that during the period from 31st Jan. 2008 to 7th Feb. 2008 the arsenic concentration varies from 1.44 ± 0.25 to 5.58 ± 0.55 ng/m3 with 95% confidence level (k = 2.

Validation of the methodology for quantitative determination of arsenic in drinking water by hydride generation

International Nuclear Information System (INIS)

Silva Trejos, Paulina

2008-01-01

The analytical methodology was validated to quantitatively determine the arsenic in drinking water. The atomic absorption method for hydride generation was used. The percentage of recovery for the digestion of the samples was determined in a microwave oven with lots of HNO 3 , the results concluded that the optimal amount to 5,00 mL of sample was 0,50 mL with a recovery rate of 90,5 ±0, 5. The field of optimal linearity was 0-30 ppb with a correlation coefficient of 0,9994. The limits of detection and quantification limits according to Miller and Miller were 1,20 ± 0,02 and 4,01±0,02, respectively. The precision was evaluated by determining the repeatability and reproducibility, the results obtained were 0,34 and 0,30, respectively. The evaluation of the accuracy can report a -1,1 bias. The drinking water sample taken from the laboratory pipe showed As concentrations below the limits of quantification reported in this investigation. (author) [es

Automated lattice data generation

Science.gov (United States)

Ayyar, Venkitesh; Hackett, Daniel C.; Jay, William I.; Neil, Ethan T.

2018-03-01

The process of generating ensembles of gauge configurations (and measuring various observables over them) can be tedious and error-prone when done "by hand". In practice, most of this procedure can be automated with the use of a workflow manager. We discuss how this automation can be accomplished using Taxi, a minimal Python-based workflow manager built for generating lattice data. We present a case study demonstrating this technology.

Mechanisms of hydrogen induced delayed cracking in hydride forming materials

International Nuclear Information System (INIS)

Dutton, R.; Nuttall, K.; Puls, M.P.; Simpson, L.A.

1977-01-01

Mechanisms which have been formulated to describe delayed hydrogen cracking in hydride-forming metals are reviewed and discussed. Particular emphasis is placed on the commercial alloy Zr--2.5% Nb (Cb) which is extensively used in nuclear reactor core components. A quantitative model for hydrogen cracking in this material is presented and compared with available experimental data. The kinetics of crack propagation are controlled by the growth of hydrides at the stressed crack tip by the diffusive ingress of hydrogen into this region. The driving force for the diffusion flux is provided by the local stress gradient which interacts with both hydrogen atoms in solution and hydrogen atoms being dissolved and reprecipitated at the crack tip. The model is developed using concepts of elastoplastic fracture mechanics. Stage I crack growth is controlled by hydrides growing in the elastic stress gradient, while Stage II is controlled by hydride growth in the plastic zone at the crack tip. Recent experimental observations are presented which indicate that the process occurs in an intermittent fashion; hydride clusters accumulate at the crack tip followed by unstable crack advance and subsequent crack arrest in repeated cycles

Mechanisms of hydrogen induced delayed cracking in hydride forming materials

International Nuclear Information System (INIS)

Dutton, R.; Nuttall, K.; Puls, M.P.; Simpson, L.A.

1977-01-01

Mechanisms which have been formulated to describe delayed hydrogen cracking in hydride-forming metals are reviewed and discussed. Particular emphasis is placed on the commercial alloy Zr-2.5 pct Nb which is extensively used in nuclear reactor core components. A quantitative model for hydrogen cracking in this material is presented and compared with available experimental data. The kinetics of crack propagation are controlled by the growth of hydrides at the stressed crack tip by the diffusive ingress of hydrogen into this region. The driving force for the diffusion flux is provided by the local stress gradient which interacts with both hydrogen atoms in solution and hydrogen atoms being dissolved and reprecipitated at the crack tip. The model is developed using concepts of elastoplastic fracture mechanics. Stage I crack growth is controlled by hydrides growing in the elastic stress gradient, while Stage II is controlled by hydride growth in the plastic zone at the crack tip. Recent experimental observations are presented which indicate that the process occurs in an intermittent fashion; hydride clusters accumulate at the crack tip followed by unstable crack advance and subsequent crack arrest in repeated cycles. 55 refs., 6 figs

Rechargeable metal hydrides for spacecraft application

Science.gov (United States)

Perry, J. L.

1988-01-01

Storing hydrogen on board the Space Station presents both safety and logistics problems. Conventional storage using pressurized bottles requires large masses, pressures, and volumes to handle the hydrogen to be used in experiments in the U.S. Laboratory Module and residual hydrogen generated by the ECLSS. Rechargeable metal hydrides may be competitive with conventional storage techniques. The basic theory of hydride behavior is presented and the engineering properties of LaNi5 are discussed to gain a clear understanding of the potential of metal hydrides for handling spacecraft hydrogen resources. Applications to Space Station and the safety of metal hydrides are presented and compared to conventional hydride storage. This comparison indicates that metal hydrides may be safer and require lower pressures, less volume, and less mass to store an equivalent mass of hydrogen.

On-line pre-reduction of Se(VI) by thiourea for selenium speciation by hydride generation

Energy Technology Data Exchange (ETDEWEB)

Qiu Jianhua [Department of Chemistry and the MOE Key Laboratory of Analytical Sciences, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, Fujian 361005 (China); Wang Qiuquan [Department of Chemistry and the MOE Key Laboratory of Analytical Sciences, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, Fujian 361005 (China)]. E-mail: qqwang@xmu.edu.cn; Ma Yuning [Department of Chemistry and the MOE Key Laboratory of Analytical Sciences, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, Fujian 361005 (China); Yang Limin [Department of Chemistry and the MOE Key Laboratory of Analytical Sciences, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, Fujian 361005 (China); Huang Benli [Department of Chemistry and the MOE Key Laboratory of Analytical Sciences, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, Fujian 361005 (China)

2006-07-15

In this study, thiourea (TU) was novelly developed as a reduction reagent for on-line pre-reduction of selenium(VI) before conventional hydride generation (HG) by KBH{sub 4}/NaOH-HCl. After TU on-line pre-reduction, the HG efficiency of Se(VI) has been greatly improved and because even higher than that of the same amount of Se(IV) obtained in the conventional HG system. The possible pre-reduction mechanism is discussed. The detection limit (DL) of selenate reaches 10 pg mL{sup -1} when using on-line TU pre-reduction followed by HG atomic fluorescence detection. When TU pre-reduction followed by HG is used as an interface between ion-pair high performance liquid chromatography and atomic fluorescence spectrometry, selenocystine, selenomethionine, selenite and selenate can be measured simultaneously and quantitatively. The DLs of these are 0.06, 0.08, 0.05 and 0.04 ng mL{sup -1}, respectively, and the relative standard deviations of 9 duplicate runs for all the 4 species are less than 5%. Furthermore, it was successfully applied to Se speciation analysis of cultured garlic samples, and validated by determination of total selenium and selenium species in certified reference material NIST 1946.

Automated lattice data generation

Directory of Open Access Journals (Sweden)

Ayyar Venkitesh

2018-01-01

Full Text Available The process of generating ensembles of gauge configurations (and measuring various observables over them can be tedious and error-prone when done “by hand”. In practice, most of this procedure can be automated with the use of a workflow manager. We discuss how this automation can be accomplished using Taxi, a minimal Python-based workflow manager built for generating lattice data. We present a case study demonstrating this technology.

Experimental investigations of helium cryotrapping by argon frost

International Nuclear Information System (INIS)

Mack, A.; Perinic, D.; Murdoch, D.; Boissin, J.C.

1992-01-01

At the Karlsruhe Nuclear Research Centre (KfK) cryopumping techniques are being investigated by which the gaseous exhausts from the NET/ITER reactor can be pumped out during the burn-and dwell-times. Cryosorption and cryotrapping are techniques which are suitable for this task. It is the target of the investigations to test the techniques under NET/ITER conditions and to determine optimum design data for a prototype. They involve measurement of the pumping speed as a function of the gas composition, gas flow and loading condition of the pump surfaces. The following parameters are subjected to variations: Ar/He ratio, specific helium volume flow rate, cryosurface temperature, process gas composition, impurities in argon trapping gas, three-stage operation and two-stage operation. This paper is a description of the experiments on argon trapping techniques started in 1990. Eleven tests as well as the results derived from them are described

Hydride embrittlement in zircaloy components

Energy Technology Data Exchange (ETDEWEB)

Lobo, Raquel M.; Andrade, Arnaldo H.P.; Castagnet, Mariano, E-mail: rmlobo@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2011-07-01

Zirconium alloys are used in nuclear reactor cores under high-temperature water environment. During service, hydrogen is generated by corrosion processes, and it is readily absorbed by these materials. When hydrogen concentration exceeds the terminal solid solubility, the excess hydrogen precipitates as zirconium hydride (ZrH{sub 2}) platelets or needles. Zirconium alloys components can fail by hydride cracking if they contain large flaws and are highly stressed. Zirconium alloys are susceptible to a mechanism for crack initiation and propagation termed delayed hydride cracking (DHC). The presence of brittle hydrides, with a K{sub Ic} fracture toughness of only a few MPa{radical}m, results in a severe loss in ductility and toughness when platelet normal is oriented parallel to the applied stress. In plate or tubing, hydrides tend to form perpendicular to the thickness direction due to the texture developed during fabrication. Hydrides in this orientation do not generally cause structural problems because applied stresses in the through-thickness direction are very low. However, the high mobility of hydrogen in a zirconium lattice enables redistribution of hydrides normal to the applied stress direction, which can result in localized embrittlement. When a platelet reaches a critical length it ruptures. If the tensile stress is sufficiently great, crack initiation starts at some of these hydrides. Crack propagation occurs by repeating the same process at the crack tip. Delayed hydride cracking can degrade the structural integrity of zirconium alloys during reactor service. The paper focuses on the fracture mechanics and fractographic aspects of hydride material. (author)

Hydrogen storage in metallic hydrides: the hydrides of magnesium-nickel alloys

International Nuclear Information System (INIS)

Silva, E.P. da.

1981-01-01

The massive and common use of hydrogen as an energy carrier requires an adequate solution to the problem of storing it. High pressure or low temperatures are not entirely satisfactory, having each a limited range of applications. Reversible metal hydrides cover a range of applications intermediate to high pressure gas and low temperature liquid hydrogen, retaining very favorable safety and energy density characteristics, both for mobile and stationary applications. This work demonstrates the technical viability of storing hydrogen in metal hydrides of magnesium-nickel alloys. Also, it shows that technology, a product of science, can be generated within an academic environment, of the goal is clear, the demand outstanding and the means available. We review briefly theoretical models relating to metal hydride properties, specially the thermodynamics properties relevant to this work. We report our experimental results on hydrides of magnesium-nickel alloys of various compositions including data on structure, hydrogen storage capacities, reaction kinetics, pressure-composition isotherms. We selected a promising alloy for mass production, built and tested a modular storage tank based on the hydrides of the alloy, with a capacity for storing 10 Nm sup(3) of hydrogen of 1 atm and 20 sup(0)C. The tank weighs 46,3 Kg and has a volume of 21 l. (author)

Flow injection electrochemical hydride generation inductively coupled plasma time-of-flight mass spectrometry for the simultaneous determination of hydride forming elements and its application to the analysis of fresh water samples

International Nuclear Information System (INIS)

Bings, Nicolas H.; Stefanka, Zsolt; Mallada, Sergio Rodriguez

2003-01-01

A flow injection (FI) method was developed using electrochemical hydride generation (EcHG) as a sample introduction system, coupled to an inductively coupled plasma time-of-flight mass spectrometer (ICP-TOFMS) for rapid and simultaneous determination of six elements forming hydrides (As, Bi, Ge, Hg, Sb and Se). A novel low volume electrolysis cell, especially suited for FI experiments was designed and the conditions for simultaneous electrochemical hydride generation (EcHG; electrolyte concentrations and flow rates, electrolysis voltage and current) as well as the ICP-TOFMS operational parameters (carrier gas flow rate, modulation pulse width (MPW)) for the simultaneous determination of 12 isotopes were optimized. The compromise operation parameters of the electrolysis were found to be 1.4 and 3 ml min -1 for the anolyte and catholyte flow rates, respectively, using 2 M sulphuric acid. An optimum electrolysis current of 0.7 A (16 V) and an argon carrier gas flow rate of 0.91 l min -1 were chosen. A modulation pulse width of 5 μs, which influences the sensitivity through the amount of ions being collected by the MS per single analytical cycle, provided optimum results for the detection of transient signals. The achieved detection limits were compared with those obtained by using FI in combination with conventional nebulization (FI-ICP-TOFMS); values for chemical hydride generation (FI-CHG-ICP-TOFMS) were taken from the literature. By using a 200 μl sample loop absolute detection limits (3σ) in the range of 10-160 pg for As, Bi, Ge, Hg, Sb and 1.1 ng for Se and a precision of 4-8% for seven replicate injections of 20-100 ng ml -1 multielemental sample solutions were achieved. The analysis of a standard reference material (SRM) 1643d (NIST, 'Trace Elements in Water') showed good agreement with the certified values for As and Sb. Se showed a drastic difference, which is probably due to the presence of hydride-inactive Se species in the sample. Recoveries better than

Activated aluminum hydride hydrogen storage compositions and uses thereof

Science.gov (United States)

Sandrock, Gary; Reilly, James; Graetz, Jason; Wegrzyn, James E.

2010-11-23

In one aspect, the invention relates to activated aluminum hydride hydrogen storage compositions containing aluminum hydride in the presence of, or absence of, hydrogen desorption stimulants. The invention particularly relates to such compositions having one or more hydrogen desorption stimulants selected from metal hydrides and metal aluminum hydrides. In another aspect, the invention relates to methods for generating hydrogen from such hydrogen storage compositions.

Electrocatalytic hydride-forming compounds for rechageable batteries

NARCIS (Netherlands)

Notten, P.H.L.; Einerhand, R.E.F.

1991-01-01

Non-toxic intermetallic hydride-forming compounds are attractive alternatives to cadmium as the negative electrode materials in the new generation of Ni/metal hydride rechargeable batteries. High exchange currents and discharge efficiencies even at low temperatures can be achieved using highly

A comparative evaluation of different ionic liquids for arsenic species separation and determination in wine varietals by liquid chromatography - hydride generation atomic fluorescence spectrometry.

Science.gov (United States)

Castro Grijalba, Alexander; Fiorentini, Emiliano F; Martinez, Luis D; Wuilloud, Rodolfo G

2016-09-02

The application of different ionic liquids (ILs) as modifiers for chromatographic separation and determination of arsenite [As(III)], arsenate [As(V)], dimethylarsonic acid (DMA) and monomethylarsonic acid (MMA) species in wine samples, by reversed-phase high performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry detection (RP-HPLC-HG-AFS) was studied in this work. Several factors influencing the chromatographic separation of the As species, such as pH of the mobile phase, buffer solution concentration, buffer type, IL concentration and length of alkyl groups in ILs were evaluated. The complete separation of As species was achieved using a C18 column in isocratic mode with a mobile phase composed of 0.5% (v/v) 1-octyl-3-methylimidazolium chloride ([C8mim]Cl) and 5% (v/v) methanol at pH 8.5. A multivariate methodology was used to optimize the variables involved in AFS detection of As species after they were separated by HPLC. The ILs showed remarkable performance for the separation of As species, which was obtained within 18min with a resolution higher than 0.83. The limits of detection for As(III), As(V), MMA and DMA were 0.81, 0.89, 0.62 and 1.00μg As L(-1). The proposed method was applied for As speciation analysis in white and red wine samples originated from different grape varieties. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of inorganic arsenic in algae using bromine halogenation and on-line nonpolar solid phase extraction followed by hydride generation atomic fluorescence spectrometry.

Science.gov (United States)

Zhang, Weihong; Qi, Yuehan; Qin, Deyuan; Liu, Jixin; Mao, Xuefei; Chen, Guoying; Wei, Chao; Qian, Yongzhong

2017-08-01

Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and on-line nonpolar solid phase extraction (SPE) followed by hydride generation atomic fluorescence spectrometry (HG-AFS). The separation of iAs from algae was first performed by nonpolar SPE sorbent using Br - for arsenic halogenation. Algae samples were extracted with 1% perchloric acid. Then, 1.5mL extract was reduced by 1% thiourea, and simultaneously reacted (for 30min) with 50μL of 10% KBr for converting iAs to AsBr 3 after adding 3.5mL of 70% HCl to 5mL. A polystyrene (PS) resin cartridge was employed to retain arsenicals, which were hydrolyzed, eluted from the PS resin with H 2 O, and categorized as iAs. The total iAs was quantified by HG-AFS. Under optimum conditions, the spiked recoveries of iAs in real algae samples were in the 82-96% range, and the method achieved a desirable limit of detection of 3μgkg -1 . The inter-day relative standard deviations were 4.5% and 4.1% for spiked 100 and 500μgkg -1 respectively, which proved acceptable for this method. For real algae samples analysis, the highest presence of iAs was found in sargassum fusiforme, followed by kelp, seaweed and laver. Copyright © 2017 Elsevier B.V. All rights reserved.

The Production of Uranium Metal by Metal Hydrides Incorporated

Energy Technology Data Exchange (ETDEWEB)

Alexander, P. P.

1943-01-01

Metal Hydrides Incorporated was a pioneer in the production of uranium metal on a commercial scale and supplied it to all the laboratories interested in the original research, before other methods for its production were developed. Metal Hydrides Inc. supplied the major part of the metal for the construction of the first experimental pile which, on December 2, 1942, demonstrated the feasibility of the self-sustaining chain reaction and the release of atomic energy.

Investigations into the Role of Modifiers for Entrapment of Hydrides in Flow Injection Hydride Generation Electrothermal Atomic Absorption Spectrometry as Exemplified for the Determination of Germanium

DEFF Research Database (Denmark)

Hilligsøe, Bo; Andersen, Jens Enevold Thaulov; Hansen, Elo Harald

1997-01-01

Pd-conditioned graphite tubes, placed in the furnace of an atomic absorption spectrometry instrument, are used for entrapment of germane as generated in an associated flow injection system. Two different approaches are tested with the ultimate aim to allow multiple determinations, that is...

Automated drawing generation system

International Nuclear Information System (INIS)

Yoshinaga, Toshiaki; Kawahata, Junichi; Yoshida, Naoto; Ono, Satoru

1991-01-01

Since automated CAD drawing generation systems still require human intervention, improvements were focussed on an interactive processing section (data input and correcting operation) which necessitates a vast amount of work. As a result, human intervention was eliminated, the original objective of a computerized system. This is the first step taken towards complete automation. The effects of development and commercialization of the system are as described below. (1) The interactive processing time required for generating drawings was improved. It was determined that introduction of the CAD system has reduced the time required for generating drawings. (2) The difference in skills between workers preparing drawings has been eliminated and the quality of drawings has been made uniform. (3) The extent of knowledge and experience demanded of workers has been reduced. (author)

On-line solid phase extraction-gas chromatography-cryotrapping-infrared spectrometry for the trace-level determination of microcontaminants in aqueous samples

NARCIS (Netherlands)

Hankemeier, T; Hooijschuur, E.; Vreuls, R.J.J.; Brinkman, U.A.Th.; Visser, T.

1998-01-01

A large-volume on-column GC-cryotrapping-IR system was developed for injections of up to 100 μl of organic extracts. Considerable reduction of the solvent-and-water background and enhanced analyte detectability was achieved by using an open-split interface between the GC column and the IR detector

Effects of H-H interactions on the heat of H absorption by β and delta Zr hydrides

International Nuclear Information System (INIS)

Ohta, Yutaka; Mabuchi, Mahito; Naito, Shizuo; Hashino, Tomoyasu

1987-01-01

The heat of H absorption by β and delta Zr hydrides has been measured by isoperibol calorimetry over the range of H concentration 0.1 - 1.6 H/Zr at temperatures 873-1273 K. In the β hydride the heat per H atom (differential heat) increases and then decreases as the H concentration increases. In the delta hydride only a decrease at large H concentrations is clearly observed. The increase in the β hydride is related by self-consistent calculations to a pair indirect interaction between H atoms; the decreases in the β and delta hydrides are due to a pair direct interaction which is of the form of a screened Coulomb potential. The differential heat is estimated from the pair indirect and direct interactions by the use of Monte Carlo simulations and compared with the measured differential heat. (author)

Automated Liquibase Generator And ValidatorALGV

Directory of Open Access Journals (Sweden)

Manik Jain

2015-08-01

Full Text Available Abstract This paper presents an automation tool namely ALGV Automated Liquibase Generator and Validator for the automated generation and verification of liquibase scripts. Liquibase is one of the most efficient ways of applying and persisting changes to a database schema. Since its invention by Nathan Voxland 1 it has become de facto standard for database change management. The advantages of using liquibase scripts over traditional sql queries ranges from version control to reusing the same scripts over multiple database platforms. Irrespective of its advantages manual creation of liquibase scripts takes a lot of effort and sometimes is error-prone. ALGV helps to reduce the time consuming liquibase script generation manual typing efforts possible error occurrence and manual verification process and time by 75. Automating the liquibase generation process also helps to remove the burden of recollecting specific tags to be used for a particular change. Moreover developers can concentrate on the business logic and business data rather than wasting their precious efforts in writing files.

The atomic structure of protons and hydrides in Sm1.92Ca0.08Sn2O7-δ pyrochlore from DFT calculations and FTIR spectroscopy

DEFF Research Database (Denmark)

Bork, Nicolai Christian; Eurenius, K. E. J.; Rossmeisl, Jan

2012-01-01

A combined density functional theory and Fourier transform infrared spectroscopy study of the structure and specific site preference of protons and hydrides in the pyrochlore Sm1.92Ca0.08Sn2O7-δ is presented. Two protonic sites of particular high stability are identified, both located on O(1......) oxygen atoms closely associated with a Ca dopant. Further, the unexpected presence of Ho hydride defects in undoped, oxygen deficient Sm2Sn2O7 is reported. Finally, the stretching frequencies and relative intensities for these and other sites are calculated. The main features of the Fourier transform...

Reactivity patterns of transition metal hydrides and alkyls

International Nuclear Information System (INIS)

Jones, W.D. II.

1979-05-01

The complex PPN + CpV(CO) 3 H - (Cp=eta 5 -C 5 H 5 and PPN = (Ph 3 P) 2 ) was prepared in 70% yield and its physical properties and chemical reactions investigated. PPN + CpV(CO) 3 H - reacts with a wide range of organic halides. The organometallic products of these reactions are the vanadium halides PPN + [CpV(C) 3 X] - and in some cases the binuclear bridging hydride PPN + [CpV(CO) 3 ] 2 H - . The borohydride salt PPN + [CpV(CO) 3 BH 4 ] - has also been prepared. The reaction between CpV(CO) 3 H - and organic halides was investigated and compared with halide reductions carried out using tri-n-butyltin hydride. Results demonstrate that in almost all cases, the reduction reaction proceeds via free radical intermediates which are generated in a chain process, and are trapped by hydrogen transfer from CpV(CO) 3 H - . Sodium amalgam reduction of CpRh(CO) 2 or a mixture of CpRh(CO) 2 and CpCo(CO) 2 affords two new anions, PPN + [Cp 2 Rh 3 (CO) 4 ] - and PPN + [Cp 2 RhCo(CO) 2 ] - . CpMo(CO) 3 H reacts with CpMo(CO) 3 R (R=CH 3 ,C 2 H 5 , CH 2 C 6 H 5 ) at 25 to 50 0 C to produce aldehyde RCHO and the dimers [CpMo(CO) 3 ] 2 and [CpMo(CO) 2 ] 2 . In general, CpV(CO) 3 H - appears to transfer a hydrogen atom to the metal radical anion formed in an electron transfer process, whereas CpMo(CO) 3 H transfers hydride in a 2-electron process to a vacant coordination site. The chemical consequences are that CpV(CO) 3 H - generally reacts with metal alkyls to give alkanes via intermediate alkyl hydride species whereas CpMo(CO) 3 H reacts with metal alkyls to produce aldehyde, via an intermediate acyl hydride species

Speciation without chromatography using selective hydride generation: Inorganic arsenic in rice and samples of marine origin

Czech Academy of Sciences Publication Activity Database

Musil, Stanislav; Pétursdóttir, A. H.; Raab, A.; Gunnlaugsdóttir, H.; Krupp, E.; Feldmann, J.

2014-01-01

Roč. 86, č. 2 (2014), s. 993-999 ISSN 0003-2700 Grant - others:GA AV ČR(CZ) M200311271 Institutional support: RVO:68081715 Keywords : inorganic arsenic * hydride generation * inductively coupled plasma mass spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

[Cloud Point extraction for determination of mercury in Chinese herbal medicine by hydride generation atomic fluorescence spectrometry with optimization using Box-Behnken design].

Science.gov (United States)

Wang, Mei; Li, Shan; Zhou, Jian-dong; Xu, Ying; Long, Jun-biao; Yang, Bing-yi

2014-08-01

Cloud point extraction (CPE) is proposed as a pre-concentration procedure for the determination of Hg in Chinese herbal medicine samples by hydride generation-atomic fluorescence spectrometry (HG-AFS). Hg2+ was reacted with dithizone to form hydrophobic chelate under the condition of pH. Using Triton X-114, as surfactant, chelate was quantitatively extracted into small volume of the surfactant-rich phase by heating the solution in a water bath for 15 min and centrifuging. Four variables including pH, dithizone concentration, Triton X-114 concentration and equilibrium temperature (T) showed the significant effect on extraction efficiency of total Hg evaluated by single-factor experiment, and Box-Behnken design and response surface method- ology were adopted to further investigate the mutual interactions between these variables and to identify their optimal values that would generate maximum extraction efficiency. The results showed that the binomial was used to fit the response to experimental levels of each variable. ALL linear, quadratic terms of four variables, and interactions between pH and Trion X-114, pH and di- thizone affected the response value(extraction efficiency) significantly at 5% level. The optimum extraction conditions were as follows: pH 5.1, Triton X-114 concentration of 1.16 g x L(-1), dithizone concentration of 4.87 mol x L(-1), and T 58.2 degrees C, the predicted value of fluorescence was 4528.74 under the optimum conditions, and the experimental value had only 2.1% difference with it. Under the conditions, fluorescence was linear to mercury concentration in the range of 1-5 microg x L(-1). The limit of detection obtained was 0.01247 microg x L(-1) with the relative standard deviations (R.S.D.) for six replicate determinations of 1.30%. The proposed method was successfully applied to determination of Hg in morindae Radix, Andrographitis and dried tangerine samples with the recoveries of 95.0%-100.0%. Apparently Box-Behnken design combined with

Simultaneous determination of hydride and non-hydride forming elements by inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Benzo, Z. [Instituto Venezolano de Investigaciones Cientificas, IVIC, Altos de Pipe, Caracas (Venezuela, Bolivarian Republic of); Matos-Reyes, M.N.; Cervera, M.L.; Guardia, M. de la, E-mail: m.luisa.cervera@uv.es [Department of Analytical Chemistry, University of Valencia, Valencia (Spain)

2011-09-15

The operating characteristics of a dual nebulization system were studied including instrumental and chemical conditions for the hydride generation and analytical figures of merit for both, hydride and non hydride forming elements. Analytical performance of the nebulization system was characterized by detection limits from 0.002 to 0.0026 {mu}g mL{sup -1} for the hydride forming elements and between 0.0034 and 0.0121 {mu}g mL{sup -1} for the non-hydride forming elements, relative standard deviation for 10 replicate measurements at 0.25 mg L{sup -1} level and recovery percentages between 97 and 103%. The feasibility of the system was demonstrated in the simultaneous determination of Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Zn, As, Bi, Sb, Se, and Te in the NIST 1549 (non-fat milk powder), NIST 1570a (spinach leaves), DORM-2 (dogfish muscle) and TORT-2 (lobster hepatopancreas) certified samples for trace elements. Results found were in good agreement with the certified ones. (author)

Electrolytic hydriding and hydride distribution in zircaloy-4

International Nuclear Information System (INIS)

Gomes, M.H.L.

1974-01-01

A study has been made of the electrolytic hydriding of zircaloy-4 in the range 20-80 0 C, for reaction times from 5 to 30 hours, and the effect of potential, pH and dissolved oxygen has been investigated. The hydriding reaction was more sensitive to time and temperature conditions than to the electrochemical variables. It has been shown that a controlled introduction of hydrides in zircaloy is feasible. Hydrides were found to be plate like shaped and distributed mainly along grain-boundaries. It has been shown that hydriding kinetics do not follow a simple law but may be described by a Johnson-Mehl empirical equation. On the basis of this equation an activation energy of 9.400 cal/mol has been determined, which is close to the activation energy for diffusion of hydrogen in the hydride. (author)

Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

International Nuclear Information System (INIS)

Sigrist, Mirna; Albertengo, Antonela; Beldomenico, Horacio; Tudino, Mabel

2011-01-01

A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH 3 generation using 3.5 mol L -1 HCl as carrier solution and 0.35% (m/v) NaBH 4 in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl - , SO 4 2- , NO 3 - , HPO 4 2- , HCO 3 - on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C 6 H 8 O 6 solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 μg L -1 and 0.6 μg L -1 for As(III) and inorganic total As, respectively, were obtained for a 500 μL sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h -1 . The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species separation was performed through the employ of a serial connection of membrane filters and

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

OpenAIRE

2011-01-01

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

Cryotrapping assisted mass spectrometry for the analysis of complex gas mixtures

International Nuclear Information System (INIS)

Ferreira, Jose A.; Tabares, Francisco L.

2007-01-01

A simple method is described for the unambiguous identification of the individual components in a gas mixture showing strong overlapping of their mass spectrometric cracking patterns. The method, herein referred to as cryotrapping assisted mass spectrometry, takes advantage of the different vapor pressure values of the individual components at low temperature (78 K for liquid nitrogen traps), and thus of the different depletion efficiencies and outgassing patterns during the fast cooling and slow warming up of the trap, respectively. Examples of the use of this technique for gas mixtures with application to plasma enhanced chemical vapor deposition of carbon and carbon-nitrogen hard films are shown. Detection of traces of specific C 3 hydrocarbons ( 2 containing deposition plasmas are addressed as representative examples of specific applications of the technique

Sodium-based hydrides for thermal energy applications

Science.gov (United States)

Sheppard, D. A.; Humphries, T. D.; Buckley, C. E.

2016-04-01

Concentrating solar-thermal power (CSP) with thermal energy storage (TES) represents an attractive alternative to conventional fossil fuels for base-load power generation. Sodium alanate (NaAlH4) is a well-known sodium-based complex metal hydride but, more recently, high-temperature sodium-based complex metal hydrides have been considered for TES. This review considers the current state of the art for NaH, NaMgH3- x F x , Na-based transition metal hydrides, NaBH4 and Na3AlH6 for TES and heat pumping applications. These metal hydrides have a number of advantages over other classes of heat storage materials such as high thermal energy storage capacity, low volume, relatively low cost and a wide range of operating temperatures (100 °C to more than 650 °C). Potential safety issues associated with the use of high-temperature sodium-based hydrides are also addressed.

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%

The new concept of hyphenated analytical system: Simultaneous determination of inorganic arsenic(III), arsenic(V), selenium(IV) and selenium(VI) by high performance liquid chromatography-hydride generation-(fast sequential) atomic absorption spectrometry during single analysis

International Nuclear Information System (INIS)

Niedzielski, P.

2005-01-01

The paper presents a new conception of determination of inorganic speciation forms of arsenic: As(III) and As(V) as well selenium Se(IV) and Se(VI) by means of the high performance liquid chromatography hyphenated with a detection by the atomic absorption spectrometry with hydride generation (HPLC-HG-AAS). The application of optimization procedure conditions of chromatographic separation of arsenic and selenium speciation forms (using anion-exchange Supelco LC-SAX1 column and phosphate buffer at pH 5.40 as a mobile phase) as well as the use of the atomic absorption spectrometry as a detector, which enables work in fast sequential mode, allowed to develop original detection methodology of simultaneous determination of arsenic As(III), As(V) and selenium Se(IV) and Se(VI) speciation forms within a 220 s single analysis. The obtained detection limits were 7.8 ng mL -1 for As(III); 12.0 ng mL -1 for As(V); 2.4 ng mL -1 for Se(IV) and 18.6 ng mL -1 for Se(VI) and precision 10.5%, 12.1%, 14.2% and 17.3%, respectively, for 100 ng mL -1 . The described method was used for ground water analysis

Hydrogen storage in the form of metal hydrides

Science.gov (United States)

Zwanziger, M. G.; Santana, C. C.; Santos, S. C.

1984-01-01

Reversible reactions between hydrogen and such materials as iron/titanium and magnesium/ nickel alloy may provide a means for storing hydrogen fuel. A demonstration model of an iron/titanium hydride storage bed is described. Hydrogen from the hydride storage bed powers a converted gasoline electric generator.

Preferred hydride growth orientations on oxide-coated gadolinium surfaces

International Nuclear Information System (INIS)

Benamar, G.M.; Schweke, D.; Kimmel, G.; Mintz, M.H.

2012-01-01

Highlights: ► The preferred hydride growth orientations on gadolinium metal coated by a thin oxide layer are presented. ► A preferred growth of the (1 0 0) h plane of the face centered cubic (FCC) GdH 2 is observed for the hydride spots forming below the oxidation layer. ► A change to the (1 1 1) h plane of the cubic hydride dominates for the hydride's Growth Centers. ► The texture change is attributed to the surface normal compressive stress component exerted by the oxidation layer on the developing hydride. - Abstract: The initial development of hydrides on polycrystalline gadolinium (Gd), as on some other hydride forming metals, is characterized by two sequential steps. The first step involves the rapid formation of a dense pattern of small hydride spots (referred to as the “small family” of hydrides) below the native oxidation layer. The second stage takes place when some of the “small family” nucleants (referred to as “growth centers”, GCs) break the oxide layer, leading to their rapid growth and finally to the massive hydriding of the sample. In the present study, the texture of the two hydride families was studied, by combining X-ray diffraction (XRD) analysis with a microscopic analysis of the hydride, using scanning electron microscopy (SEM) and atomic force microscopy (AFM). It has been observed that for the “small family”, a preferred growth of the (1 0 0) h plane of the cubic GdH 2 takes place, whereas for the GCs, a change to the (1 1 1) h plane of the cubic hydride dominates. These preferred growth orientations were analyzed by their structure relation with the (0 0 .1) m basal plane of the Gd metal. It has been concluded that the above texture change is due to the surface normal compressive stress component exerted by the oxidation overlayer on the developing hydride, preventing the (0 0 .1) m ||(1 1 1) h growth orientation. This stress is relieved upon the rupture of that overlayer and the development of the GCs, leading to

Automated Test Case Generation

CERN Multimedia

CERN. Geneva

2015-01-01

I would like to present the concept of automated test case generation. I work on it as part of my PhD and I think it would be interesting also for other people. It is also the topic of a workshop paper that I am introducing in Paris. (abstract below) Please note that the talk itself would be more general and not about the specifics of my PhD, but about the broad field of Automated Test Case Generation. I would introduce the main approaches (combinatorial testing, symbolic execution, adaptive random testing) and their advantages and problems. (oracle problem, combinatorial explosion, ...) Abstract of the paper: Over the last decade code-based test case generation techniques such as combinatorial testing or dynamic symbolic execution have seen growing research popularity. Most algorithms and tool implementations are based on finding assignments for input parameter values in order to maximise the execution branch coverage. Only few of them consider dependencies from outside the Code Under Test’s scope such...

PAC and μSr investigations of light interstitial diffusion in intermetallic hydrides

International Nuclear Information System (INIS)

Boyer, P.; Baudry, A.

1988-01-01

Specific aspects of the Perturbed Angular Correlation (PAC) of gamma rays concerning its application to the study of atomic diffusion in solids are presented. PAC results recently obtained on the 181 Ta probe in several crystalline and amorphous phases of Zr 2 Ni hydrides are briefly summarized. Preliminary μSR results relative to these intermetallic hydrides are presented and compared to the PAC data

Influence of uranium hydride oxidation on uranium metal behaviour

International Nuclear Information System (INIS)

Patel, N.; Hambley, D.; Clarke, S.A.; Simpson, K.

2013-01-01

This work addresses concerns that the rapid, exothermic oxidation of active uranium hydride in air could stimulate an exothermic reaction (burning) involving any adjacent uranium metal, so as to increase the potential hazard arising from a hydride reaction. The effect of the thermal reaction of active uranium hydride, especially in contact with uranium metal, does not increase in proportion with hydride mass, particularly when considering large quantities of hydride. Whether uranium metal continues to burn in the long term is a function of the uranium metal and its surroundings. The source of the initial heat input to the uranium, if sufficient to cause ignition, is not important. Sustained burning of uranium requires the rate of heat generation to be sufficient to offset the total rate of heat loss so as to maintain an elevated temperature. For dense uranium, this is very difficult to achieve in naturally occurring circumstances. Areas of the uranium surface can lose heat but not generate heat. Heat can be lost by conduction, through contact with other materials, and by convection and radiation, e.g. from areas where the uranium surface is covered with a layer of oxidised material, such as burned-out hydride or from fuel cladding. These rates of heat loss are highly significant in relation to the rate of heat generation by sustained oxidation of uranium in air. Finite volume modelling has been used to examine the behaviour of a magnesium-clad uranium metal fuel element within a bottle surrounded by other un-bottled fuel elements. In the event that the bottle is breached, suddenly, in air, it can be concluded that the bulk uranium metal oxidation reaction will not reach a self-sustaining level and the mass of uranium oxidised will likely to be small in relation to mass of uranium hydride oxidised. (authors)

Influence of uranium hydride oxidation on uranium metal behaviour

Energy Technology Data Exchange (ETDEWEB)

Patel, N.; Hambley, D. [National Nuclear Laboratory (United Kingdom); Clarke, S.A. [Sellafield Ltd (United Kingdom); Simpson, K.

2013-07-01

This work addresses concerns that the rapid, exothermic oxidation of active uranium hydride in air could stimulate an exothermic reaction (burning) involving any adjacent uranium metal, so as to increase the potential hazard arising from a hydride reaction. The effect of the thermal reaction of active uranium hydride, especially in contact with uranium metal, does not increase in proportion with hydride mass, particularly when considering large quantities of hydride. Whether uranium metal continues to burn in the long term is a function of the uranium metal and its surroundings. The source of the initial heat input to the uranium, if sufficient to cause ignition, is not important. Sustained burning of uranium requires the rate of heat generation to be sufficient to offset the total rate of heat loss so as to maintain an elevated temperature. For dense uranium, this is very difficult to achieve in naturally occurring circumstances. Areas of the uranium surface can lose heat but not generate heat. Heat can be lost by conduction, through contact with other materials, and by convection and radiation, e.g. from areas where the uranium surface is covered with a layer of oxidised material, such as burned-out hydride or from fuel cladding. These rates of heat loss are highly significant in relation to the rate of heat generation by sustained oxidation of uranium in air. Finite volume modelling has been used to examine the behaviour of a magnesium-clad uranium metal fuel element within a bottle surrounded by other un-bottled fuel elements. In the event that the bottle is breached, suddenly, in air, it can be concluded that the bulk uranium metal oxidation reaction will not reach a self-sustaining level and the mass of uranium oxidised will likely to be small in relation to mass of uranium hydride oxidised. (authors)

Development of transmutation technologies of radioactive waste by actinoid hydride

International Nuclear Information System (INIS)

Konashi, Kenji; Matsui, Hideki; Yamawaki, Michio

2001-01-01

Two waste treatment methods, geological disposal and transmutation, have been studied. The transmutation method changes long-lived radioactive nuclides to short-lived one or stabilizes them by nuclear transformation. The transmutation by actinoid hydride is exactly alike that transformation method from actinoid disposal waste to Pu fuel. For this object, OMEGA project is processing now. The transmutation is difficult by two causes such as large amount of long-lived radioactive nuclides and not enough development of control technologies of nuclear reaction except atomic reactor. The transmutation using actinoid hydride has merits that the amount of actinoid charged in the target increases and the effect of thermal neutrons on fuel decreases depending on homogeneous transmutation velocity in the target. Development of stable actinoid hydride under the conditions of reactor temperature and irradiation environment is important. The experimental results of U-ZrH 1.6 are shown in this paper. The irradiation experiment using Th hydride has been proceeding. (S.Y.)

