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Sample records for hydride generation-atomic absorption

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

    Czech Academy of Sciences Publication Activity Database

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

    2006-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2015-01-01

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

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

    Science.gov (United States)

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

  4. 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.

  5. 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.

  6. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-01-15

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

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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

  13. 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.

  14. 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.)

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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...

  2. 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%

  3. 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.

  4. 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.

  5. [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.

  6. 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

  7. 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.

  8. 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

  9. 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

  10. 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

  11. 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.

  12. 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.)

  13. 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.

  14. 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

  15. Development of an automated technique for the speciation of arsenic using flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Ruede, T.R. (Inst. of Petrography and Geochemistry, Univ. of Karlsruhe (Germany)); Puchelt, H. (Inst. of Petrography and Geochemistry, Univ. of Karlsruhe (Germany))

    1994-09-01

    An automated method for the determination of arsenic acid (AsV), arsenous acid (AsIII), monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA) was developed using a commercial available flow injection hydride generation system. By carrying out the hydride generation in selected acid media the determination of As(III) alone, of MMAA and DMAA by sum and by different sensitivities, and of all four species is possible. (orig.)

  16. 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.

  17. 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

  18. 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...

  19. [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.

  20. Multipumping flow system for improving hydride generation atomic fluorescence spectrometric determinations

    International Nuclear Information System (INIS)

    Lopez-Garcia, Ignacio; Ruiz-Alcaraz, Irene; Hernandez-Cordoba, Manuel

    2006-01-01

    The advantages of using membrane micropumps rather than peristaltic pumps to introduce both sample and reagent solutions for hydride generation atomic fluorescence spectrometry are discussed. Arsenic was used as a test analyte to check the performance of the proposed manifold. Sample and reagent consumption was reduced 8-9 fold compared with continuous mode measurements made with peristaltic pumps, with no deterioration in sensitivity. The calibration graph was linear in the 0.05 to 2.5 μg l -1 As range using peak area as the analytical signal and maximum gain in the detector setting. A limit of detection (3σ) of 0.02 μg l -1 and relative standard deviation values close to 2% for 10 independent measurements of a 1 μg l -1 As solution were obtained. The sampling frequency increased from 45 to 102 h -1 with the subsequent saving in carrier gas used and reduction in wastes generated. The instrumental modification, which could be used for other elements currently determined by atomic fluorescence spectrometry, will permit hydride generators of more reduced dimensions to be constructed

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-12-15

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  3. 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

  4. 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

  5. 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

  6. 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

  7. 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.

  8. 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.)

  9. 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.

  10. 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.

  11. 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

  12. 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)

  13. 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.)

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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

  19. 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.

  20. 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.

  1. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-12-04

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

  3. 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

  4. [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

  5. 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...

  6. 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

  7. 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

  8. 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)

  9. Optimización y validación metodológica de la cuantificación de arsénico por inyección en flujo-generación de hidruros- espectrometría de absorción atómicas (IF-GH-EAA previa derivatizacíon con L-Cisteína Optimización and validation method for arsenic quantification by flow injection-hydride generation - atomic absorption spectrometry (fi-hg-aas after L-Cysteine derivatization

    Directory of Open Access Journals (Sweden)

    Julio A Navoni

    2009-12-01

    Full Text Available El arsénico (As es un contaminante natural que afecta una amplia zona de Argentina. El nivel de As en agua de consumo es utilizado para evaluar la fuente de exposición y en orina para evaluar exposición a este tóxico. El presente trabajo tuvo como objetivo la optimización y validación metodológica de una técnica para la cuantificación de As [As suma = As inorgánico (AsI + especies metiladas: ácido monometilarsónico (MMA y ácido dimetilarsínico (DMA], producto del metabolismo del AsI, por inyección en flujo- generación de hidruros- espectrometría de absorción atómica (IF-GH-EAA, previa derivatización con L-cisteína. La recuperación de las especies estudiadas: AsI (AsIII y AsV, MMA y DMA fue cercana al 100% en todos los casos. Los límites de detección y cuantificación encontrados fueron para agua y orina: 2 y 3 μg/L; 5 y 8 μg/L respectivamente y el rango dinámico de trabajo establecido fue desde 5 a 75 μg/L, permitiendo cuantificar As en muestras de agua cercanos a los estándares internacionales vigentes para valores máximos de As en agua de consumo y en orina en niveles comparables con los establecidos en población laboralmente no expuesta. Esta propuesta metodológica es una alternativa para evaluar la exposición al As en muestras de agua y orina, sin necesidad de utilizar prolongados pre-tratamientos de muestra, de forma más rápida y económica.Arsenic (As is a natural contaminant that affects a large area of Argentina. Quantification of As in drinking water has been used to evaluate the source of exposure and As in urine to assess exposure to this toxic. This study aimed to optimize and validate a methodological technique for the quantification of As [As sum = inorganic As (AsI + methylated species: monometilarsonic acid (MMA and dimetilarsinic acid (DMA], product of AsI metabolism by flow injectionhydride generation-atomic absorption spectrometry (FI-GH-AAS, after derivatization with L-cysteine. The recovery

  10. 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

  11. 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.

  12. 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

  13. 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)

  14. 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.

  15. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-15

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

  17. 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 ...

  18. 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

  19. 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.

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

    Science.gov (United States)

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

  1. 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

  2. Solid phase extraction of cadmium on 2-mercaptobenzothiazole loaded on sulfur powder in the medium of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate and cold vapor generation-atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    Pourreza, N.; Ghanemi, K.

    2010-01-01

    A novel solid phase extractor for preconcentration of cadmium at ng L -1 levels has been developed. Cadmium ions were retained on a column packed with sulfur powder modified with 2-mercaptobenzothiazole (2-MBT) in the medium of 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim] + PF 6 - ) ionic liquid. The presence of ionic liquid during modification of sulfur enhanced the retention of cadmium ions on the column. The retained cadmium ions were eluted with 2 mol L -1 solution of HCl and measured by cold vapor generation-atomic absorption spectrometry (CVG-AAS). By using reaction cell-gas liquid separator (RC-GLS), gaseous cadmium vapors were produced and reached the atomic absorption spectrometer, instantaneously. The influence of different variables on both processes of solid phase extraction and CVG-AAS determination of cadmium ions was investigated. The calibration curve was linear in the range of 10-200 ng L -1 of cadmium in the initial solution with r = 0.9992 (n = 8) under optimum conditions. The limit of detection based on three times the standard deviation of the blank (3S b , n = 10) was 4.6 ng L -1 . The relative standard deviation (R.S.D.) of 25 and 150 ng L -1 of cadmium was 4.1 and 2.2% (n = 8), respectively. The procedure was validated by the analysis of a certified reference material (DORM-3), water and fish samples.

  3. 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)

  4. 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

  5. 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.

  6. 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

  7. 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

  8. Studies of hydrogen absorption and desorption processes in advanced intermetallic hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Sato, Masashi

    2005-07-01

    This work is a part of the research program performed in the Department of Energy Systems, Institute for Energy Technology (Kjeller, Norway), which is focused on the development of the advanced hydrogen storage materials. The activities are aimed on studies of the mechanisms of hydrogen interactions with intermetallic alloys with focus on establishing an interrelation between the crystal structure, thermodynamics and kinetics of the processes in the metal-hydrogen systems, on the one hand, and hydrogen storage properties (capacity, rates of desorption, hysteresis). Many of the materials under investigation have potential to be applied in applications, whereas some already have been commercialised in the world market. A number of metals take up considerable amounts of hydrogen and form chemical compounds with H, metal hydrides. Unfortunately, binary hydrides are either very stable (e.g. for the rare earth metals [RE], Zr, Ti, Mg: metal R) or are formed at very high applied pressures of hydrogen gas (e.g. for the transition metals, Ni, Co, Fe, etc.: Metal T). However, hydrogenation process becomes easily reversible at very convenient from practical point of view conditions, around room temperature and at H2 pressures below 1 MPa for the two-component intermetallic alloys R{sub x}T{sub y}. This raised and maintains further interest to the intermetallic hydrides as solid H storage materials. Materials science research of this thesis is focused on studies of the reasons staying behind the beneficial effect of two non-transition elements M(i.e., In and Sn) contributing to the formation of the ternary intermetallic alloys R{sub x}T{sub y}M{sub 2}., on the hydrogen storage behaviours. Particular focus is on two aspects where the remarkable improvement of ordinary metal hydrides is achieved via introduction of In and Sn: a) Increase of the volume density of stored hydrogen in solid materials to the record high level. b) Improvement of the kinetics of hydrogen charge and

  9. Actuation of Pneumatic Artificial Muscle via Hydrogen Absorption/Desorption of Metal Hydride-LaNi5

    Directory of Open Access Journals (Sweden)

    Thanana Nuchkrua

    2015-01-01

    Full Text Available This paper presents experimental studies on mechanical actuations of a pneumatic artificial muscle (PAM, which is driven by hydrogen gas based metal hydride (MH. The dynamic performances of hydrogen absorption/desorption, taking place within a MH reactor, are controlled via implementing cooling/heating effects of a thermoelectric module (TEM. Hydrogen pressure is applied as a driving force to commanding work outputs of the PAM as desired mechanical actuations. Due to strong inherent nonlinearity, a conventional proportional integral derivative (PID control law is not capable of regulating thermodynamic variables of the HM reaction according to desired performances of the PAM. In this study, the fuzzy adaptive PID control is proposed in manipulating the MH reaction via the TEM. This viability of the proposed methodology is confirmed by the fact that the gains of PID control law are adapted by fuzzy rule-based tuning scheme at various operating conditions of the MH reactor. The experimental results show that the proposed control technique is much more effective than a PID control in both transient and steady state performances of the MH reactor for servo mechanical actuation of the PAM.

  10. 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.

  11. Determination of Ultra-trace Amounts of Arsenic(III) by Flow Injection Hydride Generation Atomic Absorption Spectrometry with On-line Preconcentration by Coprecipitation with Lanthanum Hydroxide or Hafnium Hydroxide

    DEFF Research Database (Denmark)

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

    1996-01-01

    -dissolution in a filterless knotted Microline reactor. The sample and coprecipitating agent are mixed on-line and merged with an ammonium buffer solution, which promotes a controllable and quantitative collection of the generated hydroxide on the inner walls of the knotted reactor incorporated into the FI-HG-AAS system....../h. The limit of detection (3s) was 0.003 µg/l and the precision (relative standard deviation) was 1.0% (n = 11)at the 0.1 µg/l level....

  12. Direct analysis of methylated trivalent arsenicals in mouse liver by hydride generation-cryotrapping- atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Currier, J. M.; Svoboda, Milan; de Moraes, D. P.; Matoušek, Tomáš; Dědina, Jiří; Stýblo, M.

    2011-01-01

    Roč. 24, č. 4 (2011), s. 478-480 ISSN 0893-228X R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation * tissue * hydride generation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.779, year: 2011

  13. 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...

  14. 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.

  15. 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.

  16. Nonflame atomic absorption determination of total mercury in natural waters using an HS-3 mercury-hydride system

    Energy Technology Data Exchange (ETDEWEB)

    Evdokimova, E.V.; Solov`eva, M.Kh.; Telegin, G.F. [Institute of Problems in the Technology of Microelectronics and High-Purity Materials, Moscow (Russian Federation)

    1995-02-01

    A method for nonflame atomic absorption determination of mercury with a detection limit of 1 x 10{sup -3} {mu}g/ml in natural waters without preconcentration is described. The method can be applied successfully in analysis of the environment.

  17. 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).

  18. 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

  19. 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

  20. Oxidation state specific generation of arsines from methylated arsenicals based on L-cysteine treatment in buffered media for speciation analysis by hydride generation-automated cryotrapping-gas chromatography-atomic absorption spectrometry with the multiatomizer

    Energy Technology Data Exchange (ETDEWEB)

    Matousek, Tomas [Institute of Analytical Chemistry of the ASCR, v.v.i., Videnska 1083, 14220 Prague (Czech Republic)], E-mail: matousek@biomed.cas.cz; Hernandez-Zavala, Araceli [Center for Environmental Medicine, Asthma, and Lung Biology, University of North Carolina at Chapel Hill, Chapel Hill, NC 27599-7310 (United States); Svoboda, Milan; Langrova, Lenka [Institute of Analytical Chemistry of the ASCR, v.v.i., Videnska 1083, 14220 Prague (Czech Republic); Charles University, Faculty of Science, Albertov 8, 12840 Prague 2 (Czech Republic); Adair, Blakely M. [Pharmacokinetics Branch, Experimental Toxicology Division, National Health and Environmental Effects Laboratory, Office of Research and Development, U.S. Environmental Protection Agency, Research Triangle Park, NC 27711 (United States); Drobna, Zuzana [Department of Nutrition, School of Medicine, University of North Carolina at Chapel Hill, Chapel Hill, NC 27599-7461 (United States); Thomas, David J. [Pharmacokinetics Branch, Experimental Toxicology Division, National Health and Environmental Effects Laboratory, Office of Research and Development, U.S. Environmental Protection Agency, Research Triangle Park, NC 27711 (United States); Styblo, Miroslav [Center for Environmental Medicine, Asthma, and Lung Biology, University of North Carolina at Chapel Hill, Chapel Hill, NC 27599-7310 (United States); Department of Nutrition, School of Medicine, University of North Carolina at Chapel Hill, Chapel Hill, NC 27599-7461 (United States); Dedina, Jiri [Institute of Analytical Chemistry of the ASCR, v.v.i., Videnska 1083, 14220 Prague (Czech Republic)

    2008-03-15

    An automated system for hydride generation-cryotrapping-gas chromatography-atomic absorption spectrometry with the multiatomizer is described. Arsines are preconcentrated and separated in a Chromosorb filled U-tube. An automated cryotrapping unit, employing nitrogen gas formed upon heating in the detection phase for the displacement of the cooling liquid nitrogen, has been developed. The conditions for separation of arsines in a Chromosorb filled U-tube have been optimized. A complete separation of signals from arsine, methylarsine, dimethylarsine, and trimethylarsine has been achieved within a 60 s reading window. The limits of detection for methylated arsenicals tested were 4 ng l{sup -1}. Selective hydride generation is applied for the oxidation state specific speciation analysis of inorganic and methylated arsenicals. The arsines are generated either exclusively from trivalent or from both tri- and pentavalent inorganic and methylated arsenicals depending on the presence of L-cysteine as a prereductant and/or reaction modifier. A TRIS buffer reaction medium is proposed to overcome narrow optimum concentration range observed for the L-cysteine modified reaction in HCl medium. The system provides uniform peak area sensitivity for all As species. Consequently, the calibration with a single form of As is possible. This method permits a high-throughput speciation analysis of metabolites of inorganic arsenic in relatively complex biological matrices such as cell culture systems without sample pretreatment, thus preserving the distribution of tri- and pentavalent species.

  1. Hydride Molecules towards Nearby Galaxies

    Science.gov (United States)

    Monje, Raquel R.; La, Ngoc; Goldsmith, Paul

    2018-06-01

    Observations carried out by the Herschel Space Observatory revealed strong spectroscopic signatures from light hydride molecules within the Milky Way and nearby active galaxies. To better understand the chemical and physical conditions of the interstellar medium, we conducted the first comprehensive survey of hydrogen fluoride (HF) and water molecular lines observed through the SPIRE Fourier Transform Spectrometer. By collecting and analyzing the sub-millimeter spectra of over two hundred sources, we found that the HF J = 1 - 0 rotational transition which occurs at approximately 1232 GHz was detected in a total of 39 nearby galaxies both in absorption and emission. The analysis will determine the main excitation mechanism of HF in nearby galaxies and provide steady templates of the chemistry and physical conditions of the ISM to be used in the early universe, where observations of hydrides are more scarce.

  2. 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.)

  3. 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

  4. 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.

  5. 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

  6. 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.)

  7. 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)

  8. The electrochemical impedance of metal hydride electrodes

    DEFF Research Database (Denmark)

    Valøen, Lars Ole; Lasia, Andrzej; Jensen, Jens Oluf

    2002-01-01

    The electrochemical impedance responses for different laboratory type metal hydride electrodes were successfully modeled and fitted to experimental data for AB5 type hydrogen storage alloys as well as one MgNi type electrode. The models fitted the experimental data remarkably well. Several AC......, explaining the experimental impedances in a wide frequency range for electrodes of hydride forming materials mixed with copper powder, were obtained. Both charge transfer and spherical diffusion of hydrogen in the particles are important sub processes that govern the total rate of the electrochemical...... hydrogen absorption/desorption reaction. To approximate the experimental data, equations describing the current distribution in porous electrodes were needed. Indications of one or more parallel reduction/oxidation processes competing with the electrochemical hydrogen absorption/desorption reaction were...

  9. 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

  10. 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.)

  11. In-situ X-ray diffraction : a useful tool to investigate hydride-formation reactions

    NARCIS (Netherlands)

    Notten, P.H.L.; Daams, J.L.C.; Veirman, de A.E.M.; Staals, A.A.

    1994-01-01

    A high-pressure X-ray diffraction (XRD) cell has been designed which allowed us to study simultaneously hydrogen absorption/desorption isotherms and XRD powder diffraction patterns on (de)hydrided intermetallic compounds. The hydride formation reaction was investigated in the case of LaNi5 under

  12. 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.)

  13. 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.)

  14. Metal Hydrides for Rechargeable Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Valoeen, Lars Ole

    2000-03-01

    the electrochemical hydride absorption/desorption reaction were observed. The results indicated rather large variations in the kinetic parameters for the process at different states of charge of the hydride material. The optimum energy efficiency for an alloy with composition MmNi3.5-3.7Co0.7-0.8Mn0.3-0.4A10.3-0.4 intended for utilisation in batteries was obtained in the range of 40 to 95% depth of discharge. (author)

  15. 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.

  16. 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)

  17. 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

  18. Preparation of beryllium hydride

    International Nuclear Information System (INIS)

    Bergeron, C.R.; Baker, R.W.

    1975-01-01

    Beryllium hydride of high bulk density, suitable for use as a component of high-energy fuels, is prepared by the pyrolysis, in solution in an inert solvent, of a ditertiary-alkyl beryllium. An agitator introduces mechanical energy into the reaction system, during the pyrolysis, at the rate of 0.002 to 0.30 horsepower per gallon of reaction mixture. (U.S.)

  19. 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.)

  20. 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)

  1. 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.

  2. Zircaloy-4 hydridation

    International Nuclear Information System (INIS)

    Vizcaino, Pablo

    1997-01-01

    The objectives of this work can be summarized as: 1) To reproduce, by heat treatments, matrix microstructures and hydride morphologies similar to those observed in structural components of the CNA-1 and CNE nuclear power plants; 2) To study the evolution of the mechanical properties of the original material with different hydrogen concentrations, such as microhardness, and its capacity to distinguish these materials; 3) To find parameters that allow to estimate the hydrogen content of a material by quantitative metallographic techniques, to be used as complementary in the study of the radioactive materials from reactors

  3. New ternary hydride formation in U-Ti-H system

    International Nuclear Information System (INIS)

    Yamamoto, Takuya; Kayano, Hideo; Yamawaki, Michio.

    1991-01-01

    Hydrogen absorption properties of two titanium-rich uranium alloys, UTi 2 and UTi 4 , were studied in order to prepare and identify the recently found ternary hydride. They slowly reacted with hydrogen of the initial pressure of 10 5 Pa at 873K to form the ternary hydride. The hydrogenated specimen mainly consisted of the pursued ternary hydride but contained also U(or UO 2 ), TiH x , and some transient phases. X-ray powder diffraction and Electron Probe Micro Analysis proved that it was the UTi 2 H x with the expected MgCu 2 structure, though all the X-ray peaks were broad probably because of inhomogeneity. This compound had extremely high resistance to powdering on its formation, which showed high potential utilities for a non-powdering tritium storage system or for other purposes. (author)

  4. 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)

  5. The use of atomic absorption spectroscopy to measure arsenic, selenium, molybdenum, and vanadium in water and soil samples from uranium mill tailings sites

    International Nuclear Information System (INIS)

    Hollenbach, M.H.

    1988-01-01

    The Technical Measurements Center (TMC) was established to support the environmental measurement needs of the various DOE remedial action programs. A laboratory intercomparison study conducted by the TMC, using soil and water samples from sites contaminated by uranium mill tailings, indicated large discrepancies in analytical results reported by participating laboratories for arsenic, selenium, molybdenum, and vanadium. The present study was undertaken to investigate the most commonly used analytical techniques for measuring these four elements, ascertain routine and reliable quantification, and assess problems and successes of analysts. Based on a survey of the technical literature, the analytical technique of atomic absorption spectroscopy was selected for detailed study. The application of flame atomic absorption, graphite furnace atomic absorption, and hydride generation atomic absorption to the analysis of tailings-contaminated samples is discussed. Additionally, laboratory sample preparation methods for atomic absorption spectroscopy are presented. The conclusion of this report is that atomic absorption can be used effectively for the determination of arsenic, selenium, molybdenum, and vanadium in water and soil samples if the analyst understands the measurement process and is aware of potential problems. The problem of accurate quantification of arsenic, selenium, molybdenum, and vanadium in water and soil contaminated by waste products from uranium milling operations affects all DOE remedial action programs [Surplus Facilities Management Program (SFMP), Formerly Utilized Site Remedial Action Program (FUSRAP), and Uranium Mill Tailings Remedial Action Program (UMTRAP)], since all include sites where uranium was processed. 96 refs., 9 figs

  6. 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)

  7. 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...

  8. 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

  9. Erbium hydride decomposition kinetics.

    Energy Technology Data Exchange (ETDEWEB)

    Ferrizz, Robert Matthew

    2006-11-01

    Thermal desorption spectroscopy (TDS) is used to study the decomposition kinetics of erbium hydride thin films. The TDS results presented in this report are analyzed quantitatively using Redhead's method to yield kinetic parameters (E{sub A} {approx} 54.2 kcal/mol), which are then utilized to predict hydrogen outgassing in vacuum for a variety of thermal treatments. Interestingly, it was found that the activation energy for desorption can vary by more than 7 kcal/mol (0.30 eV) for seemingly similar samples. In addition, small amounts of less-stable hydrogen were observed for all erbium dihydride films. A detailed explanation of several approaches for analyzing thermal desorption spectra to obtain kinetic information is included as an appendix.

  10. 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

  11. Hydrogen storage in complex hydrides

    International Nuclear Information System (INIS)

    Lupu, D.; Biris, A. R.; Misan, I.

    2005-01-01

    Full text: Hydrogen storage is a key enabling technology for the advancement of hydrogen and fuel cell power technologies in mobile and stationary applications. A relevant role of the fuel cell powered vehicles on the market of the transportation systems will be achieved only if the research and development of on-board vehicular hydrogen storage are able to allow a driving range of at least 500 km. The on-board hydrogen storage systems are more challenging due to the space, weight and cost limitations. This range of autonomy between refueling requires materials able to store at least 6.5% weight hydrogen, available at moderate pressures, at the working temperature of the fuel cells and with acceptable cycling stability. The intensive research on the hydrogen storage in alloys and intermetallic of the LaNi 5 , FeTi or Laves phase type compounds, which started more than three decades ago did not resulted in materials of more than about 3% H storage capacities. The 7.5% H content of the Mg hydride is still of attracting interest but though the absorption has been achieved at lower temperatures by ball milling magnesium with various amounts of nickel, the desorption can not be attained at 1 bar H 2 below 280 deg. C and the kinetics of the process is too slow. In the last decade, the attention is focused on another class of compounds, the complex hydrides of aluminum with alkali metals (alanates), due to their high hydrogen content. It was found that doping with Ti-based catalysts improve the hydrogenation/dehydrogenation conditions of NaAlH 4 . Later on, it was shown that ball milling with solid state catalysts greatly improve the hydrogen desorption kinetics of NaAlH 4 , and this also helps to the rehydriding process. The hydrogen desorption from NaAlH 4 occurs in three steps, it shows a reversible storage capacity of 5.5% H and this led to further research work for a better knowledge of its application relating properties. In this work, ball milling experiments on Na

  12. Complex Hydrides for Hydrogen Storage

    Energy Technology Data Exchange (ETDEWEB)

    Slattery, Darlene; Hampton, Michael

    2003-03-10

    This report describes research into the use of complex hydrides for hydrogen storage. The synthesis of a number of alanates, (AIH4) compounds, was investigated. Both wet chemical and mechano-chemical methods were studied.

  13. 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.

  14. 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)

  15. 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

  16. 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)

  17. Hydrogen Storage using Metal Hydrides in a Stationary Cogeneration System

    International Nuclear Information System (INIS)

    Botzung, Maxime; Chaudourne, Serge; Perret, Christian; Latroche, Michel; Percheron-Guegan, Annick; Marty Philippe

    2006-01-01

    In the frame of the development of a hydrogen production and storage unit to supply a 40 kW stationary fuel cell, a metal hydride storage tank was chosen according to its reliability and high energetic efficiency. The study of AB5 compounds led to the development of a composition adapted to the project needs. The absorption/desorption pressures of the hydride at 75 C (2 / 1.85 bar) are the most adapted to the specifications. The reversible storage capacity (0.95 %wt) has been optimized to our work conditions and chemical kinetics is fast. The design of the Combined Heat and Power CHP system requires 5 kg hydrogen storage but in a first phase, only a 0.1 kg prototype has been realised and tested. Rectangular design has been chosen to obtain good compactness with an integrated plate fin type heat exchanger designed to reach high absorption/desorption rates. In this paper, heat and mass transfer characteristics of the Metal Hydride tank (MH tank) during absorption/desorption cycles are given. (authors)

  18. 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)

  19. Activation and discharge kinetics of metal hydride electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Johnsen, Stein Egil

    2003-07-01

    Potential step chronoamperometry and Electrochemical Impedance Spectroscopy (eis) measurements were performed on single metal hydride particles. For the {alpha}-phase, the bulk diffusion coefficient and the absorption/adsorption rate parameters were determined. Materials produced by atomisation, melt spinning and conventional casting were investigated. The melt spun and conventional cast materials were identical and the atomised material similar in composition. The particles from the cast and the melt spun material were shaped like parallelepipeds. A corresponding equation, for this geometry, for diffusion coupled to an absorption/adsorption reaction was developed. It was found that materials produced by melt spinning exhibited lower bulk diffusion (1.7E-14 m2/s) and absorption/adsorption reaction rate (1.0E-8 m/s), compared to materials produced by conventionally casting (1.1E-13 m2/s and 5.5E-8 m/s respectively). In addition, the influence of particle active surface and relative diffusion length were discussed. It was concluded that there are uncertainties connected to these properties, which may explain the large distribution in the kinetic parameters measured on metal hydride particles. Activation of metal hydride forming materials has been studied and an activation procedure, for porous electrodes, was investigated. Cathodic polarisation of the electrode during a hot alkaline surface treatment gave the maximum discharge capacity on the first discharge of the electrode. The studied materials were produced by gas atomisation and the spherical shape was retained during the activation. Both an AB{sub 5} and an AB{sub 2} alloy was successfully activated and discharge rate properties determined. The AB{sub 2} material showed a higher maximum discharge capacity, but poor rate properties, compared to the AB{sub 5} material. Reduction of surface oxides, and at the same time protection against corrosion of active metallic nickel, can explain the satisfying results of

  20. 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.)

  1. 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

  2. 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.

  3. 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).

  4. 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-.

  5. Optical and photoemission studies of lanthanum hydrides

    International Nuclear Information System (INIS)

    Peterman, D.J.; Peterson, D.T.; Weaver, J.H.

    1980-01-01

    The results of optical absorptivity and photoemission measurements on lanthanum hydrides, LaH/sub x/ (1.98 less than or equal to x less than or equal to 2.89) are reported. The low energy (hν less than or equal to 0.5 eV) optical features in LaH/sub x/ are attributed to the filling of octahedral sites. Higher energy interband absorption involves states within the d-band complex, analogous to other dihydrides. As x increases above 2.0, the optical features change rapidly due to the increase in the number of occupied octahedral sites. Various band structure studies suggest that LaH 3 might be a semiconductor. Photoemission results show that as x increases, the d-derived states at E/sub F/ are drawn down and that for LaH 2 89 only very weak valence band emission is observed. The hydrogen-derived bonding bands are shown centered approx. 5 eV below E/sub F/. Observed chemical shifts in the La 5p/sub 1/2 3/2/ cores are discussed for 1.98 less than or equal to x less than or equal to 2.89

  6. 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.

  7. Simultaneous determination of total arsenic and total selenium in Chinese medicinal herbs by hydride generation atomic fluorescence spectrometry in tartaric acid medium

    International Nuclear Information System (INIS)

    Liu Zhanfeng; Sun Hanwen; Shen Shigang; Li Liqing; Shi Hongmei

    2005-01-01

    By HG-AFS, a new method was proposed for simultaneous determination of total arsenic and total selenium existed in the Chinese medicinal herbs in tartaric acid medium. The effects of analytical conditions and coexisting ions on the fluorescence signal intensity of analytes were investigated. The proposed method was provided with linear response ranges above 22 μg l -1 for As and 44 μg l -1 for Se, and the detection limits of 0.13 and 0.12 μg l -1 were obtained for As and Se respectively. The recoveries of 93.8-96.1% for As and 95.3-99.1% for Se, and the precision of 1.2-3.8% and 2.4-5.3% (R.S.D., n = 8) respectively, were obtained via simultaneous determined four samples of Chinese medicinal herbs and three certified botanic reference materials successfully. The proposed method has the advantages of simple operation, high sensitivity and high efficiency

  8. 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

  9. Investigations of intermetallic alloy hydriding mechanisms. Annual progress report, May 1 1979-April 30, 1980

    International Nuclear Information System (INIS)

    Livesay, B.R.; Larsen, J.W.

    1980-05-01

    Investigations are being conducted on mechanisms involved with the hydrogen-metal interactions which control the absorption and desorption processes in intermetallic compounds. The status of the following investigations is reported: modeling of hydride formation; microbalance investigations; microstructure investigations; flexure experiments; resistivity experiments; and nuclear backscattering measurements. These investigations concern fundamental hydrogen interaction mechanisms involved in storage alloys

  10. Tritium processing using metal hydrides

    International Nuclear Information System (INIS)

    Mallett, M.W.

    1986-01-01

    E.I. duPont de Nemours and Company is commissioned by the US Department of Energy to operate the Savannah River Plant and Laboratory. The primary purpose of the plant is to produce radioactive materials for national defense. In keeping with current technology, new processes for the production of tritium are being developed. Three main objectives of this new technology are to ease the processing of, ease the storage of, and to reduce the operating costs of the tritium production facility. Research has indicated that the use of metal hydrides offers a viable solution towards satisfying these objectives. The Hydrogen and Fuels Technology Division has the responsibility to conduct research in support of the tritium production process. Metal hydride technology and its use in the storage and transportation of hydrogen will be reviewed

  11. 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.

  12. Complex hydrides for hydrogen storage

    Science.gov (United States)

    Zidan, Ragaiy

    2006-08-22

    A hydrogen storage material and process of forming the material is provided in which complex hydrides are combined under conditions of elevated temperatures and/or elevated temperature and pressure with a titanium metal such as titanium butoxide. The resulting fused product exhibits hydrogen desorption kinetics having a first hydrogen release point which occurs at normal atmospheres and at a temperature between 50.degree. C. and 90.degree. C.

  13. 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.

  14. 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.

  15. 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.)

  16. 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.

  17. 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

  18. Flame emission, atomic absorption and fluorescence spectrometry

    International Nuclear Information System (INIS)

    Horlick, G.

    1980-01-01

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

  19. 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.)

  20. 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.

