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Sample records for hydride generation quartz

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-11-01

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

  2. 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.

  3. 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...

  4. 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).

  5. 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.

  6. Metal Hydrides for High-Temperature Power Generation

    Directory of Open Access Journals (Sweden)

    Ewa C. E. Rönnebro

    2015-08-01

    Full Text Available Metal hydrides can be utilized for hydrogen storage and for thermal energy storage (TES applications. By using TES with solar technologies, heat can be stored from sun energy to be used later, which enables continuous power generation. We are developing a TES technology based on a dual-bed metal hydride system, which has a high-temperature (HT metal hydride operating reversibly at 600–800 °C to generate heat, as well as a low-temperature (LT hydride near room temperature that is used for hydrogen storage during sun hours until there is the need to produce electricity, such as during night time, a cloudy day or during peak hours. We proceeded from selecting a high-energy density HT-hydride based on performance characterization on gram-sized samples scaled up to kilogram quantities with retained performance. COMSOL Multiphysics was used to make performance predictions for cylindrical hydride beds with varying diameters and thermal conductivities. Based on experimental and modeling results, a ~200-kWh/m3 bench-scale prototype was designed and fabricated, and we demonstrated the ability to meet or exceed all performance targets.

  7. 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.

  8. 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.

  9. Hydrogen generation from magnesium hydride by using organic acid

    Science.gov (United States)

    Ho, Yen-Hsi

    In this paper, the hydrolysis of solid magnesium hydride has been studied with the high concentration of catalyst at the varying temperature. An organic acid (acetic acid, CH3COOH) has been chosen as the catalyst. The study has three objectives: first, using three different weights of MgH 2 react with aqueous solution of acid for the hydrogen generation experiments. Secondly, utilizing acetic acid as the catalyst accelerates hydrogen generation. Third, emphasizing the combination of the three operating conditions (the weight of MgH2, the concentration of acetic acid, and the varying temperature) influence the amount of hydrogen generation. The experiments results show acetic acid truly can increase the rate of hydrogen generation and the weight of MgH2 can affect the amount of hydrogen generation more than the varying temperature.

  10. Arsenic speciation analysis by HPLC postcolumn hydride generation and detection by atomic fluorescence spectrometry

    OpenAIRE

    Marschner, K; Musil, S. (Stanislav); Rychlovský, P.; Dědina, J. (Jiří)

    2014-01-01

    The aim of this contribution is to present a new method of hydride generation that enables to generate arsines from iAs , iAs , MMA and DMA in a flow injection mode with the same efficiency and in the next step connection of this hydride generator with HPLC column.

  11. [Investigation of enhancing effect for hydride generation-atomic fluorescence of transition metal elements].

    Science.gov (United States)

    Sun, Han-Wen; Suo, Ran

    2008-11-01

    A mechanism of hydride generation based on disassembly reaction of hydrogen-transferred interim state [M(BH4)m]* was developed by investigating the effect of reaction medium acidity on hydride generation. The effects of Co2+ and Ni2+, phenanthroline and 8-hydroxyquinoline on hydride generation-atomic fluorescence signals of Zn, Cd, Cu and Ni were studied, respectively, and their enhancing mechnism was discussed. The enhancing effect Co2+ and Ni2+ on the fluorescence signals of Zn and Cd was due to the increase in transmission efficiency of hydride of Zn and Cd. There was a synergic enhancing effect between phenanthroline or 8-hydroxyquinoline and Co2+ on the fluorescence signals of Zn and Cd, however no synergic enhancing effect between phenanthroline and 8-hydroxyquinoline on the fluorescence signals of Zn and Cd. The simulative action of cationic surfactant, anion surfactant and non-ionic surfactant surfactant to hydride generation was investigated. It is shown that both cationic surfactant and non-ionic surfactant have obvious enhancing effect on the fluorescence signals of analytes because of the decrease in surface tension of reaction solution. The release characteristics of hydride from the absorption solution containing surfactant was ulteriorly examined by using graphite furnace atomic absorption spectrometry, and the mechanism of enhancing effect of surfactant on hydride generation and transmission was proposed.

  12. Dual-mode chemical vapor generation for simultaneous determination of hydride-forming and non-hydride-forming elements by atomic fluorescence spectrometry.

    Science.gov (United States)

    Wang, Yu; Xu, Kailai; Jiang, Xiaoming; Hou, Xiandeng; Zheng, Chengbin

    2014-05-21

    A dual-mode chemical vapor generation integrating hydride generation and photochemical vapor generation was developed for simultaneous multi-element analysis of hydride-forming and non-hydride-forming elements by atomic fluorescence spectrometry. Four elements were selected as model elements of hydride-forming (As, Cd) and non-hydride-forming (Ni, Fe) elements to validate this proposed method. Standard or sample solutions were separately pumped to mix with tetrahydroborate, and concentrated formic acid and ammonia, and then directed to a hydride generator and a photochemical reactor to realize simultaneous hydride generation and photochemical vapor generation, respectively. Optimum conditions for dual-mode chemical vapor generation were carefully investigated. Under the optimized conditions, limits of detection of 0.05, 0.008, 0.8 and 0.1 μg L(-1) were obtained for As, Cd, Fe and Ni, respectively. The precisions were 5.0, 5.5, 4.3 and 4.5% (n = 6, RSDs) for 2 μg L(-1) of As, 1 μg L(-1) of Cd, 50 μg L(-1) of Fe and 10 μg L(-1) of Ni, respectively. This method was validated for accuracy with three certified reference water samples and applied to the simultaneous determination of these elements in a tap water sample with spike recoveries in the range of 95-99%.

  13. 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.

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

    Science.gov (United States)

    Patki, Gauri Dilip

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

  15. Direct generation of oxygen-stabilized radicals by H• transfer from transition metal hydrides.

    Science.gov (United States)

    Kuo, Jonathan L; Hartung, John; Han, Arthur; Norton, Jack R

    2015-01-28

    Transition-metal hydrides generate α-alkoxy radicals by H• transfer to enol ethers. We have measured the rate constant for transfer from CpCr(CO)3H to n-butyl vinyl ether and have examined the chemistry of radicals generated by such transfers. Radicals from appropriate substrates undergo 5-exo cyclization, with higher diastereoselectivity than the analogous all-carbon radicals. From such radicals it is straightforward to make substituted tetrahydrofurans.

  16. Determination of lead in wine and rum samples by flow injection-hydride generation-atomic absorption spectrometry.

    Science.gov (United States)

    Elçi, Latif; Arslan, Zikri; Tyson, Julian F

    2009-03-15

    A method for direct determination of lead in wine and rum samples was developed, using a flow injection hydride generation system coupled to an atomic absorption spectrometer with flame-quartz atomizer (FI-HG-AAS). Lead hyride (PbH(4)) was generated using potassium ferricyanide (K(3)Fe(CN)(6)), as oxidant and sodium tetrahydroborate (NaBH(4)) as reductant. Samples were acidified to 0.40% (v/v) HCl for wine and to 0.30% (v/v) HCl for rum, which were then mixed on-line with 3% (m/v) K(3)Fe(CN)(6) solution in 0.03% (v/v) HCl prior to reaction with 0.2% (m/v) alkaline NaBH(4) solution. Lead contents of a rum and two different red wine samples were determined by FI-HG-AAS agreed with those obtained by ICP-MS. The analytical figures of merit of method developed were determined. The calibration curve was linear up to 8.0 microg L(-1) Pb with a regression coefficient of 0.998. The relative error was lower than 4.58%. The relative standard deviation (n=7) was better than 12%. A detection limit of 0.16 microg L(-1) was achieved for a sample volume of 170 microL.

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

    Energy Technology Data Exchange (ETDEWEB)

    Carrion, Nereida E-mail: ncarrion@strix.ciens.ucv.ve; Murillo, Miguel; Montiel, Edie; Diaz, Dorfe

    2003-08-15

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

  18. Dealloyed Ruthenium Film Catalysts for Hydrogen Generation from Chemical Hydrides

    Directory of Open Access Journals (Sweden)

    Ramis B. Serin

    2017-07-01

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

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

    Directory of Open Access Journals (Sweden)

    Chi-Chang Wang

    2014-05-01

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

  20. Experimental Hydrogen Plant with Metal Hydrides to Store and Generate Electrical Power

    Science.gov (United States)

    Gonzatti, Frank; Nizolli, Vinícius; Ferrigolo, Fredi Zancan; Farret, Felix Alberto; de Mello, Marcos Augusto Silva

    2016-02-01

    Generation of electrical energy with renewable sources is interruptible due to the primary energy characteristics (sun, wind, hydro, etc.). In these cases, it is necessary to use energy storage so increasing penetrability of these sources connected to the distribution system. This paper discusses in details some equipment and accessories of an integrated power plant using fuel cell stack, electrolyzer and metal hydrides. During the plant operation were collected the power consumption data and established the efficiency of each plant component. These data demonstrated an overall efficiency of about 11% due to the low efficiencies of the commercial electrolyzers and power inverters used in the experiments.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-09-01

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

  2. Automated determinations of selenium in thermal power plant wastewater by sequential hydride generation and chemiluminescence detection.

    Science.gov (United States)

    Ezoe, Kentaro; Ohyama, Seiichi; Hashem, Md Abul; Ohira, Shin-Ichi; Toda, Kei

    2016-02-01

    After the Fukushima disaster, power generation from nuclear power plants in Japan was completely stopped and old coal-based power plants were re-commissioned to compensate for the decrease in power generation capacity. Although coal is a relatively inexpensive fuel for power generation, it contains high levels (mgkg(-1)) of selenium, which could contaminate the wastewater from thermal power plants. In this work, an automated selenium monitoring system was developed based on sequential hydride generation and chemiluminescence detection. This method could be applied to control of wastewater contamination. In this method, selenium is vaporized as H2Se, which reacts with ozone to produce chemiluminescence. However, interference from arsenic is of concern because the ozone-induced chemiluminescence intensity of H2Se is much lower than that of AsH3. This problem was successfully addressed by vaporizing arsenic and selenium individually in a sequential procedure using a syringe pump equipped with an eight-port selection valve and hot and cold reactors. Oxidative decomposition of organoselenium compounds and pre-reduction of the selenium were performed in the hot reactor, and vapor generation of arsenic and selenium were performed separately in the cold reactor. Sample transfers between the reactors were carried out by a pneumatic air operation by switching with three-way solenoid valves. The detection limit for selenium was 0.008 mg L(-1) and calibration curve was linear up to 1.0 mg L(-1), which provided suitable performance for controlling selenium in wastewater to around the allowable limit (0.1 mg L(-1)). This system consumes few chemicals and is stable for more than a month without any maintenance. Wastewater samples from thermal power plants were collected, and data obtained by the proposed method were compared with those from batchwise water treatment followed by hydride generation-atomic fluorescence spectrometry.

  3. High-harmonic generation in alpha-quartz by the electron-hole recombination

    CERN Document Server

    Otobe, T

    2016-01-01

    The first-principle calculation for the high-harmonic generation (HHG) in an alpha-quartz employing the time-dependent density-functional theory is reported. The photon energy is set to 1.55 eV, and the cutoff energy of the plateau region is found to be limited at the 19th harmonics (30 eV). The laser intensity dependence of HHG efficiency at the cutoff energy region is consistent with that of the hole density in the lowest-lying valence band. Numerical results indicate that the electron-hole recombination plays a crucial role in HHG in alpha-quartz. It is found that the 200 attosecond pulse train is generated utilizing HHG around the plateau cutoff energy.

  4. [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.

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

    Science.gov (United States)

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

    2007-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-03-15

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

  7. Spectrophotometric detection of arsenic using flow-injection hydride generation following sorbent extraction preconcentration.

    Science.gov (United States)

    Neto, J A; Montes, R; Cardoso, A A

    1999-12-06

    An automated system with a C(18) bonded silica gel packed minicolumn is proposed for spectrophotometric detection of arsenic using flow-injection hydride generation following sorbent extraction preconcentration. Complexes formed between arsenic(III) and ammonium diethyl dithiophosphate (ADDP) are retained on a C(18) sorbent. The eluted As-DDP complexes are merged with a 1.5% (w/v) NaBH(4) and the resulting solution is thereafter injected into the hydride generator/gas-liquid separator. The arsine generated is carried out by a stream of N(2) and trapped in an alkaline iodine solution in which the analyte is determined by the arsenomolybdenum blue method. With preconcentration time of 120 s, calibration in the 5.00-50.0 mug As l(-1) range and sampling rate of about 20 samples h(-1) are achieved, corresponding to 36 mg ADDP plus 36 mg ammonium heptamolybdate plus 7 mg hydrazine sulfate plus 0.7 mg stannous chloride and about 7 ml sample consumed per determination. The detection limit is 0.06 mug l(-1) and the relative standard deviation (n=12) for a typical 17.0 mug As l(-1) sample is ca. 6%. The accuracy was checked for arsenic determination in plant materials from the NIST (1572 citrus leaves; 1573 tomato leaves) and the results were in agreement with the certified values at 95% confidence level. Good recoveries (94-104%) of spiked tap waters, sugars and synthetic mixtures of trivalent and pentavalent arsenic were also found.

  8. High-harmonic generation in α -quartz by electron-hole recombination

    Science.gov (United States)

    Otobe, T.

    2016-12-01

    A calculation of the high-harmonic generation (HHG) in α -quartz using the time-dependent density functional theory is reported. The interband process is attributed to the dominant in HHG above the band gap. The photon energy is set to 1.55 eV, and the cutoff energy of the plateau region is found to be limited at the 19th harmonic (30 eV). The dependence of the HHG efficiency at the cutoff energy region on laser intensity is consistent with that of the hole density in the lowest-lying valence band. Numerical results indicate that electron-hole recombination plays a crucial role in HHG in α -quartz. It is found that a 200 attosecond pulse train is produced using HHG around the plateau cutoff energy.

  9. Laser ultrasonic analysis of normal modes generated by a voltage pulse on an AT quartz sensor.

    Science.gov (United States)

    Goossens, Jozefien; Martinez, Loïc; Glorieux, Christ; Wilkie-Chancellier, Nicolas; Ehssein, Chighali Ould; Serfaty, Stéphane

    2006-12-22

    Laser ultrasonic detection is a versatile and highly sensitive tool for the observation of surface waves. In the following study, laser ultrasonic detection is used for the experimental study of spurious normal vibration modes of a disk quartz sensor excited by a voltage pulse. The AT cut crystal (cut of the crystal relative to the the main crystallographic axis is 35.25 degrees) is optimal for generating mainly thickness-shear vibrations (central frequency 6 MHz) on the quartz surface. However, resulting from shear-to-longitudinal and shear-to-surface mode conversion, and from the weak coupling with the other crystallographic axes, other modes (thickness-compressional and bending modes) are always present in the plate response. Since the laser vibrometer is sensitive to normal displacements, the laser investigation shows waves that can be considered as unwanted for the AT quartz used as a shear sensor. The scanned three dimensional (3D) amplitude-space-time signals are carefully analysed using their representation in three dual Fourier domains (space-time, wave number-frequency). Results on the transient analysis of the waves, the normal bending modes and the dispersion curves are shown.

  10. Reduced enthalpy of metal hydride formation for Mg-Ti nanocomposites produced by spark discharge generation.

    Science.gov (United States)

    Anastasopol, Anca; Pfeiffer, Tobias V; Middelkoop, Joost; Lafont, Ugo; Canales-Perez, Roger J; Schmidt-Ott, Andreas; Mulder, Fokko M; Eijt, Stephan W H

    2013-05-29

    Spark discharge generation was used to synthesize Mg-Ti nanocomposites consisting primarily of a metastable body-centered-cubic (bcc) alloy of Mg and Ti. The bcc Mg-Ti alloy transformed upon hydrogenation into the face-centered-cubic fluorite Mg1-yTiyHx phase with favorable hydrogen storage properties. Both metal and metal hydride nanocomposites showed a fractal-like porous morphology, with a primary particle size of 10-20 nm. The metal content of 70 atom % (at %) Mg and 30 at % Ti, consistently determined by XRD, TEM-EDS, and ICP-OES, was distributed uniformly across the as-prepared sample. Pressure-composition isotherms for the Mg-Ti-H nanocomposites revealed large differences in the thermodynamics relative to bulk MgH2, with a much less negative enthalpy of formation of the hydride as small as -45 ± 3 kJ/molH2 as deduced from van't Hoff plots. The plateau pressures of hydrogenation were substantially higher than those for bulk MgH2 in the low temperature range from 150 to 250 °C. The reaction entropy was simultaneously reduced to values down to 84 ± 5 J/K mol H2, following a linear relationship between the enthalpy and entropy. Plausible mechanisms for the modified thermodynamics are discussed, including the effect of lattice strains, the presence of interfaces and hydrogen vacancies, and the formation of excess free volume due to local deformations. These mechanisms all rely on the finely interdispersed nanocomposite character of the samples which is maintained by grain refinement.

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

    Science.gov (United States)

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

    1992-08-01

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

  12. Application of metal hydride paper to simple pressure generator for use in soft actuator systems.

    Science.gov (United States)

    Ino, Shuichi; Sakaki, Kouji; Hosono, Minako; Doi, Kouki; Shimada, Shigenobu; Chikai, Manabu

    2015-01-01

    Metal hydride (MH) actuators have a simple structure and a number of features that make them attractive for use in rehabilitation engineering and assistive technology. The MH actuator provides a high power-to-weight ratio, high-strain actuation, human-compatible softness, and noiseless operation, while being environmentally benign. On the other hand, there remain technical challenges to be overcome to improve the MH actuator regarding its speed of operation and energy efficiency, given the low heat conductivity of the MH powder that is used as the pressure generator for soft actuation. To overcome the issues of low heat conductivity and the handling of MH powder, we developed an MH paper, which is a special paper incorporating MH powder and carbon fiber, for use as a new pressure-generating element for a soft MH actuator system. In addition, the basic properties and structure of the proposed MH paper were investigated through scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and several thermodynamic experiments. The results of these experiments showed that the hydrogen absorption and desorption rates of the MH paper were significantly higher than those of the MH powder around room temperature.

  13. Aerosol generation of As and Se hydrides using a new Flow Blurring® multiple nebulizer for sample introduction in inductively coupled plasma optical emission spectrometry

    OpenAIRE

    Pereira, Catarinie D.; Aguirre Pastor, Miguel Ángel; NÓBREGA, Joaquim A.; Hidalgo Núñez, Montserrat; Canals Hernández, Antonio

    2014-01-01

    A new Flow Blurring® multiple nebulizer (FBMN) has been used for the efficient generation of As and Se hydrides directly into the aerosol formed inside the spray chamber before detection by inductively coupled plasma optical emission spectrometry (ICP OES). The FBMN allowed the hydride generation directly into the spray chamber without using any additional device either for solution and gas control or for gas phase separation. Synthetic solutions containing As and Se plus Ca, Mg and K were us...

  14. Determination of inorganic species of Sb and Te in cereals by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reyes, Mariela N.M.; Cervera, Maria L.; Guardia, Miguel de la, E-mail: m.luisa.cervera@uv.e [University of Valencia, Valencia (Spain). Dept. of Analytical Chemistry

    2011-07-01

    A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L{sup -1} phosphoric acid, 1 mol L{sup -1} nitric acid, aqua regia, 1 mol L{sup -1} sulfuric acid and 6 mol L{sup -1} hydrochloric acid. The extraction with aqua regia showed a clear interconversion of the species during the process, being H{sub 2}SO{sub 4} the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g{sup -1} with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species. (author)

  15. Investigation of the direct hydride generation nebulizer for the determination of arsenic, antimony and selenium in inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rojas, Illiana; Murillo, Miguel; Carrion, Nereida; Chirinos, Jose [Centro de Quimica Analitica, Escuela de Quimica, Facultad de Ciencias, Universidad Central de Venezuela, P.O. Box 47102, 1041a, Caracas (Venezuela)

    2003-05-01

    A direct hydride generation nebulizer (DHGN) was explored for introduction of the sample in inductively coupled plasma-optical emission spectrometry (ICP-OES) using radially viewed mode. This simple hydride generation system was constructed in our laboratory and requires similar plasma operating conditions to conventional nebulizer-spray-chamber arrangements. This work was focused on the optimization of the operating conditions for hydride generation and evaluation of the main analytical figures of merit for the determination of As, Sb and Se. The excitation conditions of the ICP-OES instrument operated with the DHGN were also explored. Results showed that the analytical performance of the new system for the determination of As, Sb and Se was superior to that of conventional nebulization systems. The DHGN also enabled the determination of elements that do not form volatile hydrides, but with less sensitivity than conventional nebulization systems. Evaluation of the plasma robustness showed that gases generated in hydride generation do not significantly affects the plasma discharge. Similar to conventional hydride generation techniques, analysis with DHGN was susceptible to non-spectroscopic interferences produced by transition metals. Finally, the utility of the DHGN in practical ICP-OES studies was demonstrated in the determination of trace elements in an oyster tissue standard reference material. (orig.)

  16. The influence of vibrations on time reference signals generated using quartz crystals

    Science.gov (United States)

    Drumea, Andrei; Marcu, Alina; Plotog, Ioan

    2016-12-01

    32.768 kHz low frequency crystals are found in a large part of today's embedded systems that use microcontrollers especially in battery supplied applications which need low power consumption1]. Their main role is to offer a stable time reference. There are situations in which time measurement is needed when the system works in a mechanically unstable environment (cars, industrial equipment). The paper presents the studies done on the behavior of 32.768 kHz quartz crystals that are part of embedded systems which operate in a vibrating environment, in terms of period and long-time jitter of the generated time reference signal. The investigations of this effect were done using a test bench especially designed for this purpose which can measure the presented parameters determined by controlled mechanical stimulus (waveform, amplitude and frequency of the vibrations).

  17. Determination of arsenic and selenium by hydride generation and headspace solid phase microextraction coupled with optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tyburska, Anna; Jankowski, Krzysztof, E-mail: kj@ch.pw.edu.pl; Rodzik, Agnieszka

    2011-07-15

    A hydride generation headspace solid phase microextraction technique has been developed in combination with optical emission spectrometry for determination of total arsenic and selenium. Hydrides were generated in a 10 mL volume septum-sealed vial and subsequently collected onto a polydimethylsiloxane/Carboxen solid phase microextraction fiber from the headspace of sample solution. After completion of the sorption, the fiber was transferred into a thermal desorption unit and the analytes were vaporized and directly introduced into argon inductively coupled plasma or helium microwave induced plasma radiation source. Experimental conditions of hydride formation reaction as well as sorption and desorption of analytes have been optimized showing the significant effect of the type of the solid phase microextraction fiber coating, the sorption time and hydrochloric acid concentration of the sample solution on analytical characteristics of the method developed. The limits of detection of arsenic and selenium were 0.1 and 0.8 ng mL{sup -1}, respectively. The limit of detection of selenium could be improved further using biosorption with baker's yeast Saccharomyces cerevisiae for analyte preconcentration. The technique was applied for the determination of total As and Se in real samples.

  18. Flow injection on-line solid phase extraction for ultra-trace lead screening with hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Wan, Zhuo; Xu, Zhangrun; Wang, Jianhua

    2006-01-01

    A flow injection (FI) on-line solid phase extraction (SPE) procedure for ultra-trace lead separation and preconcentration was developed, followed by hydride generation and atomic fluorescence spectrometric (AFS) detection. Lead is retained on an iminodiacetate chelating resin packed microcolumn, and is afterward eluted with 2.5% (v/v) hydrochloric acid to facilitate the hydride generation by reaction with alkaline tetrahydroborate solution with 1% (m/v) potassium ferricyanide as an oxidizing (or sensitizing) reagent. The hydride was separated from the reaction medium in the gas-liquid separator and swept into the atomizer for quantification. The chemical variables and the FI flow parameters were carefully optimized. With a sample loading volume of 4.8 ml, quantitative retention of lead was obtained, along with an enrichment factor of 11.3 and a sampling frequency of 50 h(-1). A detection limit of 4 ng l(-1), defined as 3 times the blank standard deviation (3 sigma), was achieved along with a RSD value of 1.6% at the 0.4 microg l(-1) level. The procedure was validated by determining lead contents in two certified reference materials, and its practical applicability was further demonstrated by analysing a variety of biological and environmental samples.

  19. Hydride and ethylated species generation from ordered media: application to the enhanced ICP-AES determination of bismuth

    Energy Technology Data Exchange (ETDEWEB)

    Villanueva Tagle, M.; Fernandez de la Campa, M.R.; Sanz-Medel, A. [Department of Physical and Analytical Chemistry, University of Oviedo, Oviedo (Spain)

    1996-11-01

    Earlier work to enhance the efficiency of volatile species generation for atomic spectrometry has demonstrated that organised media, micelles and vesicles, offer a new chemical microenvironment able to improve the thermodynamics and/or kinetics of volatile species generation (hydrides and alkyl compounds). Detection limit can be further improved in this way for ICP-AES detection. In this line the characteristics of volatile species generation of Bi, Ge and In in micellar and vesicular media are studies and critically compared with those obtained in the absence of organized media, Both NaBH{sub 4} and NaBEt{sub 4} reagents for volatile species production have been tested. Bismuth determination was clearly improved by using cationic sufactants, both with NaBH{sub 4} and NaBEt{sub 4} as reducing agents. Thus, the determination of Bi enhanced by either NaBH{sub 4} or NaBEt{sub 4} in organized media with ICP-AES for final specific detection, is described in detail. Bismuth hydride generated from Triton X-100 allowed decrease of detection limits of Bi by ICP-AES from 4 to 1 ng ml``-1. The calibration graphs were linear up to 200 ng ml``-1, with RDS of 1% at 60 ng ml``-1 level. Improved tolerance to interfering elements in organized media, as compared to more conventional hydride generation, was observed. Bi ethylation using NaBEt{sub 4} provided volatile species generation-ICP-AEs detection of the metal characterized by a detection limit of 2 ng ml``-1 eventually attained for Bi. The calibration graphs were linear up to 200 ng ml``-1 with a RDS of 2% at 60 ng ml``-1 level. Effects of addition of different organised media to improve volatile Bi species generation with the ethylation agent NaBEt{sub 4} are reported for the first time. (Author) 29 refs.

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

    Institute of Scientific and Technical Information of China (English)

    LI Xun; WANG Zheng-Hao

    2007-01-01

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

  1. Combined optical second harmonic generation/quartz crystal microbalance study of underpotential deposition processes: copper electrodeposition on polycrystalline gold.

    Science.gov (United States)

    Lakkaraju, S; Bennahmias, M J; Borges, G L; Gordon Ii, J G; Lazaga, M; Stone, B M; Ashley, K

    1990-11-20

    Optical second harmonic generation and quartz crystal microbalance techniques are used as in situ probes of copper underpotential deposition on polycrystalline gold surfaces in sulfuric acid electrolyte. The second harmonic signal from a polished bulk gold substrate is observed to decrease by >60% as a result of copper underpotential deposition on gold. Also, the mass of an underpotentially deposited copper adlayer is monitored in situ by an oscillating quartz crystal microbalance, yielding an estimated coverage of ~8.0 x 10(-10) mol cm(-2) and an electrosorption valency of 1.5 for a copper adlayer on the surface of vapor-deposited polycrystalline gold.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1998-08-01

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

  3. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Potin-Gautier, M. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Pannier, F. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France)]. E-mail: Florence.pannier@univ-pau.fr; Quiroz, W. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Pinochet, H. [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Gregori, I. de [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile)

    2005-11-30

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

  5. 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.

  6. A novel analytical system involving hydride generation and gold-coated W-coil trapping atomic absorption spectrometry for selenium determination at ng l{sup -1} level

    Energy Technology Data Exchange (ETDEWEB)

    Kula, I. [Department of Chemistry, Mugla University, 48000 Mugla (Turkey); Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Arslan, Y. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Atatuerk University, 25240 Erzurum (Turkey); Bakirdere, S. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Zonguldak Karaelmas University, 67100 Zonguldak (Turkey); Ataman, O.Y. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey)], E-mail: ataman@metu.edu.tr

    2008-08-15

    A novel analytical technique was developed where gaseous hydrogen selenide formed by sodium tetrahydroborate reduction is transported to and trapped on a resistively heated gold-coated W-coil atom trap for in situ preconcentration. Gold coating on W-coil was prepared by using an organic solution of Au. The atom trap is held at 165 {sup o}C during the collection stage and is heated up to 675 deg. C for revolatilization; analyte species formed are transported to an externally heated quartz T-tube where the atomization takes place and the transient signal is obtained. The carrier gas consisted of 112.5 ml min{sup -1} Ar with 75 ml min{sup -1} H{sub 2} during the collection step and 112.5 ml min{sup -1} Ar with 450 ml min{sup -1} H{sub 2} in the revolatilization step. The half width of the transient signal obtained is less than 0.5 s. The RSD for the measurements was found to be 3.9% (n = 11) for 0.10 {mu}g l{sup -1} Se using peak height measurements. The calibration plot for 27.0 ml of sample collected in 4.0 min using a flow rate of 6.75 ml min{sup -1} was linear between 0.13 and 2.0 {mu}g l{sup -1} of Se. The limit of detection (3 s) is 39 ng l{sup -1}. The enhancement factor for the characteristic concentration (C{sub o}) was found to be 20.1 when compared to conventional hydride generation atomic absorption spectrometry system without trap. In order to check the accuracy of the method, standard reference material, natural water NIST 1640 was employed; the result was found to be in good agreement with the certified value at the 95% confidence level.

  7. A novel analytical system involving hydride generation and gold-coated W-coil trapping atomic absorption spectrometry for selenium determination at ng l - 1 level

    Science.gov (United States)

    Kula, İ.; Arslan, Y.; Bakırdere, S.; Ataman, O. Y.

    2008-08-01

    A novel analytical technique was developed where gaseous hydrogen selenide formed by sodium tetrahydroborate reduction is transported to and trapped on a resistively heated gold-coated W-coil atom trap for in situ preconcentration. Gold coating on W-coil was prepared by using an organic solution of Au. The atom trap is held at 165 °C during the collection stage and is heated up to 675 °C for revolatilization; analyte species formed are transported to an externally heated quartz T-tube where the atomization takes place and the transient signal is obtained. The carrier gas consisted of 112.5 ml min - 1 Ar with 75 ml min - 1 H 2 during the collection step and 112.5 ml min - 1 Ar with 450 ml min - 1 H 2 in the revolatilization step. The half width of the transient signal obtained is less than 0.5 s. The RSD for the measurements was found to be 3.9% ( n = 11) for 0.10 µg l - 1 Se using peak height measurements. The calibration plot for 27.0 ml of sample collected in 4.0 min using a flow rate of 6.75 ml min - 1 was linear between 0.13 and 2.0 µg l - 1 of Se. The limit of detection (3 s) is 39 ng l - 1 . The enhancement factor for the characteristic concentration ( Co) was found to be 20.1 when compared to conventional hydride generation atomic absorption spectrometry system without trap. In order to check the accuracy of the method, standard reference material, natural water NIST 1640 was employed; the result was found to be in good agreement with the certified value at the 95% confidence level.

  8. Synchrotron generated X-ray Excited Optical Luminescence (XEOL) from Quartz

    Science.gov (United States)

    King, Georgina; Finch, Adrian; Robinson, Ruth

    2010-05-01

    Quartz is the preferred mineral for optically stimulated luminescence (OSL) dating, due to its well constrained behaviour as a radiation dosimeter. However, despite the plethora of successful quartz OSL applications, no solution has been found to the problem that some quartz luminesce more brightly than others, which has limited the application of OSL in certain settings. This has been addressed through examination of the luminescence emission using a variety of excitation techniques and emission spectroscopy. X-ray Excited Optical Luminescence (XEOL) is luminescence excited by x-rays produced by a synchrotron. XEOL analyses were conducted upon a suite of quartz samples at Diamond, Great Britain, which had previously been analysed with Ionoluminescence (IL), at Sussex University. The samples were selected to include quartz of both poor and excellent OSL sensitivities. Therefore, two Scottish glacial outwash samples prepared at St Andrews, and a calibration quartz sample, prepared at the Risø National Laboratory in Denmark were analysed for these properties respectively. The XEOL emission spectra comprised three major emissions at 3.32, 3.81 and 4.05 eV, and one weaker emission at 1.94 eV in all samples. The calibration quartz sample had the most intense emission by an order of magnitude. Throughout increased exposure to x-rays, the intensity of the UV emission reduced, and an increase in the red (1.94 eV) emission was recorded. The derived XEOL spectra complement the IL spectra obtained previously. The IL spectra were dominated by only two broad emissions at 3.2-3.1 eV and 1.8-1.7 eV. However, throughout the IL experiments a dose dependent effect was also observed, whereby the UV emission was depleted to the benefit of the red with increasing exposure. Furthermore the gradient of the power law relationship between the UV and red emission change with dose is similar for both the IL and XEOL data: at -1.15 and -1.05 respectively for calibration quartz, when plotted

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

    Science.gov (United States)

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

    2001-10-01

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

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

    Directory of Open Access Journals (Sweden)

    Santos Éder José dos

    2001-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Miguel Murillo

    2008-01-01

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

  12. 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.

  13. Fundamental investigations of natural and laboratory generated SAR dose response curves for quartz OSL in the high dose range

    DEFF Research Database (Denmark)

    Timar-Gabor, Alida; Constantin, Daniela; Buylaert, Jan-Pieter

    2015-01-01

    SAR-OSL investigations on quartz from Romanian loess resulted in non concordant fine and coarse-grain ages for equivalent doses higher than ~100 Gy. The laboratory dose response for both grain sizes is well represented by a sum of two saturating exponential functions, fine and coarse grains chara...... equivalent dose of 2000e2500 Gy were found to be below the saturation level of the laboratory dose response curve for both grain sizes; this also applied to the luminescence signals measured after >5000 Gy given on top of natural doses. © 2015 Elsevier Ltd. All rights reserved....... characterised by D01 and D02 values of ~140 and ~1400 Gy and ~65 and ~650 Gy respectively. Pulsed OSL experiments confirmed that this behaviour is almost certainly inherent to quartz and not caused by contamination with another mineral. Natural doseeresponse curves do not follow the same pattern and enter...... saturation much earlier. Analysis of time resolved spectra indicated similar luminescence lifetimes for both fine and coarse quartz grains, and natural and laboratory generated OSL signals seem to use the same non-dosedependent recombination pathways. The natural signals of a sample with an expected...

  14. Method of producing a chemical hydride

    Science.gov (United States)

    Klingler, Kerry M.; Zollinger, William T.; Wilding, Bruce M.; Bingham, Dennis N.; Wendt, Kraig M.

    2007-11-13

    A method of producing a chemical hydride is described and which includes selecting a composition having chemical bonds and which is capable of forming a chemical hydride; providing a source of a hydrocarbon; and reacting the composition with the source of the hydrocarbon to generate a chemical hydride.

  15. Enhanced Hydrogen Generation Properties of MgH2-Based Hydrides by Breaking the Magnesium Hydroxide Passivation Layer

    Directory of Open Access Journals (Sweden)

    Liuzhang Ouyang

    2015-05-01

    Full Text Available Due to its relatively low cost, high hydrogen yield, and environmentally friendly hydrolysis byproducts, magnesium hydride (MgH2 appears to be an attractive candidate for hydrogen generation. However, the hydrolysis reaction of MgH2 is rapidly inhibited by the formation of a magnesium hydroxide passivation layer. To improve the hydrolysis properties of MgH2-based hydrides we investigated three different approaches: ball milling, synthesis of MgH2-based composites, and tuning of the solution composition. We demonstrate that the formation of a composite system, such as the MgH2/LaH3 composite, through ball milling and in situ synthesis, can improve the hydrolysis properties of MgH2 in pure water. Furthermore, the addition of Ni to the MgH2/LaH3 composite resulted in the synthesis of LaH3/MgH2/Ni composites. The LaH3/MgH2/Ni composites exhibited a higher hydrolysis rate—120 mL/(g·min of H2 in the first 5 min—than the MgH2/LaH3 composite— 95 mL/(g·min—without the formation of the magnesium hydroxide passivation layer. Moreover, the yield rate was controlled by manipulation of the particle size via ball milling. The hydrolysis of MgH2 was also improved by optimizing the solution. The MgH2 produced 1711.2 mL/g of H2 in 10 min at 298 K in the 27.1% ammonium chloride solution, and the hydrolytic conversion rate reached the value of 99.5%.

  16. 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

  17. 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.

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

    Science.gov (United States)

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

    2007-06-01

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

  19. Field cryofocussing hydride generation applied to the simultaneous multi-elemental determination of alkyl-metal(loid) species in natural waters using ICP-MS detection.

    Science.gov (United States)

    Tseng, C M; Amouroux, D; Brindle, I D; Donard, O F

    2000-12-01

    Two hydride generation manifold systems, utilizing flow injection and cryotrapping techniques for alkyl-metal(loid) speciation analysis in natural waters, are described in this paper. They provide shipboard capacity for simultaneous derivatization of analytes with NaBH4 and cryotrapping of the generated products in a field packed column at -196 degrees C. The first system is a large-volume hydride generator, using a reagent-injection flow technique as a flow batch type, that has been fully optimized and applied to the simultaneous detection of alkylated species in estuarine waters. The technique permits the analysis of a large volume sample (0.5-11) at a sampling rate of 3 h-1. The second is an online continuous flow hydride generator. A sampling rate of 3-12 h-1 can be achieved with samples of 0.1-0.51. In addition, shipboard operation eliminates major problems related to sample pretreatment, transport and storage. Ultra-trace multi-element determination is finally performed in the laboratory by cryogenic GC hyphenated with ICP-MS. Routine detection limits of 0.5-10 pg (as metal) for 0.51 water samples were achieved for the selected alkyl-metal(loid) species of arsenic, germanium, mercury and tin. Concentrations of various species, obtained from water samples taken from the Rhine estuary, are also presented. These species include alkylated arsenic compounds, other than methyl derivatives, that have been tentatively identified and are reported here for the first time.

  20. Determination of trace selenium in high purity tellurium by hydride generation atomic fluorescence spectrometry after solid phase extraction of a diaminobenzidine-selenium chelate

    Science.gov (United States)

    Tong, Wang; Ying, Zeng; Jinyong, Xu

    2016-09-01

    Macroporous adsorption resin was used as the sorbent for solid phase extraction and determination of the trace Se content in high purity tellurium prior to hydride generation atomic fluorescence spectrometry analysis. Selenium was converted into an organic Se chelate using 3,3‧-diaminobenzidine and was separated from the tellurium matrix by solid phase extraction. The resin was packed as a column for solid phase extraction. Under optimum conditions, trace Se can be quantitatively extracted and the tellurium matrix can be removed. The Se in the eluate was determined by hydride generation atomic fluorescence spectrometry. The limit of detection (3σ) of this method was 0.22 ng g- 1 and the relative standard deviation (RSD, n = 5) ranged from 2.0 to 2.5% for the three investigated tellurium samples. The proposed method was successfully applied for the determination of the trace Se content in high purity tellurium samples.

  1. [Determination of trace lead in traditional Chinese herbal medicine Astragalus by microwave digestion-CTAB enhancing-continual flow ingection hydride generation-ICP-AES].

    Science.gov (United States)

    Liu, Dong-Lian; Ke, Shao-Ying; Ye, Rong; Ding, Ming-Yu

    2007-11-01

    A new method using microwave digestion technique was developed for the determination of lead in Astragalus by CTAB enhancing-continual flow hydride generation-inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). The experimental conditions of microwave digestion and hydride generation were optimized. This method shows a linear range of 0.23-800 microg x L(-1) and the correlation coefficient is 0.999 9. It is satisfactory to apply the microwave digestion procedure to the determination of Pb under the optimized conditions. The detection limit of the method is 0.23 microg x L(-1) and the RSD is 1.02%. The recovery obtained is 98.8%-100.1%. The results show that this method is rapid and simple with low environmental contamination and complete digestion of samples.

  2. Determination of Mecruy at Trace Level in Natural Water Samples by Hydride Generation Atomic Absorption Spectrophotometry after Cloud Point Extraction Preconcentration

    Institute of Scientific and Technical Information of China (English)

    Ji Ying SONG; Ming HOU; Li Xiang ZHANG

    2006-01-01

    A method for the determination of trace mercury in water samples by hydride generation atomic absorption spectrophotometry after cloud point extraction was proposed in the present work.The effects of pH, concentration of surfactant, and equilibration time on cloud point extraction were discussed. The enhancement factor of 20 and the detection limit of 0.039 μg/L were obtained for mercury with relative standard deviation of 4.8% (n = 11).

  3. Development of an analytical method for antimony speciation in vegetables by HPLC-hydride generation-atomic fluorescence spectrometry.

    Science.gov (United States)

    Olivares, David; Bravo, Manuel; Feldmann, Jorg; Raab, Andrea; Neaman, Alexander; Quiroz, Waldo

    2012-01-01

    A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 microg/L and 5.0, 5.2, and 4.7%, respectively, for a 100 microL sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts.

  4. Determination of total arsenic in coal and wood using oxygen flask combustion method followed by hydride generation atomic absorption spectrometry.

    Science.gov (United States)

    Geng, Wenhua; Furuzono, Takuya; Nakajima, Tsunenori; Takanashi, Hirokazu; Ohki, Akira

    2010-04-15

    A simple and sensitive procedure for the determination of total arsenic in coal and wood was conducted by use of oxygen flask combustion (OFC) followed by hydride generation atomic absorption spectrometry (HGAAS). The effect of various items (composition of absorbent, standing time between the combustion and filtration, particle size and mass of sample) was investigated. Under the optimized conditions of the OFC method, nine certified reference materials were analyzed, and the values of arsenic concentration obtained by this method were in good accordance with the certified values. The limit of detection (LOD) and relative standard deviation (RSD) of the method were 0.29 microg g(-1) and less than 8%, respectively. In addition, eight kinds of coals and four chromated copper arsenate (CCA)-treated wood wastes were analyzed by the present method, and the data were compared to those from the microwave-acid digestion (MW-AD) method. The determination of arsenic in solid samples was discussed in terms of applicable scope and concentration range of arsenic.

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

    Science.gov (United States)

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

    2015-09-01

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

  6. 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.

  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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-07-15

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

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

    Science.gov (United States)

    Yilmaz, Vedat; Arslan, Zikri; Rose, LaKeysha

    2013-01-25

    A hydride generation (HG) procedure has been described for determination of Pb by ICP-MS using potassium hexacyanomanganate(III), K(3)Mn(CN)(6), as an additive to facilitate the generation of plumbane (PbH(4)). Potassium hexacyanomanganate(III) was prepared in acidic medium as it was unstable in water. The stability of hexacyanomanganate(III) was examined in dilute solutions of HCl, HNO(3) and H(2)SO(4). The solutions prepared in 1% v/v H(2)SO(4) were found to be stable for over a period of 24h. The least suitable medium was 1% v/v HNO(3). For generation of plumbane, acidic hexacyanomanganate(III) and sample solutions were mixed on-line along a 5-cm long tygon tubing (1.14 mm i.d.) and then reacted with 2% m/v sodium borohydride (NaBH(4)). A concentration of 0.5% m/v K(3)Mn(CN)(6) facilitated the generation of PbH(4) remarkably. In comparison to H(2)SO(4), HCl provided broader working range for which optimum concentration was 1% v/v. No significant interferences were noted from transition metals and hydride forming elements, up to 0.5 μg mL(-1) levels, except Cu which depressed the signals severely. The depressive effects in the presence of 0.1 μg mL(-1) Cu were alleviated by increasing the concentration of K(3)Mn(CN)(6) to 2% m/v. Under these conditions, the sensitivity was enhanced by a factor of at least 42 to 48. The detection limit (3s) was 0.008 μg L(-1) for (208)Pb isotope. Average signal-to-noise ratio (S/N) ranged between 18 and 20 for 1.0 μg mL(-1) Pb solution. The accuracy of the method was verified by analysis of several certified reference materials, including Nearshore seawater (CASS-4), Bone ash (SRM 1400), and Mussel tissue (SRM 2976). The procedure was also successfully applied to the determination of Pb in coastal seawater samples by ICP-MS.

  10. Generation of Optical Vortex Using a Spiral Phase Plate Fabricated in Quartz by Direct Laser Writing and Inductively Coupled Plasma Etching

    Institute of Scientific and Technical Information of China (English)

    CHEN Jun; KUANG Deng-Feng; GUI Min; FANG Zhi-Liang

    2009-01-01

    A simple, economical and reliable technique is proposed for fabricating a spiral phase plate (SPP) in a quartz substrate to generate optical vortex with a unit topological charge at the wavelengths of 632.8nm. The spiral phase plate is first formed in the photoresist by direct laser writing lithography and then transferred into the quartz substrate by inductively coupled plasma etching. The performance of the fabricated SPP is verified by using beam intensity distribution, which is in agreement with the theoretical calculation result. The interference measurement suggests that we have succeeded to generate opticM vortex with a unit topological charge with the fabricated SPP.

  11. Studies in hydride generation atomic fluorescence determination of selenium and tellurium. Part 1 — self interference effect in hydrogen telluride generation and the effect of KI

    Science.gov (United States)

    D'Ulivo, A.; Marcucci, K.; Bramanti, E.; Lampugnani, L.; Zamboni, R.

    2000-08-01

    The effects of tetrahydroborate (0.02-1%) and iodide (0-3 M) were investigated in determination of tellurium and selenium by hydride generation atomic fluorescence spectrometry. The effect of tetrahydroborate and iodide concentration were tested on the shape of calibration curves in concentration range of 1-1000 ng ml -1 analyte. Reductant deficiency resulted in a moderate sensitivity depression for tellurium but dramatically reduced the useful dynamic range down to 50 ng ml -1. On the contrary, selenium calibration curves retained a linear character even under conditions generating strong sensitivity depression. Curvature and rollover of tellurium calibration curves has been addressed to a self-interference effect caused by the formation of finely dispersed elemental tellurium. Iodide ions were found to have beneficial or no negative effects in the hydrogen telluride generation. Addition of iodide on-line to the sample has been proved effective in the control of the self-interference effect and allows to work in mild reaction conditions. Moreover, it allows a good control of Cu(II) interference and eliminates Ni(II) and Co(II) interferences. The method has been successfully applied to determination of tellurium in copper and lead ores certified reference materials.

  12. Determination of Phosphorus by Inductively Coupled Plasma Atomic Emission Spectroscopy after Hydride Generation

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A continuous phosphine (PH3) generation was developed and applied to the sensitive detection of phosphorus by ICP-AES. Phosphate ion in aqueous solution was converted to phosphine by passing the sample solution through an incandescent copper silica-tube. Detection limit is 2 ng/mL. The relative standard deviation is 4.2% for 20 ng/mL. The method is rapid and simple with low contamination and high sensitivity.

  13. 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.

  14. 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.

  15. 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.

  16. Simple decomposition procedure for determination of selenium in whole blood, serum and urine by hydride generation atomic absorption spectroscopy.

    Science.gov (United States)

    Tiran, B; Tiran, A; Rossipal, E; Lorenz, O

    1993-12-01

    A digestion procedure for selenium determination by hydride generation atomic absorption spectroscopy (AAS) in whole blood, serum and urine is described, it employs sulfuric acid, hydrogen peroxide and vanadium (V) sulfuric acid reagent solution. The method is rapid, uses no explosive reagents and can be performed at a constant temperature of 100 degrees C. Therefore, it is easily applicable in a routine clinical laboratory for a large amount of samples. The coefficient of intra-assay variation was 4.3-5.6%, the coefficient for inter-assay variation was 5-5.9% in the medium and high concentration range, and 5.8-8.6% in the low range. In analyzing several commercial reference materials our results showed good agreement with the target values. Analytical recovery by addition of sodium selenite and seleno-DL-methionine to samples ranged between 97 and 104%. The correlation between the described digestion procedure and the nitric, sulfuric and perchloric acid digestion procedure recommended by the International Union of Pure and Applied Chemistry showed good agreement for whole blood, serum and for urine. We determined selenium in serum (n = 58) and whole blood (n = 50) in a collective of healthy children from 1 to 5 years living in Styria, Austria. The low values in serum (35 +/- 11 micrograms/L) and whole blood (42 +/- 6 micrograms/L) at one year of life increased significantly to 48 +/- 13 mu/L (p = 0.033) and 55 +/- 6 micrograms/L (p = 0.004) at three years of life in serum and whole blood, respectively. The selenium concentration showed no further increase up to five years of age.(ABSTRACT TRUNCATED AT 250 WORDS)

  17. Probing the cerium/cerium hydride interface using nanoindentation

    Energy Technology Data Exchange (ETDEWEB)

    Brierley, Martin, E-mail: martin.brierley@awe.co.uk [Atomic Weapons Establishment, Aldermaston, Berkshire RG7 4PR (United Kingdom); University of Manchester, Manchester M13 9PL (United Kingdom); Knowles, John, E-mail: john.knowles@awe.co.uk [Atomic Weapons Establishment, Aldermaston, Berkshire RG7 4PR (United Kingdom)

    2015-10-05

    Highlights: • A disparity exists between the minimum energy and actual shape of a cerium hydride. • Cerium hydride is found to be harder than cerium metal by a ratio of 1.7:1. • A zone of material under compressive stress was identified surrounding the hydride. • No distribution of hardness was apparent within the hydride. - Abstract: A cerium hydride site was sectioned and the mechanical properties of the exposed phases (cerium metal, cerium hydride, oxidised cerium hydride) were measured using nanoindentation. An interfacial region under compressive stress was observed in the cerium metal surrounding a surface hydride that formed as a consequence of strain energy generated by the volume expansion associated with precipitation of the hydride phase.

  18. Quantitation of toxic arsenic species and arsenobetaine in Pacific oysters using an off-line process with hydride generation-atomic absorption spectroscopy.

    Science.gov (United States)

    Hsiung, Tung-Ming; Huang, Chia-Wei

    2006-04-05

    An off-line process-based speciation technique was devised here to quantitatively determine toxic inorganic arsenic (iAs), methylarsonic acid (MA), dimethylarsinic acid (DMA), and the dominant, albeit virtually nontoxic, arsenobetaine (AB) in Pacific oysters (Crassostrea gigas). Oysters were extracted with fresh methanol-water (8+2), and this was replicated three times. They were then evaporated to near dryness and subsequently redissolved in pure water; defatting was then performed with a C18 cartridge. The trace hydride active arsenic species, that is, iAs, MA, and DMA, in the defatted solutions were determined with a sensitive hydride generation-packed coldfinger trap-atomic absorption spectrometric (HG-PCFT-AAS) coupled system. The arsenicals that were desorbed from the cation-exchange resin (Dowex 50W-X8) in the washings of 4 M NH3 were categorized on the basis of AB + DMA. The total quantity of arsenic in the recovered AB + DMA was determined with a commercial hydride generation-atomic absorption spectrometric (HG-AAS) system, and finally, AB was calculated from (AB + DMA) - DMA. The average concentrations of iAs, MA, DMA, AB, and total arsenic (TAs) in the oysters collected from six aquacultural sites along the west coast of Taiwan were, respectively, 0.15, 0.06, 0.64, 6.93, and 13.74 mg kg(-1) of dry weight. AB was the major species, whereas iAs (arsenite + arsenate) were the most toxic species, although the iAs made up only approximately 1% of the TAs in the oysters. The lifetime target cancer risk, as determined by the concentration of iAs on a fresh weight basis in the oysters, was well below the ordinary health protection criteria (10(-6)).

  19. 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.

  20. Next Generation Energetic Materials: New Cluster Hydrides and Metastable Alloys of Aluminum in Very Low Oxidation States

    Science.gov (United States)

    2016-10-01

    studies (M = Mg, Au, Sn, Mo, Ni, Zn) that preliminarily show similarities to the solution chemistry (Fig. 1c). These results show that AlM hydrides and...oxidation chemistry and thermodynamics. Our studies on the oxidation of Li2Al3(PPh2)61- showed that initial reactivity occurs at the reduced...nanoparticle nucleation on functionalized graphene surfactants from aluminum monochloride solutions. This data shows a strong affinity of AlCl units for

  1. 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.)

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

    Science.gov (United States)

    Yeşiller, Semira Unal; Yalçın, Serife

    2013-04-03

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

  3. Organotin speciation in environmental matrices by automated on-line hydride generation-programmed temperature vaporization-capillary gas chromatography-mass spectrometry detection.

    Science.gov (United States)

    Serra, H; Nogueira, J M F

    2005-11-11

    In the present contribution, a new automated on-line hydride generation methodology was developed for dibutyltin and tributyltin speciation at the trace level, using a programmable temperature-vaporizing inlet followed by capillary gas chromatography coupled to mass spectrometry in the selected ion-monitoring mode acquisition (PTV-GC/MS(SIM)). The methodology involves a sequence defined by two running methods, the first one configured for hydride generation with sodium tetrahydroborate as derivatising agent and the second configured for speciation purposes, using a conventional autosampler and data acquisition controlled by the instrument's software. From the method-development experiments, it had been established that injector configuration has a great effect on the speciation of the actual methodology, particularly, the initial inlet temperature (-20 degrees C; He: 150 ml/min), injection volume (2 microl) and solvent characteristics using the solvent venting mode. Under optimized conditions, a remarkable instrumental performance including very good precision (RSD CRM 462, Nr. 330 dibutyltin: 68+/-12 ng/g; tributyltin: 54+/-15 ng/g on dry mass basis), using liquid-liquid extraction (LLE) and solid-phase extraction (SPE) sample enrichment and multiple injections (2 x 5 microl) for sensitivity enhancement. The methodology evidenced high reproducibility, is easy to work-up, sensitive and showed to be a suitable alternative to replace the currently dedicated analytical systems for organotin speciation in environmental matrices at the trace level.

  4. Boron Hydrides

    Science.gov (United States)

    1946-07-01

    of direct interest could be b.P.4d. ’Thus the discovory of a now proj.ect, since silano is probably too readily infla-zmablo for practical usc’ this...devoted, ho specc4fie compounds vhitih a’-ould be tocdte at prescnt arc: nron tiy * silano , %;2.SiFi3 , diothyl sila~no, (C2 115 )2 Si112, mono r.-rop; ! (n...Bcrohydrido or Li h.... I .A-4A- The prepuation of Silano med of Stannane by the interaction or lithium aluzirun hydride v-ithl silicon tetrtchiorido and

  5. Thermodynamic Hydricity of Transition Metal Hydrides.

    Science.gov (United States)

    Wiedner, Eric S; Chambers, Matthew B; Pitman, Catherine L; Bullock, R Morris; Miller, Alexander J M; Appel, Aaron M

    2016-08-10

    Transition metal hydrides play a critical role in stoichiometric and catalytic transformations. Knowledge of free energies for cleaving metal hydride bonds enables the prediction of chemical reactivity, such as for the bond-forming and bond-breaking events that occur in a catalytic reaction. Thermodynamic hydricity is the free energy required to cleave an M-H bond to generate a hydride ion (H(-)). Three primary methods have been developed for hydricity determination: the hydride transfer method establishes hydride transfer equilibrium with a hydride donor/acceptor pair of known hydricity, the H2 heterolysis method involves measuring the equilibrium of heterolytic cleavage of H2 in the presence of a base, and the potential-pKa method considers stepwise transfer of a proton and two electrons to give a net hydride transfer. Using these methods, over 100 thermodynamic hydricity values for transition metal hydrides have been determined in acetonitrile or water. In acetonitrile, the hydricity of metal hydrides spans a range of more than 50 kcal/mol. Methods for using hydricity values to predict chemical reactivity are also discussed, including organic transformations, the reduction of CO2, and the production and oxidation of hydrogen.

  6. Determination of Trace Germanium in Marine Sediments by Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS)

    Institute of Scientific and Technical Information of China (English)

    LI Jing; ZHAO Shilan; ZHANG Zhaohui; ZENG Xianjie

    2004-01-01

    A method for the analysis of trace germanium in marine sediments by HG-AFS has been investigated. The experimental conditions such as the acidity of reduction reaction, the amount of sodium boro-hydride, the carrier gas flow rate, etc., were tested and optimized by using a kind of orthogonal design. The detection limit of the presented method is 0.95 μg L-1 for germanium. The calibration curve shows a satisfactory line in the concentration range 0-320 μg L-1 Ge with a variation coefficient of ±2.1%.

  7. Development of an analytical method for the determination of arsenic in gasoline samples by hydride generation-graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Becker, Emilene M. [Universidade Federal do Pampa, Bage, RS (Brazil); Universidade Federal de Pelotas, Pelotas, RS (Brazil); Dessuy, Morgana B.; Boschetti, Wiliam [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Ferreira, Sergio L.C. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil)

    2012-05-15

    The purpose of the present work was to optimize the conditions for the determination of arsenic in gasoline with hydride generation-graphite furnace atomic absorption spectrometry after acid digestion using a full two-level factorial design with center point. The arsine was generated in a batch system and collected in a graphite tube coated with 150 {mu}g Ir as a permanent modifier. The sample volume, the pre-reduction conditions, the temperature program and modifier mass were kept fixed for all experiments. The estimated main effects were: reducing agent concentration (negative effect), acid concentration (negative effect) and trapping temperature (positive effect). It was observed that there were interactions between the variables. Moreover, the curvature was significant, indicating that the best conditions were at the center point. The optimized parameters for arsine generation were 2.7 mol L{sup -1} hydrochloric acid and 1.6% (w/v) sodium tetrahydroborate. The optimized conditions to collect arsine in the graphite furnace were a trapping temperature of 250 Degree-Sign C and a collection time of 30 s. The limit of detection was 6.4 ng L{sup -1} and the characteristic mass was 24 pg. Two different systems for acid digestion were used: a digester block with cold finger and a microwave oven. The concentration of arsenic found with the proposed method was compared with that obtained using a detergentless microemulsion and direct graphite furnace determination. The results showed that the factorial design is a simple tool that allowed establishing the appropriate conditions for sample preparation and also helped in evaluating the interaction between the factors investigated. - Highlights: Black-Right-Pointing-Pointer We determined As in gasoline using hydride generation-graphite furnace AAS. Black-Right-Pointing-Pointer We compared three sample preparation procedures. Black-Right-Pointing-Pointer A multivariate approach was used to optimize the conditions. Black

  8. Fundamental investigations of natural and laboratory generated SAR dose response curves for quartz OSL in the high dose range

    DEFF Research Database (Denmark)

    Timar-Gabor, Alida; Constantin, Daniela; Buylaert, Jan-Pieter;

    2015-01-01

    SAR-OSL investigations on quartz from Romanian loess resulted in non concordant fine and coarse-grain ages for equivalent doses higher than ~100 Gy. The laboratory dose response for both grain sizes is well represented by a sum of two saturating exponential functions, fine and coarse grains chara...