On-line pre-reduction of pentavalent arsenicals by thioglycolic acid for speciation analysis by selective hydride generation-cryotrapping-atomic absorption spectrometry

Czech Academy of Sciences Publication Activity Database

Musil, Stanislav; Matoušek, Tomáš

2008-01-01

Roč. 63, č. 6 (2008), s. 685-691 ISSN 0584-8547 R&D Projects: GA AV ČR IAA400310507 Grant - others:NIH-FIRCA(US) 1 R03 TW007057-01 Institutional research plan: CEZ:AV0Z40310501 Keywords : HG-AAS * methylated arsenic species * on-line pre-reduction Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.853, year: 2008

Determination of lead by hydride generation inductively coupled plasma mass spectrometry (HG-ICP-MS): On-line generation of plumbane using potassium hexacyanomanganate(III)

Energy Technology Data Exchange (ETDEWEB)

Yilmaz, Vedat [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States); Erciyes University, Faculty of Pharmacy, Department of Analytical Chemistry, 38039 Kayseri (Turkey); Arslan, Zikri, E-mail: zikri.arslan@jsums.edu [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States); Rose, LaKeysha [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States)

2013-01-25

Highlights: Black-Right-Pointing-Pointer Potassium hexacyanomanganate(III), (K{sub 3}Mn(CN){sub 6}, was utilized first time for hydride generation (HG). Black-Right-Pointing-Pointer Hexacyanomanganate(III) promoted generation of lead hydride (PbH{sub 4}) remarkably. Black-Right-Pointing-Pointer The HG method using K{sub 3}Mn(CN){sub 6} enhanced sensitivity by at least 40-fold. Black-Right-Pointing-Pointer The method detection limits for Pb were as low as 8 ng L{sup -1} by ICP-MS. Black-Right-Pointing-Pointer The method is highly suitable for quantitative determination of Pb in various samples and salt matrices by ICP-MS. - Abstract: A hydride generation (HG) procedure has been described for determination of Pb by ICP-MS using potassium hexacyanomanganate(III), K{sub 3}Mn(CN){sub 6}, as an additive to facilitate the generation of plumbane (PbH{sub 4}). Potassium hexacyanomanganate(III) was prepared in acidic medium as it was unstable in water. The stability of hexacyanomanganate(III) was examined in dilute solutions of HCl, HNO{sub 3} and H{sub 2}SO{sub 4}. The solutions prepared in 1% v/v H{sub 2}SO{sub 4} were found to be stable for over a period of 24 h. The least suitable medium was 1% v/v HNO{sub 3}. For generation of plumbane, acidic hexacyanomanganate(III) and sample solutions were mixed on-line along a 5-cm long tygon tubing (1.14 mm i.d.) and then reacted with 2% m/v sodium borohydride (NaBH{sub 4}). A concentration of 0.5% m/v K{sub 3}Mn(CN){sub 6} facilitated the generation of PbH{sub 4} remarkably. In comparison to H{sub 2}SO{sub 4}, HCl provided broader working range for which optimum concentration was 1% v/v. No significant interferences were noted from transition metals and hydride forming elements, up to 0.5 {mu}g mL{sup -1} levels, except Cu which depressed the signals severely. The depressive effects in the presence of 0.1 {mu}g mL{sup -1} Cu were alleviated by increasing the concentration of K{sub 3}Mn(CN){sub 6} to 2% m/v. Under these conditions

"First generation" automated DNA sequencing technology.

Science.gov (United States)

Slatko, Barton E; Kieleczawa, Jan; Ju, Jingyue; Gardner, Andrew F; Hendrickson, Cynthia L; Ausubel, Frederick M

2011-10-01

Beginning in the 1980s, automation of DNA sequencing has greatly increased throughput, reduced costs, and enabled large projects to be completed more easily. The development of automation technology paralleled the development of other aspects of DNA sequencing: better enzymes and chemistry, separation and imaging technology, sequencing protocols, robotics, and computational advancements (including base-calling algorithms with quality scores, database developments, and sequence analysis programs). Despite the emergence of high-throughput sequencing platforms, automated Sanger sequencing technology remains useful for many applications. This unit provides background and a description of the "First-Generation" automated DNA sequencing technology. It also includes protocols for using the current Applied Biosystems (ABI) automated DNA sequencing machines. © 2011 by John Wiley & Sons, Inc.

Modelling zirconium hydrides using the special quasirandom structure approach

KAUST Repository

Wang, Hao; Chroneos, Alexander I.; Jiang, Chao; Schwingenschlö gl, Udo

2013-01-01

The study of the structure and properties of zirconium hydrides is important for understanding the embrittlement of zirconium alloys used as cladding in light water nuclear reactors. Simulation of the defect processes is complicated due to the random distribution of the hydrogen atoms. We propose the use of the special quasirandom structure approach as a computationally efficient way to describe this random distribution. We have generated six special quasirandom structure cells based on face centered cubic and face centered tetragonal unit cells to describe ZrH2-x (x = 0.25-0.5). Using density functional theory calculations we investigate the mechanical properties, stability, and electronic structure of the alloys. © the Owner Societies 2013.

Decomposition kinetics of plutonium hydride

Energy Technology Data Exchange (ETDEWEB)

Haschke, J.M.; Stakebake, J.L.

1979-01-01

Kinetic data for decomposition of PuH/sub 1/ /sub 95/ provides insight into a possible mechanism for the hydriding and dehydriding reactions of plutonium. The fact that the rate of the hydriding reaction, K/sub H/, is proportional to P/sup 1/2/ and the rate of the dehydriding process, K/sub D/, is inversely proportional to P/sup 1/2/ suggests that the forward and reverse reactions proceed by opposite paths of the same mechanism. The P/sup 1/2/ dependence of hydrogen solubility in metals is characteristic of the dissociative absorption of hydrogen; i.e., the reactive species is atomic hydrogen. It is reasonable to assume that the rates of the forward and reverse reactions are controlled by the surface concentration of atomic hydrogen, (H/sub s/), that K/sub H/ = c'(H/sub s/), and that K/sub D/ = c/(H/sub s/), where c' and c are proportionality constants. For this surface model, the pressure dependence of K/sub D/ is related to (H/sub s/) by the reaction (H/sub s/) reversible 1/2H/sub 2/(g) and by its equilibrium constant K/sub e/ = (H/sub 2/)/sup 1/2//(H/sub s/). In the pressure range of ideal gas behavior, (H/sub s/) = K/sub e//sup -1/(RT)/sup -1/2/ and the decomposition rate is given by K/sub D/ = cK/sub e/(RT)/sup -1/2/P/sup 1/2/. For an analogous treatment of the hydriding process with this model, it can be readily shown that K/sub H/ = c'K/sub e//sup -1/(RT)/sup -1/2/P/sup 1/2/. The inverse pressure dependence and direct temperature dependence of the decomposition rate are correctly predicted by this mechanism which is most consistent with the observed behavior of the Pu--H system.

Advanced chemical hydride-based hydrogen generation/storage system for fuel cell vehicles

Energy Technology Data Exchange (ETDEWEB)

Breault, R.W.; Rolfe, J. [Thermo Power Corp., Waltham, MA (United States)

1998-08-01

Because of the inherent advantages of high efficiency, environmental acceptability, and high modularity, fuel cells are potentially attractive power supplies. Worldwide concerns over clean environments have revitalized research efforts on developing fuel cell vehicles (FCV). As a result of intensive research efforts, most of the subsystem technology for FCV`s are currently well established. These include: high power density PEM fuel cells, control systems, thermal management technology, and secondary power sources for hybrid operation. For mobile applications, however, supply of hydrogen or fuel for fuel cell operation poses a significant logistic problem. To supply high purity hydrogen for FCV operation, Thermo Power`s Advanced Technology Group is developing an advanced hydrogen storage technology. In this approach, a metal hydride/organic slurry is used as the hydrogen carrier and storage media. At the point of use, high purity hydrogen will be produced by reacting the metal hydride/organic slurry with water. In addition, Thermo Power has conceived the paths for recovery and regeneration of the spent hydride (practically metal hydroxide). The fluid-like nature of the spent hydride/organic slurry will provide a unique opportunity for pumping, transporting, and storing these materials. The final product of the program will be a user-friendly and relatively high energy storage density hydrogen supply system for fuel cell operation. In addition, the spent hydride can relatively easily be collected at the pumping station and regenerated utilizing renewable sources, such as biomass, natural, or coal, at the central processing plants. Therefore, the entire process will be economically favorable and environmentally friendly.

Chemical generation of iodine atoms

Energy Technology Data Exchange (ETDEWEB)

Hewett, Kevin B. [Directed Energy Directorate, Air Force Research Laboratory, 3550 Aberdeen Avenue SE, Kirtland AFB, NM 87117-5776 (United States)]. E-mail: kevin.hewett@kirtland.af.mil; Hager, Gordon D. [Directed Energy Directorate, Air Force Research Laboratory, 3550 Aberdeen Avenue SE, Kirtland AFB, NM 87117-5776 (United States); Crowell, Peter G. [Northrup Grumman Information Technology, Science and Technology Operating Unit, Advanced Technology Division, P.O. Box 9377, Albuquerque, NM 87119-9377 (United States)

2005-01-10

The chemical generation of atomic iodine using a chemical combustor to generate the atomic fluorine intermediate, from the reaction of F{sub 2} + H{sub 2}, followed by the production of atomic iodine, from the reaction of F + HI, was investigated. The maximum conversion efficiency of HI into atomic iodine was observed to be approximately 75%, which is in good agreement with the theoretical model. The conversion efficiency is limited by the formation of iodine monofluoride at the walls of the combustor where the gas phase temperature is insufficient to dissociate the IF.

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

International Nuclear Information System (INIS)

Dedina, Jiri

2007-01-01

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

Metal Hydride assited contamination on Ru/Si surfaces

NARCIS (Netherlands)

Pachecka, Malgorzata; Lee, Christopher James; Sturm, Jacobus Marinus; Bijkerk, Frederik

2013-01-01

In extreme ultraviolet lithography (EUVL) residual tin, in the form of particles, ions, and atoms, can be deposited on nearby EUV optics. During the EUV pulse, a reactive hydrogen plasma is formed, which may be able to react with metal contaminants, creating volatile and unstable metal hydrides that

Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Sigrist, Mirna, E-mail: msigrist@fiq.unl.edu.ar [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Albertengo, Antonela; Beldomenico, Horacio [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Tudino, Mabel [Laboratorio de Analisis de Trazas, Departamento de Quimica Inorganica, Analitica y Quimica Fisica/INQUIMAE, Facultad de Ciencias Exactas y Naturales, Pabellon II, Ciudad Universitaria (1428), Buenos Aires (Argentina)

2011-04-15

A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH{sub 3} generation using 3.5 mol L{sup -1} HCl as carrier solution and 0.35% (m/v) NaBH{sub 4} in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl{sup -}, SO{sub 4}{sup 2-}, NO{sub 3}{sup -}, HPO{sub 4}{sup 2-}, HCO{sub 3}{sup -} on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C{sub 6}H{sub 8}O{sub 6} solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 {mu}g L{sup -1} and 0.6 {mu}g L{sup -1} for As(III) and inorganic total As, respectively, were obtained for a 500 {mu}L sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h{sup -1}. The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species

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.

Mechanochemical synthesis of nanostructured chemical hydrides in hydrogen alloying mills

International Nuclear Information System (INIS)

Wronski, Z.; Varin, R.A.; Chiu, C.; Czujko, T.; Calka, A.

2007-01-01

Mechanical alloying of magnesium metal powders with hydrogen in specialized hydrogen ball mills can be used as a direct route for mechanochemical synthesis of emerging chemical hydrides and hydride mixtures for advanced solid-state hydrogen storage. In the 2Mg-Fe system, we have successfully synthesized the ternary complex hydride Mg 2 FeH 6 in a mixture with nanometric Fe particles. The mixture of complex magnesium-iron hydride and nano-iron released 3-4 wt.%H 2 in a thermally programmed desorption experiment at the range 285-295 o C. Milling of the Mg-2Al powder mixture revealed a strong competition between formation of the Al(Mg) solid solution and the β-MgH 2 hydride. The former decomposes upon longer milling as the Mg atoms react with hydrogen to form the hydride phase, and drive the Al out of the solid solution. The mixture of magnesium dihydride and nano-aluminum released 2.1 wt.%H 2 in the temperature range 329-340 o C in the differential scanning calorimetry experiment. The formation of MgH 2 was suppressed in the Mg-B system; instead, a hydrogenated amorphous phase (Mg,B)H x , was formed in a mixture with nanometric MgB 2 . Annealing of the hydrogen-stabilized amorphous mixture produced crystalline MgB 2

Hydride generation ICP-MS as a simple method for determination of inorganic arsenic in rice for routine biomonitoring

Czech Academy of Sciences Publication Activity Database

Pétursdóttir, Á. H.; Friedrich, N.; Musil, Stanislav; Raab, A.; Gunnlaugsdóttir, H.; Krupp, E. M.; Feldmann, J.

2014-01-01

Roč. 6, č. 14 (2014), s. 5392-5396 ISSN 1759-9660 Grant - others:GA AV ČR(CZ) M200311271 Institutional support: RVO:68081715 Keywords : inorganic arsenic * hydride generation inductively coupled plasma mass spectrometry * rice samples Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 1.821, year: 2014

Pulsed laser deposition of air-sensitive hydride epitaxial thin films: LiH

Energy Technology Data Exchange (ETDEWEB)

Oguchi, Hiroyuki, E-mail: oguchi@nanosys.mech.tohoku.ac.jp [Department of Nanomechanics, Tohoku University, Sendai 980-8579 (Japan); Micro System Integration Center (muSIC), Tohoku University, Sendai 980-0845 (Japan); Isobe, Shigehito [Creative Research Institution, Hokkaido University, Sapporo 001-0021 (Japan); Graduate School of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Kuwano, Hiroki [Department of Nanomechanics, Tohoku University, Sendai 980-8579 (Japan); Shiraki, Susumu; Hitosugi, Taro [Advanced Institute for Materials Research (AIMR), Tohoku University, Sendai 980-8577 (Japan); Orimo, Shin-ichi [Advanced Institute for Materials Research (AIMR), Tohoku University, Sendai 980-8577 (Japan); Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan)

2015-09-01

We report on the epitaxial thin film growth of an air-sensitive hydride, lithium hydride (LiH), using pulsed laser deposition (PLD). We first synthesized a dense LiH target, which is key for PLD growth of high-quality hydride films. Then, we obtained epitaxial thin films of [100]-oriented LiH on a MgO(100) substrate at 250 °C under a hydrogen pressure of 1.3 × 10{sup −2} Pa. Atomic force microscopy revealed that the film demonstrates a Stranski-Krastanov growth mode and that the film with a thickness of ∼10 nm has a good surface flatness, with root-mean-square roughness R{sub RMS} of ∼0.4 nm.

Pulsed laser deposition of air-sensitive hydride epitaxial thin films: LiH

International Nuclear Information System (INIS)

Oguchi, Hiroyuki; Isobe, Shigehito; Kuwano, Hiroki; Shiraki, Susumu; Hitosugi, Taro; Orimo, Shin-ichi

2015-01-01

We report on the epitaxial thin film growth of an air-sensitive hydride, lithium hydride (LiH), using pulsed laser deposition (PLD). We first synthesized a dense LiH target, which is key for PLD growth of high-quality hydride films. Then, we obtained epitaxial thin films of [100]-oriented LiH on a MgO(100) substrate at 250 °C under a hydrogen pressure of 1.3 × 10 −2 Pa. Atomic force microscopy revealed that the film demonstrates a Stranski-Krastanov growth mode and that the film with a thickness of ∼10 nm has a good surface flatness, with root-mean-square roughness R RMS of ∼0.4 nm

Speciation of the immediately mobilisable As(III), As(V), MMA and DMA in river sediments by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry following ultrasonic extraction

International Nuclear Information System (INIS)

Huerga, A.; Lavilla, I.; Bendicho, C.

2005-01-01

In this work, a fast method is developed for the speciation of As(III), As(V), MMA and DMA in the immediately mobilisable fraction of river sediments (i.e. water-soluble and phosphate-exchangeable) by high performance liquid chromatography-hydride generation-atomic fluorescence detection (HPLC-HG-AFD) after extraction using focused ultrasound. The influence of relevant parameters influencing an ion-pairing chromatographic separation following isocratic elution (i.e. amount of MeOH in the mobile phase, ion pair reagent concentration, pH, flow rate) was studied. Focused ultrasound transmitted from an ultrasonic probe provided the same extractable contents as conventional extraction with no changes in the species distribution. The effect of the drying step over extraction of As species was investigated. The following drying procedures were compared: freeze-, oven-, microwave- and air-drying. No influence of the drying operation on the water-extractable fraction was observed. However, freeze- and air-drying yielded significantly higher phosphate-extractable amounts of As(III) and As(V) as compared to oven and microwaves. Detection limits for the As species were in the range 1.3-4.1 ng/g for the water-soluble fraction and 1.6-4.8 ng/g for the phosphate buffer exchangeable fraction. The method was applied to the speciation of immediately mobilisable As(III), As(V), DMA and MMA in 11 sediment samples collected along the beds of the Louro River (southern Galicia, Spain)

Predicting Hydride Donor Strength via Quantum Chemical Calculations of Hydride Transfer Activation Free Energy.

Science.gov (United States)

Alherz, Abdulaziz; Lim, Chern-Hooi; Hynes, James T; Musgrave, Charles B

2018-01-25

We propose a method to approximate the kinetic properties of hydride donor species by relating the nucleophilicity (N) of a hydride to the activation free energy ΔG ⧧ of its corresponding hydride transfer reaction. N is a kinetic parameter related to the hydride transfer rate constant that quantifies a nucleophilic hydridic species' tendency to donate. Our method estimates N using quantum chemical calculations to compute ΔG ⧧ for hydride transfers from hydride donors to CO 2 in solution. A linear correlation for each class of hydrides is then established between experimentally determined N values and the computationally predicted ΔG ⧧ ; this relationship can then be used to predict nucleophilicity for different hydride donors within each class. This approach is employed to determine N for four different classes of hydride donors: two organic (carbon-based and benzimidazole-based) and two inorganic (boron and silicon) hydride classes. We argue that silicon and boron hydrides are driven by the formation of the more stable Si-O or B-O bond. In contrast, the carbon-based hydrides considered herein are driven by the stability acquired upon rearomatization, a feature making these species of particular interest, because they both exhibit catalytic behavior and can be recycled.

Roles of texture in controlling oxidation, hydrogen ingress and hydride formation in Zr alloys

International Nuclear Information System (INIS)

Szpunar, Jerzy A.; Qin, Wen; Li, Hualong; Kumar, Kiran

2011-01-01

Experimental observations shows that the oxide formed on Zr alloys are strongly textured. The texture and grain-boundary characteristics of oxide are dependent on the texture of metal substrate. Computer simulation and thermodynamic modeling clarify the effect of metal substrate on structure of oxide film, and intrinsic factors affecting the microstructure. Models of diffusion process of hydrogen atoms and oxygen diffusion through oxide are presented. Both intra-granular and inter-granular hydrides were found following (0001) α-Zr //(111) δ-ZrH1.5 relationship. The through-thickness texture inhomogeneity in cladding tubes, the effects of hoop stress on the hydride orientation and the formation of interlinked hydride structure were studied. A thermodynamic model was developed to analyze the nucleation and the stress-induced reorientation of intergranular hydrides. These works provide a framework for understanding the oxidation, the hydrogen ingress and the hydride formation in Zr alloys. (author)

Cerebellum engages in automation of verb-generation skill.

Science.gov (United States)

Yang, Zhi; Wu, Paula; Weng, Xuchu; Bandettini, Peter A

2014-03-01

Numerous studies have shown cerebellar involvement in item-specific association, a form of explicit learning. However, very few have demonstrated cerebellar participation in automation of non-motor cognitive tasks. Applying fMRI to a repeated verb-generation task, we sought to distinguish cerebellar involvement in learning of item-specific noun-verb association and automation of verb generation skill. The same set of nouns was repeated in six verb-generation blocks so that subjects practiced generating verbs for the nouns. The practice was followed by a novel block with a different set of nouns. The cerebellar vermis (IV/V) and the right cerebellar lobule VI showed decreased activation following practice; activation in the right cerebellar Crus I was significantly lower in the novel challenge than in the initial verb-generation task. Furthermore, activation in this region during well-practiced blocks strongly correlated with improvement of behavioral performance in both the well-practiced and the novel blocks, suggesting its role in the learning of general mental skills not specific to the practiced noun-verb pairs. Therefore, the cerebellum processes both explicit verbal associative learning and automation of cognitive tasks. Different cerebellar regions predominate in this processing: lobule VI during the acquisition of item-specific association, and Crus I during automation of verb-generation skills through practice.

Nuclear power generation and automation technology

International Nuclear Information System (INIS)

Korei, Yoshiro

1985-01-01

The proportion of nuclear power in the total generated electric power has been increasing year after year, and the ensuring of its stable supply has been demanded. For the further development of nuclear power generation, the heightening of economical efficiency which is the largest merit of nuclear power and the public acceptance as a safe and stable electric power source are the important subjects. In order to solve these subjects, in nuclear power generation, various automation techniques have been applied for the purpose of the heightening of reliability, labor saving and the reduction of radiation exposure. Meeting the high needs of automation, the automation technology aided by computers have been applied to the design, manufacture and construction, operation and maintenance of nuclear power plants. Computer-aided design and the examples of design of a reactor building, pipings and a fuel assembly, an automatic welder for pipings of all position TIG welding type, a new central monitoring and control system, an automatic exchanger of control rod-driving mechanism, an automatic in-service inspection system for nozzles and pipings, and a robot for steam generator maintenance are shown. The trend of technical development and an intelligent moving robot, a system maintenance robot and a four legs walking robot are explained. (Kako, I.)

Zirconium-hydride solid zero power reactor and its application research

International Nuclear Information System (INIS)

Lin Shenghuo; Luo Zhanglin; Su Zhuting

1994-10-01

The Zirconium Hydride Solid Zero Power Reactor built at China Institute of Atomic Energy is introduced. In the reactor Zirconium-hydride is used as moderator, plexiglass as reflector and U 3 O 8 with enrichment of 20% as the fuel, Since its initial criticality, the physical characteristics and safety features have been measured with the result showing that the reactor has sound stability and high sensitivity, etc. It has been successfully used for the personnel training and for the testing of reactor control instruments and experiment devices. It also presents the special advantage for the pre-research of some applications

Solubility of hydrogen isotopes in stressed hydride-forming metals

International Nuclear Information System (INIS)

Coleman, C.E.; Ambler, J.F.R.

1983-01-01

Components made from hydride-forming metals can be brittle when particles of hydride are present. The solid solubility limit of hydrogen in these metals needs to be known so that fracture resistance can be properly assessed. Stress affects the solubility of hydrogen in metals. As hydrogen dissolves the metal volume increases, an applied hydrostatic tensile stress supplies work to increase the solubility. Precipitation of hydrides increases the volume further. A hydrostatic tensile stress promotes the formation of hydrides and tends to reduce the terminal solubility. For materials containing hydrogen in solution in equilibrium with hydrides, the effect of stress on the terminal solubility is given. Hydrogen migrates up tensile stress gradients because of the effect of stress on the solubility and solubility limit. Consequently, hydrogen concentrates at flaws. When hydrides are present in the metal matrix, those remote from the flaw tip will preferentially dissolve in favor of those precipitated at the flaw. If the stress is large enough, at some critical condition the hydrides at the flaw will crack. This is delayed hydrogen cracking. Notched and fatigue-cracked cantilever beam specimens (6) (38 x 4 x 3 mm) were machined from the circumferential direction of several cold-worked Zr-2.5 at. % Nb pressure tubes. The chemical compositions had the ranges (in atomic %) Nb - 2.5 to 2.7; O - 0.58 to 0.71; H - 0.018 to 0.18. The effect of test temperature is for a specimen containing 0.13 at. % protium and 0.29 at .% deuterium. Between 505 K and 530 K was less than 1 hr, between 530 K and 537 K it increased to 25.8 h, while at 538 K no cracking was observed up to the 54 h

Reactivity patterns of transition metal hydrides and alkyls

Energy Technology Data Exchange (ETDEWEB)

Jones, W.D. II

1979-05-01

The complex PPN/sup +/ CpV(CO)/sub 3/H/sup -/ (Cp=eta/sup 5/-C/sub 5/H/sub 5/ and PPN = (Ph/sub 3/P)/sub 2/) was prepared in 70% yield and its physical properties and chemical reactions investigated. PPN/sup +/ CpV(CO)/sub 3/H/sup -/ reacts with a wide range of organic halides. The organometallic products of these reactions are the vanadium halides PPN/sup +/(CpV(C)/sub 3/X)/sup -/ and in some cases the binuclear bridging hydride PPN/sup +/ (CpV(CO)/sub 3/)/sub 2/H/sup -/. The borohydride salt PPN/sup +/(CpV(CO)/sub 3/BH/sub 4/)/sup -/ has also been prepared. The reaction between CpV(CO)/sub 3/H/sup -/ and organic halides was investigated and compared with halide reductions carried out using tri-n-butyltin hydride. Results demonstrate that in almost all cases, the reduction reaction proceeds via free radical intermediates which are generated in a chain process, and are trapped by hydrogen transfer from CpV(CO)/sub 3/H/sup -/. Sodium amalgam reduction of CpRh(CO)/sub 2/ or a mixture of CpRh(CO)/sub 2/ and CpCo(CO)/sub 2/ affords two new anions, PPN/sup +/ (Cp/sub 2/Rh/sub 3/(CO)/sub 4/)/sup -/ and PPN/sup +/(Cp/sub 2/RhCo(CO)/sub 2/)/sup -/. CpMo(CO)/sub 3/H reacts with CpMo(CO)/sub 3/R (R=CH/sub 3/,C/sub 2/H/sub 5/, CH/sub 2/C/sub 6/H/sub 5/) at 25 to 50/sup 0/C to produce aldehyde RCHO and the dimers (CpMo(CO)/sub 3/)/sub 2/ and (CpMo(CO)/sub 2/)/sub 2/. In general, CpV(CO)/sub 3/H/sup -/ appears to transfer a hydrogen atom to the metal radical anion formed in an electron transfer process, whereas CpMo(CO)/sub 3/H transfers hydride in a 2-electron process to a vacant coordination site. The chemical consequences are that CpV(CO)/sub 3/H/sup -/ generally reacts with metal alkyls to give alkanes via intermediate alkyl hydride species whereas CpMo(CO)/sub 3/H reacts with metal alkyls to produce aldehyde, via an intermediate acyl hydride species.

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

International Nuclear Information System (INIS)

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

1981-01-01

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

The Oxidation Products of Aluminum Hydride and Boron Aluminum Hydride Clusters

Science.gov (United States)

2016-01-04

AFRL-AFOSR-VA-TR-2016-0075 The Oxidation Products of Aluminum Hydride and Boron Aluminum Hydride Clusters KIT BOWEN JOHNS HOPKINS UNIV BALTIMORE MD...2. REPORT TYPE Final Performance 3. DATES COVERED (From - To) 30-09-2014 to 29-09-2015 4. TITLE AND SUBTITLE The Oxidation Products of Aluminum ...Hydride and Boron Aluminum Hydride Clusters 5a.  CONTRACT NUMBER 5b.  GRANT NUMBER FA9550-14-1-0324 5c.  PROGRAM ELEMENT NUMBER 61102F 6. AUTHOR(S) KIT

Determination of sub-ng g-1 levels of total inorganic arsenic and selenium in foods by hydride-generation atomic absorption spectrometry after pre-concentration.

Science.gov (United States)

Altunay, Nail; Gürkan, Ramazan

2017-03-01

A new and simple ultrasonic-assisted extraction (UAE) procedure was developed for the determination of inorganic arsenic and selenium in foods by hydride-generation atomic absorption spectrometry (HG-AAS). The various analytical variables affecting complex formation and extraction efficiency were investigated and optimised. The method is based on selective complex formation of As(III) and Se(IV) in the presence of excess As(V) and Se(VI) with toluidine red in the presence of tartaric acid at pH 4.5, and then extraction of the resulting condensation products into the micellar phase of non-ionic surfactant, polyethylene glycol dodecyl ether, Brij 35. Under optimised conditions, good linear relationships were obtained in the ranges of 4-225 and 12-400 ng l - 1 with limits of detection of 1.1 and 3.5 ng l - 1 for As(III) and Se(IV), respectively. The repeatability was better than 3.9% for both analytes (n = 10, 25 ng l - 1 ) while reproducibility ranged from 4.2% to 4.8%. The recoveries of As(III) and Se(IV) spiked at 25-100 ng l - 1 were in the range of 94.2-104.8%. After pre-concentration of a 5.0 ml sample, the sensitivity enhancement factors for As(III) and Se(IV) were 185 and 140, respectively. Accuracy was assessed by analysis of two standard reference materials (SRMs) and spiked recovery experiments. The method was successfully applied to the accurate and reliable determination of total As and total Se by HG-AAS after pre-reduction with a mixture of L-cysteine and tartaric acid. Finally, the method was shown to be rapid and sensitive, with good results for extraction, pre-concentration and determination of total As and Se contents (as As(III) and Se(IV)) from food samples.

Precipitation of γ-zirconium hydride in zirconium

International Nuclear Information System (INIS)

Carpenter, G.J.C.

1978-01-01

A mechanism for the precipitation of γ-zirconium hydride in zirconium is presented which does not require the diffusion of zirconium. The transformation is completed by shears caused by 1/3 (10 anti 10) Shockley partial dislocations on alternate zirconium basal planes, either by homogeneous nucleation or at lattice imperfections. Homogeneous nucleation is considered least likely in view of the large nucleation barrier involved. Hydrides may form at dislocations by the generation of partials by means of either a pole or ratchet mechanism. The former requires dislocations with a component of Burgers vector along the c-axis, but contrast experiments show that these are not normally observed in annealed zirconium. It is therefore most likely that intragranular hydrides form at the regular 1/3 (11 anti 20) dislocations, possibly by means of a ratchet mechanism. Contrast experiments in the electron microscope show that the precipitates have a shear character consistent with the mechanism suggested. The possibility that the shear dislocations associated with the hydrides are emissary dislocations is considered and a model suggested in which this function is satisfied together with the partial relief of misfit stresses. The large shear strains associated with the precipitation mechanism may play an important role in the preferential orientation of hydrides under stress

Redox speciation analysis of antimony in soil extracts by hydride generation atomic fluorescence spectrometry

International Nuclear Information System (INIS)

Fuentes, Edwar; Pinochet, Hugo; Gregori, Ida de; Potin-Gautier, Martine

2003-01-01

A sensitive atomic spectrometric method for the redox speciation analysis of antimony in soils is described. The method is based on the selective generation of stibine from Sb(III) in a continuous flow system using atomic fluorescence spectrometry for detection. Sb(V) is masked by citric or oxalic acid in HCl medium. The procedure was optimized with synthetic solutions of Sb(III) and Sb(V). The effect of carboxylic acid and HCl concentration on the recovery of Sb(III) and Sb(V) species from standard solutions, and on the fluorescence signal were studied. Both species were extracted from soil with H 2 O, 0.05 mol l -1 EDTA and 0.25 mol l -1 H 2 SO 4 . Since the soil samples were collected from sites impacted by copper mining activities, the effect of Cu 2+ on the determination of antimony in synthetic solutions and soil extracts was studied. Cu 2+ decreased the Sb(III) signal, but had no effect on the total antimony determination. Therefore, the selective determination of Sb(III) was carried out in citric acid-HCl medium, using the analyte addition technique. Total antimony in soil extracts was determined using the standard calibration technique after reducing Sb(V) to Sb(III) at room temperature with KI-ascorbic acid. The Sb(V) concentration was calculated from the difference between total antimony and Sb(III). The limits of detection (PS Analytical, Excalibur Millennium model) were 17 and 10 ng l -1 for Sb(III) and total antimony, respectively, and the R.S.D. at the 0.5-μg l -1 level were 2.5 and 2.4%, respectively. The total antimony concentration of soils is in the mg kg -1 range; the Sb recovery from the different soils by the extracting solutions was between less than 0.02% and approximately 10%. Similar recoveries were obtained using EDTA and sulfuric acid solutions. Sb(V) was found to be the main antimony species extracted from soils

High-pressure hydriding of Zircaloy

International Nuclear Information System (INIS)

Kim, Y.S.

1996-01-01

The hydriding characteristics of Zircaloy-2(Zry), sponge zirconium (as a liner on Zry plate), and crystal-bar zirconium exposed to pure H 2 at 0.1 MPa or 7 MPa and 400 C were determined in a thermogravimetric apparatus. The morphology of the hydrided specimens was also examined by optical microscopy. For all specimen types, the rate of hydriding in 7 MPa H 2 was two orders of magnitude greater than in 0.1 MPa H 2 . For Zry, uniform bulk hydriding was revealed by hydride precipitates at room temperature and on one occasion, a sunburst hydride. In addition, all specimen types exhibited a hydride surface layer. In a duplex Zry/sponge-Zr specimen, Zry is more heavily hydrided than the sponge Zr layer. (orig.)

Automated Test Case Generation for an Autopilot Requirement Prototype

Science.gov (United States)

Giannakopoulou, Dimitra; Rungta, Neha; Feary, Michael

2011-01-01

Designing safety-critical automation with robust human interaction is a difficult task that is susceptible to a number of known Human-Automation Interaction (HAI) vulnerabilities. It is therefore essential to develop automated tools that provide support both in the design and rapid evaluation of such automation. The Automation Design and Evaluation Prototyping Toolset (ADEPT) enables the rapid development of an executable specification for automation behavior and user interaction. ADEPT supports a number of analysis capabilities, thus enabling the detection of HAI vulnerabilities early in the design process, when modifications are less costly. In this paper, we advocate the introduction of a new capability to model-based prototyping tools such as ADEPT. The new capability is based on symbolic execution that allows us to automatically generate quality test suites based on the system design. Symbolic execution is used to generate both user input and test oracles user input drives the testing of the system implementation, and test oracles ensure that the system behaves as designed. We present early results in the context of a component in the Autopilot system modeled in ADEPT, and discuss the challenges of test case generation in the HAI domain.

Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

International Nuclear Information System (INIS)

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

2003-01-01

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

Poisoning Experiments Aimed at Discriminating Active and Less-Active Sites of Silica-Supported Tantalum Hydride for Alkane Metathesis

KAUST Repository

Saggio, Guillaume

2010-10-04

Only 50% of the silica-supported tantalum hydride sites are active in the metathesis of propane. Indeed, more than 45% of the tantalum hydride can be eliminated by a selective oxygen poisoning of inactive sites with no significant decrease in the global turnover. Conversely, cyclopentane induces no such selective poisoning. Hence, the active tantalum hydride sites that show greater resistance to oxygen poisoning correspond to the νTa-H bands of higher wavenumbers, particularly that at 1860cm-1. These active tantalum hydride sites should correspond to tris- or monohydride species relatively far from silica surface oxygen atoms. © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Application of automated reasoning software: procedure generation system verifier

International Nuclear Information System (INIS)

Smith, D.E.; Seeman, S.E.

1984-09-01

An on-line, automated reasoning software system for verifying the actions of other software or human control systems has been developed. It was demonstrated by verifying the actions of an automated procedure generation system. The verifier uses an interactive theorem prover as its inference engine with the rules included as logic axioms. Operation of the verifier is generally transparent except when the verifier disagrees with the actions of the monitored software. Testing with an automated procedure generation system demonstrates the successful application of automated reasoning software for verification of logical actions in a diverse, redundant manner. A higher degree of confidence may be placed in the verified actions gathered by the combined system

Theoretical study of hydrogen storage in metal hydrides.

Science.gov (United States)

Oliveira, Alyson C M; Pavão, A C

2018-05-04

Adsorption, absorption and desorption energies and other properties of hydrogen storage in palladium and in the metal hydrides AlH 3 , MgH 2 , Mg(BH 4 ) 2 , Mg(BH 4 )(NH 2 ) and LiNH 2 were analyzed. The DFT calculations on cluster models show that, at a low concentration, the hydrogen atom remains adsorbed in a stable state near the palladium surface. By increasing the hydrogen concentration, the tetrahedral and the octahedral sites are sequentially occupied. In the α phase the tetrahedral site releases hydrogen more easily than at the octahedral sites, but the opposite occurs in the β phase. Among the hydrides, Mg(BH 4 ) 2 shows the highest values for both absorption and desorption energies. The absorption energy of LiNH 2 is higher than that of the palladium, but its desorption energy is too high, a recurrent problem of the materials that have been considered for hydrogen storage. The release of hydrogen, however, can be favored by using transition metals in the material structure, as demonstrated here by doping MgH 2 with 3d and 4d-transition metals to reduce the hydrogen atomic charge and the desorption energy.

Determination of inorganic arsenic in algae using bromine halogenation and on-line nonpolar solid phase extraction followed by hydride generation atomic flourescence spectrometry

Science.gov (United States)

Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and on-line nonpolar solid phase extraction (SPE) followed by hydrid...

Insight into destabilization mechanism of Mg-based hydrides interstitially co-doped with nonmetals: a DFT study

Science.gov (United States)

Wu, Zhen; Zhu, Luying; Yang, Fusheng; Zhang, Zaoxiao; Nyamsi, Serge N.

2018-04-01

Mg-based metal hydride is one of the most promising materials for hydrogen energy storage. However, the high thermal stability due to strong bonding effects between the atoms limits its practical application. In order to reduce the thermal stability, a method of doping double nonmetals into Mg-based system was proposed in this study. The density functional theory (DFT) calculation results showed that the thermal stabilities of both the B-N co-doped Mg-based alloy and its hydride are reduced compared with pure Mg-based system. The relative formation enthalpies of the alloy and its hydride are 0.323 and 0.595 eV atom-1, respectively. The values are much higher than those for either singly B- or N-doped Mg-based system. The more significant destabilization by doping double nonmetal elements than single element is mainly attributed to a dual effect in weakening Mg-Ni/NiH4 bonds, caused by criss-cross interactions between B-Ni and N-Mg bonds.

A thermal neutron scattering law for yttrium hydride

Science.gov (United States)

Zerkle, Michael; Holmes, Jesse

2017-09-01

Yttrium hydride (YH2) is of interest as a high temperature moderator material because of its superior ability to retain hydrogen at elevated temperatures. Thermal neutron scattering laws for hydrogen bound in yttrium hydride (H-YH2) and yttrium bound in yttrium hydride (Y-YH2) prepared using the ab initio approach are presented. Density functional theory, incorporating the generalized gradient approximation (GGA) for the exchange-correlation energy, is used to simulate the face-centered cubic structure of YH2 and calculate the interatomic Hellmann-Feynman forces for a 2 × 2 × 2 supercell containing 96 atoms. Lattice dynamics calculations using PHONON are then used to determine the phonon dispersion relations and density of states. The calculated phonon density of states for H and Y in YH2 are used to prepare H-YH2 and Y-YH2 thermal scattering laws using the LEAPR module of NJOY2012. Analysis of the resulting integral and differential scattering cross sections demonstrates adequate resolution of the S(α,β) function. Comparison of experimental lattice constant, heat capacity, inelastic neutron scattering spectra and total scattering cross section measurements to calculated values are used to validate the thermal scattering laws.

Trace determination of antimony by hydride generation atomic absorption spectrometry with analyte preconcentration/atomization in a dielectric barrier discharge atomizer

Czech Academy of Sciences Publication Activity Database

Zurynková, Pavla; Dědina, Jiří; Kratzer, Jan

2018-01-01

Roč. 1010, JUN (2018), s. 11-19 ISSN 0003-2670 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * Stibane * atomization and preconcentration Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 4.950, year: 2016

Influence of hydrides orientation on strain, damage and failure of hydrided zircaloy-4

International Nuclear Information System (INIS)

Racine, A.

2005-09-01

In pressurized water reactors of nuclear power plants, fuel pellets are contained in cladding tubes, made of Zirconium alloy, for instance Zircaloy-4. During their life in the primary water of the reactor (155 bars, 300 C), cladding tubes are oxidized and consequently hydrided. A part of the hydrogen given off precipitates as Zirconium hydrides in the bulk material and embrittles the material. This embrittlement depends on many parameters, among which hydrogen content and orientation of hydrides with respect to the applied stress. This investigation is devoted to the influence of the orientation of hydrides with respect to the applied stress on strain, damage and failure mechanisms. Macroscopic and SEM in-situ ring tensile tests are performed on cladding tube material (unirradiated cold worked stress-relieved Zircaloy-4) hydrided with about 200 and 500 wppm hydrogen, and with different main hydrides orientation: either parallel or perpendicular to the circumferential tensile direction. We get the mechanical response of the material as a function of hydride orientation and hydrogen content and we investigate the deformation, damage and failure mechanisms. In both cases, digital image correlation techniques are used to estimate local and global strain distributions. Neither the tensile stress-strain response nor the global and local strain modes are significantly affected by hydrogen content or hydride orientation, but the failure modes are strongly modified. Indeed, only 200 wppm radial hydrides embrittle Zy-4: sample fail in the elastic domain at about 350 MPa before strain bands could develop; whereas in other cases sample reach at least 750 MPa before necking and final failure, in ductile or brittle mode. To model this particular heterogeneous material behavior, a non-coupled damage approach which takes into account the anisotropic distribution of the hydrides is proposed. Its parameters are identified from the macroscopic strain field measurements and a

Automated installation for atomic emission determination of gold, silver and platinum group metals

International Nuclear Information System (INIS)

Zayakina, S.B.; Anoshin, G.N.; Gerasimov, P.A.; Smirnov, A.V.