  1. Protein Nano-Object Integrator (ProNOI for generating atomic style objects for molecular modeling

    Directory of Open Access Journals (Sweden)

    Smith Nicholas

    2012-12-01

    Full Text Available Abstract Background With the progress of nanotechnology, one frequently has to model biological macromolecules simultaneously with nano-objects. However, the atomic structures of the nano objects are typically not available or they are solid state entities. Because of that, the researchers have to investigate such nano systems by generating models of the nano objects in a manner that the existing software be able to carry the simulations. In addition, it should allow generating composite objects with complex shape by combining basic geometrical figures and embedding biological macromolecules within the system. Results Here we report the Protein Nano-Object Integrator (ProNOI which allows for generating atomic-style geometrical objects with user desired shape and dimensions. Unlimited number of objects can be created and combined with biological macromolecules in Protein Data Bank (PDB format file. Once the objects are generated, the users can use sliders to manipulate their shape, dimension and absolute position. In addition, the software offers the option to charge the objects with either specified surface or volumetric charge density and to model them with user-desired dielectric constants. According to the user preference, the biological macromolecule atoms can be assigned charges and radii according to four different force fields: Amber, Charmm, OPLS and PARSE. The biological macromolecules and the atomic-style objects are exported as a position, charge and radius (PQR file, or if a default dielectric constant distribution is not selected, it is exported as a position, charge, radius and epsilon (PQRE file. As illustration of the capabilities of the ProNOI, we created a composite object in a shape of a robot, aptly named the Clemson Robot, whose parts are charged with various volumetric charge densities and holds the barnase-barstar protein complex in its hand. Conclusions The Protein Nano-Object Integrator (ProNOI is a convenient tool for

  2. Zirconium hydride containing explosive composition

    Science.gov (United States)

    Walker, Franklin E.; Wasley, Richard J.

    1981-01-01

    An improved explosive composition is disclosed and comprises a major portion of an explosive having a detonation velocity between about 1500 and 10,000 meters per second and a minor amount of a donor additive comprising a non-explosive compound or mixture of non-explosive compounds which when subjected to an energy fluence of 1000 calories/cm.sup.2 or less is capable of releasing free radicals each having a molecular weight between 1 and 120. Exemplary donor additives are dibasic acids, polyamines and metal hydrides.

  3. Room temperature and thermal decomposition of magnesium hydride/deuteride thin films

    Energy Technology Data Exchange (ETDEWEB)

    Ares, J.R.; Leardini, F.; Bodega, J.; Macia, M.D.; Diaz-Chao, P.; Ferrer, I.J.; Fernandez, J.F.; Sanchez, C. [Universidad Autonoma de Madrid (Spain). Lab. de Materiales de Interes en Energias Renovables

    2010-07-01

    Magnesium hydride (MgH{sub 2}) can be considered an interesting material to store hydrogen as long as two main drawbacks were solved: (i) its high stability and (ii) slow (de)hydriding kinetics. In that context, magnesium hydride films are an excellent model system to investigate the influence of structure, morphology and dimensionality on kinetic and thermodynamic properties. In the present work, we show that desorption mechanism of Pd-capped MgH{sub 2} at room temperature is controlled by a bidimensional interphase mechanism and a similar rate step limiting mechanism is observed during thermal decomposition of MgH{sub 2}. This mechanism is different to that occurring in bulk MgH{sub 2} (nucleation and growth) and obtained activation energies are lower than those reported in bulk MgH{sub 2}. We also investigated the Pd-capping properties upon H-absorption/desorption by means of RBS and isotope experiments. (orig.)

  4. Titanium tritide radioisotope heat source development: palladium-coated titanium hydriding kinetics and tritium loading tests

    International Nuclear Information System (INIS)

    Van Blarigan, Peter; Shugard, Andrew D.; Walters, R. Tom

    2012-01-01

    We have found that a 180 nm palladium coating enables titanium to be loaded with hydrogen isotopes without the typical 400-500 C vacuum activation step. The hydriding kinetics of Pd coated Ti can be described by the Mintz-Bloch adherent film model, where the rate of hydrogen absorption is controlled by diffusion through an adherent metal-hydride layer. Hydriding rate constants of Pd coated and vacuum activated Ti were found to be very similar. In addition, deuterium/tritium loading experiments were done on stacks of Pd coated Ti foil in a representative-size radioisotope heat source vessel. The experiments demonstrated that such a vessel could be loaded completely, at temperatures below 300 C, in less than 10 hours, using existing department-of-energy tritium handling infrastructure.

  5. Structural and magnetic transformations in NdMn2Hx hydrides

    International Nuclear Information System (INIS)

    Budziak, A.; Zachariasz, P.; Pełka, R.; Figiel, H.; Żukrowski, J.; Woch, M.W.

    2012-01-01

    Highlights: ► Full structural phase diagram is presented for the NdMn 2 H x (2.0 ≤ x ≤ 4.0) hydrides in the temperature range of 70–385 K. ► For samples x = 2.0, 2.5, and 4.0 a splitting into two phases with different hydrogen concentrations are observed. ► Only for samples with x = 3.0 and 3.5 no spinodal decompositions are detected. ► The effects of hydrogen absorption on structural properties are shown to be reflected in magnetic behavior. ► A huge jump of magnetic ordering temperatures from ∼104 K for host NdMn 2 to above 200 K for its hydrides is observed or anticipated. - Abstract: X-ray powder diffraction and bulk magnetization measurements were used to study structural and magnetic properties of hydrides NdMn 2 H x (2.0 ≤ x ≤ 4.0). The X-ray investigations performed in the temperature range 70–385 K have revealed many structural transformations at low temperatures. In particular, a transformation from the hexagonal to the monoclinic phase and spinodal decompositions were observed. The magnetic behavior of the hydrides is correlated with the structural transitions. A tentative structural diagram is presented. The obtained results are compared with the properties of other cubic and hexagonal RMn 2 H x hydrides.

  6. Hydrogen-storing hydride complexes

    Science.gov (United States)

    Srinivasan, Sesha S [Tampa, FL; Niemann, Michael U [Venice, FL; Goswami, D Yogi [Tampa, FL; Stefanakos, Elias K [Tampa, FL

    2012-04-10

    A ternary hydrogen storage system having a constant stoichiometric molar ratio of LiNH.sub.2:MgH.sub.2:LiBH.sub.4 of 2:1:1. It was found that the incorporation of MgH.sub.2 particles of approximately 10 nm to 20 nm exhibit a lower initial hydrogen release temperature of 150.degree. C. Furthermore, it is observed that the particle size of LiBNH quaternary hydride has a significant effect on the hydrogen sorption concentration with an optimum size of 28 nm. The as-synthesized hydrides exhibit two main hydrogen release temperatures, one around 160.degree. C. and the other around 300.degree. C., with the main hydrogen release temperature reduced from 310.degree. C. to 270.degree. C., while hydrogen is first reversibly released at temperatures as low as 150.degree. C. with a total hydrogen capacity of 6 wt. % to 8 wt. %. Detailed thermal, capacity, structural and microstructural properties have been demonstrated and correlated with the activation energies of these materials.

  7. 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.

  8. 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...

  9. 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(+).

  10. 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.)

  11. 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.

  12. 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

  13. 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)

  14. Achievement report for 1st phase (fiscal 1974-80) Sunshine Program research and development - Hydrogen energy. Research on transportation of hydrogen in the form of metallic hydride; 1974-1980 nendo kinzoku suisokabutsu ni yoru suiso no yuso gijutsu no kenkyu seika hokokusho

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1981-03-01

    This report concerns the transportation and storage of hydrogen using metallic hydrides that perform absorption and desorption of hydrogen. Alloys useable for this purpose have to be capable of reversibly absorbing and desorbing hydrogen within a certain temperature range. In the absence of guidelines to follow in the quest for such alloys, the efforts at discovering them turned out to be a continual series of trials and errors. Researches were conducted into the hydrogenation reaction of Mg and Mg-based alloys and into hydrides of V-based alloys, and into Zr-based alloy hydrides such as the ZrMn{sub 2} hydride, ZrNiMn hydride, Zr(Fe{sub x}Mn{sub 1-x}){sub 2} hydrides, TiZrFe{sub 2} hydride, Zr{sub x}Ti{sub 1-x}(Fe{sub y}Mn{sub 1-y}) hydrides, etc. Also studied were the electronics of hydrogen in metallic hydrides, rates of reaction between Mg-Ni-based alloys and hydrogen systems, endurance tests for hydrides of Mg-Ni-based alloys, effects exerted by absorbed gas molecules during the storage of hydrogen in Mg-Ni-based alloys, effective thermal conductivity in a layer filled with a metallic hydride, metallic hydride-aided hydrogen transportation systems, chemical boosters, etc. (NEDO)

  15. 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

  16. Tritium removal using vanadium hydride

    International Nuclear Information System (INIS)

    Hill, F.B.; Wong, Y.W.; Chan, Y.N.

    1978-01-01

    The results of an initial examination of the feasibility of separation of tritium from gaseous protium-tritium mixtures using vanadium hydride in cyclic processes is reported. Interest was drawn to the vanadium-hydrogen system because of the so-called inverse isotope effect exhibited by this system. Thus the tritide is more stable than the protide, a fact which makes the system attractive for removal of tritium from a mixture in which the light isotope predominates. The initial results of three phases of the research program are reported, dealing with studies of the equilibrium and kinetics properties of isotope exchange, development of an equilibrium theory of isotope separation via heatless adsorption, and experiments on the performance of a single heatless adsorption stage. In the equilibrium and kinetics studies, measurements were made of pressure-composition isotherms, the HT--H 2 separation factors and rates of HT--H 2 exchange. This information was used to evaluate constants in the theory and to understand the performance of the heatless adsorption experiments. A recently developed equilibrium theory of heatless adsorption was applied to the HT--H 2 separation using vanadium hydride. Using the theory it was predicted that no separation would occur by pressure cycling wholly within the β phase but that separation would occur by cycling between the β and γ phases and using high purge-to-feed ratios. Heatless adsorption experiments conducted within the β phase led to inverse separations rather than no separation. A kinetic isotope effect may be responsible. Cycling between the β and γ phases led to separation but not to the predicted complete removal of HT from the product stream, possibly because of finite rates of exchange. Further experimental and theoretical work is suggested which may ultimately make possible assessment of the feasibility and practicability of hydrogen isotope separation by this approach

  17. 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

  18. Method of making alkali metal hydrides

    Science.gov (United States)

    Pecharsky, Vitalij K.; Gupta, Shalabh; Pruski, Marek; Hlova, Ihor; Castle, Andra

    2017-05-30

    A method is provided for making alkali metal hydrides by mechanochemically reacting alkali metal and hydrogen gas under mild temperature (e.g room temperature) and hydrogen pressure conditions without the need for catalyst, solvent, and intentional heating or cooling.

  19. Ultrapure hydrogen thermal compressor based on metal hydrides for fuel cells and hybrid vehicles

    International Nuclear Information System (INIS)

    Almasan, V.; Biris, A.; Coldea, I.; Lupu, D.; Misan, I.; Popeneciu, G.; Ardelean, O.

    2007-01-01

    Full text: In hydrogen economy, efficient compressors are indispensable elements in the storage, transport and distribution of the produced hydrogen. Energetic efficient technologies can contribute to H 2 pipelines transport to the point of use and to distribute H 2 by refuelling stations. Characteristic for metal hydrides systems is the wide area of possibilities to absorb hydrogen at low pressure from any source of hydrogen, to store and deliver it hydrogen at high pressure (compression ratio more than 30). On the basis of innovative concepts and advanced materials for H 2 storage/compression (and fast thermal transfer), a fast mass (H 2 ) and heat transfer unit will be developed suitable to be integrated in a 3 stage thermal compressor. Metal hydrides used for a three stage hydrogen compression system must have different equilibrium pressures, namely: for stage 1, low pressure H 2 absorption and resistant to poisoning with impurities of hydrogen, for stage 2, medium pressure H 2 absorption and for stage 3, high pressure hydrogen delivery (120 bar). In the case of compression device based on metallic hydrides the most important properties are the hydrogen absorption/desorption rate, a smaller process enthalpy and a great structural stability on long term hydrogen absorption/desorption cycling. These properties require metal hydrides with large differences between the hydrogen absorption and desorption pressures at equilibrium, within a rather small temperature range. The main goal of this work is to search and develop metal hydride integrated systems for hydrogen purification, storage and compression. After a careful screening three hydrogen absorbing alloys will be selected. After selection, the work up of the alloys composition on the bases of detailed solid state studies, new multi-component alloys will be developed, with suitable thermodynamic and kinetic properties for a hydrogen compressor. The results of the study are the following: new types of hydrogen

  20. Infrared diode laser spectroscopy of lithium hydride

    International Nuclear Information System (INIS)

    Yamada, C.; Hirota, E.

    1988-01-01

    The fundamental and hot bands of the vibration--rotation transitions of 6 LiH, 7 LiH, 6 LiD, and 7 LiD were observed by infrared diode laser spectroscopy at Doppler-limited resolution. Lithium hydride molecules were produced by the reaction of the Li vapor with hydrogen at elevated temperatures. Some 40 transitions were observed and, after combined with submillimeter-wave spectra reported by G. M. Plummer et al. [J. Chem. Phys. 81, 4893 (1984)], were analyzed to yield Dunham-type constants with accuracies more than an order of magnitude higher than those published in the literature. It was clearly demonstrated that the Born--Oppenheimer approximation did not hold, and some parameters representing the breakdown were evaluated. The Born--Oppenheimer internuclear distance r/sup BO//sub e/ was derived to be 1.594 914 26 (59) A, where a new value of Planck's constant recommended by CODATA was employed. The relative intensity of absorption lines was measured to determine the ratio of the permanent dipole moment to its first derivative with respect to the internuclear distance: μ/sub e/ [(partialμpartialr)/sub e/ r/sub e/ ] = 1.743(86). The pressure broadening parameter Δν/sub p/ P was determined to be 6.40 (22) MHzTorr by measuring the linewidth dependence on the pressure of hydrogen, which was about four times larger than the value for the dipole--quadrupole interaction estimated by Kiefer and Bushkovitch's theory

  1. 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)

  2. 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

  3. Hydriding and structural characteristics of thermally cycled and cold-worked V-0.5 at.%C alloy

    International Nuclear Information System (INIS)

    Chandra, Dhanesh; Sharma, Archana; Chellappa, Raja; Cathey, William N.; Lynch, Franklin E.; Bowman, Robert C.; Wermer, Joseph R.; Paglieri, Stephen N.

    2008-01-01

    High pressure hydrides of V 0.995 C 0.005 were thermally cycled between β 2 - and γ-phases hydrides for potential use in cryocoolers/heat pumps for space applications. The effect of addition of carbon to vanadium, on the plateau enthalpies of the high pressure β 2 + γ region is minimal. This is in contrast to the calculated plateau enthalpies for low pressure (α + β 1 ) mixed phases which showed a noticeable lowering of the values. Thermal cycling between β 2 -and γ-phase hydrides increased the absorption pressures but desorption pressure did not change significantly and the free energy loss due to hysteresis also increased. Hydriding of the alloy with prior cold-work increased the pressure hysteresis significantly and lowered the hydrogen capacity. In contrast to the alloy without any prior straining (as-cast), desorption pressure of the alloy with prior cold-work also decreased significantly. Microstrains, 2 > 1/2 , in the β 2 -phase lattice of the thermally cycled hydrides decreased after 778 cycles and the domain sizes increased. However, in the γ-phase, both the microstrains and the domain sizes decreased after thermal cycling indicating no particle size effect. The dehydrogenated α-phase after 778 thermal cycles also showed residual microstrains in the lattice, similar to those observed in intermetallic hydrides. The effect of thermal cycling (up to 4000 cycles between β 2 - and γ-phases) and cold working on absorption/desorption pressures, hydrogen storage capacity, microstrains, long-range strains, and domain sizes of β 2 - and γ-phase hydrides of V 0.995 C 0.005 alloys are presented

  4. 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....

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

    Czech Academy of Sciences Publication Activity Database

    Šíma, Jan; Rychlovský, P.

    2003-01-01

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

  6. 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...

  7. Application of hafnium hydride control rod to large sodium cooled fast breeder reactor

    Energy Technology Data Exchange (ETDEWEB)

    Ikeda, Kazumi, E-mail: kazumi_ikeda@mfbr.mhi.co.jp [Mitsubishi FBR Systems, Inc., 34-17, Jingumae 2-Chome, Shibuya-ku, Tokyo 150-0001 (Japan); Moriwaki, Hiroyuki, E-mail: hiroyuki_moriwaki@mfbr.mhi.co.jp [Mitsubishi FBR Systems, Inc., 34-17, Jingumae 2-Chome, Shibuya-ku, Tokyo 150-0001 (Japan); Ohkubo, Yoshiyuki, E-mail: yoshiyuki_okubo@mfbr.mhi.co.jp [Mitsubishi FBR Systems, Inc., 34-17, Jingumae 2-Chome, Shibuya-ku, Tokyo 150-0001 (Japan); Iwasaki, Tomohiko, E-mail: tomohiko.iwasaki@qse.tohoku.ac.jp [Department of Quantum Science and Energy Engineering, Tohoku University, Aoba, Aramaki, Aoba-ku, Sendai-shi, Miyagi-ken 980-8579 (Japan); Konashi, Kenji, E-mail: konashi@imr.tohoku.ac.jp [Institute for Materials Research, Tohoku University, Narita-cho, Oarai-machi, Higashi-Ibaraki-gun, Ibaraki-ken 311-1313 (Japan)

    2014-10-15

    Highlights: • Application of hafnium hydride control rod to large sodium cooled fast breeder reactor. • This paper treats application of an innovative hafnium hydride control rod to a large sodium cooled fast breeder reactor. • Hydrogen absorption triples the reactivity worth by neutron spectrum shift at H/Hf ratio of 1.3. • Lifetime of the control rod quadruples because produced daughters of hafnium isotopes are absorbers. • Nuclear and thermal hydraulic characteristics of the reactor are as good as or better than B-10 enriched boron carbide. - Abstract: This study treats the feasibility of long-lived hafnium hydride control rod in a large sodium-cooled fast breeder reactor by nuclear and thermal analyses. According to the nuclear calculations, it is found that hydrogen absorption of hafnium triples the reactivity by the neutron spectrum shift at the H/Hf ratio of 1.3, and a hafnium transmutation mechanism that produced daughters are absorbers quadruples the lifetime due to a low incineration rate of absorbing nuclides under irradiation. That is to say, the control rod can function well for a long time because an irradiation of 2400 EFPD reduces the reactivity by only 4%. The calculation also reveals that the hafnium hydride control rod can apply to the reactor in that nuclear and thermal characteristics become as good as or better than 80% B-10 enriched boron carbide. For example, the maximum linear heat rate becomes 3% lower. Owing to the better power distribution, the required flow rate decreases approximately by 1%. Consequently, it is concluded on desk analyses that the long lived hafnium hydride control rod is feasible in the large sodium-cooled fast breeder reactor.

  8. A comparison of simultaneous plasma, atomic absorption, and iron colorimetric determinations of major and trace constituents in acid mine waters

    Science.gov (United States)

    Ball, J.W.; Nordstrom, D. Kirk

    1994-01-01

    Sixty-three water samples collected during June to October 1982 from the Leviathan/Bryant Creek drainage basin were originally analyzed by simultaneous multielement direct-current plasma (DCP) atomic-emission spectrometry, flame atomic-absorption spectrometry, graphite-furnace atomic-absorption spectrometry (GFAAS) (thallium only), ultraviolet-visible spectrometry, and hydride-generation atomic-absorption spectrometry.Determinations were made for the following metallic and semi-metallic constituents: AI, As, B, Ba, Be, Bi, Cd, Ca, Cr, Co, Cu, Fe(11), Fe(total), Li, Pb, Mg, Mn, Mo, Ni, K, Sb, Se, Si, Na, Sr, TI, V, and Zn. These samples were re-analyzed later by simultaneous multielement inductively coupled plasma (ICP) atomic-emission spectrometry and Zeeman-corrected GFAAS to determine the concentrations of many of the same constituents with improved accuracy, precision, and sensitivity. The result of this analysis has been the generation of comparative concentration values for a significant subset of the solute constituents. Many of the more recently determined values replace less-than-detection values for the trace metals; others constitute duplicate analyses for the major constituents. The multiple determinations have yielded a more complete, accurate, and precise set of analytical data. They also have resulted in an opportunity to compare the performance of the plasma-emission instruments operated in their respective simultaneous multielement modes. Flame atomic-absorption spectrometry was judged best for Na and K and hydride-generation atomic-absorption spectrometry was judged best for As because of their lower detection limit and relative freedom from interelement spectral effects. Colorimetric determination using ferrozine as the color agent was judged most accurate, precise, and sensitive for Fe. Cadmium, lead, and vanadium concentrations were too low in this set of samples to enable a determination of whether ICP or DCP is a more suitable technique. Of

  9. Pressure-induced transformations of molecular boron hydride

    International Nuclear Information System (INIS)

    Nakano, Satoshi; Hemley, Russell J; Gregoryanz, Eugene A; Goncharov, Alexander F; Mao, Ho-kwang

    2002-01-01

    Decaborane, a molecular boron hydride, was compressed to 131 GPa at room temperature to explore possible non-molecular phases in this system and their physical properties. Decaborane changed its colour from transparent yellow to orange/red above 50 GPa and then to black above 100 GPa, suggesting some transformations. Raman scattering and infrared (IR) absorption spectroscopy reveal significant structural changes. Above 100 GPa, B-B skeletal, B-H and B-H-B Raman/IR peaks gradually disappeared, which implies a transformation into a non-molecular phase in which conventional borane-type bonding is lost. The optical band gap of the material at 100 GPa was estimated to be about 1.0 eV

  10. Pressure-induced transformations of molecular boron hydride

    CERN Document Server

    Nakano, S; Gregoryanz, E A; Goncharov, A F; Mao Ho Kwang

    2002-01-01

    Decaborane, a molecular boron hydride, was compressed to 131 GPa at room temperature to explore possible non-molecular phases in this system and their physical properties. Decaborane changed its colour from transparent yellow to orange/red above 50 GPa and then to black above 100 GPa, suggesting some transformations. Raman scattering and infrared (IR) absorption spectroscopy reveal significant structural changes. Above 100 GPa, B-B skeletal, B-H and B-H-B Raman/IR peaks gradually disappeared, which implies a transformation into a non-molecular phase in which conventional borane-type bonding is lost. The optical band gap of the material at 100 GPa was estimated to be about 1.0 eV.

  11. 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.

  12. 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.)

  13. 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.

  14. 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%.

  15. 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)

  16. Accuracy of a method based on atomic absorption spectrometry to determine inorganic arsenic in food: Outcome of the collaborative trial IMEP-41.

    Science.gov (United States)

    Fiamegkos, I; Cordeiro, F; Robouch, P; Vélez, D; Devesa, V; Raber, G; Sloth, J J; Rasmussen, R R; Llorente-Mirandes, T; Lopez-Sanchez, J F; Rubio, R; Cubadda, F; D'Amato, M; Feldmann, J; Raab, A; Emteborg, H; de la Calle, M B

    2016-12-15

    A collaborative trial was conducted to determine the performance characteristics of an analytical method for the quantification of inorganic arsenic (iAs) in food. The method is based on (i) solubilisation of the protein matrix with concentrated hydrochloric acid to denature proteins and allow the release of all arsenic species into solution, and (ii) subsequent extraction of the inorganic arsenic present in the acid medium using chloroform followed by back-extraction to acidic medium. The final detection and quantification is done by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS). The seven test items used in this exercise were reference materials covering a broad range of matrices: mussels, cabbage, seaweed (hijiki), fish protein, rice, wheat, mushrooms, with concentrations ranging from 0.074 to 7.55mgkg(-1). The relative standard deviation for repeatability (RSDr) ranged from 4.1 to 10.3%, while the relative standard deviation for reproducibility (RSDR) ranged from 6.1 to 22.8%. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

  17. Various magnetic behaviors of the hydrides deriving from the tetragonal CeFeSi-type compounds

    International Nuclear Information System (INIS)

    Chevalier, B.; Tence, S.; Gaudin, E.; Matar, S.F.; Bobet, J.-L.

    2009-01-01

    The hydrides RETXH (RE = rare earth, T = transition metal and X = Si, Ge) crystallizing in the tetragonal ZrSiCuAs-type are obtained by hydrogen absorption of the intermetallics adopting the tetragonal CeFeSi-type. The H-insertion induces interesting magnetic transitions governed by two effects: the increase of the unit cell volume linked to the H-absorption and the occurrence of the RE-H chemical bonding. Some typical examples are reported in this present brief review.

  18. 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)

  19. 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

  20. 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.

  1. Crystal structure solution of hydrides containing natEu from neutron powder diffraction data

    International Nuclear Information System (INIS)

    Kohlmann, H.

    1999-01-01

    Complete text of publication follows. The location of hydrogen in crystal structures of metal hydrides usually requires neutron diffraction data. Some elements, however, show excessively high absorption cross sections, σ a , for neutrons, thus making this technique seemingly impractical. Therefore no complete, refined crystal structure data of europium hydrides (σ a ( nat Eu) = .4530 barns at λ = 179.8 pm [1]) have been reported so far. It is shown that the absorption can be reduced to a value reasonable for neutron diffraction experiments by taking advantage of the wavelength dependence of σ a combined with the use of annular samples at advanced diffractometers. Neutron powder diffraction data on several nat Eu containing deuterides suitable for the ab initio crystal structure solution and refinement have been taken at D20 and D4 (ILL, Grenoble). The crystal chemistry of these europium hydrides, among them the two new compounds EuMg 2 H 6 and EuMgH 4 [2], is discussed. (author) [1] V.F. Sears, Neutron News 1992, 3, 26-37.; [2] H. Kohlmann, F. Gingl, T. Hansen, K. Yvon, Angew. Chem. Int. Ed. Eng. 1999, 38, accepted

  2. 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.

  3. Multi-scale characterization of nanostructured sodium aluminum hydride

    Science.gov (United States)

    NaraseGowda, Shathabish

    instruments were utilized for this work and their data collection and analysis are reported. Quasielastic neutron scattering experiments were conducted at NIST Center for Neutron Research to characterize atomic hydrogen diffusion in bulk and nano-confined NaAlH4. It was observed that upon confinement of NaAlH4, a significantly higher fraction of hydrogen atoms were involved in diffusive motion on the pico-second to nano-second timescales. However, the confinement had no impact on the lattice diffusivities (jump/hopping rates) of atomic hydrogen, indicating that the improved hydrogen release rates were not due to any kinetic destabilization effects. Instead, the investigation strongly suggested thermodynamic destabilization as the major effect of nano-confinement. The local interaction of the metal sites in metal organic frameworks with the infiltrated hydride was studied using extended x-ray absorption spectroscopy technique. The experiments were conducted at Center for Advanced Microstructures and Devices at Louisiana State University. The metal sites were found to be chemically un-altered, hence ruling out any catalytic role in the dehydrogenation at room temperatures. The fractal morphology of NaAlH4 was characterized by ultra-small angle x-ray scattering experiments performed at Argonne National Lab. The studies quantitatively estimated the extent of densification in the course of one desorption cycle. The particle sizes were found to increase two-fold during heat treatment. Also, the nano-confinement procedure was shown to produce dense mass fractals as opposed to pristine NaAlH4, exhibiting a surface fractal morphology. Based on this finding, a new method to identify confined material from un-confined material in nano-composites was developed and is presented. Preliminary results of modeling and correlating multi-scale phenomena using a phase-field approach are also presented as the foundation for future work.

  4. 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

  5. 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)

  6. 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.

  7. 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.

  8. Method for preparation of uranium hydride

    International Nuclear Information System (INIS)

    Gorski, M.S.; Goncalves, Miriam; Mirage, A.; Lima, W. de.

    1985-01-01

    A method for preparation of Uranium Hydride starting from Hidrogen and Uranium is described. In the temperature range of 250 0 up to 350 0 C, and pressures above 10torr, Hydrogen reacts smoothly with Uranium turnings forming a fine black or dark gray powder (UH 3 ). Samples containing a significant amount of oxides show a delay before the reaction begging. (Author) [pt

  9. 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%

  10. Magnesium hydrides and their phase transitions

    Czech Academy of Sciences Publication Activity Database

    Paidar, Václav

    2016-01-01

    Roč. 41, č. 23 (2016), s. 9769-9773 ISSN 0360-3199 R&D Projects: GA MŠk(CZ) LD13069 Institutional support: RVO:68378271 Keywords : hydrogen * magnesium and transition metal hydrides * crystal structure stability * displacive phase transformations Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.582, year: 2016

  11. Are RENiAl hydrides metallic?

    Czech Academy of Sciences Publication Activity Database

    Eichinger, K.; Havela, L.; Prokleška, J.; Stelmakhovych, O.; Daniš, S.; Šantavá, Eva; Miliyanchuk, K.

    2009-01-01

    Roč. 100, č. 9 (2009), s. 1200-1202 ISSN 1862-5282 Grant - others:GA ČR(CZ) GA202/07/0418 Institutional research plan: CEZ:AV0Z10100520 Keywords : rare earth metals * magnetism * hydrides Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.862, year: 2009

  12. Lithium hydride hydrolysis: experimental and kinetic study

    International Nuclear Information System (INIS)

    Charton, S.; Maupoix, C.; Brevet, A.; Delaunay, F.; Heintz, O.; Saviot, L.

    2006-01-01

    In this work has been studied the contribution of various analyses techniques in the framework, on the one hand of revealing the mechanisms implied in lithium hydride hydrolysis, and on the other hand of studying the kinetics of hydrogen production. Among the methods recently investigated, Raman spectroscopy, XPS and SIMS seem to be particularly attractive. (O.M.)

  13. Rapid hydrogen charging on metal hydride negative electrode of Fuel Cell/Battery (FCB) systems

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Bokkyu; Lee, Sunmook; Kawai, Hiroyuki; Fushimi, Chihiro; Tsutsumi, Atsushi [Collaborative Research Center for Energy Engineering, Institute of Industrial Science, The University of Tokyo, 4-6-1 Komaba, Meguro-ku, Tokyo 153-8505 (Japan)

    2009-02-15

    The characteristics of rapid gaseous H{sub 2} charging/electrochemical discharging of the metal hydride negative electrode were investigated for the application in Fuel Cell/Battery (FCB) systems. They were evaluated with the H{sub 2} gas absorption, followed by the subsequent electrochemical discharging in the electrolyte solution (6M KOH). Then, the cyclability of charge-discharge was also examined. It was observed that more than 70% of the theoretical capacity was charged within 10 min with 0.3 MPa and 0.5 MPa of the initial H{sub 2} pressures. The electrochemical discharge curve showed that more than 86% of the absorbed H{sub 2} was discharged. Furthermore, the cycled charge-discharge process indicated that the H{sub 2} gas charge and electrochemical discharge process is an effective way to rapidly charge and activate the metal hydride without degeneration. (author)

  14. Alternatives for metal hydride storage bed heating and cooling

    International Nuclear Information System (INIS)

    Fisher, I.A.; Ramirez, F.B.; Koonce, J.E.; Ward, D.E.; Heung, L.K.; Weimer, M.; Berkebile, W.; French, S.T.

    1991-01-01

    The reaction of hydrogen isotopes with the storage bed hydride material is exothermic during absorption and endothermic during desorption. Therefore, storage bed operation requires a cooling system to remove heat during absorption, and a heating system to add the heat needed for desorption. Three storage bed designs and their associated methods of heating and cooling and accountability are presented within. The first design is the current RTF (Replacement Tritium Facility) nitrogen heating and cooling system. The second design uses natural convection cooling with ambient glove box nitrogen and electrical resistance for heating. This design is referred to as the Naturally Cooled/Electrically Heated (NCEH) design. The third design uses forced convection cooling with ambient glove box nitrogen and electrical resistance for heating. The design is referred to as the Forced Convection Cooled/Electrically Heated (FCCEH) design. In this report the operation, storage bed design, and equipment required for heating, cooling, and accountability of each design are described. The advantages and disadvantages of each design are listed and discussed. Based on the information presented within, it is recommended that the NCEH design be selected for further development

  15. 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)

  16. 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

  17. Hydridation of Ti-6Al-4V

    International Nuclear Information System (INIS)

    Domizzi, G; Luppo, M.I; Ortiz, M; Vigna, G

    2004-01-01

    The production of Ti pieces or their alloys through powder metallurgy is an economical alternative that replaces the costly methods commonly used. The Ti-6AI-4V alloy is widely used in the aerospace, chemical and medical industries. The use of powder from the alloy instead of using more pure alloyed titanium powders, further simplifies the production process. The presence of V allows the phase β to stabilize at very low temperatures and both alloys alter the Ti-H equilibrium diagram. This work analyzes to what degree these effects influence the obtaining of powders from this alloy from that of hydridation and dehydridation. Although it has slower kinetics, powders can be produced in times similar to those found for grade 2 Ti since the distribution of hydrides in the sample is uniform and the material is fragile enough for concentrations of approximately 0.7 H/Ti (CW)

  18. 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

  19. Hydrides and Borohydrides of Light Elements

    Science.gov (United States)

    1947-12-04

    Troy, Attn: Inst. of Naval Science (30) Solar Aircraft Cu,, San Diego, Attn: Dr. M. A. Williamson " (31) INSMAT. N. J. for Itandard Oil Co., Esso Lab...with the other# iLD F.Re p. 8 ilt -ms" #61ggSotod that.. ir addition to thc impurity in the t~y..thr, an impurkty, prosumably aluminum hydride, in

  20. Facile Synthesis of Permethyl Yttrocene Hydride

    NARCIS (Netherlands)

    Haan, Klaas H. den; Teuben, Jan H.