  9. 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

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

    Science.gov (United States)

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

  11. Simultaneous determination of p-arsanilic acid and roxarsone in feed by liquid chromatography-hydride generation online coupled with atomic fluorescence spectrometry.

    Science.gov (United States)

    Liu, Jianjing; Yu, Hongxia; Song, Haibin; Qiu, Jing; Sun, Fengmei; Li, Ping; Yang, Shuming

    2008-08-01

    A novel, simple and sensitive liquid chromatography-hydride generation online coupled with atomic fluorescence spectrometry (LC-HG-AFS) method was developed for simultaneous determination of p-arsanilic acid (p-ASA) and roxarsone in feed. 20% Methanol aqueous was used as extraction reagent, after preprocessing samples by ultrasonic oscillation, then injected into the chromatography Waters symmetry shield RP18 analytical column (150mm x 4.6mm, 5 microm), finally detected by an atomic fluorescence spectrometer. The calibration curves of analyses were linear over a range of concentrations (0.2-4mg L-1 and the correlation coefficients were higher than 0.9990. The limits of detection were 0.2 mg L-1. The method has been validated by linearity, precision and recovery. p-ASA and roxarsone in feed can be successfully and simultaneously determined using the developed method without a tedious pretreatment procedure.

  12. A renewed search for short-lived 126Sn in the early Solar System: Hydride generation MC-ICPMS for high sensitivity Te isotopic analysis

    Science.gov (United States)

    Brennecka, Gregory A.; Borg, Lars E.; Romaniello, Stephen J.; Souders, Amanda K.; Shollenberger, Quinn R.; Marks, Naomi E.; Wadhwa, Meenakshi

    2017-03-01

    Although there is limited direct evidence for supernova input into the nascent Solar System, many models suggest it formed by the gravitational collapse of a molecular cloud that was triggered by a nearby supernova. Existing lines of evidence, mostly in the form of short-lived radionuclides present in the early Solar System, are potentially consistent with this hypothesis, but still allow for alternative explanations. Since the natural production of 126Sn is thought to occur only in supernovae and this isotope has a short half-life (126Sn→126Te, t1/2 = 235 ky), the discovery of extant 126Sn would provide unequivocal proof of supernova input to the early Solar System. Previous attempts to quantify the initial abundance of 126Sn by examining Sn-Te systematics in early solids have been hampered by difficulties in precisely measuring Te isotope ratios in these materials. Thus, here we describe a novel technique that uses hydride generation to dramatically increase the ionization efficiency of Te-an approximately 30-fold increase over previous work. This introduction system, when coupled to a MC-ICPMS, enables high-precision Te isotopic analyses on samples with expected concentrations of Sn and Te, as well as the lack of nucleosynthetic anomalies in other isotopes of Te suggest that the bulk of the Sn and Te recovered from these particular refractory inclusions is not of primary origin and thus does not represent a primary signature of Sn-Te systematics of the protosolar nebula during condensation of CAIs or their precursors. Although no evidence of supernova input was found based on Sn-Te systematics in this sample set, hydride generation represents a powerful tool that can now be used to further explore Te isotope systematics in less altered materials.

  13. Understanding the effects of potassium ferricyanide on lead hydride formation in tetrahydroborate system and its application for determination of lead in milk using hydride generation inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Deng, Biyang; Xu, Xiangshu; Xiao, Yan; Zhu, Pingchuan; Wang, Yingzi

    2015-01-01

    To understand the formation of plumbane in the Pb(II)-NaBH4-K3Fe(CN)6 system, the intermediate products produced in the reaction of lead(II) and NaBH4 in the presence of K3Fe(CN)6 were studied. The produced plumbane and elemental lead were measured through continuous flow hydride generation (HG)-inductively coupled plasma optical emission spectrometry (ICP OES) and X-ray diffraction spectrometry techniques, respectively. Based on the experimental results, the explanations can be depicted in the following steps: (1) plumbane and black lead sediment (black Pb) are formed in the reaction of lead(II) and NaBH4; (2) the black Pb is oxidized by K3Fe(CN)6 to form Pb2[Fe(CN)6], which further reacts with NaBH4 to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K3Fe(CN)6 to form more Pb2[Fe(CN)6] complex, which would produce more plumbane. In short, the black Pb and Pb2[Fe(CN)6] complex are the key intermediate products for the formation of plumbane in the Pb(II)-NaBH4-K3Fe(CN)6 system. Based on the enhancement effect of potassium ferricyanide and potassium ferrocyanide, a method was developed to analyze lead in milk with HG-ICP OES technique. The detection limit of the method was observed as 0.081 μg L(-1). The linearity range of lead was found between 0.3 and 50,000 μg L(-1) with correlation coefficient of 0.9993. The recovery of lead was determined as 97.6% (n=5) for adding 10 μg L(-1) lead into the milk sample.

  14. Advanced Hydride Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Motyka, T.

    1989-01-01

    Metal hydrides have been used at the Savannah River Tritium Facilities since 1984. However, the most extensive application of metal hydride technology at the Savannah River Site is being planned for the Replacement Tritium Facility, a $140 million facility schedules for completion in 1990 and startup in 1991. In the new facility, metal hydride technology will be used to store, separate, isotopically purify, pump, and compress hydrogen isotopes. In support of the Replacement Tritium Facility, a $3.2 million, cold,'' process demonstration facility, the Advanced Hydride Laboratory began operation in November of 1987. The purpose of the Advanced Hydride Laboratory is to demonstrate the Replacement Tritium Facility's metal hydride technology by integrating the various unit operations into an overall process. This paper will describe the Advanced Hydride Laboratory, its role and its impact on the application of metal hydride technology to tritium handling.

  15. Advanced Hydride Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Motyka, T.

    1989-12-31

    Metal hydrides have been used at the Savannah River Tritium Facilities since 1984. However, the most extensive application of metal hydride technology at the Savannah River Site is being planned for the Replacement Tritium Facility, a $140 million facility schedules for completion in 1990 and startup in 1991. In the new facility, metal hydride technology will be used to store, separate, isotopically purify, pump, and compress hydrogen isotopes. In support of the Replacement Tritium Facility, a $3.2 million, ``cold,`` process demonstration facility, the Advanced Hydride Laboratory began operation in November of 1987. The purpose of the Advanced Hydride Laboratory is to demonstrate the Replacement Tritium Facility`s metal hydride technology by integrating the various unit operations into an overall process. This paper will describe the Advanced Hydride Laboratory, its role and its impact on the application of metal hydride technology to tritium handling.

  16. Nanosecond pulsed power generator for a voltage amplitude up to 300 kV and a repetition rate up to 16 Hz for fine disintegration of quartz

    Energy Technology Data Exchange (ETDEWEB)

    Krastelev, E. G., E-mail: ekrastelev@yandex.ru; Sedin, A. A.; Tugushev, V. I. [Russian Academy of Sciences, Joint Institute for High Temperatures (Russian Federation)

    2015-12-15

    A generator of high-power high-voltage nanosecond pulses is intended for electrical discharge disintegration of mineral quartz and other nonconducting minerals. It includes a 320 kV Marx pulsed voltage generator, a high-voltage glycerin-insulated coaxial peaking capacitor, and an output gas spark switch followed by a load, an electric discharge disintegration chamber. The main parameters of the generator are as follows: a voltage pulse amplitude of up to 300 kV, an output impedance of ≈10 Ω, a discharge current amplitude of up to 25 kA for a half-period of 80–90 ns, and a pulse repetition rate of up to 16 Hz.

  17. An evaluation of the bioaccessibility of arsenic in corn and rice samples based on cloud point extraction and hydride generation coupled to atomic fluorescence spectrometry.

    Science.gov (United States)

    Castor, José Martín Rosas; Portugal, Lindomar; Ferrer, Laura; Hinojosa-Reyes, Laura; Guzmán-Mar, Jorge Luis; Hernández-Ramírez, Aracely; Cerdà, Víctor

    2016-08-01

    A simple, inexpensive and rapid method was proposed for the determination of bioaccessible arsenic in corn and rice samples using an in vitro bioaccessibility assay. The method was based on the preconcentration of arsenic by cloud point extraction (CPE) using o,o-diethyldithiophosphate (DDTP) complex, which was generated from an in vitro extract using polyethylene glycol tert-octylphenyl ether (Triton X-114) as a surfactant prior to its detection by atomic fluorescence spectrometry with a hydride generation system (HG-AFS). The CPE method was optimized by a multivariate approach (two-level full factorial and Doehlert designs). A photo-oxidation step of the organic species prior to HG-AFS detection was included for the accurate quantification of the total As. The limit of detection was 1.34μgkg(-1) and 1.90μgkg(-1) for rice and corn samples, respectively. The accuracy of the method was confirmed by analyzing certified reference material ERM BC-211 (rice powder). The corn and rice samples that were analyzed showed a high bioaccessible arsenic content (72-88% and 54-96%, respectively), indicating a potential human health risk.

  18. Intensity of quartz cathodoluminescence and trace-element content in quartz from the porphyry copper deposit at Butte, Montana

    Science.gov (United States)

    Rusk, B.G.; Reed, M.H.; Dilles, J.H.; Kent, A.J.R.

    2006-01-01

    Textures of hydrothermal quartz revealed by cathodoluminescence using a scanning electron microscope (SEM-CL) reflect the physical and chemical environment of quartz formation. Variations in intensity of SEM-CL can be used to distinguish among quartz from superimposed mineralization events in a single vein. In this study, we present a technique to quantify the cathodoluminescent intensity of quartz within individual and among multiple samples to relate luminescence intensity to specific mineralizing events. This technique has been applied to plutonic quartz and three generations of hydrothermal veins at the porphyry copper deposit in Butte, Montana. Analyzed veins include early quartz-molybdenite veins with potassic alteration, pyrite-quartz veins with sericitic alteration, and Main Stage veins with intense sericitic alteration. CL intensity of quartz is diagnostic of each mineralizing event and can be used to fingerprint quartz and its fluid inclusions, isotopes, trace elements, etc., from specific mineralizing episodes. Furthermore, CL intensity increases proportional to temperature of quartz formation, such that plutonic quartz from the Butte quartz monzonite (BQM) that crystallized at temperatures near 750 ??C luminesces with the highest intensity, whereas quartz that precipitated at ???250 ??C in Main Stage veins luminesces with the least intensity. Trace-element analyses via electron microprobe and laser ablation-ICP-MS indicate that plutonic quartz and each generation of hydrothermal quartz from Butte is dominated by characteristic trace amounts of Al, P, Ti, and Fe. Thus, in addition to CL intensity, each generation of quartz can be distinguished based on its unique trace-element content. Aluminum is generally the most abundant element in all generations of quartz, typically between 50 and 200 ppm, but low-temperature, Main Stage quartz containing 400 to 3600 ppm Al is enriched by an order of magnitude relative to all other quartz generations. Phosphorous

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

    Energy Technology Data Exchange (ETDEWEB)

    Lavilla, I. [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas - Marcosende s/n, 36310 Vigo (Spain); Gonzalez-Costas, J.M. [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas - Marcosende s/n, 36310 Vigo (Spain); Bendicho, C. [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas - Marcosende s/n, 36310 Vigo (Spain)]. E-mail: bendicho@uvigo.es

    2007-05-22

    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{sub 3} or the mixture HNO{sub 3}/H{sub 2}O{sub 2} and further thermal reduction of the Se(VI) formed to Se(IV) were evaluated. These procedures were as follows: (I) without H{sub 2}O{sub 2} and without heating to dryness; (II) without H{sub 2}O{sub 2} and with heating to dryness; (III) with H{sub 2}O{sub 2} and without heating to dryness; (IV) with H{sub 2}O{sub 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

  20. Ultrasound- and microwave-assisted extractions followed by hydride generation inductively coupled plasma optical emission spectrometry for lead determination in geological samples.

    Science.gov (United States)

    Welna, Maja; Borkowska-Burnecka, Jolanta; Popko, Malgorzata

    2015-11-01

    Followed the current idea of simplified sample pretratmet before analysis we evaluated the procedure for the determination of Pb in calcium-rich materials such as dolomites after ultrasound- or microwave- assisted extraction with diluted acids using hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP-OES). Corresponding Pb hydride was generated in the reaction of an acidified sample solution with NaBH4 after pre-oxidation of Pb(II) to Pb(IV) by K3[Fe(CN)6]. Several chemical (acidic media: HCl, HNO3 or CH3COOH, concentration of the reductant as well as type and concentration of oxidazing agents) and physical (reagents flow rates, reaction coil length) parameters affecting the efficiency of plumbane formation were optimized in order to improve the detectability of Pb using HG-ICP-OES. Limitation of the method derived from the matrix effects was pointed out. Employing Pb separation by HG technique allows the significant reduction of interferences caused by sample matrix constituents (mainly Ca and Mg), nevertheless they could not be overcame at all, hence calibration based on the standard addition method was recommended for Pb quantification in dolomites. Under the selected conditions, i.e. 0.3 mol L(-1) HCl, HNO3 or CH3COOH, 1.5% NaBH4 and 3.0% K3[Fe(CN)6] the limits of detection (LODs) between 2.3-5.6 μg L(-1) (3.4-6.8 μg L(-1) considering matrix effects) and the precision below 5% were achieved. The accuracy of the procedure was verified by analysis of certified reference materials (NCS DC70308 (Carbonate Rock) and NIST 14000 (Bone Ash)) and recovery test with satisfactory results of Pb recoveries ranging between 94-108% (CRMs analysis) and 92-114% (standard addition method). The applicability of the proposed method was demonstrated by the determination of Pb in dolomites used by different fertiliser factories.

  1. Understanding the effects of potassium ferricyanide on lead hydride formation in tetrahydroborate system and its application for determination of lead in milk using hydride generation inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Biyang, E-mail: dengby16@163.com; Xu, Xiangshu; Xiao, Yan; Zhu, Pingchuan; Wang, Yingzi

    2015-01-01

    Highlights: • Proposed a novel explanation for plumbane generation. • Expounded the role of K{sub 3}Fe(CN){sub 6} in plumbane generation. • Clarified the controversial aspects in the mechanism of K{sub 3}Fe(CN){sub 6} enhancement. • Used X-ray diffractometry to analyze the intermediates. • Developed a method to analyze lead in milk using K{sub 3}Fe(CN){sub 6} and K{sub 4}Fe(CN){sub 6} as new additives. - Absract: To understand the formation of plumbane in the Pb{sup II}-NaBH{sub 4}-K{sub 3}Fe(CN){sub 6} system, the intermediate products produced in the reaction of lead(II) and NaBH{sub 4} in the presence of K{sub 3}Fe(CN){sub 6} were studied. The produced plumbane and elemental lead were measured through continuous flow hydride generation (HG)-inductively coupled plasma optical emission spectrometry (ICP OES) and X-ray diffraction spectrometry techniques, respectively. Based on the experimental results, the explanations can be depicted in the following steps: (1) plumbane and black lead sediment (black Pb) are formed in the reaction of lead(II) and NaBH{sub 4}; (2) the black Pb is oxidized by K{sub 3}Fe(CN){sub 6} to form Pb{sub 2}[Fe(CN){sub 6}], which further reacts with NaBH{sub 4} to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K{sub 3}Fe(CN){sub 6} to form more Pb{sub 2}[Fe(CN){sub 6}] complex, which would produce more plumbane. In short, the black Pb and Pb{sub 2}[Fe(CN){sub 6}] complex are the key intermediate products for the formation of plumbane in the Pb{sup II}-NaBH{sub 4}-K{sub 3}Fe(CN){sub 6} system. Based on the enhancement effect of potassium ferricyanide and potassium ferrocyanide, a method was developed to analyze lead in milk with HG-ICP OES technique. The detection limit of the method was observed as 0.081 μg L{sup −1}. The linearity range of lead was found between 0.3 and 50,000 μg L{sup −1} with correlation coefficient of 0

  2. 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

  3. 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.

  4. [Determination of arsenic, mercury and selenium in Gynostemma pentaphyllum and rhizospheric soil samples collected from different regions by hydride generation atomic fluorescence spectrometry].

    Science.gov (United States)

    Wang, Jing; Xiao, Ya-ping; Liang, Xiao-qing; Shao, Xian-hui; Zhang, Ke

    2012-03-01

    The contents of arsenic (As), mercury (Hg) and selenium (Se) in Gynostemma pentaphyllum and rhizospheric soil samples collected from seven provinces were determined, through the optimization of the hydride generation atomic fluorescence spectrometry working conditions. The results show that: the contents of As, Hg and Se in Gynostemma pentaphyllum from seven provinces revealed large differences, but compared with the limits of the two kinds of heavy metal element: As and Hg set by the Green Trade Standards of Importing & Exporting Medicinal Plants & Preparations (As Gynostemma pentaphyllum samples are both lower than them. The Se content in Gynostemma pentaphyllum samples and in rhizospheric soil samples revealed significant correlation, and as a result, the Gynostemma pentaphyllum from the Fu Xi area Enshi in Hu Bei province had obviously higher Se content than others in the 6 provinces. From this study, a preliminary conclusion can be drawn that Se in Gynostemma pentaphyllum is mainly from the soil, moreover, the As and Hg show the difference from Se, possibly they are still affected by the dry and wet deposition of atmospheric aerosols.

  5. Speciation analysis of inorganic arsenic in coal samples by microwave-assisted extraction and high performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Sun, Mei; Liu, Guijian; Wu, Qianghua; Liu, Wenqi

    2013-03-15

    A new method was developed for the speciation analysis of inorganic arsenic in coal samples by high performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry after microwave-assisted extraction. Effective extract of As(III) and As(V) in coal sample was achieved by 1.0 mol L(-1)H₃PO₄ and 0.1 mol L(-1)ascorbic acid. Under the optimized conditions, the limits of detection (LOD) were 0.01 μg L(-1) and 0.02 μg L(-1), the relative standard deviations (RSD) were 2.4% and 3.3% (c=10.0 μg L(-1), n=7), recoveries were 102.5% and 96.5% for As(III) and As(V). The proposed method was successfully applied for the determination of speciation of inorganic arsenic in coal samples and GBW11117 coal standard reference material with complex matrix. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. A practical method for the determination of total selenium in environmental samples using isotope dilution-hydride generation-inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Kleckner, Amy E.; Kakouros, Evangelos; Stewart, A. Robin

    2017-01-01

    A safe, practical, and accurate method for the determination of selenium (Se) in range of environmental samples was developed. Small sample masses, 5–20 mg, were amended with 82Se enriched isotope for the isotope dilution (ID), preceding a multi-step wet digestion with nitric acid (HNO3) and hydrogen peroxide (H2O2). Samples were incubated in an autoclave for 3 h at 20 psi and 126°C. Digestates were subsequently reduced with concentrated hydrochloric acid to Se(IV) the most favorable valence for hydride generation (HG). The solutions were then analyzed on an ICP-MS equipped with Flow Injection system (FIAS-400). Polyatomic, isobaric, and background interferences were removed through the use of HG and ID with an 82Se enriched isotope spike. Recoveries for certified reference materials were determined and averaged 96% for biological tissues (NRCC DOLT3, DOLT4, DORM2, TORT2, and TORT3, and NIST 2976) and 108% for estuarine sediment (NRCC PACS2) with an average coefficient of variation for replicate measurements of ∼ 3.5%. Limit of detection was 0.13 ng Se g−1 dry weight or 0.19 ng Se L−1. This method can be broadly applied to biological tissues, sediments, suspended particulates, and water samples with minimal modifications making this method highly useful for assessing the ecotoxicology of total Se in aquatic ecosystems.

  7. Masking Agents Evaluation for Lead Determination by Flow Injection-Hydride Generation-Atomic Fluorescence Spectrometry Technique: Effect of KI, L-Cysteine, and 1,10-Phenanthroline.

    Science.gov (United States)

    Beltrán, Blanca G; Leal, Luz O; Ferrer, Laura; Cerdà, Víctor

    2016-01-01

    Hydride generation (HG) of lead technique presents interferences from foreign ions of complex matrix samples. In order to minimize these interferences, the effect of masking agents such as KI, L-cysteine, and 1,10-phenanthroline was studied in the absence and in the presence of selected interfering species (As, Cr, Cu, and Fe). Different modes of addition of masking agents were accomplished, that is, to either sample or KBH4 reducing solution. The lead determinations were performed using a flow injection analysis (FIA) system coupled to HG and atomic fluorescence spectrometry (AFS). The linearity of calibration curves (1-10 μg Pb L(-1)) was not affected by the addition of the masking agents. The use of KI in the reducing solution diminished interferences from concentrations of As and Cu, while 1,10-phenanthroline showed a positive effect on the interference by As. Moreover, Cr and Cu appeared to be the most serious interfering ions for plumbane (PbH4), because they drastically reduced the analytical signal of lead. Fe did not present any interference under the employed experimental conditions, even at high levels. The accuracy was established through the analysis of certified reference material (i.e., BCR-610, groundwater) using KI as masking agent. The detection limit reached by FIA-HG-AFS proposed methodology was 0.03 μg Pb L(-1).

  8. Synthesis of ruthenium hydride

    Science.gov (United States)

    Kuzovnikov, M. A.; Tkacz, M.

    2016-02-01

    Ruthenium hydride was synthesized at a hydrogen pressure of about 14 GPa in a diamond-anvil cell. Energy-dispersive x-ray diffraction was used to monitor the ruthenium crystal structure as a function of hydrogen pressure up to 30 GPa. The hydride formation was accompanied by phase transition from the original hcp structure of the pristine metal to the fcc structure. Our results confirmed the theoretical prediction of ruthenium hydride formation under hydrogen pressure. The standard Gibbs free energy of the ruthenium hydride formation reaction was calculated assuming the pressure of decomposition as the equilibrium pressure.

  9. Hydride generation coupled to microfunnel-assisted headspace liquid-phase microextraction for the determination of arsenic with UV-Vis spectrophotometry.

    Science.gov (United States)

    Hashemniaye-Torshizi, Reihaneh; Ashraf, Narges; Arbab-Zavar, Mohammad Hossein

    2014-12-01

    In this research, a microfunnel-assisted headspace liquid-phase microextraction technique has been used in combination with hydride generation to determine arsenic (As) by UV-Vis spectrophotometry. The method is based on the reduction of As to arsine (AsH3) in acidic media by sodium tetrahydroborate (NaBH4) followed by its subsequent reaction with silver diethyldithiocarbamate (AgDDC) to give an absorbing complex at 510 nm. The complexing reagent (AgDDC) has been dissolved in a 1:1 (by the volume ratio) mixture of chloroform/chlorobenzene microdroplet and exposed to the generated gaseous arsine via a reversed microfunnel in the headspace of the sample solution. Several operating parameters affecting the performance of the method have been examined and optimized. Acetonitrile solvent has been added to the working samples as a sensitivity enhancement agent. Under the optimized operating conditions, the detection limit has been measured to be 0.2 ng mL(-1) (based on 3sb/m criterion, n b = 8), and the calibration curve was linear in the range of 0.5-12 ng mL(-1). The relative standard deviation for eight replicate measurements was 1.9 %. Also, the effects of several potential interferences have been studied. The accuracy of the method was validated through the analysis of JR-1 geological standard reference material. The method has been successfully applied for the determination of arsenic in raw and spiked soft drink and water samples with the recoveries that ranged from 91 to 106 %.

  10. Hysteresis in Metal Hydrides.

    Science.gov (United States)

    Flanagan, Ted B., And Others

    1987-01-01

    This paper describes a reproducible process where the irreversibility can be readily evaluated and provides a thermodynamic description of the important phenomenon of hysteresis. A metal hydride is used because hysteresis is observed during the formation and decomposition of the hydride phase. (RH)

  11. 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.

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

    Science.gov (United States)

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

    2014-10-21

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

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

    Science.gov (United States)

    Rosas-Castor, J M; Portugal, L; Ferrer, L; Guzmán-Mar, J L; Hernández-Ramírez, A; Cerdà, V; Hinojosa-Reyes, L

    2015-05-18

    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(-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(-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(-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 soil samples from an arsenic-contaminated mining zone to evaluate its extractability. The frequency of analysis of the proposed method was eight times higher than that of the conventional BCR method (6 vs 48 h), and the kinetics of lixiviation were established for each fraction.

  14. Selective hydride generation- cryotrapping- ICP-MS for arsenic speciation analysis at picogram levels: analysis of river and sea water reference materials and human bladder epithelial cells

    Science.gov (United States)

    Matoušek, Tomáš; Currier, Jenna M.; Trojánková, Nikola; Saunders, R. Jesse; Ishida, María C.; González-Horta, Carmen; Musil, Stanislav; Mester, Zoltán; Stýblo, Miroslav; Dědina, Jiří

    2013-01-01

    An ultra sensitive method for arsenic (As) speciation analysis based on selective hydride generation (HG) with preconcentration by cryotrapping (CT) and inductively coupled plasma- mass spectrometry (ICP-MS) detection is presented. Determination of valence of the As species is performed by selective HG without prereduction (trivalent species only) or with L-cysteine prereduction (sum of tri- and pentavalent species). Methylated species are resolved on the basis of thermal desorption of formed methyl substituted arsines after collection at −196°C. Limits of detection of 3.4, 0.04, 0.14 and 0.10 pg mL−1 (ppt) were achieved for inorganic As, mono-, di- and trimethylated species, respectively, from a 500 μL sample. Speciation analysis of river water (NRC SLRS-4 and SLRS-5) and sea water (NRC CASS-4, CASS-5 and NASS-5) reference materials certified to contain 0.4 to 1.3 ng mL−1 total As was performed. The concentrations of methylated As species in tens of pg mL−1 range obtained by HG-CT-ICP-MS systems in three laboratories were in excellent agreement and compared well with results of HG-CT-atomic absorption spectrometry and anion exchange liquid chromatography- ICP-MS; sums of detected species agreed well with the certified total As content. HG-CT-ICP-MS method was successfully used for analysis of microsamples of exfoliated bladder epithelial cells isolated from human urine. Here, samples of lysates of 25 to 550 thousand cells contained typically tens pg up to ng of iAs species and from single to hundreds pg of methylated species, well within detection power of the presented method. A significant portion of As in the cells was found in the form of the highly toxic trivalent species. PMID:24014931

  15. Method development and optimization for the determination of selenium in bean and soil samples using hydride generation electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Shaltout, Abdallah A; Castilho, Ivan N B; Welz, Bernhard; Carasek, Eduardo; Martens, Irland B Gonzaga; Martens, Andreas; Cozzolino, Silvia M F

    2011-09-15

    The present investigation is the first part of an initiative to prepare a regional map of the natural abundance of selenium in various areas of Brazil, based on the analysis of bean and soil samples. Continuous-flow hydride generation electrothermal atomic absorption spectrometry (HG-ET AAS) with in situ trapping on an iridium-coated graphite tube has been chosen because of the high sensitivity and relative simplicity. The microwave-assisted acid digestion for bean and soil samples was tested for complete recovery of inorganic and organic selenium compounds (selenomethionine). The reduction of Se(VI) to Se(IV) was optimized in order to guarantee that there is no back-oxidation, which is of importance when digested samples are not analyzed immediately after the reduction step. The limits of detection and quantification of the method were 30 ng L(-1) Se and 101 ng L(-1) Se, respectively, corresponding to about 3 ng g(-1) and 10 ng g(-1), respectively, in the solid samples, considering a typical dilution factor of 100 for the digestion process. The results obtained for two certified food reference materials (CRM), soybean and rice, and for a soil and sediment CRM confirmed the validity of the investigated method. The selenium content found in a number of selected bean samples varied between 5.5±0.4 ng g(-1) and 1726±55 ng g(-1), and that in soil samples varied between 113±6.5 ng g(-1) and 1692±21 ng g(-1).

  16. New features of different frequency generating systems due to the use of electrodeless rigidly mounted VBA quartz crystal resonator

    Science.gov (United States)

    Jendly, A.; Graf, E.; Busca, G.; Brownsea, D. A.

    1984-01-01

    The BVA 5 MHz crystal equipped frequency sources exhibit a new blend of performances such as 10 to 11 daily stability, 5x10-13 short term stability (1 to 30 s time intervals) and close to the carrier low phase noise (1 Hz : -120 dBc, 10 Hz : -140 dBc), whereby retaining the customary crystal oscillator benefits of small volume, high reliability and low price, as opposed to more sophisticated frequency generators which would be required to achieve comparable performances. Examples illustrating the impact of the Oscilloquartz BVA oven-controlled crystal oscillator in different frequency generating systems are presented: cesium frequency standards; hydrogen frequency standard; a precision distribution sub-system for satellite ground stations; and high hierarchy exchanges of digital networks, synchronized by the master-slave method are discussed.

  17. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of antimony by automated-hydride atomic absorption spectrophotometry

    Science.gov (United States)

    Brown, G.E.; McLain, B.J.

    1994-01-01

    The analysis of natural-water samples for antimony by automated-hydride atomic absorption spectrophotometry is described. Samples are prepared for analysis by addition of potassium and hydrochloric acid followed by an autoclave digestion. After the digestion, potassium iodide and sodium borohydride are added automatically. Antimony hydride (stibine) gas is generated, then swept into a heated quartz cell for determination of antimony by atomic absorption spectrophotometry. Precision and accuracy data are presented. Results obtained on standard reference water samples agree with means established by interlaboratory studies. Spike recoveries for actual samples range from 90 to 114 percent. Replicate analyses of water samples of varying matrices give relative standard deviations from 3 to 10 percent.

  18. In Situ Monitoring of the Generation of Monodisperse Silica Particles during the Hydrolysis of Tetraethyl Orthosilicate with Piezoelectric Quartz Crystal Impedance Analyzer

    Institute of Scientific and Technical Information of China (English)

    姚守拙; 张友玉; 谢青季

    2003-01-01

    The piezoelectric quartz crystal(PQC)impedance analyzer was used to monitor in situ the generation of monodisperse silica particles during the hydrolysis of tetraethyl orthosilicate (TEOS) and their adsorption onto and Au electrode in alcohol solutions containing water(6-15mol/L)and ammonia(0.2-2.0 mol/L).The equivalent circuit parameters,the resonance frequencies and the half-peak width values of the conductance spectra of the PQC resonance were obtained.The resonant frequency decreased notably while the motional resistance changed very slightly(within 1Ω during the hydrolysis reaction,suggesting that the mass effect dominated the adsorption of generated monodisperse silica particles on the gold electrode in this system.Changes in f0 indicated that the ammonia concentration affected the hydrolytic reaction obviously,and the influence of water concentration on the reaction was small while the water was significantly excessive.Kinetics of monodisperse silica particle adsorption occurring at the electrode i solution interface was analyzed using a first-order reaction scheme.In addition,the electrolyte-induced precipitation of the monodisperse silica of adsorbed particles per area and the converge of monodisperse silica particles were obtained from scanning electron nicroscope(SEM)observations.

  19. [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

  20. 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.

  1. 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.

  2. Preliminary results on the determination of ultratrace amounts of cadmium in tea samples using a flow injection on-line solid phase extraction separation and preconcentration technique to couple with a sequential injection hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Duan, Taicheng; Song, Xuejie; Jin, Dan; Li, Hongfei; Xu, Jingwei; Chen, Hangting

    2005-10-31

    In this work, a method was developed for determination of ultra-trace levels of Cd in tea samples by atomic fluorescence spectrometry (AFS). A flow injection solid phase extraction (FI-SPE) separation and preconcentration technique, to on-line couple with a sequential injection hydride generation (SI-HG) technique is employed in this study. Cd was preconcentrated on the SPE column, which was made from a neutral extractant named Cyanex 923, while other matrix ions or interfering ions were completely or mostly separated off. Conditions for the SPE separation and preconcentration, as well as conditions for the HG technique, were studied. Due to the separation of interfering elements, Cd hydride generation efficiency could be greatly enhanced with the sole presence of Co(2+) with a concentration of 200mugL(-1), which is much lower than those in other works previously reported. Interferences on both the Cd separation and preconcentration, and Cd hydride generation (HG) were investigated; it showed that both the separation and preconcentration system, and the HG system had a strong anti-interference ability. The SPE column could be repeatedly used at least 400 times, a R.S.D. of 0.97% was obtained for 6 measurements of Cd with 0.2mugL(-1) and a correlation coefficiency of 1.0000 was obtained for the measurement of a series of solutions with Cd concentrations from 0.1 to 2mugL(-1). The method has a low detection limit of 10.8ngL(-1) for a 25mL solution and was successfully validated by using two tea standard reference materials (GBW08513 and GBW07605).

  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. 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

  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. Uranium Hydride Nucleation and Growth Model FY'16 ESC Annual Report

    Energy Technology Data Exchange (ETDEWEB)

    Hill, Mary Ann [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Richards, Andrew Walter [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Holby, Edward F. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Schulze, Roland K. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-12-20

    Uranium hydride corrosion is of great interest to the nuclear industry. Uranium reacts with water and/or hydrogen to form uranium hydride which adversely affects material performance. Hydride nucleation is influenced by thermal history, mechanical defects, oxide thickness, and chemical defects. Information has been gathered from past hydride experiments to formulate a uranium hydride model to be used in a Canned Subassembly (CSA) lifetime prediction model. This multi-scale computer modeling effort started in FY’13, and the fourth generation model is now complete. Additional high-resolution experiments will be run to further test the model.

  7. Lightweight hydride storage materials

    Energy Technology Data Exchange (ETDEWEB)

    Thomas, G.J.; Guthrie, S.E.; Bauer, W. [Sandia National Labs., Livermore, CA (United States)

    1995-09-01

    The need for lightweight hydrides in vehicular applications has prompted considerable research into the use of magnesium and its alloys. Although this earlier work has provided some improved performance in operating temperature and pressure, substantial improvements are needed before these materials will significantly enhance the performance of an engineered system on a vehicle. We are extending the work of previous investigators on Mg alloys to reduce the operating temperature and hydride heat of formation in light weight materials. Two important results will be discussed in this paper: (1) a promising new alloy hydride was found which has better pressure-temperature characteristics than any previous Mg alloy and, (2) a new fabrication process for existing Mg alloys was developed and demonstrated. The new alloy hydride is composed of magnesium, aluminum and nickel. It has an equilibrium hydrogen overpressure of 1.3 atm. at 200{degrees}C and a storage capacity between 3 and 4 wt.% hydrogen. A hydrogen release rate of approximately 5 x 10{sup -4} moles-H{sub 2}/gm-min was measured at 200{degrees}C. The hydride heat of formation was found to be 13.5 - 14 kcal/mole-H{sub 2}, somewhat lower than Mg{sub 2}Ni. The new fabrication method takes advantage of the high vapor transport of magnesium. It was found that Mg{sub 2}Ni produced by our low temperature process was better than conventional materials because it was single phase (no Mg phase) and could be fabricated with very small particle sizes. Hydride measurements on this material showed faster kinetic response than conventional material. The technique could potentially be applied to in-situ hydride bed fabrication with improved packing density, release kinetics, thermal properties and mechanical stability.

  8. ORNL Interim Progress Report on Hydride Reorientation CIRFT Tests

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jy-An John [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Yan, Yong [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Wang, Hong [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2016-10-28

    A systematic study of H. B. Robinson (HBR) high burnup spent nuclear fuel (SNF) vibration integrity was performed in Phase I project under simulated transportation environments, using the Cyclic Integrated Reversible-Bending Fatigue Tester (CIRFT) hot cell testing technology developed at Oak Ridge National Laboratory in 2013–14. The data analysis on the as-irradiated HBR SNF rods demonstrated that the load amplitude is the dominant factor that controls the fatigue life of bending rods. However, previous studies have shown that the hydrogen content and hydride morphology has an important effect on zirconium alloy mechanical properties. To address the effect of radial hydrides in SNF rods, in Phase II a test procedure was developed to simulate the effects of elevated temperatures, pressures, and stresses during transfer-drying operations. Pressurized and sealed fuel segments were heated to the target temperature for a preset hold time and slow-cooled at a controlled rate. The procedure was applied to both non-irradiated/prehydrided and high-burnup Zircaloy-4 fueled cladding segments using the Nuclear Regulatory Commission-recommended 400°C maximum temperature limit at various cooling rates. Before testing high-burnup cladding, four out-of-cell tests were conducted to optimize the hydride reorientation (R) test condition with pre-hydride Zircaloy-4 cladding, which has the same geometry as the high burnup fuel samples. Test HR-HBR#1 was conducted at the maximum hoop stress of 145 MPa, at a 400°C maximum temperature and a 5°C/h cooling rate. On the other hand, thermal cycling was performed for tests HR-HBR#2, HR-HBR#3, and HR-HBR#4 to generate more radial hydrides. It is clear that thermal cycling increases the ratio of the radial hydride to circumferential hydrides. The internal pressure also has a significant effect on the radial hydride morphology. This report describes a procedure and experimental results of the four out-of-cell hydride reorientation tests of

  9. Hydrogen, lithium, and lithium hydride production

    Energy Technology Data Exchange (ETDEWEB)

    Brown, Sam W.; Spencer, Larry S.; Phillips, Michael R.; Powell, G. Louis; Campbell, Peggy J.

    2017-06-20

    A method is provided for extracting hydrogen from lithium hydride. The method includes (a) heating lithium hydride to form liquid-phase lithium hydride; (b) extracting hydrogen from the liquid-phase lithium hydride, leaving residual liquid-phase lithium metal; (c) hydriding the residual liquid-phase lithium metal to form refined lithium hydride; and repeating steps (a) and (b) on the refined lithium hydride.

  10. Simulation of quartz resonators

    Science.gov (United States)

    Weinmann, M.; Radius, R.; Mohr, R.

    Quartz resonators are suitable as novel sensor elements in the field of profilometry and three dimensional measurement techniques. This application requires a tailoring of the oscillator circuit which is performed by a network analysis program. The equivalent network parameters are computed by a finite element analysis. The mechanical loading of the quartz is modeled by a viscous damping approach.

  11. Using vein fabric and fluid inclusion characteristics as an integrated proxy to constrain the relative timing of non cross-cutting, syn- to late-orogenic quartz vein generations

    Science.gov (United States)

    Jacques, Dominique; Muchez, Philippe; Sintubin, Manuel

    2014-05-01

    Research on ancient fluid systems mainly focuses on veins, because they offer the opportunity to combine macro- and microstructural data with geochemical data to gain insight into the P-T-X conditions present during veining. By applying such an integrated petrographic and microthermometric methodology to syn- to late-orogenic quartz veins in the Palaeozoic High-Ardenne slate belt (Belgium), we were able to define the relative timing and related P-T-X conditions of different quartz vein generations, despite of the absence of any mutual cross-cutting relationships in the field (Jacques et al., 2014). The different quartz vein generations represent the meso-scale brittle accommodation during fold initiation, amplification and locking. The presence of free polycrystal growth in cavities at a midcrustal depth, and fluid-assisted brecciation indicate that veining occurred under overpressured fluid conditions during the orogeny. Significant differences in crystal-plastic deformation microstructures and P-T trapping conditions indicate that the different processes accommodating folding occurred in a progressive manner along a retrograde deformation path. While vein quartz in an extrados vein and in the peripheral part of a lenticular, fault-accommodating vein shows moderate crystal-plastic deformation (e.g. bulging recrystallisation, deformation lamellae, shear bands), crystal-plastic deformation is relatively absent in the vein quartz of a saddle reef and the core of the lenticular vein (i.e. no to minor undulose extinction). Successive veining occurred from peak metamorphic conditions (ca. 300 ° C and 190 MPa), measured in the extrados vein, to lower P-T conditions in the periphery of the lenticular vein (ca. 275 ° C and 180 MPa), the late-orogenic saddle reef (ca. 245 ° C and 160 MPa) and the core of the lenticular vein (ca. 220 ° C and 150 MPa). The relative timing and accompanying decrease in P-T conditions of the different quartz vein generations reflect the

  12. Radiation Damage of Quartz Fibers

    CERN Document Server

    Hagopian, V

    1999-01-01

    Quartz fibers are used in high energy physics experiments as the active medium in high radiation area calorimetry. Quartz fibers are also used in the transmission of optical signals. Even though quartz does not damage by moderate amounts of irradiation, the clad of the fibers and the protective coating ( buffer) do damage reducing light transmission. Various types of quartz fibers have been irradiated and measured for light transmission. The most radiation hard quartz fibers are those with quartz clad and aluminum buffer.

  13. QUARTZ FIBER ELECTROSCOPES

    Science.gov (United States)

    Henderson, R.P.

    1957-09-17

    An instrument carried unobtrusively about the person such as in a finger ring to indicate when that person has been exposed to an unusual radiation hazard is described. A metallized quartz fiber is electrically charged to indicate a full scale reading on an etched glass background. The quartz fiber and the scale may be viewed through a magnifying lens for ease of reading. Incident radiation will ionize gaseous particles in the sealed structure thereby allowing the charge to leak off the quartz fiber with its resulting movement across the scale proportionally indicating the radiation exposure.

  14. Application of multivariate techniques in the optimization of a procedure for the determination of bioavailable concentrations of Se and As in estuarine sediments by ICP OES using a concomitant metals analyzer as a hydride generator.

    Science.gov (United States)

    Lopes, Watson da Luz; Santelli, Ricardo Erthal; Oliveira, Eliane Padua; de Carvalho, Maria de Fátima Batista; Bezerra, Marcos Almeida

    2009-10-15

    A procedure has been developed for the determination of bioavailable concentrations of selenium and arsenic in estuarine sediments employing inductively coupled plasma optical emission spectrometry (ICP OES) using a concomitant metals analyzer device to perform hydride generation. The optimization of hydride generation was done in two steps: using a two-level factorial design for preliminary evaluation of studied factors and a Doehlert design to assess the optimal experimental conditions for analysis. Interferences of transition metallic ions (Cd(2+), Co(2+), Cu(2+), Fe(3+) and Ni(2+)) to selenium and arsenic signals were minimized by using higher hydrochloric acid concentrations. In this way, the procedure allowed the determination of selenium and arsenic in sediments with a detection limit of 25 and 30 microg kg(-1), respectively, assuming a 50-fold sample dilution (0.5 g sample extraction to 25 mL sample final volume). The precision, expressed as a relative standard deviation (% RSD, n=10), was 0.2% for both selenium and arsenic in 200 microg L(-1) solutions, which corresponds to 10 microg g(-1) in sediment samples after acid extraction. Applying the proposed procedure, a linear range of 0.08-10 and 0.10-10 microg g(-1) was obtained for selenium and arsenic, respectively. The developed procedure was validated by the analysis of two certified reference materials: industrial sludge (NIST 2782) and river sediment (NIST 8704). The results were in agreement with the certified values. The developed procedure was applied to evaluate the bioavailability of both elements in four sediment certified reference materials, in which there are not certified values for bioavailable fractions, and also in estuarine sediment samples collected in several sites of Guanabara Bay, an impacted environment in Rio de Janeiro, Brazil.

  15. 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.)

  16. Vacuum electrolysis of quartz

    Science.gov (United States)

    King, James Claude

    1976-01-13

    The disclosure is directed to a method for processing quartz used in fabricating crystal resonators such that transient frequency change of resonators exposed to pulse irradiation is virtually eliminated. The method involves heating the crystal quartz in a hydrogen-free atmosphere while simultaneously applying an electric field in the Z-axis direction of the crystal. The electric field is maintained during the cool-down phase of the process.

  17. Room temperature trapping of stibine and bismuthine onto quartz substrates coated with nanostructured palladium for total reflection X-ray fluorescence analysis

    Science.gov (United States)

    Romero, Vanesa; Costas-Mora, Isabel; Lavilla, Isela; Bendicho, Carlos

    2015-05-01

    In this work, a novel method for determining Sb and Bi based on the trapping of their covalent hydrides onto quartz reflectors coated with immobilized palladium nanoparticles (Pd NPs) followed by total reflection X-ray fluorescence (TXRF) analysis is proposed. Pd NPs were synthesized by chemical reduction of the metal precursor using a mixture of water:ethanol as mild reducing agent. Silanization using 3-mercaptopropyltrimethoxysilane (MPTMS) was performed for the immobilization of Pd NPs onto the quartz substrates. Volatile hydrides (stibine and bismuthine) generated by means of a continuous flow system were flushed onto the immobilized Pd NPs and retained by catalytic decomposition. As a result of the high catalytic activity of the nanostructured film, trapping can be performed at ambient temperature with good efficiency. Limits of detection (LODs) were 2.3 and 0.70 μg L- 1 for Sb and Bi, respectively. Enrichment factors of 534 and 192 were obtained for Sb and Bi, respectively. The new method was applied for the analysis of several matrices (milk, soil, sediment, cutaneous powder). Recoveries were in the range of 98.4-101% for both elements with a relative standard deviation of 2.5% (N = 5).

  18. 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.

  19. Determination of trace germanium in health protection food by hydride generation atomic fluorescence spectrometry%氢化物-原子荧光光谱法测定保健食品中痕量锗

    Institute of Scientific and Technical Information of China (English)

    宋伟明; 倪刚; 胡奇林; 全晓塞

    2001-01-01

    A new method was introduced for the determination of trace germanium by hydride generation atomic fluorescence spectrometry(HGAFS).The effect of the medium amounts of acid, action of hydride and screening agent of the determination of germanium was investigated. The operating condition of the instrument was optimized. The interference from foreign ions was eliminated by adding phosphoric acid and tartaric acid. This method was applied to the determination of germanium in some health protection and nourishing food. The detection limit (3δ) is 6.2 ng/g with a RSD of 5% .The recovery of standard addition is in 95%~105%.%提出了以氢化物-原子荧光光谱法测定保健食品中锗的新方法,研究了酸介质、氢化物发生、增敏掩蔽剂等因素对测定的影响,并选择出仪器的最佳工作条件;采用磷酸-酒石酸介质进行测定,不但可有效消除共存离子的干扰,而且起到增敏作用,方法的检出限为6.2,ng/g,相对标准偏差(RSD)在5%以内,加标回收率为95%~105%,结果令人满意.

  20. Synthesis of Renewable Energy Materials, Sodium Aluminum Hydride by Grignard Reagent of Al

    Directory of Open Access Journals (Sweden)

    Jun-qin Wang

    2015-01-01

    Full Text Available The research on hydrogen generation and application has attracted widespread attention around the world. This paper is to demonstrate that sodium aluminum hydride can be synthesized under simple and mild reaction condition. Being activated through organics, aluminum powder reacts with hydrogen and sodium hydride to produce sodium aluminum hydride under atmospheric pressure. The properties and composition of the sample were characterized by FTIR, XRD, SEM, and so forth. The results showed that the product through this synthesis method is sodium aluminum hydride, and it has higher purity, perfect crystal character, better stability, and good hydrogen storage property. The reaction mechanism is also discussed in detail.

  1. Room temperature trapping of stibine and bismuthine onto quartz substrates coated with nanostructured palladium for total reflection X-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Romero, Vanesa; Costas-Mora, Isabel; Lavilla, Isela; Bendicho, Carlos, E-mail: bendicho@uvigo.es

    2015-05-01

    In this work, a novel method for determining Sb and Bi based on the trapping of their covalent hydrides onto quartz reflectors coated with immobilized palladium nanoparticles (Pd NPs) followed by total reflection X-ray fluorescence (TXRF) analysis is proposed. Pd NPs were synthesized by chemical reduction of the metal precursor using a mixture of water:ethanol as mild reducing agent. Silanization using 3-mercaptopropyltrimethoxysilane (MPTMS) was performed for the immobilization of Pd NPs onto the quartz substrates. Volatile hydrides (stibine and bismuthine) generated by means of a continuous flow system were flushed onto the immobilized Pd NPs and retained by catalytic decomposition. As a result of the high catalytic activity of the nanostructured film, trapping can be performed at ambient temperature with good efficiency. Limits of detection (LODs) were 2.3 and 0.70 μg L{sup −1} for Sb and Bi, respectively. Enrichment factors of 534 and 192 were obtained for Sb and Bi, respectively. The new method was applied for the analysis of several matrices (milk, soil, sediment, cutaneous powder). Recoveries were in the range of 98.4–101% for both elements with a relative standard deviation of 2.5% (N = 5). - Highlights: • A novel method for trapping covalent hydrides of antimony and bismuth is proposed. • Emphasis is placed on the application of Pd nanoparticles as trapping surface. • The nanostructured surface provides high catalytic activity at ambient temperature. • Analysis by total reflection X-ray fluorescence is performed. • Determination of Bi and Sb in different matrices is carried out.

  2. 离子色谱-氢化物发生原子荧光法测定尿中形态砷%Determination of arsenic species in urine by ion chromatography-hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    魏静; 梁琼; 刘俊娓

    2013-01-01

    Objective:To develop a method for the determination of arsenic species in urine by Ion chromatography - hydride Generation - atomic fluorescence spectrometry. Methods; The urine sample was filtered by 0.45 μm membrane. Using ( NH4 ) 2 HPO4 as mobile phase to explore the best ion chromatographic separation condition and the atomic fluorescence determination condition. The content of various forms of arsenic was determined by Ion chromatography - hydride Generation - atomic fluorescence spectrometry. Results; This method had good relativity and good precision(2.60% ~4. 30% ). The detection limits of As( Ⅲ), DMA, MMA and As( V ) were 2. 0 (μg/L, 4.0 μg/L,4.0 μg/L,8.0 μg/L, the average recoveries of samples were 90.48% ~ 102.90%. Conclusion; The method had the advantages of convenience, speediness, high sensitivity, less interference and high practical value without chemical pretreatment.%目的:建立离子色谱-氢化物发生原子荧光法测定尿中形态砷的方法.方法:尿样经0.45 μm滤膜过滤,以(NH4)2HPO4为流动相,采用离子色谱-氢化物发生原子荧光联机测定不同形态砷的含量.结果:实验结果相关性好,线性范围宽,精密度RSD为2.60%~4.30%,方法检出限为As(Ⅲ)2.0 μg/L,DMA4.0 μg/L,MMA4.0 μg/L,As(V)8.0 μg/L,该方法所得回收率为90.48% ~ 102.90%.结论:方法简便、快速、无需化学预处理、干扰少、灵敏度高,有较高的实用价值.

  3. Constraints on the depth of generation and emplacement of a magmatic epidote-bearing quartz diorite pluton in the Coast Plutonic Complex, British Columbia

    Science.gov (United States)

    Chang, J.M.; Andronicos, C.L.

    2009-01-01

    Petrology and P-T estimates indicate that a magmatic epidote-bearing quartz diorite pluton from Mt. Gamsby, Coast Plutonic Complex, British Columbia, was sourced at pressures below ???1.4 GPa and cooled nearly isobarically at ???0.9 GPa. The P-T path indicates that the magma was within the stability field of magmatic epidote early and remained there upon final crystallization. The pluton formed and crystallized at depths greater than ???30 km. REE data indicate that garnet was absent in the melting region and did not fractionate during crystallization. This suggests that the crust was less than or equal to ???55 km thick at 188 Ma during the early phases of magmatism in the Coast Plutonic Complex. Late Cretaceous contractional deformation and early Tertiary extension exhumed the rocks to upper crustal levels. Textures of magmatic epidote and other magmatic phases, combined with REE data, can be important for constraining the P-T path followed by magmas. ?? 2009 Blackwell Publishing Ltd.

  4. 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.

  5. Hydride development for hydrogen storage

    Energy Technology Data Exchange (ETDEWEB)

    Thomas, G.J.; Guthrie, S.E.; Bauer, W.; Yang, N.Y.C. [Sandia National Lab., Livermore, CA (United States); Sandrock, G. [SunaTech, Inc., Ringwood, NJ (United States)

    1996-10-01

    The purpose of this project is to develop and demonstrate improved hydride materials for hydrogen storage. The work currently is organized into four tasks: hydride development, bed fabrication, materials support for engineering systems, and IEA Annex 12 activities. At the present time, hydride development is focused on Mg alloys. These materials generally have higher weight densities for storing hydrogen than rare earth or transition metal alloys, but suffer from high operating temperatures, slow kinetic behavior and material stability. The authors approach is to study bulk alloy additions which increase equilibrium overpressure, in combination with stable surface alloy modification and particle size control to improve kinetic properties. This work attempts to build on the considerable previous research in this area, but examines specific alloy systems in greater detail, with attention to known phase properties and structures. The authors have found that specific phases can be produced which have significantly improved hydride properties compared to previous studies.

  6. Differential determination of arsenic(III) and arsenic(V), and antimony(III) and antimony-(V) by hydride generation-atomic absorption spectrophotometry, and its application to the determination of these species in sea water

    Science.gov (United States)

    Yamamoto, Manabu; Urata, Keiji; Murashige, Kiyoto; Yamamoto, Yuroku

    A method is described for the differential determination of As(III) and As(V). and Sb(III) and Sb(V) by hydride generation-atomic absorption spectrophotometry with hydrogen-nitrogen flame using sodium borohydride solution as a reductant. For the determination of As(III) and Sb(III), most of the elements, other than Ag +, Cu 2+, Sn 2+, Se 4+ and Te 4+, do not interfere in an at least 30,000 fold excess with respect to As(III) or Sb(III). This method was applied to the determination of these species in sea water and it was found that a sample size of only 100 ml is enough to determine them with a precision of 1.5-2.5%. Analytical results for surface sea water of Hiroshima Bay were 0.72 μgl -1, 0.27 μgl -1 and 0.22 μgl -1 for As(total), As(III) and Sb(total), respectively, but Sb(III) was not detected in the present sample. The effect of acidification on storage was also examined.

  7. 氢化物发生-原子荧光光谱法测定红土镍矿中砷%DETERMINATION OF ARSENIC IN LATERITE NICKEL ORES BY HYDRIDE GENERATION-ATOMIC FLUORESCENCE SPECTROMETRY

    Institute of Scientific and Technical Information of China (English)

    陈殿耿; 袁玉霞; 何飞顶

    2012-01-01

    提出了以硫脲-抗坏血酸作为还原掩蔽剂,氢化物发生-原子荧光光谱法( HG-AFS)直接测定红土镍矿中砷的方法.考察了测定的最佳条件、共存元素对测定的影响及方法的精密度和回收率.方法适用于红土镍矿中0.005%~0.1%砷的测定.%A method for the determination of arsenic in laterite nickel ores by hydride generation-atomic fluorescence spectrometry (HG-AFS) directly with thiourea-ascorbic acid hydrochloride as masking is proposed. The optimum experimental parameters, the effect of coexistent elements on the determination of arsenic, the precision and recovery of the method are investigated. The method can be applied to the determination of 0. 005% ~ 0. 1% arsenic in laterite nickel ores.

  8. A simple and sensitive flow-injection on-line preconcentration coupled with hydride generation atomic fluorescence spectrometry for the determination of ultra-trace lead in water, wine, and rice.

    Science.gov (United States)

    Wu, Hong; Jin, Yan; Luo, Mingbiao; Bi, Shuping

    2007-09-01

    A simple and sensitive flow-injection on-line separation and preconcentration system coupled to hydride generation atomic fluorescence spectrometry (HG-AFS) was developed for ultra-trace lead determination in water, wine, and rice samples, with the salient advantages of its minimization of transition-metal interferences and tolerance to an ethanol matrix. A lead hydroxide precipitate was achieved by the on-line merging of a sample and an ammonium buffer solution and collected onto the inner walls of a knotted reactor (KR). Removal of the residual solution from KR was achieved by air flow, and dissolution of the precipitate was carried out by using 0.2 mol l(-1) HCl. With a sample consumption of 11.7 ml, an enhancement factor of 16 was obtained at a sample throughput of 30 h(-1). The limit of detection (3s) was 16 ng l(-1) and the precision (RSD) for 1.0 microg l(-1) Pb was 3.4%.