1999-01-01

An automated installation for the direct atomic emission determination of silver, gold and platinum-group metals (Ru) in geological and geochemical materials with software for automated data acquisition and handling is designed and developed. The installation consists of a DFS-458 diffraction spectrograph, a MAES-10 multichannel analyzer of emission spectra, and a dual-jet plasmatron. A library of spectral lines of almost all elements excited in the dual-jet plasmatron is complied [ru

Analysis of volatile organic compounds in pleural effusions by headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry.

Science.gov (United States)

Huang, Zhongping; Zhang, Jie; Zhang, Peipei; Wang, Hong; Pan, Zaifa; Wang, Lili

2016-07-01

Headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry was applied to the analysis of volatile organic compounds in pleural effusions. The highly volatile organic compounds were separated successfully with high sensitivity by the employment of a cryotrap device, with the construction of a cold column head by freezing a segment of metal capillary with liquid nitrogen. A total of 76 volatile organic compounds were identified in 50 pleural effusion samples (20 malignant effusions and 30 benign effusions). Among them, 34 more volatile organic compounds were detected with the retention time less than 8 min, by comparing with the normal headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry method. Furthermore, 24 volatile organic compounds with high occurrence frequency in pleural effusion samples, 18 of which with the retention time less than 8 min, were selected for the comparative analysis. The results of average peak area comparison and box-plot analysis showed that except for cyclohexanone, 2-ethyl-1-hexanol, and tetramethylbenzene, which have been reported as potential cancer biomarkers, cyclohexanol, dichloromethane, ethyl acetate, n-heptane, ethylbenzene, and xylene also had differential expression between malignant and benign effusions. Therefore, the proposed approach was valuable for the comprehensive characterization of volatile organic compounds in pleural effusions. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of Ultra-Trace Amounts of Selenium(IV) by Flow Injection Hydride Generation Atomic Absorption Spectrometry with On-line Preconcentration by Co-precipitation with Lanthanium Hydroxide. Part II. On-line Addition of Coprecipating Agent

DEFF Research Database (Denmark)

Nielsen, Steffen; Sloth, Jens Jørgen; Hansen, Elo Harald

1996-01-01

-line and merged with an ammonium buffer solution of pH 9.1, which promotes precipitation and quantitative collection on the inner walls of an incorporated knotted Microline reactor. The Se(IV) preconcentrated by coprecipitation with the generated lanthanum hydroxide precipitate is subsequently eluted...... with hydrochloric acid, allowing an ensuing determination via hydride generation. At different sample flow rates, i.e., 4.8, 6.4 and 8.8 ml/min, enrichment factors of 30, 40 and 46, respectively, were obtained at a sampling frequency of 33 samples/h. The detection limit (3s) was 0.005 µg/l at a sample flow rate...

Hydrogen bonding between hydrides of the upper-right part of the periodic table

Science.gov (United States)

Simončič, Matjaž; Urbic, Tomaz

2018-05-01

One of the most important electrostatic interactions between molecules is most definitely the hydrogen bond. Understanding the basis of this interaction may offer us the insight needed to understand its effect on the macroscopic scale. Hydrogen bonding is for example the reason for anomalous properties in compounds like water and naturally life as we know it. The strength of the bond depends on numerous factors, among them the electronegativity of participating atoms. In this work we calculated the strength of hydrogen bonds between hydrides of the upper-right part of the periodic table (C, N, O, F, P, S, Cl, As, Se, Br) using quantum-chemical methods. The aim was to determine what influences the strength of strong and weak hydrogen bonds in simple hydrides. Various relationships were checked. A relation between the strength of the bond and the electronegativity of the participating atoms was found. We also observed a correlation between the strength of hydrogen bonds and the inter-atomic distances, along with the dependence on the charge transfer on the atom of the donor. We also report characteristic geometries of different dimers.

First-principles calculations of niobium hydride formation in superconducting radio-frequency cavities

Science.gov (United States)

Ford, Denise C.; Cooley, Lance D.; Seidman, David N.

2013-09-01

Niobium hydride is suspected to be a major contributor to degradation of the quality factor of niobium superconducting radio-frequency (SRF) cavities. In this study, we connect the fundamental properties of hydrogen in niobium to SRF cavity performance and processing. We modeled several of the niobium hydride phases relevant to SRF cavities and present their thermodynamic, electronic, and geometric properties determined from calculations based on density functional theory. We find that the absorption of hydrogen from the gas phase into niobium is exothermic and hydrogen becomes somewhat anionic. The absorption of hydrogen by niobium lattice vacancies is strongly preferred over absorption into interstitial sites. A single vacancy can accommodate six hydrogen atoms in the symmetrically equivalent lowest energy sites and additional hydrogen in the nearby interstitial sites affected by the strain field: this indicates that a vacancy can serve as a nucleation center for hydride phase formation. Small hydride precipitates may then occur near lattice vacancies upon cooling. Vacancy clusters and extended defects should also be enriched in hydrogen, potentially resulting in extended hydride phase regions upon cooling. We also assess the phase changes in the niobium-hydrogen system based on charge transfer between niobium and hydrogen, the strain field associated with interstitial hydrogen, and the geometry of the hydride phases. The results of this study stress the importance of not only the hydrogen content in niobium, but also the recovery state of niobium for the performance of SRF cavities.

First-principles calculations of niobium hydride formation in superconducting radio-frequency cavities

International Nuclear Information System (INIS)

Ford, Denise C; Cooley, Lance D; Seidman, David N

2013-01-01

Niobium hydride is suspected to be a major contributor to degradation of the quality factor of niobium superconducting radio-frequency (SRF) cavities. In this study, we connect the fundamental properties of hydrogen in niobium to SRF cavity performance and processing. We modeled several of the niobium hydride phases relevant to SRF cavities and present their thermodynamic, electronic, and geometric properties determined from calculations based on density functional theory. We find that the absorption of hydrogen from the gas phase into niobium is exothermic and hydrogen becomes somewhat anionic. The absorption of hydrogen by niobium lattice vacancies is strongly preferred over absorption into interstitial sites. A single vacancy can accommodate six hydrogen atoms in the symmetrically equivalent lowest energy sites and additional hydrogen in the nearby interstitial sites affected by the strain field: this indicates that a vacancy can serve as a nucleation center for hydride phase formation. Small hydride precipitates may then occur near lattice vacancies upon cooling. Vacancy clusters and extended defects should also be enriched in hydrogen, potentially resulting in extended hydride phase regions upon cooling. We also assess the phase changes in the niobium–hydrogen system based on charge transfer between niobium and hydrogen, the strain field associated with interstitial hydrogen, and the geometry of the hydride phases. The results of this study stress the importance of not only the hydrogen content in niobium, but also the recovery state of niobium for the performance of SRF cavities. (paper)

Suppression of hydride precipitates in niobium superconducting radio-frequency cavities

Science.gov (United States)

Ford, Denise C.; Cooley, Lance D.; Seidman, David N.

2013-10-01

Niobium hydride is a suspected contributor to degraded niobium superconducting radio-frequency (SRF) cavity performance by Q slope and Q disease. The concentration and distribution of hydrogen atoms in niobium can be strongly affected by the cavity processing treatments. This study provides guidance for cavity processing based on density functional theory calculations of the properties of common processing impurity species—hydrogen, oxygen, nitrogen, and carbon—in the body-centered cubic (bcc) niobium lattice. We demonstrate that some fundamental properties are shared between the impurity atoms, such as anionic character in niobium. The strain field produced, however, by hydrogen atoms is both geometrically different and substantially weaker than the strain field produced by the other impurities. We focus on the interaction between oxygen and hydrogen atoms in the lattice, and demonstrate that the elastic interactions between these species and the bcc niobium lattice cause trapping of hydrogen and oxygen atoms by bcc niobium lattice vacancies. We also show that the attraction of oxygen to a lattice vacancy is substantially stronger than the attraction of hydrogen to the vacancy. Additionally, hydrogen dissolved in niobium tetrahedral interstitial sites can be trapped by oxygen, nitrogen and possibly carbon atoms dissolved in octahedral interstitial sites. These results indicate that the concentration of oxygen in the bcc lattice can have a strong impact on the ability of hydrogen to form detrimental phases. Based on our results and a literature survey, we propose a mechanism for the success of the low-temperature annealing step applied to niobium SRF cavities. We also recommend further examination of nitrogen and carbon in bcc niobium, and particularly the role that nitrogen can play in preventing detrimental hydride phase formation.

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

Directory of Open Access Journals (Sweden)

Maria Guţu Claudia

2013-10-01

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

Determination of Arsenic Content of Available Traditional Medicines ...

African Journals Online (AJOL)

Tropical Journal of Pharmaceutical Research December 2013; 12 (6): 1053- ... Medicines in Malaysia using Hydride Generation Atomic ... Keywords: Traditional medicine, Arsenic, Hydride Generation –Atomic Absorption Spectrometer HG-.

Hydride phase dissolution enthalpy in neutron irradiated Zircaloy-4

International Nuclear Information System (INIS)

Vizcaino, Pablo; Banchik, Abraham D.

2003-01-01

The differential calorimetric technique has been applied to measure the dissolution enthalpy, ΔH irrad δ→α , of zirconium hydrides precipitated in structural components removed from the Argentine Atucha 1 PHWR nuclear power plant after 10.3 EFPY. An average value of ΔH irrad δ→α = 5 kJ/mol H was obtained after the first calorimetric run. That value is seven times lower than the value of ΔH δ→α = 37.7 kJ/mol H recently determined in Zircaloy-4 specimens taken from similar unirradiated structural components using the same calorimetric technique, [1]. Post-irradiation thermal treatments gradually increase that low value towards the unirradiated value with increasing annealing temperature similar to that observed for TSSd irrad . Therefore the same H atom trapping mechanism during reactor operation already proposed to explain the evolution of TSSd irrad is also valid for Q irrad δ→α . As the ratio Q/ΔH is proportional to the number N H of H atoms precipitated as hydrides, the increment of Q irrad δ→α with the thermal treatment indicates that the value of N H also grows with the annealing reaching the value corresponding to the bulk H concentration when ΔH irrad δ→α ≅ 37 kJ/mol H. That is a direct indication that the post-irradiation thermal treatment releases the H atoms from their traps increasing the number of H atoms available to precipitate at the end of each calorimetric run and/or isothermal treatment. (author)

Trapping of antimony and bismuth hydrides on a molybdenum-foil strip

Czech Academy of Sciences Publication Activity Database

Krejčí, Pavel; Dočekal, Bohumil

2005-01-01

Roč. 99, S (2005), s148-s149 ISSN 0009-2770. [Meeting on Chemistry and Life /3./. Brno, 20.09.2005-22.09.2005] R&D Projects: GA AV ČR IAA400310507 Institutional research plan: CEZ:AV0Z40310501 Keywords : hydride generation * hydride trapping * molybdenum-foil strip device Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.445, year: 2005

Multi-scale characterization of nanostructured sodium aluminum hydride

Science.gov (United States)

NaraseGowda, Shathabish

Complex metal hydrides are the most promising candidate materials for onboard hydrogen storage. The practicality of this class of materials is counter-poised on three critical attributes: reversible hydrogen storage capacity, high hydrogen uptake/release kinetics, and favorable hydrogen uptake/release thermodynamics. While a majority of modern metallic hydrides that are being considered are those that meet the criteria of high theoretical storage capacity, the challenges lie in addressing poor kinetics, thermodynamics, and reversibility. One emerging strategy to resolve these issues is via nanostructuring or nano-confinement of complex hydrides. By down-sizing and scaffolding them to retain their nano-dimensions, these materials are expected to improve in performance and reversibility. This area of research has garnered immense interest lately and there is active research being pursued to address various aspects of nanostructured complex hydrides. The research effort documented here is focused on a detailed investigation of the effects of nano-confinement on aspects such as the long range atomic hydrogen diffusivities, localized hydrogen dynamics, microstructure, and dehydrogenation mechanism of sodium alanate. A wide variety of microporous and mesoporous materials (metal organic frameworks, porous silica and alumina) were investigated as scaffolds and the synthesis routes to achieve maximum pore-loading are discussed. Wet solution infiltration technique was adopted using tetrahydrofuran as the medium and the precursor concentrations were found to have a major role in achieving maximum pore loading. These concentrations were optimized for each scaffold with varying pore sizes and confinement was quantitatively characterized by measuring the loss in specific surface area. This work is also aimed at utilizing neutron and synchrotron x-ray characterization techniques to study and correlate multi-scale material properties and phenomena. Some of the most advanced

Conference 'Chemistry of hydrides' Proceedings

International Nuclear Information System (INIS)

1991-07-01

This collection of thesis of conference of Chemistry hydrides presents the results of investigations concerning of base questions of chemistry of nonorganic hydrides, including synthesis questions, studying of physical and chemical properties, thermodynamics, analytical chemistry, investigation of structure, equilibriums in the systems of metal-hydrogen, behaviour of nonorganic hydrides in non-water mediums and applying investigations in the chemistry area and technology of nonorganic hydrides

Speciation of inorganic antimony in polyethylene terephthalate (PET) bottled water using hydride generation atomic absorption spectrophotometry (HG-AAS)

International Nuclear Information System (INIS)

Markwo, Ali

2015-07-01

Antimony (Sb) is a regulated drinking water contaminant that has been found to leach from polyethylene terephthalate (PET) plastic containers into the waters stored in them. The common inorganic species of antimony in water are Sb(III) and Sb(V), with the former being more toxic and the latter being more soluble. In order to assess the extent to which waters stored in PET bottles are contaminated with inorganic Sb and to further examine the effect of typical storage conditions on migration rates, speciation analysis of inorganic Sb using hydride generation atomic absorption spectrophotometry (HG-AAS) was undertaken on selected PET plastic bottled waters marketed in the Greater Accra Region of Ghana. Six brands of PET plastic bottled waters were obtained at source on the day of packaging, and analyses undertaken on samples of the waters stored in the plastic containers at intervals of four weeks for twelve weeks, under three carefully chosen storage conditions distinctive of bottled water usage. Selected physicochemical properties of samples of the waters stored in the plastic containers and total Sb of samples of the plastic containers were also determined to discover the effect of some physical properties and certain major ions, and the influence of the different quality PET plastic types on Sb migration respectively. The study revealed amounts of total Sb in the PET plastic containers of the 6 brands ranging from 123.46 mg/kg to 146.45 mg/kg. The selected physicochemical properties of the waters stored in the PET plastic containers considered were pH (6.78 – 7.43), Ca2+ (1.61 – 12.39 mg/L), Mg2+ (1.00 – 4.96 mg/L), HCO3− (6.18 – 55.41 mg/L) and TDS (8.70 – 70.40 mg/L)). PET bottled waters of 5 out of the 6 brands contained Sb (initial total Sb ranging from 1.11 – 14.65 μg/L) before storage. Total Sb concentrations of the waters stored in the plastic containers were observed to increase with storage time under all the three storage conditions for

Dimethylaluminum hydride for atomic layer deposition of Al2O3 passivation for amorphous InGaZnO thin-film transistors

Science.gov (United States)

Corsino, Dianne C.; Bermundo, Juan Paolo S.; Fujii, Mami N.; Takahashi, Kiyoshi; Ishikawa, Yasuaki; Uraoka, Yukiharu

2018-06-01

Atomic layer deposition (ALD) of Al2O3 using dimethylaluminum hydride (DMAH) was demonstrated as an effective passivation for amorphous InGaZnO thin-film transistors (TFTs). Compared with the most commonly used precursor, trimethylaluminum, TFTs fabricated with DMAH showed improved stability, resulting from the lower amount of oxygen vacancies, and hence fewer trap sites, as shown by X-ray photoelectron spectroscopy (XPS) depth profiling analysis. We found that prolonged plasma exposure during ALD can eliminate the hump phenomenon, which is only present for DMAH. The higher Al2O3 deposition rate when using DMAH is in line with the requirements of emerging techniques, such as spatial ALD, for improving fabrication throughput.

Edge profiles in K shell photoabsorption spectra of gaseous hydrides of 3p elements and homologues

Science.gov (United States)

Hauko, R.; Gomilšek, J. Padežnik; Kodre, A.; Arčon, I.; Aquilanti, G.

2017-10-01

Photoabsorption spectra of gaseous hydrides of 3p elements (PH3, H2S, HCl) are measured in the energy region of photoexcitations pertaining to K edge. The analysis of the edge profile is extended to hydrides of 4p series (GeH4, AsH3, H2Se, HBr) from an earlier experiment, and to published spectra of 2p hydrides (CH4, NH3, H2O, HF) and noble gases Ar, Kr and Ne and SiH4. The edge profiles are modelled with a linear combination of lorentzian components, describing excitations to individual bound states and to continuum. Transition energies and probabilities are also calculated in the non-relativistic molecular model of the ORCA code, in good agreement with the experiment. Edge profiles in the heavier homologues are closely similar, the symmetry of the molecule governs the transitions to the lowest unoccupied orbitals. In 2p series the effect of the strong nuclear potential prevails. Transitions to higher, atomic-like levels remain very much the same as in free atoms.

Development and test of a cryogenic trap system dedicated to confinement of radioactive volatile isotopes in SPIRAL2 post-accelerator

Science.gov (United States)

Souli, M.; Dolégiéviez, P.; Fadil, M.; Gallardo, P.; Levallois, R.; Munoz, H.; Ozille, M.; Rouillé, G.; Galet, F.

2011-12-01

A cryogenic trap system called Cryotrap has been studied and developed in the framework of nuclear safety studies for SPIRAL2 accelerator. The main objective of Cryotrap is to confine and reduce strongly the migration of radioactive volatile isotopes in beam lines. These radioactive gases are produced after interaction between a deuteron beam and a fissile target. Mainly, Cryotrap is composed by a vacuum vessel and two copper thermal screens maintained separately at two temperatures T1=80 K and T2=20 K. A Cryocooler with two stages at previous temperatures is used to remove static heat losses of the cryostat and ensure an efficient cooling of the system. Due to strong radiological constraints that surround Cryotrap, the coupling system between Cryocooler and thermal screens is based on aluminum thermo-mechanical contraction. The main objective of this original design is to limit direct human maintenance interventions and provide maximum automated operations. A preliminary prototype of Cryotrap has been developed and tested at GANIL laboratory to validate its design, and determine its thermal performance and trapping efficiency. In this paper, we will first introduce briefly SPIRAL2 project and discuss the main role of Cryotrap in nuclear safety of the accelerator. Then, we will describe the proposed conceptual design of Cryotrap and its main characteristics. After that, we will focus on test experiment and analyze experimental data. Finally, we will present preliminary results of gas trapping efficiency tests.

Hydrogen Outgassing from Lithium Hydride

Energy Technology Data Exchange (ETDEWEB)

Dinh, L N; Schildbach, M A; Smith, R A; Balazs1, B; McLean II, W

2006-04-20

Lithium hydride is a nuclear material with a great affinity for moisture. As a result of exposure to water vapor during machining, transportation, storage and assembly, a corrosion layer (oxide and/or hydroxide) always forms on the surface of lithium hydride resulting in the release of hydrogen gas. Thermodynamically, lithium hydride, lithium oxide and lithium hydroxide are all stable. However, lithium hydroxides formed near the lithium hydride substrate (interface hydroxide) and near the sample/vacuum interface (surface hydroxide) are much less thermally stable than their bulk counterpart. In a dry environment, the interface/surface hydroxides slowly degenerate over many years/decades at room temperature into lithium oxide, releasing water vapor and ultimately hydrogen gas through reaction of the water vapor with the lithium hydride substrate. This outgassing can potentially cause metal hydriding and/or compatibility issues elsewhere in the device. In this chapter, the morphology and the chemistry of the corrosion layer grown on lithium hydride (and in some cases, its isotopic cousin, lithium deuteride) as a result of exposure to moisture are investigated. The hydrogen outgassing processes associated with the formation and subsequent degeneration of this corrosion layer are described. Experimental techniques to measure the hydrogen outgassing kinetics from lithium hydride and methods employing the measured kinetics to predict hydrogen outgassing as a function of time and temperature are presented. Finally, practical procedures to mitigate the problem of hydrogen outgassing from lithium hydride are discussed.

Obtaining zircaloy powder through hydriding

International Nuclear Information System (INIS)

Dupim, Ivaldete da Silva; Moreira, Joao M.L.

2009-01-01

Zirconium alloys are good options for the metal matrix in dispersion fuels for power reactors due to their low thermal neutron absorption cross-section, good corrosion resistance, good mechanical strength and high thermal conductivity. A necessary step for obtaining such fuels is producing Zr alloy powder for the metal matrix composite material. This article presents results from the Zircaloy-4 hydrogenation tests with the purpose to embrittle the alloy as a first step for comminuting. Several hydrogenation tests were performed and studied through thermogravimetric analysis. They included H 2 pressures of 25 and 50 kPa and temperatures ranging between from 20 to 670 deg C. X-ray diffraction analysis showed in the hydrogenated samples the predominant presence of ZrH 2 and some ZrO 2 . Some kinetics parameters for the Zircaloy-4 hydrogenation reaction were obtained: the time required to reach the equilibrium state at the dwell temperature was about 100 minutes; the hydrogenation rate during the heating process from 20 to 670 deg C was about 21 mg/h, and at constant temperature of 670 deg C, the hydride rate was about 1.15 mg/h. The hydrogenation rate is largest during the heating process and most of it occurs during this period. After hydrogenated, the samples could easily be comminuted indicating that this is a possible technology to obtain Zircaloy powder. The results show that only few minutes of hydrogenation are necessary to reach the hydride levels required for comminuting the Zircaloy. The final hydride stoichiometry was between 2.7 and 2.8 H for each Zr atom in the sample (author)

Mechanical properties and fracture of titanium hydrides

International Nuclear Information System (INIS)

Koketsu, Hideyuki; Taniyama, Yoshihiro; Yonezu, Akio; Cho, Hideo; Ogawa, Takeshi; Takemoto, Mikio; Nakayama, Gen

2006-01-01

Titanium hydrides tend to suffer fracture when their thicknesses reach a critical thickness. Morphology and mechanical property of the hydrides are, however, not well known. The study aims to reveal the hydride morphology and fracture types of the hydrides. Chevron shaped plate hydrides were found to be produced on the surface of pure titanium (Grade 1) and Grade 7 titanium absorbing hydrogen. There were tree types of fracture of the hydrides, i.e., crack in hydride layer, exfoliation of the layer and shear-type fracture of the hydride plates, during the growth of the hydrides and deformation. We next estimated the true stress-strain curves of the hydrides on Grade 1 and 7 titanium using the dual Vickers indentation method, and the critical strain causing the Mode-I fine crack by indentation. Fracture strength and strain of the hydrides in Grade 1 titanium were estimated as 566 MPa and 4.5%, respectively. Those of the hydride in Grade 7 titanium were 498 MPa and 16%. Though the fracture strains estimated from the plastic instability of true stress-strain curves were approximately the half of those estimated by finite element method, the titanium hydrides were estimated to possess some extent of toughness or plastic deformation capability. (author)

Domino reactions initiated by intramolecular hydride transfers from tri(di)arylmethane fragments to ketenimine and carbodiimide functions.

Science.gov (United States)

Alajarin, Mateo; Bonillo, Baltasar; Ortin, Maria-Mar; Sanchez-Andrada, Pilar; Vidal, Angel; Orenes, Raul-Angel

2010-10-21

The ability of triarylmethane and diarylmethane fragments to behave as hydride donors participating in thermal [1,5]-H shift/6π-ERC tandem processes involving ketenimine and carbodiimide functions is disclosed. C-Alkyl-C-phenyl ketenimines N-substituted by a triarylmethane substructure convert into a variety of 3,3,4,4-tetrasubstituted-3,4-dihydroquinolines, as structurally related carbodiimides transform into 3,4,4-trisubstituted-3,4-dihydroquinazolines via transient ortho-azaxylylenes. The first step of these one-pot conversions, the [1,5]-H shift, is considered to be a hydride migration on the basis of the known hydricity of the tri(di)arylmethane fragment and the electrophilicity of the central heterocumulenic carbon atom, whereas the final electrocyclization involves the formation of a sterically congested C-C or C-N bond. In the cases of C,C-diphenyl substituted triarylmethane-ketenimines the usual 6π-ERC becomes prohibited by the presence of two phenyl rings at each end of the azatrienic system. This situation opens new reaction channels: (a) following the initial hydride shift, the tandem sequence continues with an alternative electrocyclization mode to give 9,10-dihydroacridines, (b) the full sequence is initiated by a rare 1,5 migration of an electron-rich aryl group, followed by a 6π-ERC which leads to 2-aryl-3,4-dihydroquinolines, or (c) a different [1,5]-H shift/6π-ERC sequence involving the initial migration of a hydrogen atom from a methyl group at the ortho position to the nitrogen atom of the ketenimine function. Diarylmethane-ketenimines bearing a methyl group at the benzylic carbon atom experience a tandem double [1,5]-H shift, the first one being the usual benzylic hydride transfer whereas the second one involves the methyl group at the initial benzylic carbon atom, the reaction products being 2-aminostyrenes. Diarylmethane-ketenimines lacking such a methyl group convert into 3,4-dihydroquinolines by the habitual tandem [1,5]-H shift/6�

Trapping interference effects of arsenic, antimony and bismuth hydrides in collection of selenium hydride within iridium-modified transversally-heated graphite tube atomizer

Czech Academy of Sciences Publication Activity Database

Furdíková, Zuzana; Dočekal, Bohumil

2009-01-01

Roč. 64, č. 4 (2009), s. 323-328 ISSN 0584-8547 R&D Projects: GA ČR GA203/06/1441 Institutional research plan: CEZ:AV0Z40310501 Keywords : selenium hydride trapping * arsine * stibine Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.719, year: 2009

Analysis of Ni-HYDRIDE Thin Film after Surface Plasmon Generation by Laser Technique

Science.gov (United States)

Violante, V.; Castagna, E.; Sibilia, C.; Paoloni, S.; Sarto, F.

2005-12-01

A nickel hydride thin film was studied by the attenuated total reflection method. The differences in behavior between a "black" film, and a pure nickel film "blank," are shown. The black nickel hydride film has been obtained by a short electrolysis with 1 M Li2SO4 electrolyte in light water, A shift in the minimum of the observed reflected light occurs, together with a change in the minimum shape (i.e. its half-height width increases). These two phenomenon are due to the change in the electronic band structure of the metal induced by electrons added to the lattice by hydrogen. The change of the electronic structure, revealed by the laser coupling conditions, leads us to consider that a hydride phase was created. Both the blank (not hydrogenated) and black (hydrogenated) specimens were taken under He-Ne laser beam at the reflectance minimum angle for about three hours. A SIMS analysis was also implemented to reveal differences in the isotopic composition of Cu, as marker element between the blank and black films, in order to study the coupled effect of electrolysis and plasmon-polariton excitation on LENR processes in condensed matter.

Fundamental experiments on hydride reorientation in zircaloy

Science.gov (United States)

Colas, Kimberly B.

In the current study, an in-situ X-ray diffraction technique using synchrotron radiation was used to follow directly the kinetics of hydride dissolution and precipitation during thermomechanical cycles. This technique was combined with conventional microscopy (optical, SEM and TEM) to gain an overall understanding of the process of hydride reorientation. Thus this part of the study emphasized the time-dependent nature of the process, studying large volume of hydrides in the material. In addition, a micro-diffraction technique was also used to study the spatial distribution of hydrides near stress concentrations. This part of the study emphasized the spatial variation of hydride characteristics such as strain and morphology. Hydrided samples in the shape of tensile dog-bones were used in the time-dependent part of the study. Compact tension specimens were used during the spatial dependence part of the study. The hydride elastic strains from peak shift and size and strain broadening were studied as a function of time for precipitating hydrides. The hydrides precipitate in a very compressed state of stress, as measured by the shift in lattice spacing. As precipitation proceeds the average shift decreases, indicating average stress is reduced, likely due to plastic deformation and morphology changes. When nucleation ends the hydrides follow the zirconium matrix thermal contraction. When stress is applied below the threshold stress for reorientation, hydrides first nucleate in a very compressed state similar to that of unstressed hydrides. After reducing the average strain similarly to unstressed hydrides, the average hydride strain reaches a constant value during cool-down to room temperature. This could be due to a greater ease of deforming the matrix due to the applied far-field strain which would compensate for the strains due to thermal contraction. Finally when hydrides reorient, the average hydride strains become tensile during the first precipitation regime and

A Study on the Radial Hydride Assisted Delayed Hydride Cracking of Zircaloy

Energy Technology Data Exchange (ETDEWEB)

Jeong, Jin-Ho; Lee, Ji-Min; Kim, Yong-Soo [Hanyang University, Seoul (Korea, Republic of)

2015-05-15

Extensive studies have been done on understanding of DHC(Delayed hydride cracking) phenomenon since several zirconium alloy pressure tubes failed in nuclear reactor in the 1970s. Recently, long-term dry storage strategy has been considered seriously in order to manage spent nuclear fuel in Korea and other countries around the world. Consequentially, many researches have been investigated the degradation mechanisms which will threaten the spent fuel integrity during dry storage and showed that hydrogen related phenomenon such as hydride reorientation and DHC are the critical factors. Especially, DHC is the direct cracking mechanism which can cause not only a through-wall defect but also a radiation leak to the environment. In addition, DHC can be enhanced by radial hydride as reported by Kim who demonstrate that radial hydrides clearly act as crack linkage path. This phenomenon is known as the radial hydride assisted DHC (RHA-DHC). Therefore, study on DHC is essential to ensure the safety of spent fuel. Finite element analysis will be carried out for the stress gradient evaluation around notch tip. A variation in thermal cycle which leads to change in hydrogen solid solution trajectory may be required. If the radial hydride precipitates at notch tip, we will investigate what conditions should be met. Ultimately, we will suggest the regulation criteria for long-term dry storage of spent nuclear fuel.

Determination of thermodynamic affinities of various polar olefins as hydride, hydrogen atom, and electron acceptors in acetonitrile.

Science.gov (United States)

Cao, Ying; Zhang, Song-Chen; Zhang, Min; Shen, Guang-Bin; Zhu, Xiao-Qing

2013-07-19

A series of 69 polar olefins with various typical structures (X) were synthesized and the thermodynamic affinities (defined in terms of the molar enthalpy changes or the standard redox potentials in this work) of the polar olefins obtaining hydride anions, hydrogen atoms, and electrons, the thermodynamic affinities of the radical anions of the polar olefins (X(•-)) obtaining protons and hydrogen atoms, and the thermodynamic affinities of the hydrogen adducts of the polar olefins (XH(•)) obtaining electrons in acetonitrile were determined using titration calorimetry and electrochemical methods. The pure C═C π-bond heterolytic and homolytic dissociation energies of the polar olefins (X) in acetonitrile and the pure C═C π-bond homolytic dissociation energies of the radical anions of the polar olefins (X(•-)) in acetonitrile were estimated. The remote substituent effects on the six thermodynamic affinities of the polar olefins and their related reaction intermediates were examined using the Hammett linear free-energy relationships; the results show that the Hammett linear free-energy relationships all hold in the six chemical and electrochemical processes. The information disclosed in this work could not only supply a gap of the chemical thermodynamics of olefins as one class of very important organic unsaturated compounds but also strongly promote the fast development of the chemistry and applications of olefins.

gamma-Zr-Hydride Precipitate in Irradiated Massive delta- Zr-Hydride

DEFF Research Database (Denmark)

Warren, M. R.; Bhattacharya, D. K.

1975-01-01

During examination of A Zircaloy-2-clad fuel pin, which had been part of a test fuel assembly in a boiling water reactor, several regions of severe internal hydriding were noticed in the upper-plenum end of the pin. Examination of similar fuel pins has shown that hydride of this type is caused by...... to irradiation-induced swelling....

The effect of stress state on zirconium hydride reorientation

Science.gov (United States)

Cinbiz, Mahmut Nedim

Prior to storage in a dry-cask facility, spent nuclear fuel must undergo a vacuum drying cycle during which the spent fuel rods are heated up to elevated temperatures of ≤ 400°C to remove moisture the canisters within the cask. As temperature increases during heating, some of the hydride particles within the cladding dissolve while the internal gas pressure in fuel rods increases generating multi-axial hoop and axial stresses in the closed-end thin-walled cladding tubes. As cool-down starts, the hydrogen in solid solution precipitates as hydride platelets, and if the multiaxial stresses are sufficiently large, the precipitating hydrides reorient from their initial circumferential orientation to radial orientation. Radial hydrides can severely embrittle the spent nuclear fuel cladding at low temperature in response to hoop stress loading. Because the cladding can experience a range of stress states during the thermo-mechanical treatment induced during vacuum drying, this study has investigated the effect of stress state on the process of hydride reorientation during controlled thermo-mechanical treatments utilizing the combination of in situ X-ray diffraction and novel mechanical testing analyzed by the combination of metallography and finite element analysis. The study used cold worked and stress relieved Zircaloy-4 sheet containing approx. 180 wt. ppm hydrogen as its material basis. The failure behavior of this material containing radial hydrides was also studied over a range of temperatures. Finally, samples from reactor-irradiated cladding tubes were examined by X-ray diffraction using synchrotron radiation. To reveal the stress state effect on hydride reorientation, the critical threshold stress to reorient hydrides was determined by designing novel mechanical test samples which produce a range of stress states from uniaxial to "near-equibiaxial" tension when a load is applied. The threshold stress was determined after thermo-mechanical treatments by

JWST Associations overview: automated generation of combined products

Science.gov (United States)

Alexov, Anastasia; Swade, Daryl; Bushouse, Howard; Diaz, Rosa; Eisenhamer, Jonathan; Hack, Warren; Kyprianou, Mark; Levay, Karen; Rahmani, Christopher; Swam, Mike; Valenti, Jeff

2018-01-01

We are presenting the design of the James Webb Space Telescope (JWST) Data Management System (DMS) automated processing of Associations. An Association captures the relationship between exposures and higher level data products, such as combined mosaics created from dithered and tiled observations. The astronomer’s intent is captured within the Proposal Planning System (PPS) and provided to DMS as candidate associations. These candidates are converted into Association Pools and Association Generator Tables that serve as input to automated processing which create the combined data products. Association Pools are generated to capture a list of exposures that could potentially form associations and provide relevant information about those exposures. The Association Generator using definitions on groupings creates one or more Association Tables from a single input Association Pool. Each Association Table defines a set of exposures to be combined and the ruleset of the combination to be performed; the calibration software creates Associated data products based on these input tables. The initial design produces automated Associations within a proposal. Additionally this JWST overall design is conducive to eventually produce Associations for observations from multiple proposals, similar to the Hubble Legacy Archive (HLA).

Well-Defined Silica Supported Aluminum Hydride: Another Step Towards the Utopian Single Site Dream?

KAUST Repository

Werghi, Baraa; Bendjeriou-Sedjerari, Anissa; Sofack-Kreutzer, Julien; Jedidi, Abdesslem; Abou-Hamad, Edy; Cavallo, Luigi; Basset, Jean-Marie

2015-01-01

Reaction of triisobutylaluminum with SBA15700 at room temperature occurs by two parallel pathways involving either silanol or siloxane bridges. It leads to the formation of a well-defined bipodal [(≡SiO)2Al-CH2CH(CH3)2] 1a, silicon isobutyl [≡Si-CH2CH(CH3)2] 1b and a silicon hydride [≡Si-H] 1c. Their structural identity was characterized by FT-IR and advance solid-state NMR spectroscopies (1H, 13C, 29Si, 27Al and 2D multiple quantum), elemental and gas phase analysis, and DFT calculations. The reaction involves the formation of a highly reactive monopodal intermediate: [≡SiO-Al-[CH2CH(CH3)2]2], with evolution of isobutane. This intermediate undergoes two parallel routes: Transfer of either one isobutyl fragment or of one hydride to an adjacent silicon atom. Both processes occur by opening of a strained siloxane bridge, ≡Si-O-Si≡ but with two different mechanisms, showing that the reality of “single site” catalyst may be an utopia: DFT calculations indicate that isobutyl transfer occurs via a simple metathesis between the Al-isobutyl and O-Si bonds, while hydride transfer occurs via a two steps mechanism, the first one is a ß-H elimination to Al with elimination of isobutene, whereas the second is a metathesis step between the formed Al-H bond and a O-Si bond. Thermal treatment of 1a (at 250 °C) under high vacuum (10-5 mbar) generates Al-H through a ß-H elimination of isobutyl fragment. These supported well-defined Al-H which are highly stable with time, are tetra, penta and octa coordinated as demonstrated by IR and 27Al–1H J-HMQC NMR spectroscopy. All these observations indicate that surfaces atoms around the site of grafting play a considerable role in the reactivity of a single site system.

Well-Defined Silica Supported Aluminum Hydride: Another Step Towards the Utopian Single Site Dream?

KAUST Repository

Werghi, Baraa

2015-07-17

Reaction of triisobutylaluminum with SBA15700 at room temperature occurs by two parallel pathways involving either silanol or siloxane bridges. It leads to the formation of a well-defined bipodal [(≡SiO)2Al-CH2CH(CH3)2] 1a, silicon isobutyl [≡Si-CH2CH(CH3)2] 1b and a silicon hydride [≡Si-H] 1c. Their structural identity was characterized by FT-IR and advance solid-state NMR spectroscopies (1H, 13C, 29Si, 27Al and 2D multiple quantum), elemental and gas phase analysis, and DFT calculations. The reaction involves the formation of a highly reactive monopodal intermediate: [≡SiO-Al-[CH2CH(CH3)2]2], with evolution of isobutane. This intermediate undergoes two parallel routes: Transfer of either one isobutyl fragment or of one hydride to an adjacent silicon atom. Both processes occur by opening of a strained siloxane bridge, ≡Si-O-Si≡ but with two different mechanisms, showing that the reality of “single site” catalyst may be an utopia: DFT calculations indicate that isobutyl transfer occurs via a simple metathesis between the Al-isobutyl and O-Si bonds, while hydride transfer occurs via a two steps mechanism, the first one is a ß-H elimination to Al with elimination of isobutene, whereas the second is a metathesis step between the formed Al-H bond and a O-Si bond. Thermal treatment of 1a (at 250 °C) under high vacuum (10-5 mbar) generates Al-H through a ß-H elimination of isobutyl fragment. These supported well-defined Al-H which are highly stable with time, are tetra, penta and octa coordinated as demonstrated by IR and 27Al–1H J-HMQC NMR spectroscopy. All these observations indicate that surfaces atoms around the site of grafting play a considerable role in the reactivity of a single site system.

A Recommendation Algorithm for Automating Corollary Order Generation

Science.gov (United States)

Klann, Jeffrey; Schadow, Gunther; McCoy, JM

2009-01-01

Manual development and maintenance of decision support content is time-consuming and expensive. We explore recommendation algorithms, e-commerce data-mining tools that use collective order history to suggest purchases, to assist with this. In particular, previous work shows corollary order suggestions are amenable to automated data-mining techniques. Here, an item-based collaborative filtering algorithm augmented with association rule interestingness measures mined suggestions from 866,445 orders made in an inpatient hospital in 2007, generating 584 potential corollary orders. Our expert physician panel evaluated the top 92 and agreed 75.3% were clinically meaningful. Also, at least one felt 47.9% would be directly relevant in guideline development. This automated generation of a rough-cut of corollary orders confirms prior indications about automated tools in building decision support content. It is an important step toward computerized augmentation to decision support development, which could increase development efficiency and content quality while automatically capturing local standards. PMID:20351875

Effects of δ-hydride precipitation at a crack tip on crack propagation in delayed hydride cracking of Zircaloy-2

Energy Technology Data Exchange (ETDEWEB)

Kubo, T., E-mail: kubo@nfd.co.jp [Nippon Nuclear Fuel Development Co., Ltd., 2163 Narita-cho, Oarai-machi, Ibaraki 311-1313 (Japan); Kobayashi, Y. [M.O.X. Co., Ltd., 1828-520 Hirasu-cho, Mito, Ibaraki 311-0853 (Japan)

2013-08-15

Highlights: • Steady state crack velocity of delayed hydride cracking in Zircaloy-2 was analyzed. • A large stress peak is induced at an end of hydride by volume expansion of hydride. • Hydrogen diffuses to the stress peak, thereby accelerating steady hydride growth. • Crack velocity was estimated from the calculated hydrogen flux into the stress peak. • There was good agreement between calculation results and experimental data. -- Abstract: Delayed hydride cracking (DHC) of Zircaloy-2 is one possible mechanism for the failure of boiling water reactor fuel rods in ramp tests at high burnup. Analyses were made for hydrogen diffusion around a crack tip to estimate the crack velocity of DHC in zirconium alloys, placing importance on effects of precipitation of δ-hydride. The stress distribution around the crack tip is significantly altered by precipitation of hydride, which was strictly analyzed using a finite element computer code. Then, stress-driven hydrogen diffusion under the altered stress distribution was analyzed by a differential method. Overlapping of external stress and hydride precipitation at a crack tip induces two stress peaks; one at a crack tip and the other at the front end of the hydride precipitate. Since the latter is larger than the former, more hydrogen diffuses to the front end of the hydride precipitate, thereby accelerating hydride growth compared with that in the absence of the hydride. These results indicated that, after hydride was formed in front of the crack tip, it grew almost steadily accompanying the interaction of hydrogen diffusion, hydride growth and the stress alteration by hydride precipitation. Finally, crack velocity was estimated from the calculated hydrogen flux into the crack tip as a function of temperature, stress intensity factor and material strength. There was qualitatively good agreement between calculation results and experimental data.