    1984-01-01

    A convenient three step synthesis of (Cp*2YH)n (Cp* = C5Me5) is described starting with YCl3.3thf, in which Cp*2YCl.thf and Cp*2YCH(SiMe3)2 are intermediates, which could be isolated and characterized. The hydride is active in the activation of sp2 and sp3 C-H bonds as was demonstrated by the H-D

  1. 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

  2. Electrolytic hydriding of LaFe{sub 13-x}Si{sub x} alloys for energy efficient magnetic cooling

    Energy Technology Data Exchange (ETDEWEB)

    Lyubina, Julia; Hannemann, Ullrich; Ryan, Mary P. [Department of Materials, Imperial College London (United Kingdom); Cohen, Lesley F. [Department of Physics, Imperial College London (United Kingdom)

    2012-04-17

    An effective, low-temperature and readily available electrochemical method for tuning the operation temperature of LaFe{sub 13-x}Si{sub x}-type alloys is demonstrated. Electrolytically hydrided materials have the same high level magnetic properties as in high temperature gas-phase processed materials and offer an advantage of higher hydrogen absorption rate in the ferromagnetic state. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  3. 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

  4. Performance of a full-scale ITER metal hydride storage bed in comparison with requirements

    International Nuclear Information System (INIS)

    Beloglazov, S.; Glugla, M.; Fanghaenel, E.; Perevezentsev, A.; Wagner, R.

    2008-01-01

    The storage of hydrogen isotopes as metal hydride is the technique chosen for the ITER Tritium Plant Storage and Delivery System (SDS). A prototype storage bed of a full-scale has been designed, manufactured and intensively tested at the Tritium Laboratory, addressing main performance parameters specified for the ITER application. The main requirements for the hydrogen storage bed are a strict physical limitation of the tritium storage capacity (currently 70 g T 2 ), a high supply flow rate of hydrogen isotopes, in-situ calorimetry capabilities with an accuracy of 1 g and a fully tritium compatible design. The pressure composition isotherm of the ZrCo hydrogen system, as a reference material for ITER, is characterised by significant slope. As a result technical implementation of the ZrCo hydride bed in the SDS system requires further considerations. The paper presents the experience from the operation of ZrCo getter bed including loading/de-loading operation, calorimetric loop performance, and active gas cooling of the bed for fast absorption operation. The implications of hydride material characteristics on the SDS system configuration and design are discussed. (authors)

  5. 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.)

  6. Alloys for hydrogen storage in nickel/hydrogen and nickel/metal hydride batteries

    Science.gov (United States)

    Anani, Anaba; Visintin, Arnaldo; Petrov, Konstantin; Srinivasan, Supramaniam; Reilly, James J.; Johnson, John R.; Schwarz, Ricardo B.; Desch, Paul B.

    1993-01-01

    Since 1990, there has been an ongoing collaboration among the authors in the three laboratories to (1) prepare alloys of the AB(sub 5) and AB(sub 2) types, using arc-melting/annealing and mechanical alloying/annealing techniques; (2) examine their physico-chemical characteristics (morphology, composition); (3) determine the hydrogen absorption/desorption behavior (pressure-composition isotherms as a function of temperature); and (4) evaluate their performance characteristics as hydride electrodes (charge/discharge, capacity retention, cycle life, high rate capability). The work carried out on representative AB(sub 5) and AB(sub 2) type modified alloys (by partial substitution or with small additives of other elements) is presented. The purpose of the modification was to optimize the thermodynamics and kinetics of the hydriding/dehydriding reactions and enhance the stabilities of the alloys for the desired battery applications. The results of our collaboration, to date, demonstrate that (1) alloys prepared by arc melting/annealing and mechanical alloying/annealing techniques exhibit similar morphology, composition and hydriding/dehydriding characteristics; (2) alloys with the appropriate small amounts of substituent or additive elements: (1) retain the single phase structure, (2) improve the hydriding/dehydriding reactions for the battery applications, and (3) enhance the stability in the battery environment; and (3) the AB(sub 2) type alloys exhibit higher energy densities than the AB(sub 5) type alloys but the state-of-the-art, commercialized batteries are predominantly manufactured using Ab(sub 5) type alloys.

  7. Hydrogen storage in lithium hydride: A theoretical approach

    Science.gov (United States)

    Banger, Suman; Nayak, Vikas; Verma, U. P.

    2018-04-01

    First principles calculations have been carried out to analyze structural stability of lithium hydride (LiH) in NaCl phase using the full potential linearized augmented plane wave (FP-LAPW) method within the framework of density functional theory (DFT). Calculations have been extended to physiosorbed H-atom compounds LiH·H2, LiH·3H2 and LiH·4H2. The obtained results are discussed in the paper. The results for LiH are in excellent agreement with earlier reported data. The obtained direct energy band gap of LiH is 3.0 eV which is in excellent agreement with earlier reported theoretical band gap. The electronic band structure plots of the hydrogen adsorbed compounds show metallic behavior. The elastic constants, anisotropy factor, shear modulus, Young's modulus, Poisson's ratio and cohesive energies of all the compounds are calculated. Calculation of the optical spectra such as the real and imaginary parts of dielectric function, optical reflectivity, absorption coefficient, optical conductivity, refractive index, extinction coefficient and electron energy loss are performed for the energy range 0-15 eV. The obtained results for LiH·H2, LiH·3H2 and LiH·4H2, are reported for the first time. This study has been made in search of materials for hydrogen storage. It is concluded that LiH is a promising material for hydrogen storage.

  8. 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.

  9. 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.

  10. 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

  11. 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

  12. 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.

  13. 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

  14. 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....

  15. Minimizing hydride cracking in zirconium alloys

    International Nuclear Information System (INIS)

    Coleman, C.E.; Cheadle, B.A.; Ambler, J.F.R.; Eadie, R.L.

    1985-01-01

    Zirconium alloy components can fail by hydride cracking if they contain large flaws and are highly stressed. If cracking in such components is suspected, crack growth can be minimized by following two simple operating rules: components should be heated up from at least 30K below any operating temperature above 450K, and when the component requires cooling to room temperature from a high temperature, any tensile stress should be reduced as much and as quickly as is practical during cooling. This paper describes the physical basis for these rules

  16. Tritium immobilization and packaging using metal hydrides

    International Nuclear Information System (INIS)

    Holtslander, W.J.; Yaraskavitch, J.M.

    1981-04-01

    Tritium recovered from CANDU heavy water reactors will have to be packaged and stored in a safe manner. Tritium will be recovered in the elemental form, T 2 . Metal tritides are effective compounds in which to immobilize the tritium as a stable non-reactive solid with a high tritium capacity. The technology necessary to prepare hydrides of suitable metals, such as titanium and zirconium, have been developed and the properties of the prepared materials evaluated. Conceptual designs of packages for containing metal tritides suitable for transportation and long-term storage have been made and initial testing started. (author)

  17. Low-frequency excitations in zirconium hydrides

    International Nuclear Information System (INIS)

    Radulescu, A.; Padureanu, I.; Rapeanu, S.N.; Beldiman, A.; Kozlov, Zh.A.; Semenov, V.A.

    1999-01-01

    The slow inelastic neutron scattering (INS) on ZrH x systems (x = 0.38, 0.52) revealed new excitations located within the energy range 2-10 MeV. Besides the acoustic vibrations specific to α-HCP Zr and γ-FCO Zr hydride the fine structure of these excitations is clearly observed. The origin of the new observed peaks is not very clear but a proton tunneling or a resonance effect in α-Zr lattice could be taken into account

  18. Experimental determination of the phase diagram of the system sodium-sodium hydride up to 9000C and hydrogen pressures up to 800 bar

    International Nuclear Information System (INIS)

    Klostermeier, W.

    1978-01-01

    In the present work part of the sodium-sodium hydride system phase diagram has been studied at high temperatures (up to 900 0 C) and high hydrogen pressures (up to 1000 bar). The absorption isothermal curves recorded at temperatures between 650 0 C and 900 0 C show an increase in hydride solubility in sodium from 5.5 mol% at 650 0 to 19 mol% at 900 0 C. The melting point of sodium hydride has been measured giving the value 632 0 C with a hydrogen equilibrium pressure of 106 bar. In the mixing gap region the plateau equilibrium pressure, which is independent of composition, and his temperature dependence have been obtained. The enthalpy and entropy of melting are determined. (GSCH) [de

  19. Optical hydrogen sensors based on metal-hydrides

    Science.gov (United States)

    Slaman, M.; Westerwaal, R.; Schreuders, H.; Dam, B.

    2012-06-01

    For many hydrogen related applications it is preferred to use optical hydrogen sensors above electrical systems. Optical sensors reduce the risk of ignition by spark formation and are less sensitive to electrical interference. Currently palladium and palladium alloys are used for most hydrogen sensors since they are well known for their hydrogen dissociation and absorption properties at relatively low temperatures. The disadvantages of palladium in sensors are the low optical response upon hydrogen loading, the cross sensitivity for oxygen and carbon, the limited detection range and the formation of micro-cracks after some hydrogen absorption/desorption cycles. In contrast to Pd, we find that the use of magnesium or rear earth bases metal-hydrides in optical hydrogen sensors allow tuning of the detection levels over a broad pressure range, while maintaining a high optical response. We demonstrate a stable detection layer for detecting hydrogen below 10% of the lower explosion limit in an oxygen rich environment. This detection layer is deposited at the bare end of a glass fiber as a micro-mirror and is covered with a thin layer of palladium. The palladium layer promotes the hydrogen uptake at room temperature and acts as a hydrogen selective membrane. To protect the sensor for a long time in air a final layer of a hydrophobic fluorine based coating is applied. Such a sensor can be used for example as safety detector in automotive applications. We find that this type of fiber optic hydrogen sensor is also suitable for hydrogen detection in liquids. As example we demonstrate a sensor for detecting a broad range of concentrations in transformer oil. Such a sensor can signal a warning when sparks inside a high voltage power transformer decompose the transformer oil over a long period.

  20. 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

  1. Application of acoustic emission to hydride cracking

    International Nuclear Information System (INIS)

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

    1986-07-01

    Acoustic emission has been used for over a decade to study delayed hydride cracking (DHC) in zirconium alloys. At first acoustic emission was used primarily to detect the onset of DHC. This was possible because DHC was accompanied by very little plastic deformation of the material and furthermore the amplitudes of the acoustic pulses produced during cracking of the brittle hydride phase were much larger than those from dislocation motion and twinning. Acoustic emission was also used for measuring crack growth when it was found that for a suitable amplitude threshold, the total number of acoustic emission counts was linearly related to the cracked area. Once the proportionality constant was established, the acoustic counts could be converted to the crack length. Now the proportionality between the count rate and the crack growth rate is used to provide feedback between the crack length and the applied load, using computer technology. In such a system, the stress at the crack tip can be maintained constant during the test by adjusting the applied load as the crack progresses, or it can be changed in a predetermined manner, for example, to measure the threshold stress for cracking

  2. NATO Advanced Study Institute on Metal Hydrides

    CERN Document Server

    1981-01-01

    In the last five years, the study of metal hydrides has ex­ panded enormously due to the potential technological importance of this class of materials in hydrogen based energy conversion schemes. The scope of this activity has been worldwide among the industrially advanced nations. There has been a consensus among researchers in both fundamental and applied areas that a more basic understanding of the properties of metal/hydrogen syster;,s is required in order to provide a rational basis for the selection of materials for specific applications. The current worldwide need for and interest in research in metal hydrides indicated the timeliness of an Advanced Study Insti­ tute to provide an in-depth view of the field for those active in its various aspects. The inclusion of speakers from non-NATO coun­ tries provided the opportunity for cross-fertilization of ideas for future research. While the emphasis of the Institute was on basic properties, there was a conscious effort to stimulate interest in the applic...

  3. Ab-initio calculations of the hydrogen-uranium system: Surface phenomena, absorption, transport and trapping

    International Nuclear Information System (INIS)

    Taylor, Christopher D.; Scott Lillard, R.

    2009-01-01

    Density functional theory was applied to the initial steps of uranium hydriding: surface phenomena, absorption, bulk transport and trapping. H adsorbs exothermically to the (0 0 1) surface, yet H absorption into the bulk is endothermic, with off-center octahedral absorption having the lowest absorption energy of 0.39 eV, relative to molecular H 2 . H absorption in interstitial sites causes a local softening of the bulk modulus. Diffusion of H in unstrained α-U has a barrier of 0.6 eV. The energy of H absorption adjacent to the chemical impurities C, S, Si was lowered by an amount proportional to the size of the impurity atom, and the resulting lattice strain Si > S > C. Thus, impurities may promote hydriding by providing surfaces or prestrained zones for H uptake.

  4. Quantum molecular dynamics simulations of warm dense lithium hydride: Examination of mixing rules

    International Nuclear Information System (INIS)

    Horner, D. A.; Kress, J. D.; Collins, L. A.

    2008-01-01

    We have performed a systematic study of lithium hydride (LiH) in a density range from half to twice solid for temperatures from 0.5 to 3.0 eV using quantum molecular dynamics (QMD) methods and have tested density and pressure mixing rules for obtaining equations of state and optical properties such as frequency-dependent absorption coefficients and Rosseland mean opacities. The QMD simulations for the full LiH fluid served as a benchmark against which to assess the rules. In general, the mixing rule based on the pressure matching produces superior equations of state and mean opacities for the mixture except at the very lowest temperatures and densities. However, the frequency-dependent absorption coefficients displayed considerable differences in some frequency ranges except at the highest temperatures and densities

  5. Magnetic properties of (La1-xNdx)Co5 hydrides

    International Nuclear Information System (INIS)

    Fujiwara, K.; Nagai, H.; Tsujimura, A.

    1992-01-01

    Magnetization measurements have been performed on the pseudobinary compounds (La 1-x Nd x )Co 5 and their hydrides (La 1-x Nd x )Co 5 H y . The substitution of La for Nd leads to a lowering of the temperature (T R ) at which the easy magnetization direction changes (c-axis→a-axis). The value of T R decreases with La-concentration (1-x). The influence of the hydrogen absorption on T R is the same as that o of the substitution of La for Nd. The lowering of T R can be interpreted by the weakening of the Nd-Co coupling which is induced by the substitution of La for Nd and the hydrogen absorption. (orig.)

  6. 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

  7. 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.

  8. Scattering influences in quantitative fission neutron radiography for the in situ analysis of hydrogen distribution in metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Börries, S., E-mail: stefan.boerries@hzg.de [Helmholtz-Zentrum Geesthacht, Centre for Materials and Coastal Research, Max-Planck-Strasse 1, D-21502 Geesthacht (Germany); Metz, O.; Pranzas, P.K. [Helmholtz-Zentrum Geesthacht, Centre for Materials and Coastal Research, Max-Planck-Strasse 1, D-21502 Geesthacht (Germany); Bücherl, T. [ZTWB Radiochemie München (RCM), Technische Universität München (TUM), Walther-Meissner-Str. 3, D-85748 Garching (Germany); Söllradl, S. [Forschungs-Neutronenquelle Heinz Maier-Leibnitz (FRMII), Technische Universität München (TUM), Lichtenbergstr. 1, D-85748 Garching (Germany); Dornheim, M.; Klassen, T.; Schreyer, A. [Helmholtz-Zentrum Geesthacht, Centre for Materials and Coastal Research, Max-Planck-Strasse 1, D-21502 Geesthacht (Germany)

    2015-10-11

    In situ neutron radiography allows for the time-resolved study of hydrogen distribution in metal hydrides. However, for a precise quantitative investigation of a time-dependent hydrogen content within a host material, an exact knowledge of the corresponding attenuation coefficient is necessary. Additionally, the effect of scattering has to be considered as it is known to violate Beer's law, which is used to determine the amount of hydrogen from a measured intensity distribution. Within this study, we used a metal hydride inside two different hydrogen storage tanks as host systems, consisting of steel and aluminum. The neutron beam attenuation by hydrogen was investigated in these two different setups during the hydrogen absorption process. A linear correlation to the amount of absorbed hydrogen was found, allowing for a readily quantitative investigation. Further, an analysis of scattering contributions on the measured intensity distributions was performed and is described in detail.

  9. Multisyringe flow injection lab-on-valve systems coupled to hydride generation atomic fluorescence spectrometry for on-line bead-injection preconcentration and determination of total inorganic arsenic in environmental waters

    DEFF Research Database (Denmark)

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

    and 10% KI. The eluate merges downstream with a defined plug of sodium tetrahydroborate (0.3% w/v) for generation of arsine, which is subsequently quantified by AFS. An oxidation agent, namely 2x10-6 M potassium permanganate, was employed for the quantitative oxidation of As(III) to As(V) in the samples...

  10. Hydrogen storage in metal hydrides and complex hydrides; Wasserstoffspeicherung in Metall- und komplexen Hydriden - Schlussbericht

    Energy Technology Data Exchange (ETDEWEB)

    Bielmann, M.; Zuettel, A.

    2007-07-01

    This final report for the Swiss Federal Office of Energy (SFOE), reports on work done in 2007 at the Swiss Federal Laboratories for Materials Science and Technology EMPA on the storage of hydrogen in metal hydrides and complex hydrides. In particular, the use of tetrahydroborates is noted. The potential of this class of materials is stressed. The structures at room-temperature were examined using neutron and X-ray diffraction methods. Thermodynamic methods helped determine the thermodynamic stability of the materials. Also, a complete energy diagram for the materials was developed. The use of silicon oxide to reduce activation energy and its catalytic effects are discussed. The challenges placed by desorption mechanisms are noted. The authors note that reversibility is basically proven.

  11. Complex metal hydrides for hydrogen, thermal and electrochemical energy storage

    DEFF Research Database (Denmark)

    Møller, Kasper T.; Sheppard, Drew; Ravnsbæk, Dorthe B.

    2017-01-01

    field. This review illustrates that complex metal hydrides may store hydrogen in the solid state, act as novel battery materials, both as electrolytes and electrode materials, or store solar heat in a more efficient manner as compared to traditional heat storage materials. Furthermore, it is highlighted...... how complex metal hydrides may act in an integrated setup with a fuel cell. This review focuses on the unique properties of light element complex metal hydrides mainly based on boron, nitrogen and aluminum, e.g., metal borohydrides and metal alanates. Our hope is that this review can provide new...

  12. Finite difference program for calculating hydride bed wall temperature profiles

    International Nuclear Information System (INIS)

    Klein, J.E.

    1992-01-01

    A QuickBASIC finite difference program was written for calculating one dimensional temperature profiles in up to two media with flat, cylindrical, or spherical geometries. The development of the program was motivated by the need to calculate maximum temperature differences across the walls of the Tritium metal hydrides beds for thermal fatigue analysis. The purpose of this report is to document the equations and the computer program used to calculate transient wall temperatures in stainless steel hydride vessels. The development of the computer code was motivated by the need to calculate maximum temperature differences across the walls of the hydrides beds in the Tritium Facility for thermal fatigue analysis

  13. 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

  14. Process for production of a metal hydride

    Science.gov (United States)

    Allen, Nathan Tait; Butterick, III, Robert; Chin, Arthur Achhing; Millar, Dean Michael; Molzahn, David Craig

    2014-08-12

    A process for production of a metal hydride compound MH.sub.x, wherein x is one or two and M is an alkali metal, Be or Mg. The process comprises combining a compound of formula (R.sup.1O).sub.xM with aluminum, hydrogen and at least one metal selected from among titanium, zirconium, hafnium, niobium, vanadium, tantalum and iron to produce a compound of formula MH.sub.x. R.sup.1 is phenyl or phenyl substituted by at least one alkyl or alkoxy group. A mole ratio of aluminum to (R.sup.1O).sub.xM is from 0.1:1 to 1:1. The catalyst is present at a level of at least 200 ppm based on weight of aluminum.

  15. Boron hydride analogues of the fullerenes

    International Nuclear Information System (INIS)

    Quong, A.A.; Pederson, M.R.; Broughton, J.Q.

    1994-01-01

    The BH moiety is isoelectronic with C. We have studied the stability of the (BH) 60 analogue of the C 60 fullerene as well as the dual-structure (BH) 32 icosahedron, both of them being putative structures, by performing local-density-functional electronic calculations. To aid in our analysis, we have also studied other homologues of these systems. We find that the latter, i.e., the dual structure, is the more stable although the former is as stable as one of the latter's lower homologues. Boron hydrides, it seems, naturally form the dual structures used in algorithmic optimization of complex fullerene systems. Fully relaxed geometries are reported as well as electron affinities and effective Hubbard U parameters. These systems form very stable anions and we conclude that a search for BH analogues of the C 60 alkali-metal supeconductors might prove very fruitful

  16. Hydrogen storage properties of metallic hydrides

    International Nuclear Information System (INIS)

    Latroche, M.; Percheron-Guegan, A.

    2005-01-01

    Nowadays, energy needs are mainly covered by fossil energies leading to pollutant emissions mostly responsible for global warming. Among the different possible solutions for greenhouse effect reduction, hydrogen has been proposed for energy transportation. Indeed, H 2 can be seen as a clean and efficient energy carrier. However, beside the difficulties related to hydrogen production, efficient high capacity storage means are still to be developed. Many metals and alloys are able to store large amounts of hydrogen. This latter solution is of interest in terms of safety, global yield and long term storage. However, to be suitable for applications, such compounds must present high capacity, good reversibility, fast reactivity and sustainability. In this paper, we will review the structural and thermodynamic properties of metallic hydrides. (authors)

  17. Hydrogen storage in sodium aluminum hydride.

    Energy Technology Data Exchange (ETDEWEB)

    Ozolins, Vidvuds; Herberg, J.L. (Lawrence Livermore National Laboratories, Livermore, CA); McCarty, Kevin F.; Maxwell, Robert S. (Lawrence Livermore National Laboratories, Livermore, CA); Stumpf, Roland Rudolph; Majzoub, Eric H.

    2005-11-01

    Sodium aluminum hydride, NaAlH{sub 4}, has been studied for use as a hydrogen storage material. The effect of Ti, as a few mol. % dopant in the system to increase kinetics of hydrogen sorption, is studied with respect to changes in lattice structure of the crystal. No Ti substitution is found in the crystal lattice. Electronic structure calculations indicate that the NaAlH{sub 4} and Na{sub 3}AlH{sub 6} structures are complex-ionic hydrides with Na{sup +} cations and AlH{sub 4}{sup -} and AlH{sub 6}{sup 3-} anions, respectively. Compound formation studies indicate the primary Ti-compound formed when doping the material at 33 at. % is TiAl{sub 3} , and likely Ti-Al compounds at lower doping rates. A general study of sorption kinetics of NaAlH{sub 4}, when doped with a variety of Ti-halide compounds, indicates a uniform response with the kinetics similar for all dopants. NMR multiple quantum studies of solution-doped samples indicate solvent interaction with the doped alanate. Raman spectroscopy was used to study the lattice dynamics of NaAlH{sub 4}, and illustrated the molecular ionic nature of the lattice as a separation of vibrational modes between the AlH{sub 4}{sup -} anion-modes and lattice-modes. In-situ Raman measurements indicate a stable AlH{sub 4}{sup -} anion that is stable at the melting temperature of NaAlH{sub 4}, indicating that Ti-dopants must affect the Al-H bond strength.

  18. 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)

  19. 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.

  20. Electrochemical modeling of hydrogen storage in hydride-forming electrodes

    NARCIS (Netherlands)

    Ledovskikh, A.; Danilov, D.; Vermeulen, P.; Notten, P.H.L.

    2009-01-01

    An electrochemical kinetic model (EKM) is developed, describing the electrochemical hydrogen storage in hydride-forming materials under equilibrium conditions. This model is based on first principles of electrochemical reaction kinetics and statistical thermodynamics and describes the complex,

  1. 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)

  2. 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.

  3. 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

  4. Electronic structure of ternary hydrides based on light elements

    Energy Technology Data Exchange (ETDEWEB)

    Orgaz, E. [Departamento de Fisica y Quimica Teorica, Facultad de Quimica, Universidad Nacional Autonoma de Mexico, CP 04510 Coyoacan, Mexico, D.F. (Mexico)]. E-mail: orgaz@eros.pquim.unam.mx; Membrillo, A. [Departamento de Fisica y Quimica Teorica, Facultad de Quimica, Universidad Nacional Autonoma de Mexico, CP 04510 Coyoacan, Mexico, D.F. (Mexico); Castaneda, R. [Departamento de Fisica y Quimica Teorica, Facultad de Quimica, Universidad Nacional Autonoma de Mexico, CP 04510 Coyoacan, Mexico, D.F. (Mexico); Aburto, A. [Departamento de Fisica, Facultad de Ciencias, Universidad Nacional Autonoma de Mexico, CP 04510 Coyoacan, Mexico, D.F. (Mexico)

    2005-12-08

    Ternary hydrides based on light elements are interesting owing to the high available energy density. In this work we focused into the electronic structure of a series of known systems having the general formula AMH{sub 4}(A=Li,Na,M=B,Al). We computed the energy bands and the total and partial density of states using the linear-augmented plane waves method. In this report, we discuss the chemical bonding in this series of complex hydrides.

  5. Spectroscopy of helium hydride and triatomic hydrogen molecules

    International Nuclear Information System (INIS)

    Ketterle, W.

    1986-07-01

    Helium hydride and triatomic hydrogen has been produced by charge exchange between fast mass selected beams of molecular ions and alkali vapor. Using this method, the first discrete spectra of helium hydride were obtained. Fine electronic transitions with resolved rotational structure were observed in the visible and near infrared. Four isotopic mixtures were studied. Furthermore the first lifetime measurement of triatomic hydrogen states were performed and compared to theoretical predictions. (orig.)

  6. Proton location in metal hydrides using electron spin resonance

    International Nuclear Information System (INIS)

    Venturini, E.L.

    1979-01-01

    Electron spin resonance (ESR) of dilute paramagnetic ions establishes the site symmetry of these ions. In the case of metal hydrides the site symmetry is determined by the number and location of neighboring protons. Typical ESR spectra for trivalent erbium in scandium and yttrium hydrides are presented and analyzed, and this technique is shown to be a versatile microscopic probe of the location, net charge and occupation probability of nearby protons

  7. 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.

  8. Calcium absorption

    International Nuclear Information System (INIS)

    Carlmark, B.; Reizenstein, P.; Dudley, R.A.

    1976-01-01

    The methods most commonly used to measure the absorption and retention of orally administered calcium are reviewed. Nearly all make use of calcium radioisotopes. The magnitude of calcium absorption and retention depends upon the chemical form and amount of calcium administered, and the clinical and nutritional status of the subject; these influences are briefly surveyed. (author)

  9. 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

  10. 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

  11. 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.

  12. 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.

  13. Absorption studies

    International Nuclear Information System (INIS)

    Ganatra, R.D.

    1992-01-01

    Absorption studies were once quite popular but hardly anyone does them these days. It is easier to estimate the blood level of the nutrient directly by radioimmunoassay (RIA). However, the information obtained by estimating the blood levels of the nutrients is not the same that can be obtained from the absorption studies. Absorption studies are primarily done to find out whether some of the essential nutrients are absorbed from the gut or not and if they are absorbed, to determine how much is being absorbed. In the advanced countries, these tests were mostly done to detect pernicious anaemia where vitamin B 12 is not absorbed because of the lack of the intrinsic factor in the stomach. In the tropical countries, ''malabsorption syndrome'' is quire common. In this condition, several nutrients like fat, folic acid and vitamin B 12 are not absorbed. It is possible to study absorption of these nutrients by radioisotopic absorption studies

  14. 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)

  15. 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

  16. Fullerene hydride - A potential hydrogen storage material

    International Nuclear Information System (INIS)

    Nai Xing Wang; Jun Ping Zhang; An Guang Yu; Yun Xu Yang; Wu Wei Wang; Rui long Sheng; Jia Zhao

    2005-01-01

    Hydrogen, as a clean, convenient, versatile fuel source, is considered to be an ideal energy carrier in the foreseeable future. Hydrogen storage must be solved in using of hydrogen energy. To date, much effort has been put into storage of hydrogen including physical storage via compression or liquefaction, chemical storage in hydrogen carriers, metal hydrides and gas-on-solid adsorption. But no one satisfies all of the efficiency, size, weight, cost and safety requirements for transportation or utility use. C 60 H 36 , firstly synthesized by the method of the Birch reduction, was loaded with 4.8 wt% hydrogen indicating [60]fullerene might be as a potential hydrogen storage material. If a 100% conversion of C 60 H 36 is achieved, 18 moles of H 2 gas would be liberated from each mole of fullerene hydride. Pure C 60 H 36 is very stable below 500 C under nitrogen atmosphere and it releases hydrogen accompanying by other hydrocarbons under high temperature. But C 60 H 36 can be decomposed to generate H 2 under effective catalyst. We have reported that hydrogen can be produced catalytically from C 60 H 36 by Vasks's compound (IrCl(CO)(PPh 3 ) 2 ) under mild conditions. (RhCl(CO)(PPh 3 ) 2 ) having similar structure to (IrCl(CO)(PPh 3 ) 2 ), was also examined for thermal dehydrogenation of C 60 H 36 ; but it showed low catalytic activity. To search better catalyst, palladium carbon (Pd/C) and platinum carbon (Pt/C) catalysts, which were known for catalytic hydrogenation of aromatic compounds, were tried and good results were obtained. A very big peak of hydrogen appeared at δ=5.2 ppm in 1 H NMR spectrum based on Evans'work (fig 1) at 100 C over a Pd/C catalyst for 16 hours. It is shown that hydrogen can be produced from C 60 H 36 using a catalytic amount of Pd/C. Comparing with Pd/C, Pt/C catalyst showed lower activity. The high cost and limited availability of Vaska's compounds, Pd and Pt make it advantageous to develop less expensive catalysts for our process based on

  17. 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.

  18. Metal Hydride Nanoparticles with Ultrahigh Structural Stability and Hydrogen Storage Activity Derived from Microencapsulated Nanoconfinement.

    Science.gov (United States)

    Zhang, Jiguang; Zhu, Yunfeng; Lin, Huaijun; Liu, Yana; Zhang, Yao; Li, Shenyang; Ma, Zhongliang; Li, Liquan

    2017-06-01

    Metal hydrides (MHs) have recently been designed for hydrogen sensors, switchable mirrors, rechargeable batteries, and other energy-storage and conversion-related applications. The demands of MHs, particular fast hydrogen absorption/desorption kinetics, have brought their sizes to nanoscale. However, the nanostructured MHs generally suffer from surface passivation and low aggregation-resisting structural stability upon absorption/desorption. This study reports a novel strategy named microencapsulated nanoconfinement to realize local synthesis of nano-MHs, which possess ultrahigh structural stability and superior desorption kinetics. Monodispersed Mg 2 NiH 4 single crystal nanoparticles (NPs) are in situ encapsulated on the surface of graphene sheets (GS) through facile gas-solid reactions. This well-defined MgO coating layer with a thickness of ≈3 nm efficiently separates the NPs from each other to prevent aggregation during hydrogen absorption/desorption cycles, leading to excellent thermal and mechanical stability. More interestingly, the MgO layer shows superior gas-selective permeability to prevent further oxidation of Mg 2 NiH 4 meanwhile accessible for hydrogen absorption/desorption. As a result, an extremely low activation energy (31.2 kJ mol -1 ) for the dehydrogenation reaction is achieved. This study provides alternative insights into designing nanosized MHs with both excellent hydrogen storage activity and thermal/mechanical stability exempting surface modification by agents. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Thermal enhancement cartridge heater modified (TECH Mod) tritium hydride bed development, Part 1 - Design and fabrication

    Energy Technology Data Exchange (ETDEWEB)

    Klein, J.E.; Estochen, E.G. [Savannah River National Laboratory, Aiken, SC (United States)

    2015-03-15

    The Savannah River Site (SRS) tritium facilities have used first generation (Gen1) LaNi{sub 4.25}Al{sub 0.75} (LANA0.75) metal hydride storage beds for tritium absorption, storage, and desorption. The Gen1 design utilizes hot and cold nitrogen supplies to thermally cycle these beds. Second and third generation (Gen2 and Gen3) storage bed designs include heat conducting foam and divider plates to spatially fix the hydride within the bed. For thermal cycling, the Gen2 and Gen3 beds utilize internal electric heaters and glovebox atmosphere flow over the bed inside the bed external jacket for cooling. The currently installed Gen1 beds require replacement due to tritium aging effects on the LANA0.75 material, and cannot be replaced with Gen2 or Gen3 beds due to different designs of these beds. At the end of service life, Gen1 bed desorption efficiencies are limited by the upper temperature of hot nitrogen supply. To increase end-of-life desorption efficiency, the Gen1 bed design was modified, and a Thermal Enhancement Cartridge Heater Modified (TECH Mod) bed was developed. Internal electric cartridge heaters in the new design to improve end-of-life desorption, and also permit in-bed tritium accountability (IBA) calibration measurements to be made without the use of process tritium. Additional enhancements implemented into the TECH Mod design are also discussed. (authors)

  20. Folate absorption

    International Nuclear Information System (INIS)

    Baker, S.J.