  9. 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...... volume is 100 mu l while the total sample consumption per assay is 1.33 ml, and the sampling frequency is 180 samples per hour. The detection limit (3 sigma) for the on-line reduction procedure was 37 ng l(-1) and at the 5.0 mu g l(-1), the relative standard deviation (RSD) was 1.1% (n=10) by calibrating...... with As(III) standards; by calibrating with As(V) standards the detection limit was 33 ng l(-1) and the RSD was 1.3% (n=10). For the selective determination of As(III) the detection limit was 111 ng l(-1) and the RSD was 0.7% (n=10) at 5.0 mu g l(-1). Both procedures are most tolerant to potential...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-12-01

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

  11. Real-time measurement of desorption temperature and kinetics of magnesium hydride powder sample based on optical reflection

    Energy Technology Data Exchange (ETDEWEB)

    Poh, Chung-Kiak [Institute for Superconducting and Electronic Materials, University of Wollongong, Innovation Campus, Squires Way, Fairy Meadow, NSW 2519 (Australia); Guo, Zaiping; Liu, Hua-Kun [Institute for Superconducting and Electronic Materials, University of Wollongong, Innovation Campus, Squires Way, Fairy Meadow, NSW 2519 (Australia); CSIRO National Hydrogen Materials Alliance, CSIRO Energy Centre, 10 Murray Dwyer Circuit, Steel River Estate, Mayfield West, NSW 2304 (Australia)

    2009-11-15

    We demonstrate the proof-of-principle that interaction between visible light and a magnesium hydride sample in reflective mode can be used to determine the desorption temperature and kinetics of magnesium hydride in powder form. The demonstrated optical technique requires only milligrams of sample and can potentially be used to measure the de/absorption temperature and kinetics of magnesium nanostructures, which are often fabricated via the physical vapor deposition method inside an optically transparent quartz tube. This would help to eliminate the common problem of oxidation associated with removal and transport of the freshly fabricated nanostructures into an inert protective environment. This optical technique could be applied to any hydrogen-storage material in the form of powder which shows a significant difference in its optical absorption between the hydride and the non-hydride phase. (author)

  12. Metal hydride air conditioner

    Institute of Scientific and Technical Information of China (English)

    YANG; Ke; DU; Ping; LU; Man-qi

    2005-01-01

    The relationship among the hydrogen storage properties, cycling characteristics and thermal parameters of the metal hydride air conditioning systems was investigated. Based on a new alloy selection model, three pairs of hydrogen storage alloys, LaNi4.4 Mn0.26 Al0.34 / La0.6 Nd0.4 Ni4.8 Mn0.2 Cu0. 1, LaNi4.61Mn0. 26 Al0.13/La0.6 Nd0.4 Ni4.8 Mn0.2 Cu0. 1 and LaNi4.61 Mn0.26 Al0.13/La0.6 Y0.4 Ni4.8 Mn0. 2, were selected as the working materials for the metal hydride air conditioning system. Studies on the factors affecting the COP of the system showed that higher COP and available hydrogen content need the proper operating temperature and cycling time,large hydrogen storage capacity, flat plateau and small hysterisis of hydrogen alloys, proper original input hydrogen content and mass ratio of the pair of alloys. It also needs small conditioning system was established by using LaNi4.61 Mn0.26 Al0. 13/La0.6 Y0.4 Ni4.8 Mn0.2 alloys as the working materials, which showed that under the operating temperature of 180℃/40℃, a low temperature of 13℃ was reached, with COP =0.38 and Wnet =0.09 kW/kg.

  13. Geoneutrino and Hydridic Earth model

    CERN Document Server

    Bezrukov, Leonid

    2013-01-01

    Uranium, Thorium and Potassium-40 abundances in the Earth were calculated in the frame of Hydridic Earth model. Terrestrial heat producton from U, Th and K40 decays was calculated also. We must admit the existance of Earth expansion process to understand the obtained large value of terrestrial heat producton. The geoneutrino detector with volume more than 5 kT (LENA type) must be constructed to definitely separate between Bulk Silicat Earth model and Hydridic Earth model.

  14. Quartz crystal growth

    Science.gov (United States)

    Baughman, Richard J.

    1992-01-01

    A process for growing single crystals from an amorphous substance that can undergo phase transformation to the crystalline state in an appropriate solvent. The process is carried out in an autoclave having a lower dissolution zone and an upper crystallization zone between which a temperature differential (.DELTA.T) is maintained at all times. The apparatus loaded with the substance, solvent, and seed crystals is heated slowly maintaining a very low .DELTA.T between the warmer lower zone and cooler upper zone until the amorphous substance is transformed to the crystalline state in the lower zone. The heating rate is then increased to maintain a large .DELTA.T sufficient to increase material transport between the zones and rapid crystallization. .alpha.-Quartz single crystal can thus be made from fused quartz in caustic solvent by heating to 350.degree. C. stepwise with a .DELTA.T of 0.25.degree.-3.degree. C., increasing the .DELTA.T to about 50.degree. C. after the fused quartz has crystallized, and maintaining these conditions until crystal growth in the upper zone is completed.

  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. Physics of hydride fueled PWR

    Science.gov (United States)

    Ganda, Francesco

    The first part of the work presents the neutronic results of a detailed and comprehensive study of the feasibility of using hydride fuel in pressurized water reactors (PWR). The primary hydride fuel examined is U-ZrH1.6 having 45w/o uranium: two acceptable design approaches were identified: (1) use of erbium as a burnable poison; (2) replacement of a fraction of the ZrH1.6 by thorium hydride along with addition of some IFBA. The replacement of 25 v/o of ZrH 1.6 by ThH2 along with use of IFBA was identified as the preferred design approach as it gives a slight cycle length gain whereas use of erbium burnable poison results in a cycle length penalty. The feasibility of a single recycling plutonium in PWR in the form of U-PuH2-ZrH1.6 has also been assessed. This fuel was found superior to MOX in terms of the TRU fractional transmutation---53% for U-PuH2-ZrH1.6 versus 29% for MOX---and proliferation resistance. A thorough investigation of physics characteristics of hydride fuels has been performed to understand the reasons of the trends in the reactivity coefficients. The second part of this work assessed the feasibility of multi-recycling plutonium in PWR using hydride fuel. It was found that the fertile-free hydride fuel PuH2-ZrH1.6, enables multi-recycling of Pu in PWR an unlimited number of times. This unique feature of hydride fuels is due to the incorporation of a significant fraction of the hydrogen moderator in the fuel, thereby mitigating the effect of spectrum hardening due to coolant voiding accidents. An equivalent oxide fuel PuO2-ZrO2 was investigated as well and found to enable up to 10 recycles. The feasibility of recycling Pu and all the TRU using hydride fuels were investigated as well. It was found that hydride fuels allow recycling of Pu+Np at least 6 times. If it was desired to recycle all the TRU in PWR using hydrides, the number of possible recycles is limited to 3; the limit is imposed by positive large void reactivity feedback.

  17. Assessing nanoparticle size effects on metal hydride thermodynamics using the Wulff construction.

    Science.gov (United States)

    Kim, Ki Chul; Dai, Bing; Karl Johnson, J; Sholl, David S

    2009-05-20

    The reaction thermodynamics of metal hydrides are crucial to the use of these materials for reversible hydrogen storage. In addition to altering the kinetics of metal hydride reactions, the use of nanoparticles can also change the overall reaction thermodynamics. We use density functional theory to predict the equilibrium crystal shapes of seven metals and their hydrides via the Wulff construction. These calculations allow the impact of nanoparticle size on the thermodynamics of hydrogen release from these metal hydrides to be predicted. Specifically, we study the temperature required for the hydride to generate a H(2) pressure of 1 bar as a function of the radius of the nanoparticle. In most, but not all, cases the hydrogen release temperature increases slightly as the particle size is reduced.

  18. Development of Quartz Fiber Calorimetry

    CERN Multimedia

    2002-01-01

    % RD40 \\\\ \\\\ Very Forward Calorimeters (VFCs) in LHC detectors should cover the pseudorapidity range from $\\eta$~=~2.5 to at least $\\eta$~=~5 in order to compute missing transverse energy and for jet tagging. Operation at such high rapidity requires the use of a calorimetry technique that is very radiation resistant, fast and insensitive to radioactivity (especially to neutrons). This can be accomplished through the Quartz-Calorimeter~(Q-Cal) concept of embedding silica core fibers, that resist to the Gigarad radiation level, into an absorber. In this calorimeter the shower particles produce light through the Cherenkov effect generating a signal less than 10~ns in duration. Unique to this new technology the visible energy of hadronic showers has a transverse dimension nearly an order of magnitude smaller than that in conventional calorimeters, enabling precise spatial resolution, sharper isolation cuts and better jet recognition against the minimum bias events background. Last but not least, most radioactive ...

  19. Iron Hydride Detection and Intramolecular Hydride Transfer in a Synthetic Model of Mono-Iron Hydrogenase with a CNS Chelate.

    Science.gov (United States)

    Durgaprasad, Gummadi; Xie, Zhu-Lin; Rose, Michael J

    2016-01-19

    We report the identification and reactivity of an iron hydride species in a synthetic model complex of monoiron hydrogenase. The hydride complex is derived from a phosphine-free CNS chelate that includes a Fe-C(NH)(═O) bond (carbamoyl) as a mimic of the active site iron acyl. The reaction of [((O═)C(HN)N(py)S(Me))Fe(CO)2(Br)] (1) with NaHBEt3 generates the iron hydride intermediate [((O═)C(HN)N(py)S(Me))Fe(H)(CO)2] (2; δFe-H = -5.08 ppm). Above -40 °C, the hydride species extrudes CH3S(-) via intramolecular hydride transfer, which is stoichiometrically trapped in the structurally characterized dimer μ2-(CH3S)2-[((O═)C(HN)N(Ph))Fe(CO)2]2 (3). Alternately, when activated by base ((t)BuOK), 1 undergoes desulfurization to form a cyclometalated species, [((O═)C(NH)NC(Ph))Fe(CO)2] (5); derivatization of 5 with PPh3 affords the structurally characterized species [((O═)C(NH)NC)Fe(CO)(PPh3)2] (6), indicating complex 6 as the common intermediate along each pathway of desulfurization.

  20. 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)

  1. First-principles study of superabundant vacancy formation in metal hydrides.

    Science.gov (United States)

    Zhang, Changjun; Alavi, Ali

    2005-07-13

    Recent experiments have established the generality of superabundant vacancies (SAV) formation in metal hydrides. Aiming to elucidate this intriguing phenomenon and to clarify previous interpretations, we employ density-functional theory to investigate atomic mechanisms of SAV formation in fcc hydrides of Ni, Cu, Rh, Pd, Ag, Ir, Pt, and Au. We have found that upon H insertion, vacancy formation energies reduce substantially. This is consistent with experimental suggestions. We demonstrate that the entropy effect, which has been proposed to explain SAV formation, is not the main cause. Instead, it is the drastic change of electronic structure induced by the H in the SAV hydrides, which is to a large extent responsible. Interesting trends in systems investigated are also found: ideal hydrides of 5d metals and noble metals are unstable compared to the corresponding pure metals, but the SAV hydrides are more stable than the corresponding ideal hydrides, whereas opposite results exist in the cases of Ni, Rh, and Pd. These trends of stabilities of the SAV hydrides are discussed in detail and a general understanding for SAV formation is provided. Finally, we propose an alternative reaction pathway to generate a SAV hydride from a metal alloy.

  2. A New Reducing Regent: Dichloroindium Hydride

    Institute of Scientific and Technical Information of China (English)

    A. BABA; I. SHIBATA; N. HAYASHI

    2005-01-01

    @@ 1Introduction Among the hydride derivatives of group 13 elements, various types of aluminum hydrides and boron hydrides have been employed as powerful reduction tools. Indium hydrides have not received much attention,whereas the synthesis of indium trihydride (InH3) was reported several decades ago[1]. There have been no precedents for monometallic indium hydrides having practical reactivity, while activated hydrides such as an ate complex LiPhn InH4-n (n = 0- 2) and phosphine-coordinated indium hydrides readily reduce carbonyl compounds. In view of this background, we focused on the development of dichloroindium hydrides (Cl2InH) as novel reducing agents that bear characteristic features in both ionic and radical reactions.

  3. 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

  4. Complex and liquid hydrides for energy storage

    Energy Technology Data Exchange (ETDEWEB)

    Callini, Elsa; Atakli, Zuleyha Özlem Kocabas; Hauback, Bjørn C.; Orimo, Shin-ichi; Jensen, Craig; Dornheim, Martin; Grant, David; Cho, Young Whan; Chen, Ping; Hjörvarsson, Bjørgvin; de Jongh, Petra; Weidenthaler, Claudia; Baricco, Marcello; Paskevicius, Mark; Jensen, Torben R.; Bowden, Mark E.; Autrey, Thomas S.; Züttel, Andreas

    2016-03-10

    The research on complex hydrides for hydrogen storage was imitated by the discovery of Ti as a hydrogen sorption catalyst in NaAlH4 by Boris Bogdanovic in 1996. A large number of new complex hydride materials in various forms and combinations have been synthesized and characterized and the knowledge on the properties of complex hydrides and the synthesis methods has grown enormously since then. A significant part of the research groups active in the field of complex hydrides are collaborators in the IEA task 32. This paper reports about the important issues in the field of the complex hydride research, i.e. the synthesis of borohydrides, the thermodynamics of complex hydrides and their thermodynamic properties, the effects of size and confinement, the hydrogen sorption mechanism and the complex hydride composites as well as the properties of liquid complex hydrides. This paper is the result of the collaboration of several groups and excellent summary of the recent achievements.

  5. Luminescent properties of aluminum hydride

    Energy Technology Data Exchange (ETDEWEB)

    Baraban, A.P.; Gabis, I.E.; Dmitriev, V.A. [Saint-Petersburg State University, Department of Physics, Saint-Petersburg 198504 (Russian Federation); Dobrotvorskii, M.A., E-mail: mstislavd@gmail.com [Saint-Petersburg State University, Department of Physics, Saint-Petersburg 198504 (Russian Federation); Kuznetsov, V.G. [Saint-Petersburg State University, Department of Physics, Saint-Petersburg 198504 (Russian Federation); Matveeva, O.P. [National Mineral Resources University, Saint Petersburg 199106 (Russian Federation); Titov, S.A. [Petersburg State University of Railway Transport, Saint-Petersburg 190031 (Russian Federation); Voyt, A.P.; Elets, D.I. [Saint-Petersburg State University, Department of Physics, Saint-Petersburg 198504 (Russian Federation)

    2015-10-15

    We studied cathodoluminescence and photoluminescence of α-AlH{sub 3}– a likely candidate for use as possible hydrogen carrier in hydrogen-fueled vehicles. Luminescence properties of original α-AlH{sub 3} and α-AlH{sub 3} irradiated with ultraviolet were compared. The latter procedure leads to activation of thermal decomposition of α-AlH{sub 3} and thus has a practical implementation. We showed that the original and UV-modified aluminum hydride contain luminescence centers ‐ structural defects of the same type, presumably hydrogen vacancies, characterized by a single set of characteristic bands of radiation. The observed luminescence is the result of radiative intracenter relaxation of the luminescence center (hydrogen vacancy) excited by electrons or photons, and its intensity is defined by the concentration of vacancies, and the area of their possible excitation. UV-activation of the dehydrogenation process of aluminum hydride leads to changes in the spatial distribution of the luminescence centers. For short times of exposure their concentration increases mainly in the surface regions of the crystals. At high exposures, this process extends to the bulk of the aluminum hydride and ends with a decrease in concentration of luminescence centers in the surface region. - Highlights: • Aluminum hydride contains hydrogen vacancies which serve as luminescence centers. • The luminescence is the result of radiative relaxation of excited centers. • Hydride UV-irradiation alters distribution and concentration of luminescence centers.

  6. Photochemistry of Transition Metal Hydrides.

    Science.gov (United States)

    Perutz, Robin N; Procacci, Barbara

    2016-08-10

    Photochemical reactivity associated with metal-hydrogen bonds is widespread among metal hydride complexes and has played a critical part in opening up C-H bond activation. It has been exploited to design different types of photocatalytic reactions and to obtain NMR spectra of dilute solutions with a single pulse of an NMR spectrometer. Because photolysis can be performed on fast time scales and at low temperature, metal-hydride photochemistry has enabled determination of the molecular structure and rates of reaction of highly reactive intermediates. We identify five characteristic photoprocesses of metal monohydride complexes associated with the M-H bond, of which the most widespread are M-H homolysis and R-H reductive elimination. For metal dihydride complexes, the dominant photoprocess is reductive elimination of H2. Dihydrogen complexes typically lose H2 photochemically. The majority of photochemical reactions are likely to be dissociative, but hydride complexes may be designed with equilibrated excited states that undergo different photochemical reactions, including proton transfer or hydride transfer. The photochemical mechanisms of a few reactions have been analyzed by computational methods, including quantum dynamics. A section on specialist methods (time-resolved spectroscopy, matrix isolation, NMR, and computational methods) and a survey of transition metal hydride photochemistry organized by transition metal group complete the Review.

  7. Quartz Crystal Microbalance Data

    Energy Technology Data Exchange (ETDEWEB)

    Baxamusa, S H

    2011-11-16

    We are using a Qpod quartz crystal microbalance (manufactured by Inficon) for use as a low-volume non-volatile residue analysis tool. Inficon has agreed to help troubleshoot some of our measurements and are requesting to view some sample data, which are attached. The basic principle of an NVR analysis is to evaporate a known volume of solvent, and weigh the remaining residue to determine the purity of the solvent. A typical NVR analysis uses 60 g of solvent and can measure residue with an accuracy of +/- 0.01 mg. The detection limit is thus (0.01 mg)/(60 g) = 0.17 ppm. We are attempting to use a quartz crystal microbalance (QCM) to make a similar measurement. The attached data show the response of the QCM as a 5-20 mg drop of solvent evaporates on its surface. The change in mass registered by the QCM after the drop evaporates is the residue that deposits on the crystal. On some measurements, the change in mass in less than zero, which is aphysical since the drop will leave behind {>=}0 mass of residue. The vendor, Inficon, has agreed to look at these data as a means to help troubleshoot the cause.

  8. Hydrogen, lithium, and lithium hydride production

    Science.gov (United States)

    Brown, Sam W; Spencer, Larry S; Phillips, Michael R; Powell, G. Louis; Campbell, Peggy J

    2014-03-25

    A method of producing high purity lithium metal is provided, where gaseous-phase lithium metal is extracted from lithium hydride and condensed to form solid high purity lithium metal. The high purity lithium metal may be hydrided to provide high purity lithium hydride.

  9. Simultaneous Determination of Arsenic and Antimony in Water by Hydride Generation-Atomic Fluorescence Spectrometry%氢化物发生-原子荧光光谱法同时测定水中砷和锑

    Institute of Scientific and Technical Information of China (English)

    黄选忠; 万忠卫; 杜宏山; 郑丽

    2013-01-01

    建立在硝酸介质中用氢化物发生-原子荧光光谱法同时测定水中砷和锑的方法。优化了仪器工作条件、酸度、硼氢化钾及还原剂浓度。砷、锑的线性范围为0~10.0µg/L;检出限分别为0.02,0.01µg/L;测定结果的相对标准偏差分别为1.77%~3.72%,2.95%~4.87%(n=6);加标回收率分别为98%~106%,96%~105%。该法操作简便,灵敏度高,快速,便于推广,适用于水中砷和锑的同时测定。%The method for simultaneous determination of arsenic and antimony in water was established by hydride-generation atomic fluorescence spectrometry in nitric acid medium. Instrument condition,acidity,concentration of potassium borohydride and thiourea-ascorbic acid were selected. The linear relationship of arsenic and antimony was 0-10.0 µg/L. The detection limit of arsenic and antimony was 0.02 µg/L and 0.01 µg/L, the relative standard deviation of arsenic and antimony determination results was 1.77%-3.72%and 2.95%-4.87%(n=6) , the recovery of standard addition of arsenic and antimony was 98%-106%and 96%-105%respectively. This method has the advantages of simple operation and high sensitivity,it is rapid and easy to spread,which is suitable for simultaneous determination of arsenic and antimony in water.

  10. 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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-04-04

    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)

  11. Determination of Se in Saffron by Using Hydride Generation Atomic Fluorescence Spectrometry%氢化物发生原子荧光光谱法测定西红花柱头中的硒

    Institute of Scientific and Technical Information of China (English)

    张宏; 张新申; 颜钫; 陈放

    2001-01-01

    A method for determination of Se in saffron using AFS-230 hydride generation atomic fluorescence spectrometry was introduced.Detections were completed made in every possible best condition.The optimal analytical conditions in HClO4-HNO3 were examined.The detection limit is 0.5μg/L.The linear range is 1.5~15.0 μg/L.The correlation coefficient is 0.9999,and the recovery rate is about 90%~97%.Se of saffrons from 4 regions was determined by standard curve method.The experiment results show that this method has low detection limit,high accurate,simple operation,fast and low cost.It's easy to be spread.%应用AFS-230型双道原子荧光光谱计进行了氢化物发生原子荧光光谱法测定西红花柱头中硒的研究,方法中采用硝酸做介质,并对各种最佳分析条件进行了测定。线性范围为1.5~15μg/L,相关系数R=0.9999,回收率为90%~97%。采用标准曲线法对4种不同产地的西红花干燥柱头中硒进行了测定。该方法操作简单、快速,精密度好,准确性高,检出限较低,经济,便于推广应用。

  12. Simultaneous speciation of inorganic arsenic and antimony in water samples by hydride generation-double channel atomic fluorescence spectrometry with on-line solid-phase extraction using single-walled carbon nanotubes micro-column

    Energy Technology Data Exchange (ETDEWEB)

    Wu Hong, E-mail: wuhong1968@hotmail.com; Wang Xuecui; Liu Bing; Liu Yueling; Li Shanshan; Lu Jusheng; Tian Jiuying; Zhao Wenfeng; Yang Zonghui

    2011-01-15

    A new method was developed for the simultaneous speciation of inorganic arsenic and antimony in water by on-line solid-phase extraction coupled with hydride generation-double channel atomic fluorescence spectrometry (HG-DC-AFS). The speciation scheme involved the on-line formation and retention of the ammonium pyrrolidine dithiocarbamate complexes of As(III) and Sb(III) on a single-walled carbon nanotubes packed micro-column, followed by on-line elution and simultaneous detection of As(III) and Sb(III) by HG-DC-AFS; the total As and total Sb were determined by the same protocol after As(V) and Sb(V) were reduced by thiourea, with As(V) and Sb(V) concentrations obtained by subtraction. Various experimental parameters affecting the on-line solid-phase extraction and determination of the analytes species have been investigated in detail. With 180 s preconcentration time, the enrichment factors were found to be 25.4 for As(III) and 24.6 for Sb(III), with the limits of detection (LODs) of 3.8 ng L{sup -1} for As(III) and 2.1 ng L{sup -1} for Sb(III). The precisions (RSD) for five replicate measurements of 0.5 {mu}g L{sup -1} of As(III) and 0.2 {mu}g L{sup -1} of Sb(III) were 4.2 and 4.8%, respectively. The developed method was validated by the analysis of standard reference materials (NIST SRM 1640a), and was applied to the speciation of inorganic As and Sb in natural water samples.

  13. Optimize parameters of hydride generation-atomic fluorescence spectrometry for inorganic arsenic determination in grain%氢化物发生-原子荧光法测定粮食中无机砷条件的研究

    Institute of Scientific and Technical Information of China (English)

    杨庆惠

    2012-01-01

    应用氢化物发生—原子荧光分析技术进行粮食中无机砷测定的研究,通过优化酸度、硼氢化钾、载气流量、灯电流以及原子化器高度等分析条件,结果表明,砷浓度在0~30 ng/ml内呈线性关系,相关系数为0.999 9,相对标准偏差为1.6%,检出限为0.054 μg/L,用此方法测定粮食中无机砷,回收率为96.5%~103.5%.该方法简便、快速、灵敏,在实际样品测定中获得到了满意的结果,便于推广应用.%Hydride generation- atomic fluorescence spectrometry was adopted for determine the inorganic arsenic in grain. The experimental parameters such as Ph, KHB4 concentration, flow rate, lamp current and the height of atomizer were optimized. There is linear relation when the arsenic concentration was between 0~30 ng/ml with a correlation coefficient of 0. 999 9. The relative standard deviation was 1. 6%, and the detection limit was 0. 054μg/L. The recovery rate reached to 96. 5%~103. 5%. This method is simple,rapid and sensitive, and got satisfactory results in practicle,it is worth for generalize.

  14. 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

  15. 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...... by annealing at 700°C for 12 hours. The alloys appeared to be nanocrystalline with an average crystallite size around 10 nm before annealing. Special steel containers was developed for the annealing of the metal powders in inert atmosphere. The use of various annealing temperatures was investigated...

  16. Hydrogen Storage in Metal Hydrides

    Science.gov (United States)

    1990-08-01

    Hydrogen Storage Capacity Hydride by weight (%) [1) by volume (g/ml) [2] MgH2 7.00 0.101 Mg2NiH4 3.84 0,081 Mg2CuH4 2.04 - - 27 ...Include Security Classification) Hydrogen Storage in Metal Hydrides (U) 12. PERSONAL AUTHOR(S) DelaRosa, Mark J. 13a. TYPE OF REPORT 13b. TIME...objective of this program was to develop an economical process for pr-ducing a lightweight hydrogen storage medium by the chemical vapor infiltration

  17. Graphite furnace and hydride generation atomic absorption spectrometric determination of cadmium, lead, and tin traces in natural surface waters: study of preconcentration technique performance.

    Science.gov (United States)

    Tsogas, George Z; Giokas, Dimosthenis L; Vlessidis, Athanasios G

    2009-04-30

    In this study three major types of preconcentration methods based upon different principles (cation exchange, physical absorption and hydrophobic extraction) were evaluated and optimized for the extraction and determination of three highly toxic heavy metals namely Cd, Pb and Sn by graphite furnace and hybrid generation atomic absorption spectrometry in real samples. The optimum analytical conditions were examined and the analytical features of each method were revealed and compared. Detection limits as low as 0.003-0.025 microg L(-1) for Cd(2+), 0.05-0.10 microg L(-1) for Pb(2+) and 0.1-0.25 microg L(-1) for Sn(4+) depending on the extraction method were obtained with RSD values between 3.08% and 6.11%. A preliminary assessment of the pollution status of three important natural ecosystems in Epirus region (NW Greece) was performed and some early conclusions were drawn and discussed.

  18. Quartz resonator processing system

    Science.gov (United States)

    Peters, Roswell D. M.

    1983-01-01

    Disclosed is a single chamber ultra-high vacuum processing system for the oduction of hermetically sealed quartz resonators wherein electrode metallization and sealing are carried out along with cleaning and bake-out without any air exposure between the processing steps. The system includes a common vacuum chamber in which is located a rotatable wheel-like member which is adapted to move a plurality of individual component sets of a flat pack resonator unit past discretely located processing stations in said chamber whereupon electrode deposition takes place followed by the placement of ceramic covers over a frame containing a resonator element and then to a sealing stage where a pair of hydraulic rams including heating elements effect a metallized bonding of the covers to the frame.

  19. Crystallography of shear transformations in zirconium hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Cassidy, Michael Philip [Univ. of Illinois, Urbana-Champaign, IL (United States)

    1978-01-01

    The crystallography and substructure of the transformations which have been hypothesized as involving a martensitic shear, and which occur between zirconium hydrides were investigated. Specifically, the formation of gamma zirconium hydride from delta hydride and the delta hydride to epsilon hydride transformation were studied. The habit planes, orientation relationships, lattice invariant shears, and interface structures were determined by transmission electron microscopy and diffraction. Surface tilts were observed and measured with an interference microscope. The direction and magnitude of the shape strain produced by the formation of gamma were determined by the measurement of fiducial scratch displacements. These results were compared with the phenomenological crystallographic theory of martensitic transformations.

  20. Characteristics and Applications of Metal Hydrides

    Science.gov (United States)

    Egan, G. J.; Lynch, F. E.

    1987-01-01

    Report discusses engineering principles of uses of metal hydrides in spacecraft. Metal hydrides absorb, store, pump, compress, and expand hydrogen gas. Additionally, they release or absorb sizeable amounts of heat as they form and decompose - property adapted for thermal-energy management or for propulsion. Describes efforts to: Identify heat sources and sinks suitable for driving metal hydride thermal cycles in spacecraft; develop concepts for hydride subsystems employing available heating and cooling methods; and produce data base on estimated sizes, masses, and performances of hydride devices for spacecraft.

  1. Optimization of Internal Cooling Fins for Metal Hydride Reactors

    Directory of Open Access Journals (Sweden)

    Vamsi Krishna Kukkapalli

    2016-06-01

    Full Text Available Metal hydride alloys are considered as a promising alternative to conventional hydrogen storage cylinders and mechanical hydrogen compressors. Compared to storing in a classic gas tank, metal hydride alloys can store hydrogen at nearly room pressure and use less volume to store the same amount of hydrogen. However, this hydrogen storage method necessitates an effective way to reject the heat released from the exothermic hydriding reaction. In this paper, a finned conductive insert is adopted to improve the heat transfer in the cylindrical reactor. The fins collect the heat that is volumetrically generated in LaNi5 metal hydride alloys and deliver it to the channel located in the center, through which a refrigerant flows. A multiple-physics modeling is performed to analyze the transient heat and mass transfer during the hydrogen absorption process. Fin design is made to identify the optimum shape of the finned insert for the best heat rejection. For the shape optimization, use of a predefined transient heat generation function is proposed. Simulations show that there exists an optimal length for the fin geometry.

  2. Characterization of hydrides and delayed hydride cracking in zirconium alloys

    Science.gov (United States)

    Fang, Qiang

    This thesis tries to fill some of the missing gaps in the study of zirconium hydrides with state-of-art experiments, cutting edge tomographical technique, and a novel numerical algorithm. A new hydriding procedure is proposed. The new anode material and solution combination overcomes many drawbacks of the AECLRTM hydriding method and leads to superior hydriding result compared to the AECL RTM hydriding procedure. The DHC crack growth velocity of as-received Excel alloy and Zr-2.5Nb alloy together with several different heat treated Excel alloy samples are measured. While it already known that the DHC crack growth velocity increases with the increase of base metal strength, the finding that the transverse plane is the weaker plane for fatigue crack growth despite having higher resistance to DHC crack growth was unexpected. The morphologies of hydrides in a coarse grained Zircally-2 sample have been studied using synchrotron x-rays at ESRF with a new technique called Diffraction Contrast Tomography that uses simultaneous collection of tomographic data and diffraction data to determine the crystallographic orientation of crystallites (grains) in 3D. It has been previously limited to light metals such as Al or Mg (due to the use of low energy x-rays). Here we show the first DCT measurements using high energy x-rays (60 keV), allowing measurements in zirconium. A new algorithm of a computationally effcient way to characterize distributions of hydrides - in particular their orientation and/or connectivity - has been proposed. It is a modification of the standard Hough transform, which is an extension of the Hough transform widely used in the line detection of EBSD patterns. Finally, a basic model of hydrogen migration is built using ABAQUS RTM, which is a mature finite element package with tested modeling modules of a variety of physical laws. The coupling of hydrogen diffusion, lattice expansion, matrix deformation and phase transformation is investigated under

  3. Antimony speciation in soils: improving the detection limits using post-column pre-reduction hydride generation atomic fluorescence spectroscopy (HPLC/pre-reduction/HG-AFS).

    Science.gov (United States)

    Quiroz, Waldo; Olivares, David; Bravo, Manuel; Feldmann, Jorg; Raab, Andrea

    2011-04-15

    HG-AFS is highly sensitive and low cost detection system and its use for antimony chemical speciation coupled to HPLC is gaining popularity. However speciation analysis in soils is strongly hampered because the most efficient extractant reported in the literature (oxalic acid) strongly inhibits the generation of SbH(3) by Sb(V), the major species in this kind of matrix, severely affecting its detection limits. The purpose of this research is to reduce the detection limit of Sb(V), by using a post column on-line reduction system with l-cysteine reagent (HPLC/pre-reduction/HG-AFS). The system was optimized by experimental design, optimum conditions found were 2% (w/v) and 10°C temperature coil. Detection limits of Sb(V) and Sb(III) in oxalic acid (0.25 mol L(-1)) were improved from 0.3 and 0.1 μg L(-1) to 0.07 and 0.07 μg L(-1), respectively. The methodology developed was applied to Chilean soils, where Sb(V) was the predominant species. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Properties of nanoscale metal hydrides.

    Science.gov (United States)

    Fichtner, Maximilian

    2009-05-20

    Nanoscale hydride particles may exhibit chemical stabilities which differ from those of a macroscopic system. The stabilities are mainly influenced by a surface energy term which contains size-dependent values of the surface tension, the molar volume and an additional term which takes into account a potential reduction of the excess surface energy. Thus, the equilibrium of a nanoparticular hydride system may be shifted to the hydrogenated or to the dehydrogenated side, depending on the size and on the prefix of the surface energy term of the hydrogenated and dehydrogenated material. Additional complexity appears when solid-state reactions of complex hydrides are considered and phase segregation has to be taken into account. In such a case the reversibility of complex hydrides may be reduced if the nanoparticles are free standing on a surface. However, it may be enhanced if the system is enclosed by a nanoscale void which prevents the reaction partners on the dehydrogenated side from diffusing away from each other. Moreover, the generally enhanced diffusivity in nanocrystalline systems may lower the kinetic barriers for the material's transformation and, thus, facilitate hydrogen absorption and desorption.

  5. Electrochemical hydride generation atomic fluorescence spectrometry with a polyanline modified electrode for detection of tin%聚苯胺修饰电极-电化学氢化物发生原子荧光光谱法测定食品中锡含量

    Institute of Scientific and Technical Information of China (English)

    姜宪娟; 淦五二

    2012-01-01

    An electrochemical hydride generation (EC-HG) system with a polyaniline modified electrode (Pan-ME) as cathode material was developed for Sn ( Ⅳ) determination by couped with atomic fluorescence spectrometry. The electrochemical hydride generation efficiency for Sn (Ⅳ) was improved evidently as the Pan membrane could obstruct the aggradation of Sn atom on cathode surface and facilitate the hydride generation. The effects of experimental parameters and interferences have been studied. The limit of detection ( LOD) was 1. 2 ng/mL (3σ) and the relative standard deviation (RSD) was 2. 3% for eleven consecutive measurements of 50 ng/mL Sn(IV) standard solution.%运用以聚苯胺修饰的石墨电极为阴极的电化学氢化物发生装置实现了锡元素的电化学氢化物发生.在电极表面聚合一层聚苯胺,能够有效地提高锡元素的电化学氢化物发生效率,通过与原子荧光光谱仪联用,成功地测定了食品中的锡含量.本工作对各种实验参数和干扰情况进行了详细研究.方法对锡的检出限为1.2 ng/mL(3σ);样品分析精密度(RSD)为2.3% (50 ng/mL,n=11).

  6. Electrochemical Quartz Crystal Nanobalance

    Science.gov (United States)

    Inzelt, György

    The method of piezoelectric microgravimetry (nanogravimetry) using an electrochemical quartz crystal microbalance (EQCM) or nanobalance (EQCN) can be considered as a novel and much more sensitive version of electrogravimetry. The EQCN technique has become a widely used technique in several areas of electrochemistry, electroanalytical chemistry, bioelectrochemistry, etc. [1-10]. Obviously, mass changes occurring during adsorption, sorption, electrosorption, electrodeposition, or spontaneous deposition can be followed, which is very helpful for the elucidation of reaction mechanism via identification of the species accumulated on the surface. These investigations include metal and alloy deposition, underpotential deposition, electroplating, synthesis of conducting polymers by electropolymerization, adsorption of biologically active materials, and analytical determination of small ions and biomolecules. Of course, the opposite processes, i.e., spontaneous dissolution, electrodissolution, corrosion, can also be studied. Electrochemical oscillations, in which the formation and oxidation of chemisorbed molecular fragments play a determining role, have been studied, too. The majority of the investigations have been devoted to ion and solvent transport associated with the redox transformations of electrochemically active polymers. Similar studies have been carried out regarding polynuclear surface layers such as metal hexacyanometalates as well as inorganic and organic microcrystals of different compositions.

  7. Hydride encapsulation by molecular alkali-metal clusters.

    Science.gov (United States)

    Haywood, Joanna; Wheatley, Andrew E H

    2008-07-14

    The sequential treatment of group 12 and 13 Lewis acids with alkali-metal organometallics is well established to yield so-called ''ate' complexes, whereby the Lewis-acid metal undergoes nucleophilic attack to give an anion, at least one group 1 metal acting to counter this charge. However, an alternative, less well recognised, reaction pathway involves the Lewis acid abstracting hydride from the organolithium reagent via a beta-elimination mechanism. It has recently been shown that in the presence of N,N'-bidentate ligands this chemistry can be harnessed to yield a new type of molecular main-group metal cluster in which the abstracted LiH is effectively trapped, with the hydride ion occupying an interstitial site in the cluster core. Discussion focuses on the development of this field, detailing advances in our understanding of the roles of Lewis acid, organolithium, and amine substrates in the syntheses of these compounds. Structure-types are discussed, as are efforts to manipulate cluster geometry and composition as well as hydride-coordination. Embryonic mechanistic studies are reported, as well as attempts to generate hydride-encapsulation clusters under catalytic control.

  8. Optical emission spectrometric determination of arsenic and antimony by continuous flow chemical hydride generation and a miniaturized microwave microstrip argon plasma operated inside a capillary channel in a sapphire wafer

    Energy Technology Data Exchange (ETDEWEB)

    Pohl, Pawel; Zapata, Israel Jimenez; Bings, Nicolas H. [Universitaet Hamburg, Institut fuer Anorganische und Angewandte Chemie, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Voges, Edgar [Universitaet Dortmund, Fakultaet fuer Elektrotechnik und Informationstechnik, Friedrich-Woehler-Weg 4, D-44221 Dortmund (Germany); Broekaert, Jose A.C. [Universitaet Hamburg, Institut fuer Anorganische und Angewandte Chemie, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)], E-mail: jose.broekaert@chemie.uni-hamburg.de

    2007-05-15

    Continuous flow chemical hydride generation coupled directly to a 40 W, atmospheric pressure, 2.45 GHz microwave microstrip Ar plasma operated inside a capillary channel in a sapphire wafer has been optimized for the emission spectrometric determination of As and Sb. The effect of the NaBH{sub 4} concentration, the concentration of HCl, HNO{sub 3} and H{sub 2}SO{sub 4} used for sample acidification, the Ar flow rate, the reagent flow rates, the liquid volume in the separator as well as the presence of interfering metals such as Fe, Cu, Ni, Co, Zn, Cd, Mn, Pb and Cr, was investigated in detail. A considerable influence of Fe(III) (enhancement of up to 50 %) for As(V) and of Fe(III), Cu(II) and Cr(III) (suppression of up to 75%) as well as of Cd(II) and Mn(II) (suppression by up to 25%) for Sb(III) was found to occur, which did not change by more than a factor of 2 in the concentration range of 2-20 {mu}g ml{sup -1}. The microstrip plasma tolerated the introduction of 4.2 ml min{sup -1} of H{sub 2} in the Ar working gas, which corresponded to an H{sub 2}/Ar ratio of 28%. Under these conditions, the excitation temperature as measured with Ar atom lines and the electron number density as determined from the Stark broadening of the H{sub {beta}} line was of the order of 5500 K and 1.50 . 10{sup 14} cm{sup -3}, respectively. Detection limits (3{sigma}) of 18 ng ml{sup -1} for As and 31 ng ml{sup -1} for Sb were found and the calibration curves were linear over 2 orders of magnitude. With the procedure developed As and Sb could be determined at the 45 and 6.4 {mu}g ml{sup -1} level in a galvanic bath solution containing 2.5% of NiSO{sub 4}. Additionally, As was determined in a coal fly ash reference material (NIST SRM 1633a) with a certified concentration of As of 145 {+-} 15 {mu}g g{sup -1} and a value of 144 {+-} 4 {mu}g g{sup -1} was found.

  9. Determination of Tetraethyl Lead in Water by Hydride Generation-Atomic Absorption Spectrophotometry%水中痕量铜的SBA-15修饰碳糊电极溶出伏安测定法

    Institute of Scientific and Technical Information of China (English)

    杨振兴

    2011-01-01

    Objective To establish a method for the determination of tetraethyl lead in water by hydride generation-atomic absorption spectrophotometry. Methods By solvent extraction of trichloromethane and low-temperature degradation,the best optimum experimental condition of optimal design of orthogonal test: wavelength was 217 nm, lamp current was 3.0 mA, band pass was 0.2 nm, supporting gas was argon GAS (99.99%), argon gas flux was 0.8 L/min, peak height measurement, oxidizing flame, 20 g/L NaBH4 solution,5 mi HNO3 (1.42 g/mi) solution, 1.5 ml HCl(1.19 g/ml) solution, 100 g/L K3Fe(CN)6 solution. Results The limit of detection was 0.049 μg/L,the average recovery rates were 89.7%-101.4% and RSDs were 3.3%-5.3%. Conclusion This method is simple, sensitive, accurate and applicable to the determination of the tetraethyl lead in water.%目的 建立介孔材料修饰碳糊电极测定水中痕量铜的方法.方法 制备SBA-15修饰碳糊电极,并在pH值为4.2的乙酸-乙酸钠缓冲溶液中,采用溶出伏安法对水中痕量铜进行测定.结果 优化实验条件下,相关系数达到0.997 3,测得Cu2+的线性范围和最低检出限分别为2.0×10-10~4.0×10-8mol/L和1.0×10-10mol/L,样品加标回收率为97.0%~101.8%.结论该方法简单、快速、灵敏,可用于实际水样中痕量铜的测定.

  10. 氢化物发生-原子荧光光谱法测定Inconel 718合金中痕量硒%Determination of trace selenium in 718 alloy by hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    向祥蓉; 刘虹; 王佼

    2012-01-01

    本文采用氢化物发生-原子荧光光谱法测定Inconel718合金中痕量硒.对影响其测定的负高压、灯电流、载气流量、屏蔽气流量、载流酸类酸度、硼氢化钾等因素进行了较为详细的研究,优化了测定条件,考察了Inconel718合金主要组成元素和基体元素对硒测定的影响.结果表明,用氟化氨溶液络合,柠檬酸溶液作干扰抑制剂能基本消除基体元素和主要组成元素的干扰.硒浓度在0~100μg/L与荧光强度有良好的线性关系,方法的检出限为0.0083μg/L.对铁镍基高温合金标准样品和Inconel 718合金样品进行9次测定,相对标准偏差为1.6%~3.5%.%In this paper a simple and fast analytical procedure for the determination of selenium in Inconel 718 alloy by hydride generation atomic fluorescence spectrometry(HG-AFS) was developed. The in fluence of instrument parameters such as voltage of PMT, current of lamp, atomizer height, carrier gas rate,shield gas rate and concentration of HCI and KBH4 on the determination of selenium were studied, and the optimized conditions were obtained. Interference of coexistent elements and methods to eliminate the interference were investigated in detail. The results showed that ammonium fluoride and citric acid mo nohydrate were the best masking. Under the optimized conditions, the linear range of selenium is 0 ~ 100μg/L, and the detection limit is 0. 0083 μg/L. The relative standard deviation is 1. 6%~3. 5%(n=9) for the standard sample and the sample of Inconel 718 alloy.

  11. Spectrophotometric Determination of Trace Germanium in Chinese Medicine by Hydride Generation Technique%氢化物发生-分光光度法测定中药中微量锗

    Institute of Scientific and Technical Information of China (English)

    仇佩虹; 张华杰; 谢夏丰

    2001-01-01

    研究了在L-半胱氨酸存在下,锗与硼氢化钠反应产生锗化氢挥发分离,再用显色剂2-(5-NO2-2-吡啶偶氮)-5-二乙氨基酚(5-NO2-PADAP),次氯酸钠,六次甲基四胺的混合液吸收显色,有色溶液在564nm处有最大吸收;摩尔吸光系数为1.84×105L·mol/-1·cm-1,锗在0~500μg/L范围内服从比尔定律;样品标准加入回收率为89%~97%;相对标准偏差小于6.3%;用本法对中药材中微量锗的测定,结果令人满意。%The hydride generation technique was used to determination of germanium in the presence of L-cysteine.The GeH4 was absorbed and coloured by a mixed solution of 2-(5-NO2-2-pyridylazo)-5-diethylaminophenyl(5-NO2-PADAP),NaClO and (CH2)6NH+.The maximum absorption of the colour complex was at 564nm.Its apparent molar absorption coefficient was 1.84×105L·mol-1·cm-1.Beer's law was obeyed for 0~500μg/L germanium.The recoveries of spiked samples were in the range of 89%~97%,while the relative standard deviation was less than 6.3%.This method is sensitive,simple and reproducible.The method has been applied to the determination of Ge in the chinese medicine with satisfactory result.

  12. Determination of Inorganic Arsenic in Atmospheric Particles by Hydride Generation-atomic Fluorescence Spectrometry%氢化物发生-原子荧光光谱法测定大气颗粒物中的砷形态

    Institute of Scientific and Technical Information of China (English)

    梁淑轩; 吴虹; 齐学先; 郑璇; 何晓娇

    2011-01-01

    Concentration of atmospheric particles is one of the atmospheric pollution indicators. Heavy metals in the atmospheric particles can risk for human health in both direct and indirect way. Arsenic is one of the higher metal content in them. The inorganic compounds are far more toxic than their organic metabolites. In this paper, the hydride generation atomic fluorescence spectrometric method was employed to the determination of As ( Ⅲ ) and As (V) in the Atmospheric particles. The amount of reducing agent,acid medium and its acidity, carrier gas and shield gas flow rate and observation height of the fluorescence intensity were investigated, and the interference experiment was carried out for concomitant elements. In the best conditions, the detection limit was 0. 34 μg/L, the recovery ranged from 98.18% ~ 102.54%,and the relative standard deviation was about 0.8%. The method was featured by easy operation, fast speed and it has been applied to the analysis of arsenic in the particles with satisfactory results.%采用氢化物发生原子荧光法直接测定不同粒径大气颗粒物中As(Ⅲ)和As(Ⅴ)的含量.研究了还原剂用量、酸介质及其酸度、载气及屏蔽气流量和观测高度等对荧光强度的影响,探讨了共存离子对砷测定的干扰.在选定的最佳条件下,得到检出限为0.34μg/L,方法检出限为0.21μg/g,加标回收率为98.18%~102.54%,相对标准偏差为0.8%左右.用该方法测定大气颗粒物中不同形态的砷,操作简便,快速,灵敏度高.

  13. The renaissance of hydrides as energy materials

    Science.gov (United States)

    Mohtadi, Rana; Orimo, Shin-Ichi

    2017-02-01

    Materials based on hydrides have been the linchpin in the development of several practical energy storage technologies, of which the most prominent example is nickel-metal hydride batteries. Motivated by the need to meet the future's energy demand, the past decade has witnessed substantial advancements in the research and development of hydrides as media for hydrogen energy storage. More recently, new and rapidly evolving discoveries have positioned hydrides as highly promising materials for future electrochemical energy storage, such as electrolytes for mono- and divalent batteries, and anodes for lithium-ion batteries. In addition, the potential of hydrides in efficient power transmission has been recently revealed. In this Review, we highlight key advances and illustrate how the versatility of hydrides has not only yielded a meaningful past, but also ensures a very bright future.

  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. Inhibited solid propellant composition containing beryllium hydride

    Science.gov (United States)

    Thompson, W. W. (Inventor)

    1978-01-01

    An object of this invention is to provide a composition of beryllium hydride and carboxy-terminated polybutadiene which is stable. Another object of this invention is to provide a method for inhibiting the reactivity of beryllium hydride toward carboxy-terminated polybutadiene. It was found that a small amount of lecithin inhibits the reaction of beryllium hydride with the acid groups in carboxy terminated polybutadiene.

  16. Using a titanium-in-quartz geothermometer for crystallization temperature estimation of the Palaeoproterozoic Suursaari quartz porphyry

    Directory of Open Access Journals (Sweden)

    Kairi Ehrlich

    2012-11-01

    Full Text Available The Suursaari volcanic sequence represents volcanic activity related to Wiborg Batholith rapakivi intrusions in the southern part of the Fennoscandian Shield. The estimated pressure conditions for batholith granitic rocks are 1–5 kbar and crystallization temperatures range from 670 to 890 °C. To describe the temperature regime of the Suursaari volcanic system, a rock sample was taken from the Mäkiinpäällys Mountain outcrop and analysed with laser ablation inductively coupled plasma mass spectrometry. Sample spots were selected from quartz phenocrysts and groundmass. Quartz crystallization temperatures were calculated by the Ti-in-quartz method that takes into account rutile equilibrium and Ti activity in each phase. The calculated crystallization temperatures of the Suursaari quartz porphyry are in the range of 647–738 °C. The results show that the Suursaari quartz porphyry contains two generations of quartz which can be distinguished on the basis of crystallization temperatures: phenocrysts crystallized at higher and groundmass quartz at lower temperature.

  17. Anodematerials for Metal Hydride Batteries

    DEFF Research Database (Denmark)

    Jensen, Jens Oluf

    1997-01-01

    by annealing at 700°C for 12 hours. The alloys appeared to be nanocrystalline with an average crystallite size around 10 nm before annealing. Special steel containers was developed for the annealing of the metal powders in inert atmosphere. The use of various annealing temperatures was investigated......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...... was developed. The parameters milling time, milling intensity, number of balls and form of the alloying metals were investigated. Based on this a final alloying technique for the subsequent preparation of electrode materials was established. The technique comprises milling for 4 hours twice possibly followed...

  18. Predicting formation enthalpies of metal hydrides

    DEFF Research Database (Denmark)

    Andreasen, A.

    2004-01-01

    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 formedby chemical reaction between hydrogen...... and metal and for the stable hydrides this is associated with release of heat (#DELTA#H_f ). The more thermodynamically stable the hydride, the larger DHf, and the higher temperature is needed in order to desorphydrogen (reverse reaction) and vice versa. For practical application the temperature needed...

  19. Research on Metal Hydride Compressor System

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    Ti-Zr series Laves phase hydrogen storage alloys with good hydrogen storage properties, such as large hydrogen capacity, rapid hydriding and dehydriding rate, high compression ratio, gentle plateau, small hysteresis, easily being activated and long cyclic stability etc. for metal hydride compressor have been investigated. In addition, a hydride compressor with special characteristics, namely, advanced filling method, good heat transfer effect and reasonable structural design etc. has also been constructed. A hydride compressor cryogenic system has been assembled coupling the compressor with a J-T micro-throttling refrigeration device and its cooling capacity can reach 0.4 W at 25 K.

  20. Coinage Metal Hydrides: Synthesis, Characterization, and Reactivity.

    Science.gov (United States)

    Jordan, Abraham J; Lalic, Gojko; Sadighi, Joseph P

    2016-08-10

    Hydride complexes of copper, silver, and gold encompass a broad array of structures, and their distinctive reactivity has enabled dramatic recent advances in synthesis and catalysis. This Review summarizes the synthesis, characterization, and key stoichiometric reactions of isolable or observable coinage metal hydrides. It discusses catalytic processes in which coinage metal hydrides are known or probable intermediates, and presents mechanistic studies of selected catalytic reactions. The purpose of this Review is to convey how developments in coinage metal hydride chemistry have led to new organic transformations, and how developments in catalysis have in turn inspired the synthesis of reactive new complexes.

  1. Crystal structure of gold hydride

    Energy Technology Data Exchange (ETDEWEB)

    Degtyareva, Valentina F., E-mail: degtyar@issp.ac.ru

    2015-10-05

    Highlights: • Volume expansion of metal hydrides is due to the increase in the s-band filling. • AuH structure is similar to that of Hg having one more s electron compared to Au. • Structure stability of both Hg and AuH is governed by the Hume-Rothery rule. - Abstract: A number of transition metal hydrides with close-packed metal sublattices of fcc or hcp structures with hydrogen in octahedral interstitial positions were obtained by the high-pressure-hydrogen technique described by Ponyatovskii et al. (1982). In this paper we consider volume increase of metals by hydrogenation and possible crystal structure of gold hydride in relation with the structure of mercury, the nearest neighbor of Au in the Periodic table. Suggested structure of AuH has a basic tetragonal body-centered cell that is very similar to the mercury structure Hg-t I 2. The reasons of stability for this structure are discussed within the model of Fermi sphere–Brillouin zone interactions.

  2. Photoelectron spectroscopic study of carbon aluminum hydride cluster anions

    Science.gov (United States)

    Zhang, Xinxing; Wang, Haopeng; Ganteför, Gerd; Eichhorn, Bryan W.; Kiran, Boggavarapu; Bowen, Kit H.

    2016-10-01

    Numerous previously unknown carbon aluminum hydride cluster anions were generated in the gas phase, identified by time-of-flight mass spectrometry and characterized by anion photoelectron spectroscopy, revealing their electronic structure. Density functional theory calculations on the CAl5-9H- and CAl5-7H2- found that several of them possess unusually high carbon atom coordination numbers. These cluster compositions have potential as the basis for new energetic materials.

  3. Degradation of glycine and alanine on irradiated quartz.

    Science.gov (United States)

    Pawlikowski, Maciej; Benko, Aleksandra; Wróbel, Tomasz P

    2013-04-01

    Recent researches suggest participation of minerals in the formation of life under primordial conditions. Among all of the minerals, quartz seems to be one of the most probable to take part in such processes. However, an external source of energy is needed, e.g. electric discharge. A device simulating the proposed conditions was designed and was used to simulate prebiotic conditions. Investigation of processes occurring during the stimulation of quartz with electric discharge was studied by means of Ultraviolet-visible (UV-VIS) spectroscopy, in order to monitor the generation kinetics of free radicals. Additionally, infrared spectroscopy was applied to identify chemical reaction products created in a solution of alanine or glycine, in the presence of quartz treated with electric discharge. Formation of increased amounts of free radicals, compared to experiments performed without quartz and/or amino acid, is reported, along with identification of possible degradation products of alanine. No synthetic reactions were observed.

  4. 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

  5. In Situ Adsorption Studies at the Solid/Liquid Interface:Characterization of Biological Surfaces and Interfaces Using SumFrequency Generation Vibrational Spectroscopy, Atomic Force Microscopy,and Quartz Crystal Microbalance

    Energy Technology Data Exchange (ETDEWEB)

    Phillips, Diana Christine [Univ. of California, Berkeley, CA (United States)

    2006-01-01

    Sum frequency generation (SFG) vibrational spectroscopy, atomic force microscopy (AFM), and quartz crystal microbalance (QCM) have been used to study the molecular surface structure, surface topography and mechanical properties, and quantitative adsorbed amount of biological molecules at the solid-liquid interface. The molecular-level behavior of designed peptides adsorbed on hydrophobic polystyrene and hydrophilic silica substrates has been examined as a model of protein adsorption on polymeric biomaterial surfaces. Proteins are such large and complex molecules that it is difficult to identify the features in their structure that lead to adsorption and interaction with solid surfaces. Designed peptides which possess secondary structure provide simple model systems for understanding protein adsorption. Depending on the amino acid sequence of a peptide, different secondary structures (α-helix and β-sheet) can be induced at apolar (air/liquid or air/solid) interfaces. Having a well-defined secondary structure allows experiments to be carried out under controlled conditions, where it is possible to investigate the affects of peptide amino acid sequence and chain length, concentration, buffering effects, etc. on adsorbed peptide structure. The experiments presented in this dissertation demonstrate that SFG vibrational spectroscopy can be used to directly probe the interaction of adsorbing biomolecules with a surface or interface. The use of well designed model systems aided in isolation of the SFG signal of the adsorbing species, and showed that surface functional groups of the substrate are sensitive to surface adsorbates. The complementary techniques of AFM and QCM allowed for deconvolution of the effects of surface topography and coverage from the observed SFG spectra. Initial studies of biologically relevant surfaces are also presented: SFG spectroscopy was used to study the surface composition of common soil bacteria for use in bioremediation of nuclear waste.

  6. Metal Hydrides for Rechargeable Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Valoeen, Lars Ole

    2000-03-01

    Rechargeable battery systems are paramount in the power supply of modern electronic and electromechanical equipment. For the time being, the most promising secondary battery systems for the future are the lithium-ion and the nickel metal hydride (NiMH) batteries. In this thesis, metal hydrides and their properties are described with the aim of characterizing and improving those. The thesis has a special focus on the AB{sub 5} type hydrogen storage alloys, where A is a rare earth metal like lanthanum, or more commonly misch metal, which is a mixture of rare earth metals, mainly lanthanum, cerium, neodymium and praseodymium. B is a transition metal, mainly nickel, commonly with additions of aluminium, cobalt, and manganese. The misch metal composition was found to be very important for the geometry of the unit cell in AB{sub 5} type alloys, and consequently the equilibrium pressure of hydrogen in these types of alloys. The A site substitution of lanthanum by misch metal did not decrease the surface catalytic properties of AB{sub 5} type alloys. B-site substitution of nickel with other transition elements, however, substantially reduced the catalytic activity of the alloy. If the internal pressure within the electrochemical test cell was increased using inert argon gas, a considerable increase in the high rate charge/discharge performance of LaNi{sub 5} was observed. An increased internal pressure would enable the utilisation of alloys with a high hydrogen equivalent pressure in batteries. Such alloys often have favourable kinetics and high hydrogen diffusion rates and thus have a potential for improving the high current discharge rates in metal hydride batteries. The kinetic properties of metal hydride electrodes were found to improve throughout their lifetime. The activation properties were found highly dependent on the charge/discharge current. Fewer charge/discharge cycles were needed to activate the electrodes if a small current was used instead of a higher

  7. Metal Hydrides for Rechargeable Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Valoeen, Lars Ole

    2000-03-01

    Rechargeable battery systems are paramount in the power supply of modern electronic and electromechanical equipment. For the time being, the most promising secondary battery systems for the future are the lithium-ion and the nickel metal hydride (NiMH) batteries. In this thesis, metal hydrides and their properties are described with the aim of characterizing and improving those. The thesis has a special focus on the AB{sub 5} type hydrogen storage alloys, where A is a rare earth metal like lanthanum, or more commonly misch metal, which is a mixture of rare earth metals, mainly lanthanum, cerium, neodymium and praseodymium. B is a transition metal, mainly nickel, commonly with additions of aluminium, cobalt, and manganese. The misch metal composition was found to be very important for the geometry of the unit cell in AB{sub 5} type alloys, and consequently the equilibrium pressure of hydrogen in these types of alloys. The A site substitution of lanthanum by misch metal did not decrease the surface catalytic properties of AB{sub 5} type alloys. B-site substitution of nickel with other transition elements, however, substantially reduced the catalytic activity of the alloy. If the internal pressure within the electrochemical test cell was increased using inert argon gas, a considerable increase in the high rate charge/discharge performance of LaNi{sub 5} was observed. An increased internal pressure would enable the utilisation of alloys with a high hydrogen equivalent pressure in batteries. Such alloys often have favourable kinetics and high hydrogen diffusion rates and thus have a potential for improving the high current discharge rates in metal hydride batteries. The kinetic properties of metal hydride electrodes were found to improve throughout their lifetime. The activation properties were found highly dependent on the charge/discharge current. Fewer charge/discharge cycles were needed to activate the electrodes if a small current was used instead of a higher

  8. Kinetics of hydride front in Zircaloy-2 and H release from a fractional hydrided surface

    Energy Technology Data Exchange (ETDEWEB)

    Diaz, M.; Gonzalez-Gonzalez, A.; Moya, J. S.; Remartinez, B.; Perez, S.; Sacedon, J. L. [Instituto de Ciencia de Materiales de Madrid (CSIC), Sor Juana Ines de la Cruz 3, Cantoblanco, 28049 Madrid (Spain); Iberdrola, Tomas Redondo 3, 28033 Madrid (Spain); Instituto de Ciencia de Materiales de Madrid (CSIC), Sor Juana Ines de la Cruz 3, Cantoblanco, 28049 Madrid (Spain)

    2009-07-15

    The authors study the hydriding process on commercial nuclear fuel claddings from their inner surface using an ultrahigh vacuum method. The method allows determining the incubation and failure times of the fuel claddings, as well as the dissipated energy and the partial pressure of the desorbed H{sub 2} from the outer surface of fuel claddings during the hydriding process. The correlation between the hydriding dissipated energy and the amount of zirconium hydride (formed at different stages of the hydriding process) leads to a near t{sup 1/2} potential law corresponding to the time scaling of the reaction for the majority of the tested samples. The calibrated relation between energy and hydride thickness allows one to calculate the enthalpy of the {delta}-ZrH{sub 1.5} phase. The measured H{sub 2} desorption from the external surface is in agreement with a proposed kinetic desorption model from the hydrides precipitated at the surface.