Automating Visualization Service Generation with the WATT Compiler

Science.gov (United States)

Bollig, E. F.; Lyness, M. D.; Erlebacher, G.; Yuen, D. A.

2007-12-01

As tasks and workflows become increasingly complex, software developers are devoting increasing attention to automation tools. Among many examples, the Automator tool from Apple collects components of a workflow into a single script, with very little effort on the part of the user. Tasks are most often described as a series of instructions. The granularity of the tasks dictates the tools to use. Compilers translate fine-grained instructions to assembler code, while scripting languages (ruby, perl) are used to describe a series of tasks at a higher level. Compilers can also be viewed as transformational tools: a cross-compiler can translate executable code written on one computer to assembler code understood on another, while transformational tools can translate from one high-level language to another. We are interested in creating visualization web services automatically, starting from stand-alone VTK (Visualization Toolkit) code written in Tcl. To this end, using the OCaml programming language, we have developed a compiler that translates Tcl into C++, including all the stubs, classes and methods to interface with gSOAP, a C++ implementation of the Soap 1.1/1.2 protocols. This compiler, referred to as the Web Automation and Translation Toolkit (WATT), is the first step towards automated creation of specialized visualization web services without input from the user. The WATT compiler seeks to automate all aspects of web service generation, including the transport layer, the division of labor and the details related to interface generation. The WATT compiler is part of ongoing efforts within the NSF funded VLab consortium [1] to facilitate and automate time-consuming tasks for the science related to understanding planetary materials. Through examples of services produced by WATT for the VLab portal, we will illustrate features, limitations and the improvements necessary to achieve the ultimate goal of complete and transparent automation in the generation of web

Hydride effect on crack instability of Zircaloy cladding

Energy Technology Data Exchange (ETDEWEB)

Tseng, Che-Chung, E-mail: cctseng@iner.gov.tw [Institute of Nuclear Energy Research, No. 1000, Wunhua Road, Jiaan Village, Lungtan, Township, Taoyuan County 32546, Taiwan (China); Sun, Ming-Hung [Institute of Nuclear Energy Research, No. 1000, Wunhua Road, Jiaan Village, Lungtan, Township, Taoyuan County 32546, Taiwan (China); Chao, Ching-Kong [Department of Mechanical Engineering, National Taiwan University of Science and Technology, 43 Keelung Road, Section 4, Taipei 106, Taiwan (China)

2014-04-01

Highlights: • Radial hydrides near the crack tip had a significant effect on crack propagation. • For radial hydrides off the crack line vertically, the effect on crack propagation was notably reduced. • The longer hydride platelet resulted in a remarkable effect on crack propagation. • A long split in the radial hydride precipitate would enhance crack propagation. • The presence of circumferential hydride among radial hydrides may play an important role in crack propagation. - Abstract: A methodology was proposed to investigate the effect of hydride on the crack propagation in fuel cladding. The analysis was modeled based on an outside-in crack with radial hydrides located near its crack tip. The finite element method was used in the calculation; both stress intensity factor K{sub I} and J integral were applied to evaluate the crack stability. The parameters employed in the analysis included the location of radial hydride, hydride dimensions, number of hydrides, and the presence of circumferential hydride, etc. According to our study, the effective distance between a radial hydride and the assumed cladding surface crack for the enhancement of crack propagation proved to be no greater than 0.06 mm. For a hydride not on the crack line, it would induce a relatively minor effect on crack propagation if the vertical distance was beyond 0.05 mm. However, a longer hydride precipitate as well as double radial hydrides could have a remarkable effect on crack propagation. A combined effect of radial and circumferential hydrides was also discussed.

A new ternary magnesium-titanium hydride Mg{sub 7}TiH{sub x} with hydrogen desorption properties better than both binary magnesium and titanium hydrides

Energy Technology Data Exchange (ETDEWEB)

Kyoi, Daisuke; Sato, Toyoto; Roennebro, Ewa; Kitamura, Naoyuki; Ueda, Atsushi; Ito, Mikio; Katsuyama, Shigeru; Hara, Shigeta; Noreus, Dag; Sakai, Tetsuo

2004-06-09

A magnesium based titanium doped hydride was prepared in a high-pressure anvil cell by reacting a mixture of MgH{sub 2} and TiH{sub 1.9} at 8 GPa and 873 K. The metal structure has a Ca{sub 7}Ge type structure (a=9.532(2) A, space group Fm3-barm (no. 225), Z=4, V=866.06 A{sup 3}). The refined metal atom composition Mg{sub 7}Ti was almost in line with EDS analysis. This means that the new magnesium-titanium hydride has a structure that is more related to TiH{sub 1.9} than to MgH{sub 2}. The thermal properties of the new compound were also studied by TPD analysis. The new hydride, Mg{sub 7}TiH{sub x} exhibits 5.5 mass% (x{approx}12.7) and decomposes into Mg and TiH{sub 1.9} upon releasing 4.7 mass% of hydrogen around 605 K, that is at a 130 and 220 K lower desorption temperature compared to MgH{sub 2} and TiH{sub 1.9}, respectively.

Experimental investigation of strain, damage and failure of hydrided zircaloy-4 with various hydride orientations

International Nuclear Information System (INIS)

Racine, A; Catherine, C.S.; Cappelaere, C.; Bornert, M.; Caldemaison, D.

2005-01-01

This experimental investigation is devoted to the influence of the orientation of hydrides on the mechanical response of Zircaloy-4. Ring tensile tests are performed on unirradiated CWSR Zircaloy-4, charged with about 200 or 500wppm hydrogen. Hydrides are oriented either parallel ('tangential'), or perpendicular ('radial') to the circumferential tensile direction. Tangential hydrides are usually observed in cladding tubes, however, hydrides can be reoriented after cooling under stress to become radial and then trigger brittle behavior. In this investigation, we perform, 'macroscopic' or SEM in-situ tensile tests on smooth rings, at room temperature. We get the mechanical response of the material as a function of hydride orientation and hydrogen content and we investigate the deformation, damage and failure mechanisms. In both cases, digital image correlation techniques are used to estimate local and global strain distributions. The results lead to the following conclusions: neither the tensile stress-strain response nor the strain modes are affected by hydrogen content or hydride orientation, but the failure modes are. Indeed, only 200wppm radial hydrides embrittle Zy-4: sample fails in the elastic domain at about 350 MPa before strain bands could develop; whereas in other cases samples reach at least 750 MPa before failure, with ductile or brittle mode. (authors)

Automated generation of lattice QCD Feynman rules

Energy Technology Data Exchange (ETDEWEB)

Hart, A.; Mueller, E.H. [Edinburgh Univ. (United Kingdom). SUPA School of Physics and Astronomy; von Hippel, G.M. [Deutsches Elektronen-Synchrotron (DESY), Zeuthen (Germany); Horgan, R.R. [Cambridge Univ. (United Kingdom). DAMTP, CMS

2009-04-15

The derivation of the Feynman rules for lattice perturbation theory from actions and operators is complicated, especially for highly improved actions such as HISQ. This task is, however, both important and particularly suitable for automation. We describe a suite of software to generate and evaluate Feynman rules for a wide range of lattice field theories with gluons and (relativistic and/or heavy) quarks. Our programs are capable of dealing with actions as complicated as (m)NRQCD and HISQ. Automated differentiation methods are used to calculate also the derivatives of Feynman diagrams. (orig.)

Automated generation of lattice QCD Feynman rules

International Nuclear Information System (INIS)

Hart, A.; Mueller, E.H.; Horgan, R.R.

2009-04-01

The derivation of the Feynman rules for lattice perturbation theory from actions and operators is complicated, especially for highly improved actions such as HISQ. This task is, however, both important and particularly suitable for automation. We describe a suite of software to generate and evaluate Feynman rules for a wide range of lattice field theories with gluons and (relativistic and/or heavy) quarks. Our programs are capable of dealing with actions as complicated as (m)NRQCD and HISQ. Automated differentiation methods are used to calculate also the derivatives of Feynman diagrams. (orig.)

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

Science.gov (United States)

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

Automated test data generation for branch testing using incremental

Indian Academy of Sciences (India)

Cost of software testing can be reduced by automated test data generation to find a minimal set of data that has maximum coverage. Search-based software testing (SBST) is one of the techniques recently used for automated testing task. SBST makes use of control flow graph (CFG) and meta-heuristic search algorithms to ...

Cassini Tour Atlas Automated Generation

Science.gov (United States)

Grazier, Kevin R.; Roumeliotis, Chris; Lange, Robert D.

2011-01-01

During the Cassini spacecraft s cruise phase and nominal mission, the Cassini Science Planning Team developed and maintained an online database of geometric and timing information called the Cassini Tour Atlas. The Tour Atlas consisted of several hundreds of megabytes of EVENTS mission planning software outputs, tables, plots, and images used by mission scientists for observation planning. Each time the nominal mission trajectory was altered or tweaked, a new Tour Atlas had to be regenerated manually. In the early phases of Cassini s Equinox Mission planning, an a priori estimate suggested that mission tour designers would develop approximately 30 candidate tours within a short period of time. So that Cassini scientists could properly analyze the science opportunities in each candidate tour quickly and thoroughly so that the optimal series of orbits for science return could be selected, a separate Tour Atlas was required for each trajectory. The task of manually generating the number of trajectory analyses in the allotted time would have been impossible, so the entire task was automated using code written in five different programming languages. This software automates the generation of the Cassini Tour Atlas database. It performs with one UNIX command what previously took a day or two of human labor.

Hydriding failure in water reactor fuel elements

International Nuclear Information System (INIS)

Sah, D.N.; Ramadasan, E.; Unnikrishnan, K.

1980-01-01

Hydriding of the zircaloy cladding has been one of the important causes of failure in water reactor fuel elements. This report reviews the causes, the mechanisms and the methods for prevention of hydriding failure in zircaloy clad water reactor fuel elements. The different types of hydriding of zircaloy cladding have been classified. Various factors influencing zircaloy hydriding from internal and external sources in an operating fuel element have been brought out. The findings of post-irradiation examination of fuel elements from Indian reactors, with respect to clad hydriding and features of hydriding failure are included. (author)

[Study on Content Determination of Lead and Arsenic in Four Traditional Tibetan Medicine Prescription Preparations by Wet Digestion Flow Injection-Hydride Generation-Atomic Absorption Spectrometry].

Science.gov (United States)

Zheng, Zhi-yuan; Du, Yu-zhi; Zhang, Ming; Yu, Ming-jie; Li, Cen; Yang, Hong-xia; Zhao, Jing; Xia, Zheng-hua; Wei, Li-xin

2015-04-01

Four common traditional tibetan medicine prescription preparations "Anzhijinghuasan, Dangzuo, Renqingchangjue and Rannasangpei" in tibetan areas were selected as study objects in the present study. The purpose was to try to establish a kind of wet digestion and flow injection-hydride generation-atomic absorption spectrometry (FI-HAAS) associated analysis method for the content determinations of lead and arsenic in traditional tibetan medicine under optimized digestion and measurement conditions and determine their contents accurately. Under these optimum operating conditions, experimental results were as follows. The detection limits for lead and arsenic were 0.067 and 0.012 µg · mL(-1) respectively. The quantification limits for lead and arsenic were 0.22 and 0.041 µg · mL(-1) respectively. The linear ranges for lead and arsenic were 25-1,600 ng · mL(-1) (r = 0.9995) and 12.5-800 ng · mL(-1) (r = 0.9994) respectively. The degrees of precision(RSD) for lead and arsenic were 2.0% and 3.2% respectively. The recovery rates for lead and arsenic were 98.00%-99.98% and 96.67%-99.87% respectively. The content determination results of lead and arsenic in four traditional tibetan medicine prescription preparations were as fol- lows. The contents of lead and arsenic in Anzhijinghuasan are 0.63-0.67 µg · g(-1) and 0.32-0.33 µg · g(-1) in Anzhijinghua- san, 42.92-43.36 µg · g(-1) and 24.67-25.87 µg · g(-1) in Dangzuo, 1,611. 39-1,631.36 µg · g(-1) and 926.76-956.52 µg- g(-1) in Renqing Changjue, and 1,102.28-1,119.127 µg-g(-1) and 509.96-516.87 µg · g(-1) in Rannasangpei, respectively. This study established a method for content determination of lead and arsenic in traditional tibetan medicine, and determined the content levels of lead and arsenic in four tibetan medicine-prescription preparations accurately. In addition, these results also provide the basis for the safe and effective use of those medicines in clinic.

Comparative oxidation state specific analysis of arsenic species by high-performance liquid chromatography-inductively coupled-mass spectrometry and hydride generation-cryotrapping-atomic absorption spectrometry

Science.gov (United States)

The formation of methylarsonous acid (MAsIII) and dimethylarsinous acid (DMAsIII) in the course of inorganic arsenic (iAs) metabolism plays an important role in the adverse effects of chronic exposure to iAs. High-performance liquid chromatography-inductively coupled plasma-mass ...

Preparation of beryllium hydride

International Nuclear Information System (INIS)

Roberts, C.B.

1975-01-01

A process is described for preparing beryllium hydride by the direct reaction of beryllium borohydride and aluminum hydride trimethylamine adduct. Volatile by-products and unreacted reactants are readily removed from the product mass by sublimation and/or evaporation. (U.S.)

Kinetics of hydrogen evolution in the thermal dissociation of the hydride ZrNiH /SUB 2.8/

International Nuclear Information System (INIS)

Chernavskii, P.A.; Lunin, V.V.

1985-01-01

The kinetics of hydrogen evolution in the thermal decomposition of ZrNiH /SUB 2.8/ has been studied. The kinetic curve has two rate maxima. It is presumed that the second maximum is related to the phenomenon of critical inhibition that accompanies the phase transition. Apparent activation energies were determined for hydrogen evolution in argon and argon-ethylene atmospheres. The apparent energy increases in the argon-ethylene mixture. On the basis of the activation energy measurements it is presumed that the rate-determining step in hydrogen evolution is either the formation of hydrogen molecules from atoms on the surface of the lateral diffusion of atomic hydrogen. In the region of hydrogen concentration in the hydride corresponding to the phase transition, the rate-determining step is hydrogen diffusion in the hydride

Arsine and selenium hydride trapping in a novel quartz device for atomic-absorption spectrometry

Czech Academy of Sciences Publication Activity Database

Kratzer, Jan; Dědina, Jiří

2007-01-01

Roč. 388, č. 4 (2007), s. 793-800 ISSN 1618-2642 R&D Projects: GA AV ČR IAA400310507 Institutional research plan: CEZ:AV0Z40310501 Keywords : HG-AAS * quartz surface * hydride trapping Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.867, year: 2007

The influence of surface morphology and oxide microstructure on the nucleation and growth of uranium hydride on alpha uranium

International Nuclear Information System (INIS)

Hanrahan, R.J. Jr.; Hawley, M.E.; Brown, G.W.

1998-01-01

While the bulk kinetics of the uranium-hydrogen reaction are well understood, the mechanisms underlying the initial nucleation of uranium hydride on uranium remain controversial. In this study, the authors have employed environmental cell optical microscopy, Scanning Electron Microscopy (SEM) and Atomic Force Microscopy, (AFM) in an attempt to relate the structure of the surface and the microstructure of the substrate with the susceptibility and site of hydride nucleation. Samples have been investigated with varying grain size, inclusion (carbide) concentration, and thermal history. There is a clear correlation to heat treatment immediately prior to hydrogen exposure. Susceptibility to hydride formation also appears to be related to impurities in the uranium. The oxidized surface is very complex, exhibiting wide variations in thickness and topography between samples, between grains in the same sample, and within individual grains. It is, however, very difficult to relate this fine scale variability to the relatively sparse hydride initiation sites. Therefore, the surface oxide layer itself does not appear to control the sites where hydride attack is initiated, although it must play a role in the induction period prior to hydride initiation

The influence of surface morphology and oxide microstructure on the nucleation and growth of uranium hydride on alpha uranium

Energy Technology Data Exchange (ETDEWEB)

Hanrahan, R.J. Jr.; Hawley, M.E.; Brown, G.W. [Los Alamos National Lab., NM (United States). Materials Science and Technology Div.

1998-12-31

While the bulk kinetics of the uranium-hydrogen reaction are well understood, the mechanisms underlying the initial nucleation of uranium hydride on uranium remain controversial. In this study the authors have employed environmental cell optical microscopy, Scanning Electron Microscopy (SEM) and Atomic Force Microscopy, (AFM) in an attempt to relate the structure of the surface and the microstructure of the substrate with the susceptibility and site of hydride nucleation. Samples have been investigated with varying grain size, inclusion (carbide) concentration, and thermal history. There is a clear correlation to heat treatment immediately prior to hydrogen exposure. Susceptibility to hydride formation also appears to be related to impurities in the uranium. The oxidized surface is very complex, exhibiting wide variations in thickness and topography between samples, between grains in the same sample, and within individual grains. It is, however, very difficult to relate this fine scale variability to the relatively sparse hydride initiation sites. Therefore, the surface oxide layer itself does not appear to control the sites where hydride attack is initiated, although it must play a role in the induction period prior to hydride initiation.

The influence of surface morphology and oxide microstructure on the nucleation and growth of uranium hydride on alpha uranium

Energy Technology Data Exchange (ETDEWEB)

Hanrahan, R.J. Jr.; Hawley, M.E.; Brown, G.W.

1998-12-31

While the bulk kinetics of the uranium-hydrogen reaction are well understood, the mechanisms underlying the initial nucleation of uranium hydride on uranium remain controversial. In this study, the authors have employed environmental cell optical microscopy, Scanning Electron Microscopy (SEM) and Atomic Force Microscopy, (AFM) in an attempt to relate the structure of the surface and the microstructure of the substrate with the susceptibility and site of hydride nucleation. Samples have been investigated with varying grain size, inclusion (carbide) concentration, and thermal history. There is a clear correlation to heat treatment immediately prior to hydrogen exposure. Susceptibility to hydride formation also appears to be related to impurities in the uranium. The oxidized surface is very complex, exhibiting wide variations in thickness and topography between samples, between grains in the same sample, and within individual grains. It is, however, very difficult to relate this fine scale variability to the relatively sparse hydride initiation sites. Therefore, the surface oxide layer itself does not appear to control the sites where hydride attack is initiated, although it must play a role in the induction period prior to hydride initiation.

Rapid PMR determination of hydrogen in titanium hydride and dehydrogenated titanium powders

International Nuclear Information System (INIS)

Il'enko, V.S.; Demidenko, L.M.

1987-01-01

Proton magnetic resonance (PMR) enables determining hydrogen quantitatively in titanium hydride and dehydrogenated titanium powders without destroying the specimen and is also more informative than high-temperature extraction methods. PMR provides data on the electron-nuclear interactions and the activation energies for hydrogen diffusion while also providing conclusions on the forms and positives of the hydrogen in the lattice and the binding to the metal atoms. The authors have developed a rapid method for determining hydrogen in titanium hydride and dehydrogenated titanium powders which reduces the analysis time and improves the metrological characteristics. The authors use a YaMR-5535 spectrometer working at 40 MHz upgraded for use with hydrogen in solids. The authors used specimens of mass about 2 g ground to 0.1 mm powder

Performance study of a hydrogen powered metal hydride actuator

International Nuclear Information System (INIS)

Bhuiya, Md Mainul Hossain; Kim, Kwang J

2016-01-01

A thermally driven hydrogen powered actuator integrating metal hydride hydrogen storage reactor, which is compact, noiseless, and able to generate smooth actuation, is presented in this article. To test the plausibility of a thermally driven actuator, a conventional piston type actuator was integrated with LaNi 5 based hydrogen storage system. Copper encapsulation followed by compaction of particles into pellets, were adopted to improve overall thermal conductivity of the reactor. The operation of the actuator was thoroughly investigated for an array of operating temperature ranges. Temperature swing of the hydride reactor triggering smooth and noiseless actuation over several operating temperature ranges were monitored for quantification of actuator efficiency. Overall, the actuator generated smooth and consistent strokes during repeated cycles of operation. The efficiency of the actuator was found to be as high as 13.36% for operating a temperature range of 20 °C–50 °C. Stress–strain characteristics, actuation hysteresis etc were studied experimentally. Comparison of stress–strain characteristics of the proposed actuator with traditional actuators, artificial muscles and so on was made. The study suggests that design modification and use of high pressure hydride may enhance the performance and broaden the application horizon of the proposed actuator in future. (paper)

Generation of atom-photon entangled states in atomic Bose-Einstein condensate via electromagnetically induced transparency

International Nuclear Information System (INIS)

Kuang Leman; Zhou Lan

2003-01-01

In this paper, we present a method to generate continuous-variable-type entangled states between photons and atoms in atomic Bose-Einstein condensate (BEC). The proposed method involves an atomic BEC with three internal states, a weak quantized probe laser, and a strong classical coupling laser, which form a three-level Λ-shaped BEC system. We consider a situation where the BEC is in electromagnetically induced transparency with the coupling laser being much stronger than the probe laser. In this case, the upper and intermediate levels are unpopulated, so that their adiabatic elimination enables an effective two-mode model involving only the atomic field at the lowest internal level and the quantized probe laser field. Atom-photon quantum entanglement is created through laser-atom and interatomic interactions, and two-photon detuning. We show how to generate atom-photon entangled coherent states and entangled states between photon (atom) coherent states and atom-(photon-) macroscopic quantum superposition (MQS) states, and between photon-MQS and atom-MQS states

Air and metal hydride battery

Energy Technology Data Exchange (ETDEWEB)

Lampinen, M.; Noponen, T. [Helsinki Univ. of Technology, Otaniemi (Finland). Lab. of Applied Thermodynamics

1998-12-31

The main goal of the air and metal hydride battery project was to enhance the performance and manufacturing technology of both electrodes to such a degree that an air-metal hydride battery could become a commercially and technically competitive power source for electric vehicles. By the end of the project it was possible to demonstrate the very first prototype of the air-metal hydride battery at EV scale, achieving all the required design parameters. (orig.)

Determination of hydrogen in zirconium hydride and uranium-zirconium hydride by inert gas exraction-gravimetric method

International Nuclear Information System (INIS)

Hoshino, Akira; Iso, Shuichi

1976-01-01

An inert gas extraction-gravimetric method has been applied to the determination of hydrogen in zirconium hydride and uranium-zirconium hydride which are used as neutron moderator and fuel of nuclear safety research reactor (NSRR), respectively. The sample in a graphite-enclosed quartz crucible is heated inductively to 1200 0 C for 20 min in a helium stream. Hydrogen liberated from the sample is oxidized to water by copper(I) oxide-copper(II) oxide at 400 0 C, and the water is determined gravimetrically by absorption in anhydrone. The extraction curves of hydrogen for zirconium hydride and uranium-zirconium hydride samples are shown in Figs. 2 and 3. Hydrogen in the samples is extracted quantitatively by heating at (1000 -- 1250) 0 C for (10 -- 40) min. Recoveries of hydrogen in the case of zirconium hydride were examined as follows: a weighed zirconium rod (5 phi x 6 mm, hydrogen -5 Torr. After the chamber was filled with purified hydrogen to 200 Torr, the rod was heated to 400 0 C for 15 h, and again weighed to determine the increase in weight. Hydrogen in the rod was then determined by the proposed method. The results are in excellent agreement with the increase in weight as shown in Table 1. Analytical results of hydrogen in zirconium hydride samples and an uranium-zirconium hydride sample are shown in Table 2. (auth.)

Arrested α-hydride migration activates a phosphido ligand for C–H insertion

Energy Technology Data Exchange (ETDEWEB)

Hickey, Anne K. [Indiana Univ., Bloomington, IN (United States); Muñoz, Salvador B. [Indiana Univ., Bloomington, IN (United States); Lutz, Sean A. [Indiana Univ., Bloomington, IN (United States); Pink, Maren [Indiana Univ., Bloomington, IN (United States); Chen, Chun-Hsing [Indiana Univ., Bloomington, IN (United States); Smith, Jeremy M. [Indiana Univ., Bloomington, IN (United States)

2016-12-05

Bulky tris(carbene)borate ligands provide access to high spin iron(II) phosphido complexes. The complex PhB(MesIm)₃FeP(H)Ph is thermally unstable, and we observed [PPh] group insertion into a C–H bond of the supporting ligand. An arrested α-hydride migration mechanism suggests increased nucleophilicity of the phosphorus atom facilitates [PPh] group transfer reactivity.

Research and development of peripheral technology for photovoltaic power systems. Study of nickel-hydride storage battery for photovoltaic generation systems; Shuhen gijutsu no kenkyu kaihatsu. Taiyoko hatsuden`yo suiso denchi no kenkyu kaihatsu

Energy Technology Data Exchange (ETDEWEB)

Tatsuta, M [New Energy and Industrial Technology Development Organization, Tokyo (Japan)

1994-12-01

This paper reports the study results on R and D of nickel-hydride storage battery for photovoltaic generation systems in fiscal 1994. (1) On the study on low-cost electrode materials, the physical properties and electrode characteristics were studied of the prototype hydrogen absorbing alloys prepared by substituting Cu or Ni for Co in Mm(Ni-Co-Mn-Al)5 (Mm: mixture of rare earth elements). The result clarified that it is difficult to reduce Co content in the alloy to 0.4 atom or less. Simple heat treatment and milling processes in production of hydrogen absorbing alloy electrodes were achieved by adopting an improved metal mold and gas atomization method. Characteristics and cycle life of the Ni positive electrode prepared by applying active paste material of Ni(OH)2 were studied, however, the result showed only lives of nearly 300 cycles. (2) On the study on electrode structure for high-performance (long-life) battery, the 3-D porous metal electrode support was evaluated, and various battery configurations were studied. 11 figs., 1 tab.

Nanoindentation measurements of the mechanical properties of zirconium matrix and hydrides in unirradiated pre-hydrided nuclear fuel cladding

International Nuclear Information System (INIS)

Rico, A.; Martin-Rengel, M.A.; Ruiz-Hervias, J.; Rodriguez, J.; Gomez-Sanchez, F.J.

2014-01-01

It is well known that the mechanical properties of the nuclear fuel cladding may be affected by the presence of hydrides. The average mechanical properties of hydrided cladding have been extensively investigated from a macroscopic point of view. In addition, the mechanical and fracture properties of bulk hydride samples fabricated from zirconium plates have also been reported. In this paper, Young’s modulus, hardness and yield stress are measured for each phase, namely zirconium hydrides and matrix, of pre-hydrided nuclear fuel cladding. To this end, nanoindentation tests were performed on ZIRLO samples in as-received state, on a hydride blister and in samples with 150 and 1200 ppm of hydrogen homogeneously distributed along the hoop direction of the cladding. The results show that the measured mechanical properties of the zirconium hydrides and ZIRLO matrix (Young’s modulus, hardness and yield stress) are rather similar. From the experimental data, the hydride volume fraction in the cladding samples with 150 and 1200 ppm was estimated and the average mechanical properties were calculated by means of the rule of mixtures. These values were compared with those obtained from ring compression tests. Good agreement between the results obtained by both methods was found

Manganese Silylene Hydride Complexes: Synthesis and Reactivity with Ethylene to Afford Silene Hydride Complexes.

Science.gov (United States)

Price, Jeffrey S; Emslie, David J H; Britten, James F

2017-05-22

Reaction of the ethylene hydride complex trans-[(dmpe) 2 MnH(C 2 H 4 )] (1) with Et 2 SiH 2 at 20 °C afforded the silylene hydride [(dmpe) 2 MnH(=SiEt 2 )] (2 a) as the trans-isomer. By contrast, reaction of 1 with Ph 2 SiH 2 at 60 °C afforded [(dmpe) 2 MnH(=SiPh 2 )] (2 b) as a mixture of the cis (major) and trans (minor) isomers, featuring a Mn-H-Si interaction in the former. The reaction to form 2 b also yielded [(dmpe) 2 MnH 2 (SiHPh 2 )] (3 b); [(dmpe) 2 MnH 2 (SiHR 2 )] (R=Et (3 a) and Ph (3 b)) were accessed cleanly by reaction of 2 a and 2 b with H 2 , and the analogous reactions with D 2 afforded [(dmpe) 2 MnD 2 (SiHR 2 )] exclusively. Both 2 a and 2 b engaged in unique reactivity with ethylene, generating the silene hydride complexes cis-[(dmpe) 2 MnH(R 2 Si=CHMe)] (R=Et (4 a), Ph (4 b)). Compounds trans-2 a, cis-2 b, 3 b, and 4 b were crystallographically characterized, and bonding in 2 a, 2 b, 4 a, and 4 b was probed computationally. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Metal Hydride Compression

Energy Technology Data Exchange (ETDEWEB)

Johnson, Terry A. [Sandia National Lab. (SNL-CA), Livermore, CA (United States); Bowman, Robert [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Smith, Barton [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Anovitz, Lawrence [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jensen, Craig [Hawaii Hydrogen Carriers LLC, Honolulu, HI (United States)

2017-07-01

Conventional hydrogen compressors often contribute over half of the cost of hydrogen stations, have poor reliability, and have insufficient flow rates for a mature FCEV market. Fatigue associated with their moving parts including cracking of diaphragms and failure of seal leads to failure in conventional compressors, which is exacerbated by the repeated starts and stops expected at fueling stations. Furthermore, the conventional lubrication of these compressors with oil is generally unacceptable at fueling stations due to potential fuel contamination. Metal hydride (MH) technology offers a very good alternative to both conventional (mechanical) and newly developed (electrochemical, ionic liquid pistons) methods of hydrogen compression. Advantages of MH compression include simplicity in design and operation, absence of moving parts, compactness, safety and reliability, and the possibility to utilize waste industrial heat to power the compressor. Beyond conventional H2 supplies of pipelines or tanker trucks, another attractive scenario is the on-site generating, pressuring and delivering pure H₂ at pressure (≥ 875 bar) for refueling vehicles at electrolysis, wind, or solar generating production facilities in distributed locations that are too remote or widely distributed for cost effective bulk transport. MH hydrogen compression utilizes a reversible heat-driven interaction of a hydride-forming metal alloy with hydrogen gas to form the MH phase and is a promising process for hydrogen energy applications [1,2]. To deliver hydrogen continuously, each stage of the compressor must consist of multiple MH beds with synchronized hydrogenation & dehydrogenation cycles. Multistage pressurization allows achievement of greater compression ratios using reduced temperature swings compared to single stage compressors. The objectives of this project are to investigate and demonstrate on a laboratory scale a two-stage MH hydrogen (H₂) gas compressor with a

Design and integration of a hydrogen storage on metallic hydrides

International Nuclear Information System (INIS)

Botzung, M.

2008-01-01

This work presents a hydrogen storage system using metal hydrides for a Combined Heat and Power (CHP) system. Hydride storage technology has been chosen due to project specifications: high volumetric capacity, low pressures (≤ 3.5 bar) and low temperatures (≤ 75 C: fuel cell temperature). During absorption, heat from hydride generation is dissipated by fluid circulation. An integrated plate-fin type heat exchanger has been designed to obtain good compactness and to reach high absorption/desorption rates. At first, the storage system has been tested in accordance with project specifications (absorption 3.5 bar, desorption 1.5 bar). Then, the hydrogen charge/discharge times have been decreased to reach system limits. System design has been used to simulate thermal and mass comportment of the storage tank. The model is based on the software Fluent. We take in consideration heat and mass transfers in the porous media during absorption/desorption. The hydride thermal and mass behaviour has been integrated in the software. The heat and mass transfers experimentally obtained have been compared to results calculated by the model. The influence of experimental and numerical parameters on the model behaviour has also been explored. (author) [fr

Hydride generation-atomic absorption spectrometry for determination of trace arsenic in draining waste water of uranium hydrometallurgical plant

International Nuclear Information System (INIS)

Sun Suqing; Sun Shiying; Xue Jingxia

1986-01-01

The arsenate is reduced to the arsenite by potassium iodide-sulfourea in dilute sulphuric acid. Then the arsenite is reduced to arsine by sodium borohydride. The arsine carried into silica tube atomizer by nitrogen is atomized at 920 deg C and determined by the homemade atomic absorption instrument. It is shown that the sensitivity of the mentioned method is 0.2 ng/ml (1% absorption). The recovery is 88-103% and the relative standard deviation is ≤ 10%

The Effect of Hydrogen and Hydrides on the Integrity of Zirconium Alloy Components Delayed Hydride Cracking

CERN Document Server

Puls, Manfred P

2012-01-01

By drawing together the current theoretical and experimental understanding of the phenomena of delayed hydride cracking (DHC) in zirconium alloys, The Effect of Hydrogen and Hydrides on the Integrity of Zirconium Alloy Components: Delayed Hydride Cracking provides a detailed explanation focusing on the properties of hydrogen and hydrides in these alloys. Whilst the focus lies on zirconium alloys, the combination of both the empirical and mechanistic approaches creates a solid understanding that can also be applied to other hydride forming metals.   This up-to-date reference focuses on documented research surrounding DHC, including current methodologies for design and assessment of the results of periodic in-service inspections of pressure tubes in nuclear reactors. Emphasis is placed on showing that our understanding of DHC is supported by progress across a broad range of fields. These include hysteresis associated with first-order phase transformations; phase relationships in coherent crystalline metallic...

Epitaxial thin film growth of LiH using a liquid-Li atomic template

International Nuclear Information System (INIS)

Oguchi, Hiroyuki; Ikeshoji, Tamio; Orimo, Shin-ichi; Ohsawa, Takeo; Shiraki, Susumu; Hitosugi, Taro; Kuwano, Hiroki

2014-01-01

We report on the synthesis of lithium hydride (LiH) epitaxial thin films through the hydrogenation of a Li melt, forming abrupt LiH/MgO interface. Experimental and first-principles molecular dynamics studies reveal a comprehensive microscopic picture of the crystallization processes, which sheds light on the fundamental atomistic growth processes that have remained unknown in the vapor-liquid-solid method. We found that the periodic structure that formed, because of the liquid-Li atoms at the film/MgO-substrate interface, serves as an atomic template for the epitaxial growth of LiH crystals. In contrast, films grown on the Al 2 O 3 substrates indicated polycrystalline films with a LiAlO 2 secondary phase. These results and the proposed growth process provide insights into the preparation of other alkaline metal hydride thin films on oxides. Further, our investigations open the way to explore fundamental physics and chemistry of metal hydrides including possible phenomena that emerge at the heterointerfaces of metal hydrides

Identification and characterization of a new Zirconium hydride

International Nuclear Information System (INIS)

Zhao, Z.

2007-01-01

In order to control the integrity of the fuel clad, alloy of zirconium, it is necessary to predict the behavior of zirconium hydrides in the environment (temperature, stress...), at a microscopic scale. A characterization study by TEM of hydrides has been realized. It shows little hydrides about 500 nm, in hydride Zircaloy 4. Then a more detailed study identified a new hydride phase presented in this paper. (A.L.B.)

ADGEN: An automated adjoint code generator for large-scale sensitivity analysis

International Nuclear Information System (INIS)

Pin, F.G.; Oblow, E.M.; Horwedel, J.E.; Lucius, J.L.

1987-01-01

This paper describes a new automated system, named ADGEN, which makes use of the strengths of computer calculus to automate the costly and time-consuming calculation of derivatives in FORTRAN computer codes, and automatically generate adjoint solutions of computer codes

Density functional calculations of hypothetical neutral hollow octahedral molecules with a 48-atom framework: Hydrides and oxides of boron, carbon, nitrogen, aluminum, and silicon

International Nuclear Information System (INIS)

LaViolette, Randall A.; Benson, Michael T.

2000-01-01

We computed via first-principles density functional theory calculations (employing both the local density and generalized gradient approximations) the dimensions, bond lengths and angles, binding energy, and HOMO-LUMO gap of the following hypothetical neutral hollow octahedral molecules: B 48 H 24 , C 48 H 48 , C 96 H 80 (formed by bonding two C 48 H 48 molecules), N 48 H 24 , Al 48 H 24 , and Si 48 H 48 ; B 24 O 24 , C 24 O 24 , N 24 O 24 , Al 24 O 24 , and Si 24 O 24 . Each molecule consists of a large hollow framework of six puckered eight-membered rings whose planes are either mutually perpendicular or parallel, so that each molecule possesses only eight- and nine-membered rings. The hydrides have their hydrogen atoms attached only to the two-atom bridging sites on the framework. The oxides have their oxygen atoms occupying exclusively the two-atom bridging sites of the framework alternating with the (B, C, N, Al, Si) atoms exclusively occupying the three-atom bridging sites. We also calculated the infrared spectra of the C 48 H 48 and the C 24 O 24 molecules. For the sake of comparison, we also examined the hypothetical octahedral C 48 fullerene cuboctohedron (possessing four-, six-, and eight-membered rings) studied by Dunlap and Taylor. The molecules based on carbon would be the most stable; those based on nitrogen would be the least stable, if at all. (c) 2000 American Institute of Physics

Electrochemical generation of mercury cold vapor and its in-situ trapping in gold-covered graphite tube atomizers

International Nuclear Information System (INIS)

Cerveny, Vaclav; Rychlovsky, Petr; Netolicka, Jarmila; Sima, Jan

2007-01-01

The combination of more efficient flow-through electrochemical mercury cold vapor generation with its in-situ trapping in a graphite tube atomizer is described. This coupled technique has been optimized to attain the maximum sensitivity for Hg determination and to minimize the limits of detection and determination. A laboratory constructed thin-layer flow-through cell with a platinum cathode served as the cold vapor generator. Various cathode arrangements with different active surface areas were tested. Automated sampling equipment for the graphite atomizer with an untreated fused silica capillary was used for the introduction of the mercury vapor. The inner surface of the graphite tube was covered with a gold foil placed against the sampling hole. The results attained for the electrochemical mercury cold vapor generation (an absolute limit of detection of 80 pg; peak absorbance, 3σ criterion) were compared with the traditional vapor generation using NaBH 4 as the reducing agent (an absolute limit of detection of 124 pg; peak absorbance, 3σ criterion). The repeatability at the 5 ng ml -1 level was better than 4.1% (RSD) for electrochemical mercury vapor generation and better than 5.6% for the chemical cold vapor generation. The proposed method was applied to the determination the of Hg contents in a certified reference material and in spiked river water samples

A programmable Gaussian random pulse generator for automated performance measurements

International Nuclear Information System (INIS)

Abdel-Aal, R.E.

1989-01-01

This paper describes a versatile random signal generator which produces logic pulses with a Gaussian distribution for the pulse spacing. The average rate at the pulse generator output can be software-programmed, which makes it useful in performing automated measurements of dead time and CPU time performance of data acquisition systems and modules over a wide range of data rates. Hardware and software components are described and data on the input-output characteristics and the statistical properties of the pulse generator are given. Typical applications are discussed together with advantages over using radioactive test sources. Results obtained from an automated performance run on a VAX 11/785 data acquisition system are presented. (orig.)

Effects of Cooling Rates on Hydride Reorientation and Mechanical Properties of Zirconium Alloy Claddings under Interim Dry Storage Conditions

International Nuclear Information System (INIS)

Min, Su-Jeong; Kim, Myeong-Su; Won, Chu-chin; Kim, Kyu-Tae

2013-01-01

As-received Zr-Nb cladding tubes and 600 ppm hydrogen-charged tubes were employed to evaluate the effects of cladding cooling rates on the extent of hydride reorientation from circumferential hydrides to radial ones and mechanical property degradations with the use of cooling rates of 2, 4 and 15 °C/min from 400 °C to room temperature simulating cladding cooling under interim dry storage conditions. The as-received cladding tubes generated nearly the same ultimate tensile strengths and plastic elongations, regardless of the cooling rates, because of a negligible hydrogen content in the cladding. The 600 ppm-H cladding tubes indicate that the slower cooling rate generated the larger radial hydride fraction and the longer radial hydrides, which resulted in greater mechanical performance degradations. The cooling rate of 2 °C/min generates an ultimate tensile strength of 758 MPa and a plastic elongation of 1.0%, whereas the cooling rate of 15 °C/min generates an ultimate tensile strength of 825 MPa and a plastic elongation of 15.0%. These remarkable mechanical property degradations of the 600 ppm-H cladding tubes with the slowest cooling rate may be characterized by cleavage fracture surface appearance enhanced by longer radial hydrides and their higher fraction that have been precipitated through a relatively larger nucleation and growth rate.

Metal hydride compositions and lithium ion batteries

Energy Technology Data Exchange (ETDEWEB)

Young, Kwo; Nei, Jean

2018-04-24

Heterogeneous metal hydride (MH) compositions comprising a main region comprising a first metal hydride and a secondary region comprising one or more additional components selected from the group consisting of second metal hydrides, metals, metal alloys and further metal compounds are suitable as anode materials for lithium ion cells. The first metal hydride is for example MgH.sub.2. Methods for preparing the composition include coating, mechanical grinding, sintering, heat treatment and quenching techniques.