    1976-01-01

    Folate is the generic term given to numerous compounds of pteroic acid with glutamic acid. Knowledge of absorption is limited because of the complexities introduced by the variety of compounds and because of the inadequacy of investigational methods. Two assay methods are in use, namely microbiological and radioactive. Techniques used to study absorption include measurement of urinary excretion, serum concentration, faecal excretion, intestinal perfusion, and haematological response. It is probably necessary to test absorption of both pteroylmonoglutamic acid and one or more polyglutamates, and such tests would be facilitated by availability of synthesized compounds labelled with radioactive tracers at specifically selected sites. (author)

  1. 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

  2. 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

  3. 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)

  4. 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)

  5. 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)

  6. 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.

  7. X-ray investigation of intermetallides and their hydrides under hydrogen pressure in H2-LaNi5 system

    International Nuclear Information System (INIS)

    Karonik, V.V.; Tsypin, M.I.; Prokof'ev, M.V.; Kazakov, D.N.

    1983-01-01

    X-ray phase analysis has been used to investigate phase composition of LaNi 5 -H 2 system; comparison of X-ray diffraction data with the results of plotting absorption and desorption isotherms is conducted. Technique of the X-ray diffraction study of intermetallide-hydrogen system using special X-ray chamber to diffractometer DRON-1.5 (GUR-5) is worked out. The parameters of elementary cell of the LaNisub(5)Hsub(6.2) hydride are determined: a=0.541(2) pm, c=0.430(2) nm, c/a=0.795, V=0.109 nm 3 (hexagonal syngony)

  8. Permeation rates for RTF metal hydride vessels

    International Nuclear Information System (INIS)

    Klein, J.E.

    1992-01-01

    Contamination rates have been estimated for the RTF nitrogen heating and cooling system (NH and CS) due to tritium permeation through the walls of metal hydride vessels. Tritium contamination of the NH and CS will be seen shortly after start-up of the RTF with the majority of it coming from the TCAP units. Contamination rates of the NH and CS are estimated to exceed 400 Ci/year after three years of operation and will elevate tritium concentrations in the NH and CS above 6 x 10 -3 μCi/cc. To reduce tritium activity in the NH and CS, a stripper or ''getter'' bed may need to be installed in the NH and CS. Increasing the purge rate of nitrogen from the NH and CS is shown to be an impractical method for reducing tritium activity due to the high purge rates required. Stripping of the NH and CS nitrogen in the glove box stripper system will give a temporary lowering of tritium activity in the NH and CS, but tritium activity will return to its previous level in approximately two weeks

  9. Hydriding and neutron irradiation in zircaloy-4

    International Nuclear Information System (INIS)

    Ramos, Ruben Fortunato; Martin, Juan Ezequiel; Orellano, Pablo; Dorao, Carlos; Analia Soldati; Ghilarducci, Ada Albertina; Corso, Hugo Luis; Peretti, Hernan Americo; Bolcich, Juan Carlos

    2003-01-01

    The composition of Zircaloy-4 for nuclear applications is specified by the ASTM B350 Standard, that fixes the amount of alloying elements (Sn, Fe, Cr) and impurities (Ni, Hf, O, N, C, among others) to optimize good corrosion and mechanical behavior.The recycling of zircaloy-4 scrap and chips resulting from cladding tube fabrication is an interesting issue.However, changes in the final composition of the recycled material may occur due to contamination with tool pieces, stainless steel chips, turnings, etc. while scrap is stored and handled. Since the main components of the possible contaminants are Fe, Cr and Ni, it arises the interest in studying up to what limit the Fe, Ni and Cr contents could be exceeded beyond the standard specification without affecting significantly the alloy properties.Zircaloy-4 alloys elaborated with Fe, Cr and Ni additions and others of standard composition in use in nuclear plants are studied by tensile tests, SEM observations and EDS microanalysis.Some samples are tested in the initial condition and others after hydriding treatments and neutron irradiation in the RA6

  10. Development of advanced neutron radiography for inspection on irradiated fuels and materials (2). Observation of hydride and oxide film on zircaloy cladding by using neutron radiography

    International Nuclear Information System (INIS)

    Yasuda, Ryou; Nakata, Masahito; Mastubayashi, Masahito; Harada, Katsuya

    2001-02-01

    Neutron radiography has been used as available diagnosis method of integrity on irradiated fuels, and has not been employed for estimating hydride and oxide film, which are influenced on integrity of Zircaloy cladding. Preliminary tests for PIE were carried out to assess possibility of neutron radiography as evaluation tool for hydrided and oxide film on the cladding. In these experiments, Zircaloy claddings with controlled amount of hydrogen absorption (200, 500, and 1000ppm) and thickness of oxide film were radiographed in center axis and in side directions of cladding tube by neutron imaging plate method. It is noted that thickness of oxide film was formed range from 7 μ m to 70 μ m at various temperatures (973, 1173, and 1323K) under steam atmosphere on the Zircaloy claddings. CT (Computed Tomography) restructure calculation was carried out to obtain cross section image of the claddings non-destructively. The Radiographs were qualitatively investigated about structure formation area and dependence of hydrogen absorption amount on PSL (Photo Simulated Luminescence) and CT values using by image analysis processor. At the results of imaging plate test, obvious difference was not found out between hydride formation (except for 1000ppm cladding) and standard claddings in side direction image. However, on the center axis direction image, outer circumference in the cladding cross-section that corresponded with hydride segregation area became blacker. In the case of oxide film formed cladding images, although oxide film could not find out on all speciments in the radiographs taken at the center axis and side directions, cross-section of claddings heat-processed at 973K showed appreciable blackness increasing with oxide film thickness on the radiographs. On the other hand, there is no effective difference between images of oxide film formed claddings processed at 1173K and 1323K and that of standard cladding. In CT image of 1000ppm hydrogen absorbed cladding, it is

  11. Recyclable hydrogen storage system composed of ammonia and alkali metal hydride

    Energy Technology Data Exchange (ETDEWEB)

    Yamamoto, Hikaru [Department of Quantum Matter, AdSM, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima, Hiroshima 739-8530 (Japan); Miyaoka, Hiroki; Hino, Satoshi [Institute for Advanced Materials Research, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima, Hiroshima 739-8530 (Japan); Nakanishi, Haruyuki [Higashi-Fuji Technical Center, Toyota Motor Corporation, 1200 Misyuku, Susono, Shizuoka 410-1193 (Japan); Ichikawa, Takayuki; Kojima, Yoshitsugu [Department of Quantum Matter, AdSM, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima, Hiroshima 739-8530 (Japan); Institute for Advanced Materials Research, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima, Hiroshima 739-8530 (Japan)

    2009-12-15

    Ammonia (NH{sub 3}) reacts with alkali metal hydrides MH (M = Li, Na, and K) in an exothermic reaction to release hydrogen (H{sub 2}) at room temperature, resulting that alkali metal amides (MNH{sub 2}) which are formed as by-products. In this work, hydrogen desorption properties of these systems and the condition for the recycle from MNH{sub 2} back to MH were investigated systematically. For the hydrogen desorption reaction, the reactivities of MH with NH{sub 3} were better following the atomic number of M on the periodic table, Li < Na < K. It was confirmed that the hydrogen absorption reaction of all the systems proceeded under 0.5 MPa of H{sub 2} flow condition below 300 C. (author)

  12. Hydrogen storage as a hydride. Citations from the International Aerospace Abstracts data base

    Science.gov (United States)

    Zollars, G. F.

    1980-01-01

    These citations from the international literature concern the storage of hydrogen in various metal hydrides. Binary and intermetallic hydrides are considered. Specific alloys discussed are iron titanium, lanthanium nickel, magnesium copper and magnesium nickel among others.

  13. 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

  14. 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

  15. 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.

  16. 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

  17. 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

  18. 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)

  19. A fractographic distinction between hydride cracking and stress corrosion cracking in zircaloys

    International Nuclear Information System (INIS)

    Cox, B.

    1978-06-01

    The fractographic details of SCC and delayed hydride failures are compared by scanning and replica electron microscopy. It is shown that there are distinct features ascribable to the fracture of hydride platelets which are absent from SCC fractures and which distinguish them from fractures produced by delayed hydride cracking. (author)

  20. Use of triammonium salt of aurin tricarboxylic acid as risk mitigant for aluminum hydride

    Science.gov (United States)

    Cortes-Concepcion, Jose A.; Anton, Donald L.

    2017-08-08

    A process and a resulting product by process of an aluminum hydride which is modified with by physically combining in a ball milling process an aluminum hydride with a triammonium salt of aurin tricarboxylic acid. The resulting product is an aluminum hydride which is resistant to air, ambient moisture, and liquid water while maintaining useful hydrogen storage and release kinetics.

  1. A computer model for hydride blister growth in zirconium alloys

    International Nuclear Information System (INIS)

    White, A.J.; Sawatzky, A.; Woo, C.H.

    1985-06-01

    The failure of a Zircaloy-2 pressure tube in the Pickering unit 2 reactor started at a series of zirconium hydride blisters on the outside of the pressure tube. These blisters resulted from the thermal diffusion of hydrogen to the cooler regions of the pressure tube. In this report the physics of thermal diffusion of hydrogen in zirconium is reviewed and a computer model for blister growth in two-dimensional Cartesian geometry is described. The model is used to show that the blister-growth rate in a two-phase zirconium/zirconium-hydride region does not depend on the initial hydrogen concentration nor on the hydrogen pick-up rate, and that for a fixed far-field temperature there is an optimum pressure-type/calandria-tube contact temperature for growing blisters. The model described here can also be used to study large-scale effects, such as hydrogen-depletion zones around hydride blisters

  2. Hydrides and deuterides of lithium and sodium. Pt. 1

    International Nuclear Information System (INIS)

    Haque, E.

    1990-01-01

    An interionic potential model is developed for lighter and heavier alkali hydrides and deuterides. The method uses a combination of theoretical techniques, empirical fit, and a few plausible assumptions. An assessment of the derived potentials is made by calculating the lattice statics and dynamics of the crystals and by comparing both with experiment (where available) and with other calculations. The potentials are found to describe the elastic and dielectric properties reasonably well. The phonon dispersion curves of hydride and deuteride of sodium are compared with the calculations of Dyck and Jex based on force constant model approach and the results are discussed. The need for further experiments on heavier hydrides and deuterides is stressed. (author)

  3. Research in Nickel/Metal Hydride Batteries 2017

    Directory of Open Access Journals (Sweden)

    Kwo-Hsiung Young

    2018-02-01

    Full Text Available Continuing from a special issue in Batteries in 2016, nineteen new papers focusing on recent research activities in the field of nickel/metal hydride (Ni/MH batteries have been selected for the 2017 Special Issue of Ni/MH Batteries. These papers summarize the international joint-efforts in Ni/MH battery research from BASF, Wayne State University, Michigan State University, FDK Corp. (Japan, Institute for Energy Technology (Norway, Central South University (China, University of Science and Technology Beijing (China, Zhengzhou University of Light Industry (China, Inner Mongolia University of Science and Technology (China, Shenzhen Highpower (China, and University of the Witwatersrand (South Africa from 2016–2017 through reviews of AB2 metal hydride alloys, Chinese and EU Patent Applications, as well as descriptions of research results in metal hydride alloys, nickel hydroxide, electrolyte, and new cell type, comparison work, and projections of future works.

  4. Kinetics of Hydrogen Absorption and Desorption in Titanium

    Directory of Open Access Journals (Sweden)

    Suwarno Suwarno

    2017-10-01

    Full Text Available Titanium is reactive toward hydrogen forming metal hydride which has a potential application in      energy storage and conversion. Titanium hydride has been widely studied for hydrogen storage, thermal storage, and battery electrodes applications. A special interest is using titanium for hydrogen production in a hydrogen sorption-enhanced steam reforming of natural gas. In the present work, non-isothermal dehydrogenation kinetics of titanium hydride and kinetics of hydrogenation in gaseous flow at isothermal conditions were investigated. The hydrogen desorption was studied using temperature desorption spectroscopy (TDS while the hydrogen absorption and desorption in gaseous flow were studied by temperature programmed desorption (TPD. The present work showed that the path of dehydrogenation of the TiH2 is d®b®a hydride phase with possible overlapping steps occurred. The fast hydrogen desorption rate observed at the TDS main peak temperature were correlated with the fast transformation of the d-TiH1.41 to b-TiH0.59. In the gaseous flow, hydrogen absorption and desorption were related to the transformation of b-TiH0.59 Û d-TiH1.41 with 2 wt.% hydrogen reversible content. Copyright © 2017 BCREC Group. All rights reserved Received: 21st November 2016; Revised: 20th March 2017; Accepted: 9th April 2017; Available online: 27th October 2017; Published regularly: December 2017 How to Cite: Suwarno, S., Yartys, V.A. (2017. Kinetics of Hydrogen Absorption and Desorption in Titanium. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (3: 312-317  (doi:10.9767/bcrec.12.3.810.312-317

  5. Complex Metal Hydrides for Hydrogen, Thermal and Electrochemical Energy Storage

    DEFF Research Database (Denmark)

    Moller, Kasper T.; Sheppard, Drew; Ravnsbaek, Dorthe B.

    2017-01-01

    Hydrogen has a very diverse chemistry and reacts with most other elements to form compounds, which have fascinating structures, compositions and properties. Complex metal hydrides are a rapidly expanding class of materials, approaching multi-functionality, in particular within the energy storage...... inspiration to solve the great challenge of our time: efficient conversion and large-scale storage of renewable energy....... field. This review illustrates that complex metal hydrides may store hydrogen in the solid state, act as novel battery materials, both as electrolytes and electrode materials, or store solar heat in a more efficient manner as compared to traditional heat storage materials. Furthermore, it is highlighted...

  6. Microcapsulated rare earth - nickel hydride-forming materials

    International Nuclear Information System (INIS)

    Ishikawa, H.; Oguro, K.; Kato, A.; Suzuki, H.; Ishii, E.

    1985-01-01

    Fine particles of hydride-forming alloys such as LaNi/sub 5/ and MmNi/sub 4.5/Mn/sub 0.5/ (MM : mischmetal) were coated with metallic copper thin layer by chemical plating method. Hydrogen storage capacities of alloys were not appreciably affected by the plating treatment. The capsulated alloy powders were easily pressed into pellets. The pellets obtained had high thermal conductivity and porosity enough to permeate hydrogen, leading to fast reaction kinetics. These were able to withstand more than 5,000 repeated hydriding-dehydriding cycles without disintegrating

  7. Hydriding and dehydriding properties of CaSi

    International Nuclear Information System (INIS)

    Aoki, Masakazu; Ohba, Nobuko; Noritake, Tatsuo; Towata, Shin-ichi

    2005-01-01

    The hydriding and dehydriding properties of CaSi were investigated both theoretically and experimentally. First-principles calculations suggested that CaSiH n is thermodynamically stable. Experimentally, the p -c isotherms clearly demonstrated plateau pressures in a temperature range of 473-573 K and the maximum hydrogen content was 1.9 weight % (wt.%) under a hydrogen pressure of 9 MPa at 473 K. The structure of CaSiH n is different from those of ZrNi hydrides, although CaSi has the CrB-type structure as well as ZrNi

  8. Thermophysical properties of solid lithium hydride and its isotopic modifications

    International Nuclear Information System (INIS)

    Mel'nikova, T.N.

    1981-01-01

    The theory of the anharmonic lattice is used to calculate the thermophysical properties (thermal expansivity, lattice constant, compressibility, and elastic moduli) of all the isotopic modifications of solid lithium hydride sup(6,7)Li(H,D,T) at temperatures up to the melting point. A general analysis of isotopic effects is carried out; in particular the reverse isotopic effect in the lattice constant is explained and the isotopic effect in melting is discussed. The results of the calculations agree with available experimental data and can be used for those isotopic modifications of lithium hydride for which there exist no experimental results. (author)

  9. Narrative absorption

    DEFF Research Database (Denmark)

    Narrative Absorption brings together research from the social sciences and Humanities to solve a number of mysteries: Most of us will have had those moments, of being totally absorbed in a book, a movie, or computer game. Typically we do not have any idea about how we ended up in such a state. No...

  10. 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

  11. 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)

  12. 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)

  13. In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

    Energy Technology Data Exchange (ETDEWEB)

    Cinbiz, Mahmut N., E-mail: cinbizmn@ornl.gov [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Koss, Donald A., E-mail: koss@ems.psu.edu [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Motta, Arthur T., E-mail: atm2@psu.edu [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Park, Jun-Sang, E-mail: parkjs@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States); Almer, Jonathan D., E-mail: almer@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States)

    2017-04-15

    The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. These experimental results can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix. - Highlights: •The δ{111} d-spacings aligned with the hydride plate edges exhibit a bi-linear thermal expansion. •Stress state reversal is predicted with the onset of hydride dissolution. •During dissolution, the δ{111} planes oriented parallel to the hydride plate face initially contract upon heating. •Hydride d-spacings indicate that both in-plane (circumferential) and out-of-plane (radial) hydrides are in the same strain-state and likely in the same stress state as well.

  14. 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.

  15. 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.

  16. 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)

  17. Absorptive products

    International Nuclear Information System (INIS)

    Assarsson, P.G.; King, P.A.

    1976-01-01

    Applications for hydrophile gels produced by the radiation induced cross-linking in aqueous solution of polyethylene oxide and starch, as described in Norwegian patent 133501 (INIS RN 281494), such as sanitary napkins (diapers) and sanitary towels, are discussed. The process itself is also discussed and results, expressed as the percentage of insoluble gel and its absorptive capacity for saline solution as functions of the ratio of polyethylene oxide to starch and the radiation dose, are presented. (JIW)

  18. Dislocation/hydrogen interaction mechanisms in hydrided nanocrystalline palladium films

    International Nuclear Information System (INIS)

    Amin-Ahmadi, Behnam; Connétable, Damien; Fivel, Marc; Tanguy, Döme; Delmelle, Renaud; Turner, Stuart; Malet, Loic; Godet, Stephane; Pardoen, Thomas; Proost, Joris; Schryvers, Dominique

    2016-01-01

    The nanoscale plasticity mechanisms activated during hydriding cycles in sputtered nanocrystalline Pd films have been investigated ex-situ using advanced transmission electron microscopy techniques. The internal stress developing within the films during hydriding has been monitored in-situ. Results showed that in Pd films hydrided to β-phase, local plasticity was mainly controlled by dislocation activity in spite of the small grain size. Changes of the grain size distribution and the crystallographic texture have not been observed. In contrast, significant microstructural changes were not observed in Pd films hydrided to α-phase. Moreover, the effect of hydrogen loading on the nature and density of dislocations has been investigated using aberration-corrected TEM. Surprisingly, a high density of shear type stacking faults has been observed after dehydriding, indicating a significant effect of hydrogen on the nucleation energy barriers of Shockley partial dislocations. Ab-initio calculations of the effect of hydrogen on the intrinsic stable and unstable stacking fault energies of palladium confirm the experimental observations.

  19. A system of hydrogen powered vehicles with liquid organic hydrides

    International Nuclear Information System (INIS)

    Taube, M.

    1981-07-01

    A motor car system based on the hydrogen produced by nuclear power stations during the night in the summer, and coupled with organic liquid hydride seems to be a feasible system in the near future. Such a system is discussed and the cost is compared with gasoline. (Auth.)

  20. Process of forming a sol-gel/metal hydride composite

    Science.gov (United States)

    Congdon, James W [Aiken, SC

    2009-03-17

    An external gelation process is described which produces granules of metal hydride particles contained within a sol-gel matrix. The resulting granules are dimensionally stable and are useful for applications such as hydrogen separation and hydrogen purification. An additional coating technique for strengthening the granules is also provided.

  1. Hydrogen storage alloys for nickel/metal hydride battery

    Energy Technology Data Exchange (ETDEWEB)

    Kuriyama, Nobuhiro; Sakai, Tetsuo; Myamura, Hiroshi; Tanaka, Hideaki; Ishikawa, Hiroshi; Uehara, Itsuki [Osaka National Research Inst. (Japan)

    1996-06-01

    Efforts to improve performance of metal hydride electrodes such as substitution of alloy components, heat treatment, and surface treatment intended to change surface and bulk structure of hydrogen storage alloys, mainly LaNi{sub 5} based alloys, are reviewed. The importance of control of morphology is emphasized. (author)

  2. Cascades for hydrogen isotope separation using metal hydrides

    International Nuclear Information System (INIS)

    Hill, F.B.; Grzetic, V.

    1982-01-01

    Designs are presented for continuous countercurrent hydrogen isotope separation cascades based on the use of metal hydrides. The cascades are made up of pressure swing adsorption (PSA) or temperature swing adsorption (TSA) stages. The designs were evolved from consideration of previously conducted studies of the separation performance of four types of PSA and TSA processes

  3. Deiodination reactions using tributyltin hydride for potential labelling experiments

    International Nuclear Information System (INIS)

    Zippi, E.M.; Plourde, G.W. II; Satyamurthy, N.

    1995-01-01

    2,6-Dinitro-1-iodobenzene and 2,4-dinitro-1-iodobenzene were deiodinated with tributylin hydride at different temperatures using various addition modes. The product ratios of 1,3-dinitrobenzene and the corresponding tributylstannyldinitrobenzene compounds were determined by NMR in order to evaluate the optimum conditions for impending tritiation experiments. (Author)

  4. Modeling of electrochemical hydrogen storage in metal hydride electrodes

    NARCIS (Netherlands)

    Ledovskikh, A.; Danilov, D.; Vermeulen, P.; Notten, P.H.L.

    2010-01-01

    The recently presented Electrochemical Kinetic Model (EKM), describing the electrochemical hydrogen storage in hydride-forming materials, has been extended by the description of the solid/electrolyte interface, i.e. the charge transfer kinetics and electrical double layer charging. A complete set of

  5. Modeling of electrochemical hydrogen storage in metal hydride electrodes

    NARCIS (Netherlands)

    Ledovskikh, A.; Danilov, D.; Vermeulen, P.; Notten, P.H.L.

    2010-01-01

    The recently presented electrochemical kinetic model, describing the electrochemical hydrogen storage in hydride-forming materials, was extended by the description of the solid/electrolyte interface, i.e., the charge-transfer kinetics and electrical double-layer charging. A complete set of equations

  6. 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

  7. Diastereoselectivity in the reduction of bicyclic enones with hindered hydrides

    OpenAIRE

    Camozzato, Andreza C.; Tenius, Beatriz S. M.; Oliveira, Eduardo R. de; Viegas Jr., Cláudio; Victor, Maurício M.; Silveira, Leandro G. da

    2008-01-01

    Reduction of five substituted octalones employing lithium tri-sec-butylborohydride (L-selectride®) in THF and ethyl ether led to allylic alcohols with moderate diastereoselectivity. The stereoselectivity of addition of bulky hydrides showed to be different from most examples in the literature and was strongly influenced by substitution on the octalone ring.

  8. Diastereoselectivity in the reduction of bicyclic enones with hindered hydrides

    International Nuclear Information System (INIS)

    Camozzato, Andreza C.; Tenius, Beatriz S. M.; Oliveira, Eduardo R. de; Viegas Junior, Claudio; Victor, Mauricio M.; Silveira, Leandro G. da

    2008-01-01

    Reduction of five substituted octalones employing lithium tri-sec-butylborohydride (L-selectride R ) in THF and ethyl ether led to allylic alcohols with moderate diastereoselectivity. The stereoselectivity of addition of bulky hydrides showed to be different from most examples in the literature and was strongly influenced by substitution on the octalone ring. (author)

  9. Fractal analysis of electrolytically-deposited palladium hydride dendrites

    International Nuclear Information System (INIS)

    Bursill, L.A.; Julin, Peng; Xudong, Fan.

    1990-01-01

    The fractal scaling characteristics of the surface profile of electrolytically-deposited palladium hydride dendritic structures have been obtained using conventional and high resolution transmission electron microscopy. The results are in remarkable agreement with the modified diffusion-limited aggregation model. 19 refs., 3 tabs., 13 figs

  10. 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.)

  11. 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

  12. 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.

  13. 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.

  14. Cascades for hydrogen isotope separation using metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Hill, F B; Grzetic, V [Brookhaven National Lab., Upton, NY (USA)

    1983-02-01

    Designs are presented for continuous countercurrent hydrogen isotope separation cascades based on the use of metal hydrides. The cascades are made up of pressure swing adsorption (PSA) or temperature swing adsorption (TSA) stages. The designs were evolved from consideration of previously conducted studies of the separation performance of four types of PSA and TSA processes.

  15. Diffusion model of delayed hydride cracking in zirconium alloys

    NARCIS (Netherlands)

    Shmakov, AA; Kalin, BA; Matvienko, YG; Singh, RN; De, PK

    2004-01-01

    We develop a method for the evaluation of the rate of delayed hydride cracking in zirconium alloys. The model is based on the stationary solution of the phenomenological diffusion equation and the detailed analysis of the distribution of hydrostatic stresses in the plane of a sharp tensile crack.

  16. Hydrogen Storage in Porous Materials and Magnesium Hydrides

    NARCIS (Netherlands)

    Grzech, A.

    2013-01-01

    In this thesis representatives of two different types of materials for potential hydrogen storage application are presented. Usage of either nanoporous materials or metal hydrides has both operational advantages and disadvantages. A main objective of this thesis is to characterize the hydrogen

  17. The Properties of Some Simple Covalent Hydrides: An Ab Initio ...

    African Journals Online (AJOL)

    Some properties of the monomeric binary hydrides of the elements of the first two rows of the periodic table have been determined using ab initio molecular orbital theory. The properties in question are the energetic, structural, electronic, topological and vibrational characteristics. In general, a gradual convergence towards ...

  18. 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)

  19. Hydrogen absorption-desorption properties of U2Ti

    International Nuclear Information System (INIS)

    Yamamoto, Takuya; Tanaka, Satoru; Yamawaki, Michio

    1990-01-01

    Hydrogen absorption-desorption properties of U 2 Ti intermetallic compound was examined over the temperature range of 298 to 973 K and at hydrogen pressures below 10 5 Pa. It absorbs hydrogen up to 7.6 atoms per F.U. (formula unit) by two step reactions and hence each desorption isotherm is separated into two plateau regions. In the first plateau, a newly-found ternary hydride is formed, where the hydrogen concentration, c H , reaches 2.4 H atoms/F.U. In the second plateau, UH 3 is formed and c H reaches 7.6 H atoms/F.U. The specimen is disintegrated into fine powder in the second plateau, while in the first plateau the ternary hydride which was identified to be UTi 2 H x (x=4.8 to 6.2) showed high durability against powdering. It is predicted that UTi 2 can be suitable material for tritium storage. (orig.)

  20. [Fluorescence Determination of Trace Se with the Hydride-K13-Rhodamine 6G System].

    Science.gov (United States)

    Liang, Ai-hui; Li, Yuan; Huang, Shan-shan; Luo, Yang-he; Wen, Gui-qing; Jiang, Zhi-liang

    2015-05-01

    Se is a necessary trace element for human and animals, but the excess intake of Se caused poison. Thus, it is very important to determination of Se in foods and water. The target of this study is development of a new, sensitive and selective hydride generation-molecular fluorescence method for the determination of Se. In 0. 36 mol . L-1 sulfuric acid, NaBH4 as reducing agent, Se (IV) is reduced to H2 Se. Usin3-g I solution as absorption liquid3, I- is reduced to I- by H2Se. When adding rhodamine 6G, Rhodamine 6G and I3- form association particles, which lead to the fluorescence intensity decreased. When Se(IV) existing, Rhodamine 6G and I3- bind less, And the remaining amount of Rhodamine 6G increase. So the fluorescence intensity is enhanced. The analytical conditions were optimized, a 0. 36 ml . L-1 H2SO4, 21. 6.g . L-1 NaBH4, 23.3 µm . L-1 rhodamine 6G, and 50 µmol . L-1 KI3 were chosen for use. When the excitation wavelength is at 480nm, the Rayleigh scattering peak does not affect the fluorescence recording, and was selected for determination of Se. Under the selected conditions, Se(IV) concentration in the 0. 02~0. 60 µg . mL-1 range and the increase value of the fluorescence intensity (ΔF) at 562 nm linear relationship. The linear regression equation is ΔF562 nm =12. 6c + 20. 9. The detecton limit was 0.01 µ.g . L-1. The influence of coexistence substances on the hydride generatin-molecular fluorescence determination of 5. 07 X10(-6) mol . L-1 Se(IV) was considered in details. Results showed that this new fluorescence method is of high selectivity, that is, 0. 5 mmol. L-1 Ba2+, Ca2+, Zn2+ and Fe3+, 0. 25 mmol . L-1 . Mg2+, 0. 05 mmol . L-1 K+, 0. 2 mmol . L-1 Al3+, 0. 025 mmol . L-1 Te(VI) do not interfere with the determination. The influence of Hg2+, CD2+ and Cu2+ that precipitate with Se(IV), can be eliminated by addition of complex reagent. This hydride generation-molecular fluorescence method has been applied to determination of trace Se in water

  1. Anisotropic Azimuthal Power and Temperature distribution on FuelRod. Impact on Hydride Distribution

    Energy Technology Data Exchange (ETDEWEB)

    Motta, Arthur [Pennsylvania State Univ., State College, PA (United States); Ivanov, Kostadin [Pennsylvania State Univ., State College, PA (United States); Arramova, Maria [Pennsylvania State Univ., State College, PA (United States); Hales, Jason [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2015-04-29

    The degradation of the zirconium cladding may limit nuclear fuel performance. In the high temperature environment of a reactor, the zirconium in the cladding corrodes, releasing hydrogen in the process. Some of this hydrogen is absorbed by the cladding in a highly inhomogeneous manner. The distribution of the absorbed hydrogen is extremely sensitive to temperature and stress concentration gradients. The absorbed hydrogen tends to concentrate near lower temperatures. This hydrogen absorption and hydride formation can cause cladding failure. This project set out to improve the hydrogen distribution prediction capabilities of the BISON fuel performance code. The project was split into two primary sections, first was the use of a high fidelity multi-physics coupling to accurately predict temperature gradients as a function of r, θ , and z, and the second was to use experimental data to create an analytical hydrogen precipitation model. The Penn State version of thermal hydraulics code COBRA-TF (CTF) was successfully coupled to the DeCART neutronics code. This coupled system was verified by testing and validated by comparison to FRAPCON data. The hydrogen diffusion and precipitation experiments successfully calculated the heat of transport and precipitation rate constant values to be used within the hydrogen model in BISON. These values can only be determined experimentally. These values were successfully implemented in precipitation, diffusion and dissolution kernels that were implemented in the BISON code. The coupled output was fed into BISON models and the hydrogen and hydride distributions behaved as expected. Simulations were conducted in the radial, axial and azimuthal directions to showcase the full capabilities of the hydrogen model.