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

    KAUST Repository

    Mazoyer, Etienne

    2011-12-02

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

  10. Carbon in intimate contact with quartz reduces the biological activity of crystalline silica dusts.

    Science.gov (United States)

    Ghiazza, Mara; Tomatis, Maura; Doublier, Sophie; Grendene, Francesca; Gazzano, Elena; Ghigo, Dario; Fubini, Bice

    2013-01-18

    To evaluate the effect of carbonaceous materials on the pathogenic activity of quartz dusts, mixtures of carbon soot (1 and 10%) and quartz (Min-U-Sil) were prepared and then milled so to attain an intimate association of carbon and the quartz surface. Both cellular and cell-free tests show that carbon associated to quartz completely inhibits the typical free radical generation of quartz dusts (through Fenton activity and homolytic cleavage of a C-H bond) and suppresses the oxidative stress and inflammation induced by quartz alone on MH-S murine macrophage cells (lipid peroxidation, nitric oxide release, and tumor necrosis factor-α synthesis). The cytotoxic response to quartz is also largely reduced. An extremely pure quartz milled with 10% of soot showed inactivating effects on the adverse reactions to quartz similar to Min-U-Sil quartz. None of these effects takes place when the same experiments are carried out with mechanically mixed samples, which suggests that carbon acts not just as a radical quencher but because of its association to the quartz surface.

  11. 氢化物原子荧光光谱法同时测定生活饮用水中砷和硒%Simulatneous Determination of Arsenic and selenium in Drinking Water Samples by Hydride Generation Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    张祥楼

    2014-01-01

    建立了氢化物发生原子荧光光谱法同时测定生活饮用水中砷和硒的方法.测试结果表明砷和硒在质量浓度分别为0.00μg/L~10.00μg/L和0.00μg/L~40.00μg/L范围内呈线性关系,相关系数分别为(砷r=0.9998,硒r=0.9997)。仪器检出限为砷:0.03μg/L硒:0.05μg/L。本方法检出限砷为0.075μg/L;硒为0.125μg/L。水质样品中砷的回收率为92.6%~96.5%,精密度为0.8%~1.4%;硒的回收率为91.2%~97.4%,精密度为1.0%~1.6%。应用本方法测定生活饮用水中的砷和硒方法简便、快速,结果准确可靠,较好地提高了工作效率。%A method for simulatneous determination of Arsenic and selenium in drinking water samples by hydride generation atomic fluorescence spectrometry.As a matter of fact ,the linear range of Arsenic was 0.00μg/L~10.00μg/L and the related coefficient was 0.9998;While the linear range of Selenium was 0.00μg/L~40.00μg/L and the related coefficient was0.9997. Instrument detection limit was 0.03μg/L(arsenic)and 0.05μg/L(selenium).Detection limits of the method was 0.075μg/L (arsenic)and 0.125μg/L(selenium). The rate of arsenic recovery was 92.6%~96.5%and the precision in the drinking water was in the range of 0.8%~1.4%.while the rate of selenium recovery was 92.6%~96.5%and the precision in the drinking water was in the range of 1.0%~1.6%.The experimental results shows that the method is applicable .

  12. Determination of Tetraethyl Lead in Water by Hydride Generation-Atomic Absorption Spectrophotometry%水中四乙基铅的氢化原子吸收测定法

    Institute of Scientific and Technical Information of China (English)

    公丕峰

    2011-01-01

    Objective To establish a method for the determination of tetraethyl lead in water by hydride generation-atomic absorption spectrophotometry. Methods By solvent extraction of trichloromethane and low-temperature degradation,the best optimum experimental condition of optimal design of orthogonal test: wavelength was 217 nm, lamp current was 3.0 mA, band pass was 0.2 nm, supporting gas was argon GAS (99.99%), argon gas flux was 0.8 L/min, peak height measurement, oxidizing flame, 20 g/L NaBH4 solution,5 ml HNO3 (1.42 g/ml) solution, 1.5 ml HCl(1.19 g/ml) solution, 100 g/L K3Fe(CN)6 solution. Results The limit of detection was 0.049 μg/L,the average recovery rates were 89.7%-101.4% and RSDs were 3.3%-5.3%. Conclusion This method is simple, sensitive, accurate and applicable to the determination of the tetraethyl lead in water.%目的 建立水中四乙基铅的氢化原子吸收测定方法.方法 样品经三氯甲烷萃取,低温消解后,采用氢化原子吸收法进行分析.经正交设计优化后的试验条件:波长为217.0 nm,灯电流为3.0 mA,光谱通带为0.2 nm;载气为99.99%氩气,载气流量为0.8 L/min,测量方式为峰高,氧化性蓝色焰,NaBH4溶液浓度为20g/L,1.42g/ml硝酸用量为5 ml,1.19g/ml盐酸用量为1.5 ml,K3Fe(CN)6溶液浓度为100g/L.结果 在0.049~100μg/L线性范围内,所得四乙基铅的标准曲线回归方程为γ=1.07×10-34+3.49×10-3x,相关系数为0.999 6.该方法的检出限为0.049 μg/L,平均回收率为89.7%~101.4%,RSD为3.3%~53%.结论该方法操作方便,所用试验装置价格低廉,灵敏度和准确度均较高,适合各级单位用于水中四乙基铅的测定.

  13. 氢化物发生原子荧光光谱法测量化妆品中Sb的价态%Valent speciation analysis of antimony in cosmetics by hydride generation atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    肖融; 张新智; 王昌钊; 冯礼; 秦德元; 刘霁欣

    2012-01-01

    考察了NaF、8-羟基喹啉、柠檬酸对Sb(Ⅲ)和Sb(V)原子荧光信号的掩蔽作用和还原解柠檬酸除掩蔽作用的方法.结果表明,0.10mol/L柠檬酸对Sb(V)掩蔽作用最强,且对Sb(Ⅲ)有增敏作用,最适于作为Sb价态测量的掩蔽剂,而10g/L碘化钾(KI)+ 10g/L硫脲(Tu)可在5h内完全解除柠檬酸对Sb(V)的掩蔽作用.据此建立了化妆品中Sb价态的非色谱氢化物发生原子荧光测量方法.样品经0.10mol/L柠檬酸提取两次后,离心去上清液,合并定容,得到提取液;提取液酸化后直接测得Sb(Ⅲ)含量;提取液酸化并加入KI+Tu,放置5h以上后可测得Sb(V)与Sb(Ⅲ)的含量和,此值减去Sb(Ⅲ)含量可得Sb(V)含量.计算表明,该方法对Sb(Ⅲ)和Sb(V)的检出限(3σ)均为0.32μg/L,定量限(3σ)均为1.0μg/L.对实际化妆品作了测量,Sb(Ⅲ)和Sb(V)的加标回收率在70%~130%之间.实验中存在少量Sb(Ⅲ)到Sb(V)的转化.%The masking effects of NaF, 8-hydroxygquinoline and citric acid on the atomic fluorescence signals of Sb(Ⅲ ) and Sb( V ) And the method for eliminating the masking effect of citric acid were investigated. The results show that 0. 10 mol/L citric acid has the strongest masking effect on Sb(V) and can increase the sensitivity of Sb(Ⅲ) , and l0g/L KI+l0g/L thiourea can completely eliminate the masking effect of citric acid in >5h. Based on this, a method for analyzing the valent speciation of Sb in cosmetics by hydride generation atomic fluorescence spectrometry (HGAFS) was developed. The samples were extracted twice with 0. L0ml/L citric acid. The supernatant was removed by centrifugation and the residues were merged asextract solution. After the acidification of the extract solution, the Sb(Ⅲ) content was determined directly. Then the extract solution was added with KI (10g/L)+ thiourea (l0g/L) and set aside for >5h before the total content of Sb(V) and Sb(Ⅲ) was determined. The Sb( V) content was obtained by subtracting Sb

  14. Ionic conduction of lithium hydride single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Pilipenko, G.I.; Oparin, D.V.; Zhuravlev, N.A.; Gavrilov, F.F.

    1987-09-01

    Using the electrical-conductivity- and NMR-measurement- methods, the ionic-conduction mechanism is established in stoichiometric lithium hydride single crystals. The activation energies of migration of anion- and cation-vacancies and the formation of Schottky-pair defects are determined. They assume that the mechanisms of self-diffusion and conductivity are different in lithium hydride.

  15. Performance study of a hydrogen powered metal hydride actuator

    Science.gov (United States)

    Mainul Hossain Bhuiya, Md; Kim, Kwang J.

    2016-04-01

    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 LaNi5 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.

  16. Submillimeter Spectroscopy of Hydride Molecules

    Science.gov (United States)

    Phillips, T. G.

    1998-05-01

    Simple hydride molecules are of great importance in astrophysics and astrochemistry. Physically they dominate the cooling of dense, warm phases of the ISM, such as the cores and disks of YSOs. Chemically they are often stable end points of chemical reactions, or may represent important intermediate stages of the reaction chains, which can be used to test the validity of the process. Through the efforts of astronomers, physicists, chemists, and laboratory spectroscopists we have an approximate knowledge of the abundance of some of the important species, but a great deal of new effort will be required to achieve the comprehensive and accurate data set needed to determine the energy balance and firmly establish the chemical pathways. Due to the low moment of inertia, the hydrides rotate rapidly and so have their fundamental spectral lines in the submillimeter. Depending on the cloud geometry and temperature profile they may be observed in emission or absorption. Species such as HCl, HF, OH, CH, CH(+) , NH_2, NH_3, H_2O, H_2S, H_3O(+) and even H_3(+) have been detected, but this is just a fraction of the available set. Also, most deduced abundances are not nearly sufficiently well known to draw definitive conclusions about the chemical processes. For example, the most important coolant for many regions, H_2O, has a possible range of deduced abundance of a factor of 1000. The very low submillimeter opacity at the South Pole site will be a significant factor in providing a new capabilty for interstellar hydride spectroscopy. The new species and lines made available in this way will be discussed.

  17. Kinetic equation for the reaction of titanium tetrachloride with hydride functional groups of diamond

    Energy Technology Data Exchange (ETDEWEB)

    Zhidkov, A.B.; Smirnov, E.P.

    1989-02-01

    This work is devoted to the study of the kinetics of the reaction of titanium tetrachloride with the hydride functional groups of diamond. The research was performed on submicron powders of ASM 0.7/0.3 grade synthetic diamond with a specific surface area of 8.0 m/sup 2//g as measured from the adsorption of nitrogen. The reaction was carried out in a flow-through quartz reactor in a flow of dry He. The content of the titanium in the samples was determined by a photocolorimetric method. A kinetic equation for the reaction of diamond with titanium tetrachloride was found on the basis of a statistical approach.

  18. New multiphase equation of state for polycrystalline quartz

    Energy Technology Data Exchange (ETDEWEB)

    Boettger, J.C.; Lyon, S.P.

    1990-10-01

    We have generated separate equations of state (EOS's) for the alpha quartz, coesite, and stishovite phases of polycrystalline quartz (SiO{sub 2}) using the computer program GRIZZLY. We also modified the program GRIZZLY to combine two single-phase EOS's for a given material into a single two-phase EOS via minimization of the Gibbs free energy. This new version of GRIZZLY has been used to generate a three-phase SESAME type EOS for polycrystalline quartz using the three EOS's mentioned above. All four of the EOS's produced for SiO{sub 2} are now available on request. 17 refs., 4 figs., 1 tab.

  19. Electromodulated absorption in smoky quartz

    NARCIS (Netherlands)

    Brom, W.E. van den; Volger, J.

    1974-01-01

    The optical absorption coefficient of “smoky” quartz (containing aluminium) can be modulated by applying an electric field. The effect saturates at high fields and low temperatures and reaches a maximum at 535 nm. The results are discussed in terms of a model consisting of a colour centre, dipolar i

  20. Laser welding of fused quartz

    Science.gov (United States)

    Piltch, Martin S.; Carpenter, Robert W.; Archer, III, McIlwaine

    2003-06-10

    Refractory materials, such as fused quartz plates and rods are welded using a heat source, such as a high power continuous wave carbon dioxide laser. The radiation is optimized through a process of varying the power, the focus, and the feed rates of the laser such that full penetration welds may be accomplished. The process of optimization varies the characteristic wavelengths of the laser until the radiation is almost completely absorbed by the refractory material, thereby leading to a very rapid heating of the material to the melting point. This optimization naturally occurs when a carbon dioxide laser is used to weld quartz. As such this method of quartz welding creates a minimum sized heat-affected zone. Furthermore, the welding apparatus and process requires a ventilation system to carry away the silicon oxides that are produced during the welding process to avoid the deposition of the silicon oxides on the surface of the quartz plates or the contamination of the welds with the silicon oxides.

  1. 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.

  2. Electrochemical process and production of novel complex hydrides

    Science.gov (United States)

    Zidan, Ragaiy

    2013-06-25

    A process of using an electrochemical cell to generate aluminum hydride (AlH.sub.3) is provided. The electrolytic cell uses a polar solvent to solubilize NaAlH.sub.4. The resulting electrochemical process results in the formation of AlH.sub.3. The AlH.sub.3 can be recovered and used as a source of hydrogen for the automotive industry. The resulting spent aluminum can be regenerated into NaAlH.sub.4 as part of a closed loop process of AlH.sub.3 generation.

  3. 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.

  4. On the Arsenic Amount Determination in Tungsten Concentrate by Optimal Design of Uniform-hydride Generation Atomic Absorption Spectrometry%均匀优化设计-氢化物发生原子吸收光谱法测定钨精矿中砷量

    Institute of Scientific and Technical Information of China (English)

    陈涛; 潘建忠

    2011-01-01

    A technology based on uniform design is proposed in the optimization of arsenic amount determination in tungsten concentrate by hydride generation atomic Absorption Spectrometry. The optimized analysis condition is obtained by means of experiments: the sample is decomposed by sulfuric acid-ammonium sulfate, coordinated with tungsten, iron, manganese in ammonia medium using citric acid, then reduced pentavalent arsenic to trivalent arsenic by ascorbic acid. Arsenic amount at the degree of 15 % acid solution is measured by the united equipments:flow injection-hydride generator-atomic absorption spectrophotometer. This technology has many advantages, such as high sensitivity, good accuracy, fast and simple, little elements interfering. The detection limit of arsenic amount can be 0.001%.%该方法应用均匀设计这一优化试验设计理论,采用氢化物发生原子吸收光谱法测定钨精矿中砷量.经实验确定了测定砷量的最佳分析条件:经硫酸-硫酸铵分解,用柠檬酸在氨性介质中络合钨、铁、锰等干扰元素,用抗坏血酸预还原五价的砷到三价.样品溶液在15%的酸度中,经流动注射-氢化物发生与原子吸收光谱仪联用测定砷量.该方法具有灵敏度高,准确性好,快速简便,干扰元素少等优点.

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

    OpenAIRE

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

    2015-01-01

    A detailed optimization of relevant experimental parameters of two hydride atomizers for atomic fluorescence spectrometry: flame-in-gas-shield atomizer with a two-channel shielding unit and a standard atomizer for atomic fluorescence spectrometry, miniature diffusion flame, was performed. Arsine, generated by the reaction with NaBH4 in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were ...

  6. Shock metamorphism of deformed quartz

    Science.gov (United States)

    Gratz, Andrew J.; Christie, John; Tyburczy, James; Ahrens, Thomas; Pongratz, Peter

    1988-01-01

    The effect produced by shock loading (to peak pressures of 12 and 24) on deformed synthetic quartz containing a dislocation and abundant bubbles and small inclusions was investigated, and the relationships between preexisting dislocation density shock lamellae in the target material were examined. The resultant material was found to be inhomogeneously deformed and extremely fractured. Results of TEM examinations indicate that no change in dislocation density was caused by shock loading except in regions containing shock lamellae, where the dislocation density was lowered. The shock-induced defects tend to nucleate on and be controlled by preexisting stress concentrators; shock lamellae, glassy veins, and most curviplanar defects form in tension, presumably during release. An extremely mobile silica fluid is formed and injected into fractures during release, which forcibly removes crystalline fragments from vein walls. It is concluded that shock deformation in quartz is dominated by fracture and melting.

  7. Hydrogen storage in complex metal hydrides

    National Research Council Canada - National Science Library

    Bogdanovic, Borislav; Felderhoff, Michael; Streukens, Guido

    2009-01-01

    ...) are solid-state hydrogen-storage materials with high hydrogen capacities. They can be used in combination with fuel cells as a hydrogen source thus enabling longer operation times compared with classical metal hydrides...

  8. Method of forming metal hydride films

    Science.gov (United States)

    Steinberg, R.; Alger, D. L.; Cooper, D. W. (Inventor)

    1977-01-01

    The substrate to be coated (which may be of metal, glass or the like) is cleaned, both chemically and by off-sputtering in a vacuum chamber. In an ultra-high vacuum system, vapor deposition by a sublimator or vaporizer coats a cooled shroud disposed around the substrate with a thin film of hydride forming metal which getters any contaminant gas molecules. A shutter is then opened to allow hydride forming metal to be deposited as a film or coating on the substrate. After the hydride forming metal coating is formed, deuterium or other hydrogen isotopes are bled into the vacuum system and diffused into the metal film or coating to form a hydride of metal film. Higher substrate temperatures and pressures may be used if various parameters are appropriately adjusted.

  9. Sealed aerospace metal-hydride batteries

    Science.gov (United States)

    Coates, Dwaine

    1992-01-01

    Nickel metal hydride and silver metal hydride batteries are being developed for aerospace applications. There is a growing market for smaller, lower cost satellites which require higher energy density power sources than aerospace nickel-cadmium at a lower cost than space nickel-hydrogen. These include small LEO satellites, tactical military satellites and satellite constellation programs such as Iridium and Brilliant Pebbles. Small satellites typically do not have the spacecraft volume or the budget required for nickel-hydrogen batteries. NiCd's do not have adequate energy density as well as other problems such as overcharge capability and memory effort. Metal hydride batteries provide the ideal solution for these applications. Metal hydride batteries offer a number of advantages over other aerospace battery systems.

  10. Luminescence sensitivity changes in quartz

    CERN Document Server

    Wintle, A G

    1999-01-01

    In the luminescence dating of sedimentary or heated quartz, some heat treatment is usually applied to the sample immediately prior to the measurement of the optically stimulated luminescence. In this paper we report experiments on a 30,000-year-old sedimentary quartz, in which we use the luminescence response to a test dose to monitor the changes in sensitivity that are caused by holding the quartz at temperatures from 160 to 280 deg. C for times from 10 s to 22 h. For an optically bleached sample, the monitoring is by both optically stimulated luminescence and the 110 deg. C TL peak; both luminescence signals are shown to have the same sensitisation (i.e. activation energy) characteristics. For natural or laboratory irradiated samples only the 110 deg. C TL peak can be used; sensitivity increases of up to a factor of 1.3 and 3 are observed for the natural and laboratory irradiated aliquots, respectively. Up to four exponential components are used to deconvolve the sensitivity change data; the dominant compon...

  11. Destabilization of magnesium hydride through interface engineering

    OpenAIRE

    Mooij, L.P.A.

    2013-01-01

    The aim of this thesis is to study the thermodynamics of hydrogenation of nanoconfined magnesium within a thin film multilayer model system. Magnesium hydride is a potential material for hydrogen storage, which is a key component in a renewable energy system based on hydrogen. In bulk form, magnesium hydride is very stable, which means that hydrogen is released only at elevated temperature. Furthermore, the kinetics of hydrogen sorption is slow, which further hampers the practical use of this...

  12. Water weakening in experimentally deformed milky quartz single crystals

    Science.gov (United States)

    Stunitz, H.; Thust, A.; Kilian, R.; Heilbronner, R.; Behrens, H.; Tarantola, A.; Fitz Gerald, J. D.

    2015-12-01

    Natural single crystals of quartz have been experimentally deformed in two orientations: (1) normal to one prism-plane, (2) In O+ orientation at temperatures of 900 and 1000°C, pressures of 1.0 and 1.5 GPa, and strain rates of ~1 x 10-6s-1. The starting material is milky quartz, consisting of dry quartz (H2O contents of recycling of H2O between FI´s, dislocation generation at very small fluid inclusions, incorporation of structurally bound H into dislocation cores, and release of H2O from dislocations back into FI´s during recovery. Cracking and crack healing play an important role in the recycling process and imply a close interrelationship between brittle and crystal plastic deformation. The H2O weakening by this process is of a disequilibrium nature and thus depends on the amount of H2O available.

  13. Transition-Metal Hydride Radical Cations.

    Science.gov (United States)

    Hu, Yue; Shaw, Anthony P; Estes, Deven P; Norton, Jack R

    2016-08-10

    Transition-metal hydride radical cations (TMHRCs) are involved in a variety of chemical and biochemical reactions, making a more thorough understanding of their properties essential for explaining observed reactivity and for the eventual development of new applications. Generally, these species may be treated as the ones formed by one-electron oxidation of diamagnetic analogues that are neutral or cationic. Despite the importance of TMHRCs, the generally sensitive nature of these complexes has hindered their development. However, over the last four decades, many more TMHRCs have been synthesized, characterized, isolated, or hypothesized as reaction intermediates. This comprehensive review focuses on experimental studies of TMHRCs reported through the year 2014, with an emphasis on isolated and observed species. The methods used for the generation or synthesis of TMHRCs are surveyed, followed by a discussion about the stability of these complexes. The fundamental properties of TMHRCs, especially those pertaining to the M-H bond, are described, followed by a detailed treatment of decomposition pathways. Finally, reactions involving TMHRCs as intermediates are described.

  14. 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.

  15. 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.

  16. 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...

  17. Cooldown-induced hydride reorientation of hydrogen-charged zirconium alloy cladding tubes

    Science.gov (United States)

    Won, Ju-Jin; Min, Su-Jeong; Kim, Kyu-Tae

    2015-01-01

    Radial hydride precipitation behaviors of Zr-Nb alloy cladding tubes were investigated using 250 and 500 ppm hydrogen-charged Zr-Nb alloy cladding tubes, cooldown processes from 400 to 300, 200°C and room temperature with five kinds of cooling rates of 0.3, 2.0, 4.0, 7.0 15.0 °C/min under a tensile hoop stress of 150 MPa, which can simulate various cooldown processes during an interim dry storage of PWR nuclear fuel. The slower cooling rate and the lower terminal cooldown temperature generated the more hydrides precipitated during the cooldown as well as the larger fraction and the longer length of radial hydrides. These phenomena can be explained by the difference in the terminal solid solubility of hydrogen for dissolution and precipitation occurring during the heatup and cooldown processes and the cooling rate-dependent hydride nucleation and growth rates. In addition, a drastic decrease in ultimate tensile strength and plastic strain of the tensile tested specimens experiencing the cool-down processes appear to be correlated with the amount of the radial hydrides precipitated during the cooldown.

  18. Changes in Quartz During Heating and the Possible Effects on Si Production

    Science.gov (United States)

    Ringdalen, Eli

    2015-02-01

    In Si and FeSi production, the main Si source is SiO2, in the form of quartz. Reactions with SiO2 generate SiO gas that further reacts with SiC to Si. During heating, quartz will transform to other SiO2 modifications with cristobalite as the stable high-temperature phase. Transformation to cristobalite is a slow process. Its rate has been investigated for several industrial quartz sources and has been shown to vary considerably among the different quartz types. Other differences in behavior during heating between these quartz sources, such as softening temperature and volume expansion, have also been studied. The quartz-cristobalite ratio will affect the rate of reactions involving SiO2. The industrial consequences and other implications of the observed difference between quartz types are discussed. Initial studies of industrial quartz were published by Ringdalen et al. In the current work, a new experimental method has been developed, and an investigation of several new quartz sources has confirmed the earlier observed large variation between different sources. The repeatability of the data has been studied and the effect of gas atmosphere investigated. The results from the earlier work are included as a basis for the discussion.

  19. 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...

  20. The oxidation of uranium hydride during its instantaneous or gradual exposure to oxygen

    Energy Technology Data Exchange (ETDEWEB)

    Glascott, J., E-mail: joe.glascott@awe.co.uk; Findlay, I.M.

    2015-11-15

    The oxidation behaviour of uranium hydride when exposed to oxygen gas either gradually or instantaneously at an ambient temperature of approximately 37 °C has been investigated. The proportion of the sample converted to oxide and the mean hydride mound temperature rise accompanying the oxidation process were recorded. Pressure changes in the reaction cell were used to deduce the nature of the oxide generated during the oxidation process and the nature of the gaseous reaction products. For the gradual oxidation of the hydride, typically only about 15% of the hydride mass was converted to oxide during the initial period of oxidation defined by an observed temperature excursion lasting a finite time; during this oxidation period it is concluded that, despite the only moderate recoded mean temperature rises, the generated oxide is U{sub 3}O{sub 8} rather than UO{sub 2}. Typically also for such gradual exposure experiments, hydrogen was the principal gaseous reaction product with negligible water being produced. For the instantaneous exposure of the hydride to oxygen, much higher hydride mound mean temperature rises were recorded but the proportion of hydride converted to oxide was quite variable and apparently dependent on several experimental variables; for these experiments, although hydrogen was a major reaction product typically some water was also produced. The boundary between pyrophoric and non-pyrophoric oxidation of uranium hydride for given oxidising conditions is discussed in terms of a calculated particle “thermal runaway temperature”. - Highlights: • Only about 15% of UH{sub 3} is oxidised on its gradual exposure to oxygen. • During the gradual exposure of UH{sub 3} to oxygen U{sub 3}O{sub 8} rather than UO{sub 2} is generated. • For such gradual exposure, predominantly H{sub 2} rather than H{sub 2}O was generated. • For the instantaneous exposure of UH{sub 3} to O{sub 2} the amount oxidised was variable. • For these experiments, H{sub 2

  1. HEAT-UP AND COOL-DOWN TEMPERATURE-DEPENDENT HYDRIDE REORIENTATION BEHAVIORS IN ZIRCONIUM ALLOY CLADDING TUBES

    Directory of Open Access Journals (Sweden)

    JU-JIN WON

    2014-10-01

    Full Text Available Hydride reorientation behaviors of PWR cladding tubes under typical interim dry storage conditions were investigated with the use of as-received 250 and 485ppm hydrogen-charged Zr-Nb alloy cladding tubes. In order to evaluate the effect of typical cool-down processes on the radial hydride precipitation, two terminal heat-up temperatures of 300 and 400°C, as well as two terminal cool-down temperatures of 200 and 300°C, were considered. In addition, two cooling rates of 2.5 and 8.0°C/min during the cool-down processes were taken into account along with zero stress or a tensile hoop stress of 150MPa. It was found that the 250ppm hydrogen-charged specimen experiencing the higher terminal heat-up temperature and the lower terminal cool-down temperature generated the highest number of radial hydrides during the cool-down process under 150MPa hoop tensile stress, which may be explained by terminal solid hydrogen solubilities for precipitation, and dissolution and remaining circumferential hydrides at the terminal heat-up temperatures. In addition, the slower cool-down rate generates the larger number of radial hydrides due to a cooling rate-dependent, longer residence time at a relatively high temperature that can accelerate the radial hydride nucleation and growth.

  2. Preliminary development of flaw evaluation procedures for delayed hydride cracking initiation under hydride non-ratcheting conditions

    Energy Technology Data Exchange (ETDEWEB)

    Xu, S.; Cui, J.; Kawa, D.; Shek, G.K.; Scarth, D.A. [Kinectrics Inc., Toronto, Ontario (Canada)

    2006-07-01

    The flaw evaluation procedure for Delayed Hydride Cracking (DHC) initiation currently provided in the CSA Standard N285.8 was developed for hydride ratcheting conditions, in which flaw-tip hydrides do not completely dissolve at peak temperature. Test results have shown that hydrided regions formed under non-ratcheting conditions, in which flaw-tip hydrides completely dissolve at peak temperature, have significantly higher resistance to cracking than those formed under ratcheting conditions. This paper presents some preliminary work on the development of a procedure for the evaluation of DHC initiation for flaws under hydride non-ratcheting conditions. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Gorman, R.; Moritz, P.

    1978-05-01

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

  4. Aluminum-titanium hydride-boron carbide composite provides lightweight neutron shield material

    Science.gov (United States)

    Poindexter, A. M.

    1967-01-01

    Inexpensive lightweight neutron shield material has high strength and ductility and withstands high internal heat generation rates without excessive thermal stress. This composite material combines structural and thermal properties of aluminum, neutron moderating properties of titanium hydride, and neutron absorbing characteristics of boron carbide.

  5. 氯化盐溶液中氢化燃烧合成MgH2的水解制氢性能%Hydrogen generation properties from hydrolysis of magnesium hydride in chloride salt solution

    Institute of Scientific and Technical Information of China (English)

    刘虎; 赵泽伦; 李姝; 朱云峰; 李李泉

    2015-01-01

    利用氢化燃烧合成(Hydriding Combustion Synthesis,HCS)制备的镁基氢化物(MgH2)与氯化盐溶液反应制取氢气.分别比较了NiCl2、MgCl2、CuCl2及CaCl2溶液中HCS MgH2的水解制氢量和转化率,着重研究了MgCl2溶液的浓度、温度及球磨预处理时间对HCS MgH2水解制氢性能的影响规律.研究表明:60 min球磨预处理的HCS MgH2,在30℃的0.5 mol/L MgCl2溶液中,反应30 min制氢量可达1 635 ml/g,转化率可达96%.

  6. Thin-film metal hydrides.

    Science.gov (United States)

    Remhof, Arndt; Borgschulte, Andreas

    2008-12-01

    The goal of the medieval alchemist, the chemical transformation of common metals into nobel metals, will forever be a dream. However, key characteristics of metals, such as their electronic band structure and, consequently, their electric, magnetic and optical properties, can be tailored by controlled hydrogen doping. Due to their morphology and well-defined geometry with flat, coplanar surfaces/interfaces, novel phenomena may be observed in thin films. Prominent examples are the eye-catching hydrogen switchable mirror effect, the visualization of solid-state diffusion and the formation of complex surface morphologies. Thin films do not suffer as much from embrittlement and/or decrepitation as bulk materials, allowing the study of cyclic absorption and desorption. Therefore, thin-metal hydride films are used as model systems to study metal-insulator transitions, for high throughput combinatorial research or they may be used as indicator layers to study hydrogen diffusion. They can be found in technological applications as hydrogen sensors, in electrochromic and thermochromic devices. In this review, we discuss the effect of hydrogen loading of thin niobium and yttrium films as archetypical examples of a transition metal and a rare earth metal, respectively. Our focus thereby lies on the hydrogen induced changes of the electronic structure and the morphology of the thin films, their optical properties, the visualization and the control of hydrogen diffusion and on the study of surface phenomena and catalysis.

  7. 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.

  8. Lattice contraction in photochromic yttrium hydride

    Energy Technology Data Exchange (ETDEWEB)

    Maehlen, Jan Petter, E-mail: jepe@ife.no; Mongstad, Trygve T.; You, Chang Chuan; Karazhanov, Smagul

    2013-12-15

    Highlights: •Photochromic yttrium hydride films (YH:O) were prepared by reactive sputtering. •Black and transparent YH:O films were studied by time-resolved synchrotron XRD. •Both YH:O samples showed a lattice contraction upon illumination. •Also exposure to the X-ray beam itself results in a lattice contraction. -- Abstract: A strong photochromic effect was recently discovered in thin films of oxygen-containing yttrium hydride taking place at room temperature and reacting to ultraviolet and visible light. In this paper, we report on a lattice contraction upon illumination observed for thin-film samples of photochromic yttrium hydride, recorded by time-resolved X-ray diffraction using synchrotron radiation. The time dependence of the lattice contraction is consistent with the observed photochromic response of the samples.

  9. Atom probe analysis of titanium hydride precipitates.

    Science.gov (United States)

    Takahashi, J; Kawakami, K; Otsuka, H; Fujii, H

    2009-04-01

    It is expected that the three-dimensional atom probe (3DAP) will be used as a tool to visualize the atomic scale of hydrogen atoms in steel is expected, due to its high spatial resolution and very low detection limit. In this paper, the first 3DAP analysis of titanium hydride precipitates in metal titanium is reported in terms of the quantitative detection of hydrogen. FIB fabrication techniques using the lift-out method have enabled the production of needle tips of hydride precipitates, of several tens of microns in size, within a titanium matrix. The hydrogen concentration estimated from 3DAP analysis was slightly smaller than that of the hydride phase predicted from the phase diagram. We discuss the origin of the difference between the experimental and predicted values and the performance of 3DAP for the quantitative detection of hydrogen.

  10. Hydrogen storage in complex metal hydrides

    Directory of Open Access Journals (Sweden)

    BORISLAV BOGDANOVIĆ

    2009-02-01

    Full Text Available Complex metal hydrides such as sodium aluminohydride (NaAlH4 and sodium borohydride (NaBH4 are solid-state hydrogen-storage materials with high hydrogen capacities. They can be used in combination with fuel cells as a hydrogen source thus enabling longer operation times compared with classical metal hydrides. The most important point for a wide application of these materials is the reversibility under moderate technical conditions. At present, only NaAlH4 has favourable thermodynamic properties and can be employed as a thermally reversible means of hydrogen storage. By contrast, NaBH4 is a typical non- -reversible complex metal hydride; it reacts with water to produce hydrogen.

  11. Iron Group Hydrides in Noyori Bifunctional Catalysis.

    Science.gov (United States)

    Morris, Robert H

    2016-12-01

    This is an overview of the hydride-containing catalysts prepared in the Morris group for the efficient hydrogenation of simple ketones, imines, nitriles and esters and the asymmetric hydrogenation and transfer hydrogenation of prochiral ketones and imines. The work was inspired by and makes use of Noyori metal-ligand bifunctional concepts involving the hydride-ruthenium amine-hydrogen HRuNH design. It describes the synthesis and some catalytic properties of hydridochloro, dihydride and amide complexes of ruthenium and in one case, osmium, with monodentate, bidentate and tetradentate phosphorus and nitrogen donor ligands. The iron hydride that has been identified in a very effective asymmetric transfer hydrogenation process is also mentioned. The link between the HMNH structure and the sense of enantioinduction is demonstrated by use of simple transition state models.

  12. Quartz-like Crystals Found in Planetary Disks

    Science.gov (United States)

    2008-01-01

    NASA's Spitzer Space Telescope has, for the first time, detected tiny quartz-like crystals sprinkled in young planetary systems. The crystals, which are types of silica minerals called cristobalite and tridymite, can be seen close-up in the black-and-white insets (cristobalite is on the left, and tridymite on the right). The main picture is an artist's concept of a young star and its swirling disk of planet-forming materials. Cristobalite and tridymite are thought to be two of many planet ingredients. On Earth, they are normally found as tiny crystals in volcanic lava flows and meteorites from space. These minerals are both related to quartz. For example, if you were to heat the familiar quartz crystals often sold as mystical tokens, the quartz would transform into cristobalite and tridymite. Because cristobalite and tridymite require rapid heating and cooling to form, astronomers say they were most likely generated by shock waves traveling through the planetary disks. The insets are Scanning Electron Microscope pictures courtesy of George Rossman of the California Institute of Technology, Pasadena, Calif.

  13. Evidence of stress-induced hydrogen ordering in zirconium hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Steuwer, A. [FaME38 at the ESRF-ILL, 6 rue J Horowitz, 38042 Grenoble (France); ESS Scandinavia, University of Lund, Stora Algatan 4, 22350 Lund (Sweden)], E-mail: steuwer@ill.fr; Santisteban, J.R. [Centro Atomico Bariloche, CNEA, San Carlos de Bariloche (Argentina); Preuss, M. [University of Manchester, Grosvenor Street, Manchester M1 7HS (United Kingdom); Peel, M.J.; Buslaps, T. [European Synchrotron Radiation Facility, 6 rue J Horowitz, 38042 Grenoble (France); Harada, M. [R and D Section, Chofu-Kita Plant, Kobe Special Tube Co, Shimonoseki 752-0953 (Japan)

    2009-01-15

    The formation of hydrides in zirconium alloys significantly affects their mechanical properties and is considered to play a critical role in their failure mechanisms, yet relatively little is known about the micromechanical behavior of hydrides in the bulk. This paper presents the result of in situ uniaxial mechanical tensioning experiments on hydrided zircaloy-2 and zircaloy-4 specimens using energy-dispersive synchrotron X-ray diffraction, which suggests that a stress-induced transformation of the {delta}-hydride to {gamma}-hydride via ordering of the hydrogen atoms occurs, akin to a Snoek-type relaxation. Subsequent annealing was found to reverse the ordering phenomenon.

  14. Hydroxyl radicals induced by quartz particles in lung alveolar macrophages: the role of surface iron

    Institute of Scientific and Technical Information of China (English)

    LI Yi; ZHU Tong; GUO Xinbiao; SHANG Yu

    2006-01-01

    Previous studies have shown that hydroxyl radical generation is a key step in the mechanism of pathogenic process caused by airborne particles to the lung. However, there is no direct evidence for dose-response relationship between airborne particles and hydroxyl radical generation. In this study, hydroxyl radicals generated in lung alveolar macrophages exposed to quartz particles were measured using a highly sensitive capillary electrophoresis-fluorescence detection method. The results demonstrated that quartz particles induced the generation of hydroxyl radical in a dose-dependent manner, and the amount of the hydroxyl radicals was 10-10 mol/106 cells.The viability of alveolar macrophages exposed to quartz particles decreased with the increase of quartz concentration, showing a clear doseresponse relationship. Hydroxyl radical scavenger mannitol could increase the viability of quartz-treated cells, suggesting that hydroxyl radical contributed directly to cell death. In this study this contribution accounted for about 5%-20% of cell death. The hydroxyl radical generating potential was found to be related to surface iron content of the quartz particles.

  15. The Quartz Analog Watch: A Wonder Machine.

    Science.gov (United States)

    Crane, H. Richard, Ed.

    1993-01-01

    Summarizes how a quartz watch works. Discusses the quartz crystal, its form, and how its frequency is set to a standard; the integrated circuit chip that drives the crystal in vibration, scales its frequency down, and forms pulses that turn the motor; and the motor that drives the gear train that turns the hands. (ZWH)

  16. Hydride formation on deformation twin in zirconium alloy

    Science.gov (United States)

    Kim, Ju-Seong; Kim, Sung-Dae; Yoon, Jonghun

    2016-12-01

    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.

  17. Destabilization of magnesium hydride through interface engineering

    NARCIS (Netherlands)

    Mooij, L.P.A.

    2013-01-01

    The aim of this thesis is to study the thermodynamics of hydrogenation of nanoconfined magnesium within a thin film multilayer model system. Magnesium hydride is a potential material for hydrogen storage, which is a key component in a renewable energy system based on hydrogen. In bulk form,

  18. Destabilization of magnesium hydride through interface engineering

    NARCIS (Netherlands)

    Mooij, L.P.A.

    2013-01-01

    The aim of this thesis is to study the thermodynamics of hydrogenation of nanoconfined magnesium within a thin film multilayer model system. Magnesium hydride is a potential material for hydrogen storage, which is a key component in a renewable energy system based on hydrogen. In bulk form, magnesiu

  19. Destabilization of magnesium hydride through interface engineering

    NARCIS (Netherlands)

    Mooij, L.P.A.

    2013-01-01

    The aim of this thesis is to study the thermodynamics of hydrogenation of nanoconfined magnesium within a thin film multilayer model system. Magnesium hydride is a potential material for hydrogen storage, which is a key component in a renewable energy system based on hydrogen. In bulk form, magnesiu

  20. Lab-size rechargeable metal hydride-air cells

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Wei-Kang; Noreus, Dag [Department of Materials and Enviromental Chemistry, Arrhenius Laboratory, Stockholm University, S-106 91 Stockholm (Sweden)

    2010-09-01

    Lab-size rechargeable metal hydride-air (MH-air) cells with a gas management device were designed in order to minimize the loss of electrolyte. An AB{sub 5}-type hydrogen storage alloy was used as anode materials of the MH-air. The thickness of the metal hydride electrodes was in the range of 3.0-3.4 mm. Porous carbon-based air electrodes with Ag{sub 2}O catalysts were used as bi-functional electrodes for oxygen reduction and generation. The electrodes were first examined in half-cells to evaluate their performance and then assembled into one MH-air cell. The results showed the good cycling stability of the rechargeable MH-air cell with a capacity of 1990 mAh. The discharge voltage was 0.69 V at 0.05-0.1 C. The charge efficiency was about 90%. The specific and volumetric energy densities were about 95Wh kg{sup -1} and 140 Wh L{sup -1}, respectively. (author)

  1. Rotational Symmetry and Absolute Sign of Second-Order Susceptibility of α-Quartz

    Institute of Scientific and Technical Information of China (English)

    吕荣; 王鸿飞

    2003-01-01

    We investigate the rotational symmetry and absolute sign of the effective second-order susceptibility of the righthanded z-cut α-quartz crystal in different crystal orientations through the second-harmonic-generation phase interference between standard and reference of thin α-quartz plates. The Ds rotational symmetry of the z-cut α-quartz crystal shows 6 alternating sign sections of the second-order susceptibility in the 360° rotation, which leads to two distinctive interference patterns between the reference and standard second harmonic field. From this information, the sign of the interference pattern in the second harmonic phase measurement could be readily derived.

  2. 氢化物发生-非色散原子荧光光谱法同时测定金精矿中痕量铋和汞%Simultaneous determination of trace bismuth and mercury in gold concentrates by hydride generation-nondispersive atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    马熠罡

    2012-01-01

    The method of simultaneous determination of trace bismuth and mercury in gold concentrates by hydride generation-nondispersive atomic fluorescence spectrometry was proposed. The samples were digested by HNO3/HCI and then some references were marked by potassium thiocyanate and thiourea. Calculated the detection limits are 5.6 mg/L and 0. 7 mg/L. The method detection limits are 0. 13 μg/g and 0.012 μg/g,and the precision were 1.2% and 0.6% ,respectively.%采用HNO3/HCl消解,以硫氰化钾掩蔽金,硫脲掩蔽杂质等手段,建立王水消解-双道氢化物发生原子荧光光谱同时测定金精矿中铋和汞含量的新方法.计算出Bi和Hg的检出限分别为5.6,0.7 mg/L,方法的检出限分别为0.13μg/g和0.012 μg/g,精密度分别为1.2%和0.6%.

  3. 流动注射氢化物发生-原子吸收光谱法 测定镍基合金中的硒和锡%Determination of Selenium and Tin in Nickel Alloys by Flow Injection Hydride Generation Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    陈天裕; 汪正

    2001-01-01

    建立了流动注射氢化物发生-原子吸收光谱法测定高温镍基合金中痕量硒和锡的方法。样品用HNO3和HF经微波消解后,制成以EDTA作掩蔽剂的碱性溶液(pH12~13),用标准加入法测定。方法测定硒和锡的检出限分别为1.0μg.g-1和1.8μg.g-1,RSD分别为3%~8%和3%~7%。%Determination of trace Se and Sn in high-temperature nickelalloys by flow injection hydride generation atomic absorption spectrometry was studied. The sample was dissolved by microwave digestion in HNO3 and HF. After addition of EDTA as the masking agent and adjustment of pH to 12~13, Se and Sn were determined by standard addition method. Some reference materials were analysed and satisfactory results were obtained. The detection limits of the method for Se and Sn are 1.0 μg.g-1 and 1.8 μg.g-1, respectively, the RSD of determination are 3%~8% for Se and 3%~7% for Sn.

  4. Study on determination of lead in aluminium polychlorid by continuous flow-hydride generation atomic fluorescence spectrometry%连续流动-氢化物发生原子荧光光谱法测定聚合氯化铝中铅

    Institute of Scientific and Technical Information of China (English)

    龚胜芳; 高树林; 李志华; 王红柳

    2014-01-01

    采用连续流动-氢化物发生原子荧光光谱法(CF-HGAFS)测定聚合氯化铝中的铅,优化了实验条件,在最佳实验条件下,铅的荧光强度在0~25μg /L范围内与浓度呈良好的线性关系,方法检出限为0.043μg/L ,方法回收率在95.3%~105.6%之间,本法操作简便、快捷,而且具有很好的准确性和精密度,应用前景良好。%A method for the determination of lead in aluminium polychlorid by continuous flow-hydride generation atomic fluorescence spectrometry was established .The effect of experimental conditions on the atomic fluorescence intensity were investigated and optimized .In this condition ,the calibration curve was linear up to 25μg/L ,the detection limit was 0 .043μg/L ,and the recovery was in range of 95 .3%-105.6% . The method is not only simple and rapid but also precise and accurate ,and shows good application pros-pects .

  5. Complex fragmentation and silicification structures in fault zones: quartz mineralization and repeated fragmentation along the Fountain Range Fault (Mt. Isa Inlier, Australia)

    Science.gov (United States)

    Seybold, Lina; Blenkinsop, Tom; Heuss, Soraya; Ord, Alison; Kruhl, Jörn H.

    2015-04-01

    In large-scale fault zones fracture networks are commonly generated by high volumes of pressurized fluids, followed by quartz precipitation. In this way large amounts of quartz are formed as microcrystalline masses and as complex vein systems, with partly highly different textures, as a result of different formation processes. Based on field and microstructural data and the quantification of vein patterns, the spatial and temporal connection between fragmentation, quartz crystallization and fluid and material flow along the Fountain Range Fault at Fountain Springs was investigated. Dextral strike-slip led to up to 25 km horizontal displacement along the fault. Due to various fragmentation and quartz formation processes, a ca. 100 m high, 80 - 100 m wide and km-long quartz ridge with numerous vein systems and variable microfabrics was formed. Locally, lenses of highly altered metamorphic wall-rocks occur in the quartz zone. Where exposed, the contact to wall rocks is sharp. Millimetre- to decimetre-thick quartz veins penetrate the wall-rocks only within metre distance from the contact. Several clearly distinguishable fine-grained reddish, brownish to dark and pigment-rich quartz masses form up to 50 m wide and up to several 100 m long steep lenses that build the major part of the silicified fault zone. A chronology can be established. Some of these lenses are oriented slightly oblique to the general trend of the quartz zone, in agreement with the supposed dextral strike slip along the fault. Numerous generations of typically µm-cm thick quartz veins transect the microcrystalline quartz masses and, locally, form anisotropic networks. In the quartz masses, angular fragments often composed of quartz with, again, internal fragmentation structures, indicate earlier fracturing and silicification events. Within the veins, quartz forms geodes, locally filled with fine-grained reddish quartz and palisade structures with feathery textures and fluid-inclusion zoning

  6. Mechanical twinning in small quartz crystals

    Science.gov (United States)

    Laughner, J. W.; Newnham, R. E.; Cross, L. E.

    1982-02-01

    Quartz is known to be ferrobielastic; that is, quartz crystals have domain states (Dauphiné twins) which differ in their elastic compliance values and which can be switched by an appropriately oriented stress. Polycrystalline quartz has also been reported (Tullis 1970) to show preferential orientation of these domains following application of large uniaxial stresses. These experiments were designed to study twinning of synthetic quartz “grains” (minimum size 0.07×0.07×0.02 cm) in specially-constructed composites and of grains in three natural quartz aggregates — a quartzite, a novaculite, and a jasper. Backreflection X-ray techniques were used to verify twinning in the composite grains, while special electroding and electrical detection allowed the twinning processes to be examined in “real time.” Small synthetic quartz crystals were found to behave identically to the massive samples previously studied. Electrical pulses due to the reversal of piezoelectric coefficient d 11 in twinned quartz were detected from quartzite and from the man-made composites. Novaculite also gave electrical pulses which were probably from twinning (evidenced by the correlation of expected and observed pulse sizes and shapes), while no pulses from the jaspers indicative of twinning were detected. Grain size distribution differences are considered the main structural reason for the different behaviors.

  7. Laboratory Rotational Spectroscopy of the Interstellar Diatomic Hydride Ion SH+ (X 3Σ-)

    Science.gov (United States)

    Halfen, DeWayne; Ziurys, Lucy M.

    2016-06-01

    Diatomic hydride are among the most common molecular species in the interstellar medium (ISM). The low molecular mass and thus moments of inertia cause their rotational spectra to lie principally in the submillimeter and far-infrared regions. Diatomic hydrides, both neutral (MH) and ionic (MH+) forms, are also basic building blocks of interstellar chemistry. In ionic form, they may be the “hidden” carriers of refractory elements in dense gas. They are therefore extremely good targets for space-borne and airborne platforms such as Herschel, SOFIA, and SAFIR. However, in order to detect these species in the ISM, their rotational spectra must first be measured in the laboratory. To date, there is very little high resolution data available for many hydride species, in particular the ionic form. Using submillimeter/THz direct absorption methods in the Ziurys laboratory, spectra of the interstellar diatomic hydride SH+ (X 3Σ-) have been recorded. Recent work has concerned measurement of all three fine structure components of the fundamental rotational transition N = 1 ← 0 in the range 345 - 683 GHz. SH+ was generated from H2S and argon in an AC discharge. The data have been analyzed, and spectroscopic constants for this species have been refined. SH+ is found in Photon Dominated Regions (PDRs) and X-ray Dominated Regions (XDRs) and is thought to trace energetic processes in the ISM. These current measurements confirm recent observations of this species at submillimeter/THz wavelengths with ALMA and other ground-based telescopes.

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

    Energy Technology Data Exchange (ETDEWEB)

    Clayton, J C

    1987-10-01

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

  9. 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.)

  10. Bio-inspired transition metal-organic hydride conjugates for catalysis of transfer hydrogenation: experiment and theory.

    Science.gov (United States)

    McSkimming, Alex; Chan, Bun; Bhadbhade, Mohan M; Ball, Graham E; Colbran, Stephen B

    2015-02-09

    Taking inspiration from yeast alcohol dehydrogenase (yADH), a benzimidazolium (BI(+) ) organic hydride-acceptor domain has been coupled with a 1,10-phenanthroline (phen) metal-binding domain to afford a novel multifunctional ligand (L(BI+) ) with hydride-carrier capacity (L(BI+) +H(-) ⇌L(BI) H). Complexes of the type [Cp*M(L(BI) )Cl][PF6 ]2 (M=Rh, Ir) have been made and fully characterised by cyclic voltammetry, UV/Vis spectroelectrochemistry, and, for the Ir(III) congener, X-ray crystallography. [Cp*Rh(L(BI) )Cl][PF6 ]2 catalyses the transfer hydrogenation of imines by formate ion in very goods yield under conditions where the corresponding [Cp*Ir(L(BI) )Cl][PF6 ] and [Cp*M(phen)Cl][PF6 ] (M=Rh, Ir) complexes are almost inert as catalysts. Possible alternatives for the catalysis pathway are canvassed, and the free energies of intermediates and transition states determined by DFT calculations. The DFT study supports a mechanism involving formate-driven RhH formation (90 kJ mol(-1) free-energy barrier), transfer of hydride between the Rh and BI(+) centres to generate a tethered benzimidazoline (BIH) hydride donor, binding of imine substrate at Rh, back-transfer of hydride from the BIH organic hydride donor to the Rh-activated imine substrate (89 kJ mol(-1) barrier), and exergonic protonation of the metal-bound amide by formic acid with release of amine product to close the catalytic cycle. Parallels with the mechanism of biological hydride transfer in yADH are discussed.

  11. Neutrophil-derived ROS contribute to oxidative DNA damage induction by quartz particles.

    Science.gov (United States)

    van Berlo, Damien; Wessels, Anton; Boots, Agnes W; Wilhelmi, Verena; Scherbart, Agnes M; Gerloff, Kirsten; van Schooten, Frederik J; Albrecht, Catrin; Schins, Roel P F

    2010-12-01

    The carcinogenicity of respirable quartz is considered to be driven by reactive oxygen species (ROS) generation in association with chronic inflammation. The contribution of phagocyte-derived ROS to inflammation, oxidative stress, and DNA damage responses was investigated in the lungs of C57BL/6J wild-type and p47(phox-/-) mice, 24h after pharyngeal aspiration of DQ12 quartz (100 mg/kg bw). Bone-marrow-derived neutrophils from wild-type and p47(phox-/-) mice were used for parallel in vitro investigations in coculture with A549 human alveolar epithelial cells. Quartz induced a marked neutrophil influx in both wild-type and p47(phox-/-) mouse lungs. Significant increases in mRNA expression of the oxidative stress markers HO-1 and γ-GCS were observed only in quartz-treated wild-type animals. Oxidative DNA damage in lung tissue was not affected by quartz exposure and did not differ between p47(phox-/-) and WT mice. Differences in mRNA expression of the DNA repair genes OGG1, APE-1, DNA Polβ, and XRCC1 were also absent. Quartz treatment of cocultures containing wild-type neutrophils, but not p47(phox-/-) neutrophils, caused increased oxidative DNA damage in epithelial cells. Our study demonstrates that neutrophil-derived ROS significantly contribute to pulmonary oxidative stress responses after acute quartz exposure, yet their role in the associated induction of oxidative DNA damage could be shown only in vitro.

  12. Kinetics of pulpal temperature rise during light curing of 6 bonding agents from different generations, using light emitting diode and quartz-tungsten-halogen units: An in-vitro simulation

    Science.gov (United States)

    Khaksaran, Najmeh Khatoon; Kashi, Tahereh Jafarzadeh; Rakhshan, Vahid; Zeynolabedin, Zahra Sadat; Bagheri, Hossein

    2015-01-01

    Background: Application of bonding agents (BA) into deep cavities and light curing them might increase pulpal temperature and threaten its health. The purpose of this study was to evaluate temperature rise of pulp by light curing six BA using two different light curing units (LCU), through a dent in wall of 0.5 mm. Materials and Methods: This in vitro experiment was carried out on 96 slices of the same number of human third molars (6 BAs × 2 LCUs × 8 specimens in each group). There were 6 groups of BAs: N Bond, G-Bond, OptiBond XTR, Clearfil SE, Adper Single Bond 2 and V Bond. Each group of BA (n = 16) had two subgroups of light emitting diode (LED) and quartz-tungsten-halogen light cure units (n = 8). Each of these 16 specimens were subjected to light emitting for 20 s, once without any BAs (control) and later when a BA was applied to surface of disk. Temperature rises in 140 s were evaluated. Their mean temperature change in first 20 s were calculated and analyzed using two-way repeated-measures and one-way analysis of variance (ANOVA) and Tukey (α = 0.05). Furthermore rate of temperature increase was calculated for each material and LCU. Results: Minimum and maximum temperature rises in all subgroups were 1.7 and 2.8°C, respectively. Repeated measures ANOVA showed that both of adhesive and LCU types had significant effect on temperature rise after application of adhesives. Tukey post-hoc analysis showed Clearfil SE showed significantly higher temperature rise in comparison with Adper Single bond 2 (P = 0.047) and N Bond (P = 0.038). Temperature rose in a linear fashion during first 30-40 s and after that it was non-linear. Conclusion: 20 s of light curing seems safe for pulpal health (with critical threshold of 5.5°C). However, in longer durations and especially when using LED units, the process should be broken to two sessions. PMID:25878684

  13. Kinetics of pulpal temperature rise during light curing of 6 bonding agents from different generations, using light emitting diode and quartz-tungsten-halogen units: An in-vitro simulation

    Directory of Open Access Journals (Sweden)

    Najmeh Khatoon Khaksaran

    2015-01-01

    Full Text Available Background: Application of bonding agents (BA into deep cavities and light curing them might increase pulpal temperature and threaten its health. The purpose of this study was to evaluate temperature rise of pulp by light curing six BA using two different light curing units (LCU, through a dent in wall of 0.5 mm. Materials and Methods: This in vitro experiment was carried out on 96 slices of the same number of human third molars (6 BAs × 2 LCUs × 8 specimens in each group. There were 6 groups of BAs: N Bond, G-Bond, OptiBond XTR, Clearfil SE, Adper Single Bond 2 and V Bond. Each group of BA (n = 16 had two subgroups of light emitting diode (LED and quartz-tungsten-halogen light cure units (n = 8. Each of these 16 specimens were subjected to light emitting for 20 s, once without any BAs (control and later when a BA was applied to surface of disk. Temperature rises in 140 s were evaluated. Their mean temperature change in first 20 s were calculated and analyzed using two-way repeated-measures and one-way analysis of variance (ANOVA and Tukey (α = 0.05. Furthermore rate of temperature increase was calculated for each material and LCU. Results: Minimum and maximum temperature rises in all subgroups were 1.7 and 2.8°C, respectively. Repeated measures ANOVA showed that both of adhesive and LCU types had significant effect on temperature rise after application of adhesives. Tukey post-hoc analysis showed Clearfil SE showed significantly higher temperature rise in comparison with Adper Single bond 2 (P = 0.047 and N Bond (P = 0.038. Temperature rose in a linear fashion during first 30-40 s and after that it was non-linear. Conclusion: 20 s of light curing seems safe for pulpal health (with critical threshold of 5.5°C. However, in longer durations and especially when using LED units, the process should be broken to two sessions.