Hydride formation on deformation twin in zirconium alloy

Energy Technology Data Exchange (ETDEWEB)

Kim, Ju-Seong [Korea Atomic Energy Research Institute, 989-111 Daedeokdaero, Yuseong-gu, Daejeon, 305-353 (Korea, Republic of); Kim, Sung-Dae [Korea Institute of Material Science (KIMS), 797 Changwondaero, Changwon, Gyeongnam, 642-831 (Korea, Republic of); Yoon, Jonghun, E-mail: yooncsmd@gmail.com [Department of Mechanical Engineering, Hanyang University, 1271 Sa3-dong, Sangrok-gu, Ansan-si, Gyeonggi-do, 426-791 (Korea, Republic of)

2016-12-15

Hydrides deteriorate the mechanical properties of zirconium (Zr) alloys used in nuclear reactors. Intergranular hydrides that form along grain boundaries have been extensively studied due to their detrimental effects on cracking. However, it has been little concerns on formation of Zr hydrides correlated with deformation twins which is distinctive heterogeneous nucleation site in hexagonal close-packed metals. In this paper, the heterogeneous precipitation of Zr hydrides at the twin boundaries was visualized using transmission electron microscopy. It demonstrates that intragranular hydrides in the twinned region precipitates on the rotated habit plane by the twinning and intergranular hydrides precipitate along the coherent low energy twin boundaries independent of the conventional habit planes. Interestingly, dislocations around the twin boundaries play a substantial role in the nucleation of Zr hydrides by reducing the misfit strain energy.

Generation and storage of quantum states using cold atoms

DEFF Research Database (Denmark)

Dantan, Aurelien Romain; Josse, Vincent; Cviklinski, Jean

2006-01-01

Cold cesium or rubidium atomic samples have a good potential both for generation and storage of nonclassical states of light. Generation of nonclassical states of light is possible through the high non-linearity of cold atomic samples excited close to a resonance line. Quadrature squeezing, polar...

Fully Automated Volumetric Modulated Arc Therapy Plan Generation for Prostate Cancer Patients

International Nuclear Information System (INIS)

Voet, Peter W.J.; Dirkx, Maarten L.P.; Breedveld, Sebastiaan; Al-Mamgani, Abrahim; Incrocci, Luca; Heijmen, Ben J.M.

2014-01-01

Purpose: To develop and evaluate fully automated volumetric modulated arc therapy (VMAT) treatment planning for prostate cancer patients, avoiding manual trial-and-error tweaking of plan parameters by dosimetrists. Methods and Materials: A system was developed for fully automated generation of VMAT plans with our commercial clinical treatment planning system (TPS), linked to the in-house developed Erasmus-iCycle multicriterial optimizer for preoptimization. For 30 randomly selected patients, automatically generated VMAT plans (VMAT auto ) were compared with VMAT plans generated manually by 1 expert dosimetrist in the absence of time pressure (VMAT man ). For all treatment plans, planning target volume (PTV) coverage and sparing of organs-at-risk were quantified. Results: All generated plans were clinically acceptable and had similar PTV coverage (V 95%  > 99%). For VMAT auto and VMAT man plans, the organ-at-risk sparing was similar as well, although only the former plans were generated without any planning workload. Conclusions: Fully automated generation of high-quality VMAT plans for prostate cancer patients is feasible and has recently been implemented in our clinic

Rotary-Atomizer Electric Power Generator

Science.gov (United States)

Nguyen, Trieu; Tran, Tuan; de Boer, Hans; van den Berg, Albert; Eijkel, Jan C. T.

2015-03-01

We report experimental and theoretical results on a ballistic energy-conversion method based on a rotary atomizer working with a droplet acceleration-deceleration cycle. In a rotary atomizer, liquid is fed onto the center of a rotating flat surface, where it spreads out under the action of the centrifugal force and creates "atomized" droplets at its edge. The advantage of using a rotary atomizer is that the centrifugal force exerted on the fluid on a smooth, large surface is not only a robust form of acceleration, as it avoids clogging, but also easily allows high throughput, and produces high electrical power. We successfully demonstrate an output power of 4.9 mW and a high voltage up to 3120 V. At present, the efficiency of the system is still low (0.14%). However, the conversion mechanism of the system is fully interpreted in this paper, permitting a conceptual understanding of system operation and providing a roadmap for system optimization. This observation will open up a road for building power-generation systems in the near future.

IAEA co-ordinated research program. 'Round Robin' on measuring the velocity of delayed hydride cracking (DHC)

International Nuclear Information System (INIS)

Grigoriev, V.; Jakobsson, R.

1999-09-01

The International Atomic Agency (IAEA) has initiated a new Co-ordinated Research Programme (CRP) on Hydrogen and hydride induced degradation of the mechanical and physical properties of Zirconium-based alloys. In the first phase of this CRP the methodology for measuring the velocity of Delayed Hydride Cracking (DHC) should be established and participating laboratories from about nine countries around the world carry out identical tests in 'round robin'. The objective of the present work is to establish at Studsvik laboratory the method of a constant load cracking test on unirradiated Zr-2.5Nb and attain a comparison of results between laboratories. Constant load tests are performed on specimens cut from unirradiated CANDU Zr-2.5Nb pressure tube and the rate of crack propagation is determined in each test. Pre-hydrided specimens for testing are supplied from the host laboratory. Six specimens have been tested for delayed hydride cracking (DHC) at 250 deg C. The axial crack growth velocities measured in the tests are within the interval of 8.62x10 -8 - 1.06x10 -7 m/s. The results obtained agree well with the earlier published data for similar materials and test conditions

Relativistic Spin-Orbit Heavy Atom on the Light Atom NMR Chemical Shifts: General Trends Across the Periodic Table Explained.

Science.gov (United States)

Vícha, Jan; Komorovsky, Stanislav; Repisky, Michal; Marek, Radek; Straka, Michal

2018-05-10

The importance of relativistic effects on the NMR parameters in heavy-atom (HA) compounds, particularly the SO-HALA (Spin-Orbit Heavy Atom on the Light Atom) effect on NMR chemical shifts, has been known for about 40 years. Yet, a general correlation between the electronic structure and SO-HALA effect has been missing. By analyzing 1 H NMR chemical shifts of the sixth-period hydrides (Cs-At), we discovered general electronic-structure principles and mechanisms that dictate the size and sign of the SO-HALA NMR chemical shifts. In brief, partially occupied HA valence shells induce relativistic shielding at the light atom (LA) nuclei, while empty HA valence shells induce relativistic deshielding. In particular, the LA nucleus is relativistically shielded in 5d 2 -5d 8 and 6p 4 HA hydrides and deshielded in 4f 0 , 5d 0 , 6s 0 , and 6p 0 HA hydrides. This general and intuitive concept explains periodic trends in the 1 H NMR chemical shifts along the sixth-period hydrides (Cs-At) studied in this work. We present substantial evidence that the introduced principles have a general validity across the periodic table and can be extended to nonhydride LAs. The decades-old question of why compounds with occupied frontier π molecular orbitals (MOs) cause SO-HALA shielding at the LA nuclei, while the frontier σ MOs cause deshielding is answered. We further derive connection between the SO-HALA NMR chemical shifts and Spin-Orbit-induced Electron Deformation Density (SO-EDD), a property that can be obtained easily from differential electron densities and can be represented graphically. SO-EDD provides an intuitive understanding of the SO-HALA effect in terms of the depletion/concentration of the electron density at LA nuclei caused by spin-orbit coupling due to HA in the presence of a magnetic field. Using an analogy between the SO-EDD concept and arguments from classic NMR theory, the complex question of the SO-HALA NMR chemical shifts becomes easily understandable for a wide

Metal interferences and their removal prior to the determination of As(T) and As(III) in acid mine waters by hydride generation atomic absorption spectrometry

Science.gov (United States)

McCleskey, R. Blaine; Nordstrom, D. Kirk; Ball, James W.

2003-01-01

Hydride generation atomic absorption spectrometry (HGAAS) is a sensitive and selective method for the determination of total arsenic (arsenic(III) plus arsenic(V)) and arsenic(III); however, it is subject to metal interferences for acid mine waters. Sodium borohydride is used to produce arsine gas, but high metal concentrations can suppress arsine production. This report investigates interferences of sixteen metal species including aluminum, antimony(III), antimony(V), cadmium, chromium(III), chromium(IV), cobalt, copper(II), iron(III), iron(II), lead, manganese, nickel, selenium(IV), selenium(VI), and zinc ranging in concentration from 0 to 1,000 milligrams per liter and offers a method for removing interfering metal cations with cation exchange resin. The degree of interference for each metal without cation-exchange on the determination of total arsenic and arsenic(III) was evaluated by spiking synthetic samples containing arsenic(III) and arsenic(V) with the potential interfering metal. Total arsenic recoveries ranged from 92 to 102 percent for all metals tested except antimony(III) and antimony(V) which suppressed arsine formation when the antimony(III)/total arsenic molar ratio exceeded 4 or the antimony(V)/total arsenic molar ratio exceeded 2. Arsenic(III) recoveries for samples spiked with aluminum, chromium(III), cobalt, iron(II), lead, manganese, nickel, selenium(VI), and zinc ranged from 84 to 107 percent over the entire concentration range tested. Low arsenic(III) recoveries occurred when the molar ratios of metals to arsenic(III) were copper greater than 120, iron(III) greater than 70, chromium(VI) greater than 2, cadmium greater than 800, antimony(III) greater than 3, antimony(V) greater than 12, or selenium(IV) greater than 1. Low recoveries result when interfering metals compete for available sodium borohydride, causing incomplete arsine production, or when the interfering metal oxidizes arsenic(III). Separation of interfering metal cations using

Synthesis and reactions of imines of α,β-ethylenic silicon-containing aldehydes with complex metal hydrides

International Nuclear Information System (INIS)

Surnin, V.A.; Stadnichuk, M.D.

1986-01-01

Imines of 3-trimethylsilyl-2-propenal or its hydrocarbon analog are reduced chemoselectively at the C=N double bond by sodium borohydride. The direction of lithium aluminum hydride reduction of these imines is not influenced by the nature of the element attached to the C=C bond silicon versus carbon, but rather is determined by the nature of the radical group attached to the nitrogen atom; N-arylimines undergo addition with lithium aluminum hydride at the C=N bond exclusively, whereas for N-alkylimines the addition reactions occur either partially or in full in the 1,4-position, depending on the reaction conditions, to give imines of saturated aldehydes after demetallation

Predicting formation enthalpies of metal hydrides

Energy Technology Data Exchange (ETDEWEB)

Andreasen, A.

2004-12-01

In order for the hydrogen based society viz. a society in which hydrogen is the primary energy carrier to become realizable an efficient way of storing hydrogen is required. For this purpose metal hydrides are serious candidates. Metal hydrides are formed by chemical reaction between hydrogen and metal and for the stable hydrides this is associated with release of heat ({delta}H{sub f} ). The more thermodynamically stable the hydride, the larger {delta}H{sub f}, and the higher temperature is needed in order to desorp hydrogen (reverse reaction) and vice versa. For practical application the temperature needed for desorption should not be too high i.e. {delta}H{sub f} should not be too large. If hydrogen desorption is to be possible below 100 deg C (which is the ultimate goal if hydrogen storage in metal hydrides should be used in conjunction with a PEM fuel cell), {delta}H{sub f} should not exceed -48 kJ/mol. Until recently only intermetallic metal hydrides with a storage capacity less than 2 wt.% H{sub 2} have met this criterion. However, discovering reversible hydrogen storage in complex metal hydrides such as NaAlH{sub 4} (5.5 wt. % reversible hydrogen capacity) have revealed a new group of potential candiates. However, still many combination of elements from the periodic table are yet to be explored. Since experimental determination of thermodynamic properties of the vast combinations of elements is tedious it may be advantagous to have a predictive tool for this task. In this report different ways of predicting {delta}H{sub f} for binary and ternary metal hydrides are reviewed. Main focus will be on how well these methods perform numerically i.e. how well experimental results are resembled by the model. The theoretical background of the different methods is only briefly reviewed. (au)

Electron population uncertainty and atomic covalency

International Nuclear Information System (INIS)

Chesnut, D.B.

2006-01-01

The atoms-in-molecules (AIM) index of atomic covalency is directly related to the AIM atomic population uncertainty. The covalent bond order, delocalization index, and, therefore, the atomic covalency are maximal when electron pairs are equally shared by the atoms involved. When polarization effects are present, these measures of covalent bond character decrease. We present atomic covalences for the single- and double-heavy atom hydrides of elements of the first and second low rows of the periodic table to illustrate these effects. Some usual behavior is seen in hydrogen-bridged species due in some cases to stronger than expected multicenter bonds and in other cases to many atoms contributing to the covalency index

Multislice simulations for in-situ HRTEM studies of nanostructured magnesium hydride at ambient hydrogen pressure

International Nuclear Information System (INIS)

Surrey, Alexander; Schultz, Ludwig; Rellinghaus, Bernd

2017-01-01

Highlights: • Multislice HRTEM contrast simulations of a windowed environmental cell. • Study of Mg and MgH2 nanocrystals as model system in hydrogen at ambient pressure. • Investigation of spatial resolution and contrast depending on specimen thickness, defocus, and hydrogen pressure. • Atomic resolution is expected for specimens as thin as 5  nm. - Abstract: The use of transmission electron microscopy (TEM) for the structural characterization of many nanostructured hydrides, which are relevant for solid state hydrogen storage, is hindered due to a rapid decomposition of the specimen upon irradiation with the electron beam. Environmental TEM allows to stabilize the hydrides by applying a hydrogen back pressure of up to 4.5 bar in a windowed environmental cell. The feasibility of high-resolution TEM (HRTEM) investigations of light weight metals and metal hydrides in such a “nanoreactor” is studied theoretically by means of multislice HRTEM contrast simulations using Mg and its hydride phase, MgH_2, as model system. Such a setup provides the general opportunity to study dehydrogenation and hydrogenation reactions at the nanoscale under technological application conditions. We analyze the dependence of both the spatial resolution and the HRTEM image contrast on parameters such as the defocus, the metal/hydride thickness, and the hydrogen pressure in order to explore the possibilities and limitations of in-situ experiments with windowed environmental cells. Such simulations may be highly valuable to pre-evaluate future experimental studies.

Multislice simulations for in-situ HRTEM studies of nanostructured magnesium hydride at ambient hydrogen pressure

Energy Technology Data Exchange (ETDEWEB)

Surrey, Alexander, E-mail: a.surrey@ifw-dresden.de [IFW Dresden, Institute for Metallic Materials, P.O. Box 270116, D-01171 Dresden (Germany); Institut für Festkörperphysik, Technische Universität Dresden, D-01062 Dresden (Germany); Schultz, Ludwig [IFW Dresden, Institute for Metallic Materials, P.O. Box 270116, D-01171 Dresden (Germany); Institut für Festkörperphysik, Technische Universität Dresden, D-01062 Dresden (Germany); Rellinghaus, Bernd, E-mail: b.rellinghaus@ifw-dresden.de [IFW Dresden, Institute for Metallic Materials, P.O. Box 270116, D-01171 Dresden (Germany)

2017-04-15

Highlights: • Multislice HRTEM contrast simulations of a windowed environmental cell. • Study of Mg and MgH2 nanocrystals as model system in hydrogen at ambient pressure. • Investigation of spatial resolution and contrast depending on specimen thickness, defocus, and hydrogen pressure. • Atomic resolution is expected for specimens as thin as 5  nm. - Abstract: The use of transmission electron microscopy (TEM) for the structural characterization of many nanostructured hydrides, which are relevant for solid state hydrogen storage, is hindered due to a rapid decomposition of the specimen upon irradiation with the electron beam. Environmental TEM allows to stabilize the hydrides by applying a hydrogen back pressure of up to 4.5 bar in a windowed environmental cell. The feasibility of high-resolution TEM (HRTEM) investigations of light weight metals and metal hydrides in such a “nanoreactor” is studied theoretically by means of multislice HRTEM contrast simulations using Mg and its hydride phase, MgH{sub 2}, as model system. Such a setup provides the general opportunity to study dehydrogenation and hydrogenation reactions at the nanoscale under technological application conditions. We analyze the dependence of both the spatial resolution and the HRTEM image contrast on parameters such as the defocus, the metal/hydride thickness, and the hydrogen pressure in order to explore the possibilities and limitations of in-situ experiments with windowed environmental cells. Such simulations may be highly valuable to pre-evaluate future experimental studies.

Disposal of tritium-exposed metal hydrides

International Nuclear Information System (INIS)

Nobile, A.; Motyka, T.

1991-01-01

A plan has been established for disposal of tritium-exposed metal hydrides used in Savannah River Site (SRS) tritium production or Materials Test Facility (MTF) R ampersand D operations. The recommended plan assumes that the first tritium-exposed metal hydrides will be disposed of after startup of the Solid Waste Disposal Facility (SWDF) Expansion Project in 1992, and thus the plan is consistent with the new disposal requiremkents that will be in effect for the SWDF Expansion Project. Process beds containing tritium-exposed metal hydride powder will be disposed of without removal of the powder from the bed; however, disposal of tritium-exposed metal hydride powder that has been removed from its process vessel is also addressed

Comparative oxidation state specific analysis of arsenic species by high-performance liquid chromatography- inductively coupled plasma-mass spectrometry and hydride generation-cryotrapping-atomic absorption spectrometry

Czech Academy of Sciences Publication Activity Database

Currier, J. M.; Saunders, R. J.; Ding, L.; Bodnar, W.; Cable, P.; Matoušek, Tomáš; Creed, J. T.; Stýblo, M.

2013-01-01

Roč. 28, č. 6 (2013), s. 843-852 ISSN 0267-9477 R&D Projects: GA MŠk LH12040 Institutional support: RVO:68081715 Keywords : arsenic * speciaton analysis * As metabolism Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.396, year: 2013

Generation of a slow and continuous cesium atomic beam for an atomic clock

International Nuclear Information System (INIS)

Park, Sang Eon; Lee, Ho Seong; Shin, Eun-joo; Kwon, Taeg Yong; Yang, Sung Hoon; Cho, Hyuck

2002-01-01

A thermal atomic beam from a cesium oven was slowed down by use of the Hoffnagle modified white-light cooling technique. In addition, the atomic beam was collimated by use of a two-dimensional optical molasses that was installed transverse to the atomic-beam direction. The flux of the atomic beam was 2x10 10 atoms/s, an increase of a factor of 16 as a result of the collimation. The mean longitudinal velocity was ∼24.4 m/s, and the rms velocity spread of the slowed atomic beam was ∼1 m/s. Compared with other methods, we found that the Hoffnagle method is suitable for the generation of slow atomic beams to be used in an atomic clock, which requires an ultralow magnetic field environment. This atomic beam was deflected by an angle of 30 deg. by a one-dimensional optical molasses to separate it from laser light and high-velocity atoms

Genetic algorithms in teaching artificial intelligence (automated generation of specific algebras)

Science.gov (United States)

Habiballa, Hashim; Jendryscik, Radek

2017-11-01

The problem of teaching essential Artificial Intelligence (AI) methods is an important task for an educator in the branch of soft-computing. The key focus is often given to proper understanding of the principle of AI methods in two essential points - why we use soft-computing methods at all and how we apply these methods to generate reasonable results in sensible time. We present one interesting problem solved in the non-educational research concerning automated generation of specific algebras in the huge search space. We emphasize above mentioned points as an educational case study of an interesting problem in automated generation of specific algebras.

High-dimensional atom localization via spontaneously generated coherence in a microwave-driven atomic system.

Science.gov (United States)

Wang, Zhiping; Chen, Jinyu; Yu, Benli

2017-02-20

We investigate the two-dimensional (2D) and three-dimensional (3D) atom localization behaviors via spontaneously generated coherence in a microwave-driven four-level atomic system. Owing to the space-dependent atom-field interaction, it is found that the detecting probability and precision of 2D and 3D atom localization behaviors can be significantly improved via adjusting the system parameters, the phase, amplitude, and initial population distribution. Interestingly, the atom can be localized in volumes that are substantially smaller than a cubic optical wavelength. Our scheme opens a promising way to achieve high-precision and high-efficiency atom localization, which provides some potential applications in high-dimensional atom nanolithography.

Determination of arsenic in ambient water at sub-part-per-trillion levels by hydride generation Pd coated platform collection and GFAAS detection.

Science.gov (United States)

Liang, L; Lazoff, S; Chan, C; Horvat, M; Woods, J S

1998-11-01

A method for trace determination of total arsenic in ambient waters is described. Arsenic is separated on-line from a large volume water sample by hydride generation and purging, pre-collected on a Pd coated pyrolytic platform cuvette using a simple and inexpensive system, and finally detected by GFAAS. Instrument parameters, hydride generation, transportation, and collection were optimized. The analytical behavior for major species including As(3+), As(5+), monomethyl As (MMA), and dimethyl As (DMA) were investigated individually. Problems arising from use of the system were discussed and eliminated. The necessity of sample digestion and an efficient digestion method were studied. Sample digestion for water with low organic content such as tap water and clean ground water and some clean surface water can be omitted. The method detection limit (MDL) is 0.3 ng l(-1) for a 25 ml water sample. Recoveries close to 100% with R.S.D.rain, sewage effluent, and saline water from different origins in the US, China, and Canada were collected and analyzed using ultra clean sampling and analysis techniques. The background levels of As in most water analyzed were established for the first time, and found to be far above the EPA's health effect criteria, 18 ng l(-1).

Density functional calculations of hypothetical neutral hollow octahedral molecules with a 48-atom framework: Hydrides and oxides of boron, carbon, nitrogen, aluminum, and silicon

Energy Technology Data Exchange (ETDEWEB)

LaViolette, Randall A. [Idaho National Engineering and Environmental Laboratory, P.O. Box 1625, Idaho Falls, ID 83415-2208 (United States); Benson, Michael T. [Idaho National Engineering and Environmental Laboratory, P.O. Box 1625, Idaho Falls, ID 83415-2208 (United States)

2000-06-01

We computed via first-principles density functional theory calculations (employing both the local density and generalized gradient approximations) the dimensions, bond lengths and angles, binding energy, and HOMO-LUMO gap of the following hypothetical neutral hollow octahedral molecules: B{sub 48}H{sub 24}, C{sub 48}H{sub 48}, C{sub 96}H{sub 80} (formed by bonding two C{sub 48}H{sub 48} molecules), N{sub 48}H{sub 24}, Al{sub 48}H{sub 24}, and Si{sub 48}H{sub 48}; B{sub 24}O{sub 24}, C{sub 24}O{sub 24}, N{sub 24}O{sub 24}, Al{sub 24}O{sub 24}, and Si{sub 24}O{sub 24}. Each molecule consists of a large hollow framework of six puckered eight-membered rings whose planes are either mutually perpendicular or parallel, so that each molecule possesses only eight- and nine-membered rings. The hydrides have their hydrogen atoms attached only to the two-atom bridging sites on the framework. The oxides have their oxygen atoms occupying exclusively the two-atom bridging sites of the framework alternating with the (B, C, N, Al, Si) atoms exclusively occupying the three-atom bridging sites. We also calculated the infrared spectra of the C{sub 48}H{sub 48} and the C{sub 24}O{sub 24} molecules. For the sake of comparison, we also examined the hypothetical octahedral C{sub 48} fullerene cuboctohedron (possessing four-, six-, and eight-membered rings) studied by Dunlap and Taylor. The molecules based on carbon would be the most stable; those based on nitrogen would be the least stable, if at all. (c) 2000 American Institute of Physics.

Automated microprocessor-controlled atomic absorption analysis of natural water for arsenic and selenium

International Nuclear Information System (INIS)

Morrow, R.W.; Futrell, T.L.; Adams, T.T.

1978-08-01

An automated, dual-channel atomic absorption spectrophotometer for the simultaneous determination of arsenic and selenium in natural water is now in operation. The instrument was constructed from commercially available optical components, spectral sources, and a sample changer. Automation was achieved by using an in-house-fabricated and programmed microprocessor. The instrument will analyze samples at a rate of 37 per hour, and a quantitative determination of arsenic and selenium to 0.2 μg/l (ppB) can be achieved. Arsenic can be determined with a precision of 19% at 1 μg/l and 6% at 10 μg/l, while selenium can be determined with a precision of 17% at 1 μg/l and 4% at 10 μg/l

Anodematerials for Metal Hydride Batteries

DEFF Research Database (Denmark)

Jensen, Jens Oluf

1997-01-01

This report describes the work on development of hydride forming alloys for use as electrode materials in metal hydride batteries. The work has primarily been concentrated on calcium based alloys derived from the compound CaNi5. This compound has a higher capacity compared with alloys used in today......’s hydride batteries, but a much poorer stability towards repeated charge/discharge cycling. The aim was to see if the cycleability of CaNi5 could be enhanced enough by modifications to make the compound a suitable electrode material. An alloying method based on mechanical alloying in a planetary ball mill...

AutoDipole - Automated generation of dipole subtraction terms

International Nuclear Information System (INIS)

Hasegawa, K.; Uwer, P.

2009-11-01

We present an automated generation of the subtraction terms for next-to-leading order QCD calculations in the Catani-Seymour dipole formalism. For a given scattering process with n external particles our Mathematica package generates all dipole terms, allowing for bothmassless and massive dipoles. The numerical evaluation of the subtraction terms proceeds with MadGraph, which provides Fortran code for the necessary scattering amplitudes. Checks of the numerical stability are discussed. (orig.)

AutoDipole - Automated generation of dipole subtraction terms

Energy Technology Data Exchange (ETDEWEB)

Hasegawa, K.; Uwer, P. [Humboldt-Universitaet, Berlin (Germany). Inst. fuer Physik; Moch, S. [Deutsches Elektronen-Synchrotron (DESY), Zeuthen (Germany)

2009-11-15

We present an automated generation of the subtraction terms for next-to-leading order QCD calculations in the Catani-Seymour dipole formalism. For a given scattering process with n external particles our Mathematica package generates all dipole terms, allowing for bothmassless and massive dipoles. The numerical evaluation of the subtraction terms proceeds with MadGraph, which provides Fortran code for the necessary scattering amplitudes. Checks of the numerical stability are discussed. (orig.)

Epitaxial thin film growth of LiH using a liquid-Li atomic template

Energy Technology Data Exchange (ETDEWEB)

Oguchi, Hiroyuki, E-mail: oguchi@nanosys.mech.tohoku.ac.jp [Department of Nanomechanics, Tohoku University, Sendai 980-8579 (Japan); Micro System Integration Center (muSIC), Tohoku University, Sendai 980-0845 (Japan); Ikeshoji, Tamio; Orimo, Shin-ichi [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Advanced Institute for Materials Research (AIMR), Tohoku University, Sendai 980-8577 (Japan); Ohsawa, Takeo; Shiraki, Susumu; Hitosugi, Taro [Advanced Institute for Materials Research (AIMR), Tohoku University, Sendai 980-8577 (Japan); Kuwano, Hiroki [Department of Nanomechanics, Tohoku University, Sendai 980-8579 (Japan)

2014-11-24

We report on the synthesis of lithium hydride (LiH) epitaxial thin films through the hydrogenation of a Li melt, forming abrupt LiH/MgO interface. Experimental and first-principles molecular dynamics studies reveal a comprehensive microscopic picture of the crystallization processes, which sheds light on the fundamental atomistic growth processes that have remained unknown in the vapor-liquid-solid method. We found that the periodic structure that formed, because of the liquid-Li atoms at the film/MgO-substrate interface, serves as an atomic template for the epitaxial growth of LiH crystals. In contrast, films grown on the Al{sub 2}O{sub 3} substrates indicated polycrystalline films with a LiAlO{sub 2} secondary phase. These results and the proposed growth process provide insights into the preparation of other alkaline metal hydride thin films on oxides. Further, our investigations open the way to explore fundamental physics and chemistry of metal hydrides including possible phenomena that emerge at the heterointerfaces of metal hydrides.

Atomistic modeling of zirconium hydride precipitation: methodology for deriving a tight-binding potential

International Nuclear Information System (INIS)

Dufresne, Alice

2014-01-01

The zirconium-hydrogen system is of nuclear safety interest, as the hydride precipitation leads to the cladding embrittlement, which is made of zirconium-based alloys. The cladding is the first safety barrier confining the radioactive products: its integrity shall be kept during the entire fuel-assemblies life, in reactor, including accidental situation, and post-operation (transport and storage). Many uncertainties remain regarding the hydrides precipitation kinetics and the local stress impact on their precipitation. The atomic scale modeling of this system would bring clarifications on the relevant mechanisms. The usual atomistic modeling methods are based on thermo-statistic approaches, whose precision and reliability depend on the interatomic potential used. However, there was no potential allowing a rigorous study of the Zr-H system. The present work has indeed addressed this issue: a new tight-binding potential for zirconium hydrides modeling is now available. Moreover, this thesis provides a detailed manual for deriving such potentials accounting for spd hybridization, and fitted here on DFT results. This guidebook has be written in light of modeling a pure transition metal followed by a metal-covalent coupling (metallic carbides, nitrides and silicides). (author)

Automation in trace-element chemistry - Development of a fully automated on-line preconcentration device for trace analysis of heavy metals with atomic spectroscopy

International Nuclear Information System (INIS)

Michaelis, M.R.A.

1990-01-01

Scope of this work was the development of an automated system for trace element preconcentration to be used and integrated to analytic atomic spectroscopic methods like flame atomic absorption spectrometry (FAAS), graphite furnace atomic absorption spectrometry (GFAAS) or atomic emission spectroscopy with inductively coupled plasma (ICP-AES). Based on the newly developed cellulose-based chelating cation exchangers ethylene-diamin-triacetic acid cellulose (EDTrA-Cellulose) and sulfonated-oxine cellulose a flexible, computer-controlled instrument for automation of preconcentration and/or of matrix separation of heavy metals is described. The most important properties of these materials are fast exchange kinetics, good selectivity against alkaline and alkaline earth elements, good flow characteristics and good stability of the material and the chelating functions against changes in pH-values of reagents necessary in the process. The combination of the preconcentration device for on-line determinations of Zn, Cd, Pb, Ni, Fe, Co, Mn, V, Cu, La, U, Th is described for FAAS and for ICP-AES with a simultaneous spectrometer. Signal enhancement factors of 70 are achieved from preconcentration of 10 ml and on-line determination with FAAS due to signal quantification in peak-height mode. For GFAAS and for sequential ICP methods for off-line preconcentration are given. The optimization and adaption of the interface to the different characteristics of the analytical instrumentation is emphasized. For evaluation and future developments with respect to determination and/or preconcentration of anionic species like As, Se, Sb etc. instrument modifications are proposed and a development software is described. (Author)

Characterisation of hydrides in a zirconium alloy, by EBSD

International Nuclear Information System (INIS)

Ubhi, H.S.; Larsen, K.

2012-01-01

Zirconium alloys are used in nuclear reactors owing to their low capture cross-section for thermal neutrons and good mechanical and corrosion properties. However, they do suffer from delayed hydrogen cracking (DHC) due to formation of hydride particles. This study shows how the electron back-scatter diffraction (EBSD) technique can be used to characterise hydrides and their orientation relationship with the matrix. Hydrided EB weld specimens were prepared by electro-polishing, characterised using Oxford instruments AZtecHKL EBSD apparatus and software attached to a FEG SEM. Hydrides were found to exist as fine intra granular plates and having the Blackburn orientation relationship, i.e. (0002)Zr//(111)hydride and (1120)Zr//(1-10)hydride. The hydrides were also found to contain sigma 3 boundaries as well as local misorientations. (author)

Hydrogen charging, hydrogen content analysis and metallographic examination of hydride in zirconium alloys

International Nuclear Information System (INIS)

Singh, R.N.; Kishore, R.; Mukherjee, S.; Roychowdhury, S.; Srivastava, D.; Sinha, T.K.; De, P.K.; Banerjee, S.; Gopalan, B.; Kameswaran, R.; Sheelvantra, Smita S.

2003-12-01

Gaseous and electrolytic hydrogen charging techniques for introducing controlled amount of hydrogen in zirconium alloy is described. Zr-1wt%Nb fuel tube, zircaloy-2 pressure tube and Zr-2.5Nb pressure tube samples were charged with up to 1000 ppm of hydrogen by weight using one of the aforementioned methods. These hydrogen charged Zr-alloy samples were analyzed for estimating the total hydrogen content using inert gas fusion technique. Influence of sample surface preparation on the estimated hydrogen content is also discussed. In zirconium alloys, hydrogen in excess of the terminal solid solubility precipitates out as brittle hydride phase, which acquire platelet shaped morphology due to its accommodation in the matrix and can make the host matrix brittle. The F N number, which represents susceptibility of Zr-alloy tubes to hydride embrittlement was measured from the metallographs. The volume fraction of the hydride phase, platelet size, distribution, interplatelet spacing and orientation were examined metallographically using samples sliced along the radial-axial and radial-circumferential plane of the tubes. It was observed that hydride platelet length increases with increase in hydrogen content. Considering the metallographs generated by Materials Science Division as standard, metallographs prepared by the IAEA round robin participants for different hydrogen concentration was compared. It is felt that hydride micrographs can be used to estimate not only that approximate hydrogen concentration of the sample but also its size, distribution and orientation which significantly affect the susceptibility to hydride embrittlement of these alloys. (author)

Thermal enhancement cartridge heater modified tritium hydride bed development, Part 2 - Experimental validation of key conceptual design features

Energy Technology Data Exchange (ETDEWEB)

Heroux, K.J.; Morgan, G.A. [Savannah River Laboratory, Aiken, SC (United States)

2015-03-15

The Thermal Enhancement Cartridge Heater Modified (TECH Mod) tritium hydride bed is an interim replacement for the first generation (Gen1) process hydride beds currently in service in the Savannah River Site (SRS) Tritium Facilities. 3 new features are implemented in the TECH Mod hydride bed prototype: internal electric cartridge heaters, porous divider plates, and copper foam discs. These modifications will enhance bed performance and reduce costs by improving bed activation and installation processes, in-bed accountability measurements, end-of-life bed removal, and He-3 recovery. A full-scale hydride bed test station was constructed at the Savannah River National Laboratory (SRNL) in order to evaluate the performance of the prototype TECH Mod hydride bed. Controlled hydrogen (H{sub 2}) absorption/ desorption experiments were conducted to validate that the conceptual design changes have no adverse effects on the gas transfer kinetics or H{sub 2} storage/release properties compared to those of the Gen1 bed. Inert gas expansions before, during, and after H{sub 2} flow tests were used to monitor changes in gas transfer rates with repeated hydriding/de-hydriding of the hydride material. The gas flow rates significantly decreased after initial hydriding of the material; however, minimal changes were observed after repeated cycling. The data presented herein confirm that the TECH Mod hydride bed would be a suitable replacement for the Gen1 bed with the added enhancements expected from the advanced design features. (authors)

EddyOne automated analysis of PWR/WWER steam generator tubes eddy current data

International Nuclear Information System (INIS)

Nadinic, B.; Vanjak, Z.

2004-01-01

INETEC Institute for Nuclear Technology developed software package called Eddy One which has option of automated analysis of bobbin coil eddy current data. During its development and on site use, many valuable lessons were learned which are described in this article. In accordance with previous, the following topics are covered: General requirements for automated analysis of bobbin coil eddy current data; Main approaches to automated analysis; Multi rule algorithms for data screening; Landmark detection algorithms as prerequisite for automated analysis (threshold algorithms and algorithms based on neural network principles); Field experience with Eddy One software; Development directions (use of artificial intelligence with self learning abilities for indication detection and sizing); Automated analysis software qualification; Conclusions. Special emphasis is given on results obtained on different types of steam generators, condensers and heat exchangers. Such results are then compared with results obtained by other automated software vendors giving clear advantage to INETEC approach. It has to be pointed out that INETEC field experience was collected also on WWER steam generators what is for now unique experience.(author)

Blistering and hydride embrittlement

International Nuclear Information System (INIS)

Louthan, M.R. Jr.

1975-01-01

The effects of hydrogen on the mechanical properties of metals have been categorized into several groups. Two of the groups, hydrogen blistering and hydride embrittlement, are reasonably well understood, and problems relating to their occurrence may be avoided if that understanding is used as a basis for selecting alloys for hydrogen service. Blistering and hydride embrittlement are described along with several techniques of materials selection and used to minimize their adverse effects. (U.S.)

Dependency of Delayed Hydride Crack Velocity on the Direction of an Approach to Test Temperatures in Zirconium Alloys

International Nuclear Information System (INIS)

Kim, Young Suk; Kim, Kang Soo; Im, Kyung Soo; Ahn, Sang Bok; Cheong, Yong Moo

2005-01-01

Recently, Kim proposed a new DHC model where a driving force for the DHC is a supersaturated hydrogen concentration as a result of a hysteresis of the terminal solid solubility (TSS) of hydrogen in zirconium alloys upon a heating and a cooling. This model was demonstrated to be valid through a model experiment where the prior plastic deformation facilitated nucleation of the reoriented hydrides, thus reducing the supersaturated hydrogen concentration at the plastic zone ahead of the crack tip and causing hydrogen to move to the crack tip from the bulk region. Thus, an approach to the test temperature by a cooling is required to create a supersaturation of hydrogen, which is a driving force for the DHC of zirconium alloys. However, despite the absence of the supersaturation of hydrogen due to an approach to the test temperature by a heating, DHC is observed to occur in zirconium alloys at the test temperatures below 180 .deg. C. As to this DHC phenomenon, Kim proposed that stress-induced transformation from γ-hydrides to δ-hydrides is likely to be a cause of this, based on Root's observation that the γ-hydride is a stable phase at temperatures lower than 180 .deg. C. In other words, the hydrides formed at the crack tip would be δ-hydrides due to the stressinduced transformation while the bulk region still maintains the initial hydride phase or γ-hydrides. It should be noted that Ambler has also assumed the crack tip hydrides to be δ-hydrides. When the δ-hydrides or ZrH1.66 are precipitated at the crack tip due to the transformation of the γ-hydrides or ZrH, the crack tip will have a decreased concentration of dissolved hydrogen in zirconium, considering the atomic ratio of hydrogen and zirconium in the γ- and δ-hydrides. In contrast, due to no stress-induced transformation of hydrides, the bulk region maintains the initial concentration of dissolved hydrogen. Hence, there develops a difference in the hydrogen concentration or .C between the bulk and the

Dependency of Delayed Hydride Crack Velocity on the Direction of an Approach to Test Temperatures in Zirconium Alloys

Energy Technology Data Exchange (ETDEWEB)

Kim, Young Suk; Kim, Kang Soo; Im, Kyung Soo; Ahn, Sang Bok; Cheong, Yong Moo [Korea Atomic Energy Research Institute, Taejon (Korea, Republic of)

2005-07-01

Recently, Kim proposed a new DHC model where a driving force for the DHC is a supersaturated hydrogen concentration as a result of a hysteresis of the terminal solid solubility (TSS) of hydrogen in zirconium alloys upon a heating and a cooling. This model was demonstrated to be valid through a model experiment where the prior plastic deformation facilitated nucleation of the reoriented hydrides, thus reducing the supersaturated hydrogen concentration at the plastic zone ahead of the crack tip and causing hydrogen to move to the crack tip from the bulk region. Thus, an approach to the test temperature by a cooling is required to create a supersaturation of hydrogen, which is a driving force for the DHC of zirconium alloys. However, despite the absence of the supersaturation of hydrogen due to an approach to the test temperature by a heating, DHC is observed to occur in zirconium alloys at the test temperatures below 180 .deg. C. As to this DHC phenomenon, Kim proposed that stress-induced transformation from {gamma}-hydrides to {delta}-hydrides is likely to be a cause of this, based on Root's observation that the {gamma}-hydride is a stable phase at temperatures lower than 180 .deg. C. In other words, the hydrides formed at the crack tip would be {delta}-hydrides due to the stressinduced transformation while the bulk region still maintains the initial hydride phase or {gamma}-hydrides. It should be noted that Ambler has also assumed the crack tip hydrides to be {delta}-hydrides. When the {delta}-hydrides or ZrH1.66 are precipitated at the crack tip due to the transformation of the {gamma}-hydrides or ZrH, the crack tip will have a decreased concentration of dissolved hydrogen in zirconium, considering the atomic ratio of hydrogen and zirconium in the {gamma}- and {delta}-hydrides. In contrast, due to no stress-induced transformation of hydrides, the bulk region maintains the initial concentration of dissolved hydrogen. Hence, there develops a difference in the

Generation of atomic iodine via fluorine for chemical oxygen-iodine laser

International Nuclear Information System (INIS)

Jirasek, Vit; Spalek, Otomar; Censky, Miroslav; Pickova, Irena; Kodymova, Jarmila; Jakubec, Ivo

2007-01-01

A method of the chemical generation of atomic iodine for a chemical oxygen-iodine laser (COIL) using atomic fluorine as a reaction intermediate was studied experimentally. This method is based on the reaction between F 2 and NO providing F atoms, and the reaction of F with HI resulting in iodine atoms generation. Atomic iodine was produced with efficiency exceeding 40% relative to initial F 2 flow rate. This efficiency was nearly independent on pressure and total gas flow rate. The F atoms were stable in the reactor up to 2 ms. An optimum ratio of the reactants flow rates was F 2 :NO:HI = 1:1:1. A rate constant of the reaction of F 2 with HI was determined. The numerical modelling showed that remaining HI and IF were probably consumed in their mutual reaction. The reaction system was found suitable for employing in a generator of atomic iodine with its subsequent injection into a supersonic nozzle of a COIL

SYNTHESIS AND STRUCTURE OF BIS(PHENYLTETRAMETHYLCYCLOPENTADIENYL)TITANIUM(III) HYDRIDE - THE FIRST MONOMERIC BIS(CYCLOPENTADIENYL)TITANIUM(III) HYDRIDE : The First Monomeric Bis(cyclopentadienyl)titanium(III) Hydride

NARCIS (Netherlands)

de Wolf, J.M.; Meetsma, A.; Teuben, J.H

1995-01-01

The first structurally characterized monomeric bis(cyclopentadienyl)titanium(III) hydride, (C(5)PhMe(4))(2)TiH (4), was synthesized by hydrogenolysis of (C(5)PhMe(4))(2)TiMe (5). Hydride 4 was found to be a monomeric bent sandwich by X-ray diffraction methods, and the pentamethylcyclopentadienyl

Metal hydrides based high energy density thermal battery

International Nuclear Information System (INIS)

Fang, Zhigang Zak; Zhou, Chengshang; Fan, Peng; Udell, Kent S.; Bowman, Robert C.; Vajo, John J.; Purewal, Justin J.; Kekelia, Bidzina

2015-01-01

Highlights: • The principle of the thermal battery using advanced metal hydrides was demonstrated. • The thermal battery used MgH 2 and TiMnV as a working pair. • High energy density can be achieved by the use of MgH 2 to store thermal energy. - Abstract: A concept of thermal battery based on advanced metal hydrides was studied for heating and cooling of cabins in electric vehicles. The system utilized a pair of thermodynamically matched metal hydrides as energy storage media. The pair of hydrides that was identified and developed was: (1) catalyzed MgH 2 as the high temperature hydride material, due to its high energy density and enhanced kinetics; and (2) TiV 0.62 Mn 1.5 alloy as the matching low temperature hydride. Further, a proof-of-concept prototype was built and tested, demonstrating the potential of the system as HVAC for transportation vehicles

Automated Construction of Molecular Active Spaces from Atomic Valence Orbitals.