  2. Hydrogenation of the rare earth alloys for production negative electrodes of nickel-metal hydride batteries

    International Nuclear Information System (INIS)

    Casini, Julio Cesar Serafim

    2011-01-01

    In this work were studied of La 0.7-x Mg x Pr 0.3 Al 0.3 Mn 0.4 Co 0.5 Ni 3.8 (X = 0 and 0.7) alloys for negative electrodes of the nickel-metal hydride batteries. The hydrogenation of the alloys was performed varying pressing of H 2 (2 and 10 bar) and temperature (room and 500 ℃). The discharge capacity of the nic kel-metal hydride batteries were analyzed in ARBIN BT- 4 electrical test equipment. The as-cast alloys were analyzed by scanning electron microscopy (SEM), energy disperse spectroscopy (EDX) and X-Ray diffraction. The increasing Mg addition in the alloy increases maximum discharge capacity but decrease cycle life of the batteries. The maximum discharge capacity was obtained with the Mg 0.7 Pr 0.3 Al 0.3 Mn 0.4 Co 0.5 Ni 3.8 alloy (60 mAh) and the battery which presented the best performance was La 0.4 Mg 0.3 Pr 0.3 Al 0.3 Mn 0.4 Co 0.5 Ni 3.8 alloy (53 mAh and 150 cycles). The H 2 capability of absorption was diminished for increased Mg addition and no such effect occurs for Mg 0.7 Pr 0.3 Al 0.3 Mn 0.4 Co 0.5 Ni 3.8 alloy. (author)

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

    Czech Academy of Sciences Publication Activity Database

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

    2017-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2017-01-01

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

  5. The effect of compositional changes on the structural and hydrogen storage properties of (La–Ce)Ni5 type intermetallics towards compounds suitable for metal hydride hydrogen compression

    International Nuclear Information System (INIS)

    Odysseos, M.; De Rango, P.; Christodoulou, C.N.; Hlil, E.K.; Steriotis, T.; Karagiorgis, G.; Charalambopoulou, G.; Papapanagiotou, T.; Ampoumogli, A.; Psycharis, V.; Koultoukis, E.; Fruchart, D.; Stubos, A.

    2013-01-01

    Graphical abstract: The effect of the partial substitution of La with Ce on the crystal structure and the final hydrogen storage properties of the alloys. Highlights: ► Absorption-based systems exploit the properties of reversible metal hydrides. ► AB5 intermetallics are mostly popular for thermal desorption compressors. ► Investigation of H2 absorption/desorption properties of LaNi5 and its derivatives. ► LaNi5 thermodynamic properties adjustment by partially replacing La with rare earths. -- Abstract: The present work has been aiming at the synthesis and study of a series of La 1−x Ce x Ni 5 (x = 0, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8) alloys in an attempt to investigate possible alterations of the hydrogen absorption/desorption properties The alloys were prepared by induction melting of the constituent elements. The systematic characterization of all new compounds by means of XRD and hydrogen sorption measurements revealed the effect of the partial substitution of La with Ce on the crystal structure and the final hydrogen storage properties of the alloys. Extensive absorption/desorption experiments (Van’t Hoff diagrams) have shown that such alloys can be used to build a metal hydride compressor (MHC), compressing H 2 gas from 0.2 MPa to 4.2 MPa using cold (20 °C) and hot (80 °C) water

  6. Hydriding properties of amorphous Ni-B alloy studied by DSC and thermogravimetry

    International Nuclear Information System (INIS)

    Spassov, T.; Rangelova, V.

    1999-01-01

    The hydrogenation behaviour of melt-spun Ni 81.5 B 18.5 amorphous alloy was studied by means of differential scanning calorimetry (DSC) and thermogravimetry (TG) and compared with the hydriding properties of a Fe-B-Si glass. It was found that the amorphous Ni-B alloy absorbs larger amounts of hydrogen than the Fe-B-Si glass, as the initial kinetics of hydrogen absorption and desorption of both the alloys are comparable. Hydrogen absorption and desorption reactions in Ni-B were observed to proceed with similar rates at ca. 300 K. The hydrogen desorption is revealed in DSC as an endothermic peak in the 350-450 K range, preceding the crystallization peak of the amorphous alloy. The enthalpy of hydrogen desorption (ΔH des =22 kJ/mol H 2 ) for Ni-B was found to be smaller than that for the Fe-B-Si glass, which finding is in contrast to the results on hydrogen diffusion in crystalline αFe and Fe-based alloys and Ni and Ni-based alloys. The hydrogen desorption temperature and enthalpy for Ni 81.5 B 18.5 were found to be independent of the amount of hydrogen absorbed. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  7. Hydride redistribution and crack growth in Zr-2.5 wt.% Nb stressed in torsion

    International Nuclear Information System (INIS)

    Puls, M.P.; Rogowski, A.J.

    1980-11-01

    The effect of applied shear stresses on zirconium hydride solubility in a zirconium alloy was investigated. Recent studies have shown that zirconium hydride precipiates probably nucleate and grow by means of a shear transformation mechanism. It is postulated that these transformation shear strains can interact with applied shear stress gradients in the same way that the dilatational strains can interact with a dilatational stress gradient, providing a driving force for hydride accumulation, hydride embrittlement and crack propagation. To test this proposition, crack growth experiments were carried out under torsional loading conditions on hydrided, round notched bar specimens of cold-worked Zr-2.5 wt.% Nb cut from Pickering-type pressure tube material. Postmortem metallographic examination of the hydride distribution in these samples showed that, in many cases, the hydrides appeared to have reoriented in response to the applied shear stress and that hydride accumulation at the notch tip had occurred. However, except in a few cases, the rate of accumulation of reoriented hydrides at the notch tip due to applied shear stresses was much less than the rate due to corresponding applied uniaxial stresss. Moreover, the process in shear appears to be more sensitive to the inital hydride size. Attempts to elucidate the fracture mechanism by fractographic examination using scanning and replica transmission electron microscopy proved to be inconclusive because of smearing of the fracture face. (auth)

  8. 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.

  9. Magnetic and hydrogen absorption properties of (La1-xYx) Co5-hydrides

    International Nuclear Information System (INIS)

    Fujiwara, K.; Ichinose, K.; Nagai, H.; Tsujimura, A.

    1988-01-01

    The 59 Co NMR and magnetization measurement in (La 1-x -Y x ) Co 5 H y have been performed at 77 K. The magnetizations of these compounds decrease with increasing hydrogen content (y) and are independent of Y-concentration (x). This result can be interpreted by an electron transfer effect in the direction H atom → Co atom

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

    Science.gov (United States)

    Anawar, Hossain Md

    2012-01-15

    For the past few years many studies have been performed to determine arsenic (As) speciation in drinking water, food chain and other environmental samples due to its well-recognized carcinogenic and toxic effects relating to its chemical forms and oxidation states. This review provides an overview of analytical methods, preconcentration and separation techniques, developed up to now, using HGAAS and ETAAS for the determination of inorganic As and organoarsenic species in environmental samples. Specific advantages, disadvantages, selectivity, sensitivity, efficiency, rapidity, detection limit (DL), and some aspects of recent improvements and modifications for different analytical and separation techniques, that can define their application for a particular sample analysis, are highlighted. HG-AAS has high sensitivity, selectivity and low DL using suitable separation techniques; and it is a more suitable, affordable and much less expensive technique than other detectors. The concentrations of HCl and NaBH(4) have a critical effect on the HG response of As species. Use of l-cysteine as pre-reductant is advantageous over KI to obtain the same signal response for different As species under the same, optimum and mild acid concentration, and to reduce the interference of transition metals on the arsine generation. Use of different pretreatment, digestion, separation techniques and surfactants can determine As species with DL from ngL(-1) to μgL(-1). Out of all the chromatographic techniques coupled with HGAAS/ETAAS, ion-pair reversed-phase chromatography (IP-RP) is the most popular due to its higher separation efficiency, resolution selectivity, simplicity, and ability to separate up to seven As species for both non-ionic and ionic compounds in a signal run using the same column and short time. However, a combination of anion- and cation-exchange chromatography seems the most promising for complete resolution up to eight As species. The ETAAS method using different separation techniques and chemical modifiers can determine As species in seawater with DL of 0.02 μgL(-1), eliminate interferences of transition metals, improve the selectivity of the measurement, and enhance the sensitivity. Copyright © 2011 Elsevier B.V. All rights reserved.

  11. Modeling of hydrogen isotopes separation in a metal hydride bed

    International Nuclear Information System (INIS)

    Charton, S.; Corriou, J.P.; Schweich, D.

    1999-01-01

    A predictive model for hydrogen isotopes separation in a non-isothermal bed of unsupported palladium hydride particles is derived. It accounts for the non-linear adsorption-dissociation equilibrium, hydrodynamic dispersion, pressure drop, mass transfer kinetics, heat of sorption and heat losses at the bed wall. Using parameters from the literature or estimated with classical correlations, the model gives simulated curves in agreement with previously published experiments without any parameter fit. The non-isothermal behavior is shown to be responsible for drastic changes of the mass transfer rate which is controlled by diffusion in the solid-phase lattice. For a feed at 300 K and atmospheric pressure, the endothermic hydride-to-deuteride exchange is kinetically controlled, whereas the reverse exothermic exchange is nearly at equilibrium. Finally, a simple and efficient thermodynamic model for the dissociative equilibrium between a metal and a diatomic gas is proposed. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  12. Catalytic effect of halide additives ball milled with magnesium hydride

    Energy Technology Data Exchange (ETDEWEB)

    Malka, I.E.; Bystrzycki, J. [Department of Advanced Materials and Technologies, Military University of Technology, Kaliskiego 2, 00-908 Warsaw (Poland); Czujko, T. [Department of Advanced Materials and Technologies, Military University of Technology, Kaliskiego 2, 00-908 Warsaw (Poland); CanmetENERGY, Hydrogen Fuel Cells and Transportation Energy, Natural Resources (Canada)

    2010-02-15

    The influence of various halide additives milled with magnesium hydride (MgH{sub 2}) on its decomposition temperature was studied. The optimum amount of halide additive and milling conditions were evaluated. The MgH{sub 2} decomposition temperature and energy of activation reduction were measured by temperature programmed desorption (TPD) and differential scanning calorimetry (DSC). The difference in catalytic efficiency between chlorides and fluorides of the various metals studied is presented. The effects of oxidation state, valence and position in the periodic table for selected halides on MgH{sub 2} decomposition temperature were also studied. The best catalysts, from the halides studied, for magnesium hydride decomposition were ZrF{sub 4}, TaF{sub 5}, NbF{sub 5}, VCl{sub 3} and TiCl{sub 3}. (author)

  13. Irradiation effects on thermal properties of LWR hydride fuel

    Energy Technology Data Exchange (ETDEWEB)

    Terrani, Kurt, E-mail: terrani@berkeley.edu [University of California, 4155 Etcheverry Hall, M.C. 1730, Berkeley, CA 94720-1730 (United States); Balooch, Mehdi [University of California, 4155 Etcheverry Hall, M.C. 1730, Berkeley, CA 94720-1730 (United States); Carpenter, David; Kohse, Gordon [Massachusetts Institute of Technology, 138 Albany St., Cambridge, MA 02139 (United States); Keiser, Dennis; Meyer, Mitchell [Idaho National Laboratory, Idaho Falls, ID 83415 (United States); Olander, Donald [University of California, 4155 Etcheverry Hall, M.C. 1730, Berkeley, CA 94720-1730 (United States)

    2017-04-01

    Three hydride mini-fuel rods were fabricated and irradiated at the MIT nuclear reactor with a maximum burnup of 0.31% FIMA or ∼5 MWd/kgU equivalent oxide fuel burnup. Fuel rods consisted of uranium-zirconium hydride (U (30 wt%)ZrH{sub 1.6}) pellets clad inside a LWR Zircaloy-2 tubing. The gap between the fuel and the cladding was filled with lead-bismuth eutectic alloy to eliminate the gas gap and the large temperature drop across it. Each mini-fuel rod was instrumented with two thermocouples with tips that are axially located halfway through the fuel centerline and cladding surface. In-pile temperature measurements enabled calculation of thermal conductivity in this fuel as a function of temperature and burnup. In-pile thermal conductivity at the beginning of test agreed well with out-of-pile measurements on unirradiated fuel and decreased rapidly with burnup.

  14. Positronium hydride defects in thermochemically reduced alkaline-Earth oxides

    International Nuclear Information System (INIS)

    Monge, M.A.; Pareja, R.; Gonzalez, R.; Chen, Y.

    1997-01-01

    Thermochemical reduction of both hydrogen-doped MgO and CaO single crystals results in large concentrations of hydride (H - ) ions. In MgO crystals, positron lifetime and Doppler broadening experiments show that positrons are trapped at H - centers forming positronium hydride molecules [e + - H - ]. A value of 640 ps is obtained for the lifetime of the PsH states located in an anion vacancy In MgO positrons are also trapped at H 2- sites at low temperatures. The H 2- ions were induced in the crystals by blue light illumination. The formation of PsH states in CaO could not be conclusively established. (orig.)

  15. FEASIBILITY OF RECYCLING PLUTONIUM AND MINOR ACTINIDES IN LIGHT WATER REACTORS USING HYDRIDE FUEL

    International Nuclear Information System (INIS)

    Greenspan, Ehud; Todreas, Neil; Taiwo, Temitope

    2009-01-01

    The objective of this DOE NERI program sponsored project was to assess the feasibility of improving the plutonium (Pu) and minor actinide (MA) recycling capabilities of pressurized water reactors (PWRs) by using hydride instead of oxide fuels. There are four general parts to this assessment: (1) Identifying promising hydride fuel assembly designs for recycling Pu and MAs in PWRs; (2) Performing a comprehensive systems analysis that compares the fuel cycle characteristics of Pu and MA recycling in PWRs using the promising hydride fuel assembly designs identified in Part 1 versus using oxide fuel assembly designs; (3) Conducting a safety analysis to assess the likelihood of licensing hydride fuel assembly designs; and (4) Assessing the compatibility of hydride fuel with cladding materials and water under typical PWR operating conditions Hydride fuel was found to offer promising transmutation characteristics and is recommended for further examination as a possible preferred option for recycling plutonium in PWRs

  16. Neutron scattering study of the phase transformation of LaNi3 induced by hydriding

    International Nuclear Information System (INIS)

    Ruan Jinghui; Zeng Xiangxin; Niu Shiwen

    1994-01-01

    The phase transformation of LaNi 3 induced by hydriding and de-hydriding is investigated using the neutron diffraction and the neutron inelastic scattering. The results show that the hydriding sample, LaNi 3 H x , is transformed from crystalline state of the LaNi 3 into amorphous state with a microcrystalline characteristic of LaNi 5 , and the de-hydriding sample produced by LaNi 3 H x dehydrated at 600 degree C is decomposed into new crystalline states composed by LaNi 5 -and La-hydrides. The procedure of phase transformation is that the result of the transformation of LaNi 3 induced by hydriding shows the properties of LaNi 5 -H 2 system

  17. FEASIBILITY OF RECYCLING PLUTONIUM AND MINOR ACTINIDES IN LIGHT WATER REACTORS USING HYDRIDE FUEL

    Energy Technology Data Exchange (ETDEWEB)

    Greenspan, Ehud; Todreas, Neil; Taiwo, Temitope

    2009-03-10

    The objective of this DOE NERI program sponsored project was to assess the feasibility of improving the plutonium (Pu) and minor actinide (MA) recycling capabilities of pressurized water reactors (PWRs) by using hydride instead of oxide fuels. There are four general parts to this assessment: 1) Identifying promising hydride fuel assembly designs for recycling Pu and MAs in PWRs 2) Performing a comprehensive systems analysis that compares the fuel cycle characteristics of Pu and MA recycling in PWRs using the promising hydride fuel assembly designs identified in Part 1 versus using oxide fuel assembly designs 3) Conducting a safety analysis to assess the likelihood of licensing hydride fuel assembly designs 4) Assessing the compatibility of hydride fuel with cladding materials and water under typical PWR operating conditions Hydride fuel was found to offer promising transmutation characteristics and is recommended for further examination as a possible preferred option for recycling plutonium in PWRs.

  18. Thermomechanics of hydrogen storage in metallic hydrides: modeling and analysis

    Czech Academy of Sciences Publication Activity Database

    Roubíček, Tomáš; Tomassetti, G.

    2014-01-01

    Roč. 19, č. 7 (2014), s. 2313-2333 ISSN 1531-3492 R&D Projects: GA ČR GA201/09/0917 Institutional support: RVO:61388998 Keywords : metal-hydrid phase transformation * hydrogen diffusion * swelling Subject RIV: BA - General Mathematics Impact factor: 0.768, year: 2014 http://aimsciences.org/journals/pdfs.jsp?paperID=10195&mode=full

  19. Magnetization study of UNiSi and its hydride

    Czech Academy of Sciences Publication Activity Database

    Šebek, Josef; Andreev, Alexander V.; Honda, F.; Kolomiets, A. V.; Havela, L.; Sechovský, V.

    2003-01-01

    Roč. 34, č. 2 (2003), s. 1457-1460 ISSN 0587-4254. [International Conference on Strongly Correlated Electron Systems (SCES 02). Cracow, 10.07.2002-13.07.2002] R&D Projects: GA ČR GA202/02/0739 Institutional research plan: CEZ:AV0Z1010914; CEZ:MSM 113200002 Keywords : UNiSi * magnetic measurements * hydride Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.752, year: 2003

  20. Instrinsic defect energies of lithium hydride and lithium deuteride crystals

    International Nuclear Information System (INIS)

    Pandey, R.; Stoneham, A.M.

    1985-01-01

    A theoretical study has been made of the defect structure of lithium hydride and lithium deuteride. A potential model is obtained describing the statics and dynamics of these crystals. Intrinsic defect energies are calculated using the Harwell HADES program which is based on a generalised Mott-Littleton method. The results are in good agreement with the experimental data, and suggest that the vacancy and interstitial migration mechanisms of anions and cations are all comparable in their contribution to ionic conduction. (author)

  1. Equilibrium dissociation pressures of lithium hydride and lithium deuteride

    International Nuclear Information System (INIS)

    Smith, H.M.; Webb, R.E.

    1977-12-01

    The equilibrium dissociation pressures of plateau composition lithium hydride and lithium deuteride have been measured from 450 to 750 0 C. These data were used to derive the relationship of dissociation pressure with temperature over this range and to calculate several thermodynamic properties of these materials. Thermodynamic properties determined included the enthalpy, entropy, and free energy of formation; the enthalpy and entropy of fusion; and the melting points

  2. Dendritic surface morphology of palladium hydride produced by electrolytic deposition

    International Nuclear Information System (INIS)

    Julin, Peng; Bursill, L.A.

    1990-01-01

    Conventional and high-resolution electron microscopic studies of electrolytically-deposited palladium hydride reveal a fascinating variety of surface profile morphologies. The observations provide direct information concerning the surface structure of palladium electrodes and the mechanism of electrolytic deposition of palladium black. Both classical electrochemical mechanisms and recent 'modified diffusion-limited-aggregation' computer simulations are discussed in comparison with the experimental results. 13 refs., 9 figs

  3. Secondary hydriding of defected zircaloy-clad fuel rods

    International Nuclear Information System (INIS)

    Olander, D.R.; Vaknin, S.

    1993-01-01

    The phenomenon of secondary hydriding in LWR fuel rods is critically reviewed. The current understanding of the process is summarized with emphasis on the sources of hydrogen in the rod provided by chemical reaction of water (steam) introduced via a primary defect in the cladding. As often noted in the literature, the role of hydrogen peroxide produced by steam radiolysis is to provide sources of hydrogen by cladding and fuel oxidation that are absent without fission-fragment irradiation of the gas. Quantitative description of the evolution of the chemical state inside the fuel rod is achieved by combining the chemical kinetics of the reactions between the gas and the fuel and cladding with the transport by diffusion of components of the gas in the gap. The chemistry-gas transport model provides the framework into which therate constants of the reactions between the gases in the gap and the fuel and cladding are incorporated. The output of the model calculation is the H 2 0/H 2 ratio in the gas and the degree of claddingand fuel oxidation as functions of distance from the primary defect. This output, when combined with a criterion for the onset of massive hydriding of the cladding, can provide a prediction of the time and location of a potential secondary hydriding failure. The chemistry-gas transport model is the starting point for mechanical and H-in-Zr migration analyses intended to determine the nature of the cladding failure caused by the development of the massive hydride on the inner wall

  4. Oxidation of Group 8 transition-Metal Hydrides and Ionic Hydrogenation of Ketones and Aldehydes

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Kjell-Tore

    1996-08-01

    Transition-metal hydrides have received considerable attention during the last decades because of their unusual reactivity and their potential as homogeneous catalysts for hydrogenation and other reactions of organic substrates. An important class of catalytic processes where transition-metal hydrides are involved is the homogeneous hydrogenation of alkenes, alkynes, ketones, aldehydes, arenes and nitro compounds. This thesis studies the oxidation of Group 8 transition-metal hydrides and the ionic hydrogenation of ketones and aldehydes.

  5. Powder production of U-Mo alloy, HMD process (Hydriding- Milling- Dehydriding)

    Energy Technology Data Exchange (ETDEWEB)

    Pasqualini, E. E.; Garcia, J.H.; Lopez, M.; Cabanillas, E.; Adelfang, P. [Dept. Combustibles Nucleares. Comision Nacional de Energia Atomica, Av. Gral. Paz 1499, 1650 Buenos Aires (Argentina)

    2002-07-01

    Uranium-molybdenum (U-Mo) alloys can be hydrided massively in metastable {gamma} (gamma) phase. The brittle hydride can be milled and dehydrided to acquire the desired size distributions needed for dispersion nuclear fuels. The developments of the different steps of this process called hydriding-milling- dehydriding (HMD Process) are described. Powder production scales for industrial fabrication is easily achieved with conventional equipment, small man-power and low investment. (author)

  6. Powder production of U-Mo alloy, HMD process (Hydriding- Milling- Dehydriding)

    International Nuclear Information System (INIS)

    Pasqualini, E. E.; Garcia, J.H.; Lopez, M.; Cabanillas, E.; Adelfang, P.

    2002-01-01

    Uranium-molybdenum (U-Mo) alloys can be hydrided massively in metastable γ (gamma) phase. The brittle hydride can be milled and dehydrided to acquire the desired size distributions needed for dispersion nuclear fuels. The developments of the different steps of this process called hydriding-milling- dehydriding (HMD Process) are described. Powder production scales for industrial fabrication is easily achieved with conventional equipment, small man-power and low investment. (author)

  7. First principles characterisation of brittle transgranular fracture of titanium hydrides

    International Nuclear Information System (INIS)

    Olsson, Pär A.T.; Mrovec, Matous; Kroon, Martin

    2016-01-01

    In this work we have studied transgranular cleavage and the fracture toughness of titanium hydrides by means of quantum mechanical calculations based on density functional theory. The calculations show that the surface energy decreases and the unstable stacking fault energy increases with increasing hydrogen content. This is consistent with experimental findings of brittle behaviour of titanium hydrides at low temperatures. Based on Griffith-Irwin theory we estimate the fracture toughness of the hydrides to be of the order of 1 MPa⋅m"1"/"2, which concurs well with experimental data. To investigate the cleavage energetics, we analyse the decohesion at various crystallographic planes and determine the traction-separation laws based on the Rose's extended universal binding energy relation. The calculations predict that the peak stresses do not depend on the hydrogen content of the phases, but it is rather dependent on the crystallographic cleavage direction. However, it is found that the work of fracture decreases with increasing hydrogen content, which is an indication of hydrogen induced bond weakening in the material.

  8. The effect of sample preparation on uranium hydriding

    International Nuclear Information System (INIS)

    Banos, A.; Stitt, C.A.; Scott, T.B.

    2016-01-01

    Highlights: • Distinct differences in uranium hydride growth rates and characteristics between different surface preparation methods. • The primary difference between the categories of sample preparations is the level of strain present in the surface. • Greater surface-strain, leads to higher nucleation number density, implying a preferred attack of strained vs unstrained metal. • As strain is reduced, surface features such as carbides and grain boundaries become more important in controlling the UH3 location. - Abstract: The influence of sample cleaning preparation on the early stages of uranium hydriding has been examined, by using four identical samples but concurrently prepared using four different methods. The samples were reacted together in the same corrosion cell to ensure identical exposure conditions. From the analysis, it was found that the hydride nucleation rate was proportional to the level of strain exhibiting higher number density for the more strained surfaces. Additionally, microstructure of the metal plays a secondary role regarding initial hydrogen attack on the highly strained surfaces yet starts to dominate the system while moving to more pristine samples.

  9. Metal hydride-based thermal energy storage systems

    Science.gov (United States)

    Vajo, John J.; Fang, Zhigang

    2017-10-03

    The invention provides a thermal energy storage system comprising a metal-containing first material with a thermal energy storage density of about 1300 kJ/kg to about 2200 kJ/kg based on hydrogenation; a metal-containing second material with a thermal energy storage density of about 200 kJ/kg to about 1000 kJ/kg based on hydrogenation; and a hydrogen conduit for reversibly transporting hydrogen between the first material and the second material. At a temperature of 20.degree. C. and in 1 hour, at least 90% of the metal is converted to the hydride. At a temperature of 0.degree. C. and in 1 hour, at least 90% of the metal hydride is converted to the metal and hydrogen. The disclosed metal hydride materials have a combination of thermodynamic energy storage densities and kinetic power capabilities that previously have not been demonstrated. This performance enables practical use of thermal energy storage systems for electric vehicle heating and cooling.

  10. 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.

  11. Oxidation kinetics of hydride-bearing uranium metal corrosion products

    Science.gov (United States)

    Totemeier, Terry C.; Pahl, Robert G.; Frank, Steven M.

    The oxidation behavior of hydride-bearing uranium metal corrosion products from Zero Power Physics Reactor (ZPPR) fuel plates was studied using thermo-gravimetric analysis (TGA) in environments of Ar-4%O 2, Ar-9%O 2, and Ar-20%O 2. Ignition of corrosion product samples from two moderately corroded plates was observed between 125°C and 150°C in all environments. The rate of oxidation above the ignition temperature was found to be dependent only on the net flow rate of oxygen in the reacting gas. Due to the higher net oxygen flow rate, burning rates increased with increasing oxygen concentration. Oxidation rates below the ignition temperature were much slower and decreased with increasing test time. The hydride contents of the TGA samples from the two moderately corroded plates, determined from the total weight gain achieved during burning, were 47-61 wt% and 29-39 wt%. Samples from a lightly corroded plate were not reactive; X-ray diffraction (XRD) confirmed that they contained little hydride.

  12. Oxidation kinetics of hydride-bearing uranium metal corrosion products

    International Nuclear Information System (INIS)

    Totemeier, T.C.; Pahl, R.G.; Frank, S.M.

    1998-01-01

    The oxidation behavior of hydride-bearing uranium metal corrosion products from zero power physics reactor (ZPPR) fuel plates was studied using thermo-gravimetric analysis (TGA) in environments of Ar-4%O 2 , Ar-9%O 2 , and Ar-20%O 2 . Ignition of corrosion product samples from two moderately corroded plates was observed between 125 C and 150 C in all environments. The rate of oxidation above the ignition temperature was found to be dependent only on the net flow rate of oxygen in the reacting gas. Due to the higher net oxygen flow rate, burning rates increased with increasing oxygen concentration. Oxidation rates below the ignition temperature were much slower and decreased with increasing test time. The hydride contents of the TGA samples from the two moderately corroded plates, determined from the total weight gain achieved during burning, were 47-61 wt% and 29-39 wt%. Samples from a lightly corroded plate were not reactive; X-ray diffraction (XRD) confirmed that they contained little hydride. (orig.)

  13. 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)

  14. Study on the effects of titanium oxide based nanomaterials as catalysts on the hydrogen sorption kinetics of magnesium hydride

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Anderson de Farias; Jardim, Paula Mendes; Santos, Dilson Silva dos, E-mail: anderso.n@poli.ufrj.br [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil); Conceicao, Monique Osorio Talarico da [Centro Universitario de Volta Redonda (UniFOA), RJ (Brazil)

    2016-07-01

    Full text: Magnesium hydride is highly attractive for hydrogen storage in solid state in reason of its high gravimetric capacity (7,6 wt% of H{sub 2}) and low density (1,7 g/cm³), making it a promissory candidate for mobile applications [1]. However, its low sorption kinetics and desorption temperature are the main obstacles for its application. In the present study the catalytic role of TiO{sub 2} based nanomaterials with different morphologies on the sorption kinetics of MgH{sub 2} was evaluated. The additions consisted on titanate nanotubes (TTNT-Low), TiO{sub 2} nanorods (TTNT-550) and nanoparticles (KA-100, TTNT-ACID). Transmission and Scanning Transmission Electron Microscopy (S/TEM) associated with X-ray Energy Dispersive Spectroscopy (XEDS) mapping was used to characterize the catalysts' morphology and crystalline structure and their dispersion within magnesium hydride, altogether with other characterization techniques such as X-ray diffraction (XRD) and BET technique for structure and surface area analysis. The sorption kinetics were evaluated by means of a volumetric gas absorption/desorption (Sievert-type) apparatus. The results indicated that all additives improved the sorption kinetics of MgH{sub 2}, but the samples with TTNT-550 (TiO{sub 2} nanorods) and TTNT-ACID (TiO{sub 2} nanoparticles) presented the best and the second best performances, respectively, suggesting that the 1D morphology may promote a slightly superior kinetics than particulate catalysts. (author)

  15. 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.

  16. Some new techniques in tritium gas handling as applied to metal hydride synthesis

    International Nuclear Information System (INIS)

    Nasise, J.E.

    1988-01-01

    A state-of-the-art tritium Hydriding Synthesis System (HSS) was designed and built to replace the existing system within the Tritium Salt Facility (TSF) at the Los Alamos National Laboratory. This new hydriding system utilizes unique fast-cycling 7.9 mole uranium beds (47.5g of T at 100% loading) and novel gas circulating hydriding furnaces. Tritium system components discussed include fast-cycling uranium beds, circulating gas hydriding furnaces, valves, storage volumes, manifolds, gas transfer pumps, and graphic display and control consoles. Many of the tritium handling and processing techniques incorporated into this system are directly applicable to today's fusion fuel loops. 12 refs., 7 figs

  17. Effect of the hydrogen content and cooling velocity in the hydrides precipitation in α-zirconium

    International Nuclear Information System (INIS)

    Ramanathan, L.V.

    1983-01-01

    Zirconium specimens containing 50-300 ppm hydrogen have been cooled from the hydrogen solution treatment temperature at different rates by furnace cooling, air cooling and oil quenching. Optical and electron microscopical investigations have revealed grain boundary Δ - hydrides in slowly cooled specimens. At higher cooling rates γ and Δ hydrides have been found precipitated both intergranularly and intragranularly. Grain boundary Δ hydrides have been also observed in oil quenched specimens with 300 ppm hydrogen. Quenched specimens have revealed Widmanstatten and parallel plate type hydride morphologies. (Author) [pt

  18. Zirconium hydrides and Fe redistribution in Zr-2.5%Nb alloy under ion irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Idrees, Y.; Yao, Z. [Department of Mechanical and Materials Engineering, Queen' s University, Kingston, ON, Canada, K7L 3N6 (Canada); Cui, J.; Shek, G.K. [Kinetrics, Mississauga, ON (Canada); Daymond, M.R., E-mail: daymond@queensu.ca [Department of Mechanical and Materials Engineering, Queen' s University, Kingston, ON, Canada, K7L 3N6 (Canada)

    2016-11-15

    Zr-2.5%Nb alloy is used to fabricate the pressure tubes of the CANDU reactor. The pressure tube is the primary pressure boundary for coolant in the CANDU design and is susceptible to delayed hydride cracking, reduction in fracture toughness upon hydride precipitation and potentially hydride blister formation. The morphology and nature of hydrides in Zr-2.5%Nb with 100 wppm hydrogen has been investigated using transmission electron microscopy. The effect of hydrides on heavy ion irradiation induced decomposition of the β phase has been reported. STEM-EDX mapping was employed to investigate the distribution of alloying elements. The results show that hydrides are present in the form of stacks of different sizes, with length scales from nano- to micro-meters. Heavy ion irradiation experiments at 250 °C on as-received and hydrided Zr-2.5%Nb alloy, show interesting effects of hydrogen on the irradiation induced redistribution of Fe. It was found that Fe is widely redistributed from the β phase into the α phase in the as-received material, however, the loss of Fe from the β phase and subsequent precipitation is retarded in the hydrided material. This preliminary work will further the current understanding of microstructural evolution of Zr based alloys in the presence of hydrogen. - Graphical abstract: STEM HAADF micrographs at low magnification showing the hydride structure in Zr-2.5Nb alloy.