  14. SAW Temperature Sensor on Quartz.

    Science.gov (United States)

    Zhgoon, Sergei; Shvetsov, Alexander; Ancev, Ivan; Bogoslovsky, Sergei; Sapozhnikov, Gennadiy; Trokhimets, Konstantin; Derkach, Mikhail

    2015-06-01

    For biomedical applications, narrow temperature range and high sensor accuracy requirements define the need for high temperature sensitivity. Wireless SAW sensors connected to antennas need a reference element to account for changes in electromagnetic coupling between the transmitter and receiver antennas. A pair of sensors with different temperature sensitivities may serve as a self-referenced sensor assembly. This justifies the need for materials with useful SAW resonator properties and with the largest difference between temperature coefficients of frequency (TCF) for a resonator pair on a single substrate. We have identified several cuts of quartz having useful properties with a TCF difference up to 140 ppm/°C for a pair of resonators on a single substrate. As a rule, placing such resonators on a single substrate requires their rotation by up to 90° relative to each other. The limited range of cuts presents a unique opportunity to place both resonators along the X+90° direction with one resonator using Bleustein-Gulyaev-Shimizu (BGS) waves (with electrodes placed along the x-axis) and the other one (with electrodes inclined by about ±10° to the x-axis) using quasi-Rayleigh waves. These cuts are close to the 70°Y cut where a high TCF difference is reached together with acceptable characteristics of the resonators. Resonators were designed for all useful cuts (including the 70°Y cut) and tested. The use of different periods in reflectors and interdigital transducer (IDT) together with individual choice of gaps between reflectors and IDT meant achieving low spurious content in resonator responses. The quality factors reached values up to 3500 at central frequencies around 915 MHz for both BGS and quasi-Rayleigh types of waves. The measured difference of the TCF is about 138 ppm/°C on 70°Y cut that is close to the calculated value.

  15. Quartz-Enhanced Photoacoustic Spectroscopy: A Review

    Directory of Open Access Journals (Sweden)

    Pietro Patimisco

    2014-03-01

    Full Text Available A detailed review on the development of quartz-enhanced photoacoustic sensors (QEPAS for the sensitive and selective quantification of molecular trace gas species with resolved spectroscopic features is reported. The basis of the QEPAS technique, the technology available to support this field in terms of key components, such as light sources and quartz-tuning forks and the recent developments in detection methods and performance limitations will be discussed. Furthermore, different experimental QEPAS methods such as: on-beam and off-beam QEPAS, quartz-enhanced evanescent wave photoacoustic detection, modulation-cancellation approach and mid-IR single mode fiber-coupled sensor systems will be reviewed and analysed. A QEPAS sensor operating in the THz range, employing a custom-made quartz-tuning fork and a THz quantum cascade laser will be also described. Finally, we evaluated data reported during the past decade and draw relevant and useful conclusions from this analysis.

  16. Quartz-enhanced photoacoustic spectroscopy: a review.

    Science.gov (United States)

    Patimisco, Pietro; Scamarcio, Gaetano; Tittel, Frank K; Spagnolo, Vincenzo

    2014-03-28

    A detailed review on the development of quartz-enhanced photoacoustic sensors (QEPAS) for the sensitive and selective quantification of molecular trace gas species with resolved spectroscopic features is reported. The basis of the QEPAS technique, the technology available to support this field in terms of key components, such as light sources and quartz-tuning forks and the recent developments in detection methods and performance limitations will be discussed. Furthermore, different experimental QEPAS methods such as: on-beam and off-beam QEPAS, quartz-enhanced evanescent wave photoacoustic detection, modulation-cancellation approach and mid-IR single mode fiber-coupled sensor systems will be reviewed and analysed. A QEPAS sensor operating in the THz range, employing a custom-made quartz-tuning fork and a THz quantum cascade laser will be also described. Finally, we evaluated data reported during the past decade and draw relevant and useful conclusions from this analysis.

  17. Electronic dipole resonance in smoky quartz

    NARCIS (Netherlands)

    Kerssen, J.; Volger, J.

    1967-01-01

    Microwave absorption in smoky quartz mono-crystal is ascribed to resonance transitions of trapped electrons between initially configurational degenerated states, which are Stark-splitted by a polarizing electric field.

  18. Quartz Mountain/Oklahoma Summer Arts Institute.

    Science.gov (United States)

    Frates, Mary Y.; Madeja, Stanley S.

    1982-01-01

    Describes the Quartz Mountain Oklahoma Summer Arts Institute program. It is designed to nurture artistic talent and to provide intensive arts experiences in music, dance, theater, and the visual arts for talented students aged 14-18. (AM)

  19. Modelling zirconium hydrides using the special quasirandom structure approach

    KAUST Repository

    Wang, Hao

    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.

  20. Numerical study of a magnesium hydride tank

    Science.gov (United States)

    Delhomme, Baptiste; de Rango, Patricia; Marty, Philippe

    2012-11-01

    Hydrogen storage in metal hydride tanks (MHT) is a very promising solution. Several experimental tanks, studied by different teams, have already proved the feasibility and the interesting performances of this solution. However, in much cases, an optimization of tank geometry is still needed in order to perform fast hydrogen loading. The development of efficient numerical tools is a key issue for MHT design and optimization. We propose a simple model representing a metal hydride tank exchanging its heat of reaction with a thermal fluid flow. In this model, the radial and axial discretisations have been decoupled by using Matlab® one-dimensional tools. Calculations are compared to experimental results obtained in a previous study. A good agreement is found for the loading case. The discharging case shows some discrepancies, which are discussed in this paper.

  1. 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...

  2. Nickel metal hydride LEO cycle testing

    Science.gov (United States)

    Lowery, Eric

    1995-01-01

    The George C. Marshall Space Flight Center is working to characterize aerospace AB5 Nickel Metal Hydride (NiMH) cells. The cells are being evaluated in terms of storage, low earth orbit (LEO) cycling, and response to parametric testing (high rate charge and discharge, charge retention, pulse current ability, etc.). Cells manufactured by Eagle Picher are the subjects of the evaluation. There is speculation that NiMH cells may become direct replacements for current Nickel Cadmium cells in the near future.

  3. Storing hydrogen in the form of light alloy hydrides

    Science.gov (United States)

    Freund, E.; Gillerm, C.

    1981-01-01

    Different hydrides are investigated to find a system with a sufficiently high storage density (at least 3%). The formation of hydrides with light alloys is examined. Reaction kinetics for hydride formation were defined and applied to the systems Mg-Al-H, Mg-Al-Cu-H, Ti-Al-H, Ti-Al-Cu-H, and Ti-Al-Ni-H. Results indicate that the addition of Al destabilizes MgH2 and TiH2 hydrides while having only a limited effect on the storage density.

  4. Anomalous quartz from the Roter Kamm impact crater, Namibia - Evidence for post-impact hydrothermal activity?

    Science.gov (United States)

    Koeberl, Christian; Fredriksson, Kurt; Goetzinger, Michael; Reimold, Wolf Uwe

    1989-01-01

    Quartz pebbles from the Roter Kamm impact crater (the Namib Desert, SWA/Namibia) were examined for evidence of impact-induced hydrothermal activity, using results from microprobe analyses, neutron activation analyses, transmission IR spectroscopy, and X-ray diffractometry. It was found that the pebbles consisted of pure quartz, which contains three different types of fluid inclusions. These were identified as primary inclusions (5-10 microns) that record the formation conditions of the quartz, very small (less than 1 micron) secondary inclusions associated with the grain boundaries, and late inclusions of irregular size. It is concluded that the quartz and the primary inclusions may provide evidence for a postimpact phase of extensive hydrothermal activity, generated by the residual heat from the kinetic energy of the impact.

  5. Plasmonic hydrogen sensing with nanostructured metal hydrides.

    Science.gov (United States)

    Wadell, Carl; Syrenova, Svetlana; Langhammer, Christoph

    2014-12-23

    In this review, we discuss the evolution of localized surface plasmon resonance and surface plasmon resonance hydrogen sensors based on nanostructured metal hydrides, which has accelerated significantly during the past 5 years. We put particular focus on how, conceptually, plasmonic resonances can be used to study metal-hydrogen interactions at the nanoscale, both at the ensemble and at the single-nanoparticle level. Such efforts are motivated by a fundamental interest in understanding the role of nanosizing on metal hydride formation processes in the quest to develop efficient solid-state hydrogen storage materials with fast response times, reasonable thermodynamics, and acceptable long-term stability. Therefore, a brief introduction to the thermodynamics of metal hydride formation is also given. However, plasmonic hydrogen sensors not only are of academic interest as research tool in materials science but also are predicted to find more practical use as all-optical gas detectors in industrial and medical applications, as well as in a future hydrogen economy, where hydrogen is used as a carbon free energy carrier. Therefore, the wide range of different plasmonic hydrogen sensor designs already available is reviewed together with theoretical efforts to understand their fundamentals and optimize their performance in terms of sensitivity. In this context, we also highlight important challenges to be addressed in the future to take plasmonic hydrogen sensors from the laboratory to real applications in devices, including poisoning/deactivation of the active materials, sensor lifetime, and cross-sensitivity toward other gas species.

  6. 高效液相色谱氢化物发生原子荧光光谱联用检测海藻中砷形态%Determination of arsenic speciation in seaweeds using high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    高鹭; 董伟峰; 彭心婷; 史立娟; 李妍; 庞艳华; 徐静; 曹际娟

    2015-01-01

    目的:测定14种海藻样品中总砷和无机砷的含量,同时分析样品中6种砷形态。方法将海藻样品经过微波消解的前处理方法,通过电感耦合等离子体质谱(inductively coupled plasma mass spectrometry, ICP-MS)测定总砷含量;根据国标方法中无机砷检测的前处理方法,通过原子荧光光谱(atomic fluorescence spectrometry, AFS)测定无机砷含量;最后通过酸提的前处理方法,利用高效液相色谱-氢化物发生-原子荧光光谱法(high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry, HPLC-(UV)-HG-AFS)测定海藻样品中6种形态砷含量并与国标无机砷方法比较。结果14种海藻样品中总砷含量为0.038~46.2 mg/kg;无机砷含量为0.006~19.3 mg/kg;对HPLC-(UV)-HG-AFS仪器的优化和方法的摸索后,从海藻样品中主要测得的砷形态为As(III)、As(V)和DMA, MMA含量较少,没有测出AsB和 AsC。结论在砷形态较为复杂的海藻样品检测中,通过 HPLC-(UV)-HG-AFS 检测方法可以有效避免无机砷前处理中可能出现的有机砷向无机砷转变的现象,降低干扰,增加测试的准确性,更为具体地表现海藻样品中主要的砷形态含量。%Objective The content of total arsenic and inorganic arsenic were determined in 14 seaweeds and 6 kinds of arsenic species were determined at the same time. Methods The content of total arsenic was determined by inductively coupled plasma mass spectrometry (ICP-MS) after microwave digestion. According to the pretreatment method of national standard method, the content of inorganic arsenic was determined by atomic fluorescence spectrometry (AFS). The results of 6 arsenic species were studied by high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry (HPLC-(UV)-HG-AFS) after acid extraction, which were compared with the national standard method. Results In 14

  7. Determination of Lead in Tea Garden Soil by Hydride Generation Atomic Fluorescence Spectrometry with Microwave Digestion%微波消解-氢化物发生原子荧光光谱法测定茶园土壤中的铅

    Institute of Scientific and Technical Information of China (English)

    凤海元; 时晓露; 黄勤

    2013-01-01

    样品用王水微波消解浸提,氢化物发生-原子荧光光谱法测定茶园土壤中痕量铅的含量.对样品浸取方法、实验条件、增感剂和共存元素进行了条件实验.结果表明,王水微波消解浸取,铅浸出量最大,减少了试剂用量和环境污染;铁氰化钾-盐酸羟胺体系有显著的增感作用,铁氰化钾在配制溶液时用米糠除去试剂中可能存在的铅,降低了空白;钴、锌、砷、镉等共存离子不干扰铅的测定,通过加入邻菲啰啉-硫氰酸钠消除铁和铜的干扰,提高了铅的回收率.方法检出限为0.65 μg/L,精密度(RSD,n=10)为1.89%,回收率在86.8% ~ 110.4%之间.用土壤标准物质验证,测定值与标准值相符,方法快速准确,适合于大批量样品的分析检测.%The microwave digestion system with aqua regia was developed for the determination of trace lead in tea garden soil using Hydride Generation-Atomic Fluorescence Spectrometry ( HG-AFS). The leaching methods, experimental conditions, booster and coexisting element were optimized. The largest amount of lead was leached out by microwave digestion with aqua regia, which has the advantages of less usage of reagent and less environmental pollution. An appropriate amount of potassium ferricyanide and hydroxylamine hydrochloride improved the hydride generation efficiency of Pb. The lead blank was reduced significantly when Potassium ferricyanide solution was treated with rice husk to remove Pb in the reagent. It was found that Co, Zn, As, and Cd did not interfere with the determination of lead. The addition of 1,10-phenanthroline monohydrate and sodium hydrosulfide could effectively eliminate the interferences from Fe and Cu, which improved the recovery rate of lead. The limit of detection was 0. 65 μg/L and the precision was 1. 89% (n = 10) with recoveries of 86. 8% - 110. 4% for Pb. The reliability of the method has been tested by determination of Pb in the Soils Standard Reference

  8. 人血和尿中锡的高压微波络合消解氢化物发生-原子荧光测定法%Determination of tin in human blood and urine with high-pressure microwave digestion and complexing ligand and hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    陈峰; 谢超

    2013-01-01

    Objective To establish the hydride generation-atomic fluorescence spectrometric method for the determination of tin in human blood and urine with high-pressure microwave digestion and complexing ligand.Methods Human blood and urine samples were digested by using high-pressure microwave.Then complexing ligand 1% EDTA,5 ml 150 g/L thiourea and ascorbic acid were added to mask the interfering ions such as nickel,iron,arsenic,selenium and etc.Tin concentration was determined with hydride-generation atomic fluorescence spectrometric method with sodium borohydride as the reductant in 2% sulphuric acid media.Results The linear range of tin was 10-100 μg/ml,the regression equations and correlation coefficients in blood and urine were y=9.391 1 x-16.312,r=0.999 7,y=8.244 7x-27.849 6,r=0.998 2,respectively.The limits of detection of tin in blood and urine were 0.090,0.020 μg/L respectively.The relative standard derivation of this method was 1.4%-6.1%.The rates of recovery were between 98.1% and 101.8%.Conclusion This method presents many advantages,such as completed sample digestion,rapid,less matrix disturbance,accurate,sensitive and is applicable to the determination of tin in blood and urine in grass-roots units.%目的 建立人血、尿中锡的高压微波络合消解氢化物发生-原子荧光测定法.方法 利用高压微波络合消解已加入1% EDTA溶液的人血和尿液,在样品测定液中加入150 g/L硫脲-抗坏血酸5ml来掩蔽镍、铁、砷、硒等干扰离子;以2%硫酸作为介质,以2%的硼氢化钠溶液作为还原剂,采用氢化物发生-原子荧光法测定锡浓度.结果 在10~100 μg/ml的线性范围内,血中锡所得回归方程为y=9.391 1x-16.312,r=0.999 7;尿中锡所得回归方程为y=8.244 7x-27.849 6,r=0.998 2.血、尿中锡的检出限分别为0.090、0.020 μg/L.该方法的RSD为1.4%~6.1%,回收率在98.1%~101.8%之间.结论 该方法样品消解完全,测定时间短,待测元素

  9. 微波消解-氢化物原子荧光光谱法测定粤东地区海产品中砷的研究%Determination of Arsenic in Seafood by Hydride Generation-atomic Fluorescence Spectrometry Combined with Microwave Oven Digestion

    Institute of Scientific and Technical Information of China (English)

    蔡龙飞; 徐春秀; 张应钦; 邱新红

    2011-01-01

    [目的]建立一种测定海产品中微量砷的有效方法.[方法]采用微波消解-氢化物原子荧光光谱法测定了粤东地区海产品中砷的含量.[结果]砷在1.0~50.0μg/L范围内线性关系良好,相关系数为0.995,方法的检出限为0.02107μg/L,相对标准偏差为0.932%.部分海产品的含砷量超过国家标准,其超标原因可能与沿海地区的工业污染有关.[结论]该方法试剂用量少、污染小、简便、快速、准确,适于各类海产品中砷含量的检测.%[Objective] The aim was to establish an effective determination method of arsenic in seafood. [Method] Contents of arsenic in seafood samples from eastern Guangdong area were determined by hydride generation-atomic fluorescence spectrometry combined with microwave oven digestion. [Result] The linear range for detection of arsenic was 1.0- 50.0 μg/L, which showed a good linear relationship,and its correlation coefficient was 0.995. The detection limit and relative standard deviation were 0.021 07 μg/L and 0.932% .respectively. Contents of arsenic in some seafood samples were more than the national standard,which could be caused by industrial pollution in coastal areas. [Conclusion] The method is simple,rapid and accurate,so it is applied to the determination of arsenic in seafood samples.

  10. Determination of As,Hg and Cd in FAPAS Canned Fish in UK by Hydride Generation-Atomic Fluorescence Spectrometry%氢化物-原子荧光光谱法测定英国FAPAS鱼罐头中砷汞镉

    Institute of Scientific and Technical Information of China (English)

    叶海辉; 谢德芳; 谢轶; 吴学进

    2012-01-01

    [Objective] To prove that the determination of As, Hg and Cd by the hydride generation-atomic fluorescence spectrometry (HG-AFS) has reached the international level of advanced detection instrument. [ Method] The parameters and testing methods of the HG-AFS were optimized. Through the testing of samples and the recovery test, a set of methods were established for determining the three elements in FAPAS canned fish. [Result] By comparing the detection report provided by FAPAS with the results of multiple laboratories, the Z value was -0.2 for As, 0. 5 for Hg, and 0.4 for Cd, the evaluation of results was satisfactory. [ Conclusion] It is feasible'to apply the HG-AFS method for the determination of As, Hg and Cd in seafood products.%[目的]证实原子荧光仪对这砷汞镉3种元素的检测已达到国际先进检测仪器的水平.[方法]利用氢化物-原子荧光光谱法,优化仪器条件参数和试验方法,通过测试质控样品与加标回收试验,建立一套测试英国FAPAS鱼罐头中砷汞镉的方法.[结果]根据FAPAS提供回来的检测报告,与全球众多实验室比对的结果为:砷的Z值为-0.2,汞的Z值为0.5,镉的Z值为0.4,对结果的评价为很满意.[结论]应用氢化物-原子荧光光谱法对海产品中砷汞镉进行检测是可行的.

  11. Separation/preconcentration of ultra-trace levels of inorganic Sb and Se from different sample matrices by charge transfer sensitized ion-pairing using ultrasonic-assisted cloud point extraction prior to their speciation and determination by hydride generation AAS.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan

    2016-10-01

    In the existing study, a new, simple and low cost process for separation/preconcentration of ultra-trace level of inorganic Sb and Se from natural waters, beverages and foods using ultrasonic-assisted cloud point extraction (UA-CPE) prior to their speciation and determination by hydride generation AAS, is proposed. The process is based on charge transfer sensitized complex formations of Sb(III) and Se(IV) with 3-amino-7-dimethylamino-2-methylphenazine hydrochloride (Neutral red, NRH(+)) in presence of pyrogallol and cetyltrimethylammonium bromide (CTAB) as both sensitivity enhancement and counter ion at pH 6.0. Under the optimized reagent conditions, the calibration curves were highly linear in the ranges of 8-300ngL(-1) and 12-250ngL(-1) (r(2)≥0.993) for Se(IV) and Sb(III), respectively. The limits of detection were 2.45 and 3.60ngL(-1) with sensitivity enhancement factors of 155 and 120, respectively. The recovery rate was higher than 96% with a relative standard deviation lower than 5.3% for five replicate measurements of 25, 75 and 150ngL(-1) Se(IV) and Sb(III), respectively. The method was validated by analysis of two certified reference materials (CRMs), and was successfully applied to the accurate and reliable speciation and determination of the contents of total Sb/Sb(III), and total Se/Se(IV) after UA-CPE of the pretreated sample matrices with and without pre-reduction with a mixture of l-cysteine and tartaric acid. Their Sb(V) and Se(VI) contents were calculated from the differences between total Sb and Sb(III) and/or total Se and Se(IV) levels.

  12. Application of Factorial Designs and Simplex Optimisation in the Development of Flow Injection-Hydride Generation-Graphite Furnace Atomic Absorption Spectrometry Procedures as Demonstrated for the Determination of Trace Levels of Germanium

    DEFF Research Database (Denmark)

    Hilligsøe, Bo; Hansen, Elo Harald

    1997-01-01

    The optimisation of a volume-based FI-HG-GFAAS procedure is described for the trace determination of Ge, comprising in situ collection of the generated germane in the graphite furnace. The response function is the peak area readout (A*s). Based on a preliminary study, where factorial designs were...... at a sampling frequency of 22 h-1. The sensitivity, in terms of the characteristic mass, m0, was 26 pg/0.0044 A*s, with a detection limit of 0.21 mu-g/L (3 sigma). The precision (relative standard deviation) was 2.0% (n=10) at the 1 mu-g/L level....

  13. Method of making crack-free zirconium hydride

    Science.gov (United States)

    Sullivan, Richard W.

    1980-01-01

    Crack-free hydrides of zirconium and zirconium-uranium alloys are produced by alloying the zirconium or zirconium-uranium alloy with beryllium, or nickel, or beryllium and scandium, or nickel and scandium, or beryllium and nickel, or beryllium, nickel and scandium and thereafter hydriding.

  14. 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.

  15. Electrochemical and Optical Properties of Magnesium-Alloy Hydrides Reviewed

    Directory of Open Access Journals (Sweden)

    Thirugnasambandam G. Manivasagam

    2012-10-01

    Full Text Available As potential hydrogen storage media, magnesium based hydrides have been systematically studied in order to improve reversibility, storage capacity, kinetics and thermodynamics. The present article deals with the electrochemical and optical properties of Mg alloy hydrides. Electrochemical hydrogenation, compared to conventional gas phase hydrogen loading, provides precise control with only moderate reaction conditions. Interestingly, the alloy composition determines the crystallographic nature of the metal-hydride: a structural change is induced from rutile to fluorite at 80 at.% of Mg in Mg-TM alloy, with ensuing improved hydrogen mobility and storage capacity. So far, 6 wt.% (equivalent to 1600 mAh/g of reversibly stored hydrogen in MgyTM(1-yHx (TM: Sc, Ti has been reported. Thin film forms of these metal-hydrides reveal interesting electrochromic properties as a function of hydrogen content. Optical switching occurs during (dehydrogenation between the reflective metal and the transparent metal hydride states. The chronological sequence of the optical improvements in optically active metal hydrides starts with the rare earth systems (YHx, followed by Mg rare earth alloy hydrides (MgyGd(1-yHx and concludes with Mg transition metal hydrides (MgyTM(1-yHx. In-situ optical characterization of gradient thin films during (dehydrogenation, denoted as hydrogenography, enables the monitoring of alloy composition gradients simultaneously.

  16. High energy density battery based on complex hydrides

    Science.gov (United States)

    Zidan, Ragaiy

    2016-04-26

    A battery and process of operating a battery system is provided using high hydrogen capacity complex hydrides in an organic non-aqueous solvent that allows the transport of hydride ions such as AlH.sub.4.sup.- and metal ions during respective discharging and charging steps.

  17. High energy density battery based on complex hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Zidan, Ragaiy

    2016-04-26

    A battery and process of operating a battery system is provided using high hydrogen capacity complex hydrides in an organic non-aqueous solvent that allows the transport of hydride ions such as AlH.sub.4.sup.- and metal ions during respective discharging and charging steps.

  18. Synthesis, characterization and properties of some organozinc hydride complexes

    NARCIS (Netherlands)

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

    1980-01-01

    The synthesis and characterization of the monopyridine complexes of ethylzinc hydride and phenylzinc hydride are described. On treatment with TMED these complexes are converted into R2Zn3H4. TMED species through a combination of ligand-exchange and disproportionation. The formation of organozinc hyd

  19. Hydride morphology and striation formation during delayed hydride cracking in Zr-2.5% Nb

    Energy Technology Data Exchange (ETDEWEB)

    Shek, G.K. [Ontario Hydro Technol., Ont. (Canada). Mater. Technol. Unit; Jovanovic, M.T. [Alberta Univ., Edmonton, AB (Canada). Dept. of Mining, Metallurgical and Petroleum Engineering; Seahra, H. [Ontario Hydro Technol., Ont. (Canada). Mater. Technol. Unit; Ma, Y. [Alberta Univ., Edmonton, AB (Canada). Dept. of Mining, Metallurgical and Petroleum Engineering; Li, D. [Alberta Univ., Edmonton, AB (Canada). Dept. of Mining, Metallurgical and Petroleum Engineering; Eadie, R.L. [Alberta Univ., Edmonton, AB (Canada). Dept. of Mining, Metallurgical and Petroleum Engineering

    1996-08-01

    These experiments were designed to study hydride formation at the crack tip, acoustic emission (AE), potential drop (PD) and striation formation during DHC (delayed hydride cracking) in Zr-2.5% Nb. The test material was taken from an especially extruded pressure tube, which showed similar strength properties to normal pressure tube material but somewhat coarser microstructure. In testing at K{sub I} below 12 MPa {radical}m at both 200 and 250 C very large striations (>40 {mu}m at 200 and >50 {mu}m at 250 C) were produced. In simultaneous monitoring with acoustic emission and potential drop, both AE and PD jumps were shown to be monolithic. The number of striations on the fracture surface corresponded to the number of monolithic AE/PD jumps. Tapered shaped hydrides with the thick end adjacent to the crack tip were observed. These hydrides grew in size during the incubation period until they reached the striation length and then fractured monolithically. However, when K{sub I} was increased beyond about 12 MPa {radical}m for these same specimens, the striation spacing decreased below 30 {mu}m, the monolithic jumping dissolved into more continuous changes in signals, although the smaller striations were still visible on the fracture surface. (orig.).

  20. Hydride morphology and striation formation during delayed hydride cracking in Zr-2.5% Nb

    Science.gov (United States)

    Shek, G. K.; Jovanoviċ, M. T.; Seahra, H.; Ma, Y.; Li, D.; Eadie, R. L.

    1996-08-01

    These experiments were designed to study hydride formation at the crack tip, acoustic emission (AE), potential drop (PD) and striation formation during DHC (delayed hydride cracking) in Zr-2.5% Nb. The test material was taken from an especially extrude pressure tube, which showed similar strength properties to normal pressure tube material but somewhat coarser microstructure. In testing at KI below 12 MPa √m at both 200 and 250°C very large striations (> 40 μ at 200 and >50 μm at 250°C) were produced. In simultaneous monitoring with acoustic emission and potential drop, both AE and PD jumps were shown to be monolithic. The number of striations on the fracture surface corresponded to the number of monolithic AE/PD jumps. Tapered shaped hydrides with the thick end adjacent to the crack tip were observed. These hydrides grew in size during the incubation period until they reached the striation length and then fractured monolithically. However, when KI was increased beyond about 12 MPa √m for these same specimens, the striation spacing decreased below 30 μ, the monolithic jumping dissolved into more continuous changes in signals, although the smaller striations were still visible on the fracture surface.

  1. High ramp rate thermogravimetric analysis of zirconium(II) hydride and titanium(II) hydride

    Energy Technology Data Exchange (ETDEWEB)

    Licavoli, Joseph J., E-mail: jjlicavo@mtu.edu; Sanders, Paul G., E-mail: sanders@mtu.edu

    2015-09-20

    Highlights: • A unique arc image device has been proposed for high ramp rate thermogravimetry. • Powder oxidation influences decomposition kinetics at temperatures below 933 K. • Particle size has a negligible effect on TiH{sub 2} decomposition behavior. • Improvements to the device are required to conduct accurate kinetic analysis. - Abstract: Zirconium and titanium hydride are utilized in liquid phase metal foam processing techniques. This application results in immediate exposure to molten metal and almost immediate decomposition at high temperatures. Most decomposition characterization techniques utilize slow heating rates and are unable to capture the decomposition behavior of hydrides under foam processing conditions. In order to address this issue a specialized high ramp rate thermogravimetric analyzer was created from a xenon arc image refiner. In addition to thermogravimetry, complimentary techniques including X-ray diffraction and scanning electron microscopy were used to characterize hydride decomposition and compare the results to literature. Hydrides were partially oxidized and separated into particles size ranges to evaluate the influence of these factors on decomposition. Oxidizing treatments were found to decrease decomposition rate only at temperatures below 933 K (660 °C) while particle size effects appeared to be negligible. Several improvements to the unique TGA apparatus presented in the current work are suggested to allow reliable kinetic modeling and analysis.

  2. Metal hydrides used as negative electrode materials for Li-ion batteries

    Science.gov (United States)

    Sartori, Sabrina; Cuevas, Fermin; Latroche, Michel

    2016-02-01

    Energy is a key issue for future generation. Researches are conducted worldwide to develop new efficient means for energy conversion and storage. Electrochemical storage is foreseen as an efficient way to handle intermittent renewable energy production. The most advanced batteries are nowadays based on lithium-ion technology though their specific capacities should be significantly increased to bring solution to mass storage. Conversion reactions are one way to step forward larger capacities at the anode. We here review the possibility to use metallic or complex hydrides as negative electrode using conversion reaction of hydride with lithium. Moreover, promising alloying of lithium with the metallic species might provide additional reversible capacities. Both binary and ternary systems are reviewed and results are compared in the frame of the electrochemical application.

  3. 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....

  4. Helium trapping at erbium oxide precipitates in erbium hydride

    Energy Technology Data Exchange (ETDEWEB)

    Foiles, Stephen M. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Battaile, Corbett Chandler [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2016-02-01

    The formation of He bubbles in erbium tritides is a significant process in the aging of these materials. Due to the long-standing uncertainty about the initial nucleation process of these bubbles, there is interest in mechanisms that can lead to the localization of He in erbium hydrides. Previous work has been unable to identify nucleation sites in homogeneous erbium hydride. This work builds on the experimental observation that erbium hydrides have nano- scale erbium oxide precipitates due to the high thermodynamic stability of erbium oxide and the ubiquitous presence of oxygen during materials processing. Fundamental DFT calculations indicate that the He is energetically favored in the oxide relative to the bulk hydride. Activation energies for the motion of He in the oxide and at the oxide-hydride interface indicate that trapping is kinetically feasible. A simple kinetic Monte Carlo model is developed that demonstrates the degree of trapping of He as a function of temperature and oxide fraction.

  5. Photochromism of rare-earth metal-oxy-hydrides

    Science.gov (United States)

    Nafezarefi, F.; Schreuders, H.; Dam, B.; Cornelius, S.

    2017-09-01

    Recently, thin films of yttrium oxy-hydride (YOxHy) were reported to show an unusual color-neutral photochromic effect promising for application in smart windows. Our present work demonstrates that also oxy-hydrides based on Gd, Dy, and Er have photochromic properties and crystal structures similar to YOxHy. Compared to YOxHy, the optical bandgaps of the lanthanide based oxy-hydrides are smaller while photochromic contrast and kinetics show large variation among different cations. Based on these findings, we propose that cation alloying is a viable pathway to tailor the photochromic properties of oxy-hydride materials. Furthermore, we predict that the oxy-hydrides of the other lanthanides are also potentially photochromic.

  6. Metal hydrides for concentrating solar thermal power energy storage

    Science.gov (United States)

    Sheppard, D. A.; Paskevicius, M.; Humphries, T. D.; Felderhoff, M.; Capurso, G.; Bellosta von Colbe, J.; Dornheim, M.; Klassen, T.; Ward, P. A.; Teprovich, J. A.; Corgnale, C.; Zidan, R.; Grant, D. M.; Buckley, C. E.

    2016-04-01

    The development of alternative methods for thermal energy storage is important for improving the efficiency and decreasing the cost of concentrating solar thermal power. We focus on the underlying technology that allows metal hydrides to function as thermal energy storage (TES) systems and highlight the current state-of-the-art materials that can operate at temperatures as low as room temperature and as high as 1100 °C. The potential of metal hydrides for thermal storage is explored, while current knowledge gaps about hydride properties, such as hydride thermodynamics, intrinsic kinetics and cyclic stability, are identified. The engineering challenges associated with utilising metal hydrides for high-temperature TES are also addressed.

  7. Surface iron inhibits quartz-induced cytotoxic and inflammatory responses in alveolar macrophages.

    Science.gov (United States)

    Ghiazza, Mara; Scherbart, Agnes M; Fenoglio, Ivana; Grendene, Francesca; Turci, Francesco; Martra, Gianmario; Albrecht, Catrin; Schins, Roel P F; Fubini, Bice

    2011-01-14

    The mechanism of enhancement/inhibition of quartz toxicity induced by iron is still unclear. Here the amount of iron on a fibrogenic quartz (Qz) was increased by wet impregnation (Fe(NO(3))(3) 0.67 and 6.7 wt %). X-ray diffraction (XRD), XRF diffuse reflectance, UV-vis, and infrared (IR) spectroscopies revealed dispersed ferric ions, and hematite aggregates at the higher loading. Surface features relevant to pathogenicity and cell responses were compared not only to the original quartz but also to reference quartz DQ12. Surface charge (ζ-potential) was more negative on the original and low-loaded specimen than on the high-loaded one. DQ12 had a less negative ζ-potential than Qz, ascribed to the absence of aluminium present in Qz (1.7 wt %). All quartz specimens were able to generate HO(•) radicals, iron-loaded samples being more reactive than original quartz. Iron deposition inhibited the rupture of a C-H bond. All quartzes were phagocytized by alveolar macrophages (AMΦ cell line NR8383) to the same extent, irrespective of their surface state. Conversely, iron loading increased AMΦ viability (evaluated by cytotoxicity and induction of apoptosis). Qz was found to be much less cytotoxic than DQ12. The induction of oxidative stress and inflammatory responses (evaluated by HO-1 mRNA expression and TNF-α mRNA and protein expression) revealed a reduction in inflammogenicity upon iron loading and a more inflammogenic potency of DQ12 ascribed to undissociated SiOH interacting via H-bonding with cell membrane components. The results suggest that besides aluminium also iron at the quartz surface may have an inhibitory effect on adverse health responses.

  8. Estimating Quartz Reserves Using Compositional Kriging

    Directory of Open Access Journals (Sweden)

    J. Taboada

    2013-01-01

    Full Text Available The aim of this study was to determine spatial distribution and volume of four commercial quartz grades, namely, silicon metal, ferrosilicon, aggregate, and kaolin (depending on content in impurities in a quartz seam. The chemical and mineralogical composition of the reserves in the seam were determined from samples collected from outcrops, blasting operations, and exploratory drilling, and compositional kriging was used to calculate the volume and distribution of the reserves. A more accurate knowledge of the deposit ensures better mine planning, leading to higher profitability and an improved relationship with the environment.

  9. Results of NDE Technique Evaluation of Clad Hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Kunerth, Dennis C. [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2014-09-01

    This report fulfills the M4 milestone, M4FT-14IN0805023, Results of NDE Technique Evaluation of Clad Hydrides, under Work Package Number FT-14IN080502. During service, zirconium alloy fuel cladding will degrade via corrosion/oxidation. Hydrogen, a byproduct of the oxidation process, will be absorbed into the cladding and eventually form hydrides due to low hydrogen solubility limits. The hydride phase is detrimental to the mechanical properties of the cladding and therefore it is important to be able to detect and characterize the presence of this constituent within the cladding. Presently, hydrides are evaluated using destructive examination. If nondestructive evaluation techniques can be used to detect and characterize the hydrides, the potential exists to significantly increase test sample coverage while reducing evaluation time and cost. To demonstrate the viability this approach, an initial evaluation of eddy current and ultrasonic techniques were performed to demonstrate the basic ability to these techniques to detect hydrides or their effects on the microstructure. Conventional continuous wave eddy current techniques were applied to zirconium based cladding test samples thermally processed with hydrogen gas to promote the absorption of hydrogen and subsequent formation of hydrides. The results of the evaluation demonstrate that eddy current inspection approaches have the potential to detect both the physical damage induced by hydrides, e.g. blisters and cracking, as well as the combined effects of absorbed hydrogen and hydride precipitates on the electrical properties of the zirconium alloy. Similarly, measurements of ultrasonic wave velocities indicate changes in the elastic properties resulting from the combined effects of absorbed hydrogen and hydride precipitates as well as changes in geometry in regions of severe degradation. However, for both approaches, the signal responses intended to make the desired measurement incorporate a number of contributing

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

    Science.gov (United States)

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

    2014-09-01

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Rico, A., E-mail: alvaro.rico@urjc.es [DIMME, Departamento de Tecnología Mecánica, Universidad Rey Juan Carlos, c/Tulipán s/n, E-28933 Móstoles, Madrid (Spain); Martin-Rengel, M.A., E-mail: mamartin@mater.upm.es [Departamento de Ciencia de los Materiales, UPM, E.T.S.I. Caminos, Canales y Puertos, Profesor Aranguren SN, E-28040 Madrid (Spain); Ruiz-Hervias, J., E-mail: jesus.ruiz@upm.es [Departamento de Ciencia de los Materiales, UPM, E.T.S.I. Caminos, Canales y Puertos, Profesor Aranguren SN, E-28040 Madrid (Spain); Rodriguez, J. [DIMME, Departamento de Tecnología Mecánica, Universidad Rey Juan Carlos, c/Tulipán s/n, E-28933 Móstoles, Madrid (Spain); Gomez-Sanchez, F.J., E-mail: javier.gomez@amsimulation.com [Advanced Material Simulation, S.L, Madrid (Spain)

    2014-09-15

    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.

  12. Nanostructured Magnesium Hydride for Reversible Hydrogen Storage

    Science.gov (United States)

    de Rango, P.; Chaise, A.; Fruchart, D.; Miraglia, S.; Marty, Ph.

    2013-05-01

    The aim of this work was to develop suitable materials to store hydrogen in a solid state. A systematic investigation of the co-milling process of magnesium hydride with a transition metal was undertaken in order to produce nanostructured and highly reactive powders. The initiating role of the transition metal was evidenced by in situ neutron diffraction experiments. High performances in terms of thermal and mechanical behavior were achieved introducing expanded graphite and compacting the mixture to form composite materials. Absorption and desorption kinetics have been measured versus temperature and H2 pressure.

  13. Lithium hydride - A space age shielding material

    Science.gov (United States)

    Welch, F. H.

    1974-01-01

    Men and materials performing in the environment of an operating nuclear reactor require shielding from the escaping neutron particles and gamma rays. For efficient shielding from gamma rays, dense, high atomic number elements such as iron, lead, or tungsten are required, whereas light, low atomic number elements such as hydrogen, lithium, or beryllium are required for efficient neutron shielding. The use of lithium hydride (LiH) as a highly efficient neutron-shielding material is considered. It contains, combined into a single, stable compound, two of the elements most effective in attenuating and absorbing neutrons.

  14. Highly Concentrated Palladium Hydrides/Deuterides; Theory

    Energy Technology Data Exchange (ETDEWEB)

    Papaconstantopoulos, Dimitrios

    2013-11-26

    Accomplishments are reported in these areas: tight-binding molecular dynamics study of palladium; First-principles calculations and tight-binding molecular dynamics simulations of the palladium-hydrogen system; tight-binding studies of bulk properties and hydrogen vacancies in KBH{sub 4}; tight-binding study of boron structures; development of angular dependent potentials for Pd-H; and density functional and tight-binding calculations for the light-hydrides NaAlH4 and NaBH4

  15. Development of nickel-metal hydride cell

    Science.gov (United States)

    Kuwajima, Saburo; Kamimori, Nolimits; Nakatani, Kensuke; Yano, Yoshiaki

    1993-01-01

    National Space Development Agency of Japan (NASDA) has conducted the research and development (R&D) of battery cells for space use. A new R&D program about a Nickel-Metal Hydride (Ni-MH) cell for space use from this year, based on good results in evaluations of commercial Ni-MH cells in Tsukuba Space Center (TKSC), was started. The results of those commercial Ni-MH cell's evaluations and recent status about the development of Ni-MH cells for space use are described.

  16. Crack growth through the thickness of thin-sheet Hydrided Zircaloy-4

    Science.gov (United States)

    Raynaud, Patrick A. C.

    In recent years, the limits on fuel burnup have been increased to allow an increase in the amount of energy produced by a nuclear fuel assembly thus reducing waste volume and allowing greater capacity factors. As a result, it is paramount to ensure safety after longer reactor exposure times in the case of design-basis accidents, such as reactivity-initiated accidents (RIA). Previously proposed failure criteria do not directly address the particular cladding failure mechanism during a RIA, in which crack initiation in brittle outer-layers is immediately followed by crack growth through the thickness of the thin-wall tubing. In such a case, the fracture toughness of hydrided thin-wall cladding material must be known for the conditions of through-thickness crack growth in order to predict the failure of high-burnup cladding. The fracture toughness of hydrided Zircaloy-4 in the form of thin-sheet has been examined for the condition of through-thickness crack growth as a function of hydride content and distribution at 25°C, 300°C, and 375°C. To achieve this goal, an experimental procedure was developed in which a linear hydride blister formed across the width of a four-point bend specimen was used to inject a sharp crack that was subsequently extended by fatigue pre-cracking. The electrical potential drop method was used to monitor the crack length during fracture toughness testing, thus allowing for correlation of the load-displacement record with the crack length. Elastic-plastic fracture mechanics were used to interpret the experimental test results in terms of fracture toughness, and J-R crack growth resistance curves were generated. Finite element modeling was performed to adapt the classic theories of fracture mechanics applicable to thick-plate specimens to the case of through-thickness crack growth in thin-sheet materials, and to account for non-uniform crack fronts. Finally, the hydride microstructure was characterized in the vicinity of the crack tip by

  17. Data Acquisition System for Quartz Crystal Microbalances

    Directory of Open Access Journals (Sweden)

    Kleber Romero Felizardo

    2006-02-01

    Full Text Available This work presents a data acquisition system used in a mass sensor: quartz crystal microbalance. This system reads the frequency of this sensor along the time and sends the collected data to the computer through a serial interface.

  18. Bubble Formation in Silicon-Quartz Interface

    OpenAIRE

    Kakimoto, K.; EGUCHI, M.; Ozoe, H.

    1997-01-01

    Bubble formation at an interface between silicon melt and a quartz crucible was studied by thermodynamical calculation and visualization of bubble formation using X-ray radiography. A phase diagram of silicon-oxygen (Si-O) system is also calculated from the reported thermodynamical data. Critical temperature and radius of bubble formation at the interface was discussed.

  19. Time-resolved luminescence from quartz

    NARCIS (Netherlands)

    Chithambo, M.L.; Ankjærgaard, C.; Pagonis, V.

    2016-01-01

    Time-resolved optical stimulation of luminescence has become established as a key method for measurement of optically stimulated luminescence from quartz, feldspar and α-Al2O3:C, all materials of interest in dosimetry. The aim of time-resolved optical stimulation is to separ

  20. 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...

  1. From permanent magnets to rechargeable hydride electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Willems, J.J.G.; Buschow, K.H.J.

    1987-02-15

    A brief historical survey is given of how the study of coercitivity mechanisms in SmCo/sub 5/ permanent-magnet materials eventually led to the discovery of the favourable hydrogen sorption properties of the compound LaNi/sub 5/. It is shown how continued research by many investigators dealing with a variety of different physical and chemical properties has resulted in an advanced understanding of some of the principles that govern hydrogen absorption and which are responsible for the changes in physical properties that accompany it. The problems associated with various applications of LaNi/sub 5/-based hydrogen-storage materials are also briefly discussed. A large part of this paper is devoted to the applicability of LaNi/sub 5/-type materials in batteries. Research in this area has resulted in the development of a new type of rechargeable battery: the nickel-hydride cell. This battery can be charged and discharged at high rates and is relatively insensitive to overcharging and overdischarging. Special attention is given to the nature of the electrode degradation process and the effect of composition variations in LaNi/sub 5/-related materials on the lifetime of the corresponding hydride electrodes when subjected to severe electrochemical charge-discharge cycles.

  2. Metal hydrides for lithium-ion batteries.

    Science.gov (United States)

    Oumellal, Y; Rougier, A; Nazri, G A; Tarascon, J-M; Aymard, L

    2008-11-01

    Classical electrodes for Li-ion technology operate via an insertion/de-insertion process. Recently, conversion electrodes have shown the capability of greater capacity, but have so far suffered from a marked hysteresis in voltage between charge and discharge, leading to poor energy efficiency and voltages. Here, we present the electrochemical reactivity of MgH(2) with Li that constitutes the first use of a metal-hydride electrode for Li-ion batteries. The MgH(2) electrode shows a large, reversible capacity of 1,480 mAh g(-1) at an average voltage of 0.5 V versus Li(+)/Li(o) which is suitable for the negative electrode. In addition, it shows the lowest polarization for conversion electrodes. The electrochemical reaction results in formation of a composite containing Mg embedded in a LiH matrix, which on charging converts back to MgH(2). Furthermore, the reaction is not specific to MgH(2), as other metal or intermetallic hydrides show similar reactivity towards Li. Equally promising, the reaction produces nanosized Mg and MgH(2), which show enhanced hydrogen sorption/desorption kinetics. We hope that such findings can pave the way for designing nanoscale active metal elements with applications in hydrogen storage and lithium-ion batteries.

  3. Time scales of porphyry Cu deposit formation: insights from titanium diffusion in quartz

    Science.gov (United States)

    Mercer, Celestine N.; Reed, Mark H.; Mercer, Cameron M.

    2015-01-01

    Porphyry dikes and hydrothermal veins from the porphyry Cu-Mo deposit at Butte, Montana, contain multiple generations of quartz that are distinct in scanning electron microscope-cathodoluminescence (SEM-CL) images and in Ti concentrations. A comparison of microprobe trace element profiles and maps to SEM-CL images shows that the concentration of Ti in quartz correlates positively with CL brightness but Al, K, and Fe do not. After calibrating CL brightness in relation to Ti concentration, we use the brightness gradient between different quartz generations as a proxy for Ti gradients that we model to determine time scales of quartz formation and cooling. Model results indicate that time scales of porphyry magma residence are ~1,000s of years and time scales from porphyry quartz phenocryst rim formation to porphyry dike injection and cooling are ~10s of years. Time scales for the formation and cooling of various generations of hydrothermal vein quartz range from 10s to 10,000s of years. These time scales are considerably shorter than the ~0.6 m.y. overall time frame for each porphyry-style mineralization pulse determined from isotopic studies at Butte, Montana. Simple heat conduction models provide a temporal reference point to compare chemical diffusion time scales, and we find that they support short dike and vein formation time scales. We interpret these relatively short time scales to indicate that the Butte porphyry deposit formed by short-lived episodes of hydrofracturing, dike injection, and vein formation, each with discrete thermal pulses, which repeated over the ~3 m.y. generation of the deposit.

  4. Molecular rare-earth-metal hydrides in non-cyclopentadienyl environments.

    Science.gov (United States)

    Fegler, Waldemar; Venugopal, Ajay; Kramer, Mathias; Okuda, Jun

    2015-02-02

    Molecular hydrides of the rare-earth metals play an important role as homogeneous catalysts and as counterparts of solid-state interstitial hydrides. Structurally well-characterized non-metallocene-type hydride complexes allow the study of elementary reactions that occur at rare-earth-metal centers and of catalytic reactions involving bonds between rare-earth metals and hydrides. In addition to neutral hydrides, cationic derivatives have now become available.

  5. Identifying well-bleached quartz using the different bleaching rates of quartz and feldspar luminescence signals

    DEFF Research Database (Denmark)

    Murray, A.S.; Thomsen, Kristina Jørkov; Masuda, N.;

    2012-01-01

    When dating older sedimentary deposits using quartz, there are no unambiguous methods for identifying the presence of incomplete bleaching. Current statistical analysis of dose distributions depends entirely on the assumption that incomplete bleaching and mixing are the main causes of any excess...... in relative bleaching rates of quartz optically stimulated luminescence (OSL) and feldspar luminescence stimulated at 50 °C by infrared light (IR50) and feldspar luminescence stimulated at 290 °C by infrared light after a stimulation at 50 °C (pIRIR290), and use recently deposited samples to determine...... that the large aliquot data are more likely to be correct. We conclude that a comparison of quartz and feldspar doses provides a useful independent method for identifying well-bleached quartz samples, and that it is unwise to apply statistical models to dose distributions without clear evidence for the physical...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-14

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

  7. Determination of methylmercury in seafood by HPLC coupled with hydride generation and AFS%高效液相色谱原子荧光分光光度联用法测定海产品中的甲基汞含量

    Institute of Scientific and Technical Information of China (English)

    赵凯; 杨大进

    2011-01-01

    目的 建立高效液相色谱原子荧光分光光度法在线联用技术测定海产品中甲基汞的方法.方法 以25%氢氧化钾甲醇溶液水浴加热后超声提取样品,试液中的甲基汞与2-巯基乙醇结合.以5%甲醇溶液(含60 mmol/L乙酸铵和0.1%2-巯基乙醇)作流动相,经Supelco C18色谱柱(150 mm×4.6 mm,5μm)分离,紫外消解后经KBH4还原由原子荧光光度计进行测定.结果 甲基汞的检出限为0.7 μg/L(以汞计),样品测定的相对标准偏差小于4.6%,采用两种参考物质考查方法的准确性,以测定市售海产品中甲基汞含量.结论 本研究通过简化仪器装置,改进前处理步骤,有效地提高了方法的可靠性,该方法简便、快速、可靠,可用于海产品中甲基汞的含量测定.%Objective A high performance liquid chromatography ( HPLC ) coupled with hydride generation and atomic fluorescence spectrometry is proposed for the determination of methyl mercury in seafood. Methods Samples were extracted by 25% potassium hydroxide and the methylmercury-thiol complex was separated on a Supelco C18 (150 mm x 4.6 mm, 5μm) reverse phase column and online UV-digested. After reduced to element Hg by KBH4, the element Hg was selectively detected by AFS in an Ar/H2 flame under optimized conditions. Results The detection limit for methyl mercury was 0. 7μg/L ( as mercury) with a relative standard deviation ( RSD) of lower than 4. 6%. Two standard reference materials were applied for the accuracy of study. Conclusion The content of methylmercury in seafood can be determined by the method with good convenience, rapidity and reliability.

  8. Determination of inorganic arsenic in coal by hydride generation atomic fluorescence spectrometry combined with ultrasonic extraction%超声提取-顺序注射氢化物发生-原子荧光光谱法测定煤中无机砷

    Institute of Scientific and Technical Information of China (English)

    王长芹; 刘贵勤

    2011-01-01

    A determination method of inorganic arsemc in coal was established by sequence injection hydride generation-atomic fluorescence spectrometry ( HG-AFS) , after the ultrasonic extraction with 6 mol/L HCl as extraction reagent. The ultrasonic extraction conditions were optimized, including extraction reagent, time and temperature. Under the optimized experimental condition, arsemc in concentration range of 0. 20-100 μg/L showed linearity to the fluorescence intensity with correlation coefficient of 0. 999 7. The detection limit of arsenic was 0. 025 μg/L. The relative standard deviation (RSD) for 10 μg/L As was 0. 9 % (n=11). The proposed method has been applied to the analysis of coal fly ash component analysis certified reference material (GBW08401) and coal samples with recoveries of 95%-102 %, and the result of GBW08401 was consist with the certified value.%利用6 mol/L盐酸作为提取试剂,样品经超声提取后,用顺序注射氢化物发生-原子荧光光谱法测定煤中无机砷的含量.对超声提取条件(提取试剂浓度、时间、温度)进行了优化.在优化的实验条件下,砷的浓度在0.20~100μg/L范围内与荧光强度呈线性关系,相关系数为0.999 7,砷的检出限为0.025μg/L,对10 μg/L砷标准溶液进行重复11次测量,得出相对标准偏差(RSD)为0.9%.用该法对煤飞灰成分分析标准物质GBW08401和煤样进行分析,测得回收率在95%~102%之间,标准样品的测定值和认定值相符.

  9. 氢化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)%Direct Determination of Water-Soluble Antimony(Ⅲ) and Antimony(Ⅴ) in Soil by Hydride Generation Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    于兆水; 张勤

    2009-01-01

    在HCl介质中,Sb(Ⅲ)和Sb(Ⅴ)在氢化物发生过程中的化学反应效率不同,通过测定经还原剂还原后和还原前Sb的荧光强度,求解联立方程计算出Sb(Ⅲ)和Sb(Ⅴ)的含量,据此建立了氧化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)方法,操作简便,实用性强.考察了 HCl浓度和KBH_4浓度对Sb(Ⅲ)和Sb(Ⅴ)测定灵敏度的影响以及共存元素的干扰情况,并比较了丽种还原剂对Sb(Ⅴ)的还原效果.方法检出限为Sb(Ⅲ)1.11 ng·g~(-1),Sb(Ⅴ)1.57 ng·g~(-1).加标回收试验表明方法准确、可靠.%A simple, rapid and useful method for the determination of water-soluble antimony( Ⅲ ) and antimony(Ⅴ) in soil was established using hydride generation atomic fluorescence spectrometry. The method was based on the different chemical reaction efficiency between Sb( Ⅲ ) and Sb( Ⅴ ) with KBH_4 in the media of HCL The amounts of Sb( Ⅲ) and Sb( Ⅴ ) can be obtained through measuring antimony fluorescence intensities before and after reduction with reductant. The effects of HCI and KBH_4 on the sensitivities of Sb(Ⅲ) and Sb(Ⅴ) were investigated, and the interferences from coexistent elements were studied. The re-duction efficiencies of both reductants were compared. The detection limits of the method were 1.11 ng·g~(-1) for Sb( Ⅲ ) and 1.57 ng·g~(-1) for Sb( Ⅴ ). The accuracy of the method was verified by recovery experiments on spiked real soil samples.

  10. Filiform-mode hydride corrosion of uranium surfaces

    Science.gov (United States)

    Hill, M. A.; Schulze, R. K.; Bingert, J. F.; Field, R. D.; McCabe, R. J.; Papin, P. A.

    2013-11-01

    Hydride nucleation and growth has previously been studied in uranium with an air-formed oxide. Preferred directional growth of uranium hydride has not been observed, presumably due to the constraint of the oxide layer and/or the presence of a surface layer distorted by mechanical grinding and polishing. Instead, hydrides typically first form as subsurface blisters that do not exhibit preferred growth directionality. By eliminating the strained surface layer through electropolishing, removing the natural oxide through ion sputtering, avoiding exposure of the uranium to air, and then exposing uranium to high purity hydrogen in an environmental cell, hydride growth patterns emerge that correspond to defect structures within the microstructure. These hydride growth patterns are similar to filiform corrosion, a type of corrosion that frequently forms under thin protective films. This work describes the first reported observation of filiform-like corrosion in uranium. The uranium hydride initiates at defects, but grows into filaments up to 20 μm wide, and tends to form in straight lines, largely propagating along twin boundaries. Propagation is driven by hydrogen reaction at the filament head, promoted by more efficient delivery of reactant. However, this phenomenon does not involve an electrochemical process associated with conventional filiform corrosion and is therefore described as filiform-like. Hydride growth was observed using optical microscopy for a period of nearly three years. Sample characterization included automated electron backscatter diffraction (EBSD) measurements to determine growth directions. Observation of this anomalous hydride growth provides clues as to the mechanisms operating in uranium hydriding for more conventionally prepared sample surfaces.

  11. Triphosphine-Ligated Copper Hydrides for CO2 Hydrogenation: Structure, Reactivity, and Thermodynamic Studies.

    Science.gov (United States)

    Zall, Christopher M; Linehan, John C; Appel, Aaron M

    2016-08-10

    The copper(I) triphosphine complex LCu(MeCN)PF6 (L = 1,1,1-tris(diphenylphosphinomethyl)ethane), which we recently demonstrated is an active catalyst precursor for hydrogenation of CO2 to formate, reacts with H2 in the presence of a base to form a cationic dicopper hydride, [(LCu)2H]PF6. [(LCu)2H](+) is also an active precursor for catalytic CO2 hydrogenation, with equivalent activity to that of LCu(MeCN)(+), and therefore may be a relevant catalytic intermediate. The thermodynamic hydricity of [(LCu)2H](+) was determined to be 41.0 kcal/mol by measuring the equilibrium constant for this reaction using three different bases. [(LCu)2H](+) and the previously reported dimer (LCuH)2 can be synthesized by the reaction of LCu(MeCN)(+) with 0.5 and 1 equiv of KB(O(i)Pr)3H, respectively. The solid-state structure of [(LCu)2H](+) shows threefold symmetry about a linear Cu-H-Cu axis and significant steric strain imposed by bringing two LCu(+) units together around the small hydride ligand. [(LCu)2H](+) reacts stoichiometrically with CO2 to generate the formate complex LCuO2CH and the solvento complex LCu(MeCN)(+). The rate of the stoichiometric reaction between [(LCu)2H](+) and CO2 is dramatically increased in the presence of bases that coordinate strongly to the copper center, e.g. DBU and TMG. In the absence of CO2, the addition of a large excess of DBU to [(LCu)2H](+) results in an equilibrium that forms LCu(DBU)(+) and also presumably the mononuclear hydride LCuH, which is not directly observed. Due to the significantly enhanced CO2 reactivity of [(LCu)2H](+) under these catalytically relevant conditions, LCuH is proposed to be the catalytically active metal hydride.

  12. Technical and economic aspects of hydrogen storage in metal hydrides

    Science.gov (United States)

    Schmitt, R.