Science.gov (United States)

Sayfutyarova, Elvira R; Sun, Qiming; Chan, Garnet Kin-Lic; Knizia, Gerald

2017-09-12

We introduce the atomic valence active space (AVAS), a simple and well-defined automated technique for constructing active orbital spaces for use in multiconfiguration and multireference (MR) electronic structure calculations. Concretely, the technique constructs active molecular orbitals capable of describing all relevant electronic configurations emerging from a targeted set of atomic valence orbitals (e.g., the metal d orbitals in a coordination complex). This is achieved via a linear transformation of the occupied and unoccupied orbital spaces from an easily obtainable single-reference wave function (such as from a Hartree-Fock or Kohn-Sham calculations) based on projectors to targeted atomic valence orbitals. We discuss the premises, theory, and implementation of the idea, and several of its variations are tested. To investigate the performance and accuracy, we calculate the excitation energies for various transition-metal complexes in typical application scenarios. Additionally, we follow the homolytic bond breaking process of a Fenton reaction along its reaction coordinate. While the described AVAS technique is not a universal solution to the active space problem, its premises are fulfilled in many application scenarios of transition-metal chemistry and bond dissociation processes. In these cases the technique makes MR calculations easier to execute, easier to reproduce by any user, and simplifies the determination of the appropriate size of the active space required for accurate results.

Electronic structure of the palladium hydride studied by compton scattering

CERN Document Server

Mizusaki, S; Yamaguchi, M; Hiraoka, N; Itou, M; Sakurai, Y

2003-01-01

The hydrogen-induced changes in the electronic structure of Pd have been investigated by Compton scattering experiments associated with theoretical calculations. Compton profiles (CPs) of single crystal of Pd and beta phase hydride PdH sub x (x=0.62-0.74) have been measured along the [100], [110] and [111] directions with a momentum resolution of 0.14-0.17 atomic units using 115 keV x-rays. The theoretical Compton profiles have been calculated from the wavefunctions obtained utilizing the full potential linearized augmented plane wave method within the local density approximation for Pd and stoichiometric PdH. The experimental and the theoretical results agreed well with respect to the difference in the CPs between PdH sub x and Pd, and the anisotropy in the CPs of Pd or PdH sub x. This study provides lines of evidence that upon hydride formation the lowest valance band of Pd is largely modified due to hybridization with H 1s-orbitals and the Fermi energy is raised into the sp-band. (author)

Automated voxelization of 3D atom probe data through kernel density estimation

International Nuclear Information System (INIS)

Srinivasan, Srikant; Kaluskar, Kaustubh; Dumpala, Santoshrupa; Broderick, Scott; Rajan, Krishna

2015-01-01

Identifying nanoscale chemical features from atom probe tomography (APT) data routinely involves adjustment of voxel size as an input parameter, through visual supervision, making the final outcome user dependent, reliant on heuristic knowledge and potentially prone to error. This work utilizes Kernel density estimators to select an optimal voxel size in an unsupervised manner to perform feature selection, in particular targeting resolution of interfacial features and chemistries. The capability of this approach is demonstrated through analysis of the γ / γ’ interface in a Ni–Al–Cr superalloy. - Highlights: • Develop approach for standardizing aspects of atom probe reconstruction. • Use Kernel density estimators to select optimal voxel sizes in an unsupervised manner. • Perform interfacial analysis of Ni–Al–Cr superalloy, using new automated approach. • Optimize voxel size to preserve the feature of interest and minimizing loss / noise.

Metal hydrides for hydrogen storage in nickel hydrogen batteries

International Nuclear Information System (INIS)

Bittner, H.F.; Badcock, C.C.; Quinzio, M.V.

1984-01-01

Metal hydride hydrogen storage in nickel hydrogen (Ni/H 2 ) batteries has been shown to increase battery energy density and improve battery heat management capabilities. However the properties of metal hydrides in a Ni/H 2 battery environment, which contains water vapor and oxygen in addition to the hydrogen, have not been well characterized. This work evaluates the use of hydrides in Ni/H 2 batteries by fundamental characterization of metal hydride properties in a Ni/H 2 cell environment. Hydrogen sorption properties of various hydrides have been measured in a Ni/H 2 cell environment. Results of detailed thermodynamic and kinetic studies of hydrogen sorption in LaNi 5 in a Ni/H 2 cell environment are presented. Long-term cycling studies indicate that degradation of the hydride can be minimized by cycling between certain pressure limits. A model describing the mechanism of hydride degradation is presented

Compact PEM fuel cell system combined with all-in-one hydrogen generator using chemical hydride as a hydrogen source

International Nuclear Information System (INIS)

Kim, Jincheol; Kim, Taegyu

2015-01-01

Highlights: • Compact fuel cell system was developed for a portable power generator. • Novel concept using an all-in-one reactor for hydrogen generation was proposed. • Catalytic reactor, hydrogen chamber and separator were combined in a volume. • The system can be used to drive fuel cell-powered unmanned autonomous systems. - Abstract: Compact fuel cell system was developed for a portable power generator. The power generator features a polymer electrolyte membrane fuel cell (PEMFC) using a chemical hydride as a hydrogen source. The hydrogen generator extracted hydrogen using a catalytic hydrolysis from a sodium borohydride alkaline solution. A novel concept using an all-in-one reactor was proposed in which a catalyst, hydrogen chamber and byproduct separator were combined in a volume. In addition, the reactor as well as a pump, cooling fans, valves and controller was integrated in a single module. A 100 W PEMFC stack was connected with the hydrogen generator and was evaluated at various load conditions. It was verified that the stable hydrogen supply was achieved and the developed system can be used to drive fuel cell-powered unmanned autonomous systems.

A comparison of the smeared-dislocation and super-dislocation description of a hydrided region in the context of modelling delayed hydride cracking initiation

International Nuclear Information System (INIS)

Smith, E.

1994-01-01

In quantifying the stress distribution within a hydrided region in the context of modelling delayed hydride cracking (DHC) initiation in zirconium alloys, this paper highlights the desirability of accounting for image effects, i.e. the interaction between the hydrided region and any free surface, for example a sharp crack, blunt notch or planar surface. The super-dislocation representation of a finite thickness hydrided region is ideal for accounting for image effects. It also adequately accounts for the finite thickness, t, of a hydrided region provided, as is the case in practice, we are concerned with the stress value within the hydride at distances ≥ 0.25 t from an end of the region. (Author)

Metal hydrides based high energy density thermal battery

Energy Technology Data Exchange (ETDEWEB)

Fang, Zhigang Zak, E-mail: zak.fang@utah.edu [Department of Metallurgical Engineering, The University of Utah, 135 South 1460 East, Room 412, Salt Lake City, UT 84112-0114 (United States); Zhou, Chengshang; Fan, Peng [Department of Metallurgical Engineering, The University of Utah, 135 South 1460 East, Room 412, Salt Lake City, UT 84112-0114 (United States); Udell, Kent S. [Department of Metallurgical Engineering, The University of Utah, 50 S. Central Campus Dr., Room 2110, Salt Lake City, UT 84112-0114 (United States); Bowman, Robert C. [Department of Metallurgical Engineering, The University of Utah, 135 South 1460 East, Room 412, Salt Lake City, UT 84112-0114 (United States); Vajo, John J.; Purewal, Justin J. [HRL Laboratories, LLC, 3011 Malibu Canyon Road, Malibu, CA 90265 (United States); Kekelia, Bidzina [Department of Metallurgical Engineering, The University of Utah, 50 S. Central Campus Dr., Room 2110, Salt Lake City, UT 84112-0114 (United States)

2015-10-05

Highlights: • The principle of the thermal battery using advanced metal hydrides was demonstrated. • The thermal battery used MgH{sub 2} and TiMnV as a working pair. • High energy density can be achieved by the use of MgH{sub 2} to store thermal energy. - Abstract: A concept of thermal battery based on advanced metal hydrides was studied for heating and cooling of cabins in electric vehicles. The system utilized a pair of thermodynamically matched metal hydrides as energy storage media. The pair of hydrides that was identified and developed was: (1) catalyzed MgH{sub 2} as the high temperature hydride material, due to its high energy density and enhanced kinetics; and (2) TiV{sub 0.62}Mn{sub 1.5} alloy as the matching low temperature hydride. Further, a proof-of-concept prototype was built and tested, demonstrating the potential of the system as HVAC for transportation vehicles.

On rings generating supernilpotent and special atoms | France ...

African Journals Online (AJOL)

We study prime rings which generate supernilpotent (respectively special) atoms, that is, atoms of the lattice of all supernilpotent (respectively special) radicals. A prime ring A is called a **-ring if the smallest special class containing A is closed under semiprime homomorphic images of A. A semiprime ring A whose every ...

Characteristics of hydride precipitation and reorientation in spent-fuel cladding

International Nuclear Information System (INIS)

Chung, H.M.; Daum, R.S.; Hiller, J.M.; Billone, M.C.

2002-01-01

Transmission electron microscopy (TEM) was used to examine Zircaloy fuel cladding, either discharged from several PWRs and a BWR after irradiation to fluence levels of 3.3 to 8.6 X 10 21 n cm -2 (E > 1 MeV) or hydrogen-charged and heat-treated under stress to produce radial hydrides; the goal was to determine the microstructural and crystallographic characteristics of hydride precipitation. Morphologies, distributions, and habit planes of various types of hydrides were determined by stereo-TEM. In addition to the normal macroscopic hydrides commonly observed by optical microscopy, small 'microscopic' hydrides are present in spent-fuel cladding in number densities at least a few orders of magnitude greater than that of macroscopic hydrides. The microscopic hydrides, observed to be stable at least up to 333 deg C, precipitate in association with -type dislocations. While the habit plane of macroscopic tangential hydrides in the spent-fuel cladding is essentially the same as that of unirradiated unstressed Zircaloys, i.e., the [107] Zr plane, the habit plane of tangential hydrides that precipitate under high tangential stress is the [104] Zr plane. The habit plane of radial hydrides that precipitate under tangential stress is the [011] Zr pyramidal plane, a naturally preferred plane for a cladding that has 30 basal-pole texture. Effects of texture on the habit plane and the threshold stress for hydride reorientation are also discussed. (authors)

Semi-automated ontology generation and evolution

Science.gov (United States)

Stirtzinger, Anthony P.; Anken, Craig S.

2009-05-01

Extending the notion of data models or object models, ontology can provide rich semantic definition not only to the meta-data but also to the instance data of domain knowledge, making these semantic definitions available in machine readable form. However, the generation of an effective ontology is a difficult task involving considerable labor and skill. This paper discusses an Ontology Generation and Evolution Processor (OGEP) aimed at automating this process, only requesting user input when un-resolvable ambiguous situations occur. OGEP directly attacks the main barrier which prevents automated (or self learning) ontology generation: the ability to understand the meaning of artifacts and the relationships the artifacts have to the domain space. OGEP leverages existing lexical to ontological mappings in the form of WordNet, and Suggested Upper Merged Ontology (SUMO) integrated with a semantic pattern-based structure referred to as the Semantic Grounding Mechanism (SGM) and implemented as a Corpus Reasoner. The OGEP processing is initiated by a Corpus Parser performing a lexical analysis of the corpus, reading in a document (or corpus) and preparing it for processing by annotating words and phrases. After the Corpus Parser is done, the Corpus Reasoner uses the parts of speech output to determine the semantic meaning of a word or phrase. The Corpus Reasoner is the crux of the OGEP system, analyzing, extrapolating, and evolving data from free text into cohesive semantic relationships. The Semantic Grounding Mechanism provides a basis for identifying and mapping semantic relationships. By blending together the WordNet lexicon and SUMO ontological layout, the SGM is given breadth and depth in its ability to extrapolate semantic relationships between domain entities. The combination of all these components results in an innovative approach to user assisted semantic-based ontology generation. This paper will describe the OGEP technology in the context of the architectural

Initiation of delayed hydride cracking in zirconium-2.5 wt% niobium

International Nuclear Information System (INIS)

Shalabi, A.F.; Meneley, D.A.

1990-01-01

Delayed hydride cracking in zirconium alloys is caused by the repeated precipitation and cracking of brittle hydrides. The growth kinetic of the hydrides have been measured to evaluate the critical hydride length for crack initiation. Hydride growth leading to crack initiation follows an approximate (time) 1/3 law on the average; crack propagation proceeds in a stepwise fashion. The critical length of hydride for crack initiation increases with stress and temperature. The fracture criterion for crack initiation predicts the critical hydride length at a give stress level and temperature. The fracture initiation mechanism of the hydride confirms the temperature effects for heating and cooling cycles under services loads. (orig.)

Production of propylene from 1-butene on highly active "bi-functional single active site" catalyst: Tungsten carbene-hydride supported on alumina

KAUST Repository

Mazoyer, Etienne

2011-12-02

1-Butene is transformed in a continuous flow reactor over tungsten hydrides precursor W-H/Al2O3, 1, giving a promising yield into propylene at 150 °C and different pressures. Tungsten carbene-hydride single active site operates as a "bi-functional catalyst" through 1-butene isomerization on W-hydride and 1-butene/2-butenes cross-metathesis on W-carbene. This active moiety is generated in situ at the initiation steps by insertion of 1-butene on tungsten hydrides precursor W-H/Al2O3, 1 followed by α-H and β-H abstraction. © 2011 American Chemical Society.

Ductile zirconium powder by hydride-dehydride process

Energy Technology Data Exchange (ETDEWEB)

Krishnan, T S [BHABHA ATOMIC RESEARCH CENTRE, BOMBAY (INDIA); CHAUDHARY, S [NUCLEAR FUEL COMPLEX, HYDERABAD (INDIA)

1976-09-01

The preparation of ductile zirconium powder by the hydride-dehydride process has been described. In this process massive zirconium obtained from Kroll reduction of ZrCl/sub 4/ is first rendered brittle by hydrogenation and the hydride crushed and ground in a ball mill to the required particle size. Hydrogen is then hot vacuum extracted to yield the metal powder. The process has been successfully employed for the production of zirconium powders with low oxygen content and having hardness values in the range of 115-130 BHN, starting from a zirconium sponge of 100-120 BHN hardness. Influence of surface characteristics of the starting metal on its hydriding behaviour has been studied and the optimum hydriding-dehydriding conditions established.

Optimization of chemical and instrumental parameters in hydride generation laser-induced breakdown spectrometry for the determination of arsenic, antimony, lead and germanium in aqueous samples.

Science.gov (United States)

Yeşiller, Semira Unal; Yalçın, Serife

2013-04-03

A laser induced breakdown spectrometry hyphenated with on-line continuous flow hydride generation sample introduction system, HG-LIBS, has been used for the determination of arsenic, antimony, lead and germanium in aqueous environments. Optimum chemical and instrumental parameters governing chemical hydride generation, laser plasma formation and detection were investigated for each element under argon and nitrogen atmosphere. Arsenic, antimony and germanium have presented strong enhancement in signal strength under argon atmosphere while lead has shown no sensitivity to ambient gas type. Detection limits of 1.1 mg L(-1), 1.0 mg L(-1), 1.3 mg L(-1) and 0.2 mg L(-1) were obtained for As, Sb, Pb and Ge, respectively. Up to 77 times enhancement in detection limit of Pb were obtained, compared to the result obtained from the direct analysis of liquids by LIBS. Applicability of the technique to real water samples was tested through spiking experiments and recoveries higher than 80% were obtained. Results demonstrate that, HG-LIBS approach is suitable for quantitative analysis of toxic elements and sufficiently fast for real time continuous monitoring in aqueous environments. Copyright © 2013 Elsevier B.V. All rights reserved.

Alkali metal hydride formation

International Nuclear Information System (INIS)

1976-01-01

The present invention relates to a method of producing alkali metal hydrides by absorbing hydrogen gas under pressure into a mixture of lower alkyl mono amines and alkali metal alkyl amides selected from sodium and potassium amides formed from said amines. The present invention also includes purification of a mixture of the amines and amides which contain impurities, such as is used as a catalytic exchange liquid in the enrichment of deuterium, involving the formation of the alkali metal hydride

SYSTEM OPTIMIZATION FOR THE AUTOMATIC SIMULTANEOUS DETERMINATION OF ARSENIC, SELENIUM, AND ANTIMONY, USING HYDRIDE GENERATION INTRODUCTION TO AN INDUCTIVELY COUPLED PLASMA.

Science.gov (United States)

Pyen, Grace S.; Browner, Richard F.; Long, Stephen

1986-01-01

A fixed-size simplex has been used to determine the optimum conditions for the simultaneous determination of arsenic, selenium, and antimony by hydride generation and inductively coupled plasma emission spectrometry. The variables selected for the simplex were carrier gas flow rate, rf power, viewing height, and reagent conditions. The detection limit for selenium was comparable to the preoptimized case, but there were twofold and fourfold improvements in the detection limits for arsenic and antimony, respectively. Precision of the technique was assessed with the use of artificially prepared water samples.

Automation of steam generator services at public service electric & gas

Energy Technology Data Exchange (ETDEWEB)

Cruickshank, H.; Wray, J.; Scull, D. [Public Service Electric & Gas, Hancock`s Bridge, NJ (United States)

1995-03-01

Public Service Electric & Gas takes an aggressive approach to pursuing new exposure reduction techniques. Evaluation of historic outage exposure shows that over the last eight refueling outages, primary steam generator work has averaged sixty-six (66) person-rem, or, approximately tewenty-five percent (25%) of the general outage exposure at Salem Station. This maintenance evolution represents the largest percentage of exposure for any single activity. Because of this, primary steam generator work represents an excellent opportunity for the development of significant exposure reduction techniques. A study of primary steam generator maintenance activities demonstrated that seventy-five percent (75%) of radiation exposure was due to work activities of the primary steam generator platform, and that development of automated methods for performing these activities was worth pursuing. Existing robotics systems were examined and it was found that a new approach would have to be developed. This resulted in a joint research and development project between Westinghouse and Public Service Electric & Gas to develop an automated system of accomplishing the Health Physics functions on the primary steam generator platform. R.O.M.M.R.S. (Remotely Operated Managed Maintenance Robotics System) was the result of this venture.

Use of reversible hydrides for hydrogen storage

Science.gov (United States)

Darriet, B.; Pezat, M.; Hagenmuller, P.

1980-01-01

The addition of metals or alloys whose hydrides have a high dissociation pressure allows a considerable increase in the hydrogenation rate of magnesium. The influence of temperature and hydrogen pressure on the reaction rate were studied. Results concerning the hydriding of magnesium rich alloys such as Mg2Ca, La2Mg17 and CeMg12 are presented. The hydriding mechanism of La2Mg17 and CeMg12 alloys is given.

U-8 wt %Mo and 7 wt %Mo alloys powder obtained by an hydride-de hydride process

International Nuclear Information System (INIS)

Balart, Silvia N.; Bruzzoni, Pablo; Granovsky, Marta S.; Gribaudo, Luis M. J.; Hermida, Jorge D.; Ovejero, Jose; Rubiolo, Gerardo H.; Vicente, Eduardo E.

2000-01-01

Uranium-molybdenum alloys are been tested as a component in high-density LEU dispersion fuels with very good performances. These alloys need to be transformed to powder due to the manufacturing requirements of the fuels. One method to convert ductile alloys into powder is the hydride-de hydride process, which takes advantage of the ability of the U-α phase to transform to UH 3 : a brittle and relatively low-density compound. U-Mo alloys around 7 and 8 wt % Mo were melted and heat treated at different temperature ranges in order to partially convert γ -phase to α -phase. Subsequent hydriding transforms this α -phase to UH 3 . The volume change associated to the hydride formation embrittled the material which ends up in a powdered alloy. Results of the optical metallography, scanning electron microscopy, X-ray diffraction during different steps of the process are shown. (author)

Reactions of zinc hydride and magnesium hydride with pyridine; synthesis and characterization of 1,4-dihydro-1-pyridylzinc and -magnesium complexes

NARCIS (Netherlands)

Koning, A.J. de; Boersma, J.; Kerk, G.J.M. van der

1980-01-01

The synthesis and characterization of 1,4-dihydro-1-pyridylzinc and -magnesium complexes are described. Zinc hydride and magnesium hydride dissolve in and react with pyridine, and the reaction has been studied in detail in the case of zinc hydride. Evaporation of the solvent after 1–2 hours at 0°C

Hydride Olefin complexes of tantalum and niobium

NARCIS (Netherlands)

Klazinga, Aan Hendrik

1979-01-01

This thesis describes investigations on low-valent tantalum and niobium hydride and alkyl complexes, particularly the dicyclopentadienyl tantalum hydride olefin complexes Cp2Ta(H)L (L=olefin). ... Zie: Summary

Isotope exchange between gaseous hydrogen and uranium hydride powder

International Nuclear Information System (INIS)

Shugard, Andrew D.; Buffleben, George M.; Johnson, Terry A.; Robinson, David B.

2014-01-01

Highlights: • Isotope exchange between hydrogen gas and uranium hydride powder can be rapid and reversible. • Gas–solid exchange rate is controlled by transport within ∼0.7 μm hydride particles. • Gas chromatographic separation of hydrogen isotopes using uranium hydride is feasible. - Abstract: Isotope exchange between gaseous hydrogen and solid uranium hydride has been studied by flowing hydrogen (deuterium) gas through packed powder beds of uranium deuteride (hydride). We used a residual gas analyzer system to perform real-time analysis of the effluent gas composition. We also developed an exchange and transport model and, by fitting it to the experimental data, extracted kinetic parameters for the isotope exchange reaction. Our results suggest that, from approximately 70 to 700 kPa and 25 to 400 °C, the gas-to-solid exchange rate is controlled by hydrogen and deuterium transport within the ∼0.7 μm diameter uranium hydride particles. We use our kinetic parameters to show that gas chromatographic separation of hydrogen and deuterium using uranium hydride could be feasible

Internal hydriding in irradiated defected Zircaloy fuel rods: A review (LWBR Development Program)

International Nuclear Information System (INIS)

Clayton, J.C.

1987-10-01

Although not a problem in recent commercial power reactors, including the Shippingport Light Water Breeder Reactor, internal hydriding of Zircaloy cladding was a persistent cause of gross cladding failures during the 1960s. It occurred in the fuel rods of water-cooled nuclear power reactors that had a small cladding defect. This report summarizes the experimental findings, causes, mechanisms, and methods of minimizing internal hydriding in defected Zircaloy-clad fuel rods. Irradiation test data on the different types of defected fuel rods, intentionally fabricated defected and in-pile operationally defected rods, are compared. Significant factors affecting internal hydriding in defected Zircaloy-clad fuel rods (defect hole size, internal and external sources of hydrogen, Zircaloy cladding surface properties, nickel alloy contamination of Zircaloy, the effect of heat flux and fluence) are discussed. Pertinent in-pile and out-of-pile test results from Bettis and other laboratories are used as a data base in constructing a qualitative model which explains hydrogen generation and distribution in Zircaloy cladding of defected water-cooled reactor fuel rods. Techniques for minimizing internal hydride failures in Zircaloy-clad fuel rods are evaluated

Trapping of hydride forming elements within miniature electrothermal devices. Part 2. Investigation of collection of arsenic and selenium hydrides on a surface and in a cavity of a graphite rod

International Nuclear Information System (INIS)

Docekal, Bohumil

2004-01-01

The interaction of arsenic and selenium hydrides with bare and modified graphite was investigated by atomic absorption spectrometry and by radiotracer technique using 75 Se radionuclide in a laboratory made brass cylindrical chamber equipped with a vertical quartz tube torch for supporting miniature hydrogen diffusion flame atomizer. Strong interaction was observed at elevated temperatures above 800 deg. C. In contrast to the very often-reported data for conventional graphite tube atomizers, this high temperature interaction was also accompanied by a pronounced trapping of analytes at elevated temperatures close to 1100-1200 deg. C when modified graphite was used. Comparing modifiers tested (Ir, Pt and Rh), iridium appeared the only useful permanent modifier. Among various graphite-rod traps designed, the most efficient trapping of analytes was achieved in a graphite cavity. The net selenium trapping efficiencies of approximately 53% and 70% were found by radiotracer technique for the iridium-treated graphite surface and the iridium-treated graphite cavity, respectively. In contrast to the molybdenum surface, bare graphite did not exhibit any significant trapping effect. Trapping isotherms obtained at different temperatures displayed non-linear course in the range up to the upper limit of the analytical relevance of 100 ng of an analyte, indicating a limited trapping capacity of the modified graphite surface and the same trapping mechanism at low and elevated temperatures applied (300-1300 deg. C). Radiography experiments with 75 Se radiotracer showed that a major part of selenium was collected within the small cavity of the graphite rod and that selenium was also deposited after the trapping and vaporization steps in the trap chamber and on the quartz tube wall of the burner. Complementary experiments performed with the conventional transversally heated graphite tube and with bare and thermally shielded injection capillaries for hydride introduction, showed that

In-situ study of hydriding kinetics in Pd-based thin film systems

Energy Technology Data Exchange (ETDEWEB)

Delmelle, Renaud; Proost, Joris [Univ. Catholique de Louvain, Louvain-la-Neuve (Belgium). Div. of Materials and Process Engineering

2010-07-01

The hydriding kinetics of Pd thin films has been investigated in detail. The key experimental technique used in this work consists of a high resolution curvature measurement setup, which continuously monitors the reflections of multiple laser beams coming off a cantilevered sample. After mounting the sample inside a vacuum chamber, a H-containing gas mixture is introduced to instantaneously generate a given hydrogen partial pressure (p{sub H2}) inside the chamber. The resulting interaction of H with the Pd layer then leads to a volume expansion of the thin film system. This induces in turn changes in the sample curvature as a result of internal stresses developing in the Pd film during a hydriding cycle. Based on such curvature date obtained in-situ at different p{sub H2}, a two-step model for the kinetics of Pd-hydride formation has been proposed and expressions for the hydrogen adsorption and absorption velocities have been derived. The rate-limiting steps have been identified by studying the p{sub H2}-dependence of these velocities. Furthermore, from our in-situ experimental data, relevant kinetic parameters have been calculated. The effect of dry air exposure of the Pd films on the hydriding kinetics has been considered as well. (orig.)

Chemical Hydride Slurry for Hydrogen Production and Storage

Energy Technology Data Exchange (ETDEWEB)

McClaine, Andrew W

2008-09-30

The purpose of this project was to investigate and evaluate the attractiveness of using a magnesium chemical hydride slurry as a hydrogen storage, delivery, and production medium for automobiles. To fully evaluate the potential for magnesium hydride slurry to act as a carrier of hydrogen, potential slurry compositions, potential hydrogen release techniques, and the processes (and their costs) that will be used to recycle the byproducts back to a high hydrogen content slurry were evaluated. A 75% MgH₂ slurry was demonstrated, which was just short of the 76% goal. This slurry is pumpable and storable for months at a time at room temperature and pressure conditions and it has the consistency of paint. Two techniques were demonstrated for reacting the slurry with water to release hydrogen. The first technique was a continuous mixing process that was tested for several hours at a time and demonstrated operation without external heat addition. Further work will be required to reduce this design to a reliable, robust system. The second technique was a semi-continuous process. It was demonstrated on a 2 kWh scale. This system operated continuously and reliably for hours at a time, including starts and stops. This process could be readily reduced to practice for commercial applications. The processes and costs associated with recycling the byproducts of the water/slurry reaction were also evaluated. This included recovering and recycling the oils of the slurry, reforming the magnesium hydroxide and magnesium oxide byproduct to magnesium metal, hydriding the magnesium metal with hydrogen to form magnesium hydride, and preparing the slurry. We found that the SOM process, under development by Boston University, offers the lowest cost alternative for producing and recycling the slurry. Using the H2A framework, a total cost of production, delivery, and distribution of $4.50/kg of hydrogen delivered or $4.50/gge was determined. Experiments performed at Boston

Manufacture of titanium and zirconium hydrides

International Nuclear Information System (INIS)

Mares, F.; Hanslik, T.

1973-01-01

A method is described of manufacturing titanium and zirconium hydrides by hydrogenation of said metals characterized by the reaction temperature ranging between 250 to 500 degC, hydrogen pressure of 20 to 300 atm and possibly by the presence of a hydride of the respective metal. (V.V.)

Economical Atomic Layer Deposition

Science.gov (United States)

Wyman, Richard; Davis, Robert; Linford, Matthew

2010-10-01

Atomic Layer Deposition is a self limiting deposition process that can produce films at a user specified height. At BYU we have designed a low cost and automated atomic layer deposition system. We have used the system to deposit silicon dioxide at room temperature using silicon tetrachloride and tetramethyl orthosilicate. Basics of atomic layer deposition, the system set up, automation techniques and our system's characterization are discussed.

Automated Test-Form Generation

Science.gov (United States)

van der Linden, Wim J.; Diao, Qi

2011-01-01

In automated test assembly (ATA), the methodology of mixed-integer programming is used to select test items from an item bank to meet the specifications for a desired test form and optimize its measurement accuracy. The same methodology can be used to automate the formatting of the set of selected items into the actual test form. Three different…

Hydrogen adsorption on palladium and palladium hydride at 1 bar

DEFF Research Database (Denmark)

Johansson, Martin; Skulason, Egill; Nielsen, Gunver

2010-01-01

strongly to Pd hydride than to Pd. The activation barrier for desorption at a H coverage of one mono layer is slightly lower on Pd hydride, whereas the activation energy for adsorption is similar on Pd and Pd hydride. It is concluded that the higher sticking probability on Pd hydride is most likely caused...

Hydride observations using the neutrography technique

International Nuclear Information System (INIS)

Meyer, G.; Baruj, A.; Borzone, E.M.; Cardenas, R.; Szames, E.; Somoza, J.; Rivas, S.; Sanchez, F.A.; Marin, J.

2012-01-01

Neutron radiography observations were performed at the RA-6 experimental nuclear facility in Bariloche. Images from a prototype of a hydride-based hydrogen storage device have been obtained. The technique allows visualizing the inner hydride space distribution. The hydride appeared compacted at the lower part of the prototype after several cycles of hydrogen charge and discharge. The technique has also been applied to the study of Zr/ZrH 2 samples. There is a linear relation between the sample width/hydrogen concentration and the photograph grey scale. This information could be useful for the study of nuclear engineering materials and to determine their possible degradation by hydrogen pick up (author)

Hydride heat pump with heat regenerator

Science.gov (United States)

Jones, Jack A. (Inventor)

1991-01-01

A regenerative hydride heat pump process and system is provided which can regenerate a high percentage of the sensible heat of the system. A series of at least four canisters containing a lower temperature performing hydride and a series of at least four canisters containing a higher temperature performing hydride is provided. Each canister contains a heat conductive passageway through which a heat transfer fluid is circulated so that sensible heat is regenerated. The process and system are useful for air conditioning rooms, providing room heat in the winter or for hot water heating throughout the year, and, in general, for pumping heat from a lower temperature to a higher temperature.

Monte Carlo generated spectra for QA/QC of automated NAA routine

International Nuclear Information System (INIS)

Jackman, K.R.; Biegalski, S.R.

2007-01-01

A quality check for an automated system of analyzing large sets of neutron activated samples has been developed. Activated samples are counted with an HPGe detector, in conjunction with an automated sample changer and spectral analysis tools, controlled by the Canberra GENIE 2K and REXX software. After each sample is acquired and analyzed, a Microsoft Visual Basic program imports the results into a template Microsoft Excel file where the final concentrations, uncertainties, and detection limits are determined. Standard reference materials are included in each set of 40 samples as a standard quality assurance/quality control (QA/QC) test. A select group of sample spectra are also visually reviewed to check the peak fitting routines. A reference spectrum was generated in MCNP 4c2 using an F8, pulse-height, tally with a detector model of the actual detector used in counting. The detector model matches the detector resolution, energy calibration, and counting geometry. The generated spectrum also contained a radioisotope matrix that was similar to what was expected in the samples. This spectrum can then be put through the automated system and analyzed along with the other samples. The automated results are then compared to expected results for QA/QC assurance. (author)

The use of L-ascorbic acid in speciation of arsenic compounds in drinking water

Directory of Open Access Journals (Sweden)

Marjanović Nikola J.

2009-01-01

Full Text Available Arsenic speciation, besides total arsenic content determination, is very important in analysis of water, foodstuffs, and environmental samples, because of varying degrees of toxicity of different species. For such purpose hydride generation atomic absorption spectrometry can be used based on the generation of certain types of hydride, depending on the pH value and pretreatment in different reaction media. In this study, we have investigated the effect of L-ascorbic acid as the reaction medium as well as the pre-reducing agent in speciation of arsenic by hydride generation-atomic absorption spectrometry in order to determine monomethyl arsonic acid (MMA in the presence of inorganic forms of arsenic.

Technology and automation of atomic power engineering and industry. TAAPEI-2009. Materials of branch scientific and technical conference covers the fiftieth anniversary of the Seversk State Engineering Academy

International Nuclear Information System (INIS)

2009-01-01

Materials of the branch scientific and technical conference Technology and automation of atomic power engineering and industry (18-22 May, 2009, Seversk) are performed. Scientific and practical results of investigations into chemical technological developments, creation of machinery and apparatuses, automation of technological processes, application of present-day information technologies in atomic industry as well as ecological and nuclear weapons proliferation problems are shown. Besides issues of professional education and social-economic problems of the atomic branch are considered [ru

Electronic structure, bonding and chemisorption in metallic hydrides

International Nuclear Information System (INIS)

Ward, J.W.

1980-01-01

Problems that can arise during the cycling steps for a hydride storage system usually involve events at surfaces. Chemisorption and reaction processes can be affected by small amounts of contaminants that may act as catalytic poisons. The nature of the poisoning process can vary greatly for the different metals and alloys that form hydrides. A unifying concept is offered, which satisfactorily correlates many of the properties of transition-metal, rare-earth and actinide hydrides. The metallic hydrides can be differentiated on the basis of electronegativity, metallic radius (valence) and electronic structure. For those systems where there are d (transition metals) or f (early actinides) electrons near the Fermi level a broad range of chemical and catalytic behaviors are found, depending on bandwidth and energy. The more electropositive metals (rare-earths, actinides, transition metals with d > 5) dissolve hydrogen and form hydrides by an electronically somewhat different process, and as a class tend to adsorb electrophobic molecules. The net charge-transfer in either situation is subtle; however, the small differences are responsible for many of the observed structural, chemical, and catalytic properties in these hydride systems

High pressure hydriding of sponge-Zr in steam-hydrogen mixtures

International Nuclear Information System (INIS)

Kim, Y.S.

1997-01-01

Hydriding kinetics of thin sponge-Zr layers metallurgically bonded to a Zircaloy disk has been studied by thermogravimetry in the temperature range 350-400 C in 7 MPa hydrogen-steam mixtures. Some specimens were prefilmed with a thin oxide layer prior to exposure to the reactant gas; all were coated with a thin layer of gold to avoid premature reaction at edges. Two types of hydriding were observed in prefilmed specimens, viz., a slow hydrogen absorption process that precedes an accelerated (massive) hydriding. At 7 MPa total pressure, the critical ratio of H 2 /H 2 O above which massive hydriding occurs at 400 C is ∝200. The critical H 2 /H 2 O ratio is shifted to ∝2.5 x 10 3 at 350 C. The slow hydriding process occurs only when conditions for hydriding and oxidation are approximately equally favorable. Based on maximum weight gain, the specimen is completely converted to δ-ZrH 2 by massive hydriding in ∝5 h at a hydriding rate of ∝10 -6 mol H/cm 2 s. Incubation times of 10-20 h prior to the onset of massive hydriding increases with prefilm oxide thickness in the range of 0-10 μm. By changing to a steam-enriched gas, massive hydriding that initially started in a steam-starved condition was arrested by re-formation of a protective oxide scale. (orig.)

Stress analysis of hydride bed vessels used for tritium storage

International Nuclear Information System (INIS)

McKillip, S.T.; Bannister, C.E.; Clark, E.A.

1991-01-01

A prototype hydride storage bed, using LaNi 4.25 Al 0.75 as the storage material, was fitted with strain gages to measure strains occurring in the stainless steel bed vessel caused by expansion of the storage powder upon uptake of hydrogen. The strain remained low in the bed as hydrogen was added, up to a bed loading of about 0.5 hydrogen to metal atom ratio (H/M). The strain then increased with increasing hydrogen loading (∼ 0.8 H/M). Different locations exhibited greatly different levels of maximum strain. In no case was the design stress of the vessel exceeded

A study of stress reorientation of hydrides in zircaloy

Energy Technology Data Exchange (ETDEWEB)

Yourong, Jiang; Bangxin, Zhou [Nuclear Power Inst. of China, Chengdu, SC (China)

1994-10-01

Under the conditions of circumferential tensile stress from 70 to 180 MPa for Zircaloy tubes or the tensile stress from 55 to 180 MPa for Zircaloy-4 plates and temperature cycling between 150 and 400 degree C, the effects of stress and the number of temperature cycling on hydride reorientation in Zircaloy-4 tubes and plates and Zircaloy-2 tubes containing about 220 {mu}g/g hydrogen have been investigated. With the increase of stress and/or the number of temperature cycling, the level of hydride reorientation increases. When hydride reorientation takes place, there is a threshold stress concerned with the number of temperature cycling. Below the threshold stress, hydride reorientation is not obvious. When applied stress is higher than the threshold stress, the level of hydride reorientation increases with the increase of stress and the number of temperature cycling. Hydride reorientation in Zircaloy-4 tubes develops gradually from the outer surface to inner surface. It might be related to the difference of texture between outer surface and inner surface. The threshold stress is affected by both the texture and the value of B. So controlling texture could still restrict hydride reorientation under tensile stress.