  19. Materials performance in prototype Thermal Cycling Absorption Process (TCAP) columns

    International Nuclear Information System (INIS)

    Clark, E.A.

    1992-01-01

    Two prototype Thermal Cycling Absorption Process (TCAP) columns have been metallurgically examined after retirement, to determine the causes of failure and to evaluate the performance of the column container materials in this application. Leaking of the fluid heating and cooling subsystems caused retirement of both TCAP columns, not leaking of the main hydrogen-containing column. The aluminum block design TCAP column (AHL block TCAP) used in the Advanced Hydride Laboratory, Building 773-A, failed in one nitrogen inlet tube that was crimped during fabrication, which lead to fatigue crack growth in the tube and subsequent leaking of nitrogen from this tube. The Third Generation stainless steel design TCAP column (Third generation TCAP), operated in 773-A room C-061, failed in a braze joint between the freon heating and cooling tubes (made of copper) and the main stainless steel column. In both cases, stresses from thermal cycling and local constraint likely caused the nucleation and growth of fatigue cracks. No materials compatibility problems between palladium coated kieselguhr (the material contained in the TCAP column) and either aluminum or stainless steel column materials were observed. The aluminum-stainless steel transition junction appeared to be unaffected by service in the AHL block TCAP. Also, no evidence of cracking was observed in the AHL block TCAP in a location expected to experience the highest thermal shock fatigue in this design. It is important to limit thermal stresses caused by constraint in hydride systems designed to work by temperature variation, such as hydride storage beds and TCAP columns

  20. Hydrogen storage and evolution catalysed by metal hydride complexes.

    Science.gov (United States)

    Fukuzumi, Shunichi; Suenobu, Tomoyoshi

    2013-01-07

    The storage and evolution of hydrogen are catalysed by appropriate metal hydride complexes. Hydrogenation of carbon dioxide by hydrogen is catalysed by a [C,N] cyclometalated organoiridium complex, [Ir(III)(Cp*)(4-(1H-pyrazol-1-yl-κN(2))benzoic acid-κC(3))(OH(2))](2)SO(4) [Ir-OH(2)](2)SO(4), under atmospheric pressure of H(2) and CO(2) in weakly basic water (pH 7.5) at room temperature. The reverse reaction, i.e., hydrogen evolution from formate, is also catalysed by [Ir-OH(2)](+) in acidic water (pH 2.8) at room temperature. Thus, interconversion between hydrogen and formic acid in water at ambient temperature and pressure has been achieved by using [Ir-OH(2)](+) as an efficient catalyst in both directions depending on pH. The Ir complex [Ir-OH(2)](+) also catalyses regioselective hydrogenation of the oxidised form of β-nicotinamide adenine dinucleotide (NAD(+)) to produce the 1,4-reduced form (NADH) under atmospheric pressure of H(2) at room temperature in weakly basic water. In weakly acidic water, the complex [Ir-OH(2)](+) also catalyses the reverse reaction, i.e., hydrogen evolution from NADH to produce NAD(+) at room temperature. Thus, interconversion between NADH (and H(+)) and NAD(+) (and H(2)) has also been achieved by using [Ir-OH(2)](+) as an efficient catalyst and by changing pH. The iridium hydride complex formed by the reduction of [Ir-OH(2)](+) by H(2) and NADH is responsible for the hydrogen evolution. Photoirradiation (λ > 330 nm) of an aqueous solution of the Ir-hydride complex produced by the reduction of [Ir-OH(2)](+) with alcohols resulted in the quantitative conversion to a unique [C,C] cyclometalated Ir-hydride complex, which can catalyse hydrogen evolution from alcohols in a basic aqueous solution (pH 11.9). The catalytic mechanisms of the hydrogen storage and evolution are discussed by focusing on the reactivity of Ir-hydride complexes.

  1. 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

  2. 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.

  3. Determination of essential and heavy metals in Kenyan honey by ...

    African Journals Online (AJOL)

    The samples were analysed using flame atomic absorption spectroscopy (FAAS) and flame atomic emission spectroscopy (FAES). Hydride generation -atomic absorption spectroscopy (HG - AAS) was used to determine arsenic. Results obtained from this study showed that K, Na, Ca and Mg had mean values ranged from ...

  4. 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)

  5. 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.

  6. Temperature dependence of InN growth on (0001) sapphire substrates by atmospheric pressure hydride vapor phase epitaxy

    International Nuclear Information System (INIS)

    Kumagai, Yoshinao; Adachi, Hirokazu; Otake, Aya; Higashikawa, Yoshihiro; Togashi, Rie; Murakami, Hisashi; Koukitu, Akinori

    2010-01-01

    The temperature dependence of InN growth on (0001) sapphire substrates by atmospheric pressure hydride vapor phase epitaxy (HVPE) was investigated. N-polarity single-crystal InN layers were successfully grown at temperatures ranging from 400 to 500 C. The a and c lattice constants of InN layers grown at 450 C or below were slightly larger than those of InN layers grown above 450 C due to oxygen incorporation that also increased the carrier concentration. The optical absorption edge of the InN layer decreased from above 2.0 to 0.76 eV when the growth temperature was increased from 450 to 500 C. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

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

    KAUST Repository

    Saggio, Guillaume; Taoufik, Mostafa; Basset, Jean-Marie; Thivolle-Cazat, Jean

    2010-01-01

    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

  8. Preconcentration and in-situ photoreduction of trace selenium using TiO2 nanoparticles, followed by its determination by slurry photochemical vapor generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Yang, Wulin; Wu, Li; Zhu, Xiaofan; Gao, Ying; Hou, Xiandeng; Zheng, Chengbin

    2014-01-01

    We have developed a method for the determination of trace levels of total selenium in water samples. It integrates preconcentration, in-situ photoreduction and slurry photochemical vapor generation using TiO 2 nanoparticles, and the determination of total selenium by AFS. The Se(IV) and Se(VI) species were adsorbed on a slurry of TiO 2 nanoparticles which then were exposed to UV irradiation in the presence of formic acid to form volatile selenium species. The detection limits were improved 17-fold compared to hydride generation and 56-fold compared to photochemical vapor generation, both without any preconcentration. No significant difference was found in the limits of detection (LODs) for Se(IV) and Se(VI). The LOD is as low as 0.8 ng L −1 , the precision is better than 4.5 % (at a level of 0.1 μg L −1 of selenium). The method gave good recoveries when applied to the determination of total selenium in a certified tissue reference material (DORM-3) and in spiked drinking water and wastewater samples containing high concentrations of transition and noble metal ions. It also excels by very low LODs, a significant enhancement of sample throughput, reduced reagent consumption and sample loss, and minimal interference by transition and noble metal ions. (author)

  9. Combined on-board hydride slurry storage and reactor system and process for hydrogen-powered vehicles and devices

    Science.gov (United States)

    Brooks, Kriston P; Holladay, Jamelyn D; Simmons, Kevin L; Herling, Darrell R

    2014-11-18

    An on-board hydride storage system and process are described. The system includes a slurry storage system that includes a slurry reactor and a variable concentration slurry. In one preferred configuration, the storage system stores a slurry containing a hydride storage material in a carrier fluid at a first concentration of hydride solids. The slurry reactor receives the slurry containing a second concentration of the hydride storage material and releases hydrogen as a fuel to hydrogen-power devices and vehicles.

  10. Recent advances in improving performances of the lightweight complex hydrides Li-Mg-N-H system

    Directory of Open Access Journals (Sweden)

    Bao Zhang

    2017-02-01

    Full Text Available A brief review of state-of-the art advances in improving performances of the lightweight complex hydrides Li-Mg-N-H system is reported. Among the hydrogen storage materials, Li-Mg-N-H combination systems are regarded as one of the most potential candidates for the vehicular applications owing to their high hydrogen storage capacity (>5 wt% H and a more appropriate thermodynamic properties of hydrogen absorption and desorption. In the Li-Mg-N-H systems, tremendous efforts have been devoted to improving the hydrogen storage properties by adjusting composition, revealing reaction mechanisms, adding catalysts and refining the microstructures, etc. During the studies, different mechanisms, such as the coordinated two-molecule or multimolecule reaction mechanism and the ammonia-mediated mechanism, are proposed and applied under some certain conditions. Catalysis and nanosizing are very effective in enhancing the kinetic properties and thermodynamic destabilization of Li-Mg-N-H systems. Due to nano effects, the space-confinement and nanoconfinement seems to be more effective for improving the hydrogen storage performance, and it is great significant to develop hydrogen storage materials by studying the nanoconfined effects on the Li-Mg-N-H systems.

  11. 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

  12. Exceptional Lithium Storage in a Co(OH) 2 Anode: Hydride Formation

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hyunchul; Choi, Woon Ih [Samsung Advanced Institute of Technology, Samsung Electronics, 130 Samsung-ro, Suwon 16678, South Korea; Jang, Yoonjung; Balasubramanian, Mahalingam [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439, United States; Lee, Wontae; Park, Gwi Ok; Park, Su Bin; Yoo, Jaeseung; Hong, Jin Seok [Samsung Advanced Institute of Technology, Samsung Electronics, 130 Samsung-ro, Suwon 16678, South Korea; Choi, Youn-Suk [Samsung Advanced Institute of Technology, Samsung Electronics, 130 Samsung-ro, Suwon 16678, South Korea; Lee, Hyo Sug [Samsung Advanced Institute of Technology, Samsung Electronics, 130 Samsung-ro, Suwon 16678, South Korea; Bae, In Tae; Kim, Ji Man; Yoon, Won-Sub

    2018-02-26

    Current lithium ion battery technology is tied in with conventional reaction mechanisms such as insertion, conversion, and alloying reactions even though most future applications like EVs demand much higher energy densities than current ones. Exploring the exceptional reaction mechanism and related electrode materials can be critical for pushing current battery technology to a next level. Here, we introduce an exceptional reaction with a Co(OH)(2) material which exhibits an initial charge capacity of 1112 mAh g(-1), about twice its theoretical value based on known conventional conversion reaction, and retains its first cycle capacity after 30 cycles. The combined results of synchrotron X-ray diffraction and X-ray absorption spectroscopy indicate that nanosized Co metal particles and LiOH are generated by conversion reaction at high voltages, and CoxHy, Li2O, and LiH are subsequently formed by hydride reaction between Co metal, LiOH, and other lithium species at low voltages, resulting in a anomalously high capacity beyond the theoretical capacity of Co(OH)(2). This is further corroborated by AIMD simulations, localized STEM, and XPS. These findings will provide not only further understanding of exceptional lithium storage of recent nanostructured materials but also valuable guidance to develop advanced electrode materials with high energy density for next-generation batteries.

  13. Electronic band structure and optical properties of the cubic, Sc, Y and La hydride systems

    International Nuclear Information System (INIS)

    Peterman, D.J.

    1980-01-01

    Electronic band structure calculations are used to interpret the optical spectra of the cubic Sc, Y and La hydride systems. Self-consistent band calculations of ScH 2 and YH 2 were carried out. The respective joint densities of states are computed and compared to the dielectric functions determined from the optical measurements. Additional calculations were performed in which the Fermi level or band gap energies are rigidly shifted by a small energy increment. These calculations are then used to simulate the derivative structure in thermomodulation spectra and relate the origin of experimental interband features to the calculated energy bands. While good systematic agreement is obtained for several spectral features, the origin of low-energy interband transitions in YH 2 cannot be explained by these calculated bands. A lattice-size-dependent premature occupation of octahedral sites by hydrogen atoms in the fcc metal lattice is suggested to account for this discrepancy. Various non-self-consistent calculations are used to examine the effect of such a premature occupation. Measurements of the optical absorptivity of LaH/sub x/ with 1.6 2 lattice. These experimental results also suggest that, in contrast to recent calculations, LaH 3 is a small-band-gap semiconductor

  14. 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

  15. Pore-Confined Light Metal Hydrides for Energy Storage and Catalysis

    NARCIS (Netherlands)

    Bramwell, P.L.|info:eu-repo/dai/nl/371685117

    2017-01-01

    Light metal hydrides have enjoyed several decades of attention in the field of hydrogen storage, but their applications have recently begun to diversify more and more into the broader field of energy storage. For example, light metal hydrides have shown great promise as battery materials, in sensors

  16. 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)

  17. Speculations on the existence of hydride ions in proton conducting oxides

    DEFF Research Database (Denmark)

    Poulsen, F.W.

    2001-01-01

    The chemical and physical nature of the hydride ion is briefly treated. Several reactions of the hydride ion in oxides or oxygen atmosphere are given, A number of perovskites and inverse perovskites are listed. which contain the H- ion on the oxygen or B-anion sites in the archetype ABO(3) System...

  18. 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)

  19. Hydrogen storage material and process using graphite additive with metal-doped complex hydrides

    Science.gov (United States)

    Zidan, Ragaiy [Aiken, SC; Ritter, James A [Lexington, SC; Ebner, Armin D [Lexington, SC; Wang, Jun [Columbia, SC; Holland, Charles E [Cayce, SC

    2008-06-10

    A hydrogen storage material having improved hydrogen absorbtion and desorption kinetics is provided by adding graphite to a complex hydride such as a metal-doped alanate, i.e., NaAlH.sub.4. The incorporation of graphite into the complex hydride significantly enhances the rate of hydrogen absorbtion and desorption and lowers the desorption temperature needed to release stored hydrogen.

  20. Hydride-induced degradation of hoop ductility in textured zirconium-alloy tubes: A theoretical analysis

    International Nuclear Information System (INIS)

    Qin, W.; Szpunar, J.A.; Kozinski, J.

    2012-01-01

    Hydride-induced degradation of hoop ductility in Zr-alloy tubular components has been studied for many years because of its importance in the nuclear industry. In this paper the role of intergranular and intragranular δ-hydrides in the degradation of ductility of the textured Zr-alloy tubes is investigated. The correlation among hydride distribution, orientation and morphology in the tubes is formulated based on thermodynamic modeling, and then analyzed. The results show that the applied stress, the crystallographic texture of α-Zr matrix, the grain-boundary structure, and the morphology and size of Zr grains simultaneously govern the site preference and the orientation of hydrides. A criterion is proposed to determine the threshold stress of hydride reorientation. The hoop ductility of the hydrided Zr tubes is discussed using the concept of macroscopic fracture strain. It is shown that the intergranular hydrides may be more deleterious to ductility than the intragranular ones. This work defines a general framework for understanding the relation of the microstructure of hydride-forming materials to embrittlement.

  1. 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

  2. Thermodynamic and kinetics models of hydrogen absorption bound to phase transformations

    International Nuclear Information System (INIS)

    Gondor, G.; Lexcellent, Ch.

    2007-01-01

    In order to design hydrogen gaseous pressure tanks, the absorption (desorption) of hydrogen has to be described and modelled. The equilibrium state can be described by the 'H 2 gas pressure - H 2 composition in the intermetallic compounds - isotherms' (PCI) curves. Several models of PCI curves already exist. At the beginning of the absorption, the hydrogen atoms and the intermetallic compounds form a solid solution (α phase). When the hydrogen concentration increases, a phase transformation appears changing the α solid solution into an hydride (β phase) (solid solution + H 2 ↔ hydride). When all the solid solution has been transformed into hydride, the absorbed hydrogen atoms are in β phase. A new thermodynamic model has been developed in order to take into account this transition phase. The equilibrium state is then given by a relation between the H 2 gas pressure and the H 2 concentration in the intermetallic compound for a fixed external temperature. Two kinetics models have been developed too; at first has been considered that the kinetics depend only of the entire concentration in the intermetallic compound and of the difference between the applied pressure and the equilibrium pressure. Then, has been considered that the hydrogen concentration changes in the metallic matrix. In this last case, for each hydrogenation process, the absorption velocity is calculated to determine the slowest local process which regulates the local evolution of the hydrogen concentration. These two models are based on the preceding thermodynamic model of the PCI curves. (O.M.)

  3. Searching out the hydrogen absorption/desorption limiting reaction factors: Strategies allowing to increase kinetics

    Energy Technology Data Exchange (ETDEWEB)

    Zeaiter, Ali, E-mail: ali.zeaiter@femto-st.fr; Chapelle, David; Nardin, Philippe

    2015-10-05

    Highlights: • A macro scale thermodynamic model that simulates the response of a FeTi-X hydride tank is performed, and validated experimentally. • A sensibility study to identify the most influent input variables that can changes very largely the reaction rate. - Abstract: Hydrogen gas has become one of the most promising energy carriers. Main breakthrough concerns hydrogen solid storage, specially based on intermetallic material use. Regarding the raw material abundance and cost, the AB type alloy FeTi is an auspicious candidate to store hydrogen. Its absorption/desorption kinetics is a basic hindrance to common use, compared with more usual hydrides. First, discussions based on literature help us identifying the successive steps leading to metal hydriding, and allow to introduce the physical parameters which drive or limit the reaction. This analysis leads us to suggest strategies in order to increase absorption/desorption kinetics. Attention is then paid to a thermofluidodynamic model, allowing to describe a macroscopic solid storage reactor. Thus, we can achieve a simulation which describes the overall reaction inside the hydrogen reactor and, by varying the sub-mentioned parameters (thermal conductivity, the powder granularity, environment heat exchange…), we attempt to hierarchy the reaction limiting factors. These simulations are correlated to absorption/desorption experiments for which pressure, temperature and hydrogen flow are recorded.

  4. 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.

  5. Mathematical modeling of the nickel/metal hydride battery system

    Energy Technology Data Exchange (ETDEWEB)

    Paxton, Blaine Kermit [Univ. of California, Berkeley, CA (United States). Dept. of Chemical Engineering

    1995-09-01

    A group of compounds referred to as metal hydrides, when used as electrode materials, is a less toxic alternative to the cadmium hydroxide electrode found in nickel/cadmium secondary battery systems. For this and other reasons, the nickel/metal hydride battery system is becoming a popular rechargeable battery for electric vehicle and consumer electronics applications. A model of this battery system is presented. Specifically the metal hydride material, LaNi{sub 5}H{sub 6}, is chosen for investigation due to the wealth of information available in the literature on this compound. The model results are compared to experiments found in the literature. Fundamental analyses as well as engineering optimizations are performed from the results of the battery model. In order to examine diffusion limitations in the nickel oxide electrode, a ``pseudo 2-D model`` is developed. This model allows for the theoretical examination of the effects of a diffusion coefficient that is a function of the state of charge of the active material. It is found using present data from the literature that diffusion in the solid phase is usually not an important limitation in the nickel oxide electrode. This finding is contrary to the conclusions reached by other authors. Although diffusion in the nickel oxide active material is treated rigorously with the pseudo 2-D model, a general methodology is presented for determining the best constant diffusion coefficient to use in a standard one-dimensional battery model. The diffusion coefficients determined by this method are shown to be able to partially capture the behavior that results from a diffusion coefficient that varies with the state of charge of the active material.

  6. Single-Site Tetracoordinated Aluminum Hydride Supported on Mesoporous Silica. From Dream to Reality!

    KAUST Repository

    Werghi, Baraa

    2016-09-26

    The reaction of mesoporous silica (SBA15) dehydroxylated at 700 °C with diisobutylaluminum hydride, i-Bu2AlH, gives after thermal treatment a single-site tetrahedral aluminum hydride with high selectivity. The starting aluminum isobutyl and the final aluminum hydride have been fully characterized by FT-IR, advanced SS NMR spectroscopy (1H, 13C, multiple quanta (MQ) 2D 1H-1H, and 27Al), and elemental analysis, while DFT calculations provide a rationalization of the occurring reactivity. Trimeric i-Bu2AlH reacts selectively with surface silanols without affecting the siloxane bridges. Its analogous hydride catalyzes ethylene polymerization. Indeed, catalytic tests show that this single aluminum hydride site is active in the production of a high-density polyethylene (HDPE). © 2016 American Chemical Society.

  7. 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

  8. Single-Site Tetracoordinated Aluminum Hydride Supported on Mesoporous Silica. From Dream to Reality!

    KAUST Repository

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

    2016-01-01

    The reaction of mesoporous silica (SBA15) dehydroxylated at 700 °C with diisobutylaluminum hydride, i-Bu2AlH, gives after thermal treatment a single-site tetrahedral aluminum hydride with high selectivity. The starting aluminum isobutyl and the final aluminum hydride have been fully characterized by FT-IR, advanced SS NMR spectroscopy (1H, 13C, multiple quanta (MQ) 2D 1H-1H, and 27Al), and elemental analysis, while DFT calculations provide a rationalization of the occurring reactivity. Trimeric i-Bu2AlH reacts selectively with surface silanols without affecting the siloxane bridges. Its analogous hydride catalyzes ethylene polymerization. Indeed, catalytic tests show that this single aluminum hydride site is active in the production of a high-density polyethylene (HDPE). © 2016 American Chemical Society.

  9. The status and immediate problems of the chemistry of transition metal hydrides

    International Nuclear Information System (INIS)

    Meikheeva, V.I.

    1978-01-01

    The state of the art and perspectives of the chemistry transition metal hydrides are reviewed, the hydrides being essentially compounds with interstitial hydrogen in the crystal lattice of the metals. The possibilities of hydrogenation of transition metals are considered along with that of compounds of rare earth elements with metals of the iron family. It is shown that the products of hydrogenation of many alloys are unstable and disintegrate forming simpler hydrides. The phase diagram of La-Ni-H system resembles the isotherm of a ternary metal system with the difference that no continuous series of solid solutions is formed. Most hydrogenation products across LaHsub(2-3)-NiH are X-ray amorphous. The nature of hydrogen in hydrides is discussed along with the possibilities of synthesis of new hydrides of transition metals

  10. 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

  11. Another Look at the Mechanisms of Hydride Transfer Enzymes with Quantum and Classical Transition Path Sampling.

    Science.gov (United States)

    Dzierlenga, Michael W; Antoniou, Dimitri; Schwartz, Steven D

    2015-04-02

    The mechanisms involved in enzymatic hydride transfer have been studied for years, but questions remain due, in part, to the difficulty of probing the effects of protein motion and hydrogen tunneling. In this study, we use transition path sampling (TPS) with normal mode centroid molecular dynamics (CMD) to calculate the barrier to hydride transfer in yeast alcohol dehydrogenase (YADH) and human heart lactate dehydrogenase (LDH). Calculation of the work applied to the hydride allowed for observation of the change in barrier height upon inclusion of quantum dynamics. Similar calculations were performed using deuterium as the transferring particle in order to approximate kinetic isotope effects (KIEs). The change in barrier height in YADH is indicative of a zero-point energy (ZPE) contribution and is evidence that catalysis occurs via a protein compression that mediates a near-barrierless hydride transfer. Calculation of the KIE using the difference in barrier height between the hydride and deuteride agreed well with experimental results.

  12. 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)

  13. 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

  14. 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.

  15. 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

  16. Prevention of delayed hydride cracking in zirconium alloys

    International Nuclear Information System (INIS)

    Cheadle, B.A.; Coleman, C.E.; Ambler, J.F.R.

    1987-01-01

    Zirconium alloys are susceptible to a mechanism for crack initiation and propagation called delayed hydride cracking. From a review of component failures and experimental results, we have developed the requirements for preventing this cracking. The important parameters for cracking are hydrogen concentration, flaws, and stress; each should be minimized. At the design and construction stages hydrogen pickup has to be controlled, quality assurance needs to be at a high enough level to ensure the absence of flaws, and residual stresses must be eliminated by careful fabrication and heat treatment

  17. Hydrogen isotope exchange in a metal hydride tube

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, David B. [Sandia National Lab. (SNL-CA), Livermore, CA (United States)

    2014-09-01

    This report describes a model of the displacement of one hydrogen isotope within a metal hydride tube by a different isotope in the gas phase that is blown through the tube. The model incorporates only the most basic parameters to make a clear connection to the theory of open-tube gas chromatography, and to provide a simple description of how the behavior of the system scales with controllable parameters such as gas velocity and tube radius. A single tube can be seen as a building block for more complex architectures that provide higher molar flow rates or other advanced design goals.

  18. Modification of the hydriding of uranium using ion implantation

    International Nuclear Information System (INIS)

    Musket, R.G.; Robinson-Weis, G.; Patterson, R.G.

    1983-01-01

    The hydriding of depleted uranium at 76 Torr hydrogen and 130 0 C has been significantly reduced by implantation of oxygen ions. The high-dose implanted specimens had incubation times for the initiation of the reaction after exposure to hydrogen that exceeded those of the nonimplanted specimens by more than a factor of eight. Furthermore, the nonimplanted specimens consumed enough hydrogen to cause macroscopic flaking of essentially the entire surface in times much less than the incubation time for the high-dose implanted specimens. In contrast, the ion-implanted specimens reacted only at isolated spots with the major fraction of the surface area unaffected by the hydrogen exposure

  19. Research in Nickel/Metal Hydride Batteries 2016

    Directory of Open Access Journals (Sweden)

    Kwo-Hsiung Young

    2016-10-01

    Full Text Available Nineteen papers focusing on recent research investigations in the field of nickel/metal hydride (Ni/MH batteries have been selected for this Special Issue of Batteries. These papers summarize the joint efforts in Ni/MH battery research from BASF, Wayne State University, the National Institute of Standards and Technology, Michigan State University, and FDK during 2015–2016 through reviews of basic operational concepts, previous academic publications, issued US Patent and filed Japan Patent Applications, descriptions of current research results in advanced components and cell constructions, and projections of future works.

  20. Equilibrium composition for the reaction of plutonium hydride with air

    International Nuclear Information System (INIS)

    Zou Lexi; Sun Ying; Xue Weidong; Zhu Zhenghe; Wang Rong; Luo Deli

    2002-01-01

    There are six independent constituents with 4 chemical elements, i.e. PuH 2.7 (s), PuN(s), Pu 2 O 3 (s), N 2 , O 2 and H 2 , therefore, the system described involves of 2 independent reactions, both ΔG 0 <<0. The calculated equilibrium compositions are in agreement with those of the experimental, which indicates that the chemical equilibrium is nearly completely approached. Therefore, it is believed that the reaction rate of plutonium hydride with air is extremely rapid. The author has briefly discussed the simultaneous reactions and its thermodynamic coupling effect

  1. Hydrogen storage properties of carbon nanomaterials and carbon containing metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Maehlen, Jan Petter

    2003-07-01

    The topic of this thesis is structural investigations of carbon containing materials in respect to their hydrogen storage properties. This work was initially triggered by reports of extremely high hydrogen storage capacities of specific carbon nanostructures. It was decided to try to verify and understand the mechanisms in play in case of the existence of such high hydrogen densities in carbon. Two different routes towards the goal were employed; by studying selected hydrides with carbon as one of its constituents (mainly employing powder diffraction techniques in combination with hydrogen absorption and desorption measurements) and by carefully conducting hydrogen sorption experiments on what was believed to be the most ''promising'' carbon nanomaterial sample. In the latter case, a lot of effort was attributed to characterisations of different carbon nanomaterial containing samples with the aid of electron microscopy. Three different carbon-containing metal hydride systems, Y2C-H, YCoC-H and Y5SiC0.2-H, were examined. A relation between hydrogen occupation and the local arrangement of metal and carbon atoms surrounding the hydrogen sites was established. Several characteristic features of the compounds were noted in addition to solving the structure of the former unknown deuterideY5Si3C0.2D2.0 by the use of direct methods. Several carbon-nanomaterial containing samples were studied by means of transmission electron microscopy and powder diffraction, thus gaining knowledge concerning the structural aspects of nanomaterials. Based on these investigations, a specific sample containing a large amount of open-ended single-wall carbon nanotubes was chosen for subsequent hydrogen storage experiments. The latter experiments revealed moderate hydrogen storage capacities of the nanotubes not exceeding the values obtained for more conventional forms of carbon. These two different routes in investigating the hydrogen storage properties of carbon and carbon containing alloys

  2. Hydrogen storage properties of carbon nanomaterials and carbon containing metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Maehlen, Jan Petter

    2003-07-01

    The topic of this thesis is structural investigations of carbon containing materials in respect to their hydrogen storage properties. This work was initially triggered by reports of extremely high hydrogen storage capacities of specific carbon nanostructures. It was decided to try to verify and understand the mechanisms in play in case of the existence of such high hydrogen densities in carbon. Two different routes towards the goal were employed; by studying selected hydrides with carbon as one of its constituents (mainly employing powder diffraction techniques in combination with hydrogen absorption and desorption measurements) and by carefully conducting hydrogen sorption experiments on what was believed to be the most ''promising'' carbon nanomaterial sample. In the latter case, a lot of effort was attributed to characterisations of different carbon nanomaterial containing samples with the aid of electron microscopy. Three different carbon-containing metal hydride systems, Y2C-H, YCoC-H and Y5SiC0.2-H, were examined. A relation between hydrogen occupation and the local arrangement of metal and carbon atoms surrounding the hydrogen sites was established. Several characteristic features of the compounds were noted in addition to solving the structure of the former unknown deuterideY5Si3C0.2D2.0 by the use of direct methods. Several carbon-nanomaterial containing samples were studied by means of transmission electron microscopy and powder diffraction, thus gaining knowledge concerning the structural aspects of nanomaterials. Based on these investigations, a specific sample containing a large amount of open-ended single-wall carbon nanotubes was chosen for subsequent hydrogen storage experiments. The latter experiments revealed moderate hydrogen storage capacities of the nanotubes not exceeding the values obtained for more conventional forms of carbon. These two different routes in investigating the hydrogen storage properties of carbon and

  3. Delayed hydride cracking behavior for zircaloy-2 plate

    International Nuclear Information System (INIS)

    Mills, J.W.; Huang, F.H.

    1991-01-01

    The delayed hydride cracking (DHC) behaviour for Zircaloy-2 plate was characterized at temperatures ranging from 300 to 550 o F. Specimens with a longitudinal (T-L) orientation exhibited a classic two-stage DHC response. At K values slightly above the threshold level (K th ), crack-growth rates increased dramatically with increasing K values (stage I). The K th value was found to be 11 and 14 ksi√ in at 400 and 500 o F. At high K values (stage II), cracking rates were relatively insensitive to applied K levels. Stage II crack growth was a thermally activated process described by an Arrhenius-type relationship with an activation energy of 65 kJ/mol. This energy level agreed with the theoretical activation energy for hydrogen diffusion into the triaxial stress field ahead of a crack. Above a critical temperature (300 o F), an overtemperature cycle was required to initiate DHC. The magnitude of the thermal excursion required to initiate cracking was found to increase at higher test temperatures. Specimens with a transverse(L-T) orientation showed a very low sensitivity to DHC because of an unfavorable crystallographic orientation for hydride reorientation. Metallographic and fractographic examinations were performed to understand the DHC mechanism. (author)

  4. Production of hydrogen gas from novel chemical hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Aiello, R.; Matthews, M.A. [South Carolina Univ., Chemical Engineering Dept., Columbia, SC (United States); Reger, D.L.; Collins, J.E. [South Carolina Univ., Chemistry and Biochemistry Dept., Columbia, SC (United States)

    1998-12-01

    Six ligand-stabilized complexes have been synthesized and tested for use as hydrogen storage media for portable fuel cell applications. The new hydrides are: [HC(3,5-Me{sub 2}pz){sub 3}]LiBH{sub 4} (1), [[H{sub 2}C(3,5-Me{sub 2}pz){sub 2}]LiBH{sub 4})]{sub 2} (2) (pz = pyrazolyl), [(TMEDA)Li(BH{sub 4})]{sub 2} (3) (TMEDA (CH{sub 3}){sub 2}NCH{sub 2}CH{sub 2}N(CH{sub 3}){sub 2}), [HC(pz){sub 3}]LiBH{sub 4} (4), [[H{sub 2}C(pz){sub 2}]Li(BH{sub 4})]{sub 2} (5) and Mg(BH{sub 4}){sub 2}3THF (6) (THF = tetrahydrofuran). Hydrolysis reactions of the compounds liberate hydrogen in quantities which range from 56 to 104 ({+-}5%) of the theoretical yield. Gas chromatographic analysis of the product gases from these reactions indicate that hydrogen is the only gas produced. Thermally initiated reactions of the novel compounds with NH{sub 4}Cl were unsuccessful. Although the amount of hydrogen energy which can be theoretically obtained per unit weight is lower than that of the classical hydrides such as LiBH{sub 4} and NaBH{sub 4}, the reactions are less violent and hydrolysis of compounds 1, 2, 4, 5 and 6 releases less heat per mole of hydrogen generated. (Author)

  5. Electron and nuclear magnetic resonances in compounds and metallic hydrides

    International Nuclear Information System (INIS)

    Brasil Filho, N.