    1981-01-01

    The recovery of hydrogen from such metal hydrides as LiH, MgH2, TiH2, CaH2 and FeTiH compounds is studied, with the aim of evaluating the viability of the technique for the storage of hydrogen fuel. The pressure-temperature dependence of the reactions, enthalpies of formation, the kinetics of the hydrogen absorption and desorption, and the mechanical and chemical stability of the metal hydrides are taken into account in the evaluation. Economic aspects are considered. Development of portable metal hydride hydrogen storage reservoirs is also mentioned.

  13. PIE techniques for hydride reorientation test at NDC

    Energy Technology Data Exchange (ETDEWEB)

    Tsuda, Tomohiro; Shinohara, Yasunari; Yamaguchi, Yoichiro [Nuclear Development Corporation, Ibaraki (Japan)

    2008-11-15

    Dry storage of spent fuels in the interim storage facility is being planned in Japan. However, the gradual deterioration of the mechanical property of fuel cladding due to internal pressure and temperature during the storage term is known. Therefore, the integrity of stored fuel rods should be confirmed before the start of dry storage. For the last several years, NDC had a lot of experiences on the hydride reorientation test. The specimen preparation techniques on the hydride reorientation test and the mechanical testing techniques after the hydride reorientation are shown in this paper.

  14. 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.

  15. Millimeter And Submillimeter-Wave Integrated Circuits On Quartz

    Science.gov (United States)

    Mehdi, Imran; Mazed, Mohammad; Siegel, Peter; Smith, R. Peter

    1995-01-01

    Proposed Quartz substrate Upside-down Integrated Device (QUID) relies on UV-curable adhesive to bond semiconductor with quartz. Integrated circuits including planar GaAs Schottky diodes and passive circuit elements (such as bandpass filters) fabricated on quartz substrates. Circuits designed to operate as mixers in waveguide circuit at millimeter and submillimeter wavelengths. Integrated circuits mechanically more robust, larger, and easier to handle than planar Schottky diode chips. Quartz substrate more suitable for waveguide circuits than GaAs substrate.

  16. Fast, microscale-controlled weathering of rhyolitic obsidian to quartz and alunite

    Science.gov (United States)

    Cuadros, Javier; Afsin, Beytullah; Michalski, Joseph R.; Ardakani, Mahmoud

    2012-11-01

    Six-year experiments of volcanic glass reacting with waters of different chemistry (two freshwaters, seawater and brine) at ∼22 °C have produced the thorough transformation of mm-size glass chips into quartz, with minor alunite and calcite. These results contradict the current thinking about glass weathering and quartz formation. The reaction from glass to quartz took place at an estimated velocity ranging from 300-2000 times to 106 times faster than the accepted values for quartz precipitation, depending on how rates were assessed. The most likely process taking place is the rapid transformation of cation-depleted glass into quartz. In addition, alunite formed very efficiently from low-S glass (40±15 ppm). Such effective reaction in the absence of the accepted conditions for alunite formation is attributed to the high Al and K content combined with the generation of low pH conditions at the microscale. Local, low-pH conditions may arise due to proton-for-Na substitution at the earliest stage followed by liberation of the protons as glass later corroded. The surprising results show a new pathway of glass weathering and point towards reactions controlled by microscale conditions producing high activities locally. Such conditions may be common in the mineral-fluid interface with saline waters, immobile waters or systems with low water:rock ratios. The rapid precipitation of quartz at low temperature is relevant to the origin of quartz and the silica budget in a variety of sedimentary environments and prompts their reconsideration.

  17. The quartz crystal microbalance in soft matter research fundamentals and modeling

    CERN Document Server

    Johannsmann, Diethelm

    2014-01-01

    This book describes the physics of the second-generation quartz crystal microbalance (QCM), a fundamental method of analysis for soft matter at interfaces.From a device for measuring film thickness in vacuum, the quartz crystal microbalance (QCM) has in the past two decades evolved into a versatile instrument for analyzing soft matter at solid/liquid and solid/gas interfaces that found applications in diverse fields including the life sciences, material science, polymer research and electrochemistry. As a consequence of this success, the QCM is now being used by scientists with a wide variety

  18. ESR of E' centres in unstrained geological quartz grains

    Energy Technology Data Exchange (ETDEWEB)

    Bartoll, J. E-mail: jens.bartoll@charite.de; Schwarcz, H.P.; Rink, W.J

    2002-10-01

    E{sub 1}' centres are detectable by ESR spectroscopy in unstrained quartz extracted from weathered rock of Cretaceous age. These centres completely disappear when the samples are irradiated with an artificial {gamma}-dose of about 200 Gy. The concentration of E{sub 1}' centres thermally (re)generated at 310 deg. C can be reduced drastically under the influence of {gamma}-quanta, too. The {gamma}-radiation induces thermally unstable components in the quartz matrices that start to decay at around 100 deg. C.

  19. Emission polarization study on quartz and calcite.

    Science.gov (United States)

    Vincent, R. K.

    1972-01-01

    Calculation of the spectral emission polarization of quartz and calcite polished plates for observation angles of 20 and 70 deg by the substitution of complex index of refraction values for each mineral into Fresnel's equations. The emission polarization is shown to be quite wavelength-dependent, demonstrating that selected narrow or medium-width spectral bands exhibit a significantly higher percentage of polarization than a broad spectral band for these two minerals. Field measurements with a broadband infrared radiometer yield polarizations on the order of 2% for a coarse-grained granite rock and beach sand (both quartz-rich). This implies that a more sensitive detector with a selected medium-width filter may be capable of measuring emission polarization accurately enough to make this parameter useful as a remote sensing tool for discrimination among rocks on the basis of texture.

  20. Axiomatic Design of Micro Quartz Rate Sensor

    Institute of Scientific and Technical Information of China (English)

    SHI Yang-he; ZHANG Hong-hai; LIU Sheng

    2007-01-01

    Quartz rate sensors (QRS) made out of one single piece of quartz crystal are inertial devices which can be used for general rate control, stabilization, automotive and aerospace/defense markets,etc. The mechanical design of the QRS has been investigated based on axiomatic design. The axiomatic design matrix of the mechanical structure of Coriolis Vibratory Gyroscopes (CVG) has been proposed. The mechanical function of QRS is divided into three Function Requirements ( FR ) , i. e. , FR1 is the drive mode, FR2 is the sense mode, FR3 is a coupled connection where the Coriolis force can couple the two modes with a term proportional to the rotational rate. A new QRS which is easy to be fabricated has been put forward. Furthermore, the new QRS indicated that the axiomatic design is a help to functional design of products.

  1. Acute arsenious hydride intoxication. Four cases

    Energy Technology Data Exchange (ETDEWEB)

    Gosselin, B.; Mathieu, D.; Desprez-Nolf, M.; Cosson, A.; Goudemand, J.; Haguenoer, J.M.; Wattel, F.

    1982-02-06

    While engaged in the repair of a zinc furnace, 4 workers were accidentally exposed to arsenious hydride (AsH3) fumes. Acute intravascular haemolysis developed within a few hours. On admission, the patients immediately underwent exsanguino-transfusion; 8.2 to 10.2 l of blood were exchanged through a continuous perfusion pump at the rate of 1 l/hour. Two patients resumed diuresis during transfusion, but the other two required repeated haemodialysis. Between the 10th and 30th days, while renal function was gradually returning to normal, mildly megaloblastic anaemia developed. This was followed during the 3rd month by clinical and electric signs of polyneuritis of the lower and upper limbs, which subsequently regressed. Regular measurements of arsenic levels in the blood and urine were performed between and during exsanguino-transfusion and haemodialysis.

  2. Hydrogen desorption from nanostructured magnesium hydride composites

    Directory of Open Access Journals (Sweden)

    Brdarić Tanja P.

    2007-01-01

    Full Text Available The influence of 3d transition metal addition (Fe, Co and Ni on the desorption properties of magnesium hydride were studied. The ball milling of MgH2-3d metal blends was performed under Ar. Microstructural and morphological characterization were performed by XRD and SEM analysis, while the hydrogen desorption properties were investigated by DSC. The results show a strong correlation between the morphology and thermal stability of the composites. The complex desorption behavior (the existence of more than one desorption peak was correlated with the dispersion of the metal additive particles that appear to play the main role in the desorption. The desorption temperature can be reduced by more than 100 degrees if Fe is added as additive. The activation energy for H2 desorption from the MgH2-Fe composite is 120 kJ/mol, implying that diffusion controls the dehydration process.

  3. Spontaneous formation of GaN/AlN core-shell nanowires on sapphire by hydride vapor phase epitaxy

    Science.gov (United States)

    Trassoudaine, Agnès; Roche, Elissa; Bougerol, Catherine; André, Yamina; Avit, Geoffrey; Monier, Guillaume; Ramdani, Mohammed Réda; Gil, Evelyne; Castelluci, Dominique; Dubrovskii, Vladimir G.

    2016-11-01

    Spontaneous GaN/AlN core-shell nanowires with high crystal quality were synthesized on sapphire substrates by vapor-liquid-solid hydride vapor phase epitaxy (VLS-HVPE) without any voluntary aluminum source. Deposition of aluminum is difficult to achieve in this growth technique which uses metal-chloride gaseous precursors: the strong interaction between the AlCl gaseous molecules and the quartz reactor yields a huge parasitic nucleation on the walls of the reactor upstream the substrate. We open up an innovative method to produce GaN/AlN structures by HVPE, thanks to aluminum etching from the sapphire substrate followed by redeposition onto the sidewalls of the GaN core. The paper presents the structural characterization of GaN/AlN core-shell nanowires, speculates on the growth mechanism and discusses a model which describes this unexpected behavior.

  4. The CMS forward calorimeter with quartz fibres

    CERN Multimedia

    Laurent Guiraud

    1999-01-01

    Part of the forward hadron calorimeter for the CMS experiment at the LHC is seen here. The calorimeter will be placed at the ends of the experiment barrel to measure the energy of particles produced in the 14 TeV proton-proton collisions. In consists of an iron absorber and specially designed radiation-hard quartz so that it survives the high radiation levels produced by collisions.

  5. THE FRICTION OF QUARTZ IN HIGH VACUUM

    Science.gov (United States)

    the effects of surface cleanliness . Ultra-high vacuums (to 10 to the minus 10th power torr) and high temperatures (to 350 deg C) were combined with...chemical cleaning and careful handling techniques to produce the maximum surface cleanliness . The coefficient of static friction under varying...on 30-40 mesh glass balls. The coefficient of friction of smooth quartz was found to vary from 0.1 to 1.0 depending on the surface cleanliness . The

  6. Review of magnesium hydride-based materials: development and optimisation

    NARCIS (Netherlands)

    Crivello, J. -C.; Dam, B.; Denys, R. V.; Dornheim, M.; Grant, D. M.; Huot, J.; Jensen, T. R.; de Jongh, P.|info:eu-repo/dai/nl/186125372; Latroche, M.; Milanese, C.; Milcius, D.; Walker, G. S.; Webb, C. J.; Zlotea, C.; Yartys, V. A.

    Magnesium hydride has been studied extensively for applications as a hydrogen storage material owing to the favourable cost and high gravimetric and volumetric hydrogen densities. However, its high enthalpy of decomposition necessitates high working temperatures for hydrogen desorption while the

  7. Direct observation of hydrides formation in cavity-grade niobium

    Directory of Open Access Journals (Sweden)

    F. Barkov

    2012-12-01

    Full Text Available Niobium is an important technological superconductor used to make radio frequency cavities for particle accelerators. Using laser confocal microscopy we have directly investigated hydride precipitates formation in cavity-grade niobium at 77 and 140 K. We have found that large hydrides were usually formed after chemical or mechanical treatments, which are known to lead to a strong degradation of the quality factor known as Q disease. From our experiments we can conclude that hydrides causing Q disease are islands with a characteristic thickness of ≳100  nm and in-plane dimensions 1–10  μm. Our results show that mechanical polishing uploads a lot of hydrogen into bulk niobium while electropolishing leads to a mild contamination. Vacuum treatments at 600–800°C are demonstrated to preclude large hydride formation in line with the absence of Q disease in similarly treated cavities.

  8. Materials science of Mg-Ni-based new hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Orimo, S.; Fujii, H. [Hiroshima Univ. (Japan). Faculty of Integrated Arts and Sciences

    2001-02-01

    One of the advantageous functional properties of Mg alloys (or compounds) is to exhibit the reversible hydriding reaction. In this paper, we present our systematic studies regarding the relationship between nanometer- or atomistic-scale structures and the specific hydriding properties of the Mg-Ni binary system, such as(1) nanostructured (n)-Mg{sub 2}Ni, (2) a mixture of n-Mg{sub 2}Ni and amorphous (a)-MgNi,(3) pure a-MgNi, and(4) n-MgNi{sub 2}. Further studies on(5) an a-MgNi-based system for clarifying the effect of the short-range ordering on the structural and hydriding properties and(6) a MgNi{sub 2}-based system for synthesizing the new Laves phase structure are also presented. The materials science of Mg-Ni-based new hydrides will provide indispensable knowledge for practically developing the Mg alloys as hydrogen-storage materials. (orig.)

  9. Structure and bonding of second-row hydrides

    OpenAIRE

    Blinder, S. M.

    2014-01-01

    The atomic orbitals, hybridization and chemical bonding of the most common hydrides of boron, carbon, nitrogen and oxygen are described. This can be very instructive for beginning students in chemistry and chemical physics.

  10. Artificial exomuscle investigations for applications--metal hydride.

    Science.gov (United States)

    Crevier, Marie-Charlotte; Richard, Martin; Rittenhouse, D Matheson; Roy, Pierre-Olivier; Bédard, Stéphane

    2007-03-01

    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.

  11. DETERMINATION OF METAL HYDRIDE SYSTEMS CHARACTERISTICS WHILE HEATING

    Directory of Open Access Journals (Sweden)

    Yu. Kluchka

    2012-01-01

    Full Text Available Experimental dependence of the pressure of hydrogen in the hydride cartridge when it is heated is obtained. Experimental data prove the theoretical values with an accuracy of ≈ 6%.

  12. Bipolar Nickel-Metal Hydride Battery Being Developed

    Science.gov (United States)

    Manzo, Michelle A.

    1998-01-01

    The NASA Lewis Research Center has contracted with Electro Energy, Inc., to develop a bipolar nickel-metal hydride battery design for energy storage on low-Earth-orbit satellites. The objective of the bipolar nickel-metal hydride battery development program is to approach advanced battery development from a systems level while incorporating technology advances from the lightweight nickel electrode field, hydride development, and design developments from nickel-hydrogen systems. This will result in a low-volume, simplified, less-expensive battery system that is ideal for small spacecraft applications. The goals of the program are to develop a 1-kilowatt, 28-volt (V), bipolar nickel-metal hydride battery with a specific energy of 100 watt-hours per kilogram (W-hr/kg), an energy density of 250 W-hr/liter and a 5-year life in low Earth orbit at 40-percent depth-of-discharge.

  13. High-pressure synthesis of noble metal hydrides.

    Science.gov (United States)

    Donnerer, Christian; Scheler, Thomas; Gregoryanz, Eugene

    2013-04-07

    The formation of hydride phases in the noble metals copper, silver, and gold was investigated by in situ x-ray diffraction at high hydrogen pressures. In the case of copper, a novel hexagonal hydride phase, Cu2H, was synthesised at pressures above 18.6 GPa. This compound exhibits an anti-CdI2-type structure, where hydrogen atoms occupy every second layer of octahedral interstitial sites. In contrast to chemically produced CuH, this phase does not show a change in compressibility compared to pure copper. Furthermore, repeated compression (after decomposition of Cu2H) led to the formation of cubic copper hydride at 12.5 GPa, a phenomenon attributed to an alteration of the microstructure during dehydrogenation. No hydrides of silver (up to 87 GPa) or gold (up to 113 GPa) were found at both room and high temperatures.

  14. Artificial exomuscle investigations for applications-metal hydride

    Energy Technology Data Exchange (ETDEWEB)

    Crevier, Marie-Charlotte; Richard, Martin; Rittenhouse, D Matheson; Roy, Pierre-Olivier; Bedard, Stephane [Victhom Human Bionics Inc., Saint-Augustin-de-Desmaures, QC (Canada)

    2007-03-01

    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)

  15. Out-of-pile accelerated hydriding of Zircaloy fasteners

    Energy Technology Data Exchange (ETDEWEB)

    Clayton, J.C.

    1979-10-01

    Mechanical joints between Zircaloy and nickel-bearing alloys, mainly the Zircaloy-4/Inconel-600 combination, were exposed to water at 450/sup 0/F and 520/sup 0/F to study hydriding of Zircaloy in contact with a dissimilar metal. Accelerated hydriding of the Zircaloy occurred at both temperatures. At 450/sup 0/F the dissolved hydrogen level of the water was over ten times that at 520/sup 0/F. At 520/sup 0/F the initially high hydrogen ingress rate decreased rapidly as exposure time increased and was effectively shut off in about 25 days. Severely hydrided Zircaloy components successfully withstood thermal cycling and mechanical testing. Chromium plating of the nickel-bearing parts was found to be an effective and practical barrier in preventing nickel-alloy smearing and accelerated hydriding of Zircaloy.

  16. 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.

  17. Force chain forming quartz in an ultramylonite

    Science.gov (United States)

    Kilian, Rüdiger; Morales, Luiz F. G.; Peters, Max

    2014-05-01

    Polymineralic ultramylonites often show microstructures indicative of grain size sensitive creep with dissolution precipitation or diffusion accommodated grain boundary sliding. Typically phases show an anticorrelated distribution, the grain size is small and a crystallographic preferred orientation is absent. The latter observation is usually thought to originate from rigid body rotation of grains because flow dominated by diffusion creep operates at differential stresses, which are too low to activate crystal-plastic mechanisms. Here, we present quartz texture measurements from a natural ultramylonite, deformed under upper amphibolite facies conditions from the Nordmannvik Nappe, Upper Allochton of the Norwegian Caledonides. The ultramylonite has a mean grain size crystal-plastic processes. Alternative texture forming processes (e.g. growth textures) are also discussed. The texture in the foliation parallel clusters is thought to be an inherited texture from lower strain stages in the ultramylonite, as it is mostly present in the least deformed parts of the ultramylonite. However, we suggest that the texture formed in the foliation oblique clusters is related to a dynamic formation of force chains between quartz grains, where differential stresses become high enough for plastic yielding. The presence of force chains questions whether ultramylonites necessarily need to possess a linear viscous rheology, even if microstructures would indicate a diffusion creep mechanism. Pennacchioni G., Menegon L., Leiss B., Nestola F., Bromiley G., 2010: Development of crystallographic preferred orientation and microstructure during plastic deformation of natural coarse?grained quartz veins. Journal of Geophysical Research, Vol. 115, B12405

  18. Autocrine abscisic acid plays a key role in quartz-induced macrophage activation.

    Science.gov (United States)

    Magnone, Mirko; Sturla, Laura; Jacchetti, Emanuela; Scarfì, Sonia; Bruzzone, Santina; Usai, Cesare; Guida, Lucrezia; Salis, Annalisa; Damonte, Gianluca; De Flora, Antonio; Zocchi, Elena

    2012-03-01

    Inhalation of quartz induces silicosis, a lung disease where alveolar macrophages release inflammatory mediators, including prostaglandin-E(2) (PGE(2)) and tumor necrosis factor α (TNF-α). Here we report the pivotal role of abscisic acid (ABA), a recently discovered human inflammatory hormone, in silica-induced activation of murine RAW264.7 macrophages and of rat alveolar macrophages (AMs). Stimulation of both RAW264.7 cells and AMs with quartz induced a significant increase of ABA release (5- and 10-fold, respectively), compared to untreated cells. In RAW264.7 cells, autocrine ABA released after quartz stimulation sequentially activates the plasma membrane receptor LANCL2 and NADPH oxidase, generating a Ca(2+) influx resulting in NFκ B nuclear translocation and PGE(2) and TNF-α release (3-, 2-, and 3.5-fold increase, respectively, compared to control, unstimulated cells). Quartz-stimulated RAW264.7 cells silenced for LANCL2 or preincubated with a monoclonal antibody against ABA show an almost complete inhibition of NFκ B nuclear translocation and PGE(2) and TNF-α release compared to controls electroporated with a scramble oligonucleotide or preincubated with an unrelated antibody. AMs showed similar early and late ABA-induced responses as RAW264.7 cells. These findings identify ABA and LANCL2 as key mediators in quartz-induced inflammation, providing possible new targets for antisilicotic therapy.

  19. Radiation on luminescent properties of quartz glasses and fiber light pipes

    CERN Document Server

    Abdurakhmanov, B S; Gulamova, R R; Alimov, R; Yuldashev, B S; Ashurov, M K; Rustamov, I R

    2002-01-01

    Paper contains the results of investigation into X-ray luminescence of KI and KU-1 quartz glasses and of various composition and size quartz fiber light pipes (FLP) gamma-irradiated within 10 sup 2 -10 sup 7 Gy dose range. On the basis of analysis of X-ray luminescence spectra of glasses and FLP and comparison of the experimental data one detected in spectra two luminescence bands within 410, 450-470 nm range. One determined dose dependences of X-ray luminescence intensity of every of these bands of luminescence and hypothesized about the nature of the relevant centers. The protective role of OH-groups in the process of radiation-induced generation of luminescence centres under gamma-irradiation of quartz glasses and FLP was confirmed experimentally

  20. Finishing of AT-cut quartz crystal wafer with nanometric thickness uniformity by pulse-modulated atmospheric pressure plasma etching.

    Science.gov (United States)

    Yamamura, Kazuya; Ueda, Masaki; Shibahara, Masafumi; Zettsu, Nobuyuki

    2011-04-01

    Quartz resonator is a very important device to generate a clock frequency for information and telecommunication system. Improvement of the productivity of the quartz resonator is always required because a huge amount of the resonator is demanded for installing to various electronic devices. Resonance frequency of the quartz resonator is decided by the thickness of the quartz crystal wafer. Therefore, it is necessary to uniform the thickness distribution of the wafer with nanometric level. We have proposed the improvement technique of the thickness distribution of the quartz crystal wafer by numerically controlled correction using atmospheric pressure plasma which is non-contact and chemical removal technique. Heating effects of the quartz wafer in the removal rate and the correction accuracy were investigated. The heating of the substrate and compensate of the scanning speed of the worktable according to the variation of the surface temperature enabled an increase of 50% in the etching rate and 10-nanometric-level accuracy in the correction of the thickness distribution of the quartz wafer, respectively.

  1. 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.

  2. Ab-Initio Study of the Group 2 Hydride Anions

    Science.gov (United States)

    Harris, Joe P.; Wright, Timothy G.; Manship, Daniel R.

    2013-06-01

    The beryllium hydride (BeH)- dimer has recently been shown to be surprisingly strongly bound, with an electronic structure which is highly dependent on internuclear separation. At the equilibrium distance, the negative charge is to be found on the beryllium atom, despite the higher electronegativity of the hydrogen. The current study expands this investigation to the other Group 2 hydrides, and attempts to explain these effects. M. Verdicchio, G. L. Bendazzoli, S. Evangelisti, T. Leininger J. Phys. Chem. A, 117, 192, (2013)

  3. Suppression of the critical temperature in binary vanadium hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Dolan, M.D., E-mail: michael.dolan@csiro.au [CSIRO Energy Technology, 1 Technology Court, Pullenvale, QLD 4069 (Australia); McLennan, K.G. [CSIRO Energy Technology, 1 Technology Court, Pullenvale, QLD 4069 (Australia); Chandra, D. [Department of Chemical and Materials Engineering, University of Nevada, Reno, Reno, NV 89557 (United States); Kochanek, M.A. [CSIRO Energy Technology, 1 Technology Court, Pullenvale, QLD 4069 (Australia); Song, G. [CSIRO Process Science and Engineering, Gate 4, Normanby Rd, Clayton, VIC 3168 (Australia)

    2014-02-15

    Highlights: • Addition of 10 mol% Cr to V increases the β-hydride T{sub C} to >200 °C. • Addition of 10 mol% Ni to V increases the β-hydride T{sub C} to >400 °C. • Addition of 10 mol% Al to V decreases the β-hydride T{sub C} to <30 °C. • V{sub 90}Al{sub 10} membrane can be cycled to <30 °C under H{sub 2} without β-hydride formation. -- Abstract: The tendency of vanadium-based alloy membranes to embrittle is the biggest commercialisation barrier for this hydrogen separation technology. Excessive hydrogen absorption and the α → β hydride transition both contribute to brittle failure of these membranes. Alloying is known to reduce absorption, but the influence of alloying on hydride phase formation under conditions relevant to membrane operation has not been studied in great detail previously. Here, the effect of Cr, Ni, and Al alloying additions on V–H phase equilibrium has been studied using hydrogen absorption measurements and in situ X-ray diffraction studies. The addition of 10 mol% Ni increases the critical temperature for α + β hydride formation to greater than 400 °C, compared to 170 °C for V. Cr also increases the critical temperature, to between 200 and 300 °C. The addition of 10 mol% Al, however, suppresses the critical temperature to less than 30 °C, thereby enabling this material to be cycled thermally and hydrostatically while precluding formation of the β-hydride phase. This is despite Al also decreasing hydrogen absorption. The implication of this finding is that one of the mechanisms of brittle failure in vanadium-based hydrogen-selective membranes has been eliminated, thereby increasing the robustness of this material relative to V.

  4. Method of selective reduction of polyhalosilanes with alkyltin hydrides

    Science.gov (United States)

    Sharp, Kenneth G.; D'Errico, John J.

    1989-01-01

    The invention relates to the selective and stepwise reduction of polyhalosilanes by reacting at room temperature or below with alkyltin hydrides without the use of free radical intermediates. Alkyltin hydrides selectively and stepwise reduce the Si--Br, Si--Cl, or Si--I bonds while leaving intact any Si--F bonds. When two or more different halogens are present on the polyhalosilane, the halogen with the highest atomic weight is preferentially reduced.

  5. Method of selective reduction of halodisilanes with alkyltin hydrides

    Science.gov (United States)

    D'Errico, John J.; Sharp, Kenneth G.

    1989-01-01

    The invention relates to the selective and sequential reduction of halodisilanes by reacting these compounds at room temperature or below with trialkyltin hydrides or dialkyltin dihydrides without the use of free radical intermediates. The alkyltin hydrides selectively and sequentially reduce the Si-Cl, Si-Br or Si-I bonds while leaving intact the Si-Si and Si-F bonds present.

  6. Electronic structure and optical properties of lightweight metal hydrides

    NARCIS (Netherlands)

    Setten, van M.J.; Popa, V.A.; Wijs, de G.A.; Brocks, G.

    2007-01-01

    We study the dielectric functions of the series of simple hydrides LiH, NaH, MgH2, and AlH3, and of the complex hydrides Li3AlH6, Na3AlH6, LiAlH4, NaAlH4, and Mg(AlH4)2, using first-principles density-functional theory and GW calculations. All compounds are large gap insulators with GW single-partic

  7. Optimization of Hydride Rim Formation in Unirradiated Zr 4 Cladding

    Energy Technology Data Exchange (ETDEWEB)

    Shimskey, Rick W.; Hanson, Brady D.; MacFarlan, Paul J.

    2013-09-30

    The purpose of this work is to build on the results reported in the M2 milestone M2FT 13PN0805051, document number FCRD-USED-2013-000151 (Hanson, 2013). In that work, it was demonstrated that unirradiated samples of zircaloy-4 cladding could be pre-hydrided at temperatures below 400°C in pure hydrogen gas and that the growth of hydrides on the surface could be controlled by changing the surface condition of the samples and form a desired hydride rim on the outside diameter of the cladding. The work performed at Pacific Northwest National Laboratory since the issuing of the M2 milestone has focused its efforts to optimize the formation of a hydride rim on available zircaloy-4 cladding samples by controlling temperature variation and gas flow control during pre-hydriding treatments. Surface conditioning of the outside surface was also examined as a variable. The results of test indicate that much of the variability in the hydride thickness is due to temperature variation occurring in the furnaces as well as how hydrogen gas flows across the sample surface. Efforts to examine other alloys, gas concentrations, and different surface conditioning plan to be pursed in the next FY as more cladding samples become available

  8. Mechanochemical synthesis of nanostructured chemical hydrides in hydrogen alloying mills

    Energy Technology Data Exchange (ETDEWEB)

    Wronski, Z. [CANMET' s Materials Technology Laboratory, Natural Resources Canada, Ottawa (Canada) and Department of Mechanical Engineering, University of Waterloo, Waterloo, Ont., Canada N2L 3G1 (Canada)]. E-mail: zwronski@nrcan.gc.ca; Varin, R.A. [Department of Mechanical Engineering, University of Waterloo, Waterloo, Ont., Canada N2L 3G1 (Canada); Chiu, C. [Department of Mechanical Engineering, University of Waterloo, Waterloo, Ont., Canada N2L 3G1 (Canada); Czujko, T. [Department of Mechanical Engineering, University of Waterloo, Waterloo, Ont., Canada N2L 3G1 (Canada); Calka, A. [Department of Materials Science and Engineering, University of Wollongong, NSW 2518 (Australia)

    2007-05-31

    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{sub 2}FeH{sub 6} in a mixture with nanometric Fe particles. The mixture of complex magnesium-iron hydride and nano-iron released 3-4 wt.%H{sub 2} in a thermally programmed desorption experiment at the range 285-295 {sup o}C. Milling of the Mg-2Al powder mixture revealed a strong competition between formation of the Al(Mg) solid solution and the {beta}-MgH{sub 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{sub 2} in the temperature range 329-340 {sup o}C in the differential scanning calorimetry experiment. The formation of MgH{sub 2} was suppressed in the Mg-B system; instead, a hydrogenated amorphous phase (Mg,B)H {sub x}, was formed in a mixture with nanometric MgB{sub 2}. Annealing of the hydrogen-stabilized amorphous mixture produced crystalline MgB{sub 2}.

  9. Novel fuel cell stack with coupled metal hydride containers

    Science.gov (United States)

    Liu, Zhixiang; Li, Yan; Bu, Qingyuan; Guzy, Christopher J.; Li, Qi; Chen, Weirong; Wang, Cheng

    2016-10-01

    Air-cooled, self-humidifying hydrogen fuel cells are often used for backup and portable power sources, with a metal hydride used as the hydrogen storage material. To provide a stable hydrogen flow to the fuel cell stack, heat must be provided to the metal hydride. Conventionally, the heat released from the exothermic reaction of hydrogen and oxygen in the fuel cell stack to the exhaust air is used to heat a separate metal hydride container. In this case, the heat is only partially used instead of being more closely coupled because of the heat transfer resistances in the system. To achieve better heat integration, a novel scheme is proposed whereby hydrogen storage and single fuel cells are more closely coupled. Based on this idea, metal hydride containers in the form of cooling plates were assembled between each pair of cells in the stack so that the heat could be directly transferred to a metal hydride container of much larger surface-to-volume ratio than conventional separate containers. A heat coupled fuel cell portable power source with 10 cells and 11 metal hydride containers was constructed and the experimental results show that this scheme is beneficial for the heat management of fuel cell stack.

  10. 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.

  11. 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.

  12. Generations.

    Science.gov (United States)

    Chambers, David W

    2005-01-01

    Groups naturally promote their strengths and prefer values and rules that give them an identity and an advantage. This shows up as generational tensions across cohorts who share common experiences, including common elders. Dramatic cultural events in America since 1925 can help create an understanding of the differing value structures of the Silents, the Boomers, Gen Xers, and the Millennials. Differences in how these generations see motivation and values, fundamental reality, relations with others, and work are presented, as are some applications of these differences to the dental profession.

  13. Metallographic and fractographic observations of hydrides during delayed hydride cracking in Zr-2.5% Nb alloy

    Energy Technology Data Exchange (ETDEWEB)

    Jovanovic, M.T.; Eadie, R.L. [Univ. of Alberta, Edmonton, Alberta (Canada). Dept. of Chemical and Materials Engineering; Shek, G.K.; Seahra, H. [Ontario Hydro Technologies, Toronto, Ontario (Canada)

    1998-01-01

    Potential drop measurements, optical microscopy, and scanning electron microscopy were performed to study the mechanism of delayed hydride cracking (DHC), the relation of the fracture to the hydride morphology, and the fractography of the DHC mechanism. The material used in this study was taken from modified extrusions of the material used to manufacture Zr-2.5% Nb pressure tubes. The material was electrolytically hydrided to approximately 60 {micro}g/g before testing. Cracking tests were carried out at 250 C with an applied K{sub 1} of 12 MPa {radical}m. The number of potential jumps was strongly correlated to the number of striations on the fracture surface. The results indicate that the DHC process occurs in these samples in an intermittent fashion. Brittle fracture is the operating fracture mechanism for the hydrides that cover most of the fracture surface, but there are some regions of ductile fracture both within the fracture and at the striations.

  14. Determination of Water Soluble As ( Ⅲ ) and As ( Ⅴ ) in Soil by Hydride Generation-Atomic Fluorescence Spectrometry%氢化物发生-原子荧光光谱法测定土壤中水溶态砷(Ⅲ)和砷(Ⅴ)

    Institute of Scientific and Technical Information of China (English)

    于兆水; 张勤; 刘玲

    2012-01-01

    以氢气发生器为氩-氢火焰提供纯净、稳定的氢气,原子荧光光谱法测定土壤中水溶态和可交换态Sb(Ⅲ)和Sb(Ⅴ)已有应用,本研究进一步将此方法用于测定土壤样品中的As(Ⅲ)和As(Ⅴ).在0.3mol/L NaH2PO4 - Na2HPO4缓冲液中,采用氢化物发生-原子荧光光谱法测定土壤中水溶态As(Ⅲ)和总砷的含量,通过差减法计算As(Ⅴ)的含量.实验考察了0.02~0.4 mol/L NaH2PO4 - Na2 HPO4对As(Ⅲ)和As(Ⅴ)测定的影响,结果表明0.3 mol/L NaH2PO4 - Na2HPO4可以有效掩蔽As(Ⅴ).As(Ⅲ)的检出限为2.92 ng/g,总砷的检出限为2.35 ng/g;As(Ⅲ)和As(Ⅴ)的加标回收率分别为96% ~ 104%和101% ~103%.本方法不再依靠化学反应产生氢气来点燃并维持氩氢火焰,可在发生氢化反应的任何介质中测定砷,且不需要考虑酸度问题.方法操作简便,准确度高,能满足大批量样品分析要求.%Based on the determination method of Sb ( HI) and Sb ( V ) in soil, a method for the determination of water soluble As ( M ) and total arsenic in soil has been established by using Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS) in the media of 0. 3 mol/L NaH2PO4-Na2HPO4. An amount of As( V ) was obtained by subtracting As( HI ) from total arsenic. The hydrogen was provided from a hydrogen generator instead of chemical reaction to ignite a H2-Ar flame. Therefore, arsenic in any media was measurable since the arsenic was reduced into AsH3. Effects on the determination of As ( M ) and As ( V ) were investigated for concentrations of NaH2PO4-Na2HPO4 from 0. 02 mol/L to 0. 4 mol/L. The results show As( V ) can be screened by 0. 3 mol/L NaH2PO4-Na2HPO4. The detection limits were 2. 92 ng/g for As( HJ ) and 2. 35 ng/g for total As. The recoveries of As( HI) and As( V ) are 96% - 104% and 101% - 103% , respectively. The method was simple and highly accurate, meeting the requirements for multiple sample analysis.

  15. Luminescence sensitivity changes in quartz as a result of annealing

    DEFF Research Database (Denmark)

    Bøtter-Jensen, L.; Agersnap Larsen, N.; Mejdahl, V.

    1995-01-01

    Retrospective dosimetry using optically stimulated luminescence (OSL) on quartz extracted from (for example) bricks needs to account for strong OSL sensitivity changes that are known to occur depending on the previous thermal treatment of the sample. Non-heated quartz exhibits OSL orders of magni......Retrospective dosimetry using optically stimulated luminescence (OSL) on quartz extracted from (for example) bricks needs to account for strong OSL sensitivity changes that are known to occur depending on the previous thermal treatment of the sample. Non-heated quartz exhibits OSL orders...... of magnitude less per unit radiation than that for heated material. The reason these temperature-induced sensitivity changes occur in quartz is presently not well understood. This phenomenon is also seen in the related area of luminescence dating in which sedimentary quartz and quartz from heated...

  16. Effects of citric acid on separation of sillimanite from quartz

    Institute of Scientific and Technical Information of China (English)

    李晔; 雷东升; 鲁巍; 许时

    2002-01-01

    Quartz is the main gangue mineral of sillimanite. The results show that Al3+ and Fe3+ ion can activate the floatation of quartz and make the separation of quartz and sillimanite difficult when anion collector is used, and citric acid can inhibit the quartz activated by metallic ion and have slight influence on the sillimanite. X-ray photoelectronic energy spectrum analysis indicates that there are obvious electronic energy peaks on the surface of the quartz before citric acid is added into the ore pulp in presence of Al3+ and Fe3+, and after citric acid is added, the energy peak vanished. So citric acid can make Al3+ and Fe3+ on the surface of quartz solve and decrease the active points on the surface of quartz which can adsorb anion collector.

  17. Amorphization of α-Quartz under Irradiation

    Science.gov (United States)

    Douillard, L.; Duraud, J. P.

    1996-12-01

    The course of radiation induced damage produced in α-quartz by neutrons, ions, electrons or photons — commonly known as metamictization — has been re-analyzed by careful comparison of available experimental data. Specific interest was devoted to confront experimental metamict state features with current structural models. It comes out that the metamict state of irradiated quartz should exhibit some structural characteristics of the modulated structure proposed for vitreous silica. The metamictization process is consistent with a structural relaxation process of a highly defective quartz matrix. According to this new point defect analysis, structural relaxation should be triggered by a critical concentration of oxygen vacancy point defects likely to significantly lower the connectivity of the SiO{2} network. Various experimental results are interpreted by incorporating the influence of the SiO{2} crystalline polymorph and the influence of the nature of the irradiating particle to the point defect model. Nous avons étudié les modifications de propriétés et de structures de monocristaux de quartz α, consécutives à une irradiation sévère par des neutrons, des ions, des électrons ou des photons. Ce phénomène d'altération du quartz sous irradiation porte le nom de métamictisation. Notre travail exploite les recoupements de travaux antérieurs. Une attention particulière a été portée à la confrontation entre les données structurales expérimentales disponibles sur l'état métamicte du quartz et les modèles structuraux proposés. L'état métamicte du quartz présente ainsi les caractéristiques structurales du modèle de structure modulée, avancé pour décrire la structure de la silice thermique. Le mécanisme de métamictisation procéderait par relaxation de la matrice cristalline fortement endommagée. Ce phénomène de relaxation serait initié par l'apparition de concentration critique de défauts ponctuels de type lacunes d

  18. An enhanced microfluidic control system for improving power density of a hydride-based micro fuel cell

    Energy Technology Data Exchange (ETDEWEB)

    Moghaddam, Saeed; Shannon, Mark [Mechanical Science and Engineering, 1206 West Green St., University of Illinois, Urbana, IL 61801 (United States); Chemical and Biomolecular Engineering, 213 Roger Adams Lab, 600 S. Mathews, Urbana, IL 61801 (United States); Pengwang, Eakkachai [Mechanical Science and Engineering, 1206 West Green St., University of Illinois, Urbana, IL 61801 (United States); Masel, Richard I. [Chemical and Biomolecular Engineering, 213 Roger Adams Lab, 600 S. Mathews, Urbana, IL 61801 (United States)

    2010-04-02

    Microfuel cells (MFCs) can potentially power emerging technologies that require power sources in the microliter size range. The recent development of a microfluidic mechanism for self-regulated generation of hydrogen has enabled fabrication of MFCs orders of magnitude smaller than previously possible. In this study, we report an order of magnitude enhancement in the power density of a microliter-scale fuel cell incorporating a new microfluidic design. The microfluidic mechanism is part of an on-board hydrogen generator that uses a reaction between a metal hydride, LiAlH{sub 4}, and water vapor to generate hydrogen. The hydrogen generated exits the hydride reactor through a porous silicon wall to reach a Nafion-based membrane electrode assembly (MEA). The microfluidic design increased the water vapor release rate to the hydride reactor by one order of magnitude over a previous design. A 9 {mu}L device incorporating the enhanced microfluidic design delivered a power density of 92 W L{sup -1}. Details of a parametric study conducted to improve the water vapor release rate of the microfluidic mechanism and performance analysis of the integrated device are presented in this paper. (author)

  19. An enhanced microfluidic control system for improving power density of a hydride-based micro fuel cell

    Science.gov (United States)

    Moghaddam, Saeed; Pengwang, Eakkachai; Masel, Richard I.; Shannon, Mark

    Microfuel cells (MFCs) can potentially power emerging technologies that require power sources in the microliter size range. The recent development of a microfluidic mechanism for self-regulated generation of hydrogen has enabled fabrication of MFCs orders of magnitude smaller than previously possible. In this study, we report an order of magnitude enhancement in the power density of a microliter-scale fuel cell incorporating a new microfluidic design. The microfluidic mechanism is part of an on-board hydrogen generator that uses a reaction between a metal hydride, LiAlH 4, and water vapor to generate hydrogen. The hydrogen generated exits the hydride reactor through a porous silicon wall to reach a Nafion-based membrane electrode assembly (MEA). The microfluidic design increased the water vapor release rate to the hydride reactor by one order of magnitude over a previous design. A 9 μL device incorporating the enhanced microfluidic design delivered a power density of 92 W L -1. Details of a parametric study conducted to improve the water vapor release rate of the microfluidic mechanism and performance analysis of the integrated device are presented in this paper.

  20. Trialkylborane-Assisted CO(2) Reduction by Late Transition Metal Hydrides.

    Science.gov (United States)

    Miller, Alexander J M; Labinger, Jay A; Bercaw, John E

    2011-01-01

    Trialkylborane additives promote reduction of CO(2) to formate by bis(diphosphine) Ni(II) and Rh(III) hydride complexes. The late transition metal hydrides, which can be formed from dihydrogen, transfer hydride to CO(2) to give a formate-borane adduct. The borane must be of appropriate Lewis acidity: weaker acids do not show significant hydride transfer enhancement, while stronger acids abstract hydride without CO(2) reduction. The mechanism likely involves a pre-equilibrium hydride transfer followed by formation of a stabilizing formate-borane adduct.

  1. Improved hydrogen desorption from lithium hydrazide by alkali metal hydride

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Liang, E-mail: liangzeng@hiroshima-u.ac.jp [Institute for Advanced Materials Research, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima 739-8530 (Japan); Miyaoka, Hiroki [Institute for Sustainable Sciences and Development, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima 739-8530 (Japan); Ichikawa, Takayuki; Kojima, Yoshitsugu [Institute for Advanced Materials Research, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima 739-8530 (Japan)

    2013-12-15

    Highlights: •LiH can dramatically improve the hydrogen desorption properties of LiNHNH{sub 2}. •KH doping had positive effect in promoting the hydrogen desorption properties of LiNHNH{sub 2}–LiH mixture. •The reaction mechanism between LiNHNH{sub 2} and LiH was studied and discussed. -- Abstract: Lithium hydrazide (LiNHNH{sub 2}), which is a white solid with 8.0 mass% of theoretical hydrogen content, was synthesized from a reaction between anhydrous hydrazine and n-butyllithium in diethyl ether. The thermodynamic properties of this compound and its detailed decomposition pathways had been investigated in our previous work. However, a number of undesired gaseous products such as hydrazine (N{sub 2}H{sub 4}) and ammonia (NH{sub 3}) were generated during the thermal decomposition of LiNHNH{sub 2}. In this work, alkali metal hydride was used to suppress the impurities in the desorbed hydrogen and improved the hydrogen desorption properties. The reaction mechanism between LiNHNH{sub 2} and LiH was also studied and discussed in this paper.

  2. Mechanism of H2 Production by Models for the [NiFe]-Hydrogenases: Role of Reduced Hydrides.

    Science.gov (United States)

    Ulloa, Olbelina A; Huynh, Mioy T; Richers, Casseday P; Bertke, Jeffery A; Nilges, Mark J; Hammes-Schiffer, Sharon; Rauchfuss, Thomas B

    2016-07-27

    The intermediacy of a reduced nickel-iron hydride in hydrogen evolution catalyzed by Ni-Fe complexes was verified experimentally and computationally. In addition to catalyzing hydrogen evolution, the highly basic and bulky (dppv)Ni(μ-pdt)Fe(CO)(dppv) ([1](0); dppv = cis-C2H2(PPh2)2) and its hydride derivatives have yielded to detailed characterization in terms of spectroscopy, bonding, and reactivity. The protonation of [1](0) initially produces unsym-[H1](+), which converts by a first-order pathway to sym-[H1](+). These species have C1 (unsym) and Cs (sym) symmetries, respectively, depending on the stereochemistry of the octahedral Fe site. Both experimental and computational studies show that [H1](+) protonates at sulfur. The S = 1/2 hydride [H1](0) was generated by reduction of [H1](+) with Cp*2Co. Density functional theory (DFT) calculations indicate that [H1](0) is best described as a Ni(I)-Fe(II) derivative with significant spin density on Ni and some delocalization on S and Fe. EPR spectroscopy reveals both kinetic and thermodynamic isomers of [H1](0). Whereas [H1](+) does not evolve H2 upon protonation, treatment of [H1](0) with acids gives H2. The redox state of the "remote" metal (Ni) modulates the hydridic character of the Fe(II)-H center. As supported by DFT calculations, H2 evolution proceeds either directly from [H1](0) and external acid or from protonation of the Fe-H bond in [H1](0) to give a labile dihydrogen complex. Stoichiometric tests indicate that protonation-induced hydrogen evolution from [H1](0) initially produces [1](+), which is reduced by [H1](0). Our results reconcile the required reductive activation of a metal hydride and the resistance of metal hydrides toward reduction. This dichotomy is resolved by reduction of the remote (non-hydride) metal of the bimetallic unit.

  3. A quantitative phase field model for hydride precipitation in zirconium alloys: Part II. Modeling of temperature dependent hydride precipitation

    Energy Technology Data Exchange (ETDEWEB)

    Xiao, Zhihua [The Hong Kong Polytechnic University, Shenzhen Research Institute, Shenzhen (China); PolyU Base (Shenzhen) Limited, Shenzhen (China); Department of Mechanical Engineering, Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong (China); Hao, Mingjun [The Hong Kong Polytechnic University, Shenzhen Research Institute, Shenzhen (China); Department of Mechanical Engineering, Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong (China); Guo, Xianghua [State Key Laboratory of Explosion and Safety Science, Beijing Institute of Technology, Beijing 100081 (China); Tang, Guoyi [Advanced Materials Institute, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Shi, San-Qiang, E-mail: mmsqshi@polyu.edu.hk [The Hong Kong Polytechnic University, Shenzhen Research Institute, Shenzhen (China); PolyU Base (Shenzhen) Limited, Shenzhen (China); Department of Mechanical Engineering, Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong (China)

    2015-04-15

    A quantitative free energy functional developed in Part I (Shi and Xiao, 2014 [1]) was applied to model temperature dependent δ-hydride precipitation in zirconium in real time and real length scale. At first, the effect of external tensile load on reorientation of δ-hydrides was calibrated against experimental observations, which provides a modification factor for the strain energy in free energy formulation. Then, two types of temperature-related problems were investigated. In the first type, the effect of temperature transient was studied by cooling the Zr–H system at different cooling rates from high temperature while an external tensile stress was maintained. At the end of temperature transients, the average hydride size as a function of cooling rate was compared to experimental data. In the second type, the effect of temperature gradients was studied in a one or two dimensional temperature field. Different boundary conditions were applied. The results show that the hydride precipitation concentrated in low temperature regions and that it eventually led to the formation of hydride blisters in zirconium. A brief discussion on how to implement the hysteresis of hydrogen solid solubility on hydride precipitation and dissolution in the developed phase field scheme is also presented.

  4. Feasibility study for the recycling of nickel metal hydride electric vehicle batteries. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Sabatini, J.C.; Field, E.L.; Wu, I.C.; Cox, M.R.; Barnett, B.M.; Coleman, J.T. [Little (Arthur D.), Inc., Cambridge, MA (United States)

    1994-01-01

    This feasibility study examined three possible recycling processes for two compositions (AB{sub 2} and AB{sub 5}) of nickel metal hydride electric vehicle batteries to determine possible rotes for recovering battery materials. Analysts examined the processes, estimated the costs for capital equipment and operation, and estimated the value of the reclaimed material. They examined the following three processes: (1) a chemical process that leached battery powders using hydrochloric acid, (2) a pyrometallurical process, and (3) a physical separation/chemical process. The economic analysis revealed that the physical separation/chemical process generated the most revenue.

  5. Designing metal hydride complexes for water splitting reactions: a molecular electrostatic potential approach.

    Science.gov (United States)

    Sandhya, K S; Suresh, Cherumuttathu H

    2014-08-28

    The hydridic character of octahedral metal hydride complexes of groups VI, VII and VIII has been systematically studied using molecular electrostatic potential (MESP) topography. The absolute minimum of MESP at the hydride ligand (Vmin) and the MESP value at the hydride nucleus (VH) are found to be very good measures of the hydridic character of the hydride ligand. The increasing/decreasing electron donating feature of the ligand environment is clearly reflected in the increasing/decreasing negative character of Vmin and VH. The formation of an outer sphere metal hydride-water complex showing the HH dihydrogen interaction is supported by the location and the value of Vmin near the hydride ligand. A higher negative MESP suggested lower activation energy for H2 elimination. Thus, MESP features provided a way to fine-tune the ligand environment of a metal-hydride complex to achieve high hydridicity for the hydride ligand. The applicability of an MESP based hydridic descriptor in designing water splitting reactions is tested for group VI metal hydride model complexes of tungsten.

  6. Testing the isotropy of space using rotating quartz oscillators

    CERN Document Server

    Lo, Anthony; Mizrachi, Eli; Anderegg, Loic; Müller, Holger; Hohensee, Michael; Goryachev, Maxim; Tobar, Michael E

    2014-01-01

    Violations of Lorentz invariance by matter and light can generate direction- and frame-dependent anisotropies in particles inertial masses and, hence, a measurable modulation of the oscillation frequency of rotating quartz crystal oscillators. This allows simple and low maintenance experiments that are ideally suited for long-term data taking. Using the Standard Model Extension (SME) as a parameterizing framework, we study the magnitude of this putative frequency modulation. A preliminary experiment with room-temperature SC-cut crystals yields a frequency resolution in the $10^{-15}$ range with $\\sim 120$ hours of data and a limit of $\\tilde c_Q=(-1.8 \\pm 2.2)\\times 10^{-14}$\\,GeV on the most weakly constrained neutron-sector $c-$coefficient of the SME. Future experiments with cryogenic oscillators promise additional improvements in accuracy, opening up the potential for improved tests of Lorentz symmetry in the neutron, proton, electron and photon sector.

  7. 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

  8. Hydriding and Dehydriding Properties of Zinc Borohydride, Nickel, and Titanium-Added Magnesium Hydride

    Energy Technology Data Exchange (ETDEWEB)

    Kwak, Young Jun; Kwon, Sung Nam; Song, Myoung Youp [Chonbuk National University, Jeonju (Korea, Republic of)

    2015-11-15

    A Zn(BH{sub 4}){sub 2} sample was prepared by milling ZnCl{sub 2} and NaBH{sub 4} in a planetary ball mill under Ar gas. This sample contained NaCl. Then, 90 wt% MgH{sub 2}-5 wt% Zn(BH{sub 4}){sub 2}-2.5 wt% Ni-2.5 wt% Ti samples [named 90MgH{sub 2}-5Zn(BH{sub 4}){sub 2}-2.5Ni-2.5Ti] were prepared by milling in a planetary ball mill under H{sub 2} gas. The hydrogen absorption and release properties of the prepared samples were investigated. In particular, the variations of the initial hydriding and dehydriding rates with temperature were examined. SEM micrographs and XRD patterns of 90MgH{sub 2}-5Zn(BH{sub 4}){sub 2}-2.5Ni-2.5Ti after reactive mechanical grinding and after hydriding-dehydriding were also studied. Particle size distributions and BET specific surface areas of 90MgH{sub 2}-5Zn(BH{sub 4}){sub 2}-2.5Ni-2.5Ti after reactive mechanical grinding and after 11 hydriding-dehydriding cycles were analyzed. The 90MgH{sub 2}-5Zn(BH{sub 4}){sub 2}-2.5Ni-2.5Ti had an effective hydrogen storage capacity (the quantity of hydrogen absorbed for 60 min) of near 5 wt% (4.91 wt% at 593 K).

  9. Lithium-lithium hydride process for the production of hydrogen: comparison of two concepts for 950 and 1300 deg C HTR helium outlet temperature

    Energy Technology Data Exchange (ETDEWEB)

    Oertel, M.; Weirich, W.; Kuegler, B.; Luecke, L.; Pietsch, M.; Winkelmann, U.

    1987-01-01

    The lithium-lithium hydride process serves to generate hydrogen from water efficiently, using the high temperature heat of a nuclear reactor. Thermodynamic analyses show that hydrogen can be produced with an overall thermal efficiency of 48% at conventional HTR outlet temperatures of 950/sup 0/C. Assuming helium heat of 1300/sup 0/C, 56% overall thermal efficiency can be achieved.

  10. Determination of Mercuryalkylide in Water Using High Performance Liquid Chromatography with Hydride Generation Atomic Fluorescence Detection%高效液相色谱-氢化物发生-原子荧光光谱联用技术测定水中烷基汞

    Institute of Scientific and Technical Information of China (English)

    陈邵鹏; 顾海东; 秦宏兵

    2012-01-01

    A method for the determination of Mercury species in both surface water and waste water was established by high performance liquid chromatography ( HPLC ) -hydride generation ( HG) -atomic fluorescence spectrophotometry ( AFS). Sample was extracted by dichloromethane, subsequently back-extracted by mixed extractant containing cysteine and ammonium acetate before HPLC-HG-AFS detection. Under the optimized conditions, both methyl mercury and ethyl mercury responded linearly in the concentration of 1-50μg/L. The recoveries for both standard samples and actual samples were 80%-110%. The relative standard deviations for the determination of methyl and ethylmercury with the concentration of 1μg/L were 5. 2% and 3. 9% , respectively. The detection limits for them were 0.4 ng/L and 0.7 ng/L, respectively with the American EPA methord. The proposed method is of good accuracy, high repeatability, precision, less interferences from impurities and low cost, which is benefit for expanding and applying in the common laboratory.%建立了高效液相色谱(HPLC)-氢化物发生(HG)-原子荧光光谱(AFS)联用技术分析地表水及废水中甲基汞和乙基汞的方法.样品经二氯甲烷萃取,再以半胱氨酸+乙酸铵溶液反萃取富集,并进入高效液相色谱分离,经形态分析预处理装置后,借助原子荧光光谱法检测.在优化分离条件下,甲基汞和乙基汞在1 ~ 50 μg/L范围内呈现良好的线性关系,对于标准水样、地表水和废水实际水样,加标平均回收率均为80% ~ 110%.平行进样7次1μg/L的汞混合标准溶液,甲基汞和乙基汞的色谱峰面积的相对标准偏差分别为5.2%和3.9%,检出限则分别为0.4 ng/L和0.7 ng/L.该检测方法前处理简单、回收率稳定、灵敏度和准确度高、检出限低、杂质干扰少、监测费用低,便于在普通实验室推广和应用.

  11. Determination of arsenic in antimony ingot and antimony trioxide by hydride generation-atomic fluorescence spectrometry%氢化物发生-原子荧光光谱法测定锑锭及三氧化二锑中的砷

    Institute of Scientific and Technical Information of China (English)

    钱光敏; 赵国杏

    2012-01-01

    The antimony slab and antimonous oxide samples were dissolved by sulfuric acid and hydrochloric acid, respectively. The Sb3+ in solution was precipitated with sodium hydroxide to separate trace arsenic from matrix antimony. The thiourea-ascorbic acid was added to reduce As5+ to As3+. Then, the arsenic in antimony slab and antimonous oxide was determined by atomic fluorescence spec-trometry. The hydride generation conditions were investigated: the concentration of reducing agent potassium borohydride was 25 g/L, the determination medium was 20% (V/V) hydrochloric acid, and the dosage of thiourea - ascorbic acid solution was 5 mL. The interference test of coexisting elements showed that, the interference of residual antimony in solution after precipitation could be fully eliminated by adding 1 mL of tartaric acid solution. Other impurity elements in sample did not interfere with the determination of arsenic after adding thiourea-ascorbic acid solution. The detection limit of method was 0. 156 ng/mL. The antimony slab and antimonous oxide samples were analyzed by the proposed method, and the relative standard deviation (RSD) was 0. 95%-1.2%. The determination results were consistent with those obtained by national standard methods.%采用硫酸溶解锑锭样品,盐酸溶解三氧化二锑样品,用氢氧化钠溶液使Sb3+沉淀从而使基体锑与微量砷分离,通过加入硫脲-抗坏血酸将As5+还原成As3+,然后在原子荧光仪上测定锑锭及三氧化二锑中的砷.对氢化物发生条件进行考察,确定还原剂硼氢化钾的浓度为25 g/L、测定介质为20%(V/V)盐酸、硫脲-抗坏血酸溶液用量为5 mL.共存元素干扰试验表明,沉淀后溶液中残留少量锑的干扰在加入1 mL酒石酸溶液后可以完全消除,而样品中其他杂质元素在加入硫脲-抗坏血酸溶液后不干扰砷的测定.方法的检出限为0.156 ng/mL.对锑锭及三氧化二锑样品进行分析,相对标准偏差为0.95%~1.2%,测定

  12. THE DETERMINATION OF ANTIMONY (Ⅲ) AND ANTOMONY (Ⅴ) IN GEOLOGICAL SAMPLES BY HYDRIDE GENERATION-ATOMIC FLUORESCENCE SPECTROMETRY%氢化物发生—原子荧光光谱法测定地质样品中的锑(Ⅲ)和锑(Ⅴ)

    Institute of Scientific and Technical Information of China (English)

    郝志红; 杨帆; 刑夏; 汤志勇; 张勤

    2012-01-01

    A method for the determination of antimony ( Ⅲ ) and antimony ( V ) in geological samples (stream sediments) by hydride generation-atomic fluorescence spectrometry was developed in the paper. 4. 8 mol/L HC1 could be used as the extraclant with ultrasonic-assisted extraction. In the medium of 0. 24 mol/L hydrochloric acid, antimony ( Ⅲ) could be alternatively determined with 6 g/mL sodium citrate as the masking agent for Sb (V). Then antimony ( V ) could be figured out by the subtraction method. The detection limit of the method was 0. 075 × 10 -6 for Sb ( 1) and 0. 097 × 10 -6 for Sb ( V ) , and the relative standard deviation was 1. 1 % and 0. 64% ( n = 11) for 40 ng/mL Sb ( Ⅲ ) and 40 ng/mL Sb( V ) standard solution. The proposed method was applied to the determination of antimony ( Ⅲ) and antimony ( V ) in geological samples, and a comparison between the extraction results and the aqua regia dissolution results shows that the extraction rate of antimony was higher than 80% , the recoveries were in the ranges of 83% - 107% and 98% -114% for Sb ( Ⅲ) and Sb (V) respectively.%提出了一种氢化物发生—原子荧光光谱法测定地质样品(水系沉积物)中Sb(Ⅲ)和Sb(Ⅴ)的方法.选取4.8 mol/L HC1为提取剂,采用超声波辅助提取,以6 g/mL柠檬酸钠作为Sb(Ⅴ)的掩蔽剂,在0.24 mol/L的HC1介质中选择性测定Sb(Ⅲ),用差减法求得Sb(Ⅴ).Sb(Ⅲ)的方法检出限为0.075×10-6,Sb(Ⅴ)的方法检出限为0.097×10-6.对40 ng/mL的Sb(Ⅲ)和Sb(Ⅴ)分别连续测定11次,得到相对标准偏差分别为1.1%和0.64%.应用该方法对地质样品中的Sb(Ⅲ)和Sb(Ⅴ)进行分析测定,并与王水溶解值相比较,该方法测定的总Sb提取率在80%以上,Sb(Ⅲ)和Sb(Ⅴ)的加标回收率分别为83% ~ 107%和98% ~ 114%.