Process variables in the obtention of U-Mo powder by the hydriding-milling-dehydriding method (HMD process)

International Nuclear Information System (INIS)

Pasqualini, Enrique E.; Helzel Garcia, Javier; Lopez, Marisol

2003-01-01

In the next few years nuclear fuels based on uranium oxides, aluminides and silicides for MTR reactors will be replaced by the high density alloy uranium- 7% (w/w) molybdenum (U-7 Mo). Actually there is only one commercial supplier of this raw material that has to be provided as powder containing 20% enriched uranium ( 235 U). In the Nuclear Fuels Department of the National Atomic Energy Commission (CNEA) at Buenos Aires was developed an alternative way of producing U-7 Mo powder in a production scale. Meanwhile CNEA is participating in the International Program (RERTR) for final qualification of this nuclear material. This new method of production consists in the hydriding of the alloy, milling the hydride to final size and dehydriding the powder. These results were achieved because a special technique was discovered for the massive hydriding of the U-7 Mo alloy. The production method is simple, requires conventional equipment and low investment. Argentine can have important comparative advantages for its production and exportation. A scale production plant is being planed. (author)

IAEA co-ordinated research program. 'Round Robin' on measuring the velocity of delayed hydride cracking (DHC)

Energy Technology Data Exchange (ETDEWEB)

Grigoriev, V.; Jakobsson, R. [Studsvik Material AB, Nykoeping (Sweden)

1999-09-01

The International Atomic Agency (IAEA) has initiated a new Co-ordinated Research Programme (CRP) on Hydrogen and hydride induced degradation of the mechanical and physical properties of Zirconium-based alloys. In the first phase of this CRP the methodology for measuring the velocity of Delayed Hydride Cracking (DHC) should be established and participating laboratories from about nine countries around the world carry out identical tests in 'round robin'. The objective of the present work is to establish at Studsvik laboratory the method of a constant load cracking test on unirradiated Zr-2.5Nb and attain a comparison of results between laboratories. Constant load tests are performed on specimens cut from unirradiated CANDU Zr-2.5Nb pressure tube and the rate of crack propagation is determined in each test. Pre-hydrided specimens for testing are supplied from the host laboratory. Six specimens have been tested for delayed hydride cracking (DHC) at 250 deg C. The axial crack growth velocities measured in the tests are within the interval of 8.62x10{sup -8} - 1.06x10{sup -7} m/s. The results obtained agree well with the earlier published data for similar materials and test conditions.

Preparation and hydrogen-deuterium exchange of alkyl and hydride bis(trimethylsilyl)amido derivatives of the actinide elements

International Nuclear Information System (INIS)

Simpson, S.J.; Turner, H.W.; Andersen, R.A.

1981-01-01

The monomeric, hydrocarbon-soluble monohydrides and monodeuterides of the actinide metals (thorium or uranium) of the type HM[N(SiMe 3 ) 2 ] 3 have been prepared. Their reaction chemistry - n-BuLi followed by MeBr yields MeM[N(SiMe 3 ) 2 ] 3 and borane in tetrahydrofuran yields BH 4 M[N(SiMe 3 ) 2 ] 3 - suggests that the hydrogen atom is hydridic. Pyrolysis of the hydrides yields the novel, four-membered ring metallacycle [(Me 3 Si) 2 N] 2 MCH 2 Si(Me) 2 NSiMe 3 where M is Th or U. These metallacycles are the key intermediates in the hydrogen-deuterium exchange reaction that yields ([CD 3 ) 3 Si] 2 N) 3 MD

Transmission Electron Microscopy Studies on Titanium-doped Sodium Aluminum Hydride

Science.gov (United States)

Culnane, Lance F.

Hydrogen fuel cells play an important role in today's diverse and blossoming alternative energy industry. One of the greatest technological barriers for vehicular applications is the storage of hydrogen (which is required to power hydrogen fuel cells). Storing hydrogen as a gas is not volume efficient, and storing it as a liquid is not cost effective, therefore solid-state storage of hydrogen, such as in metal hydrides offers the most potential for success since many metal hydrides have attractive qualities for hydrogen storage such as: high volumetric capacity, cost efficiency, weight efficiency, low refueling times, and most importantly, high safety. Unfortunately, a compound has not been discovered which contains all of the attractive hydrogen storage qualities for vehicular applications. Sodium aluminum hydride (NaAlH 4) is one of the few compounds which is close to meeting requirements for car manufacturers, and has perhaps been researched the most extensively out of all metal hydrides in the last 15 years. This arises from the remarkable discovery by Bogdanovic who found that doping NaAlH4 with Ti dopants enabled the reversible dehydrogenation and hydrogenation of NaAlH 4 at mild conditions. Various evidence and theories have been proposed to suggest explanations for the enhanced kinetic effect that Ti-doping and ball-milling provide. However, the research community has not reached a consensus as to the exact role of Ti-dopants. If the role of titanium in the NaAlH4 dehydrogenation/hydrogenation mechanism could be understood, then more attractive metal hydrides could be designed. To this end, we conducted Transmission Electron Microscopy (TEM) studies to explain the role of the Ti dopants. The first known thorough particle size analysis of the NaAlH4 system was conducted, as well as TEM-EELS (Electron Energy Loss Spectroscopy), TEM-EDS (Energy Dispersive X-ray Spectroscopy), and in-situ imaging studies. Preparation methods were found to be important for the

Generation of Bell, NOON and W states via atom interferometry

Energy Technology Data Exchange (ETDEWEB)

Islam, Rameez-ul; Saif, Farhan [Department of Electronics, Quaid-i-Azam University, Islamabad (Pakistan); Khosa, Ashfaq H [Centre for Quantum Physics, COMSATS Institute of Information Technology, Islamabad (Pakistan)

2008-02-14

We propose atom interferometric techniques for the generation of Bell, NOON and W states of an electromagnetic field in high-Q cavities. The fundamental constituent of these techniques is off-resonant Bragg diffraction of atomic de Broglie waves. We show good success probabilities for these schemes under the currently available experimental environment of atom interferometry.

A procedure for preparing alkali metal hydrides

International Nuclear Information System (INIS)

Lemieux, R.U.; Sanford, C.E.; Prescott, J.F.

1976-01-01

A plain low cost, procedure for the continuous, low temperature preparation of sodium or potassium hydrides using cheap reagents is presented. Said invention is especially concerned with a process of purifying of a catalytic exchange liquid used for deuterium enrichment, in which an alkali metal hydride is produced as intermediate product. The procedure for producing the sodium and potassium hydrides consists in causing high pressure hydrogen to be absorbed by a mixture of at least a lower monoalkylamine and an alkylamide of an alkali metal from at least one of said amines [fr

In situ hydride formation in titanium during focused ion milling.

Science.gov (United States)

Ding, Rengen; Jones, Ian P

2011-01-01

It is well known that titanium and its alloys are sensitive to electrolytes and thus hydrides are commonly observed in electropolished foils. In this study, focused ion beam (FIB) milling was used to prepare thin foils of titanium and its alloys for transmission electron microscopy. The results show the following: (i) titanium hydrides were observed in pure titanium, (ii) the preparation of a bulk sample in water or acid solution resulted in the formation of more hydrides and (iii) FIB milling aids the precipitation of hydrides, but there were never any hydrides in Ti64 and Ti5553.

Two-pulse atomic coherent control spectroscopy of Eley-Rideal reactions: An application of an atom laser

International Nuclear Information System (INIS)

Joergensen, Solvejg; Kosloff, Ronnie

2003-01-01

A spectroscopic application of the atom laser is suggested. The spectroscopy termed 2PACC (two-pulse atomic coherent control) employs the coherent properties of matter waves from a two-pulse atom laser. These waves are employed to control a gas-surface chemical recombination reaction. The method is demonstrated for an Eley-Rideal reaction of a hydrogen or alkali atom-laser pulse where the surface target is an adsorbed hydrogen atom. The reaction yields either a hydrogen or alkali hydride molecule. The desorbed gas-phase molecular yield and its internal state is shown to be controlled by the time and phase delay between two atom-laser pulses. The calculation is based on solving the time-dependent Schroedinger equation in a diabatic framework. The probability of desorption which is the predicted 2PACC signal has been calculated as a function of the pulse parameters

Economic analysis of hydride fueled BWR

International Nuclear Information System (INIS)

Ganda, F.; Shuffler, C.; Greenspan, E.; Todreas, N.

2009-01-01

The economic implications of designing BWR cores with hydride fuels instead of conventional oxide fuels are analyzed. The economic analysis methodology adopted is based on the lifetime levelized cost of electricity (COE). Bracketing values (1970 and 3010 $/kWe) are used for the overnight construction costs and for the power scaling factors (0.4 and 0.8) that correlate between a change in the capital cost to a change in the power level. It is concluded that a newly constructed BWR reactor could substantially benefit from the use of 10 x 10 hydride fuel bundles instead of 10 x 10 oxide fuel bundles design presently in use. The cost saving would depend on the core pressure drop constraint that can be implemented in newly constructed BWRs - it is between 2% and 3% for a core pressure drop constraint as of the reference BWR, between 9% and 15% for a 50% higher core pressure drop, and between 12% and 21% higher for close to 100% core pressure. The attainable cost reduction was found insensitive to the specific construction cost but strongly dependent on the power scaling factor. The cost advantage of hydride fuelled cores as compared to that of the oxide reference core depends only weakly on the uranium and SWU prices, on the 'per volume base' fabrication cost of hydride fuels, and on the discount rate used. To be economically competitive, the uranium enrichment required for the hydride fuelled core needs to be around 10%.

OPTIMIZATION OF INTERNAL HEAT EXCHANGERS FOR HYDROGEN STORAGE TANKS UTILIZING METAL HYDRIDES

Energy Technology Data Exchange (ETDEWEB)

Garrison, S.; Tamburello, D.; Hardy, B.; Anton, D.; Gorbounov, M.; Cognale, C.; van Hassel, B.; Mosher, D.

2011-07-14

Two detailed, unit-cell models, a transverse fin design and a longitudinal fin design, of a combined hydride bed and heat exchanger are developed in COMSOL{reg_sign} Multiphysics incorporating and accounting for heat transfer and reaction kinetic limitations. MatLab{reg_sign} scripts for autonomous model generation are developed and incorporated into (1) a grid-based and (2) a systematic optimization routine based on the Nelder-Mead downhill simplex method to determine the geometrical parameters that lead to the optimal structure for each fin design that maximizes the hydrogen stored within the hydride. The optimal designs for both the transverse and longitudinal fin designs point toward closely-spaced, small cooling fluid tubes. Under the hydrogen feed conditions studied (50 bar), a 25 times improvement or better in the hydrogen storage kinetics will be required to simultaneously meet the Department of Energy technical targets for gravimetric capacity and fill time. These models and methodology can be rapidly applied to other hydrogen storage materials, such as other metal hydrides or to cryoadsorbents, in future work.

Multidimensional simulations of hydrides during fuel rod lifecycle

International Nuclear Information System (INIS)

Stafford, D.S.

2015-01-01

In light water reactor fuel rods, waterside corrosion of zirconium-alloy cladding introduces hydrogen into the cladding, where it is slightly soluble. When the solubility limit is reached, the hydrogen precipitates into crystals of zirconium hydride which decrease the ductility of the cladding and may lead to cladding failure during dry storage or transportation events. The distribution of the hydride phase and the orientation of the crystals depend on the history of the spatial temperature and stress profiles in the cladding. In this work, we have expanded the existing hydride modeling capability in the BISON fuel performance code with the goal of predicting both global and local effects on the radial, azimuthal and axial distribution of the hydride phase. We compare results from 1D simulations to published experimental data. We demonstrate the new capability by simulating in 2D a fuel rod throughout a lifecycle that includes irradiation, short-term storage in the spent fuel pool, drying, and interim storage in a dry cask. Using the 2D simulations, we present qualitative predictions of the effects of the inter-pellet gap and the drying conditions on the growth of a hydride rim. - Highlights: • We extend BISON fuel performance code to simulate lifecycle of fuel rods. • We model hydrogen evolution in cladding from reactor through dry storage. • We validate 1D simulations of hydrogen evolution against experiments. • We show results of 2D axisymmetric simulations predicting hydride formation. • We show how our model predicts formation of a hydride rim in the cladding.

Creating nanoshell on the surface of titanium hydride bead

Directory of Open Access Journals (Sweden)

PAVLENKO Vyacheslav Ivanovich

2016-12-01

Full Text Available The article presents data on the modification of titanium hydride bead by creating titanium nanoshell on its surface by ion-plasma vacuum magnetron sputtering. To apply titanium nanoshell on the titanium hydride bead vacuum coating plant of multifunctional nanocomposite coatings QVADRA 500 located in the center of high technology was used. Analysis of the micrographs of the original surface of titanium hydride bead showed that the microstructure of the surface is flat, smooth, in addition the analysis of the microstructure of material surface showed the presence of small porosity, roughness, mainly cavities, as well as shallow longitudinal cracks. The presence of oxide film in titanium hydride prevents the free release of hydrogen and fills some micro-cracks on the surface. Differential thermal analysis of both samples was conducted to determine the thermal stability of the initial titanium hydride bead and bead with applied titanium nanoshell. Hydrogen thermal desorption spectra of the samples of the initial titanium hydride bead and bead with applied titanium nanoshell show different thermal stability of compared materials in the temperature range from 550 to 860о C. Titanium nanoshells applied in this way allows increasing the heat resistance of titanium hydride bead – the temperature of starting decomposition is 695о C and temperature when decomposition finishes is more than 1000о C. Modified in this way titanium hydride bead can be used as a filler in the radiation protective materials used in the construction or upgrading biological protection of nuclear power plants.

High H⁻ ionic conductivity in barium hydride.

Science.gov (United States)

Verbraeken, Maarten C; Cheung, Chaksum; Suard, Emmanuelle; Irvine, John T S

2015-01-01

With hydrogen being seen as a key renewable energy vector, the search for materials exhibiting fast hydrogen transport becomes ever more important. Not only do hydrogen storage materials require high mobility of hydrogen in the solid state, but the efficiency of electrochemical devices is also largely determined by fast ionic transport. Although the heavy alkaline-earth hydrides are of limited interest for their hydrogen storage potential, owing to low gravimetric densities, their ionic nature may prove useful in new electrochemical applications, especially as an ionically conducting electrolyte material. Here we show that barium hydride shows fast pure ionic transport of hydride ions (H(-)) in the high-temperature, high-symmetry phase. Although some conductivity studies have been reported on related materials previously, the nature of the charge carriers has not been determined. BaH2 gives rise to hydride ion conductivity of 0.2 S cm(-1) at 630 °C. This is an order of magnitude larger than that of state-of-the-art proton-conducting perovskites or oxide ion conductors at this temperature. These results suggest that the alkaline-earth hydrides form an important new family of materials, with potential use in a number of applications, such as separation membranes, electrochemical reactors and so on.

Understanding hydride formation in Zr-1Nb alloy through microstructural characterization

International Nuclear Information System (INIS)

Neogy, S.; Srivastava, D.; Tewari, R.; Singh, R.N.; Dey, G.K.; De, P.K.; Banerjee, S.

2003-07-01

In this study the experimental results of hydride formation and their microstructure evolution in Zr-1Nb alloy is presented. This Zr-1Nb binary alloy and other Zr-1 Nb based ternary and quaternary alloys are being used as fuel tube materials and have the potential for meeting the requirement of high burn up fuel. Hydriding of Zr-1Nb alloy having a microstructure comprising equiaxed α grains and a uniform distribution of spherical particles of the β phase has been carried out in this study. The specimens have been hydrided by gaseous charging method to different hydrogen levels. The microstructures of hydrided samples were examined as a function of hydrogen content. The formation of δ hydride in slow cooled specimens and formation of γ hydride in rapidly cooled specimens has been studied with their morphology, habit plane and orientation relationship with the α matrix in view. The habit planes of either type of hydride phase has been determined and compared with those observed in other Zr-Nb alloys. The orientation relationship between the α matrix and the δ hydride was found to be the following: (0001) α // (111) δ and [1120] α // [110] δ . The orientation relationship between the α matrix and the γ hydride was of the following type: (0001) α // (111) γ and [1120] α // [110] γ . The internal structure of both types of hydride has been examined. The effect of the presence of the spherical β phase particles in the a matrix on the growth of the hydride plates has been investigated. (author)

Development of zirconium hydride highly effective moderator materials

International Nuclear Information System (INIS)

Yin Changgeng

2005-10-01

The zirconium hydride with highly content of hydrogen and low density is new efficient moderator material for space nuclear power reactor. Russia has researched it to use as new highly moderator and radiation protection materials. Japanese has located it between the top of pressure vessel and the main protection as a shelter, the work temperature is rach to 220 degree C. The zirconium hydride moderator blocks are main parts of space nuclear power reactor. Development of zirconium hydride moderator materials have strength research and apply value. Nuclear Power Research and Design Instituteoh China (NPIC) has sep up the hydrogenation device and inspect systems, and accumurate a large of experience about zirconium hydride, also set up a strict system of QA and QC. (authors)

Hydriding of metallic thorium

International Nuclear Information System (INIS)

Miyake, Masanobu; Katsura, Masahiro; Matsuki, Yuichi; Uno, Masayoshi

1983-01-01

Powdered thorium is usually prepared through a combination of hydriding and dehydriding processes of metallic thorium in massive form, in which the hydriding process consists of two steps: the formation of ThH 2 , and the formation of Th 4 H 15 . However, little has yet been known as to on what stage of hydriding process the pulverization takes place. It is found in the present study that the formation of Th 4 H 15 by the reaction of ThH 2 with H 2 is responsible for pulverization. Temperature of 70 deg C adopted in this work for the reaction of formation Th 4 H 15 seems to be much more effective for production of powdered thorium than 200 - 300 deg C in the literature. The pressure-composition-temperature relationships for Th-H system are determined at 200, 300, 350, and 800 deg C. From these results, a tentative equilibrium phase diagram for the Th-H system is proposed, attention being focused on the two-phase region of ThH 2 and Th 4 H 15 . Pulverization process is discussed in terms of the tentative phase diagram. (author)

Artificial exomuscle investigations for applications-metal hydride

International Nuclear Information System (INIS)

Crevier, Marie-Charlotte; Richard, Martin; Rittenhouse, D Matheson; Roy, Pierre-Olivier; Bedard, Stephane

2007-01-01

In pursuing the development of bionic devices, Victhom identified a need for technologies that could replace current motorized systems and be better integrated into the human body motion. The actuators used to obtain large displacements are noisy, heavy, and do not adequately reproduce human muscle behavior. Subsequently, a project at Victhom was devoted to the development of active materials to obtain an artificial exomuscle actuator. An exhaustive literature review was done at Victhom to identify promising active materials for the development of artificial muscles. According to this review, metal hydrides were identified as a promising technology for artificial muscle development. Victhom's investigations focused on determining metal hydride actuator potential in the context of bionics technology. Based on metal hydride properties and artificial muscle requirements such as force, displacement and rise time, an exomuscle was built. In addition, a finite element model, including heat and mass transfer in the metal hydride, was developed and implemented in FEMLAB software. (review article)

Density of trapped gas in heavily-irradiated lithium hydride

International Nuclear Information System (INIS)

Bowman, R.C. Jr.; Attalla, A.; Souers, P.C.; Folkers, C.L.; McCreary, T.; Snider, G.D.; Vanderhoofven, F.; Tsugawa, R.T.

1988-01-01

We review old gamma-irradiated lithium hydride data and also display much new bulk and gas-displacement density and nuclear magnetic resonance data on Li(D, T) and LiT at 296 to 373 K. We find that: (1) Li(D, T) swells because of the formation of internal D-T and 3 He gas bubbles, but probably not because of the precipitation of lithium metal; (2) the gas bubbles are at densities of at least 3 to 4x10 4 mol/m 3 , i.e. thousands of atmospheres; (3) outgassing may be largely the result of bubbles rupturing, although diffusion of 3 He as atoms may occur at long times. (orig.)

The role of chemical free energy and elastic strain in the nucleation of zirconium hydride

International Nuclear Information System (INIS)

Barrow, A.T.W.; Toffolon-Masclet, C.; Almer, J.; Daymond, M.R.

2013-01-01

In this work a combination of synchrotron X-ray diffraction and thermodynamic modelling has been used to study the dissolution and precipitation of zirconium hydride in α-Zr establishing the role of elastic misfit strain and chemical free energy in the α → α + δ phase transformation. The nucleation of zirconium hydride is dominated by the chemical free energy where the chemical driving force for hydride precipitation is proportional to the terminal-solid solubility for precipitation and can be predicted by a function that is analogous to the universal nucleation parameter for the bainite transformation in ferrous alloys. The terminal-solid solubility for precipitation was found to be kinetically limited ⩾287 °C at a cooling rate of 5 °C min −1 or greater. The terminal solubilities were established using an offset method applied to the lattice strain data where a resolution of ∼10 wppm H can be achieved in the 〈c〉-direction. This is aided by the introduction of intra-granular strains in the 〈c〉-direction during cooling as a result of the thermal expansion anisotropy which increases the anisotropy associated with the misfitting H atoms within the α-Zr lattice

Conceptual study on deep-underground energy generation base

International Nuclear Information System (INIS)

Hayano, M.; Okawa, T.

1992-01-01

Mitsubishi Atomic Power Industries, Inc. (MAPI) and Taisei Corporation have started a conceptual study on a deep-underground energy generation base for future cities in the 21st century around the metropolitan area, which will be increasingly important from viewpoints of the autonomy and sharing of the energy supply to the future cities. The energy generation base consists of a gas cooled reactor with naturally safety features as the energy source, an electric generation base using the Alkali Metal Thermo-electric Converter (AMTEC), a hydrogen production plant with the Solid Polymer Electrolyte (SPE), a hydrogen storage plant with the Metal Hydride (MH), and a desalination plant. This paper describes a concept of the energy generation base and the structure in the deep-underground, in soft soil, then the basic system of each plant, and finally discusses the feasibility of the deep-underground energy generation base. (author)

Atomistic simulation of hydrogen dynamics near dislocations in vanadium hydrides

International Nuclear Information System (INIS)

Ogawa, Hiroshi

2015-01-01

Highlights: • Hydrogen–dislocation interaction was simulated by molecular dynamics method. • Different distribution of H atoms were observed at edge and screw dislocation. • Planner distribution of hydrogen may be caused by partialized edge dislocation. • Hydrogen diffusivity was reduced in both edge and screw dislocation models. • Pipe diffusion was observed for edge dislocation but not for screw dislocation. - Abstract: Kinetics of interstitial hydrogen atoms near dislocation cores were analyzed by atomistic simulation. Classical molecular dynamics method was applied to model structures of edge and screw dislocations in α-phase vanadium hydride. Simulation showed that hydrogen atoms aggregate near dislocation cores. The spatial distribution of hydrogen has a planner shape at edge dislocation due to dislocation partialization, and a cylindrical shape at screw dislocation. Simulated self-diffusion coefficients of hydrogen atoms in dislocation models were a half- to one-order lower than that of dislocation-free model. Arrhenius plot of self-diffusivity showed slightly different activation energies for edge and screw dislocations. Directional dependency of hydrogen diffusion near dislocation showed high and low diffusivity along edge and screw dislocation lines, respectively, hence so called ‘pipe diffusion’ possibly occur at edge dislocation but does not at screw dislocation

Dealloyed Ruthenium Film Catalysts for Hydrogen Generation from Chemical Hydrides

Directory of Open Access Journals (Sweden)

Ramis B. Serin

2017-07-01

Full Text Available Thin-film ruthenium (Ru and copper (Cu binary alloys have been prepared on a Teflon™ backing layer by cosputtering of the precious and nonprecious metals, respectively. Alloys were then selectively dealloyed by sulfuric acid as an etchant, and their hydrogen generation catalysts performances were evaluated. Sputtering time and power of Cu atoms have been varied in order to tailor the hydrogen generation performances. Similarly, dealloying time and the sulfuric acid concentration have also been altered to tune the morphologies of the resulted films. A maximum hydrogen generation rate of 35 mL min−1 was achieved when Cu sputtering power and time were 200 W and 60 min and while acid concentration and dealloying time were 18 M and 90 min, respectively. It has also been demonstrated that the Ru content in the alloy after dealloying gradually increased with the increasing the sputtering power of Cu. After 90 min dealloying, the Ru to Cu ratio increased to about 190 times that of bare alloy. This is the key issue for observing higher catalytic activity. Interestingly, we have also presented template-free nanoforest-like structure formation within the context of one-step alloying and dealloying used in this study. Last but not least, the long-time hydrogen generation performances of the catalysts system have also been evaluated along 3600 min. During the first 600 min, the catalytic activity was quite stable, while about 24% of the catalytic activity decayed after 3000 min, which still makes these systems available for the development of robust catalyst systems in the area of hydrogen generation.

YNi and its hydrides: Phase stabilities, electronic structures and chemical bonding properties from first principles

International Nuclear Information System (INIS)

Matar, S.F.; Nakhl, M.; Al Alam, A.F.; Ouaini, N.; Chevalier, B.

2010-01-01

Graphical abstract: Base centered orthorhombic YNiH X structure. For x = 3, only H1 and H2 are present. Highest hydrogen content YNiH 4 is obtained when H3 are added. - Abstract: Within density functional theory, establishing the equations of states of YNi in two different controversial structures in the literature, leads to determine the orthorhombic FeB-type as the ground state one with small energy difference. For YNiH 3 and YNiH 4 hydrides crystallizing in the orthorhombic CrB-type structure the geometry optimization and the ab initio determination of the H atomic positions show that the stability of hydrogen decreases from the tri- to the tetra- hydride. New states brought by hydrogen within the valence band lead to its broadening and to enhanced localization of metal density of states. The chemical bonding analysis shows a preferential Ni-H bonding versus Y-H.

SPECIATION OF SELENIUM AND ARSENIC COMPOUNDS BY CAPILLARY ELECTROPHORESIS WITH HYDRODYNAMICALLY MODIFIED ELECTROOSMOTIC FLOW AND ON-LINE REDUCTION OF SELENIUM(VI) TO SELENIUM(IV) WITH HYDRIDE GENERATION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRIC DETECTION

Science.gov (United States)

Capillary electrophoresis (CE) with hydride generation inductively coupled plasma mass spectrometry was used to determine four arsenicals and two selenium species. Selenate (SeVI) was reduced on-line to selenite (SeIV') by mixing the CE effluent with concentrated HCl. A microporo...

The growth of crystals of erbium hydride

International Nuclear Information System (INIS)

Grimshaw, J.A.; Spooner, F.J.; Wilson, C.G.; McQuillan, A.D.

1981-01-01

Crystals of the rare-earth hydride ErH 2 have been produced with face areas greater than a square millimetre and corresponding volumes exceeding those of earlier crystals by orders of magnitude. The hydride, which was produced in bulk polycrystalline form by hydriding erbium metal at 950 0 C, has been examined by optical and X-ray techniques. For material of composition ErH 2 and ErHsub(1.8) the size of the grains and their degree of strain appears to depend more on oxygen contamination during formation and on the subsequent cooling procedure, than on the size of erbium metal crystals in the starting material. (author)

Identification of the zirconium hydrides metallography in zircaloy-2

International Nuclear Information System (INIS)

Garcia Gonzalez, F.

1968-01-01

Technique for the Identification of the zirconium hydrides in metallographic specimens have been developed. Microhardness, quantitative estimation and relative orientation of the present hydrides as well as grain size determination of the different Zircaloy-2 tube specimens have also been made. The specimens used were corrosion- tested in water during various periods of time at 300 degree castrating, prior to the metallographic examination. Reference specimens, as received, and heavily hydride specimens in a hydrogen atmosphere at 800 degree centigrees, have been used in the previous stages of the work. No difficulties have been met in this early stage of acquaintanceship with the zirconium hydrides. (Author) 5 refs

Internal friction study of hydrides in zirconium at low hydrogen contents

International Nuclear Information System (INIS)

Peretti, H.A.; Corso, H.L.; Gonzalez, O.A.; Fernandez, L.; Ghilarducci, A.A.; Salva, H.R.

1999-01-01

Full text: Internal friction and shear modulus measurements were carried out on crystal bar zirconium in the as received and hydride conditions using an inverted forced pendulum. Hydriding was achieved in two ways: inside and out of the pendulum. The final hydrogen content determined by fusion analysis in the 'in situ' hydride sample was of 36 ppm. Another sample was hydride by the cathodic charge method with 25 ppm. The thermal solid solubility (TSS) phase boundary presents hysteresis between the precipitation (TSSP) and the dissolution (TSSD) temperatures for the zirconium hydrides. During the first thermal cycling the anelastic effects could be attributed to the δ, ε and metastable γ zirconium hydrides. After 'in situ' annealing at 490 K, these peaks completely disappear in the electrolytically charged sample, while in the 'in situ' hydride, the peaks remain with decreasing intensity. This effect can be understood in terms of the different surface conditions of the samples. (author)

Hidden Hydride Transfer as a Decisive Mechanistic Step in the Reactions of the Unligated Gold Carbide [AuC]+ with Methane under Ambient Conditions.

Science.gov (United States)

Li, Jilai; Zhou, Shaodong; Schlangen, Maria; Weiske, Thomas; Schwarz, Helmut

2016-10-10

The reactivity of the cationic gold carbide [AuC] + (bearing an electrophilic carbon atom) towards methane has been studied using Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS). The product pairs generated, that is, Au + /C 2 H 4 , [Au(C 2 H 2 )] + /H 2 , and [C 2 H 3 ] + /AuH, point to the breaking and making of C-H, C-C, and H-H bonds under single-collision conditions. The mechanisms of these rather efficient reactions have been elucidated by high-level quantum-chemical calculations. As a major result, based on molecular orbital and NBO-based charge analysis, an unprecedented hydride transfer from methane to the carbon atom of [AuC] + has been identified as a key step. Also, the origin of this novel mechanistic scenario has been addressed. The mechanistic insights derived from this study may provide guidance for the rational design of carbon-based catalysts. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An Evaluation of Automated Code Generation with the PetriCode Approach

DEFF Research Database (Denmark)

Simonsen, Kent Inge

2014-01-01

Automated code generation is an important element of model driven development methodologies. We have previously proposed an approach for code generation based on Coloured Petri Net models annotated with textual pragmatics for the network protocol domain. In this paper, we present and evaluate thr...... important properties of our approach: platform independence, code integratability, and code readability. The evaluation shows that our approach can generate code for a wide range of platforms which is integratable and readable....

Validation of Fully Automated VMAT Plan Generation for Library-Based Plan-of-the-Day Cervical Cancer Radiotherapy

OpenAIRE

Sharfo, Abdul Wahab M.; Breedveld, Sebastiaan; Voet, Peter W. J.; Heijkoop, Sabrina T.; Mens, Jan-Willem M.; Hoogeman, Mischa S.; Heijmen, Ben J. M.

2016-01-01

textabstractPurpose: To develop and validate fully automated generation of VMAT plan-libraries for plan-of-the-day adaptive radiotherapy in locally-advanced cervical cancer. Material and Methods: Our framework for fully automated treatment plan generation (Erasmus-iCycle) was adapted to create dual-arc VMAT treatment plan libraries for cervical cancer patients. For each of 34 patients, automatically generated VMAT plans (autoVMAT) were compared to manually generated, clinically delivered 9-be...

Scalable cavity-QED-based scheme of generating entanglement of atoms and of cavity fields

OpenAIRE

Lee, Jaehak; Park, Jiyong; Lee, Sang Min; Lee, Hai-Woong; Khosa, Ashfaq H.

2008-01-01

We propose a cavity-QED-based scheme of generating entanglement between atoms. The scheme is scalable to an arbitrary number of atoms, and can be used to generate a variety of multipartite entangled states such as the Greenberger-Horne-Zeilinger, W, and cluster states. Furthermore, with a role switching of atoms with photons, the scheme can be used to generate entanglement between cavity fields. We also introduce a scheme that can generate an arbitrary multipartite field graph state.

Remote Generation of Entanglement for Individual Atoms via Optical Fibres

International Nuclear Information System (INIS)

Yan-Qing, Guo; Hai-Yang, Zhong; Ying-Hui, Zhang; He-Shan, Song

2008-01-01

The generation of atomic entanglement is discussed in a system that atoms are trapped in separate cavities which are connected via optical fibres. Two distant atoms can be projected to Bell-state by synchronized turning off of the local laser fields and then performing a single quantum measurement by a distant controller. The distinct advantage of this scheme is that it works in a regime where Δ ≈ κ ≫ g, which makes the scheme insensitive to cavity strong leakage. Moreover, the fidelity is not affected by atomic spontaneous emission. (general)

What cost quality assurance

International Nuclear Information System (INIS)

Tikkanen, M.W.; Starek, R.; Liddel, P.R.; Grey, R.G.; Peile, R.C.

1991-01-01

This paper reports that the increased awareness of global environmental pollution has meant that analytical laboratories are faced with an increasing number of samples to analyze and a greater demand for quality control for their applications. In answer to these demands, more laboratory managers are turning to automation for analytical procedures and automated routines to perform quality control on individual samples. Atomic Absorption analysis, particularly by graphite furnace and hydride generation technique has proved to be adaptable to automated analysis to determine low concentrations of elements such as As, Co, Cd, Hg, Ag, Ba, Cr and Pb. Although highly sensitive, both techniques are time consuming and highly matrix dependent. They may also require extensive sample preparation prior to analysis. Additionally, government imposed methodologies e.g. those used for the USA EPA, Contract Laboratory Program, RCRA and SDWA programs, require very specific time consuming quality control measures

The use of metal hydrides in fuel cell applications

Directory of Open Access Journals (Sweden)

Mykhaylo V. Lototskyy

2017-02-01

Full Text Available This paper reviews state-of-the-art developments in hydrogen energy systems which integrate fuel cells with metal hydride-based hydrogen storage. The 187 reference papers included in this review provide an overview of all major publications in the field, as well as recent work by several of the authors of the review. The review contains four parts. The first part gives an overview of the existing types of fuel cells and outlines the potential of using metal hydride stores as a source of hydrogen fuel. The second part of the review considers the suitability and optimisation of different metal hydrides based on their energy efficient thermal integration with fuel cells. The performances of metal hydrides are considered from the viewpoint of the reversible heat driven interaction of the metal hydrides with gaseous H2. Efficiencies of hydrogen and heat exchange in hydrogen stores to control H2 charge/discharge flow rates are the focus of the third section of the review and are considered together with metal hydride – fuel cell system integration issues and the corresponding engineering solutions. Finally, the last section of the review describes specific hydrogen-fuelled systems presented in the available reference data.

Getting metal-hydrides to do what you want them to

International Nuclear Information System (INIS)

Gruen, D.M.

1981-01-01

With the discovery of AB 5 compounds, intermetallic hydrides with unusual properties began to be developed (H dissociation pressures of one to several atmospheres, extremely rapid and reversible adsorption/desorption very large amounts of H adsorbed). This paper reviews the factors that must be controlled in order to modify these hydrides to make them useful. The system LaNi 5 + H 2 is used as example. Use of AB 5 hydrides to construct a chemical heat pumps is discussed. Results of a systematic study substituting Al for Ni are reported; the HYCSOS pump is described briefly. Use of hydrides as hydrogen getters (substituted ZrV 2 ) is also discussed. Finally, possible developments in intermetallic hydride research in the 1980's and the hydrogen economy are discussed. 10 figures

Growth and decomposition of Lithium and Lithium hydride on Nickel

DEFF Research Database (Denmark)

Engbæk, Jakob; Nielsen, Gunver; Nielsen, Jane Hvolbæk

2006-01-01

In this paper we have investigated the deposition, structure and decomposition of lithium and lithium-hydride films on a nickel substrate. Using surface sensitive techniques it was possible to quantify the deposited Li amount, and to optimize the deposition procedure for synthesizing lithium......-hydride films. By only making thin films of LiH it is possible to study the stability of these hydride layers and compare it directly with the stability of pure Li without having any transport phenomena or adsorbed oxygen to obscure the results. The desorption of metallic lithium takes place at a lower...... temperature than the decomposition of the lithium-hydride, confirming the high stability and sintering problems of lithium-hydride making the storage potential a challenge. (c) 2006 Elsevier B.V. All rights reserved....

Structure of the novel ternary hydrides Li4Tt2D (Tt=Si and Ge)

International Nuclear Information System (INIS)

Wu Hui; Rush, J.J.; Maryland Univ., College Park, MD; Hartman, M.R.; Oregon State Univ., Corvallis, OR; Udovic, T.J.; Zhou Wei; Pennsylvania Univ., Philadelphia, PA; Bowman, R.C. Jr.; Vajo, J.J.

2007-01-01

The crystal structures of newly discovered Li 4 Ge 2 D and Li 4 Si 2 D ternary phases were solved by direct methods using neutron powder diffraction data. Both structures can be described using a Cmmm orthorhombic cell with all hydrogen atoms occupying Li 6 -octahedral interstices. The overall crystal structure and the geometry of these interstices are compared with those of other related phases, and the stabilization of this novel class of ternary hydrides is discussed. (orig.)

The influence of hydride on fracture toughness of recrystallized Zircaloy-4 cladding

Energy Technology Data Exchange (ETDEWEB)

Hsu, Hsiao-Hung, E-mail: 175877@mail.csc.com.tw [Institute of Nuclear Energy Research (INER), Lungtan Township, Taoyuan County 32546, Taiwan, ROC (China); China Steel Corporation, Hsiao Kang District, Kaohsiung 81233, Taiwan, ROC (China); Chiang, Ming-Feng [China Steel Corporation, Hsiao Kang District, Kaohsiung 81233, Taiwan, ROC (China); Chen, Yen-Chen [Institute of Nuclear Energy Research (INER), Lungtan Township, Taoyuan County 32546, Taiwan, ROC (China)

2014-04-01

In this work, RXA cladding tubes were hydrogen-charged to target hydrogen content levels between 150 and 800 wppm (part per million by weight). The strings of zirconium hydrides observed in the cross sections are mostly oriented in the circumferential direction. The fracture toughness of hydrided RXA Zircaloy-4 cladding was measured to evaluate its hydride embrittlement susceptibility. With increasing hydrogen content, the fracture toughness of hydrided RXA cladding decreases at both 25 °C and 300 °C. Moreover, highly localized hydrides (forming a hydride rim) aggravate the degradation of the fracture properties of RXA Zircaloy-4 cladding at both 25 °C and 300 °C. Brittle features in the form of quasi-cleavages and secondary cracks were observed on the fracture surface of the hydride rim, even for RXA cladding tested at 300 °C.

Ultra-sonic observation in niobium hydride precipitation

International Nuclear Information System (INIS)

Florencio, O.; Pinatti, Dyonisio G.

1982-01-01

The hidrogen embrittlement of exothermic ocluders, had been considered as due to applied stress induced hydride precipitates leading to brittle fracture. The results of simultaneous measurements of macroscopic deformation and elastic change due to hydride precipitation, using the ultrasonic pulse-echo technique are showed. THen it was tested the possibility of kinectis precipitation parameters evoluation. (Author) [pt

Morphology study on the depleted uranium as hydriding/dehydriding cycles

Energy Technology Data Exchange (ETDEWEB)

Chung, Dong-you, E-mail: dongyou@nfri.re.kr [National Fusion Research Institute, Daejeon (Korea, Republic of); Yun, Sei-Hun; Kang, Hyun-Goo; Chang, Min Ho; Oh, Yun Hee [National Fusion Research Institute, Daejeon (Korea, Republic of); Kang, Kweon Ho; Woo, Yoon Myung [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2016-11-01

Depleted Uranium (DU) is one of the strongest candidates as a getter material of hydrogen isotopes in the nuclear fusion reactor. In this work, small DU lump specimen with 99.8% purity was prepared for observation of morphology variation as hydriding/dehydriding cycles. Hydriding/dehydriding of DU was carried out more than 10 cycles for powder preparation. The pulverized DU specimen was safely handled in the glove box under Argon gas condition to minimize contact with oxygen and humidity. The morphology change according to hydriding/dehydriding cycles was observed by visual cell reactor, optical microscope and scanning electron microscope. The first hydriding of the small DU sample has progressed slowly with surface enlargement and volume expansion as time passes. After third hydriding/dehydriding cycles, most of DU was pulverized. The powder fineness of DU developed as hydriding/dehydriding cycle progresses. But the agglomerates of fine DU particles were observed. It was confirmed that the DU particles exist as porous agglomerates. And the particle agglomerate shows poor fluidity and even has the cohesive force.

Investigation of trapping interference effects of arsenic, antimony and bismuth in collection of selenium hydride within an iridium-modified THGA

Czech Academy of Sciences Publication Activity Database

Hrušovská, Zuzana; Dočekal, Bohumil

2005-01-01

Roč. 99, S (2005), s143-s144 ISSN 0009-2770. [Meeting on Chemistry and Life /3./. Brno, 20.09.2005-22.09.2005] R&D Projects: GA AV ČR IAA400310507 Grant - others:GA FRVŠ(CZ) G6/919/2005 Institutional research plan: CEZ:AV0Z40310501 Keywords : hydride generation * hydride trapping * mutual interference effects Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.445, year: 2005

Automated processing of data generated by molecular dynamics

International Nuclear Information System (INIS)

Lobato Hoyos, Ivan; Rojas Tapia, Justo; Instituto Peruano de Energia Nuclear, Lima

2008-01-01

A new integrated tool for automated processing of data generated by molecular dynamics packages and programs have been developed. The program allows to calculate important quantities such as pair correlation function, the analysis of common neighbors, counting nanoparticles and their size distribution, conversion of output files between different formats. The work explains in detail the modules of the tool, the interface between them. The uses of program are illustrated in application examples in the calculation of various properties of silver nanoparticles. (author)

YNi and its hydrides: Phase stabilities, electronic structures and chemical bonding properties from first principles

Energy Technology Data Exchange (ETDEWEB)

Matar, S.F., E-mail: matar@icmcb-bordeaux.cnrs.fr [CNRS, Universite de Bordeaux, ICMCB, 87 avenue du Docteur Albert Schweitzer, F-33608 Pessac (France); Nakhl, M. [Universite Libanaise, Laboratoire de Chimie-Physique des Materiaux LCPM, Fanar (Lebanon); Al Alam, A.F.; Ouaini, N. [Universite Saint-Esprit de Kaslik, Faculte des Sciences et de Genie Informatique, Jounieh (Lebanon); Chevalier, B. [CNRS, Universite de Bordeaux, ICMCB, 87 avenue du Docteur Albert Schweitzer, F-33608 Pessac (France)

2010-11-25

Graphical abstract: Base centered orthorhombic YNiH{sub X} structure. For x = 3, only H1 and H2 are present. Highest hydrogen content YNiH{sub 4} is obtained when H3 are added. - Abstract: Within density functional theory, establishing the equations of states of YNi in two different controversial structures in the literature, leads to determine the orthorhombic FeB-type as the ground state one with small energy difference. For YNiH{sub 3} and YNiH{sub 4} hydrides crystallizing in the orthorhombic CrB-type structure the geometry optimization and the ab initio determination of the H atomic positions show that the stability of hydrogen decreases from the tri- to the tetra- hydride. New states brought by hydrogen within the valence band lead to its broadening and to enhanced localization of metal density of states. The chemical bonding analysis shows a preferential Ni-H bonding versus Y-H.