    1985-11-01

    Proton pulsed Nuclear Magnetic Resonance measurements were performed on the metallic hydrides ZrCr 2 H x (x = 2, 3, 4) and ZrV 2 H y (y = 2, 3, 4, 5) as a function of temperature between 180 and 400K. The ultimate aim was the investigation of the relaxation mechanisms in these systems by means of the measurement of both the proton ( 1 H) spin-lattice (T 1 ) and spin-spin (T 2 ) relaxation times and to use these data to obtain information about the diffusive motion of the hydrogen atoms. The diffusional activation energies, the jump frequencies and the Korringa constant, C k , related with the conduction electron contribution to the 1 H relaxation were determined for the above hydrides as a function of hydrogen concentration. Our results were analysed in terms of the relaxation models described by Bloembergen, Purcell and Pound (BPP model) and by Torrey. The Korringa type relaxation due to the conduction electrons in metallic systems was also used to interpret the experimental results. We also present the Electron Paramagnetic Ressonance (EPR) study of Gd 3+ , Nd 3+ and Er 3+ ions as impurities in several AB 3 intermetallic compounds where A = LA, Ce, Y, Sc, Th, Zr and B = Rh, Ir, Pt. The results were analysed in terms of the multiband model previously suggested to explain the behaviour of the resonance parameter in AB 2 Laves Phase compounds. (author) [pt

  6. A low tritium hydride bed inventory estimation technique

    Energy Technology Data Exchange (ETDEWEB)

    Klein, J.E.; Shanahan, K.L.; Baker, R.A. [Savannah River National Laboratory, Aiken, SC (United States); Foster, P.J. [Savannah River Nuclear Solutions, Aiken, SC (United States)

    2015-03-15

    Low tritium hydride beds were developed and deployed into tritium service in Savannah River Site. Process beds to be used for low concentration tritium gas were not fitted with instrumentation to perform the steady-state, flowing gas calorimetric inventory measurement method. Low tritium beds contain less than the detection limit of the IBA (In-Bed Accountability) technique used for tritium inventory. This paper describes two techniques for estimating tritium content and uncertainty for low tritium content beds to be used in the facility's physical inventory (PI). PI are performed periodically to assess the quantity of nuclear material used in a facility. The first approach (Mid-point approximation method - MPA) assumes the bed is half-full and uses a gas composition measurement to estimate the tritium inventory and uncertainty. The second approach utilizes the bed's hydride material pressure-composition-temperature (PCT) properties and a gas composition measurement to reduce the uncertainty in the calculated bed inventory.

  7. Gas desorption properties of ammonia borane and metal hydride composites

    International Nuclear Information System (INIS)

    Matin, M.R.

    2009-01-01

    'Full text': Ammonia borane (NH 3 BH 3 ) has been of great interest owing to its ideal combination of low molecular weight and high H 2 storage capacity of 19.6 mass %, which exceeds the current capacity of gasoline. DOE's year 2015 targets involve gravimetric as well as volumetric energy densities. In this work, we have investigated thermal decomposition of ammonia borane and calcium hydride composites at different molar ratio. The samples were prepared by planetary ball milling under hydrogen gas atmosphere pressure of 1Mpa at room temperature for 2, and 10 hours. The gas desorption properties were examined by thermal desorption mass spectroscopy (TDMS). The identification of phases was carried out by X-ray diffraction. The results obtain were shown in fig (a),(b),and (c). Hydrogen desorption properties were observed at all molar ratios, but the desorption temperature is significantly lower at around 70 o C at molar ratio 1:1 as shown in fig (c), and unwanted gas (ammonia) emissions were remarkably suppressed by mixing with the calcium hydride. (author)

  8. 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)

  9. ACCEPTABILITY ENVELOPE FOR METAL HYDRIDE-BASED HYDROGEN STORAGE SYSTEMS

    Energy Technology Data Exchange (ETDEWEB)

    Hardy, B.; Corgnale, C.; Tamburello, D.; Garrison, S.; Anton, D.

    2011-07-18

    The design and evaluation of media based hydrogen storage systems requires the use of detailed numerical models and experimental studies, with significant amount of time and monetary investment. Thus a scoping tool, referred to as the Acceptability Envelope, was developed to screen preliminary candidate media and storage vessel designs, identifying the range of chemical, physical and geometrical parameters for the coupled media and storage vessel system that allow it to meet performance targets. The model which underpins the analysis allows simplifying the storage system, thus resulting in one input-one output scheme, by grouping of selected quantities. Two cases have been analyzed and results are presented here. In the first application the DOE technical targets (Year 2010, Year 2015 and Ultimate) are used to determine the range of parameters required for the metal hydride media and storage vessel. In the second case the most promising metal hydrides available are compared, highlighting the potential of storage systems, utilizing them, to achieve 40% of the 2010 DOE technical target. Results show that systems based on Li-Mg media have the best potential to attain these performance targets.

  10. The effect of hydrides on the growth of zirconia

    International Nuclear Information System (INIS)

    Ekbom, L.R.

    1982-01-01

    The purpose of the present experiment has been to verify a hypothesis that accelerated corrosion of hydride containin Zircaloy is caused by small pores formed in the oxide by the evolution of hydrogen during oxidation of hydrides. The work has been divided into two parts: specimen preparation and microscopy. ZrO 2 is difficult to work with because of the high compressive stress which exists in the oxide. The most interesting area to study if any hydrogen pores exist, is the metal-oxide interface. Both transmission and scanning electron microscopy were used in the study. Neither of these methods gave any useful information with regard to the original hypothesis. However, a few interesting observations were made on the structure of the oxide at the metal-oxide interface. When the metal had been removed by electropolishing it was seen that the inner surface of the oxide consisted of 0,2-0.3 μ long and 0.1 μ thick wormlike protuberances of oxide. These features could not be seen when the metal had been removed by chemical etching. An attempt to determine whether or not this structure is an artefact introduced by electropolishing was inconclusive but indicated that the structure probably is real. (Author)

  11. Microchip power compensated calorimetry applied to metal hydride characterization

    Energy Technology Data Exchange (ETDEWEB)

    Sepulveda, A.; Lopeandia, A.F.; Domenech-Ferrer, R.; Garcia, G.; Pi, F.; Rodriguez-Viejo, J. [Nanomaterials and Microsystems Group, Physics Department, Universitat Autonoma de Barcelona, 08193 Bellaterra (Spain); Munoz, F.J. [Instituto de Microelectronica de Barcelona, Centro Nacional de Microelectronica, Campus UAB, 08193 Bellaterra (Spain)

    2008-06-15

    In this work, we show the suitability of the thin film membrane-based calorimetric technique to measure kinetically limited phase transitions such as the dehydrogenation of metallic hydrides. Different compounds such as Mg, Mg/Al and Mg{sub 80}Ti{sub 20} have been deposited over the active area of the microchip by electron beam evaporation. After several hydrogenation treatments at different temperatures to induce the hydride formation, calorimetric measurements on the dehydrogenation process of those thin films, either in vacuum or in air, are performed at a heating rate of 10 C/min. We observe a significant reduction in the onset of dehydrogenation for Mg{sub 80}Ti{sub 20} compared with pure Mg or Mg/Al layers, which confirms the beneficial effect of Ti on dehydrogenation. We also show the suitability of the membrane-based nanocalorimeters to be used in parallel with optical methods. Quantification of the energy released during hydrogen desorption remains elusive due to the semi-insulating to metallic transition of the film which affects the calorimetric trace. (author)

  12. A quantitative phase field model for hydride precipitation in zirconium alloys: Part I. Development of quantitative free energy functional

    International Nuclear Information System (INIS)

    Shi, San-Qiang; Xiao, Zhihua

    2015-01-01

    A temperature dependent, quantitative free energy functional was developed for the modeling of hydride precipitation in zirconium alloys within a phase field scheme. The model takes into account crystallographic variants of hydrides, interfacial energy between hydride and matrix, interfacial energy between hydrides, elastoplastic hydride precipitation and interaction with externally applied stress. The model is fully quantitative in real time and real length scale, and simulation results were compared with limited experimental data available in the literature with a reasonable agreement. The work calls for experimental and/or theoretical investigations of some of the key material properties that are not yet available in the literature

  13. Absorption of hydrogen by vanadium-palladium alloys

    International Nuclear Information System (INIS)

    Artman, D.; Lynch, J.F.; Flanagan, T.B.

    1976-01-01

    Pressure composition isotherms (273-373 K) have been determined for the absorption of hydrogen by a series of six palladium alloys (f.c.c) in the composition range from 1 to 8 at.% vanadium. At a given hydrogen content, the equilibrium hydrogen pressure progressively increases with vanadium content. Thermodynamic parameters for the absorption of hydrogen are reported at infinite dilution of hydrogen and for the formation of the nonstoichiometric hydride from the hydrogen-saturated alloy. The relative, partial molar enthalpy of solution of hydrogen at infinite dilution increases slightly with vanadium content. The presence of vanadium, which absorbs hydrogen itself in its normal b.c.c. structure, greatly inhibits the ability of palladium to absorb hydrogen. For example, the isobaric solubility of hydrogen (1 atm, 298K) decreases from H/Pd=0.7 (palladium) to 0.024 (V(6%)-Pd). The lattice expansion due to the presence of interstitial hydrogen has been determined by X-ray diffraction. From these data it can be concluded that the formation of two non-stoichiometric hydride phases does not occur at vanadium contents greater that 5 at.% (298 K). Electrical resistance has been measured as a function of the hydrogen content of the alloys. The electrical resistance increases more markedly with hydrogen content for these alloys than for any of the palladium alloys previously examined. (Auth.)

  14. Hydrogen absorption in CexGd1−x alloys

    International Nuclear Information System (INIS)

    Bereznitsky, M.; Bloch, J.; Yonovich, M.; Schweke, D.; Mintz, M.H.; Jacob, I.

    2012-01-01

    Highlights: ► Ce x Gd 1−x alloys exhibit the most negative heats of hydride formation ever found. ► Thermodynamics of H absorption in Ce x Gd 1−x correlates with the alloys hardness. ► The entropies of H solution and hydride formation reflect the hydrogen vibrations. ► Terminal hydrogen solubilities change in a monotonic way between Ce and Gd. - Abstract: The effect of alloying on the thermodynamics of hydrogen absorption was studied for Ce x Gd 1−x alloys (0 ≤ x ≤ 1) at temperatures between 850 K and 1050 K in the 1–10 −4 Torr pressure range. The temperature-dependent hydrogen solubilities and plateau pressures for hydride formation were obtained from hydrogen absorption isotherms. The terminal hydrogen solubility (THS) at a given temperature changes in a monotonic way as a function of x. It is approximately three times higher in Gd, than in Ce, throughout the investigated temperature range. This monotonic behavior is opposed to that of many other substitutional alloys, for which the hydrogen terminal solubility increases with increasing solute concentrations. The enthalpies, ΔH f , and the entropies, ΔS f , of the dihydride formation exhibit a pronounced and broad negative minimum starting at x ≈ 0.15, yielding the most negative ΔH f values ever found for metal hydrides. On the other hand, the enthalpies and entropies of ideal solution display a positive trend at x = 0.15 and x = 0.3. Both behaviors are considered in view of a reported distinct variation of the Ce x Gd 1−x hardness as a function of x. The particular compositional variations of the entropies of solution and formation as a function of x reflect most likely the vibrational properties of the hydrogen atoms in the metal matrices.

  15. Spectroscopic study of low-temperature hydrogen absorption in palladium

    Energy Technology Data Exchange (ETDEWEB)

    Ienaga, K., E-mail: ienaga@issp.u-tokyo.ac.jp; Takata, H.; Onishi, Y.; Inagaki, Y.; Kawae, T. [Department of Applied Quantum Physics, Faculty of Engineering, Kyushu University, Motooka, Nishi-Ku, Fukuoka 819-0395 (Japan); Tsujii, H. [Department of Physics, Faculty of Education, Kanazawa University, Kakuma-machi, Kanazawa 920-1192 (Japan); Kimura, T. [Department of Physics, Kyushu University, Hakozaki, Higashi-Ku, Fukuoka 812-8581 (Japan)

    2015-01-12

    We report real-time detection of hydrogen (H) absorption in metallic palladium (Pd) nano-contacts immersed in liquid H{sub 2} using inelastic electron spectroscopy (IES). After introduction of liquid H{sub 2}, the spectra exhibit the time evolution from the pure Pd to the Pd hydride, indicating that H atoms are absorbed in Pd nano-contacts even at the temperature where the thermal process is not expected. The IES time and bias voltage dependences show that H absorption develops by applying bias voltage 30 ∼ 50 mV, which can be explained by quantum tunneling. The results represent that IES is a powerful method to study the kinetics of high density H on solid surface.

  16. A deformation and thermodynamic model for hydride precipitation kinetics in spent fuel cladding

    International Nuclear Information System (INIS)

    Stout, R.B.

    1989-10-01

    Hydrogen is contained in the Zircaloy cladding of spent fuel rods from nuclear reactors. All the spent fuel rods placed in a nuclear waste repository will have a temperature history that decreases toward ambient; and as a result, most all of the hydrogen in the Zircaloy will eventually precipitate as zirconium hydride platelets. A model for the density of hydride platelets is a necessary sub-part for predicting Zircaloy cladding failure rate in a nuclear waste repository. A model is developed to describe statistically the hydride platelet density, and the density function includes the orientation as a physical attribute. The model applies concepts from statistical mechanics to derive probable deformation and thermodynamic functionals for cladding material response that depend explicitly on the hydride platelet density function. From this model, hydride precipitation kinetics depend on a thermodynamic potential for hydride density change and on the inner product of a stress tensor and a tensor measure for the incremental volume change due to hydride platelets. The development of a failure response model for Zircaloy cladding exposed to the expected conditions in a nuclear waste repository is supported by the US DOE Yucca Mountain Project. 19 refs., 3 figs

  17. Influence of hydride microstructure on through-thickness crack growth in zircaloy-4 sheet

    International Nuclear Information System (INIS)

    Raynaud, P.A.; Meholic, M.J.; Koss, D.A.; Motta, A.T.; Chan, K.S.

    2007-01-01

    The fracture toughness of cold-worked and stress-relieved Zircaloy-4 sheet subject to through-thickness crack growth within a 'sunburst' hydride microstructure was determined at 25 o C. The results were obtained utilizing a novel testing procedure in which a narrow linear strip of hydride blister was fractured at small loads under bending to create a well-defined sharp pre-crack that arrested at the blister-substrate interface. The hydriding procedure also forms 'sunburst' hydrides emanating from the blister that were aligned both in the plane of the crack and in the crack growth direction. Subsequent tensile loading caused crack growth initiation into the field of 'sunburst' hydrides. Specimen failure occurred under near-linear elastic behavior, and the fracture toughness for crack growth initiation into sunburst hydrides was in the range K Q ∼10-15 MPa√m. These results, when combined with those of a previous study, indicate that the through-thickness crack growth initiation toughness at 25 o C is very sensitive to the hydride microstructure. (author)

  18. 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

  19. 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

  20. 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

  1. Study on the scattering law and scattering kernel of hydrogen in zirconium hydride

    International Nuclear Information System (INIS)

    Jiang Xinbiao; Chen Wei; Chen Da; Yin Banghua; Xie Zhongsheng

    1999-01-01

    The nuclear analytical model of calculating scattering law and scattering kernel for the uranium zirconium hybrid reactor is described. In the light of the acoustic and optic model of zirconium hydride, its frequency distribution function f(ω) is given and the scattering law of hydrogen in zirconium hydride is obtained by GASKET. The scattering kernel σ l (E 0 →E) of hydrogen bound in zirconium hydride is provided by the SMP code in the standard WIMS cross section library. Along with this library, WIMS is used to calculate the thermal neutron energy spectrum of fuel cell. The results are satisfied

  2. 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)

  3. Quantification and characterization of zirconium hydrides in Zircaloy-4 by the image analysis method

    International Nuclear Information System (INIS)

    Zhang, J.H.; Groos, M.; Bredel, T.; Trotabas, M.; Combette, P.

    1992-01-01

    The image analysis method is used to determine the hydrogen content in specimens of Zircaloy-4. Two parameters, surface density of hydride, S v , and degree of orientation, Ω, are defined to represent separately the hydrogen content and the orientation of hydrides. By analysing the stress-relieved Zircaloy-4 specimens with known hydrogen content from 100 to 1000 ppm, a relationship is established between the parameter S v and the hydrogen content when the magnifications of the optical microscope are 1000 and 250. The degree of orientation for the hydride in the stress-relieved Zircaloy-4 cladding is about 0.3. (orig.)

  4. Study of factors affecting a combustion method for determining carbon in lithium hydride

    International Nuclear Information System (INIS)

    Barringer, R.E.; Thornton, R.E.

    1975-09-01

    An investigation has been made of the factors affecting a combustion method for the determination of low levels (300 to 15,000 micrograms/gram) of carbon in highly reactive lithium hydride. Optimization of the procedure with available equipment yielded recoveries of 90 percent, with a limit of error (0.95) of +-39 percent relative for aliquants containing 35 to 55 micrograms of carbon (500 to 800 micrograms of carbon per gram of lithium hydride sample). Sample preparation, thermal decomposition of the hydride, final ignition of the carbon, and carbon-measurement steps were studied, and a detailed procedure was developed. (auth)

  5. Thermodynamics and statistical mechanics of some hydrides of the lanthanides and actinides

    International Nuclear Information System (INIS)

    Mintz, M.H.

    1976-06-01

    This work deals mainly with the thermodynamic and physical properties of the hydrides of the lanthanides and actinides. In addition, statistical models have been developed and applied to metal-hydrogen systems. A kinetic study of the uranium-hydrogen system was performed. The thermodynamic properties of the hydrides of neptunium, thorium, praseodymium, neodymium, samarium and europium were determined. In addition the samarium-europium-hydrogen ternary system was investigated. Moessbauer effect measurements of cubic neptunium hydrides were interpreted according to a model presented. A comparison. (author)

  6. Study on an innovative fast reactor utilizing hydride neutron absorber - Final report of phase I study

    International Nuclear Information System (INIS)

    Konashi, K.; Iwasaki, T.; Itoh, K.; Hirai, M.; Sato, J.; Kurosaki, K.; Suzuki, A.; Matsumura, Y.; Abe, S.

    2010-01-01

    These days, the demand to use nuclear resources efficiently is growing for long-term energy supply and also for solving the green house problem. It is indispensable to develop technologies to reduce environmental load with the nuclear energy supply for sustainable development of human beings. In this regard, the development of the fast breeder reactor (FBR) is preferable to utilize nuclear resources effectively and also to burn minor actinides which possess very long toxicity for more than thousands years if they are not extinguished. As one of the FBR developing works in Japan this phase I study started in 2006 to introduce hafnium (Hf) hydride and Gadolinium-Zirconium (Gd-Zr) hydride as new control materials in FBR. By adopting them, the FBR core control technology is improved by two ways. One is extension of control rod life time by using long life Hf hydride which leads to reduce the fabrication and disposal cost and the other is reduction of the excess reactivity by adopting Gd-Zr hydride which leads to reduce the number of control rods and simplifies the core upper structure. This three year study was successfully completed and the following results were obtained. The core design was performed to examine the applicability of the Hf hydride absorber to Japanese Sodium Fast Reactor (JSFR) and it is clarified that the control rod life time can be prolonged to 6 years by adopting Hf hydride and the excess reactivity of the beginning of the core cycle can be reduced to half and the number of the control rods is also reduced to half by using the Gd-Zr hydride burnable poison. The safety analyses also certified that the core safety can be maintained with the same reliability of JSFR Hf hydride and Gd-Zr hydride pellets were fabricated in good manner and their basic features for design use were measured by using the latest devices such as SEM-EDX. In order to reduce the hydrogen transfer through the stainless steel cladding a new technique which shares calorizing

  7. Peculiarities of formation of zirconium aluminides in hydride cycle mode

    International Nuclear Information System (INIS)

    Muradyan, G.N.

    2016-01-01

    The zirconium aluminides are promising structural materials in aerospace, mechanical engineering, chemical industry, etc. They are promising for manufacturing of heat-resistant wires, that will improve the reliability and efficiency of electrical networks. In the present work, the results of study of zirconium aluminides formation in the Hydride Cycle (HC) mode, developed in the Laboratory of high-temperature synthesis of the Institute of Chemical Physics of NAS RA, are described. The formation of zirconium aluminides in HC proceeded according to the reaction xZrH_2+(1-x)Al → alloy Zr_xAl(1-x)+H_2↑. The samples were certified using: chemical analysis to determine the content of hydrogen (pyrolysis method); differential thermal analysis (DTA, derivatograph Q-1500, T_heating = 1000°C, rate 20°C/min); X-ray analysis (XRD, diffractometer DRON-0.5). The influences of the ratio of powders ZrH_2/Al in the reaction mixture, compacting pressure, temperature and heating velocity on the characteristics of the synthesized aluminides were determined. In HC, the solid solutions of Al in Zr, single phase ZrAl_2 and ZrAl_3 aluminides and Zr_3AlH_4.49 hydride were synthesized. Formation of aluminides in HC mode took place by the solid-phase mechanism, without melting of aluminum. During processing, the heating of the initial charge up to 540°C resulted in the decomposition of zirconium hydride (ZrH_2) to HCC ZrH_1.5, that interacted with aluminum at 630°C forming FCC alumohydride of zirconium. Further increase of the temperature up to 800°C led to complete decomposition of the formed alumohydride of zirconium. The final formation of the zirconium aluminide occurred at 1000-1100°C in the end of HC process. Conclusion: in the synthesis of zirconium aluminides, the HC mode has several significant advantages over the conventional modes: lower operating temperatures (1000°C instead of 1800°C); shorter duration (1.5-2 hours instead of tens of hours); the availability of

  8. Hydrogen Storage Engineering Center of Excellence Metal Hydride Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Motyka, T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2014-05-31

    The Hydrogen Storage Engineering Center of Excellence (HSECoE) was established in 2009 by the U.S. Department of Energy (DOE) to advance the development of materials-based hydrogen storage systems for hydrogen-fueled light-duty vehicles. The overall objective of the HSECoE is to develop complete, integrated system concepts that utilize reversible metal hydrides, adsorbents, and chemical hydrogen storage materials through the use of advanced engineering concepts and designs that can simultaneously meet or exceed all the DOE targets. This report describes the activities and accomplishments during Phase 1 of the reversible metal hydride portion of the HSECoE, which lasted 30 months from February 2009 to August 2011. A complete list of all the HSECoE partners can be found later in this report but for the reversible metal hydride portion of the HSECoE work the major contributing organizations to this effort were the United Technology Research Center (UTRC), General Motors (GM), Pacific Northwest National Laboratory (PNNL), the National Renewable Energy Laboratory (NREL) and the Savannah River National Laboratory (SRNL). Specific individuals from these and other institutions that supported this effort and the writing of this report are included in the list of contributors and in the acknowledgement sections of this report. The efforts of the HSECoE are organized into three phases each approximately 2 years in duration. In Phase I, comprehensive system engineering analyses and assessments were made of the three classes of storage media that included development of system level transport and thermal models of alternative conceptual storage configurations to permit detailed comparisons against the DOE performance targets for light-duty vehicles. Phase 1 tasks also included identification and technical justifications for candidate storage media and configurations that should be capable of reaching or exceeding the DOE targets. Phase 2 involved bench-level testing and

  9. Understanding arsenic metabolism through spectroscopic determination of arsenic in human urine

    OpenAIRE

    Brima, Eid I.; Jenkins, Richard O.; Haris, Parvez I.

    2006-01-01

    In this review we discuss a range of spectroscopic techniques that are currently used for analysis of arsenic in human urine for understanding arsenic metabolism and toxicity, especially in relation to genetics/ethnicity, ingestion studies and exposure to arsenic through drinking water and diet. Spectroscopic techniques used for analysis of arsenic in human urine include inductively coupled plasma mass spectrometry (ICP-MS), hydride generation atomic absorption spectrometry (HG-AAS), hydride ...

  10. Comparison of delayed hydride cracking behavior of two zirconium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Ponzoni, L.M.E. [CNEA – Centro Atómico Constituyentes, Hidrógeno en Materiales, Av. Gral. Paz 1499, San Martín (B1650KNA), Bs. As. (Argentina); Mieza, J.I. [CNEA – Centro Atómico Constituyentes, Hidrógeno en Materiales, Av. Gral. Paz 1499, San Martín (B1650KNA), Bs. As. (Argentina); Instituto Sabato, UNSAM–CNEA, Av. Gral. Paz 1499, San Martín (B1650KNA), Bs. As. (Argentina); De Las Heras, E. [CNEA – Centro Atómico Constituyentes, Hidrógeno en Materiales, Av. Gral. Paz 1499, San Martín (B1650KNA), Bs. As. (Argentina); Domizzi, G., E-mail: domizzi@cnea.gov.ar [CNEA – Centro Atómico Constituyentes, Hidrógeno en Materiales, Av. Gral. Paz 1499, San Martín (B1650KNA), Bs. As. (Argentina); Instituto Sabato, UNSAM–CNEA, Av. Gral. Paz 1499, San Martín (B1650KNA), Bs. As. (Argentina)

    2013-08-15

    Delayed hydride cracking (DHC) is an important failure mechanism that may occur in Zr alloys during service in water-cooled reactors. Two conditions must be attained to initiate DHC from a crack: the stress intensity factor must be higher than a threshold value called K{sub IH} and, hydrogen concentration must exceed a critical value. Currently the pressure tubes for CANDU reactor are fabricated from Zr–2.5Nb. In this paper the critical hydrogen concentration for DHC and the crack velocity of a developmental pressure tube, Excel, was evaluated and compared with that of Zr–2.5Nb. The DHC velocity values measured in Excel were higher than usually reported in Zr–2.5Nb. Due to the higher hydrogen solubility limits in Excel, its critical hydrogen concentration for DHC initiation is 10–50 wppm over that of Zr–2.5Nb in the range of 150–300 °C.

  11. Hydride transport vessel vibration and shock test report

    Energy Technology Data Exchange (ETDEWEB)

    Tipton, D.G.

    1998-06-01

    Sandia National Laboratories performed vibration and shock testing on a Savannah River Hydride Transport Vessel (HTV) which is used for bulk shipments of tritium. This testing is required to qualify the HTV for transport in the H1616 shipping container. The main requirement for shipment in the H1616 is that the contents (in this case the HTV) have a tritium leak rate of less than 1x10{sup {minus}7} cc/sec after being subjected to shock and vibration normally incident to transport. Helium leak tests performed before and after the vibration and shock testing showed that the HTV remained leaktight under the specified conditions. This report documents the tests performed and the test results.

  12. Delayed hydride cracking: theoretical model testing to predict cracking velocity

    International Nuclear Information System (INIS)

    Mieza, Juan I.; Vigna, Gustavo L.; Domizzi, Gladys

    2009-01-01

    Pressure tubes from Candu nuclear reactors as any other component manufactured with Zr alloys are prone to delayed hydride cracking. That is why it is important to be able to predict the cracking velocity during the component lifetime from parameters easy to be measured, such as: hydrogen concentration, mechanical and microstructural properties. Two of the theoretical models reported in literature to calculate the DHC velocity were chosen and combined, and using the appropriate variables allowed a comparison with experimental results of samples from Zr-2.5 Nb tubes with different mechanical and structural properties. In addition, velocities measured by other authors in irradiated materials could be reproduced using the model described above. (author)

  13. Modeling of hydride precipitation and re-orientation

    Energy Technology Data Exchange (ETDEWEB)

    Tikare, Veena [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Weck, Philippe F. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Mitchell, John Anthony [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2015-09-18

    In this report, we present a thermodynamic-­based model of hydride precipitation in Zr-based claddings. The model considers the state of the cladding immediately following drying, after removal from cooling-pools, and presents the evolution of precipitate formation upon cooling as follows: The pilgering process used to form Zr-based cladding imparts strong crystallographic and grain shape texture, with the basal plane of the hexagonal α-Zr grains being strongly aligned in the rolling-­direction and the grains are elongated with grain size being approximately twice as long parallel to the rolling direction, which is also the long axis of the tubular cladding, as it is in the orthogonal directions.

  14. 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.)

  15. Final report for the DOE Metal Hydride Center of Excellence.

    Energy Technology Data Exchange (ETDEWEB)

    Keller, Jay O.; Klebanoff, Leonard E.

    2012-01-01

    This report summarizes the R&D activities within the U.S. Department of Energy Metal Hydride Center of Excellence (MHCoE) from March 2005 to June 2010. The purpose of the MHCoE has been to conduct highly collaborative and multi-disciplinary applied R&D to develop new reversible hydrogen storage materials that meet or exceed DOE 2010 and 2015 system goals for hydrogen storage materials. The MHCoE combines three broad areas: mechanisms and modeling (which provide a theoretically driven basis for pursuing new materials), materials development (in which new materials are synthesized and characterized) and system design and engineering (which allow these new materials to be realized as practical automotive hydrogen storage systems). This Final Report summarizes the organization and execution of the 5-year research program to develop practical hydrogen storage materials for light duty vehicles. Major results from the MHCoE are summarized, along with suggestions for future research areas.

  16. Hydride transport vessel vibration and shock test report

    International Nuclear Information System (INIS)

    Tipton, D.G.

    1998-06-01

    Sandia National Laboratories performed vibration and shock testing on a Savannah River Hydride Transport Vessel (HTV) which is used for bulk shipments of tritium. This testing is required to qualify the HTV for transport in the H1616 shipping container. The main requirement for shipment in the H1616 is that the contents (in this case the HTV) have a tritium leak rate of less than 1x10 -7 cc/sec after being subjected to shock and vibration normally incident to transport. Helium leak tests performed before and after the vibration and shock testing showed that the HTV remained leaktight under the specified conditions. This report documents the tests performed and the test results

  17. First principle calculations of alkali hydride electronic structures

    International Nuclear Information System (INIS)

    Novakovic, N; Radisavljevic, I; Colognesi, D; Ostojic, S; Ivanovic, N

    2007-01-01

    Electronic structure, volume optimization, bulk moduli, elastic constants, and frequencies of the transversal optical vibrations in LiH, NaH, KH, RbH, and CsH are calculated using the full potential augmented plane wave method, extended with local orbitals, and the full potential linearized augmented plane wave method. The obtained results show some common features in the electronic structure of these compounds, but also clear differences, which cannot be explained using simple empirical trends. The differences are particularly prominent in the electronic distributions and interactions in various crystallographic planes. In the light of these findings we have elaborated some selected experimental results and discussed several theoretical approaches frequently used for the description of various alkali hydride properties

  18. Metal hydride hydrogen compression: recent advances and future prospects

    Science.gov (United States)

    Yartys, Volodymyr A.; Lototskyy, Mykhaylo; Linkov, Vladimir; Grant, David; Stuart, Alastair; Eriksen, Jon; Denys, Roman; Bowman, Robert C.

    2016-04-01

    Metal hydride (MH) thermal sorption compression is one of the more important applications of the MHs. The present paper reviews recent advances in the field based on the analysis of the fundamental principles of this technology. The performances when boosting hydrogen pressure, along with two- and three-step compression units, are analyzed. The paper includes also a theoretical modelling of a two-stage compressor aimed at describing the performance of the experimentally studied systems, their optimization and design of more advanced MH compressors. Business developments in the field are reviewed for the Norwegian company HYSTORSYS AS and the South African Institute for Advanced Materials Chemistry. Finally, future prospects are outlined presenting the role of the MH compression in the overall development of the hydrogen-driven energy systems. The work is based on the analysis of the development of the technology in Europe, USA and South Africa.