  13. AEROSOL FILTRATION USING QUARTZ SAND FILTER

    Directory of Open Access Journals (Sweden)

    Abbas H. Sulaymon

    2012-01-01

    Full Text Available The cement industry is the major source of cement dust which contains heavy metals like nickel, cobalt, lead, chromium, arsenic and hazardous substances like dioxins and furans. Exposure to these substances can cause health problems to human, animals and vegetation. A continuous pilot scale quartz sand filter was constructed and uses to study the effect of important design parameters (temperature, pre-loaded dust on the collector, diameter of the filter, bed depth, collector size and superficial velocity on its performance for cleaning of cement dust from air. Initial penetration and initial pressure drop (after 180s were measured and compared for different variables used in this study. The dirty bed was cleaned by means of reverse air flow when the pressure drop across the filter rises to 20 cmH2O. A macroscopic model describes the filter clogging was used to predict the effluent histories based on initial collection efficiency (η0exp which was determined from experimental data. A removal efficiency of more than 99% was obtained. The results show that 0.4% of cement dust still adheres on the quartz sand bed after 5 min of cleaning cycle. The presence of 0.4% of pre-load dust on the quartz sand filter enhanced the efficiency and low initial penetration, moderate initial pressure drop was obtained. At given Empty Bed Contact Time (EBCT, with different filter diameters 30 and 15 cm, a sharp decrease in initial penetration from 0.41-0.03 was obtained respectively. A nonlinear relationship between penetration and temperature was found. The initial penetration can be reduced by using smaller filter diameter, small collector size and collector with pre-load dust with 0.4%. The experiment that operates at a filter diameter of 15 cm and temperature of 25°C represent the minimum penetration among all the experiments.

  14. Kinetics of the coesite to quartz transformation

    Science.gov (United States)

    Mosenfelder, J.L.; Bohlen, S.R.

    1997-01-01

    The survival of coesite in ultrahigh-pressure (UHP) rocks has important implications for the exhumation of subducted crustal rocks. We have conducted experiments to study the mechanism and rate of the coesite ??? quartz transformation using polycrystalline coesite aggregates, fabricated by devitrifying silica glass cylinders containing 2850H/106 Si at 1000??C and 3.6 GPa for 24h. Conditions were adjusted following synthesis to transform the samples at 700-1000??C at pressures 190-410 MPa below the quartz-coesite equilibrium boundary. Reaction proceeds via grain-boundary nucleation and interface-controlled growth, with characteristic reaction textures remarkably similar to those seen in natural UHP rocks. We infer that the experimental reaction mechanism is identical to that in nature, a prerequisite for reliable extrapolation of the rate data. Growth rates obtained by direct measurement differ by up to two orders of magnitude from those estimated by fitting a rate equation to the transformation-time data. Fitting the rates to Turnbull's equation for growth therefore yields two distinct sets of parameters with similar activation energies (242 or 269 kJ/mol) but significantly different pre-exponential constants. Extrapolation based on either set of growth rates suggests that coesite should not be preserved on geologic time scales if it reaches the quartz stability field at temperatures above 375-400??C. The survival of coesite has previously been linked to its inclusion in strong phases, such as garnet, that can sustain a high internal pressure during decompression. Other factors that may play a crucial role in preservation are low fluid availability - possibly even less than that of our nominally "dry" experiments - and the development of transformation stress, which inhibits nucleation and growth. These issues are discussed in the context of our experiments as well as recent observations from natural rocks. ?? 1997 Elsevier Science B.V.

  15. Calorimetric thermobarometry of experimentally shocked quartz

    Science.gov (United States)

    Ocker, Katherine D.; Gooding, James L.; Hoerz, Friedrich

    1994-01-01

    Structural damage in experimentally shock-metamorphosed, granular quartz is quantitatively measurable by differential scanning calorimetry (DSC). Shock-induced loss of crystallinity is witnessed by disappearance of the alpha/beta phase transformation and evolution of a broad endoenthalpic strain peak at 650-900 K. The strain-energy peak grows rapidly at less than 10 GPa but declines with increasing shock pressure; it approaches zero at 32 GPa where vitrification is extensive. Effects of grain size and post-shock thermal history must be better understood before calorimetric thermobarometry of naturally shocked samples becomes possible.

  16. Quartz resonator instabilities under cryogenic conditions.

    Science.gov (United States)

    Goryachev, Maxim; Galliou, Serge; Abbe, Philippe; Bourgeois, Pierre-Yves; Grop, Serge; Dubois, Benoit

    2012-01-01

    The phase noise of a quartz crystal resonator working at liquid helium temperatures is studied. Measurement methods and the device environment are explained. The phase noise is measured for different resonance modes, excitation levels, amount of operating time, device orientations in relation to the cryocooler vibration axis, and temperatures. Stability limits of a frequency source based on such devices are evaluated in the present measurement conditions. The sources of phase flicker and white noises are identified. Finally, the results are compared with previous works.

  17. Defect-free surface of quartz glass polished in elastic mode by chemical impact reaction

    Institute of Scientific and Technical Information of China (English)

    彭文强; 关朝亮; 李圣怡

    2014-01-01

    Removal of brittle materials in the brittle or ductile mode inevitably causes damaged or strained surface layers containing cracks, scratches or dislocations. Within elastic deformation, the arrangement of each atom can be recovered back to its original position without any defects introduced. Based on surface hydroxylation and chemisorption theory, material removal mechanism of quartz glass in the elastic mode is analyzed to obtain defect-free surface. Elastic contact condition between nanoparticle and quartz glass surface is confirmed from the Hertz contact theory model. Atoms on the quartz glass surface are removed by chemical bond generated by impact reaction in the elastic mode, so no defects are generated without mechanical process. Experiment was conducted on a numerically controlled system for nanoparticle jet polishing, and one flat quartz glass was polished in the elastic mode. Results show that scratches on the sample surface are completely removed away with no mechanical defects introduced, and micro-roughness (Ra) is decreased from 1.23 nm to 0.47 nm. Functional group Ce—O—Si on ceria nanoparticles after polishing was detected directly and indirectly by FTIR, XRD and XPS spectra analysis from which the chemical impact reaction is validated.

  18. 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.

  19. 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.

  20. Numerical simulation and performance test of metal hydride hydrogen storage system

    Directory of Open Access Journals (Sweden)

    Tzu-Hsiang Yen, Bin-Hao Chen, Bao-Dong Chen

    2011-05-01

    Full Text Available Metal hydride reactors are widely used in many industrial applications, such as hydrogen storage, thermal compression, heat pump, etc. According to the research requirement of metal hydride hydrogen storage, the thermal analyses have been implemented in the paper. The metal hydride reaction beds are considered as coupled cylindrical tube modules which combine the chemical absorption and desorption in metal hydride. The model is then used metal hydride LaNi5 as an example to predict the performance of metal hydride hydrogen storage devices, such as the position of hydration front and the thermal flux. Under the different boundary condition the characteristics of heat transfer and mass transfer in metal hydride have influence on the hydrogen absorption and desorption. The researches revealed that the scroll design can improve the temperature distribution in the reactor and the porous tube for directing hydrogen can increase the penetration depth of hydride reaction to decrease the hydrogen absorption time.

  1. Micro-scale fracture experiments on zirconium hydrides and phase boundaries

    Science.gov (United States)

    Chan, H.; Roberts, S. G.; Gong, J.

    2016-07-01

    Fracture properties of micro-scale zirconium hydrides and phase boundaries were studied using microcantilever testing methods. FIB-machined microcantilevers were milled on cross-sectional surfaces of hydrided samples, with the most highly-stressed regions within the δ-hydride film, within the α-Zr or along the Zr-hydride interface. Cantilevers were notched using the FIB and then tested in bending using a nanoindenter. Load-displacement results show that three types of cantilevers have distinct deformation properties. Zr cantilevers deformed plastically. Hydride cantilevers fractured after a small amount of plastic flow; the fracture toughness of the δ-hydride was found to be 3.3 ± 0.4 MPam1/2 and SEM examination showed transgranular cleavage on the fracture surfaces. Cantilevers notched at the Zr-hydride interface developed interfacial voids during loading, at loads considerably lower than that which initiate brittle fracture of hydrides.

  2. Investigation of Cracked Lithium Hydride Reactor Vessels

    Energy Technology Data Exchange (ETDEWEB)

    bird, e.l.; mustaleski, t.m.

    1999-06-01

    Visual examination of lithium hydride reactor vessels revealed cracks that were adjacent to welds, most of which were circumferentially located in the bottom portion of the vessels. Sections were cut from the vessels containing these cracks and examined by use of the metallograph, scanning electron microscope, and microprobe to determine the cause of cracking. Most of the cracks originated on the outer surface just outside the weld fusion line in the base material and propagated along grain boundaries. Crack depths of those examined sections ranged from {approximately}300 to 500 {micro}m. Other cracks were reported to have reached a maximum depth of 1/8 in. The primary cause of cracking was the creation of high tensile stresses associated with the differences in the coefficients of thermal expansion between the filler metal and the base metal during operation of the vessel in a thermally cyclic environment. This failure mechanism could be described as creep-type fatigue, whereby crack propagation may have been aided by the presence of brittle chromium carbides along the grain boundaries, which indicates a slightly sensitized microstructure.

  3. Aqueous Wetting Films on Fused Quartz.

    Science.gov (United States)

    Mazzoco; Wayner

    1999-06-15

    Using an image analyzing interferometer, IAI, the interfacial characteristics of an isothermal constrained vapor bubble, CVB, in a quartz cuvette were studied as a precursor to heat transfer research. The effects of pH and electrolyte concentration on the meniscus properties (curvature and adsorbed film thickness) and the stability of the aqueous wetting films were evaluated. The surface potential in the electric double layer was a function of the cleaning and hydroxylation of the quartz surface. The disjoining pressure isotherm for pure water was very close to that predicted by the Langmuir equation. For aqueous solutions of moderate electrolyte concentration, the Gouy-Chapman theory provided a good representation of the electrostatic effects in the film. The effect of temperature on the film properties of aqueous solutions and pure water was also evaluated: The meniscus curvature decreased with increasing temperature, while Marangoni effects, intermolecular forces, and local evaporation and condensation enhanced waves on the adsorbed film layer. Pure water wetting films were mechanically metastable, breaking into droplets and very thin films (less than 10 nm) after a few hours. Aqueous wetting films with pH 12.4 proved to be stable during a test of several months, even when subjected to temperature and mechanical perturbations. The mechanical stability of wetting films can explain the reported differences between the critical heat fluxes of pure water and aqueous solutions. The IAI-CVB technique is a simple and versatile experimental technique for studying the characteristics of interfacial systems. Copyright 1999 Academic Press.

  4. Production of quartz plates for CMS-CASTOR Experiment

    CERN Document Server

    Adiguzel, Aytul; Ayhan, Aydin; Bakirci, Mustafa Numan; Basegmez, Suzan; Beaumont, Willem; Borras, Kerstin; Campbell, Alan; De Paula Carvalho, W; Çerçi, Salim; De Jesus Damiao, Dilson; Dogangün, O; Dumanoglu, Isa; d'Enterria, David; Erchov, Y; Eskut, Eda; Figueiredo, D; Girgis, Semiray; Göttlicher, P; Gouskos, Loukas; Gurpinar, Emine; Hos, Ilknur; Katkov, Igor; Katsas, Panagiotis; Khein, Lev; Knutsson, Albert; Kuznetsov, Andrey; Lebeau, Michel; Van Mechelen, Pierre; Muhl, Carsten; Musienko, Yuri; Ochesanu, Silvia; Onengüt, G; Onengut, G Jr; Ozdemir, Kadri; Panagiotou, Apostolos; Polatoz, A; Ripert, Marion; Shileev, K; Sogut, Kenan; Tiflov, B TaliV; Kayis-Topaksu, A; Uzun, Dilber

    2008-01-01

    Light transmission rate performance of $102$ irradiated quartz samples was measured to select the best quartz plates for CMS-CASTOR calorimeter. All the produced quartz plates were originally used in a previous CERN experiment, DELPHI. Three different doses of $^{60}$Co source were used with the collaboration of PSI (Paul Scherrer Institute, Villigen PSI, Switzerland.) to study the transmission rate performance of the quartz samples after irradiation for different incident light, ranging from $250$ to $700$ nm in $5$ nm increasing steps. All samples show different decrease in the rate with wavelength for different doses. Three different steps were followed before irradiation to find out the best way of cleaning the original DELPHI Cu/Cr tracks on the samples. Results of these measurements presented here correspond to the quartz plates that will be used in one hadronic sector of CASTOR calorimeter until end of 2008. For the full calorimeter new quartz plates will be installed. We also present the light transmi...

  5. Comparison of the interactions in the rare gas hydride and Group 2 metal hydride anions.

    Science.gov (United States)

    Harris, Joe P; Manship, Daniel R; Breckenridge, W H; Wright, Timothy G

    2014-02-28

    We study both the rare gas hydride anions, RG-H(-) (RG = He-Rn) and Group 2 (Group IIa) metal hydride anions, MIIaH(-) (MIIa = Be-Ra), calculating potential energy curves at the CCSD(T) level with augmented quadruple and quintuple basis sets, and extrapolating the results to the basis set limit. We report spectroscopic parameters obtained from these curves; additionally, we study the Be-He complex. While the RG-H(-) and Be-He species are weakly bound, we show that, as with the previously studied BeH(-) and MgH(-) species, the other MIIaH(-) species are strongly bound, despite the interactions nominally also being between two closed shell species: M(ns(2)) and H(-)(1s(2)). We gain insight into the interactions using contour plots of the electron density changes and population analyses. For both series, the calculated dissociation energy is significantly less than the ion/induced-dipole attraction term, confirming that electron repulsion is important in these species; this effect is more dramatic for the MIIaH(-) species than for RG-H(-). Our analyses lead us to conclude that the stronger interaction in the case of the MIIaH(-) species arises from sp and spd hybridization, which allows electron density on the MIIa atom to move away from the incoming H(-).

  6. Multidimensional simulations of hydrides during fuel rod lifecycle

    Science.gov (United States)

    Stafford, D. S.

    2015-11-01

    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.

  7. Modeling by regression for laser cutting of quartz crystal

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Presents the theoretical models built by analysis of the mechanism of laser cutting of quartz crystal and re gression of test results for the laser cutting of quartz crystal, and comparative analysis of calculation errors for these models, and concludes with test results that these models comprehensively reflect the physical features of laser cutting of quartz crystal and satisfy the industrial production requirements, and they can be used to select right parameters for improvement of productivity and quality and saving of energy.

  8. Mineral resource of the month: cultured quartz crystal

    Science.gov (United States)

    ,

    2008-01-01

    The article presents information on cultured quartz crystals, a mineral used in mobile phones, computers, clocks and other devices controlled by digital circuits. Cultured quartz, which is synthetically produced in large pressurized vessels known as autoclaves, is useful in electronic circuits for precise filtration, frequency control and timing for consumer and military use. Several ingredients are used in producing cultured quartz, including seed crystals, lascas, a solution of sodium hydroxide or sodium carbonate, lithium salts and deionized water.

  9. Comparison of Hydrogen Elimination from Molecular Zinc and Magnesium Hydride Clusters

    NARCIS (Netherlands)

    Intemann, J.; Sirsch, Peter; Harder, Sjoerd

    2014-01-01

    In analogy to the previously reported tetranuclear magnesium hydride cluster with a bridged dianionic bis-beta-diketiminate ligand, a related zinc hydride cluster has been prepared. The crystal structures of these magnesium and zinc hydride complexes are similar: the metal atoms are situated at the

  10. 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.

  11. Comparison of Hydrogen Elimination from Molecular Zinc and Magnesium Hydride Clusters

    NARCIS (Netherlands)

    Intemann, J.; Sirsch, Peter; Harder, Sjoerd

    2014-01-01

    In analogy to the previously reported tetranuclear magnesium hydride cluster with a bridged dianionic bis-beta-diketiminate ligand, a related zinc hydride cluster has been prepared. The crystal structures of these magnesium and zinc hydride complexes are similar: the metal atoms are situated at the

  12. Investigation of metal hydride materials as hydrogen reservoirs for metal-hydrogen batteries

    Science.gov (United States)

    ONISCHAK

    1976-01-01

    The performance and suitability of various metal hydride materials were examined for use as possible hydrogen storage reservoirs for secondary metal-hydrogen batteries. Lanthanum pentanickel hydride appears as a probable candidate in terms of stable hydrogen supply under feasible thermal conditions. A kinetic model describing the decomposition rate data of the hydride has been developed.

  13. Hydrothermal quartz formation during fluctuations of brittle shear-zone activity and fluid flow: grain growth and deformation structures of the Pfahl shear zone (Germany)

    Science.gov (United States)

    Yilmaz, T.; Prosser, G.; Liotta, D.; Kruhl, J. H.

    2012-12-01

    The Bavarian Pfahl shear zone is a WNW-ESE trending dextral strike-slip shear zone at the SW margin of the Bohemian Massif (Central Europe). It was discontinuously active during decreasing PT-conditions, i.e. from ductile to brittle, from the late-Carboniferous to the late-Cretaceous - Paleocene times. Triassic hydrothermal activity produced a 150 km long and 30-100 m wide quartz dyke along the main fault, surrounded by sheared basement rocks. Within a zone of >10 m metasomatism transformed the wall rocks to mostly kaolinite, chlorite and phyllosilicates. The quartz dyke exhibits a layered to lenticular and partly symmetric structure with different types of quartz masses, transected by a complex quartz vein network. This already indicates pulses of fluid flux and fragmentation during the lifetime of the shear zone. Analyses by optical microscopy, cathodoluminescence (CL) and SEM-EDX reveal at least four subsequent stages of quartz crystallization and fragmentation. (i) The oldest generation of quartz is represented by a homogeneous dark grey to reddish quartz mass made up by ~10-20 μm-sized crystals. It contains mm- to cm-sized angular wall-rock fragments, completely altered to kaolinite, indicating intense wall-rock alteration prior to the earliest event of silica precipitation. This rules out the possibility that the quartz mass developed from silicification of the wall rocks. This first type of quartz occurs as cm- to dm-large angular fragments in (ii) a light grey to pink quartz mass formed by ~10-50 μm-sized crystals. The different colours result from variable types and amounts of inclusions. Quartz of both generations shows random crystallographic orientations and complex inclusion structures. It probably developed during two fragmentation events and possibly from a silica gel precursor that crystallized after precipitation. (iii) The third quartz generation formed as a set of mm- to dm-wide veins roughly parallel to the trend of the Pfahl zone

  14. Trace elements in quartz shed light on sediment provenance

    Science.gov (United States)

    Ackerson, Michael R.; Tailby, Nicholas D.; Watson, E. Bruce

    2015-06-01

    Quartz is one of the most common minerals on the surface of the earth, and is a primary rock-forming mineral across the rock cycle. These two factors make quartz an obvious target for sediment provenance studies. Observations from experimental and natural samples demonstrate that the trace element content of quartz often reflects the conditions of quartz formation. When quartz is weathered from its primary crystallization setting (i.e., quartz from a granitoid) it can retain many chemical signatures of formation throughout the sedimentation processes. These geochemical signatures can be used to understand the primary source of individual quartz grains within a sediment. Here we present a case study from the Bega River catchment to demonstrate that quartz grains in sediments at the mouth of the Bega River are sourced from granitoids within the drainage basin. Data presented here also indicate that a portion of the beach sediment is also derived from either (i) sedimentary rocks within the basin or; (ii) mixing with sediments at the mouth of the river. The Bega River catchment was selected for this study because it is both small and has a well-constrained bedrock lithology, making it an ideal location to test the utility of this provenance technique. However, quartz trace element provenance has broad applications to modern and ancient sediments and can be used in lieu of, or in conjunction with, other provenance techniques to elucidate sediment transport through time.

  15. Pre-biotic organic molecules in hydrothermal quartz veins from the Archaean Yilgarn province, Australia

    Science.gov (United States)

    Mayer, Christian; Schreiber, Ulrich; Dyker, Gerald; Kirnbauer, Thomas; Mulder, Ines; Sattler, Tobias; Schöler, Heinfried; Tubbesing, Christoph

    2013-04-01

    According to a model recently published by Schreiber et al. (OLEB 2012), pre-biotic organic molecules as earliest markers for a chemical evolution have been formed in tectonic faults of the first Archaean cratons. These faults are often documented by quartz- and other hydrothermal vein mineralization. During the growth of these quartzes, small portions of hydrothermal fluids are enclosed which conserve the chemical composition of the given fluid medium. According to our model, the preconditions for the geochemical formation of organic molecules are a suitable carbon source (e.g. carbon dioxide), varying P/T conditions, and catalysts. This given, rising hydrothermal fluids such as mineral-rich water and supercritical carbon dioxide in deep faults with contacts to the upper earth mantle offer conditions which allow for reactions similar to the Fischer-Tropsch synthesis. So far, the inclusions which possibly have conserved the products of these reactions have not been analyzed for possible organic constituents. First analytical results of a Mesozoic hydrothermal quartz vein from central Germany (Taunus) reveal that several organic compounds are found in fluid inclusions. However, the true origin of these compounds is unclear due to possible contamination by adjacent Corg-rich metasediments. Therefore, we have extended the study to hydrothermal quartz veins from the Archaean Yilgarn craton, to impact-generated quartz veins of the Shoemaker-Crater as well as to hydrothermal quartz boulders from a 2.7 to 3 billion years old conglomerate near Murchison (Western Australia). In one of the samples from the conglomerate, a wide spectrum of organic compounds such as bromomethane, butane, isoprene, benzene, and toluene have been detected. The time interval between the quartz formation, its erosion and its sedimentation is unknown. Possibly, the analyzed quartz sample was formed in a hydrothermal vein long before any living cells have existed on earth. In this case, the given

  16. Geospatializing The Klang Gate Quartz Ridge in Malaysia: A Technological Perspective

    Science.gov (United States)

    Azahari Razak, Khamarrul; Mohamad, Zakaria; Zaki Ibrahim, Mohd; Azad Rosle, Qalam; Hattanajmie Abd Wahab, Mohd; Abu Bakar, Rabieahtul; Mohd Akib, Wan Abdul Aziz Wan

    2015-04-01

    Establishment of inventories on geological heritage, or geoheritage resources is a step forward for a comprehensive geoheritage management leading to a better conservation at national and global levels. Compiling and updating inventory of geoheritage is a tedious process and even so in a tropical environment. Malaysia has a tremendous list of geodiversity and generating its national database is a multi-institutional effort and worthwhile investment. However, producing accurate and reliable characteristics of such landform and spectacular geological features remained elusive. The advanced and modern mapping techniques have revolutionized the mapping, monitoring and modelling of the earth surface processes and landforms. Yet the methods for quantification of geodiversity physical features are not fully utilized in Malaysia for a better understanding its processes and activity. This study provides a better insight into the use of advanced active remote sensing technology for characterizing the forested Quartz Ridge in Malaysia. We have developed the novel method and tested in the Klang Gates Quartz Ridge, Selangor. The granitic country rock made up by quartz mineral is known as the longest quartz ridge in Malaysia and characterized by rugged topography, steep slopes, densely vegetated terrain and also rich-biodiversity area. This study presents an integrated field methodological framework and processing scheme by taking into account the climatic, topographic, geologic, and anthropogenic challenges in an equatorial region. Advanced terrestrial laser scanning system was used to accurately capture, map and model the ridge carried out within a relatively stringent time period. The high frequency Global Navigation Satellite System and modern Total Station coupled with the optical satellite and radar imageries and also advanced spatial analysis were fully utilized in the field campaign and data assessment performed during the recent monsoon season. As a result, the mapping

  17. A study of advanced magnesium-based hydride and development of a metal hydride thermal battery system

    Science.gov (United States)

    Zhou, Chengshang

    Metal hydrides are a group of important materials known as energy carriers for renewable energy and thermal energy storage. A concept of thermal battery based on advanced metal hydrides is studied for heating and cooling of cabins in electric vehicles. The system utilizes a pair of thermodynamically matched metal hydrides as energy storage media. The hot hydride that is identified and developed is catalyzed MgH2 due to its high energy density and enhanced kinetics. TiV0.62Mn1.5, TiMn2, and LaNi5 alloys are selected as the matching cold hydride. A systematic experimental survey is carried out in this study to compare a wide range of additives including transitions metals, transition metal oxides, hydrides, intermetallic compounds, and carbon materials, with respect to their effects on dehydrogenation properties of MgH2. The results show that additives such as Ti and V-based metals, hydride, and certain intermetallic compounds have strong catalytic effects. Solid solution alloys of magnesium are exploited as a way to destabilize magnesium hydride thermodynamically. Various elements are alloyed with magnesium to form solid solutions, including indium and aluminum. Thermodynamic properties of the reactions between the magnesium solid solution alloys and hydrogen are investigated, showing that all the solid solution alloys that are investigated in this work have higher equilibrium hydrogen pressures than that of pure magnesium. Cyclic stability of catalyzed MgH2 is characterized and analyzed using a PCT Sievert-type apparatus. Three systems, including MgH2-TiH 2, MgH2-TiMn2, and MgH2-VTiCr, are examined. The hydrogenating and dehydrogenating kinetics at 300°C are stable after 100 cycles. However, the low temperature (25°C to 150°C) hydrogenation kinetics suffer a severe degradation during hydrogen cycling. Further experiments confirm that the low temperature kinetic degradation can be mainly related the extended hydrogenation-dehydrogenation reactions. Proof

  18. Monitoring and control of a hydrogen production and storage system consisting of water electrolysis and metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Perez-Herranz, V.; Perez-Page, M. [Departamento de Ingenieria Quimica y Nuclear. Universidad Politecnica de Valencia. Camino de Vera S/N, 46022 Valencia (Spain); Beneito, R. [Area de Energia. Departamento de Gestion e Innovacion. Instituto Tecnologico del Juguete (AIJU). Avda. Industria 23, 03440 Ibi, Alicante (Spain)

    2010-02-15

    Renewable energy sources such as wind turbines and solar photovoltaic are energy sources that cannot generate continuous electric power. The seasonal storage of solar or wind energy in the form of hydrogen can provide the basis for a completely renewable energy system. In this way, water electrolysis is a convenient method for converting electrical energy into a chemical form. The power required for hydrogen generation can be supplied through a photovoltaic array. Hydrogen can be stored as metal hydrides and can be converted back into electricity using a fuel cell. The elements of these systems, i.e. the photovoltaic array, electrolyzer, fuel cell and hydrogen storage system in the form of metal hydrides, need a control and monitoring system for optimal operation. This work has been performed within a Research and Development contract on Hydrogen Production granted by Solar Iniciativas Tecnologicas, S.L. (SITEC), to the Politechnic University of Valencia and to the AIJU, and deals with the development of a system to control and monitor the operation parameters of an electrolyzer and a metal hydride storage system that allow to get a continuous production of hydrogen. (author)

  19. Investigation of metal hydride nanoparticles templated in metal organic frameworks.

    Energy Technology Data Exchange (ETDEWEB)

    Jacobs, Benjamin W.; Herberg, Julie L. (Lawrence Livermore National Laboratory, Livermore, CA); Highley, Aaron M.; Grossman, Jeffrey (MIT, Cambridge, MA); Wagner, Lucas (MIT, Cambridge, MA); Bhakta, Raghu; Peaslee, D. (University of Missouri, St. Louis, MO); Allendorf, Mark D.; Liu, X. (University of Missouri, St. Louis, MO); Behrens, Richard, Jr.; Majzoub, Eric H. (University of Missouri, St. Louis, MO)

    2010-11-01

    Hydrogen is proposed as an ideal carrier for storage, transport, and conversion of energy. However, its storage is a key problem in the development of hydrogen economy. Metal hydrides hold promise in effectively storing hydrogen. For this reason, metal hydrides have been the focus of intensive research. The chemical bonds in light metal hydrides are predominantly covalent, polar covalent or ionic. These bonds are often strong, resulting in high thermodynamic stability and low equilibrium hydrogen pressures. In addition, the directionality of the covalent/ionic bonds in these systems leads to large activation barriers for atomic motion, resulting in slow hydrogen sorption kinetics and limited reversibility. One method for enhancing reaction kinetics is to reduce the size of the metal hydrides to nano scale. This method exploits the short diffusion distances and constrained environment that exist in nanoscale hydride materials. In order to reduce the particle size of metal hydrides, mechanical ball milling is widely used. However, microscopic mechanisms responsible for the changes in kinetics resulting from ball milling are still being investigated. The objective of this work is to use metal organic frameworks (MOFs) as templates for the synthesis of nano-scale NaAlH4 particles, to measure the H2 desorption kinetics and thermodynamics, and to determine quantitative differences from corresponding bulk properties. Metal-organic frameworks (MOFs) offer an attractive alternative to traditional scaffolds because their ordered crystalline lattice provides a highly controlled and understandable environment. The present work demonstrates that MOFs are stable hosts for metal hydrides and their reactive precursors and that they can be used as templates to form metal hydride nanoclusters on the scale of their pores (1-2 nm). We find that using the MOF HKUST-1 as template, NaAlH4 nanoclusters as small as 8 formula units can be synthesized inside the pores. A detailed picture of

  20. Theoretical Estimate of Hydride Affinities of Aromatic Carbonyl Compounds

    Institute of Scientific and Technical Information of China (English)

    AI Teng; ZHU Xiao-Qing; CHENG Jin-Pei

    2003-01-01

    @@ Aromatic carbonyl compounds are one type of the most important organic compounds, and the reductions ofthem by hydride agents such as LiAlH4 or NaBH4 are widely used in organic synthesis. The reactivity of carbonyl compounds generally increases in the following order: ketone < aldehyde, and amide < acid < ester < acid halide, which could be related to their hydride affinities (HA). In the previous paper, Robert[1] calculated the absolute HAof a series of small non-aromatic carbonyl compounds. In this paper, we use DFT method at B3LYP/6-311 + + G (2d, 2p)∥B3LYP/6-31 + G* level to estimate hydride affinities of five groups of aromatic carbonyl compounds. The detailed results are listed in Table 1.

  1. A nickel metal hydride battery for electric vehicles.

    Science.gov (United States)

    Ovshinsky, S R; Fetcenko, M A; Ross, J

    1993-04-09

    Widespread use of electric vehicles can have significant impact on urban air quality, national energy independence, and international balance of trade. An efficient battery is the key technological element to the development of practical electric vehicles. The science and technology of a nickel metal hydride battery, which stores hydrogen in the solid hydride phase and has high energy density, high power, long life, tolerance to abuse, a wide range of operating temperature, quick-charge capability, and totally sealed maintenance-free operation, is described. A broad range of multi-element metal hydride materials that use structural and compositional disorder on several scales of length has been engineered for use as the negative electrode in this battery. The battery operates at ambient temperature, is made of nontoxic materials, and is recyclable. Demonstration of the manufacturing technology has been achieved.

  2. CO2 hydrogenation on a metal hydride surface.

    Science.gov (United States)

    Kato, Shunsuke; Borgschulte, Andreas; Ferri, Davide; Bielmann, Michael; Crivello, Jean-Claude; Wiedenmann, Daniel; Parlinska-Wojtan, Magdalena; Rossbach, Peggy; Lu, Ye; Remhof, Arndt; Züttel, Andreas

    2012-04-28

    The catalytic hydrogenation of CO(2) at the surface of a metal hydride and the corresponding surface segregation were investigated. The surface processes on Mg(2)NiH(4) were analyzed by in situ X-ray photoelectron spectroscopy (XPS) combined with thermal desorption spectroscopy (TDS) and mass spectrometry (MS), and time-of-flight secondary ion mass spectrometry (ToF-SIMS). CO(2) hydrogenation on the hydride surface during hydrogen desorption was analyzed by catalytic activity measurement with a flow reactor, a gas chromatograph (GC) and MS. We conclude that for the CO(2) methanation reaction, the dissociation of H(2) molecules at the surface is not the rate controlling step but the dissociative adsorption of CO(2) molecules on the hydride surface.

  3. Zirconium hydride formation in Hanford production reactor process tubes

    Energy Technology Data Exchange (ETDEWEB)

    Winegardner, W.K.; Griggs, B.

    1967-12-01

    Examination of Zircaloy-2 process tubes from Hanford Production Reactors has revealed extensive zirconium hydride formation. In general, attack is limited to the downstream portions of tubes where aluminum spacers are located. Most of the hydride platelets are contained in a case or layer on the inner surface of the tube. It is not unusual to find cases 0.004 to 0.005 in. thick. Analyses of the 0.037 in. wall tubes with such cases intact often reveal hydrogen concentrations greater than 1000 ppM. Investigation indicates that the hydriding is the result of galvanic contact between aluminum and Zircaloy-2. The galvanic couple (contact between dissimilar metals in the presence of reactor cooling water which serves as the electrolyte) results in the cathodic charging of hydrogen into the Zircaloy.

  4. NUMERICAL ANALYSIS FOR HYDRIDING IN METAL HYDRIDE HYDROGEN STORAGE TANK%金属氢化物储氢器吸氢过程的数值分析

    Institute of Scientific and Technical Information of China (English)

    叶建华; 蒋利军; 李志念; 刘晓鹏; 王树茂

    2011-01-01

    Based on the principle of hydride adsorption, a one-dimensional mathematical model for hydriding in a cylindrical metal hydride hydrogen storage tank was established. The heat and mass transfer of metal hydride beds was computed by finite difference method. The variation in temperature and hydrogen concentration at different radial positions of the hydride layer was analyzed during the process of hydriding. The effects of supply pressure, heat convection coefficient and hydride layer radial thickness on the hydriding was studied. It is shown that hydride formation initially takes place uniformly all over the metal hydride layer, but with the process of hydriding, the hydriding rate at the core region is gradually slower than one at surface region. The increase of supply pressure and heat convection coefficient can accelerate the hydriding of the hydrogen storage tank. The effect of hydride layer radial thickness is significant on the hydriding rate, and the thinner hydride layer, the higher the hydriding rate.%基于金属氢化物吸氢基本特性,建立圆柱形金属氢化物储氢器吸氢过程的-维数学物理模型.采用有限差分法对金属氢化物床体的传热传质进行计算.分别研究金属氢化物床体各处温度和氢含量在吸氢过程中的变化以及氢气压力、对流传热系数和金属氢化物床体径向厚度对金属氢化物吸氢过程的影响.计算结果表明:初始阶段金属氢化物床均匀吸氢,但随着氢化过程的进行,其中心区域的吸氢速率逐渐低于边缘区域;增加吸氢压力、提高对流传热系数均可促进储氢器的吸氢;金属氢化物床的径向厚度对吸氢速率影响很大,金属氢化物床越薄,氢化反应的速度越快.

  5. Evaluation of Diffuse Reflection Infrared Spectrometry for End-of-Shift Measurement of α-quartz in Coal Dust Samples.

    Science.gov (United States)

    Miller, Arthur L; Murphy, Nathaniel C; Bayman, Sean J; Briggs, Zachary P; Kilpatrick, Andrew D; Quinn, Courtney A; Wadas, Mackenzie R; Cauda, Emanuele G; Griffiths, Peter R

    2015-01-01

    The inhalation of toxic substances is a major threat to the health of miners, and dust containing respirable crystalline silica (α-quartz) is of particular concern, due to the recent rise in cases of coal workers' pneumoconiosis and silicosis in some U.S. mining regions. Currently, there is no field-portable instrument that can measure airborne α-quartz and give miners timely feedback on their exposure. The U.S. National Institute for Occupational Safety and Health (NIOSH) is therefore conducting studies to investigate technologies capable of end-of-shift or real-time measurement of airborne quartz. The present study focuses on the potential application of Fourier transform infrared (FT-IR) spectrometry conducted in the diffuse reflection (DR) mode as a technique for measuring α-quartz in respirable mine dust. A DR accessory was used to analyze lab-generated respirable samples of Min-U-Sil 5 (which contains more than 90% α-quartz) and coal dust, at mass loadings in the ranges of 100-600 μg and 600-5300 μg, respectively. The dust samples were deposited onto three different types of filters, borosilicate fiberglass, nylon, and polyvinyl chloride (PVC). The reflectance, R, was calculated by the ratio of a blank filter and a filter with deposited mine dust. Results suggest that for coal and pure quartz dusts deposited on 37 mm PVC filters, measurements of -log R correlate linearly with known amounts of quartz on filters, with R(2) values of approximately 0.99 and 0.94, respectively, for samples loaded up to ∼4000 μg. Additional tests were conducted to measure quartz in coal dusts deposited onto the borosilicate fiberglass and nylon filter media used in the NIOSH-developed Personal Dust Monitor (PDM). The nylon filter was shown to be amenable to DR analysis, but quantification of quartz is more accurate when the filter is "free," as opposed to being mounted in the PDM filter holder. The borosilicate fiberglass filters were shown to produce excessive

  6. Relative influence of surficial, climatic, and plate tectonic processes on the development of thick Paleoproterozoic quartz arenite successions

    Science.gov (United States)

    Corcoran, P.; Bynoe, L.

    2010-12-01

    Quartz arenites are significant components of the rock record and appear to be most abundant during specific time intervals in Earth history. Thick quartz arenite successions are typical in Precambrian strata and have been associated with extensive cratonization during the late Archean to early Proterozoic. These supermature sandstones can also be attributed to the intense weathering conditions of early Earth’s atmosphere, source rocks rich in quartz, recycling and diagenesis, or simply the higher preservation potential of quartz compared with other minerals. Modern quartz-rich sands develop in low relief settings where high residence times contribute to chemical breakdown of labile grains. The lack of land vegetation during the Precambrian would have precluded confined sedimentation patterns and stabilization of soils, both of which enhance sediment residence times. Thus, the generation of first-cycle late Archean quartz arenites in fault-controlled, high relief basins necessitates periods of intense chemical weathering. The inferred change from a greenhouse to oxygenated atmosphere at around 2.3-2.2 Ga could have been the major control on the relative change to thinner units of pure sandstones with time. In order to test this hypothesis, detailed facies and compositional analyses are being conducted on the ca. 2.2 Ga Bar River Formation of the Huronian Supergroup, Canada. Four groups comprise Huronian stratigraphy, three of which contain basal glaciogenic conglomerates, followed by mudstone-dominated then quartz-rich formations. It has been suggested that these tripartite cycles could have been climatically controlled. Detailed facies analysis of the 500-750 m thick quartz arenite indicates shallow water, wave-influenced settings, akin to shoreface environments along extensive stable shelves. Thin mudstone interbeds, representing brief periods of suspension sedimentation, have been sampled for geochemical analysis in order to determine the degree of chemical

  7. A Z-axis Quartz Cross-fork Micromachined Gyroscope Based on Shear Stress Detection

    Directory of Open Access Journals (Sweden)

    Peitao Dong

    2010-03-01

    Full Text Available Here we propose a novel quartz micromachined gyroscope. The sensor has a simple cross-fork structure in the x-y plane of quartz crystal. Shear stress rather than normal stress is utilized to sense Coriolis’ force generated by the input angular rate signal. Compared to traditional quartz gyroscopes, which have two separate sense electrodes on each sidewall, there is only one electrode on each sidewall of the sense beam. As a result, the fabrication of the electrodes is simplified and the structure can be easily miniaturized. In order to increase sensitivity, a pair of proof masses is attached to the ends of the drive beam, and the sense beam has a tapered design. The structure is etched from a z-cut quartz wafer and the electrodes are realized by direct evaporation using the aperture mask method. The drive mode frequency of the prototype is 13.38 kHz, and the quality factor is approximately 1,000 in air. Therefore, the gyroscope can work properly without a vacuum package. The measurement ability of the shear stress detection design scheme is validated by the Coriolis’ force test. The performance of the sensor is characterized on a precision rate table using a specially designed readout circuit. The experimentally obtained scale factor is 1.45 mV/°/s and the nonlinearity is 3.6% in range of ±200 °/s.

  8. Phase-referenced nonlinear spectroscopy of the α-quartz/water interface

    Science.gov (United States)

    Ohno, Paul E.; Saslow, Sarah A.; Wang, Hong-Fei; Geiger, Franz M.; Eisenthal, Kenneth B.

    2016-12-01

    Probing the polarization of water molecules at charged interfaces by second harmonic generation spectroscopy has been heretofore limited to isotropic materials. Here we report non-resonant nonlinear optical measurements at the interface of anisotropic z-cut α-quartz and water under conditions of dynamically changing ionic strength and bulk solution pH. We find that the product of the third-order susceptibility and the interfacial potential, χ(3) × Φ(0), is given by (χ1(3)-iχ2(3)) × Φ(0), and that the interference between this product and the second-order susceptibility of bulk quartz depends on the rotation angle of α-quartz around the z axis. Our experiments show that this newly identified term, iχ(3) × Φ(0), which is out of phase from the surface terms, is of bulk origin. The possibility of internally phase referencing the interfacial response for the interfacial orientation analysis of species or materials in contact with α-quartz is discussed along with the implications for conditions of resonance enhancement.

  9. High-Spin Cobalt Hydrides for Catalysis

    Energy Technology Data Exchange (ETDEWEB)

    Holland, Patrick L. [Univ. of Rochester, NY (United States)

    2013-08-29

    Organometallic chemists have traditionally used catalysts with strong-field ligands that give low-spin complexes. However, complexes with a weak ligand field have weaker bonds and lower barriers to geometric changes, suggesting that they may lead to more rapid catalytic reactions. Developing our understanding of high-spin complexes requires the use of a broader range of spectroscopic techniques, but has the promise of changing the mechanism and/or selectivity of known catalytic reactions. These changes may enable the more efficient utilization of chemical resources. A special advantage of cobalt and iron catalysts is that the metals are more abundant and cheaper than those currently used for major industrial processes that convert unsaturated organic molecules and biofeedstocks into useful chemicals. This project specifically evaluated the potential of high-spin cobalt complexes for small-molecule reactions for bond rearrangement and cleavage reactions relevant to hydrocarbon transformations. We have learned that many of these reactions proceed through crossing to different spin states: for example, high-spin complexes can flip one electron spin to access a lower-energy reaction pathway for beta-hydride elimination. This reaction enables new, selective olefin isomerization catalysis. The high-spin cobalt complexes also cleave the C-O bond of CO2 and the C-F bonds of fluoroarenes. In each case, the detailed mechanism of the reaction has been determined. Importantly, we have discovered that the cobalt catalysts described here give distinctive selectivities that are better than known catalysts. These selectivities come from a synergy between supporting ligand design and electronic control of the spin-state crossing in the reactions.

  10. Diagenetic Quartz Morphologies and Zeolite formation

    DEFF Research Database (Denmark)

    Kazerouni, Afsoon Moatari; Hansen, Rikke Weibel; Friis, Henrik

    ; the core of the zeolite crystals appears to have been more unstable than the rim and dissolved first.  Later the entire crystal dissolved and left an impression of the euhedral zeolite crystal in the microquartz coating.  Such openings in the microquartz coating are nucleation points for macroquartz.  Thus......, the precipitation of zeolite may later facilitate further quartz cementation, which might otherwise be retarded by the presence of disordered microquartz. The silica activity of pore fluids can influence zeolite precipitation.  Although zeolite formation is clearly related to volcanic ash, zeolite has also formed...... are abundant in some of associated shales; and 2) volcanic ash. The dissolution of biogenic silica may result in a rapid release of silica thereby promoting the formation of diagenetic opal/microquartz, but there may be a limited release of Al. A limited release of Al may result in precipitation of Si...

  11. Quartz tuning fork based microwave impedance microscopy

    Science.gov (United States)

    Cui, Yong-Tao; Ma, Eric Yue; Shen, Zhi-Xun

    2016-06-01

    Microwave impedance microscopy (MIM), a near-field microwave scanning probe technique, has become a powerful tool to characterize local electrical responses in solid state samples. We present the design of a new type of MIM sensor based on quartz tuning fork and electrochemically etched thin metal wires. Due to a higher aspect ratio tip and integration with tuning fork, such design achieves comparable MIM performance and enables easy self-sensing topography feedback in situations where the conventional optical feedback mechanism is not available, thus is complementary to microfabricated shielded stripline-type probes. The new design also enables stable differential mode MIM detection and multiple-frequency MIM measurements with a single sensor.

  12. Phase I. Lanthanum-based Start Materials for Hydride Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Gschneidner, K. A. [Ames Lab., Ames, IA (United States); Schmidt, F. A. [Ames Lab., Ames, IA (United States); Frerichs, A. E. [Ames Lab., Ames, IA (United States); Ament, K. A. [Ames Lab., Ames, IA (United States)

    2013-08-20

    The purpose of Phase I of this work is to focus on developing a La-based start material for making nickel-metal (lanthanum)-hydride batteries based on our carbothermic-silicon process. The goal is to develop a protocol for the manufacture of (La1-xRx)(Ni1-yMy)(Siz), where R is a rare earth metal and M is a non-rare earth metal, to be utilized as the negative electrode in nickel-metal hydride (NiMH) rechargeable batteries.

  13. Review of magnesium hydride-based materials: development and optimisation

    Science.gov (United States)

    Crivello, J.-C.; Dam, B.; Denys, R. V.; Dornheim, M.; Grant, D. M.; Huot, J.; Jensen, T. R.; de Jongh, P.; Latroche, M.; Milanese, C.; Milčius, D.; Walker, G. S.; Webb, C. J.; Zlotea, C.; Yartys, V. A.

    2016-02-01

    Magnesium hydride has been studied extensively for applications as a hydrogen storage material owing to the favourable cost and high gravimetric and volumetric hydrogen densities. However, its high enthalpy of decomposition necessitates high working temperatures for hydrogen desorption while the slow rates for some processes such as hydrogen diffusion through the bulk create challenges for large-scale implementation. The present paper reviews fundamentals of the Mg-H system and looks at the recent advances in the optimisation of magnesium hydride as a hydrogen storage material through the use of catalytic additives, incorporation of defects and an understanding of the rate-limiting processes during absorption and desorption.

  14. Hydride formation in core-shell alloyed metal nanoparticles

    Science.gov (United States)

    Zhdanov, Vladimir P.

    2016-07-01

    The model and analysis presented are focused on hydride formation in nanoparticles with a Pd shell and a core formed by another metal. The arrangement of metal atoms is assumed to be coherent (no dislocations). The lattice strain distribution, elastic energy, and chemical potential of hydrogen atoms are scrutinized. The slope of the chemical potential (as a function of hydrogen uptake) is demonstrated to decrease with increasing the core volume, and accordingly the critical temperature for hydride formation and the corresponding hysteresis loops are predicted to decrease as well.

  15. Hydrogen Desorption from Mg Hydride: An Ab Initio Study

    Directory of Open Access Journals (Sweden)

    Simone Giusepponi

    2012-07-01

    Full Text Available Hydrogen desorption from hydride matrix is still an open field of research. By means of accurate first-principle molecular dynamics (MD simulations an Mg–MgH2 interface is selected, studied and characterized. Electronic structure calculations are used to determine the equilibrium properties and the behavior of the surfaces in terms of structural deformations and total energy considerations. Furthermore, extensive ab-initio molecular dynamics simulations are performed at several temperatures to characterize the desorption process at the interface. The numerical model successfully reproduces the experimental desorption temperature for the hydride.

  16. Ab-initio study of transition metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Ramesh [Dept. of Physics, Feroze Gandhi Insititute of Engineering and Technology, Raebareli-229001 (India); Shukla, Seema, E-mail: sharma.yamini62@gmail.com; Dwivedi, Shalini, E-mail: sharma.yamini62@gmail.com; Sharma, Yamini, E-mail: sharma.yamini62@gmail.com [Theoretical Condensed Matter Physics Laboratory, Dept. of Physics Feroze Gandhi College, Raebareli-229001 (India)

    2014-04-24

    We have performed ab initio self consistent calculations based on Full potential linearized augmented plane wave (FP-LAPW) method to investigate the optical and thermal properties of yttrium hydrides. From the band structure and density of states, the optical absorption spectra and specific heats have been calculated. The band structure of Yttrium metal changes dramatically due to hybridization of Y sp orbitals with H s orbitals and there is a net charge transfer from metal to hydrogen site. The electrical resistivity and specific heats of yttrium hydrides are lowered but the thermal conductivity is slightly enhanced due to increase in scattering from hydrogen sites.

  17. Metal hydride heat pump engineering demonstration and evaluation model

    Science.gov (United States)

    Lynch, Franklin E.

    1993-01-01

    Future generations of portable life support systems (PLSS's) for space suites (extravehicular mobility units or EMU's) may require regenerable nonventing thermal sinks (RNTS's). For purposes of mobility, a PLSS must be as light and compact as possible. Previous venting PLSS's have employed water sublimators to reject metabolic and equipment heat from EMU's. It is desirable for long-duration future space missions to minimize the use of water and other consumables that need to be periodically resupplied. The emission of water vapor also interferes with some types of instrumentation that might be used in future space exploration. The test article is a type of RNTS based on a metal hydride heat pump (MHHP). The task of reservicing EMU's after use must be made less demanding in terms of time, procedures, and equipment. The capability for quick turnaround post-EVA servicing (30 minutes) is a challenging requirement for many of the RNTS options. The MHHP is a very simple option that can be regenerated in the airlock within the 30 minute limit by the application of a heating source and a cooling sink. In addition, advanced PLSS's must provide a greater degree of automatic control, relieving astronauts of the need to manually adjust temperatures in their liquid cooled ventilation garments (LCVG's). The MHHP includes automatic coolant controls with the ability to follow thermal load swings from minimum to maximum in seconds. The MHHP includes a coolant loop subsystem with pump and controls, regeneration equipment for post-EVA servicing, and a PC-based data acquisition and control system (DACS).

  18. Exploring "aerogen-hydride" interactions between ZOF2 (Z = Kr, Xe) and metal hydrides: An ab initio study

    Science.gov (United States)

    Esrafili, Mehdi D.; Mohammadian-Sabet, Fariba

    2016-06-01

    In this work, a new σ-hole interaction formed between ZOF2 (Z = Kr and Xe) as the Lewis acid and a series of metal-hydrides HMX (M = Be, Mg, Zn and X = H, F, CN, CH3) is reported. The nature of this interaction, called "aerogen-hydride" interaction, is unveiled by molecular electrostatic potential, non-covalent interaction, quantum theory of atoms in molecules and natural bond orbital analyses. Our results indicate that the aerogen-hydride interactions are quite strong and can be comparable in strength to other σ-hole bonds. An important charge-transfer interaction is also associated with the formation of OF2Z⋯HMX complexes.

  19. Facile preparation of an immobilized surfactant-free palladium nanocatalyst for metal hydride trapping: a novel sensing platform for TXRF analysis.

    Science.gov (United States)

    Romero, V; Costas-Mora, I; Lavilla, I; Bendicho, C

    2015-02-07

    In this work, a simple route for the synthesis of surfactant-free immobilized palladium nanoparticles (Pd NPs) and their use as effective nanocatalysts for metal hydride decomposition is described. A mixture of ethanol : water was used as the reducing agent. Ethanol was added in a large excess to reduce the ionic Pd and stabilize the obtained Pd NPs. Ethanol is adsorbed on the surface of Pd allowing steric stabilization. Freshly prepared Pd NPs were immobilized onto quartz substrates modified with 3-mercaptopropyltrimethoxysilane. Pd interacts with the thiol group of the alkoxysilane that is adsorbed on the surface of NPs without the dissociation of the S-H bond. Different parameters affecting the synthesis of Pd NPs and their immobilization onto quartz substrates were evaluated. A comprehensive characterization of the synthesized Pd NPs was carried out by transmission electron microscopy (TEM), whereas total reflection X-ray fluorescence (TXRF) spectrometry was applied in order to evaluate their catalytic activity for solid-gas reactions. Immobilized Pd NPs were applied as nanocatalysts for the dissociative chemisorption of arsine at room temperature, yielding the formation of As-Pd bonds. Quartz substrates coated with nanosized Pd could be used as novel sensing platforms for total reflection X-ray fluorescence analysis. Arsenic can be detected in situ in natural water with a limit of detection of 0.08 μg L(-1).

  20. Quartz enhanced photoacoustic spectroscopy based trace gas sensors using different quartz tuning forks.

    Science.gov (United States)

    Ma, Yufei; Yu, Guang; Zhang, Jingbo; Yu, Xin; Sun, Rui; Tittel, Frank K

    2015-03-27

    A sensitive trace gas sensor platform based on quartz-enhanced photoacoustic spectroscopy (QEPAS) is reported. A 1.395 μm continuous wave (CW), distributed feedback pigtailed diode laser was used as the excitation source and H2O was selected as the target analyte. Two kinds of quartz tuning forks (QTFs) with a resonant frequency (f0) of 30.72 kHz and 38 kHz were employed for the first time as an acoustic wave transducer, respectively for QEPAS instead of a standard QTF with a f0 of 32.768 kHz. The QEPAS sensor performance using the three different QTFs was experimentally investigated and theoretically analyzed. A minimum detection limit of 5.9 ppmv and 4.3 ppmv was achieved for f0 of 32.768 kHz and 30.72 kHz, respectively.

  1. A new irradiated quartz for beta source calibration

    DEFF Research Database (Denmark)

    Hansen, Vicki; Murray, Andrew Sean; Buylaert, Jan-Pieter;

    2015-01-01

    laboratories have used the various different batches of Risø calibration quartz for the calibration of beta and X-ray sources, but these have been largely undescribed. Here we describe in detail the preparation and luminescence characteristics of a new quartz standard, based on a North Sea beach sand collected...

  2. Quartz exposure in agriculture: literature review and South African survey.

    NARCIS (Netherlands)

    Swanepoel, A.J.; Rees, D.; Renton, K.; Swanepoel, C.; Kromhout, H.; Gardiner, K.

    2010-01-01

    OBJECTIVES: To review the published literature on respirable quartz exposure and associated disease in agricultural related settings systematically and to describe personal respirable dust and quartz measurements collected on a sandy soil farm in the Free State province of South Africa. METHODS: The

  3. Thermal quenching of thermoluminescence in quartz samples of various origin

    Energy Technology Data Exchange (ETDEWEB)

    Subedi, B. [Aristotle University of Thessaloniki, Nuclear Physics Laboratory, 54124-Thessaloniki (Greece); Oniya, E. [Archaeometry Laboratory, Cultural and Educational Technology Institute (C.E.T.I.), R.C. ' Athena' , Tsimiski 58, 67100 Xanthi (Greece); Physics and Electronics Department, Adekunle Ajasin University, PMB 01, Akungba Akoko (Nigeria); Polymeris, G.S. [ISIK University, Physics Department, Faculty of Science and Arts, 34980-Sile, Istanbul (Turkey); Afouxenidis, D.; Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute (C.E.T.I.), R.C. ' Athena' , Tsimiski 58, 67100 Xanthi (Greece); Kitis, G., E-mail: gkitis@auth.g [Aristotle University of Thessaloniki, Nuclear Physics Laboratory, 54124-Thessaloniki (Greece)

    2011-03-15

    The effect of thermal quenching stands among the most important properties in the thermoluminescence (TL) of quartz on which many applications of TL are based. Since the quartz samples used in various applications are all of different origin it is useful to investigate whether the values of the thermal quenching parameters, i.e. the activation energy for thermal quenching W and a parameter C which describes the ratio of non-radiative to radiative luminescence transitions, evaluated mainly in specific quartz samples can be extrapolated to quartz samples of unknown origin as well as to quartz samples which are annealed at high temperatures. In the present work the TL glow curve of a series of un-annealed and annealed natural and synthetic quartz samples were studied as a function of the heating rate between 0.25 K/s and 16 K/s. Using an indirect fitting method it was found that the thermal quenching parameters W and C in most of the quartz samples are very similar to the values accepted in the literature. Furthermore, in some cases the thermal quenching parameters W and C are not the same for all TL glow-peaks in the same glow-curve. Finally, the strong external treatment of annealing the quartz samples at very high temperature can also influence at least one of the thermal quenching parameters.