Influence of temperature on δ-hydride habit plane in α-Zirconium

International Nuclear Information System (INIS)

Singh, R. N.; Stahle, P.; Banerjee, S.; Ristmanaa, Matti; Sauramd, K.

2008-01-01

Dilute Zr-alloy with hcp α-Zr as major phase is used as pressure boundary for hot coolant in CANDU, PHWR and RBMK reactors. Hydrogen / deuterium ingress during service makes the pressure boundary components like pressure tubes of the aforementioned reactors susceptible to hydride embrittlement. Hydride acquires plate shaped morphology and the broad face of the hydride plate coincides with certain crystallographic plane of α-Zr crystal, which is called habit plane. Hydride plate oriented normal to tensile stress significantly increases the degree of embrittlement. Thus key to mitigating the damage due to hydride embrittlement is to avoid the formation of hydride plates normal to tensile stress. Two different theoretical approaches are used to determine the habit plane of precipitates viz., geometrical and solid mechanics. For the geometrical approach invariant plane and invariant-line criteria have been applied successfully and for the solid mechanics approach strain energy minimization criteria have been used successfully. Solid mechanics approach using strain energy computed by FEM technique has been applied to hydride precipitation in Zr-alloys, but the emphasis has been to understand the solvus hysteresis. The objective of the present investigation is to predict the habit plane of δ-hydride precipitating in α-Zr at 25, 300, 400 and 450 .deg. C. using strain energy minimization technique. The δ-hydride phase is modeled to undergo isotropic elastic and plastic deformation. The α-Zr phase was modeled to undergo transverse isotropic elastic deformation. Both isotropic plastic and transverse isotropic plastic deformations of α-Zr were considered. Further, both perfect and linear work-hardening plastic behaviors were considered. Accommodation strain energy of δ-hydrides forming in α-Zr crystal was computed using initial strain method as a function of hydride nuclei orientation. Hydride was modeled as disk with circular edge. The simulation was carried out

Investigation process of alcoholysis of hydride aluminium-adobe

International Nuclear Information System (INIS)

Numanov, M.I.; Normatov, I.Sh.; Mirsaidov, U.M.

2001-01-01

Considering of that process of acid treatment of aluminium-adobe hydride realizes in the ethyl alcohol media it was necessary study the process of alcoholysis of AlH 3 and aluminium additives. In the end of article authors became to conclusion that deficiency of spontaneous alcoholysis of AlH 3 in adobe caused by protective action of fiber; solvate ability of LiCl and alkoxy aluminium hydride of lithium-LiCl·CO 2 H 5 OH, Li Al(OC 2 H 5 ) 4 ·nC 2 H 5 OH decreasing the expectancy of responding of alcohol with aluminium hydride

A self-regulating hydrogen generator for micro fuel cells

Energy Technology Data Exchange (ETDEWEB)

Moghaddam, Saeed; Pengwang, Eakkachai; Shannon, Mark A. [Mechanical Science and Engineering, University of Illinois at Urbana-Champaign, 1206 West Green Street, Urbana, IL 61801 (United States); Masel, Richard I. [Chemical and Biomolecular Engineering, University of Illinois at Urbana-Champaign, 213 Roger Adams Lab, 600 S. Mathews, Urbana, IL 61801 (United States)

2008-10-15

The ever-increasing power demands and miniaturization of portable electronics, micro-sensors and actuators, and emerging technologies such as cognitive arthropods have created a significant interest in development of micro fuel cells. One of the major challenges in development of hydrogen micro fuel cells is the fabrication and integration of auxiliary systems for generating, regulating, and delivering hydrogen gas to the membrane electrode assembly (MEA). In this paper, we report the development of a hydrogen gas generator with a micro-scale control system that does not consume any power. The hydrogen generator consists of a hydride reactor and a water reservoir, with a regulating valve separating them. The regulating valve consists of a port from the water reservoir and a movable membrane with via holes that permit water to flow from the reservoir to the hydride reactor. Water flows towards the hydride reactor, but stops within the membrane via holes due to capillary forces. Water vapor then diffuses from the via holes into the hydride reactor resulting in generation of hydrogen gas. When the rate of hydrogen consumed by the MEA is lower than the generation rate, gas pressure builds up inside the hydride reactor, deflecting the membrane, closing the water regulator valve, until the pressure drops, whereby the valve reopens. We have integrated the self-regulating micro hydrogen generator to a MEA and successfully conducted fuel cell tests under varying load conditions. (author)

Hydrogen desorption kinetics from zirconium hydride and zirconium metal in vacuum

International Nuclear Information System (INIS)

Hu, Xunxiang; Terrani, Kurt A.; Wirth, Brian D.

2014-01-01

The kinetics of hydrogen desorption from zirconium hydride is important in many nuclear design and safety applications. In this paper, a coordinated experimental and modeling study has been used to explicitly demonstrate the applicability of existing kinetic theories for hydrogen desorption from zirconium hydride and α-zirconium. A static synthesis method was used to produce δ-zirconium hydride, and the crystallographic phases of the zirconium hydride were confirmed by X-ray diffraction (XRD). Three obvious stages, involving δ-zirconium hydride, a two-phase region, and α-zirconium, were observed in the hydrogen desorption spectra of two zirconium hydride specimens with H/Zr ratios of 1.62 and 1.64, respectively, which were obtained using thermal desorption spectroscopy (TDS). A continuous, one-dimensional, two-phase moving boundary model, coupled with the zero- and second-order kinetics of hydrogen desorption from δ-zirconium hydride and α-zirconium, respectively, has been developed to reproduce the TDS experimental results. A comparison of the modeling predictions with the experimental results indicates that a zero-order kinetic model is valid for description of hydrogen flux away from the δ-hydride phase, and that a second-order kinetic model works well for hydrogen desorption from α-Zr if the activation energy of desorption is optimized to be 70% of the value reported in the literature

Observations on Hydride Structures at the Tip of Arrested Cracks Grown under Conditions of Delayed Hydride Cracking

International Nuclear Information System (INIS)

Pettersson, Kjell; Oskarsson, Magnus; Bergqvist, Hans

2003-04-01

One sample of Zr2.5%Nb and one sample of cold worked and stress relieved Zircaloy-4 which have been tested for hydrogen induced crack growth have been examined in the crack tip region with the aim of determining the mechanism behind the growth of cracks. The proposed mechanisms are brittle failure of a crack tip hydride and hydrogen enhanced localized shear. The examinations were done by TEM and SEM. However attempts to produce a TEM specimen with a thinned region at the tip of the crack were unsuccessful in both samples. One feature observed in the Zr2.5%Nb material may however be an indication of intense shear deformation at the tip of the crack. On the other hand all observations on the Zircaloy-4 sample indicate precipitation of hydrides ahead of the crack tip and the presence of hydrides on the crack flanks

Hydrogen and dihydrogen bonding of transition metal hydrides

Science.gov (United States)

Jacobsen, Heiko

2008-04-01

Intermolecular interactions between a prototypical transition metal hydride WH(CO) 2NO(PH 3) 2 and a small proton donor H 2O have been studied using DFT methodology. The hydride, nitrosyl and carbonyl ligand have been considered as site of protonation. Further, DFT-D calculations in which empirical corrections for the dispersion energy are included, have been carried out. A variety of pure and hybrid density functionals (BP86, PW91, PBE, BLYP, OLYP, B3LYP, B1PW91, PBE0, X3LYP) have been considered, and our calculations indicate the PBE functional and its hybrid variation are well suited for the calculation of transition metal hydride hydrogen and dihydrogen bonding. Dispersive interactions make up for a sizeable portion of the intermolecular interaction, and amount to 20-30% of the bond energy and to 30-40% of the bond enthalpy. An energy decomposition analysis reveals that the H⋯H bond of transition metal hydrides contains both covalent and electrostatic contributions.

Hydrogen and dihydrogen bonding of transition metal hydrides

International Nuclear Information System (INIS)

Jacobsen, Heiko

2008-01-01

Intermolecular interactions between a prototypical transition metal hydride WH(CO) 2 NO(PH 3 ) 2 and a small proton donor H 2 O have been studied using DFT methodology. The hydride, nitrosyl and carbonyl ligand have been considered as site of protonation. Further, DFT-D calculations in which empirical corrections for the dispersion energy are included, have been carried out. A variety of pure and hybrid density functionals (BP86, PW91, PBE, BLYP, OLYP, B3LYP, B1PW91, PBE0, X3LYP) have been considered, and our calculations indicate the PBE functional and its hybrid variation are well suited for the calculation of transition metal hydride hydrogen and dihydrogen bonding. Dispersive interactions make up for a sizeable portion of the intermolecular interaction, and amount to 20-30% of the bond energy and to 30-40% of the bond enthalpy. An energy decomposition analysis reveals that the H...H bond of transition metal hydrides contains both covalent and electrostatic contributions

Fluorescence In Situ Hybridization (FISH Signal Analysis Using Automated Generated Projection Images

Directory of Open Access Journals (Sweden)

Xingwei Wang

2012-01-01

Full Text Available Fluorescence in situ hybridization (FISH tests provide promising molecular imaging biomarkers to more accurately and reliably detect and diagnose cancers and genetic disorders. Since current manual FISH signal analysis is low-efficient and inconsistent, which limits its clinical utility, developing automated FISH image scanning systems and computer-aided detection (CAD schemes has been attracting research interests. To acquire high-resolution FISH images in a multi-spectral scanning mode, a huge amount of image data with the stack of the multiple three-dimensional (3-D image slices is generated from a single specimen. Automated preprocessing these scanned images to eliminate the non-useful and redundant data is important to make the automated FISH tests acceptable in clinical applications. In this study, a dual-detector fluorescence image scanning system was applied to scan four specimen slides with FISH-probed chromosome X. A CAD scheme was developed to detect analyzable interphase cells and map the multiple imaging slices recorded FISH-probed signals into the 2-D projection images. CAD scheme was then applied to each projection image to detect analyzable interphase cells using an adaptive multiple-threshold algorithm, identify FISH-probed signals using a top-hat transform, and compute the ratios between the normal and abnormal cells. To assess CAD performance, the FISH-probed signals were also independently visually detected by an observer. The Kappa coefficients for agreement between CAD and observer ranged from 0.69 to 1.0 in detecting/counting FISH signal spots in four testing samples. The study demonstrated the feasibility of automated FISH signal analysis that applying a CAD scheme to the automated generated 2-D projection images.

In situ Generated Ruthenium Catalyst Systems Bearing Diverse N-Heterocyclic Carbene Precursors for Atom-Economic Amide Synthesis from Alcohols and Amines.

Science.gov (United States)

Cheng, Hua; Xiong, Mao-Qian; Cheng, Chuan-Xiang; Wang, Hua-Jing; Lu, Qiang; Liu, Hong-Fu; Yao, Fu-Bin; Chen, Cheng; Verpoort, Francis

2018-02-16

The transition-metal-catalyzed direct synthesis of amides from alcohols and amines is herein demonstrated as a highly environmentally benign and atom-economic process. Among various catalyst systems, in situ generated N-heterocyclic carbene (NHC)-based ruthenium (Ru) halide catalyst systems have been proven to be active for this transformation. However, these existing catalyst systems usually require an additional ligand to achieve satisfactory results. In this work, through extensive screening of a diverse variety of NHC precursors, we discovered an active in situ catalyst system for efficient amide synthesis without any additional ligand. Notably, this catalyst system was found to be insensitive to the electronic effects of the substrates, and various electron-deficient substrates, which were not highly reactive with our previous catalyst systems, could be employed to afford the corresponding amides efficiently. Furthermore, mechanistic investigations were performed to provide a rationale for the high activity of the optimized catalyst system. NMR-scale reactions indicated that the rapid formation of a Ru hydride intermediate (signal at δ=-7.8 ppm in the 1 H NMR spectrum) after the addition of the alcohol substrate should be pivotal in establishing the high catalyst activity. Besides, HRMS analysis provided possible structures of the in situ generated catalyst system. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

Fishman, M.

1977-01-01

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

Regenerative Hydride Heat Pump

Science.gov (United States)

Jones, Jack A.

1992-01-01

Hydride heat pump features regenerative heating and single circulation loop. Counterflow heat exchangers accommodate different temperatures of FeTi and LaNi4.7Al0.3 subloops. Heating scheme increases efficiency.

Developments in delayed hydride cracking in zirconium alloys

International Nuclear Information System (INIS)

Puls, Manfred P.

2008-01-01

Delayed hydride cracking (DHC) is a process of diffusion assisted localized hydride embrittlement at flaws or regions of high stress. Models of DHC propagation and initiation have been developed that capture the essential elements of this phenomenon in terms of parameters describing processes occurring at the micro-scale. The models and their predictions of experimental results applied to Zr alloys are assessed. The propagation model allows rationalization of the effect of direction of approach to temperature and of the effect of the state and morphology of the beta phase in Zr-2.5Nb on DHC velocity. The K I dependence of the DHC velocity can only be approximately rationalized by the propagation models. This is thought to be because these models approximate the DHC velocity by a constant and shape-invariant rate of growth of the hydride at the flaw and have not incorporated a coupling between the applied stress field due to the flaw alone and the precipitated hydrides that would result in a variation of the shape and density of the hydrided region with K I . Separately, models have been developed for DHC initiation at cracks and blunt flaws. Expressions are obtained for the threshold stress intensity factor, K IH , for DHC initiation at a crack. A model for K IH has been used to rationalize the experimental result that DHC initiation is not possible above a certain temperature, even when hydrides can form at the crack tip. For blunt flaws with root radii in the μm range, and engineering process zone procedure has been derived to determine the initiation conditions requiring that both a critical stress and a critical flaw tip displacement must be achieved for hydride fracture. The engineering process zone procedure takes account of the dependence of DHC initiation on the flaw's root radius. Although all of the foregoing models are capable of describing the essential features of DHC, they are highly idealized and in need of further refinement. (author)

HYDRIDE-RELATED DEGRADATION OF SNF CLADDING UNDER REPOSITORY CONDITIONS

International Nuclear Information System (INIS)

McCoy, K.

2000-01-01

The purpose and scope of this analysis/model report is to analyze the degradation of commercial spent nuclear fuel (CSNF) cladding under repository conditions by the hydride-related metallurgical processes, such as delayed hydride cracking (DHC), hydride reorientation and hydrogen embrittlement, thereby providing a better understanding of the degradation process and clarifying which aspects of the process are known and which need further evaluation and investigation. The intended use is as an input to a more general analysis of cladding degradation

Hydrogen isotope exchange in metal hydride columns

International Nuclear Information System (INIS)

Wiswall, R.; Reilly, J.; Bloch, F.; Wirsing, E.

1977-01-01

Several metal hydrides were shown to act as chromatographic media for hydrogen isotopes. The procedure was to equilibrate a column of hydride with flowing hydrogen, inject a small quantity of tritium tracer, and observe its elution behavior. Characteristic retention times were found. From these and the extent of widening of the tritium band, the heights equivalent to a theoretical plate could be calculated. Values of around 1 cm were obtained. The following are the metals whose hydrides were studied, together with the temperature ranges in which chromatographic behavior was observed: vanadium, 0 to 70 0 C; zirconium, 500 to 600 0 C; LaNi 5 , -78 to +30 0 C; Mg 2 Ni, 300 to 375 0 C; palladium, 0 to 70 0 C. A dual-temperature isotope separation process based on hydride chromatography was demonstrated. In this, a column was caused to cycle between two temperatures while being supplied with a constant stream of tritium-traced hydrogen. Each half-cycle was continued until ''breakthrough,'' i.e., until the tritium concentration in the effluent was the same as that in the feed. Up to that point, the effluent was enriched or depleted in tritium, by up to 20%

M073: Monte Carlo generated spectra for QA/QC of automated NAA routine

International Nuclear Information System (INIS)

Jackman, K.R.; Biegalski, S.R.

2004-01-01

A quality check for an automated system of analyzing large sets of neutron activated samples has been developed. Activated samples are counted with an HPGe detector, in conjunction with an automated sample changer and spectral analysis tools, controlled by the Canberra GENIE 2K and REXX software. After each sample is acquired and analyzed, a Microsoft Visual Basic program imports the results into a template Microsoft Excel file where the final concentrations, uncertainties, and detection limits are determined. Standard reference materials are included in each set of 40 samples as a standard quality assurance/quality control (QA/QC) test. A select group of sample spectra are also visually reviewed to check the peak fitting routines. A reference spectrum was generated in MCNP 4c2 using an F8, pulse height, tally with a detector model of the actual detector used in counting. The detector model matches the detector resolution, energy calibration, and counting geometry. The generated spectrum also contained a radioisotope matrix that was similar to what was expected in the samples. This spectrum can then be put through the automated system and analyzed along with the other samples. The automated results are then compared to expected results for QA/QC assurance.

Spectrophotometric determination of volautile inorganic hydrides in binary gaseous mixtures

International Nuclear Information System (INIS)

Rezchikov, V.G.; Skachkova, I.N.; Kuznetsova, T.S.; Khrushcheva, V.V.

1985-01-01

A study was made on possibility of single and continuons analysis of binary mixtures (hydride-gas) for the content of volatile inorganic hydrides (VIH) from absorption spectra in the 185-280 nm band. Dependences of the percentage of VIH transmission on the wavelength are presented. It is shown that the maximum of their absorption depends on the element-hydrogen the bond length and binding energy. Detection limit for boron hydride was established to be n x 10 -3 % vol at 185-190 nm wavelength. Technique for spectrophotometric hydride determination in binary mixtures with hydrogen, argon, helium was developed. The technique provides the continuous control of gaseous mixture composition

Pyrophoric behaviour of uranium hydride and uranium powders

Science.gov (United States)

Le Guyadec, F.; Génin, X.; Bayle, J. P.; Dugne, O.; Duhart-Barone, A.; Ablitzer, C.

2010-01-01

Thermal stability and spontaneous ignition conditions of uranium hydride and uranium metal fine powders have been studied and observed in an original and dedicated experimental device placed inside a glove box under flowing pure argon. Pure uranium hydride powder with low amount of oxide (Oxidation mechanisms are proposed.

Hydride Transfer versus Deprotonation Kinetics in the Isobutane–Propene Alkylation Reaction: A Computational Study

Science.gov (United States)

2017-01-01

The alkylation of isobutane with light alkenes plays an essential role in modern petrochemical processes for the production of high-octane gasoline. In this study we have employed periodic DFT calculations combined with microkinetic simulations to investigate the complex reaction mechanism of isobutane–propene alkylation catalyzed by zeolitic solid acids. Particular emphasis was given to addressing the selectivity of the alkylate formation versus alkene formation, which requires a high rate of hydride transfer in comparison to the competitive oligomerization and deprotonation reactions resulting in catalyst deactivation. Our calculations reveal that hydride transfer from isobutane to a carbenium ion occurs via a concerted C–C bond formation between a tert-butyl fragment and an additional olefin, or via deprotonation of the tert-butyl fragment to generate isobutene. A combination of high isobutane concentration and low propene concentration at the reaction center favor the selective alkylation. The key reaction step that has to be suppressed to increase the catalyst lifetime is the deprotonation of carbenium intermediates that are part of the hydride transfer reaction cycle. PMID:29226012

Hydride Transfer versus Deprotonation Kinetics in the Isobutane-Propene Alkylation Reaction: A Computational Study.

Science.gov (United States)

Liu, Chong; van Santen, Rutger A; Poursaeidesfahani, Ali; Vlugt, Thijs J H; Pidko, Evgeny A; Hensen, Emiel J M

2017-12-01

The alkylation of isobutane with light alkenes plays an essential role in modern petrochemical processes for the production of high-octane gasoline. In this study we have employed periodic DFT calculations combined with microkinetic simulations to investigate the complex reaction mechanism of isobutane-propene alkylation catalyzed by zeolitic solid acids. Particular emphasis was given to addressing the selectivity of the alkylate formation versus alkene formation, which requires a high rate of hydride transfer in comparison to the competitive oligomerization and deprotonation reactions resulting in catalyst deactivation. Our calculations reveal that hydride transfer from isobutane to a carbenium ion occurs via a concerted C-C bond formation between a tert -butyl fragment and an additional olefin, or via deprotonation of the tert -butyl fragment to generate isobutene. A combination of high isobutane concentration and low propene concentration at the reaction center favor the selective alkylation. The key reaction step that has to be suppressed to increase the catalyst lifetime is the deprotonation of carbenium intermediates that are part of the hydride transfer reaction cycle.

Synthesis of Nano-Light Magnesium Hydride for Hydrogen Storage ...

African Journals Online (AJOL)

Abstract. Nano-light magnesium hydride that has the capability for hydrogen storage was synthesized from treatment of magnesium ribbon with hydrogen peroxide. The optimum time for complete hydrogenation of the magnesium hydride was 5 hours.

Optimizing Decision Preparedness by Adapting Scenario Complexity and Automating Scenario Generation

Science.gov (United States)

Dunne, Rob; Schatz, Sae; Flore, Stephen M.; Nicholson, Denise

2011-01-01

Klein's recognition-primed decision (RPD) framework proposes that experts make decisions by recognizing similarities between current decision situations and previous decision experiences. Unfortunately, military personnel arQ often presented with situations that they have not experienced before. Scenario-based training (S8T) can help mitigate this gap. However, SBT remains a challenging and inefficient training approach. To address these limitations, the authors present an innovative formulation of scenario complexity that contributes to the larger research goal of developing an automated scenario generation system. This system will enable trainees to effectively advance through a variety of increasingly complex decision situations and experiences. By adapting scenario complexities and automating generation, trainees will be provided with a greater variety of appropriately calibrated training events, thus broadening their repositories of experience. Preliminary results from empirical testing (N=24) of the proof-of-concept formula are presented, and future avenues of scenario complexity research are also discussed.

Stress induced reorientation of vanadium hydride

International Nuclear Information System (INIS)

Beardsley, M.B.

1977-10-01

The critical stress for the reorientation of vanadium hydride was determined for the temperature range 180 0 to 280 0 K using flat tensile samples containing 50 to 500 ppM hydrogen by weight. The critical stress was observed to vary from a half to a third of the macroscopic yield stress of pure vanadium over the temperature range. The vanadium hydride could not be stress induced to precipitate above its stress-free precipitation temperature by uniaxial tensile stresses or triaxial tensile stresses induced by a notch

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

International Nuclear Information System (INIS)

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

1977-01-01

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

Low-Cost Metal Hydride Thermal Energy Storage System for Concentrating Solar Power Systems

Energy Technology Data Exchange (ETDEWEB)

Zidan, Ragaiy [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Hardy, B. J. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Corgnale, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Teprovich, J. A. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Ward, P. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Motyka, Ted [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

2016-01-31

The objective of this research was to evaluate and demonstrate a metal hydride-based TES system for use with a CSP system. A unique approach has been applied to this project that combines our modeling experience with the extensive material knowledge and expertise at both SRNL and Curtin University (CU). Because of their high energy capacity and reasonable kinetics many metal hydride systems can be charged rapidly. Metal hydrides for vehicle applications have demonstrated charging rates in minutes and tens of minutes as opposed to hours. This coupled with high heat of reaction allows metal hydride TES systems to produce very high thermal power rates (approx. 1kW per 6-8 kg of material). A major objective of this work is to evaluate some of the new metal hydride materials that have recently become available. A problem with metal hydride TES systems in the past has been selecting a suitable high capacity low temperature metal hydride material to pair with the high temperature material. A unique aspect of metal hydride TES systems is that many of these systems can be located on or near dish/engine collectors due to their high thermal capacity and small size. The primary objective of this work is to develop a high enthalpy metal hydride that is capable of reversibly storing hydrogen at high temperatures (> 650 °C) and that can be paired with a suitable low enthalpy metal hydride with low cost materials. Furthermore, a demonstration of hydrogen cycling between the two hydride beds is desired.

Hydride precipitation crack propagation in zircaloy cladding during a decreasing temperature history

International Nuclear Information System (INIS)

Stout, R.B.

2001-01-01

An assessment of safety, design, and cost tradeoff issues for short (ten to fifty years) and longer (fifty to hundreds of years) interim dry storage of spent nuclear fuel in Zircaloy rods shall address potential failures of the Zircaloy cladding caused by the precipitation response of zirconium hydride platelets. To perform such assessment analyses rigorously and conservatively will be necessarily complex and difficult. For Zircaloy cladding, a model for zirconium hydride induced crack propagation velocity was developed for a decreasing temperature field and for hydrogen, temperature, and stress dependent diffusive transport of hydrogen to a generic hydride platelet at a crack tip. The development of the quasi-steady model is based on extensions of existing models for hydride precipitation kinetics for an isolated hydride platelet at a crack tip. An instability analysis model of hydride-crack growth was developed using existing concepts in a kinematic equation for crack propagation at a constant thermodynamic crack potential subject to brittle fracture conditions. At the time an instability is initiated, the crack propagation is no longer limited by hydride growth rate kinetics, but is then limited by stress rates. The model for slow hydride-crack growth will be further evaluated using existing available data. (authors)

Hydride precipitation crack propagation in zircaloy cladding during a decreasing temperature history

Energy Technology Data Exchange (ETDEWEB)

Stout, R.B. [California Univ., Livermore, CA (United States). Lawrence Livermore National Lab

2001-07-01

An assessment of safety, design, and cost tradeoff issues for short (ten to fifty years) and longer (fifty to hundreds of years) interim dry storage of spent nuclear fuel in Zircaloy rods shall address potential failures of the Zircaloy cladding caused by the precipitation response of zirconium hydride platelets. To perform such assessment analyses rigorously and conservatively will be necessarily complex and difficult. For Zircaloy cladding, a model for zirconium hydride induced crack propagation velocity was developed for a decreasing temperature field and for hydrogen, temperature, and stress dependent diffusive transport of hydrogen to a generic hydride platelet at a crack tip. The development of the quasi-steady model is based on extensions of existing models for hydride precipitation kinetics for an isolated hydride platelet at a crack tip. An instability analysis model of hydride-crack growth was developed using existing concepts in a kinematic equation for crack propagation at a constant thermodynamic crack potential subject to brittle fracture conditions. At the time an instability is initiated, the crack propagation is no longer limited by hydride growth rate kinetics, but is then limited by stress rates. The model for slow hydride-crack growth will be further evaluated using existing available data. (authors)

Precipitation of hydrides in high purity niobium after different treatments

Energy Technology Data Exchange (ETDEWEB)

Barkov, F.; Romanenko, A.; Trenikhina, Y.; Grassellino, A.

2013-01-01

Precipitation of lossy non-superconducting niobium hydrides represents a known problem for high purity niobium in superconducting applications. Using cryogenic optical and laser confocal scanning microscopy we have directly observed surface precipitation and evolution of niobium hydrides in samples after different treatments used for superconducting RF cavities for particle acceleration. Precipitation is shown to occur throughout the sample volume, and the growth of hydrides is well described by the fast diffusion-controlled process in which almost all hydrogen is precipitated at $T=140$~K within $\\sim30$~min. 120$^{\\circ}$C baking and mechanical deformation are found to affect hydride precipitation through their influence on the number of nucleation and trapping centers.

Analytical and numerical models of uranium ignition assisted by hydride formation

International Nuclear Information System (INIS)

Totemeier, T.C.; Hayes, S.L.

1996-01-01

Analytical and numerical models of uranium ignition assisted by the oxidation of uranium hydride are described. The models were developed to demonstrate that ignition of large uranium ingots could not occur as a result of possible hydride formation during storage. The thermodynamics-based analytical model predicted an overall 17 C temperature rise of the ingot due to hydride oxidation upon opening of the storage can in air. The numerical model predicted locally higher temperature increases at the surface; the transient temperature increase quickly dissipated. The numerical model was further used to determine conditions for which hydride oxidation does lead to ignition of uranium metal. Room temperature ignition only occurs for high hydride fractions in the nominally oxide reaction product and high specific surface areas of the uranium metal

Evaluation of hydride blisters in zirconium pressure tube in CANDU reactor

International Nuclear Information System (INIS)

Cheong, Y. M.; Kim, Y. S.; Gong, U. S.; Kwon, S. C.; Kim, S. S.; Choo, K.N.

2000-09-01

When the garter springs for maintaining the gap between the pressure tube and the calandria tube are displaced in the CANDU reactor, the sagging of pressure tube results in a contact to the calandria tube. This causes a temperature difference between the inner and outer surface of the pressure tube. The hydride can be formed at the cold spot of outer surface and the volume expansion by hydride dormation causes the blistering in the zirconium alloys. An incident of pressure tube rupture due to the hydride blisters had happened in the Canadian CANDU reactor. This report describes the theoretical development and models on the formation and growth of hydride blister and some experimental results. The evaluation methodology and non-destructive testing for hydride blister in operating reactors are also described

Evaluation of hydride blisters in zirconium pressure tube in CANDU reactor

Energy Technology Data Exchange (ETDEWEB)

Cheong, Y M; Kim, Y S; Gong, U S; Kwon, S C; Kim, S S; Choo, K N

2000-09-01

When the garter springs for maintaining the gap between the pressure tube and the calandria tube are displaced in the CANDU reactor, the sagging of pressure tube results in a contact to the calandria tube. This causes a temperature difference between the inner and outer surface of the pressure tube. The hydride can be formed at the cold spot of outer surface and the volume expansion by hydride dormation causes the blistering in the zirconium alloys. An incident of pressure tube rupture due to the hydride blisters had happened in the Canadian CANDU reactor. This report describes the theoretical development and models on the formation and growth of hydride blister and some experimental results. The evaluation methodology and non-destructive testing for hydride blister in operating reactors are also described.

Zr - based alloys as hydride electrodes in Ni-MH batteries

International Nuclear Information System (INIS)

Biris, A.R.; Biris, A.S.; Misan, I.; Lupu, D.

1999-01-01

Hydrogen storage alloys, MH, are already used in Ni-MH alkaline batteries conquering an important share of the rechargeable nickel-cadmium battery market. This remarkable success is due not only to the replacement of the toxic material, cadmium, by metal hydrides but also to an increased specific energy, which makes them attractive for electric vehicles. Many research groups are concerned in the improvement of the hydride electrode characteristics: hydrogen storage capacity, high-rate discharge ability, increased cycle life. These properties can be modified by substitution of the base components of a given alloy. A comparison of two types of alloys suitable for MH electrodes LaNi 5 able to store 1.36 w/o hydrogen with Zr(Ti)-Ni alloys of the AB 2 Laves phase type structure showed that the latter could absorb higher amounts of hydrogen. We report part of studies on Zr-V-Cr-Ni of the 15 C type Laves phase structure using our original procedure for pasted electrodes. The substitution of Cr for V atoms in ZrV 0.5 Ni 1 . 5 did not increase the discharge capacity. However, it proved to have a remarkable effect on the discharge capacity C at low temperatures. C at - 12 deg. C as compared to 20 deg.C increases up to ∼ 65 % for Cr containing alloys. (authors)

On the performance of atomic natural orbital basis sets: A full configuration interaction study

International Nuclear Information System (INIS)

Illas, F.; Ricart, J.M.; Rubio, J.; Bagus, P.S.

1990-01-01

The performance of atomic natural orbital (ANO) basis sets has been studied by comparing self-consistant field (SCF) and full configuration interaction (CI) results obtained for the first row atoms and hydrides. The ANO results have been compared with those obtained using a segmented basis set containing the same number of contracted basis functions. The total energies obtained with the ANO basis sets are always lower than the one obtained by using the segmented one. However, for the hydrides, differential electronic correlation energy obtained with the ANO basis set may be smaller than the one recovered with the segmented set. We relate this poorer differential correlation energy for the ANO basis set to the fact that only one contracted d function is used for the ANO and segmented basis sets

Evaluation of delayed hydride cracking and fracture toughness in zirconium alloys

International Nuclear Information System (INIS)

Oh, Je Yong

2000-02-01

The tensile, fracture toughness, and delayed hydride cracking (DHC) test were carried at various temperatures to understand the effect of hydrides on zirconium alloys. And the effects of yield stress and texture on the DHC velocity were discussed. The tensile properties of alloy A were the highest, and the difference between directions in alloy C was small due to texture. The fracture toughness at room temperature decreased sharply when hydrided. Although the alignment of hydride plates was parallel to loading direction, the hydrides were fractured due to the triaxiality at the crack tip region. The fracture toughness over 200 .deg. C was similar regardless of the hydride existence, because the triaxiality region was lost due to the decrease of yield stress with temperature. As the yield stress decreased, the threshold stress intensity factor and the striation spacing increased in alloy A, and the fracture surfaces and striations were affected by microstructures in all alloys. To evaluate the effect of the yield stress on DHC velocity, a normalization method was proposed. When the DHC velocity was normalized with dividing by the terminal solid solubility and the diffusion coefficient of hydrogen, the relationship between the yield stress and the DHC velocity was representable on one master curve. The equation from the master curve was able to explain the difference between the theoretical activation energy and the experimental activation energy in DHC. The difference was found to be ascribed to the decrease of yield stress with temperature. texture affected the delayed hydride cracking velocity by yield stress and by hydride reprecipitation. The relationship between the yield stress and the DHC velocity was expressed as an exponential function, and the relationship between the reprecipitation of hydride and the DHC velocity was expressed as a linear function

Analysis of strain field around. beta. -hydride in Nb-H by Electron Channeling

Energy Technology Data Exchange (ETDEWEB)

Akune, K; Bulhoes, I A.M.

1985-06-01

The strain field in Nb-H system generated by the precipitation of ..beta..-hydride has been evaluated quantitatively by Electron Channeling experiment. The results were analyzed in terms of the effective deformation of the Levi-Mises solid by making use of an elasto-plastic model of the strain field around the misfitting cylindrical precipitate.

Simulating spontaneously generated coherence in a four-level atomic system

International Nuclear Information System (INIS)

Li Aijun; Gao Jinyue; Wu Jinhui; Wang Lei

2005-01-01

We study the spontaneous emission property of a four-level atomic system driven by two coherent fields. By numerical calculations in the bare state picture, we show that such interesting phenomena as extremely narrow peaks and spontaneous emission quenching can be realized, which are well understood by qualitative explanations in the partially and fully dressed state pictures. Especially, this coherently driven atomic system has two close-lying levels in the partially dressed state picture so that spontaneously generated coherence arises. Using our considered scheme it is feasible to carry out experiments based on spontaneously generated coherence because all rigorous requirements have been avoided in the bare state picture

Hydrogen and dihydrogen bonding of transition metal hydrides

Energy Technology Data Exchange (ETDEWEB)

Jacobsen, Heiko [KemKom, Libellenweg 2, 25917 Leck, Nordfriesland (Germany)], E-mail: jacobsen@kemkom.com

2008-04-03

Intermolecular interactions between a prototypical transition metal hydride WH(CO){sub 2}NO(PH{sub 3}){sub 2} and a small proton donor H{sub 2}O have been studied using DFT methodology. The hydride, nitrosyl and carbonyl ligand have been considered as site of protonation. Further, DFT-D calculations in which empirical corrections for the dispersion energy are included, have been carried out. A variety of pure and hybrid density functionals (BP86, PW91, PBE, BLYP, OLYP, B3LYP, B1PW91, PBE0, X3LYP) have been considered, and our calculations indicate the PBE functional and its hybrid variation are well suited for the calculation of transition metal hydride hydrogen and dihydrogen bonding. Dispersive interactions make up for a sizeable portion of the intermolecular interaction, and amount to 20-30% of the bond energy and to 30-40% of the bond enthalpy. An energy decomposition analysis reveals that the H...H bond of transition metal hydrides contains both covalent and electrostatic contributions.

Synthesis, properties, and assimilation methods of aluminium hydride

International Nuclear Information System (INIS)

Mirsaidov, U.M.

2013-01-01

We have discovered a new source of aluminium hydride-conversion of tetrahydrofurane under influence of halogenous alkyls. We have proposed the chlorbenzene method of synthesis of AlH 3 , which excludes adhesion and ensure high quality of the product with respect to its purity, thermal stability, habits of crystals (round shape), and granulometric composition. We determined capability of benzyl chloride to fix AlH 4 -groups by the way of complexes formation. This allows increasing efficient concentration of AlH 3 solutions and their productivity. We have carried out 'direct' crystallization of aluminium hydride in one stage using interaction of binary metal hydride with aluminium chloride in the medium of ether-toluene at 60-100 d ig C a nd using solvent distillation. In the reaction of Li H with AlCl 3 , we achieved output of pure crystal AlH 3 of hexagonal modification, which was close to quantitative. We have discovered the assimilation methods of aluminium hydride in carrying out of solid-phase chemical reactions. (author)

Quantifying the stress fields due to a delta-hydride precipitate in alpha-Zr matrix

Energy Technology Data Exchange (ETDEWEB)

Tummala, Hareesh [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Capolungo, Laurent [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Tome, Carlos N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2017-10-19

This report is a preliminary study on δ-hydride precipitate in zirconium alloy performed using 3D discrete dislocation dynamics simulations. The ability of dislocations in modifying the largely anisotropic stress fields developed by the hydride particle in a matrix phase is addressed for a specific dimension of the hydride. The influential role of probable dislocation nucleation at the hydride-matrix interface is reported. Dislocation nucleation around a hydride was found to decrease the shear stress (S₁₃) and also increase the normal stresses inside the hydride. We derive conclusions on the formation of stacks of hydrides in zirconium alloys. The contribution of mechanical fields due to dislocations was found to have a non-negligible effect on such process.

Effect of electronegativity on the mechanical properties of metal hydrides with a fluorite structure

International Nuclear Information System (INIS)

Ito, Masato; Setoyama, Daigo; Matsunaga, Junji; Muta, Hiroaki; Kurosaki, Ken; Uno, Masayoshi; Yamanaka, Shinsuke

2006-01-01

Bulk titanium, yttrium, and zirconium hydrides, which have the same structure as that of fluorite-type fcc C 1, were produced and their mechanical properties were investigated. With an increase in the hydrogen content, the lattice parameters of titanium and zirconium hydrides increased, whereas those of yttrium hydride decreased. The elastic moduli of titanium and zirconium hydrides decreased by hydrogen addition, whereas those of yttrium hydride increased. There are linear relations between the electronegativities and hydrogen content dependence of the properties. Therefore, the mechanical properties of the metal hydrides are considered to be determined by a common rule based on the electronegativity

Analysis of strain field around β-hydride in Nb-H by electron channeling

International Nuclear Information System (INIS)

Akune, K.; Bulhoes, I.A.M.

1985-01-01

The strain field in Nb-H system generated by the precipitation of β-hydride has been evaluated quantitatively by Electron Channelling experiment. The results were analyzed in terms of the effective deformation of the Levi-Mises solid by making use of an elasto-plastic model of the strain fiedl around the misfitting cylindrical precipitate. (Author) [pt

Automated Item Generation with Recurrent Neural Networks.

Science.gov (United States)

von Davier, Matthias

2018-03-12

Utilizing technology for automated item generation is not a new idea. However, test items used in commercial testing programs or in research are still predominantly written by humans, in most cases by content experts or professional item writers. Human experts are a limited resource and testing agencies incur high costs in the process of continuous renewal of item banks to sustain testing programs. Using algorithms instead holds the promise of providing unlimited resources for this crucial part of assessment development. The approach presented here deviates in several ways from previous attempts to solve this problem. In the past, automatic item generation relied either on generating clones of narrowly defined item types such as those found in language free intelligence tests (e.g., Raven's progressive matrices) or on an extensive analysis of task components and derivation of schemata to produce items with pre-specified variability that are hoped to have predictable levels of difficulty. It is somewhat unlikely that researchers utilizing these previous approaches would look at the proposed approach with favor; however, recent applications of machine learning show success in solving tasks that seemed impossible for machines not too long ago. The proposed approach uses deep learning to implement probabilistic language models, not unlike what Google brain and Amazon Alexa use for language processing and generation.