  19. Interface Enthalpy-Entropy Competition in Nanoscale Metal Hydrides

    Directory of Open Access Journals (Sweden)

    Nicola Patelli

    2018-01-01

    Full Text Available We analyzed the effect of the interfacial free energy on the thermodynamics of hydrogen sorption in nano-scaled materials. When the enthalpy and entropy terms are the same for all interfaces, as in an isotropic bi-phasic system, one obtains a compensation temperature, which does not depend on the system size nor on the relative phase abundance. The situation is different and more complex in a system with three or more phases, where the interfaces have different enthalpy and entropy. We also consider the possible effect of elastic strains on the stability of the hydride phase and on hysteresis. We compare a simple model with experimental data obtained on two different systems: (1 bi-phasic nanocomposites where ultrafine TiH2 crystallite are dispersed within a Mg nanoparticle and (2 Mg nanodots encapsulated by different phases.

  20. Work function in niobium, tantalum and vanadium hydrides

    International Nuclear Information System (INIS)

    Kucherov, Ya.R.; Markin, V.Ya.; Savin, V.I.; Topil'skij, N.D.

    1978-01-01

    The concentration dependences of the work function of electrons in hydrides of Nb, Ta and V are presented. The work function of electrons was studied at room temperature by the contact Kelvin potential difference method to an accuracy of +-0.02 eV. The effect of hydrogen on the work function variations in the systems investigated has been analyzed. It is shown that a higher hydrogen concentration in solid solutions based on the Nb-H and Ta-H systems increases the effective total positive dipole moment, whereby the work function decreases. The abnormal changes in the work function in the region of solid solutions of hydrogen in vanadium seem to be due to the specific electronic structure of vanadium and its interaction with hydrogen

  1. 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.

  2. 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)

  3. Neutron diffraction studies of transition metal hydride complexes

    International Nuclear Information System (INIS)

    Koetzle, T.F.; Bau, R.

    1976-01-01

    Investigations of H 3 Ta(C 5 H 5 ) 2 (III), HW 2 (CO) 9 (NO) (IV), and HW 2 (CO) 8 (NO) (P(OCH 3 ) 3 ) (V) have been completed. Preliminary results are available for HFeCo 3 (CO) 9 [P(OCH 3 ) 3 ] 3 (VII). This work, together with studies of HMo 2 (C 5 H 5 ) 2 (CO) 4 (P(CH 3 ) 2 ) (VI) and [(C 2 H 5 ) 4 N] + [HCr 2 (CO) 10 ] - carried out at Argonne has led to some general observations on the geometry and the nature of bonding in these compounds. For example, in the structures of IV and V, both of which have bent W--H--W linkages (less than W--H--W in the range 125-130 0 ), there is conclusive evidence for the existence of a closed three-center W--H--W bond with significant metal-metal interaction. Such is the case, because extensions of the axial W--C and W--N bonds trans to the hydride intersect at a point near the center of the W--H--W triangle. The geometry of VI, which also contains a bent M--H--M bond, is consistent with that of IV and V. Bridging M--H bonds in these second- and third-row hydrides range in length from 1.85 to 1.89 A, compared to 1.75 A in the first-row polynuclear complex VII. For metals of corresponding rows, bridging M--H bonds are about 0.1 A longer than terminal bonds, which are classified as single covalent bonds

  4. Solutions to commercializing metal hydride hydrogen storage products

    International Nuclear Information System (INIS)

    Tomlinson, J.J.; Belanger, R.

    2004-01-01

    'Full text:' Whilst the concept of a Hydrogen economy in the broad sense may for some analysts and Fuel Cell technology developers be an ever moving target the use of hydrogen exists and is growing in other markets today. The use of hydrogen is increasing. Who are the users? What are their unique needs? How can they better be served? As the use of hydrogen increases there are things we can do to improve the perception and handling of hydrogen as an industrial gas that will impact the future issues of hydrogen as a fuel thereby assisting the mainstream availability of hydrogen fuel a reality. Factors that will induce change in the way hydrogen is used, handled, transported and stored are the factors to concentrate development efforts on. Other factors include: cost; availability; safety; codes and standards; and regulatory authorities acceptance of new codes and standards. New methods of storage and new devices in which the hydrogen is stored will influence and bring about change and increased use. New innovative products based on Metal Hydride hydrogen storage will address some of the barriers to widely distributed hydrogen as a fuel or energy carrier to which successful fuel cell product commercialization is subject. Palcan has developed innovative products based on it's Rare Earth Metal Hydride alloy. Some of these innovations will aid the distribution of hydrogen as a fuel and offer alternatives to the existing hydrogen user and to the Fuel Cell product developer. An overview of the products and how these products will affect the distribution and use of hydrogen as an industrial gas and fuel is presented. (author)

  5. Sorption properties of nanocrystalline metal hydrides for the storage of hydrogen; Sorptionseigenschaften von nanokristallinen Metallhydriden fuer die Wasserstoffspeicherung

    Energy Technology Data Exchange (ETDEWEB)

    Oelerich, W.

    2000-07-01

    For the utilisation of hydrogen in emission-free automobiles new nanostructured Mg-based metal hydrides were developed. These materials show significantly faster absorption and desorption kinetics, which can be even further enhanced by additions of suitable catalysts. Contrary to conventional magnesium powder, hydrogenation at room temperature is demonstrated for the first time. During dehydrogenation at 250 C a desorption rate of 3 to 8 kW/kg with a capacity of 2.5 kWh/kg is achieved, that fulfills the technical requirements for automobile application. (orig.) [German] Im Hinblick auf den Einsatz von Wasserstoff in emissionsfreien Kraftfahrzeugen wurden neuartige nanostrukturierte Metallhydride auf Basis von Magnesium hergestellt. Diese Materialien zeigen eine deutlich schnellere Absorptions- und Desorptionskinetik, die sich durch den Zusatz von geeigneten Katalysatoren noch weiter steigern laesst. Im Gegensatz zu konventionellem Magnesiumpulver konnte erstmals eine Hydrierung bei Raumtemperatur demonstriert werden. Bei der Dehydrierung bei 250 C wird eine Desorptionsrate von 3 bis 8 kW/kg bei einer Kapazitaet von 2,5 kWh/kg erreicht, die die technischen Leistungsanforderungen von Kraftfahrzeugen erfuellt. (orig.)

  6. Hydride reorientation in Zircaloy-4 examined by in situ synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Weekes, H.E. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Jones, N.G. [Department of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom); Lindley, T.C. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Dye, D., E-mail: david.dye@imperial.ac.uk [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom)

    2016-09-15

    The phenomenon of stress-reorientation has been investigated using in situ X-ray diffraction during the thermomechanical cycling of hydrided Zircaloy-4 tensile specimens. Results have shown that loading along a sample’s transverse direction (TD) leads to a greater degree of hydride reorientation when compared to rolling direction (RD)-aligned samples. The elastic lattice micro-strains associated with radially oriented hydrides have been revealed to be greater than those oriented circumferentially, a consequence of strain accommodation. Evidence of hydride redistribution after cycling, to α-Zr grains oriented in a more favourable orientation when under an applied stress, has also been observed and its behaviour has been found to be highly dependent on the loading axis. Finally, thermomechanical loading across multiple cycles has been shown to reduce the difference in terminal solid solubility of hydrogen during dissolution (TSS{sub D,H}) and precipitation (TSS{sub P,H}).

  7. Corrosion behavior of Zircaloy 4 cladding material. Evaluation of the hydriding effect

    International Nuclear Information System (INIS)

    Blat, M.

    1997-04-01

    In this work, particular attention has been paid to the hydriding effect in PIE and laboratory test to validate a detrimental hydrogen contribution on Zircaloy 4 corrosion behavior at high burnup. Laboratory corrosion tests results confirm that hydrides have a detrimental role on corrosion kinetics. This effect is particularly significant for cathodic charged samples with a massive hydride outer layer before corrosion test. PIE show that at high burnup a hydride layer is formed underneath the metal/oxide interface. The results of the metallurgical examinations are discussed with respect to the possible mechanisms involved in this detrimental effect of hydrogen. Therefore, according to the laboratory tests results and PIE, hydrogen could be a strong contributor to explain the increase in corrosion rate at high burnup. (author)

  8. Quantum-chemical study of hydride transfer in catalytic transformation of paraffins on zeolites

    NARCIS (Netherlands)

    Kazansky, V.B.; Frash, M.V.; Santen, van R.A.; Chon, H.; Ihm, S.-K.; Uh, Y.S.

    1997-01-01

    Ab initio quantum-chemical cluster calculations demonstrate that the activated complexes of hydride transfer reaction in catalytic transformation of paraffins on zeolites very much resembles adsorbed nonclassical carbonium ions. The calculated activation energies for reactions involving propane and

  9. Hydrogen metal hydride storage with integrated catalytic recombiner for mobile application

    Energy Technology Data Exchange (ETDEWEB)

    Marinescu-Pasoi, L.; Behrens, U.; Langer, G.; Gramatte, W.; Rastogi, A.K.; Schmitt, R.E. (Battelle-Institut e.V., Frankfurt am Main (DE). Dept. of Energy Technology)

    1991-01-01

    A novel, thermodynamically efficient device is under development at Battelle in Frankfurt, by which the range of hydrogen-driven cars with a metal hydride tank might be roughly doubled. The device makes use of the properties of metal hydrides, combined with catalytic combustion. Its development is funded by the Hessian Ministry of Economic Affairs and Technology; it is to be completed by the end of 1990. High-temperature hydrides (HTH) have about three times the storage capacity of low temperature hydrides (LTH), but require relatively large amounts of heat at high temperatures to release the hydrogen. The exhaust heat from combustion-engine-driven vehicles is insufficient for this, and vehicles with electric (fuel cell) drive produce practically no exhaust heat at all. The Battelle-developed device is a combination of an HTH storage cell, an LTH storage cell and a catalyst. (author).

  10. Unexpected formation of hydrides in heavy rare earth containing magnesium alloys

    Directory of Open Access Journals (Sweden)

    Yuanding Huang

    2016-09-01

    Full Text Available Mg–RE (Dy, Gd, Y alloys show promising for being developed as biodegradable medical applications. It is found that the hydride REH2 could be formed on the surface of samples during their preparations with water cleaning. The amount of formed hydrides in Mg–RE alloys is affected by the content of RE and heat treatments. It increases with the increment of RE content. On the surface of the alloy with T4 treatment the amount of formed hydride REH2 is higher. In contrast, the amount of REH2 is lower on the surfaces of as-cast and T6-treated alloys. Their formation mechanism is attributed to the surface reaction of Mg–RE alloys with water. The part of RE in solid solution in Mg matrix plays an important role in influencing the formation of hydrides.

  11. The uranium zirconium hydride research reactor and its applications in research and education

    Energy Technology Data Exchange (ETDEWEB)

    Chen Wei; Wang Daohua; Jiang Xinbiao; A Jinyan; Yang Jun; Chen Da [Northwest Institute of Nuclear Technology, Xi' an (China)

    2003-03-01

    This paper describes briefly the performance, the configuration and the prospects of extensive applications in science, technology and education of the Uranium Zirconium Hydride research reactor in China. (author)

  12. The uranium zirconium hydride research reactor and its applications in research and education

    International Nuclear Information System (INIS)

    Chen Wei; Wang Daohua; Jiang Xinbiao; A Jinyan; Yang Jun; Chen Da

    2003-01-01

    This paper describes briefly the performance, the configuration and the prospects of extensive applications in science, technology and education of the Uranium Zirconium Hydride research reactor in China. (author)

  13. Non-Precious Bimetallic Catalysts for Selective Dehydrogenation of an Organic Chemical Hydride System

    KAUST Repository

    Shaikh Ali, Anaam; Jedidi, Abdesslem; Cavallo, Luigi; Takanabe, Kazuhiro

    2015-01-01

    Methylcyclohexane (MCH)-Toluene (TOL) chemical hydride cycles as a hydrogen carrier system is successful with the selective dehydrogenation reaction of MCH to TOL, which has been achieved only using precious Pt-based catalysts. Herein, we report

  14. Theoretical study of the chemical properties of cesium hydride; Teoreticke studium chemickych vlastnosti hydridu cezia

    Energy Technology Data Exchange (ETDEWEB)

    Skoviera, J [Univerzita Komenskeho v Bratislave, Prirodovedecka fakulta, Katedra fyzikalnej a teoretickej chemie, 84215 Bratislava (Slovakia)

    2012-04-25

    A theoretical study of radiofrequency source of hydrogen ions in the International Thermonuclear Experimental Reactor (ITER) used a cesium grid as a source of electrons for ionization of hydrogen. In the process of ionization of hydrogen, however, there is a weathering of cesium grid, resulting into a group of undesired products - cesium hydrides and materials derived from cesium hydride. We calculated the potential curves of cesium hydride and of its anion and cation, their spectroscopic properties and partly their electrical properties. To make electrical properties comparable with the experiment, we calculated for all also the vibration corrections. Lack of convergence in RASSCF step caused, that the electrical properties of excited states are still an open question of chemical properties of cesium hydride. (authors)

  15. D-xylose absorption

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003606.htm D-xylose absorption To use the sharing features on this page, please enable JavaScript. D-xylose absorption is a laboratory test to determine ...

  16. The formation and characteristics of hydride blisters in c.w. Zircaloy-2 pressure tubes

    Energy Technology Data Exchange (ETDEWEB)

    Price, E G [ed.

    1994-09-01

    Under the auspices of the IAEA, a consultants` meeting was arranged in Vienna, 1994 July 25-29, at which a Canadian delegation, consisting of AECL and Ontario Hydro Technologies personnel, presented information on their knowledge of the behaviour of hydride blisters in Zircaloy-2 pressure tubes. This document contains the 10 papers presented by the Canadian delegation to the meeting. It is believed that they represent a good reference document on hydride blister phenomena.

  17. 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

  18. A review of uranium corrosion by hydrogen and the formation of uranium hydride

    OpenAIRE

    Banos, A.; Harker, N. J.; Scott, T. B.

    2018-01-01

    Uranium hydride (UH3) is the direct product of the reaction between uranium metal and gaseous hydrogen. In the context of uranium storage, this corrosion reaction is considered deleterious, not just because the structure of the metal may become significantly degraded but also because the resulting hydride is pyrophoric and therefore potentially flammable in air if present in significant quantity. The current review draws from the literature surrounding the uranium-hydrogen system accrued over...

  19. An Investigation on the Persistence of Uranium Hydride during Storage of Simulant Nuclear Waste Packages

    OpenAIRE

    Stitt , C. A.; Harker , N. J.; Hallam , K. R.; Paraskevoulakos , C.; Banos , A.; Rennie , S.; Jowsey , J.; Scott , T. B.

    2015-01-01

    International audience; Synchrotron X-rays have been used to study the oxidation of uranium and uranium hydride when encapsulated in grout and stored in de-ionised water for 10 months. Periodic synchrotron X-ray tomography and X-ray powder diffraction have allowed measurement and identification of the arising corrosion products and the rates of corrosion. The oxidation rates of the uranium metal and uranium hydride were slower than empirically derived rates previously reported for each reacta...

  20. 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

  1. Synthesis of intermetallic hydrides of Zr-Ni system in the burning regime

    Energy Technology Data Exchange (ETDEWEB)

    Akopyan, A.G.; Dolukhanyan, S.K.; Karapetyan, A.K.; Merzhanov, A.G.

    1983-06-01

    Conditions for production of intermetallides in the Zr-Ni system and their hydrides in the burning regime are studied. Burning regularities of Zr/sub 2/Ni and ZrNi intermetallides in hydrogen are studied, the burning mechanism is found. It is shown that burning proceeds at abnormally low temperatures. Optimum synthesis conditions for Zr/sub 2/NiH/sub 5/ and ZrNiH/sub 3/ hydrides are determined.

  2. Delayed hydride cracking in Zr-2.5Nb pressure tubes

    International Nuclear Information System (INIS)

    Mieza, Juan I.; Domizzi, Gladys; Vigna, Gustavo L.

    2007-01-01

    Zr-2.5 Nb alloy from CANDU pressure tubes are prone to failure by hydrogen intake. One of the degradation mechanisms is delayed hydride cracking, which is characterized by the velocity of cracking. In this work, we study the effect of beta zirconium phase transformation over delayed hydride cracking velocity in Zr-2.5 Nb alloy from pressure tubes. Acoustic emission technique was used for cracking detection. (author) [es

  3. Absorption and excretion tests

    International Nuclear Information System (INIS)

    Berberich, R.

    1988-01-01

    The absorption and excretion of radiopharmaceuticals is still of interest in diagnostic investigations of nuclear medicine. In this paper the most common methods of measuring absorption and excretion are described. The performance of the different tests and their standard values are discussed. More over the basic possibilities of measuring absorption and excretion including the needed measurement equipments are presented. (orig.) [de

  4. 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

  5. Experimental study of a metal hydride driven braided artificial pneumatic muscle

    Science.gov (United States)

    Vanderhoff, Alexandra; Kim, Kwang J.

    2009-12-01

    This paper reports the experimental study of a new actuation system that couples a braided artificial pneumatic muscle (BAPM) with a metal hydride driven hydrogen compressor to create a compact, lightweight, noiseless system capable of high forces and smooth actuation. The results indicate that the metal hydride-BAPM system has relatively good second law efficiency average of 30% over the desorption cycle. The thermal efficiency is low, due mainly to the highly endothermic chemical reaction that releases the stored hydrogen gas from the metal hydride. The force to metal hydride weight is very high (~14 000 NForce/kgMH) considering that this system has not been optimized to use the minimum amount of metal hydride required for a full actuation stroke of the fluidic muscle. Also, a thermodynamic model for the complete system is developed. The analysis is restricted in some aspects concerning the complexity of the hydriding/dehydriding chemical process of the system and the three-dimensional geometry of the reactor, but it provides a useful comparison to other actuation devices and clearly reveals the parameters necessary for optimization of the actuation system in future work. The system shows comparable work output and has the benefits of biological muscle-like properties for potential use in robotic systems.

  6. 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)

  7. Modelling the gas transport and chemical processes related to clad oxidation and hydriding

    Energy Technology Data Exchange (ETDEWEB)

    Montgomery, R O; Rashid, Y R [ANATECH Research Corp., San Diego, CA (United States)

    1997-08-01

    Models are developed for the gas transport and chemical processes associated with the ingress of steam into a LWR fuel rod through a small defect. These models are used to determine the cladding regions in a defective fuel rod which are susceptible to massive hydriding and the creation of sunburst hydrides. The brittle nature of zirconium hydrides (ZrH{sub 2}) in these susceptible regions produces weak spots in the cladding which can act as initiation sites for cladding cracks under certain cladding stress conditions caused by fuel cladding mechanical interaction. The modeling of the axial gas transport is based on gaseous bimolar diffusion coupled with convective mass transport using the mass continuity equation. Hydrogen production is considered from steam reaction with cladding inner surface, fission products and internal components. Eventually, the production of hydrogen and its diffusion along the length results in high hydrogen concentration in locations remote from the primary defect. Under these conditions, the hydrogen can attack the cladding inner surface and breakdown the protective ZrO{sub 2} layer locally, initiating massive localized hydriding leading to sunburst hydride. The developed hydrogen evolution model is combined with a general purpose fuel behavior program to integrate the effects of power and burnup into the hydriding kinetics. Only in this manner can the behavior of a defected fuel rod be modeled to determine the conditions the result in fuel rod degradation. (author). 14 refs, 6 figs.

  8. The effect of texture on delayed hydride cracking in Zr-2.5Nb alloy

    Energy Technology Data Exchange (ETDEWEB)

    Resta Levi, R.; Sagat, S

    1999-09-01

    Pressure tubes for CANDU reactors are made of Zr-2.5Nb alloy. They are produced by hot extrusion followed by cold work, which results in a material with a pronounced crystallographic texture with basal plane normals of its hexagonal structure around the circumferential direction. Under certain conditions, this material is susceptible to a cracking mechanism called delayed hydride cracking (DHC). Our work investigated the susceptibility of Zr-2.5Nb alloy pressure tube to DHC in this pressure tube material, in terms of crystallographic texture and grain shape. The results are presented in terms of crack velocity obtained on different planes and directions of the pressure tube. The results show that it is more difficult for a crack to propagate at right angles to crystallographic basal planes (which are close to the precipitation habit plane of hydrides) than for it to propagate parallel to the basal plane. However, if the cracking plane is oriented parallel to preexisting hydrides (hydrides formed as a result of the manufacturing process), the crack propagates along these hydrides easily, even if the hydride habit planes are not oriented favourably. (author)

  9. Investigation of the effect of hydride and iodine on the mechanical behaviour of the zircaloy-4

    International Nuclear Information System (INIS)

    Soares, M.I.

    1981-12-01

    To investigate the effect of hydride and iodine on the mechanical behaviour of the zircaloy-4 tubes, deformation tests under pressure of samples hydrided in autoclave and of samples containing iodine were carried out, in order to simulate the fission product. The same tests were carried out in samples without hydride and iodine contents that were used as reference samples in the temperature range of 650 0 C-950 0 C. The hydrided samples and the samples containing iodine tested at 650 0 C and 750 0 C showed a higher ductility than the samples of reference. The hydrided samples tested at 850 0 C and 950 0 C showed a higher embritlement than the samples of reference and than the samples containing iodine tested at the same temperatures. A mechanical test has been developed to investigate the effect of hydride and iodine on the mechanical behaviour of the zircaloy-4 tubes. The mechanical test were carried out at room temperature. At room temperature the hydrition decreased the ductility of zircaloy-4. At room temperature the sample containing iodine showed a higher ductility than the sample without iodine. The combined action of hydrogen and iodine at room temperature enhanced the embrittlment of the samples zircaloy-4. (Author) [pt

  10. Investigation of Lithium Metal Hydride Materials for Mitigation of Deep Space Radiation

    Science.gov (United States)

    Rojdev, Kristina; Atwell, William

    2016-01-01

    Radiation exposure to crew, electronics, and non-metallic materials is one of many concerns with long-term, deep space travel. Mitigating this exposure is approached via a multi-faceted methodology focusing on multi-functional materials, vehicle configuration, and operational or mission constraints. In this set of research, we are focusing on new multi-functional materials that may have advantages over traditional shielding materials, such as polyethylene. Metal hydride materials are of particular interest for deep space radiation shielding due to their ability to store hydrogen, a low-Z material known to be an excellent radiation mitigator and a potential fuel source. We have previously investigated 41 different metal hydrides for their radiation mitigation potential. Of these metal hydrides, we found a set of lithium hydrides to be of particular interest due to their excellent shielding of galactic cosmic radiation. Given these results, we will continue our investigation of lithium hydrides by expanding our data set to include dose equivalent and to further understand why these materials outperformed polyethylene in a heavy ion environment. For this study, we used HZETRN 2010, a one-dimensional transport code developed by NASA Langley Research Center, to simulate radiation transport through the lithium hydrides. We focused on the 1977 solar minimum Galactic Cosmic Radiation environment and thicknesses of 1, 5, 10, 20, 30, 50, and 100 g/cm2 to stay consistent with our previous studies. The details of this work and the subsequent results will be discussed in this paper.

  11. Criteria for fracture initiation at hydrides in zirconium alloys. Pt. 1

    International Nuclear Information System (INIS)

    Shi, S.Q.; Puls, M.P.

    1994-01-01

    A theoretical framework for the initiation of delayed hydride cracking (DHC) in zirconium is proposed for two different types of initiating sites, i.e., a sharp crack tip (considered in this part) and a shallow notch (considered in part II). In the present part I, an expression for K IH is derived which shows that K IH depends on the size and shape of the hydride precipitated at the crack tip, the yield stress and elastic moduli of the material and the fracture stress of the hydride. If the hydride at the crack tip extends in length at constant thickness, then K IH increases as the square root of the hydride thickness. Thus a microstructure favouring the formation of thicker hydrides at the crack tip would result in an increased K IH . K IH increases slightly with temperature up to a temperature at which there is a more rapid increase. The temperature at which there is a more rapid increase in K IH will increase as the yield stress increases. The model also predicts that an increase in yield stress due to irradiation will cause an overall slight decrease in K IH compared to unirradiated material. There is good agreement between the overall predictions of the theory and experimental results. It is suggested that more careful evaluations of some key parameters are required to improve on the theoretical estimates. (orig.)

  12. 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.

  13. Synthesis, spectroscopy, and hydrogen/deuterium exchange in high-spin iron(II) hydride complexes.

    Science.gov (United States)

    Dugan, Thomas R; Bill, Eckhard; MacLeod, K Cory; Brennessel, William W; Holland, Patrick L

    2014-03-03

    Very few hydride complexes are known in which the metals have a high-spin electronic configuration. We describe the characterization of several high-spin iron(II) hydride/deuteride isotopologues and their exchange reactions with one another and with H2/D2. Though the hydride/deuteride signal is not observable in NMR spectra, the choice of isotope has an influence on the chemical shifts of distant protons in the dimers through the paramagnetic isotope effect on chemical shift. This provides the first way to monitor the exchange of H and D in the bridging positions of these hydride complexes. The rate of exchange depends on the size of the supporting ligand, and this is consistent with the idea that H2/D2 exchange into the hydrides occurs through the dimeric complexes rather than through a transient monomer. The understanding of H/D exchange mechanisms in these high-spin iron hydride complexes may be relevant to postulated nitrogenase mechanisms.

  14. 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.

  15. 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.

  16. Influence of Zircaloy cladding composition on hydride formation during aqueous hydrogen charging

    Energy Technology Data Exchange (ETDEWEB)

    Rajasekhara, S. [Intel Corporation, 2501 NW 229th Av., Hillsboro, OR 97124 (United States); Kotula, P.G.; Enos, D.G.; Doyle, B.L. [Sandia National Laboratories, Albuquerque, NM, 87185 (United States); Clark, B.G., E-mail: blyclar@sandia.gov [Sandia National Laboratories, Albuquerque, NM, 87185 (United States)

    2017-06-15

    Although hydrogen uptake in Zirconium (Zr) based claddings has been a topic of many studies, hydrogen uptake as a function of alloy composition has received little attention. In this work, commercial Zr-based cladding alloys (Zircaloy-2, Zircaloy-4 and ZIRLO™), differing in composition but with similar initial textures, grain sizes, and surface roughness, were aqueously charged with hydrogen for 100, 300, and 1000 s at nominally 90 °C to produce hydride layers of varying thicknesses. Transmission electron microscope characterization following aqueous charging showed hydride phase and orientation relationship were identical in all three alloys. However, elastic recoil detection measurements confirmed that surface hydride layers in Zircaloy-2 and Zircaloy-4 were an order of magnitude thicker relative to ZIRLO™. - Highlights: •Aqueous charging was performed to produce a layer of zirconium hydride for three different Zr-alloy claddings. •Hydride thicknesses were analyzed by elastic recoil detection and transmission electron microscopy. •Zircaloy-2 and Zircaloy-4 formed thicker hydride layers than ZIRLO™ for the same charging durations.

  17. Determination of Arsenic Content of Available Traditional Medicines ...

    African Journals Online (AJOL)

    Purpose: To determine the content of arsenic (As) in some locally available traditional medicines in the East Coast region of Malaysia. Methods: The determination of As was conducted using hydride generation-atomic absorption spectrometry (HG-AAS). Sample preparation entailed mineral acid digestion using ...

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

    Science.gov (United States)

    Patki, Gauri Dilip

    mole of Si. We compare our silicon nanoparticles (˜10nm diameter) with commercial silicon nanopowder (rate upon decreasing the particle size to 10 nm was even greater than would be expected based upon the increase in surface area. While specific surface area increased by a factor of 6 in going from rate increased by a factor of 150. However, in all cases, silicon requires a base (e.g. NaOH, KOH, hydrazine) to catalyze its reaction with water. Metal hydrides are also promising hydrogen storage materials. The optimum metal hydride would possess high hydrogen storage density at moderate temperature and pressure, release hydrogen safely and controllably, and be stable in air. Alkali metal hydrides have high hydrogen storage density, but exhibit high uncontrollable reactivity with water. In an attempt to control this explosive nature while maintaining high storage capacity, we mixed our silicon nanoparticles with the hydrides. This has dual benefits: (1) the hydride- water reaction produces the alkali hydroxide needed for base-catalyzed silicon oxidation, and (2) dilution with 10nm coating by, the silicon may temper the reactivity of the hydride, making the process more controllable. Initially, we analyzed hydrolysis of pure alkali metal hydrides and alkaline earth metal hydrides. Lithium hydride has particularly high hydrogen gravimetric density, along with faster reaction kinetics than sodium hydride or magnesium hydride. On analysis of hydrogen production we found higher hydrogen yield from the silicon nanoparticle—metal hydride mixture than from pure hydride hydrolysis. The silicon-hydride mixtures using our 10nm silicon nanoparticles produced high hydrogen yield, exceeding the theoretical yield. Some evidence of slowing of the hydride reaction rate upon addition of silicon nanoparticles was observed.

  19. Complex Hydride Compounds with Enhanced Hydrogen Storage Capacity

    Energy Technology Data Exchange (ETDEWEB)

    Mosher, Daniel A.; Opalka, Susanne M.; Tang, Xia; Laube, Bruce L.; Brown, Ronald J.; Vanderspurt, Thomas H.; Arsenault, Sarah; Wu, Robert; Strickler, Jamie; Anton, Donald L.; Zidan, Ragaiy; Berseth, Polly

    2008-02-18

    The United Technologies Research Center (UTRC), in collaboration with major partners Albemarle Corporation (Albemarle) and the Savannah River National Laboratory (SRNL), conducted research to discover new hydride materials for the storage of hydrogen having on-board reversibility and a target gravimetric capacity of ≥ 7.5 weight percent (wt %). When integrated into a system with a reasonable efficiency of 60% (mass of hydride / total mass), this target material would produce a system gravimetric capacity of ≥ 4.5 wt %, consistent with the DOE 2007 target. The approach established for the project combined first principles modeling (FPM - UTRC) with multiple synthesis methods: Solid State Processing (SSP - UTRC), Solution Based Processing (SBP - Albemarle) and Molten State Processing (MSP - SRNL). In the search for novel compounds, each of these methods has advantages and disadvantages; by combining them, the potential for success was increased. During the project, UTRC refined its FPM framework which includes ground state (0 Kelvin) structural determinations, elevated temperature thermodynamic predictions and thermodynamic / phase diagram calculations. This modeling was used both to precede synthesis in a virtual search for new compounds and after initial synthesis to examine reaction details and options for modifications including co-reactant additions. The SSP synthesis method involved high energy ball milling which was simple, efficient for small batches and has proven effective for other storage material compositions. The SBP method produced very homogeneous chemical reactions, some of which cannot be performed via solid state routes, and would be the preferred approach for large scale production. The MSP technique is similar to the SSP method, but involves higher temperature and hydrogen pressure conditions to achieve greater species mobility. During the initial phases of the project, the focus was on higher order alanate complexes in the phase space

  20. Calcium absorption and achlorhydria

    International Nuclear Information System (INIS)

    Recker, R.R.

    1985-01-01

    Defective absorption of calcium has been thought to exist in patients with achlorhydria. The author compared absorption of calcium in its carbonate form with that in a pH-adjusted citrate form in a group of 11 fasting patients with achlorhydria and in 9 fasting normal subjects. Fractional calcium absorption was measured by a modified double-isotope procedure with 0.25 g of calcium used as the carrier. Mean calcium absorption (+/- S.D.) in the patients with achlorhydria was 0.452 +/- 0.125 for citrate and 0.042 +/- 0.021 for carbonate (P less than 0.0001). Fractional calcium absorption in the normal subjects was 0.243 +/- 0.049 for citrate and 0.225 +/- 0.108 for carbonate (not significant). Absorption of calcium from carbonate in patients with achlorhydria was significantly lower than in the normal subjects and was lower than absorption from citrate in either group; absorption from citrate in those with achlorhydria was significantly higher than in the normal subjects, as well as higher than absorption from carbonate in either group. Administration of calcium carbonate as part of a normal breakfast resulted in completely normal absorption in the achlorhydric subjects. These results indicate that calcium absorption from carbonate is impaired in achlorhydria under fasting conditions. Since achlorhydria is common in older persons, calcium carbonate may not be the ideal dietary supplement