  4. Recent developments of OSL techniques for dating quartz and feldspars

    DEFF Research Database (Denmark)

    Bøtter-Jensen, L.; Jungner, H.; Mejdahl, V.

    1993-01-01

    The construction of a unit for measuring optically stimulated luminescence from quartz and feldspar is described. The light sources used for stimulation are infrared diodes for feldspar and green light from a halogen lamp (obtained with a system of filters) for both quartz and feldspar. The unit ...

  5. Speciation and phase separation of water in quartz (A review ...

    African Journals Online (AJOL)

    Speciation and phase separation of water in quartz (A review) ... of quartz at temperatures in excess of 500 °C. leading to decomposition of the ... The nucleation is a first order phase transition of creating liquid nucleus within the vapour phase, ...

  6. Removal of Ozone by Carbon Nanotubes/Quartz Fiber Film.

    Science.gov (United States)

    Yang, Shen; Nie, Jingqi; Wei, Fei; Yang, Xudong

    2016-09-01

    Ozone is recognized as a harmful gaseous pollutant, which can lead to severe human health problems. In this study, carbon nanotubes (CNTs) were tested as a new approach for ozone removal. The CNTs/quartz fiber film was fabricated through growth of CNTs upon pure quartz fiber using chemical vapor deposition method. Ozone conversion efficiency of the CNTs/quartz fiber film was tested for 10 h and compared with that of quartz film, activated carbon (AC), and a potassium iodide (KI) solution under the same conditions. The pressure resistance of these materials under different airflow rates was also measured. The results showed that the CNTs/quartz fiber film had better ozone conversion efficiency but also higher pressure resistance than AC and the KI solution of the same weight. The ozone removal performance of the CNTs/quartz fiber film was comparable with AC at 20 times more weight. The CNTs played a dominant role in ozone removal by the CNTs/quartz fiber film. Its high ozone conversion efficiency, lightweight and free-standing properties make the CNTs/quartz fiber film applicable to ozone removal. Further investigation should be focused on reducing pressure resistance and studying the CNT mechanism for removing ozone.

  7. Analysis of Rare Earth Elements (REE) in vein quartz and quartz-sandstone host rock in the Zhelannoe high purity quartz deposit, Russia

    Science.gov (United States)

    Zemskova, Marina; Prokofiev, Vsevolod; Bychkov, Andrey

    2015-04-01

    The Zhelannoe high purity quartz deposit is located on the western slope of the Polar Urals. It is one of the largest deposits of vein quartz and rock crystal in Russia. Most of the mineralization is hosted within a single horizon of very firm quartz-sandstone, where plastic deformation did not occur almost entirely. All tectonic stress was released by the development of numerous thrust faults of different scales. Cavities formed during this process were later filled with quartz and rock crystal. In order to obtain more details on conditions under which mineralization took place, analysis of trace element contents in vein quartz and host rocks, and the micro-thermometric study of fluid inclusions in quartz have been carried out. The trace element composition of vein quartz and of the host rock has been determined by ICP-MS. The results have shown that concentrations of most of the 46 studied elements in quartz are two orders of magnitude lower than in chondrite, and more than three orders of magnitude lower than in the upper crust. Even though Pb and Li have the highest concentrations in quartz samples, levels are only nearly comparable in chondrite, and substantially lower in the upper crust. At the same time, negative anomalies of Pb and Li concentrations in the host rock may indicate the removal of these elements during vein quartz formation. Contents of most REEs are two orders of magnitude lower than in chondrite, and three orders of magnitude lower than in the host rock. Generally, the patterns of REE distribution in vein quartz and the host rock express a clear correlation; confirming the genetic link between vein quartz and quartz-sandstone host rock. However, the process of quartz recrystallization led to an intense decrease of REEs content, and of all other impurities, which consequently influenced industrial value of the Zhelannoe deposit. As a result of the micro-thermometric study of fluid inclusions in quartz, the following physical

  8. Mg含量对氢化燃烧合成MgH2水解制氢性能的影响%Effect of Mg Additive on Hydrogen Generation via Hydrolysis of MgH2 Prepared by Hydriding Combustion Synthesis

    Institute of Scientific and Technical Information of China (English)

    孙陈诚; 王金; 刘虎; 朱云峰; 李李泉

    2015-01-01

    系统研究了Mg的添加量及球磨时间对氢化燃烧合成(Hydriding Combustion Synthesis,HCS) MgH2在MgC12溶液中水解释氢动力学性能的影响.MgH2-60%Mg(质量分数,下同)经3h球磨后在5 min内释氢量为993 mL/g(转化率达80%),经15 min可完全水解,副产物为单一的Mg(OH)2.研究表明:镁的添加在降低制氢成本的同时,一方面可提高释氢动力学性能,另一方面也便于副产物回收再生.

  9. 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

  10. 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.

  11. Quartz in coal dust deposited on internal surface of respirable size selective samplers.

    Science.gov (United States)

    Soo, Jhy-Charm; Lee, Taekhee; Kashon, Michael; Kusti, Mohannad; Harper, Martin

    2014-01-01

    The objective of the present study is to quantify quartz mass in coal dust deposited on the internal cassette surface of respirable size-selective samplers. Coal dust was collected with four different respirable size-selective samplers (10 mm Dorr-Oliver nylon [Sensidyne, St. Petersburg, Fla.], SKC Aluminum [SKC Inc., Eighty Four, Pa.], BGI4L [BGI USA Inc., Waltham, Mass.], and GK2.69 cyclones [BGI USA Inc.]) with two different cassette types (polystyrene and static-dissipative polypropylene cassettes). The coal dust was aerosolized in a calm air chamber by using a fluidized bed aerosol generator without neutralization under the assumption that the procedure is similar to field sampling conditions. The mass of coal dust was measured gravimetrically and quartz mass was determined by Fourier transform infrared spectroscopy according to the National Institute for Occupational Safety and Health (NIOSH) Manual of Analytical Methods, Method 7603. The mass fractions of the total quartz sample on the internal cassette surface are significantly different between polystyrene and static-dissipative cassettes for all cyclones (p quartz mass on cassette internal surface and coal dust filter mass was observed. The BGI4L cyclone showed a higher (but not significantly) and the GK2.69 cyclone showed a significantly lower (p quartz mass fraction for polystyrene cassettes compared to other cyclones. This study confirms previous observations that the interior surface deposits in polystyrene cassettes attached to cyclone pre-selectors can be a substantial part of the sample, and therefore need to be included in any analysis for accurate exposure assessment. On the other hand, the research presented here supports the position that the internal surface deposits in static-dissipative cassettes used with size-selective cyclones are negligible and that it is only necessary to analyze the filter catch.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-01

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

  13. 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

  14. Pore confined synthesis of magnesium boron hydride nanoparticles

    NARCIS (Netherlands)

    Au, Yuen S.; Yan, Yigang; De Jong, Krijn P.; Remhof, Arndt; De Jongh, Petra E.

    2014-01-01

    Nanostructured materials based on light elements such as Li, Mg, and Na are essential for energy storage and conversion applications, but often difficult to prepare with control over size and structure. We report a new strategy that is illustrated for the formation of magnesium boron hydrides,

  15. Novel baker's yeast catalysed hydride reduction of an epoxide moiety

    CSIR Research Space (South Africa)

    Horak, RM

    1995-02-27

    Full Text Available -4039(95)00043-7 Tetrahedron Letters, Vol. 36, No. 9, pp. 1541-1544, 1995 Elsevier Science Ltd Printed in Great Britain 0040-4039/95 $9.50+0.00 A Novel Baker's Yeast Catalysed Hydride Reduction of an Epoxide Moiety R. Marthinus Horak, Robin A...

  16. Release of hydrogen from nanoconfined hydrides by application of microwaves

    Science.gov (United States)

    Sanz-Moral, Luis Miguel; Navarrete, Alexander; Sturm, Guido; Link, Guido; Rueda, Miriam; Stefanidis, Georgios; Martín, Ángel

    2017-06-01

    The release of hydrogen from solid hydrides by thermolysis can be improved by nanoconfinement of the hydride in a suitable micro/mesoporous support, but the slow heat transfer by conduction through the support can be a limitation. In this work, a C/SiO2 mesoporous material has been synthesized and employed as matrix for nanoconfinement of hydrides. The matrix showed high surface area and pore volume (386 m2/g and 1.41 cm3/g), which enabled the confinement of high concentrations of hydride. Furthermore, by modification of the proportion between C and SiO2, the dielectric properties of the complex could be modified, making it susceptible to microwave heating. As with this heating method the entire sample is heated simultaneously, the heat transfer resistances associated to conduction were eliminated. To demonstrate this possibility, ethane 1,2-diaminoborane (EDAB) was embedded on the C/SiO2 matrix at concentrations ranging from 11 to 31%wt using a wet impregnation method, and a device appropriate for hydrogen release from this material by application of microwaves was designed with the aid of a numerical simulation. Hydrogen liberation tests by conventional heating and microwaves were compared, showing that by microwave heating hydrogen release can be initiated and stopped in shorter times.

  17. 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 stora

  18. Review of magnesium hydride-based materials: development and optimisation

    NARCIS (Netherlands)

    Crivello, J. -C.; Dam, B.; Denys, R. V.; Dornheim, M.; Grant, D. M.; Huot, J.; Jensen, T. R.; de Jongh, P.; Latroche, M.; Milanese, C.; Milcius, D.; Walker, G. S.; Webb, C. J.; Zlotea, C.; Yartys, V. A.

    2016-01-01

    Magnesium hydride has been studied extensively for applications as a hydrogen storage material owing to the favourable cost and high gravimetric and volumetric hydrogen densities. However, its high enthalpy of decomposition necessitates high working temperatures for hydrogen desorption while the slo

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

    Science.gov (United States)

    Congdon, James W.

    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.

  20. Hydrogen adsorption on palladium and palladium hydride at 1 bar

    DEFF Research Database (Denmark)

    Johansson, Martin; Skulason, Egill; Nielsen, Gunver

    2010-01-01

    The dissociative sticking probability for H-2 on Pd films supported on sputtered Highly Ordered Pyrolytic Graphite (HOPG) has been derived from measurements of the rate of the H-D exchange reaction at 1 bar. The sticking probability for H-2, S. is higher on Pd hydride than on Pd (a factor of 1...

  1. Pore confined synthesis of magnesium boron hydride nanoparticles

    NARCIS (Netherlands)

    Au, Yuen S.; Yan, Yigang; De Jong, Krijn P.; Remhof, Arndt; De Jongh, Petra E.

    2014-01-01

    Nanostructured materials based on light elements such as Li, Mg, and Na are essential for energy storage and conversion applications, but often difficult to prepare with control over size and structure. We report a new strategy that is illustrated for the formation of magnesium boron hydrides, relev

  2. Superconductivity and unexpected chemistry of germanium hydrides under pressure

    Science.gov (United States)

    Davari Esfahani, M. Mahdi; Oganov, Artem R.; Niu, Haiyang; Zhang, Jin

    2017-04-01

    Following the idea that hydrogen-rich compounds might be high-Tc superconductors at high pressures, and the very recent breakthrough in predicting and synthesizing hydrogen sulfide with record-high Tc=203 K , an ab initio evolutionary algorithm for crystal structure prediction was employed to find stable germanium hydrides. In addition to the earlier structure of germane with space group Ama2, we propose a C2/m structure, which is energetically more favorable at pressures above 278 GPa (with inclusion of zero-point energy). Our calculations indicate that the C2/m phase of germane is a superconductor with Tc=67 K at 280 GPa. Germane is found to become thermodynamically unstable to decomposition to hydrogen and the compound Ge3H11 at pressures above 300 GPa. Ge3H11 with space group I 4 ¯m 2 is found to become stable at above 285 GPa with Tc=43 K . We find that the pressure-induced phase stability of germanium hydrides is distinct from analogous isoelectronic systems, e.g., Si hydrides and Sn hydrides. Superconductivity stems from large electron-phonon coupling associated with the wagging, bending, and stretching intermediate-frequency modes derived mainly from hydrogen.

  3. Structural stability of complex hydrides LiBH4 revisited

    DEFF Research Database (Denmark)

    Lodziana, Zbigniew; Vegge, Tejs

    2004-01-01

    A systematic approach to study the phase stability of LiBH4 based on ab initio calculations is presented. Three thermodynamically stable phases are identified and a new phase of Cc symmetry is proposed for the first time for a complex hydride. The x-ray diffraction pattern and vibrational spectra...

  4. Optimizing Misch-Metal Compositions In Metal Hydride Anodes

    Science.gov (United States)

    Bugga, Ratnakumar V.; Halpert, Gerald

    1995-01-01

    Electrochemical cells based on metal hydride anodes investigated experimentally in effort to find anode compositions maximizing charge/discharge-cycle performances. Experimental anodes contained misch metal alloyed with various proportions of Ni, Co, Mn, and Al, and experiments directed toward optimization of composition of misch metal.

  5. Well-defined transition metal hydrides in catalytic isomerizations.

    Science.gov (United States)

    Larionov, Evgeny; Li, Houhua; Mazet, Clément

    2014-09-07

    This Feature Article intends to provide an overview of a variety of catalytic isomerization reactions that have been performed using well-defined transition metal hydride precatalysts. A particular emphasis is placed on the underlying mechanistic features of the transformations discussed. These have been categorized depending upon the nature of the substrate and in most cases discussed following a chronological order.

  6. Nanocrystalline Metal Hydrides Obtained by Severe Plastic Deformations

    Directory of Open Access Journals (Sweden)

    Jacques Huot

    2012-01-01

    Full Text Available It has recently been shown that Severe Plastic Deformation (SPD techniques could be used to obtain nanostructured metal hydrides with enhanced hydrogen sorption properties. In this paper we review the different SPD techniques used on metal hydrides and present some specific cases of the effect of cold rolling on the hydrogen storage properties and crystal structure of various types of metal hydrides such as magnesium-based alloys and body centered cubic (BCC alloys. Results show that generally cold rolling is as effective as ball milling to enhance hydrogen sorption kinetics. However, for some alloys such as TiV0.9Mn1.1 alloy ball milling and cold rolling have detrimental effect on hydrogen capacity. The exact mechanism responsible for the change in hydrogenation properties may not be the same for ball milling and cold rolling. Nevertheless, particle size reduction and texture seems to play a leading role in the hydrogen sorption enhancement of cold rolled metal hydrides.

  7. Metal hydrides for smart window and sensor applications

    NARCIS (Netherlands)

    Yoshimura, K.; Langhammer, C.; Dam, B.

    2013-01-01

    The hydrogenation of metals often leads to changes in optical properties in the visible range. This allows for fundamental studies of the hydrogenation process, as well as the exploration of various applications using these optical effects. Here, we focus on recent developments in metal hydride-base

  8. Tribochemical Decomposition of Light Ionic Hydrides at Room Temperature.

    Science.gov (United States)

    Nevshupa, Roman; Ares, Jose Ramón; Fernández, Jose Francisco; Del Campo, Adolfo; Roman, Elisa

    2015-07-16

    Tribochemical decomposition of magnesium hydride (MgH2) induced by deformation at room temperature was studied on a micrometric scale, in situ and in real time. During deformation, a near-full depletion of hydrogen in the micrometric affected zone is observed through an instantaneous (t MgH2 with reduced crystal size by mechanical deformation.

  9. KNH2-KH: a metal amide-hydride solid solution.

    Science.gov (United States)

    Santoru, Antonio; Pistidda, Claudio; Sørby, Magnus H; Chierotti, Michele R; Garroni, Sebastiano; Pinatel, Eugenio; Karimi, Fahim; Cao, Hujun; Bergemann, Nils; Le, Thi T; Puszkiel, Julián; Gobetto, Roberto; Baricco, Marcello; Hauback, Bjørn C; Klassen, Thomas; Dornheim, Martin

    2016-09-27

    We report for the first time the formation of a metal amide-hydride solid solution. The dissolution of KH into KNH2 leads to an anionic substitution, which decreases the interaction among NH2(-) ions. The rotational properties of the high temperature polymorphs of KNH2 are thereby retained down to room temperature.

  10. Metal hydride hydrogen and heat storage systems as enabling technology for spacecraft applications

    Energy Technology Data Exchange (ETDEWEB)

    Reissner, Alexander, E-mail: reissner@fotec.at [FOTEC Forschungs- und Technologietransfer GmbH, Viktor Kaplan Straße 2, 2700 Wiener Neustadt (Austria); University of Applied Sciences Wiener Neustadt, Johannes Gutenberg-Straße 3, 2700 Wiener Neustadt (Austria); Pawelke, Roland H.; Hummel, Stefan; Cabelka, Dusan [FOTEC Forschungs- und Technologietransfer GmbH, Viktor Kaplan Straße 2, 2700 Wiener Neustadt (Austria); Gerger, Joachim [University of Applied Sciences Wiener Neustadt, Johannes Gutenberg-Straße 3, 2700 Wiener Neustadt (Austria); Farnes, Jarle, E-mail: Jarle.farnes@prototech.no [CMR Prototech AS, Fantoftvegen 38, PO Box 6034, 5892 Bergen (Norway); Vik, Arild; Wernhus, Ivar; Svendsen, Tjalve [CMR Prototech AS, Fantoftvegen 38, PO Box 6034, 5892 Bergen (Norway); Schautz, Max, E-mail: max.schautz@esa.int [European Space Agency, ESTEC – Keplerlaan 1, 2201 AZ Noordwijk Zh (Netherlands); Geneste, Xavier, E-mail: xavier.geneste@esa.int [European Space Agency, ESTEC – Keplerlaan 1, 2201 AZ Noordwijk Zh (Netherlands)

    2015-10-05

    Highlights: • A metal hydride tank concept for heat and hydrogen storage is presented. • The tank is part of a closed-loop reversible fuel cell system for space application. • For several engineering issues specific to the spacecraft application, solutions have been developed. • The effect of water contamination has been approximated for Ti-doped NaAlH{sub 4}. • A novel heat exchanger design has been realized by Selective Laser Melting. - Abstract: The next generation of telecommunication satellites will demand a platform payload performance in the range of 30+ kW within the next 10 years. At this high power output, a Regenerative Fuel Cell Systems (RFCS) offers an efficiency advantage in specific energy density over lithium ion batteries. However, a RFCS creates a substantial amount of heat (60–70 kJ per mol H{sub 2}) during fuel cell operation. This requires a thermal hardware that accounts for up to 50% of RFCS mass budget. Thus the initial advantage in specific energy density is reduced. A metal hydride tank for combined storage of heat and hydrogen in a RFCS may overcome this constraint. Being part of a consortium in an ongoing European Space Agency project, FOTEC is building a technology demonstrator for such a combined hydrogen and heat storage system.

  11. Electrochemical Detection of Transient Cobalt Hydride Intermediates of Electrocatalytic Hydrogen Production.

    Science.gov (United States)

    Wiedner, Eric S; Bullock, R Morris

    2016-07-06

    A large variety of molecular cobalt complexes are used as electrocatalysts for H2 production, but the key cobalt hydride intermediates are frequently difficult to detect and characterize due to their high reactivity. We report that a combination of variable scan rate cyclic voltammetry and foot-of-the-wave analysis (FOWA) can be used to detect transient Co(III)H and Co(II)H intermediates of electrocatalytic H2 production by [Co(II)(P(tBu)2N(Ph)2)(CH3CN)3](2+) and Co(II)(dmgBF2)2(CH3CN)2. In both cases, reduction of a transient catalytic intermediate occurs at a potential that coincides with the Co(II/I) couple. Each reduction displays quasireversible electron-transfer kinetics, consistent with reduction of a Co(III)H intermediate to Co(II)H, which is then protonated by acid to generate H2. A bridge-protonated Co(I) species was ruled out as a catalytic intermediate for Co(II)(dmgBF2)2(CH3CN)2 from voltammograms recorded at 1000 psi of H2. Density functional theory was used to calculate Co(III)-H and Co(II)-H bond strengths for both catalysts. Despite having very different ligands, the cobalt hydrides of both catalysts possess nearly identical heterolytic and homolytic Co-H bond strengths for the Co(III)H and Co(II)H intermediates.

  12. Rat strain differences in levels and effects of chronic inflammation due to intratracheal instillation of quartz on lung tumorigenesis induced by DHPN.

    Science.gov (United States)

    Nakano, Yuko; Yokohira, Masanao; Hashimoto, Nozomi; Yamakawa, Keiko; Kishi, Sosuke; Ninomiya, Fumiko; Kanie, Shohei; Saoo, Kousuke; Imaida, Katsumi

    2014-10-01

    Chronic inflammatory effects of single intratracheal instillation (i.t.) of quartz on rat lung tumorigenesis were examined using 4 different animal models. At first, in order to determine an appropriate dose of quartz i.t. to promote lung tumorigenesis, F344 male rats were administrated single 0, 0.5, 1, 2 or 4 mg quartz/rat after initiation by N-bis(2-hydroxypropyl) nitrosamine (DHPN). Further studies were performed to examine strain differences of the effects of chronic inflammation caused by quartz i.t. in 3 strains of rat, i.e. F344, Wistar-Hannover and SD. Each was instilled with 2mg quartz/rat after DHPN administration and sacrificed in week 24. In addition, strain differences in generation of inflammation were determined at days 1 and 28. Finally, for determination of long-term effects period, F344 and Wistar-Hannover rats were similarly treated, but the experiment was terminated at week 52. In F344 rats, the tumor areas in DHPN treated groups showed a tendency to increase along with the dose of quartz. F344 rats demonstrated the highest and Wistar-Hannover rats the lowest sensitivity to quartz in acute and chronic phases in the 3 strains. In 52 week, in F344 rats, the multiplicity of tumors and the serum concentration of IL-6 in the group treated with DHPN and quartz were significantly increased. The present experiments indicated that chronic inflammation due to quartz instillation exerted promoting effects on lung carcinogenesis in F344, SD and Wistar-Hannover rats. The strain differences in tumor promotion appeared to correlate with inflammatory reactions to quartz and increase of IL-6.

  13. Physico-chemical properties of quartz from industrial manufacturing and its cytotoxic effects on alveolar macrophages: The case of green sand mould casting for iron production.

    Science.gov (United States)

    Di Benedetto, Francesco; Gazzano, Elena; Tomatis, Maura; Turci, Francesco; Pardi, Luca A; Bronco, Simona; Fornaciai, Gabriele; Innocenti, Massimo; Montegrossi, Giordano; Muniz Miranda, Maurizio; Zoleo, Alfonso; Capacci, Fabio; Fubini, Bice; Ghigo, Dario; Romanelli, Maurizio

    2016-07-15

    Industrial processing of materials containing quartz induces physico-chemical modifications that contribute to the variability of quartz hazard in different plants. Here, modifications affecting a quartz-rich sand during cast iron production, have been investigated. Composition, morphology, presence of radicals associated to quartz and reactivity in free radical generation were studied on a raw sand and on a dust recovered after mould dismantling. Additionally, cytotoxicity of the processed dust and ROS and NO generation were evaluated on MH-S macrophages. Particle morphology and size were marginally affected by casting processing, which caused only a slight increase of the amount of respirable fraction. The raw sand was able to catalyze OH and CO2(-) generation in cell-free test, even if in a lesser extent than the reference quartz (Min-U-Sil), and shows hAl radicals, conventionally found in any quartz-bearing raw materials. Enrichment in iron and extensive coverage with amorphous carbon were observed during processing. They likely contributed, respectively, to increasing the ability of processed dust to release CO2- and to suppressing OH generation respect to the raw sand. Carbon coverage and repeated thermal treatments during industrial processing also caused annealing of radiogenic hAl defects. Finally, no cellular responses were observed with the respirable fraction of the processed powder.

  14. Thin-film metal hydrides for solar energy applications

    Energy Technology Data Exchange (ETDEWEB)

    Mongstad, Trygve Tveiteraas

    2012-11-01

    Thin-film metal hydrides may become important solar energy materials in the future. This thesis demonstrates interesting material properties of metal hydride films, relevant for applications as semiconducting materials for photovoltaic (PV) solar cells and for regulation of light using smart window technology.The work presented here has comprised an experimental study, focusing on three different materials: Magnesium hydride (MgH2), magnesium nickel hydride (Mg2NiH4) and yttrium hydride (YHx). Reactive sputter deposition was used to prepare the metal hydride film samples.This synthesis method is relatively uncommon for metal hydrides. Here,the first demonstration of reactive sputtering synthesis for YHx and Mg2NiH4 is given. Different challenges in forming singlephase, pure metal hydrides were identified: MgH2 could not be deposited without 3-16% metallic Mg present in the films, and YHx was found to react strong-ly to oxygen (O) during the deposition process. On the other hand, Mg2NiH4 films formed easily and apparently without major metallic clusters and with low O content.Mg2NiH4 is a semiconductor with an optical band gap that is suitable for PV solar cells. This study has showed that films with promising electrical and optical properties can be synthesized using reactive cosputtering of Mg and Ni. Using optical methods, the band gap for the as deposited samples was estimated to 1.54-1.76 eV, depending on the Mg-Ni composition. The asdeposited films were amorphous or nano-crystalline, but could be crystallized into the high-temperature fcc structure of Mg2NiH4 using heat treatment at 523 K. The band gap of the crystalline films was 2.1-2.2 eV, depending on the composition.A pronounced photochromic reaction to visible and UV light was observed for transparent yttrium hydride (T-YHx) samples. The optical transmission was reduced when the samples were illuminated, and the original optical transmission was restored when the samples were kept under dark conditions

  15. 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

  16. Metal Hydrides as hot carrier cell absorber materials

    Science.gov (United States)

    Wang, Pei; Wen, Xiaoming; Shrestha, Santosh; Conibeer, Gavin; Aguey-Zinsou, Kondo-Francois

    2016-09-01

    The hot Carrier Solar Cell (HCSC) allows the photon-induced hot carriers (the carriers with energy larger than the band gap) to be collected before they completely thermalise. The absorber of the HCSC should have a large phononic band gap to supress Klemens Decay, which results in a slow carrier cooling speed. In fact, a large phononic band gap likely exists in a binary compound whose constituent elements have a large mass ratio between each other. Binary hydrides with their overwhelming mass ratio of the constituent elements are important absorber candidates. Study on different types of binary hydrides as potential absorber candidates is presented in this paper. Many binary transition metal hydrides have reported theoretical or experimental phonon dispersion charts which show large phononic band gaps. Among these hydrides, the titanium hydride (TiHX) is outstanding because of its low cost, easy fabrication process and is relatively inert to air and water. A TiHX thin film is fabricated by directly hydrogenating an evaporated titanium thin film. Characterisation shows good crystal quality and the hydrogenation process is believed to be successful. Ultrafast transient absorption (TA) spectroscopy is used to study the electron cooling time of TiHX. The result is very noisy due to the low absorption and transmission of the sample. The evolution of the TA curves has been explained by band to band transition using the calculated band structure of TiH2. Though not reliable due to the high noise, decay time fitting at 700nm and 600nm shows a considerably slow carrier cooling speed of the sample.

  17. Synthesis of hydrides by interaction of intermetallic compounds with ammonia

    Energy Technology Data Exchange (ETDEWEB)

    Tarasov, Boris P., E-mail: tarasov@icp.ac.ru [Institute of Problems of Chemical Physics of the Russian Academy of Sciences, Chernogolovka 142432 (Russian Federation); Fokin, Valentin N.; Fokina, Evelina E. [Institute of Problems of Chemical Physics of the Russian Academy of Sciences, Chernogolovka 142432 (Russian Federation); Yartys, Volodymyr A., E-mail: volodymyr.yartys@ife.no [Institute for Energy Technology, Kjeller NO 2027 (Norway); Department of Materials Science and Engineering, Norwegian University of Science and Technology, Trondheim NO 7491 (Norway)

    2015-10-05

    Highlights: • Interaction of the intermetallics A{sub 2}B, AB, AB{sub 2}, AB{sub 5} and A{sub 2}B{sub 17} with NH{sub 3} was studied. • The mechanism of interaction of the alloys with ammonia is temperature-dependent. • Hydrides, hydridonitrides, disproportionation products or metal–N–H compounds are formed. • NH{sub 4}Cl was used as an activator of the reaction between ammonia and intermetallics. • Interaction with ammonia results in the synthesis of the nanopowders. - Abstract: Interaction of intermetallic compounds with ammonia was studied as a processing route to synthesize hydrides and hydridonitrides of intermetallic compounds having various stoichiometries and types of crystal structures, including A{sub 2}B, AB, AB{sub 2}, AB{sub 5} and A{sub 2}B{sub 17} (A = Mg, Ti, Zr, Sc, Nd, Sm; B = transition metals, including Fe, Co, Ni, Ti and nontransition elements, Al and B). In presence of NH{sub 4}Cl used as an activator of the reaction between ammonia and intermetallic alloys, their interaction proceeds at rather mild P–T conditions, at temperatures 100–200 °C and at pressures of 0.6–0.8 MPa. The mechanism of interaction of the alloys with ammonia appears to be temperature-dependent and, following a rise of the interaction temperature, it leads to the formation of interstitial hydrides; interstitial hydridonitrides; disproportionation products (binary hydride; new intermetallic hydrides and binary nitrides) or new metal–nitrogen–hydrogen compounds like magnesium amide Mg(NH{sub 2}){sub 2}. The interaction results in the synthesis of the nanopowders where hydrogen and nitrogen atoms become incorporated into the crystal lattices of the intermetallic alloys. The nitrogenated materials have the smallest particle size, down to 40 nm, and a specific surface area close to 20 m{sup 2}/g.

  18. Intracavity quartz-enhanced photoacoustic sensor

    Energy Technology Data Exchange (ETDEWEB)

    Borri, S., E-mail: simone.borri@ino.it; Galli, I.; Mazzotti, D.; Giusfredi, G.; De Natale, P. [CNR-INO UOS Sesto Fiorentino and LENS, via Carrara 1, 50019 Sesto Fiorentino FI (Italy); Patimisco, P.; Scamarcio, G.; Spagnolo, V. [CNR-IFN UOS Bari and Dipartimento Interateneo di Fisica, Università degli Studi di Bari e Politecnico di Bari, via Amendola 173, 70126 Bari BA (Italy); Akikusa, N. [Development Bureau Laser Device R and D Group, Hamamatsu Photonics KK, Shizuoka 434-8601 (Japan); Yamanishi, M. [Central Research Laboratories, Hamamatsu Photonics KK, Shizuoka 434-8601 (Japan)

    2014-03-03

    We report on a spectroscopic technique named intracavity quartz-enhanced photoacoustic spectroscopy (I-QEPAS) employed for sensitive trace-gas detection in the mid-infrared spectral region. It is based on a combination of QEPAS with a buildup optical cavity. The sensor includes a distributed feedback quantum cascade laser emitting at 4.33 μm. We achieved a laser optical power buildup factor of ∼500, which corresponds to an intracavity laser power of ∼0.75 W. CO{sub 2} has been selected as the target molecule for the I-QEPAS demonstration. We achieved a detection sensitivity of 300 parts per trillion for 4 s integration time, corresponding to a noise equivalent absorption coefficient of 1.4 × 10{sup −8} cm{sup −1} and a normalized noise-equivalent absorption of 3.2 × 10{sup −10} W cm{sup −1} Hz{sup −1/2}.

  19. Identification of color development potential of quartz by Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Alkmim, Danielle G.; Lameiras, Fernando S.; Almeida, Frederico O.T., E-mail: alkmia@yahoo.com.br, E-mail: fsl@cdtn.br [Centro e Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horionte, MG (Brazil)

    2013-07-01

    Colorless quartz is usually exposed to ionizing radiation (gamma rays or high energy electron beams) to acquire different colors for jewelry. Color development is due to the presence of traces of some elements such as aluminum, iron, hydrogen, lithium, or sodium. Most quartz crystals are extracted colorless from nature and it is necessary to separate those that can develop colors from those that cannot. Irradiation tests can be used to accomplish this separation, but they take a long time. Infrared signature of colorless quartz can also be used. However, infrared spectroscopy is quite expensive, especially when using portable devices. Raman spectroscopy is now available as an inexpensive and portable technique that could provide identification of the samples of colorless quartz still in the field, facilitating the prediction for their economic exploitation. In addition, Raman spectroscopy usually requires a minimum or no sample preparation. This paper presents an investigation of the feasibility of using Raman spectroscopy as a substitute for infrared spectroscopy to predict the potential for color development of quartz. A band at 3595 cm{sup -1} in the Raman shift spectrum was observed only along the c axis of a prasiolite excited by a high power 514 nm laser. This band was not observed in quartz samples that do not develop color after irradiation. Further studies are required to identify the potential for color development by Raman spectroscopy of other types of colorless quartz. (author)

  20. Synergic effects of ion irradiations (La, Ce) and alkaline pretreatment (KOH) on hydriding kinetic property of a Mm–Ni based alloy

    Energy Technology Data Exchange (ETDEWEB)

    Abe, H., E-mail: abe.hiroshi10@jaea.go.jp [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1233 Watanuki, Takasaki, Gunma 370-1292 (Japan); Aone, S.; Morimoto, R.; Uchida, H. [Course of Applied Science, Graduate School of Engineering, Tokai University, 4-1-1 Kitakaname, Hiratsuka, Kanagawa 259-1292 (Japan)

    2013-12-15

    Highlights: •Ion irradiations by various ions onto a Mm–Ni based hydrogen storage alloy. •The generation of vacancy type defects by ion irradiations in the surface of a Mm–Ni based alloy. •The enhancement of the initial rate by the ion irradiations of the Mm surface. •The enhancement of the initial rate by an alkaline treatment of the Mm surface. -- Abstract: The ion beam irradiation is known to produce a high density of vacancy type defects in the surface region of a metal and found to be an effective method as a surface modification in order to enhance the hydriding rate of a metal. In this study, we examined synergic effects of both surface modifications of ion irradiations and alkaline treatment on the initial hydriding rate of a Mm–Ni based alloy. In this study, the irradiations by lanthanum (La) and cerium (Ce) ions combined with an alkaline KOH pretreatment were found much more effective in the enhancement of the initial hydriding rate compared with irradiations with other ions. This study reports the synergic effects of the surface modifications by the both the surface irradiations with rare earth ions of La and Ce, and an alkaline surface treatment on the hydriding kinetics.

  1. Hydride structures in Ti-aluminides subjected to high temperature and hydrogen pressure charging conditions

    Science.gov (United States)

    Legzdina, D.; Robertson, I. M.; Birnbaum, H. K.

    1991-01-01

    The distribution and chemistry of hydrides produced in single and dual phase alloys with a composition near TiAl have been investigated by using a combination of TEM and X-ray diffraction techniques. The alloys were exposed at 650 C to 13.8 MPa of gaseous H2 for 100 h. In the single-phase gamma alloy, large hydrides preferentially nucleated on the grain boundaries and matrix dislocations and a population of small hydrides was distributed throughout the matrix. X-ray and electron diffraction patterns from these hydrides indicated that they have an fcc structure with a lattice parameter of 0.45 nm. EDAX analysis of the hydrides showed that they were enriched in Ti. The hydrides were mostly removed by vacuum annealing at 800 C for 24 h. On dissolution of the hydrides, the chemistry of hydride-free regions of the grain boundary returned to the matrix composition, suggesting that Ti segregation accompanied the hydride formation rather than Ti enrichment causing the formation of the hydride.

  2. Hydriding performances and modeling of a small-scale ZrCo bed

    Energy Technology Data Exchange (ETDEWEB)

    Koo, D.; Lee, J.; Park, J.; Paek, S.; Chung, H. [KAERI-UST, Yuseong, Daejeon (Korea, Republic of); Chang, M.H.; Yun, S.H.; Cho, S.; Jung, K.J. [NFRI, Yuseong, Daejeon (Korea, Republic of)

    2015-03-15

    In order to evaluate the performance of the hydriding of a ZrCo bed, a small-scale getter bed of ZrCo was designed and fabricated. The results show that the hydriding time at room temperature was somewhat shorter than that at higher temperatures of ZrCo and that the performance of hydriding at low temperatures of ZrCo was better than that at high temperatures of ZrCo. The experimental results of the hydrogen pressure of hydriding (ZrCoH{sub 2.8}) at different temperatures were in agreement with the computed values using a numerical modeling equation but with a small difference during the first 10 minutes of the hydriding of ZrCo. The model is based on the Kozeny-Carman equation. The effect of a helium blanket on hydriding was measured and analyzed. The hydriding with no helium blanket in the primary vessel of ZrCo is much faster than that with a helium blanket. The hydriding at a helium concentration of 8% is slower than that at 0%. As the helium concentration increases, the hydriding of ZrCo decreases. The experimental results of the hydriding with 0 %, 4%, and 8% of helium concentration are in agreement with the calculated values but with minimal differences during the first 10 minutes.

  3. Effect of Nb on Cracking and Hydrogen Content of Zirconium Hydride%铌对氢化锆裂纹行为和氢含量的影响

    Institute of Scientific and Technical Information of China (English)

    王建伟; 王力军; 陈伟东; 张建东

    2012-01-01

    Zirconium hydride was one of the most ideal moderators, especially for the space nuclear power system. But the high hydrogen level zirconium hydride was easy to crack during its preparation. Nb was the main adding element in the zirconium hydride moderator and affected the cracking behaviors and hydrogen content of the zirconium hydride, which was determined by the existing status of Nb in the zirconium hydride. The issues mentioned were investigated at present It indicated that the hydriding products of Zr-Nb alloys with different Nb content were all composed of mixed s phase zirconium hydrides of ZrH2, ZrH1.950 and ZrH1.801. Nb improved the structure and morphology of the zirconium hydride, decreased the defects and inhibited the cracking. In the case of high Nb level, the generated NbR, solid solution with low hydrogen content downgraded the whole hydrogen content of the alloy. The solubility of Nb in the zirconium hydride was low. For the zirconium hydride with low Nb content, majority of Nb was scattered on the surface of the zirconium hydride as small white grains of H-containing Zr-Nb solid solutioa.%氢化锫是一种理想的固体中子慢化材料,尤其适用于空间核电源的反应堆,但是高氢含量的氢化锫在制备过程中很容易形成裂纹.Nb是氢化锆中的主要添加元素,对氢化锆的裂纹形成和氢含量有一定影响,这是由Nb在氢化锆中的存在形式决定的,对此进行了研究.结果表明,在吸氢充分的情况下,不同Nb含量的Zr - Nb合金氢化后产物的主要组成都是ZrH2,ZrH1.950和ZrH1.801的ε相氢化锆混合物,Nb的添加对氢化锫的晶格常数和晶胞大小影响不大.Nb改善了氢化锫的多缺陷状态,减少了氢富集的位置,从而起到抑制裂纹产生的作用.常压下,Nb的添加会影响合金的最大吸氢量,尤其当Nb含量在10%以上时,会生成低氢含量的NbHx固溶体,影响锆合金的整体吸氢量.Nb在氢化锆中的固溶度较小,Nb含量较

  4. A spectroscopic method for determining thickness of quartz wave plate

    Institute of Scientific and Technical Information of China (English)

    Weiwei Feng; Lihuang Lin; Ligang Chen; Huafeng Zhu; Ruxin Li; Zhizhan Xu

    2006-01-01

    A spectroscopic method to determine thickness of quartz wave plate is presented. The method is based on chromatic polarization interferometry. With the polarization-resolved transmission spectrum (PRTS)curve, the phase retardation of quartz wave plate can be determined at a wide spectral range from 200 to2000 nm obviously. Through accurate judgment of extreme points of PRTS curve at long-wave band, the physical thickness of quartz wave plates can be obtained exactly. We give a measuring example and the error analysis. It is found that the measuring precision of thickness is mainly determined by the spectral resolution of spectrometer.

  5. Dissociation potential curves of low-lying states in transition metal hydrides. 3. Hydrides of groups 6 and 7.

    Science.gov (United States)

    Koseki, Shiro; Matsushita, Takeshi; Gordon, Mark S

    2006-02-23

    The dissociation curves of low-lying spin-mixed states in monohydrides of groups 6 and 7 were calculated by using an effective core potential (ECP) approach. This approach is based on the multiconfiguration self-consistent field (MCSCF) method, followed by first-order configuration interaction (FOCI) calculations, in which the method employs an ECP basis set proposed by Stevens and co-workers (SBKJC) augmented by a set of polarization functions. Spin-orbit coupling (SOC) effects are estimated within the one-electron approximation by using effective nuclear charges, since SOC splittings obtained with the full Breit-Pauli Hamitonian are underestimated when ECP basis sets are used. The ground states of group 6 hydrides have Omega = (1)/(2)(X(6)Sigma(+)(1/2)), where Omega is the z component of the total angular momentum quantum number. Although the ground states of group 7 hydrides have Omega = 0(+), their main adiabatic components are different; the ground state in MnH originates from the lowest (7)Sigma(+), while in TcH and ReH the main component of the ground state is the lowest (5)Sigma(+). The present paper reports a comprehensive set of theoretical results including the dissociation energies, equilibrium distances, electronic transition energies, harmonic frequencies, anharmonicities, and rotational constants for several low-lying spin-mixed states in these hydrides. Transition dipole moments were also computed among the spin-mixed states and large peak positions of electronic transitions are suggested theoretically for these hydrides. The periodic trends of physical properties of metal hydrides are discussed, based on the results reported in this and other recent studies.

  6. Explosive volcanism and associated pressures - Implications for models of endogenically shocked quartz

    Science.gov (United States)

    De Silva, S. L.; Wolff, J. A.; Sharpton, V. L.

    1990-01-01

    The nature of explosive volcanic phenomena and associated pressures, both from field and theoretical perspectives, is discussed. An endogenic origin for shocked quartz at the K/T boundary requires impulsive pressures greater than 60 kbars to be generated during explosive volcanism. Explosive volcanic eruptions which are events of sustained decompression may be initiated by impulsive explosions while the magnitudes of the overpressures are small. These maximum overpressures can be controlled mainly by the tensile strength of the rock surrounding the magma chamber-conduit system. Thus maximum overpressures in the volcanic environment are limited to less than 500 bars which are orders of magnitude less than those required for shock quartz (greater than 60 kbars). This observation is found to be consistent with the complete lack of field or petrographic evidence in support of shock metamorphism associated with volcanic eruptions and their products.

  7. Heavy hydrides: H2Te ultraviolet photochemistry

    Science.gov (United States)

    Underwood, J.; Chastaing, D.; Lee, S.; Wittig, C.

    2005-08-01

    The room-temperature ultraviolet absorption spectrum of H2Te has been recorded. Unlike other group-6 hydrides, it displays a long-wavelength tail that extends to 400 nm. Dissociation dynamics have been examined at photolysis wavelengths of 266 nm (which lies in the main absorption feature) and 355 nm (which lies in the long-wavelength tail) by using high-n Rydberg time-of-flight spectroscopy to obtain center-of-mass translational energy distributions for the channels that yield H atoms. Photodissociation at 355 nm yields TeH(Π1/22) selectively relative to the TeH(Π3/22) ground state. This is attributed to the role of the 3A' state, which has a shallow well at large RH-TeH and correlates to H +TeH(Π1/22). Note that the Π1/22 state is analogous to the P1/22 spin-orbit excited state of atomic iodine, which is isoelectronic with TeH. The 3A' state is crossed at large R only by 2A″, with which it does not interact. The character of 3A' at large R is influenced by a strong spin-orbit interaction in the TeH product. Namely, Π1/22 has a higher degree of spherical symmetry than does Π3/22 (recall that I(P1/22) is spherically symmetric), and consequently Π1/22 is not inclined to form either strongly bonding or antibonding orbitals with the H atom. The 3A'←X transition dipole moment dominates in the long-wavelength region and increases with R. Structure observed in the absorption spectrum in the 380-400 nm region is attributed to vibrations on 3A'. The main absorption feature that is peaked at ˜240nm might arise from several excited surfaces. On the basis of the high degree of laboratory system spatial anisotropy of the fragments from 266 nm photolysis, as well as high-level theoretical studies, the main contribution is believed to be due to the 4A″ surface. The 4A″←X transition dipole moment dominates in the Franck-Condon region, and its polarization is in accord with the experimental observations. An extensive secondary photolysis (i.e., of nascent TeH) is

  8. Composite Materials for Hazard Mitigation of Reactive Metal Hydrides.

    Energy Technology Data Exchange (ETDEWEB)

    Pratt, Joseph William; Cordaro, Joseph Gabriel; Sartor, George B.; Dedrick, Daniel E.; Reeder, Craig L.

    2012-02-01

    In an attempt to mitigate the hazards associated with storing large quantities of reactive metal hydrides, polymer composite materials were synthesized and tested under simulated usage and accident conditions. The composites were made by polymerizing vinyl monomers using free-radical polymerization chemistry, in the presence of the metal hydride. Composites with vinyl-containing siloxane oligomers were also polymerized with and without added styrene and divinyl benzene. Hydrogen capacity measurements revealed that addition of the polymer to the metal hydride reduced the inherent hydrogen storage capacity of the material. The composites were found to be initially effective at reducing the amount of heat released during oxidation. However, upon cycling the composites, the mitigating behavior was lost. While the polymer composites we investigated have mitigating potential and are physically robust, they undergo a chemical change upon cycling that makes them subsequently ineffective at mitigating heat release upon oxidation of the metal hydride. Acknowledgements The authors would like to thank the following people who participated in this project: Ned Stetson (U.S. Department of Energy) for sponsorship and support of the project. Ken Stewart (Sandia) for building the flow-through calorimeter and cycling test stations. Isidro Ruvalcaba, Jr. (Sandia) for qualitative experiments on the interaction of sodium alanate with water. Terry Johnson (Sandia) for sharing his expertise and knowledge of metal hydrides, and sodium alanate in particular. Marcina Moreno (Sandia) for programmatic assistance. John Khalil (United Technologies Research Corp) for insight into the hazards of reactive metal hydrides and real-world accident scenario experiments. Summary In an attempt to mitigate and/or manage hazards associated with storing bulk quantities of reactive metal hydrides, polymer composite materials (a mixture of a mitigating polymer and a metal hydride) were synthesized and tested

  9. Acoustic Tests of Lorentz Symmetry Using Quartz Oscillators

    Directory of Open Access Journals (Sweden)

    Anthony Lo

    2016-02-01

    Full Text Available We propose and demonstrate a test of Lorentz symmetry based on new, compact, and reliable quartz oscillator technology. Violations of Lorentz invariance in the matter and photon sector of the standard model extension generate anisotropies in particles’ inertial masses and the elastic constants of solids, giving rise to measurable anisotropies in the resonance frequencies of acoustic modes in solids. A first realization of such a “phonon-sector” test of Lorentz symmetry using room-temperature stress-compensated-cut crystals yields 120 h of data at a frequency resolution of 2.4×10^{−15} and a limit of c[over ˜]_{Q}^{n}=(−1.8±2.2×10^{−14}  GeV on the most weakly constrained neutron-sector c coefficient of the standard model extension. Future experiments with cryogenic oscillators promise significant improvements in accuracy, opening up the potential for improved limits on Lorentz violation in the neutron, proton, electron, and photon sector.

  10. SEM-Cathodoluminescence and fluid inclusion study of quartz veins in Hugo Dummett porphyry Cu-Au deposit,South Mongolia

    Science.gov (United States)

    Sanjaa, M.; Fujimaki, H.; Ken-Ichiro, H.

    2010-12-01

    The Hugo Dummett porphyry copper-gold deposit in Oyu Tolgoi, South Mongolia is a high-sulfidation type deposit which consists of Cu-Au bearing quartz veins. Cathodoluminescence (CL) analysis using scanning electron microscope (SEM) and fluid inclusion microthermometer were performed to elucidate the relationship between CL structures, fluid inclusion microthermometer of different quartz generations, and ore forming process of the Hugo Dummett deposit. Hydrothermal quartz from quartz-sulfide veins in the porphyry Cu-Au deposit in Hugo Dummett, revealing the following textures: (1) euhedral growth zones (2) embayed and rounded CL-bright cores, with CL-dark and CL-gray overgrowths, (3) concentric and non concentric growth zones, and (4) CL dark/bright microfractures. These textures indicate that many veins have undergone fracturing, growth of quartz into fluid-filled space and quartz dissolution of quartz. SEM-CL imaging indicates vein quartz in the Hugo Dummett deposit, initially grew as individual CL-bright crystals 356 ± 10°C liquid-reservoir (average Th value for fluid inclusions in the crystal cores is 359°C). In contract, SEM-CL imaging shows the edges of the micron-scale growth zones of varying CL intensity, reflecting quartz precipitation at some later time, when the Hugo Dummett deposit hydrothermal system had cooled, when reservoir conditions were about 211 ± 25°C (average Th value of 212°C). Crystal growth is SEM-CL evidence of the vein quartz having been partly dissolved. Pressure change has a large effect on quartz solubility and may have been responsible for quartz dissolution and precipitation textures in the cooling hydrothermal system. CL-dark microfractures homogenization temperatures lower 169 ± 16°C (average Th value 170°C) than CL bright and CL gray. Temperature and pressure of the mineralized fluid estimates a pressure of formation of 0.3-0.5 kbar (lithostatic), was formed at approximately 2 km depth, as well as a formation temperature

  11. Structure optimization and simulation analysis of the quartz micromachined gyroscope

    Science.gov (United States)

    Wu, Xuezhong; Wang, Haoxu; Xie, Liqiang; Dong, Peitao

    2014-03-01

    Structure optimization and simulation analysis of the quartz micromachined gyroscope are reported in this paper. The relationships between the structure parameters and the frequencies of work mode were analysed by finite element analysis. The structure parameters of the quartz micromachined gyroscope were optimized to reduce the difference between the frequencies of the drive mode and the sense mode. The simulation results were proved by testing the prototype gyroscope, which was fabricated by micro-electromechanical systems (MEMS) technology. Therefore, the frequencies of the drive mode and the sense mode can match each other by the structure optimization and simulation analysis of the quartz micromachined gyroscope, which is helpful in the design of the high sensitivity quartz micromachined gyroscope.

  12. Origin of organism-dependent biogenic silica quartz formation.

    Science.gov (United States)

    Sato, Kiminori

    2011-12-15

    Organism-dependent biogenic quartz formation in the steady-state environment is a phenomenon that can address the global environmental issues such as diagenetic evolution, biogeochemical cycling, and reservoir formation, but detailed studies have not been performed so far. Here, steady-state quartz formation is studied for amorphous silica of different biogenic origin on the basis of the recently established mechanistic model [Sato et al., J. Phys. Chem. C 2011, 115, 18131]. Amorphous silica originated from rice husks possesses angstrom-scale pores larger by 1.3 Å than those originated from diatom algae. The slight difference of pore size dramatically reduces activation energies of water diffusion by 78% and reactions of water molecules at pore surfaces by 47%, resulting in the reduction of activation energy of biogenic quartz formation by 64%. The present findings evidence that angstrom-scale pores intrinsically residing in the amorphous matrix are the organism-dependent origin of steady-state biogenic quartz formation.

  13. Quartz Fibers For Laser Therapy In Tissue Contact

    Science.gov (United States)

    Lenz, P.; Sabber, G.; Lambert, R.; Berger, F.

    1984-03-01

    Quartz fibers not protected by a gas stream and used in tissue contact can work virtually indefinitely due to "self cleaning" and "regeneration". Tissue lesions are similar to those obtained with conventional devices.

  14. Structure optimization and simulation analysis of the quartz micromachined gyroscope

    Directory of Open Access Journals (Sweden)

    Xuezhong Wu

    2014-02-01

    Full Text Available Structure optimization and simulation analysis of the quartz micromachined gyroscope are reported in this paper. The relationships between the structure parameters and the frequencies of work mode were analysed by finite element analysis. The structure parameters of the quartz micromachined gyroscope were optimized to reduce the difference between the frequencies of the drive mode and the sense mode. The simulation results were proved by testing the prototype gyroscope, which was fabricated by micro-electromechanical systems (MEMS technology. Therefore, the frequencies of the drive mode and the sense mode can match each other by the structure optimization and simulation analysis of the quartz micromachined gyroscope, which is helpful in the design of the high sensitivity quartz micromachined gyroscope.

  15. Low-temperature intracrystalline deformation microstructures in quartz

    NARCIS (Netherlands)

    Derez, Tine; Pennock, Gill; Drury, Martyn; Sintubin, Manuel

    A review of numerous genetic interpretations of the individual low-temperature intracrystalline deformation microstructures in quartz shows that there is no consensus concerning their formation mechanisms. Therefore, we introduce a new, purely descriptive terminology for the three categories of

  16. The Characteristics of the Shear-Vibrating Quartz Crystal Resonator

    Institute of Scientific and Technical Information of China (English)

    Wenjie Tian; Lingling Liu; Junling Lu; Fuxue Zhang

    2006-01-01

    According to the piezoelectric equation and the vibration theory of the quartz crystal, the relations between the vibrating frequency and structural parameters under the thickness-shear-vibration of AT-cut quartz crystal have been studied.The frequency conditions under which quartz crystal resonator formed stationary wave inside the electrode district and the transmission characteristics of wave outside the electrode district have also been discussed. A quartz crystal resonator was developed based on this analysis. The experiment showed that the force-sensing characteristics were independent of the fixation of the crystal edge. The detecting distinguish ability was up to 0.001 °, and the short-term frequency stability was up to 1.38x 10-10/min.

  17. Effect of thermo-mechanical cycling on zirconium hydride reorientation studied in situ with synchrotron X-ray diffraction

    Science.gov (United States)

    Colas, Kimberly B.; Motta, Arthur T.; Daymond, Mark R.; Almer, Jonathan D.

    2013-09-01

    The circumferential hydrides normally present in nuclear reactor fuel cladding after reactor exposure may dissolve during drying for dry storage and re-precipitate when cooled under load into a more radial orientation, which could embrittle the fuel cladding. It is necessary to study the rates and conditions under which hydride reorientation may happen in order to assess fuel integrity in dry storage. The objective of this work is to study the effect of applied stress and thermal cycling on the hydride morphology in cold-worked stress-relieved Zircaloy-4 by combining conventional metallography and in situ X-ray diffraction techniques. Metallography is used to study the evolution of hydride morphology after several thermo-mechanical cycles. In situ X-ray diffraction performed at the Advanced Photon Source synchrotron provides real-time information on the process of hydride dissolution and precipitation under stress during several thermal cycles. The detailed study of diffracted intensity, peak position and full-width at half-maximum provides information on precipitation kinetics, elastic strains and other characteristics of the hydride precipitation process. The results show that thermo-mechanical cycling significantly increases the radial hydride fraction as well as the hydride length and connectivity. The radial hydrides are observed to precipitate at a lower temperature than circumferential hydrides. Variations in the magnitude and range of hydride strains due to reorientation and cycling have also been observed. These results are discussed in light of existing models and experiments on hydride reorientation. The study of hydride elastic strains during precipitation shows marked differences between circumferential and radial hydrides, which can be used to investigate the reorientation process. Cycling under stress above the threshold stress for reorientation drastically increases both the reoriented hydride fraction and the hydride size. The reoriented hydride

  18. A self-regulating hydrogen generator for micro fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Moghaddam, Saeed; Pengwang, Eakkachai; Shannon, Mark A. [Mechanical Science and Engineering, University of Illinois at Urbana-Champaign, 1206 West Green Street, Urbana, IL 61801 (United States); Masel, Richard I. [Chemical and Biomolecular Engineering, University of Illinois at Urbana-Champaign, 213 Roger Adams Lab, 600 S. Mathews, Urbana, IL 61801 (United States)

    2008-10-15

    The ever-increasing power demands and miniaturization of portable electronics, micro-sensors and actuators, and emerging technologies such as cognitive arthropods have created a significant interest in development of micro fuel cells. One of the major challenges in development of hydrogen micro fuel cells is the fabrication and integration of auxiliary systems for generating, regulating, and delivering hydrogen gas to the membrane electrode assembly (MEA). In this paper, we report the development of a hydrogen gas generator with a micro-scale control system that does not consume any power. The hydrogen generator consists of a hydride reactor and a water reservoir, with a regulating valve separating them. The regulating valve consists of a port from the water reservoir and a movable membrane with via holes that permit water to flow from the reservoir to the hydride reactor. Water flows towards the hydride reactor, but stops within the membrane via holes due to capillary forces. Water vapor then diffuses from the via holes into the hydride reactor resulting in generation of hydrogen gas. When the rate of hydrogen consumed by the MEA is lower than the generation rate, gas pressure builds up inside the hydride reactor, deflecting the membrane, closing the water regulator valve, until the pressure drops, whereby the valve reopens. We have integrated the self-regulating micro hydrogen generator to a MEA and successfully conducted fuel cell tests under varying load conditions. (author)

  19. A self-regulating hydrogen generator for micro fuel cells

    Science.gov (United States)

    Moghaddam, Saeed; Pengwang, Eakkachai; Masel, Richard I.; Shannon, Mark A.

    The ever-increasing power demands and miniaturization of portable electronics, micro-sensors and actuators, and emerging technologies such as cognitive arthropods have created a significant interest in development of micro fuel cells. One of the major challenges in development of hydrogen micro fuel cells is the fabrication and integration of auxiliary systems for generating, regulating, and delivering hydrogen gas to the membrane electrode assembly (MEA). In this paper, we report the development of a hydrogen gas generator with a micro-scale control system that does not consume any power. The hydrogen generator consists of a hydride reactor and a water reservoir, with a regulating valve separating them. The regulating valve consists of a port from the water reservoir and a movable membrane with via holes that permit water to flow from the reservoir to the hydride reactor. Water flows towards the hydride reactor, but stops within the membrane via holes due to capillary forces. Water vapor then diffuses from the via holes into the hydride reactor resulting in generation of hydrogen gas. When the rate of hydrogen consumed by the MEA is lower than the generation rate, gas pressure builds up inside the hydride reactor, deflecting the membrane, closing the water regulator valve, until the pressure drops, whereby the valve reopens. We have integrated the self-regulating micro hydrogen generator to a MEA and successfully conducted fuel cell tests under varying load conditions.

  20. 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.