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Sample records for purity-enhanced bulk synthesis

  1. Purity Evaluation of Bulk Single Wall Carbon Nanotube Materials

    International Nuclear Information System (INIS)

    Dettlaff-Weglikowska, U.; Hornbostel, B.; Cech, J.; Roth, S.; Wang, J.; Liang, J.

    2005-01-01

    We report on our experience using a preliminary protocol for quality control of bulk single wall carbon nanotube (SWNT) materials produced by the electric arc-discharge and laser ablation method. The first step in the characterization of the bulk material is mechanical homogenization. Quantitative evaluation of purity has been performed using a previously reported procedure based on solution phase near-infrared spectroscopy. Our results confirm that this method is reliable in determining the nanotube content in the arc-discharge sample containing carbonaceous impurities (amorphous carbon and graphitic particles). However, the application of this method to laser ablation samples gives a relative purity value over 100 %. The possible reason for that might be different extinction coefficient meaning different oscillator strength of the laser ablation tubes. At the present time, a 100 % pure reference sample of laser ablation SWNT is not available, so we chose to adopt the sample showing the highest purity as a new reference sample for a quantitative purity evaluation of laser ablation materials. The graphitic part of the carbonaceous impurities has been estimated using X-ray diffraction of 1:1 mixture of nanotube material and C60 as an internal reference. To evaluate the metallic impurities in the as prepared and homogenized carbon nanotube soot inductive coupled plasma (ICP) has been used

  2. Native oxidation of ultra high purity Cu bulk and thin films

    International Nuclear Information System (INIS)

    Iijima, J.; Lim, J.-W.; Hong, S.-H.; Suzuki, S.; Mimura, K.; Isshiki, M.

    2006-01-01

    The effect of microstructure and purity on the native oxidation of Cu was studied by using angle-resolved X-ray photoelectron spectroscopy (AR-XPS) and spectroscopic ellipsometry (SE). A high quality copper film prepared by ion beam deposition under a substrate bias voltage of -50 V (IBD Cu film at V s = -50 V) showed an oxidation resistance as high as an ultra high purity copper (UHP Cu) bulk, whereas a Cu film deposited without substrate bias voltage (IBD Cu film at V s = 0 V) showed lower oxidation resistance. The growth of Cu 2 O layer on the UHP Cu bulk and both types of the films obeyed in principle a logarithmic rate law. However, the growth of oxide layer on the IBD Cu films at V s = 0 and -50 V deviated upward from the logarithmic rate law after the exposure time of 320 and 800 h, respectively. The deviation from the logarithmic law is due to the formation of CuO on the Cu 2 O layer after a critical time

  3. Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants.

    Science.gov (United States)

    Wang, Junlian; Xie, Meiying; Liu, Xinyu; Xu, Shengming

    2017-10-19

    We present the synthesis of (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid as an example to demonstrate a method for the synthesis of high purity nonsymmetric dialkylphosphinic acid extractants. Low toxic sodium hypophosphite was chosen as the phosphorus source to react with olefin A (2,3-dimethyl-1-butene) to generate a monoalkylphosphinic acid intermediate. Amantadine was adopted to remove the dialkylphosphinic acid byproduct, as only the monoalkylphosphinic acid can react with amantadine to form an amantadine∙mono-alkylphosphinic acid salt, while the dialkylphosphinic acid cannot react with amantadine due to its large steric hindrance. The purified monoalkylphosphinic acid was then reacted with olefin B (diisobutylene) to yield nonsymmetric dialkylphosphinic acid (NSDAPA). The unreacted monoalkylphosphinic acid can be easily removed by a simple base-acid post-treatment and other organic impurities can be separated out through the precipitation of the cobalt salt. The structure of the (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid was confirmed by 31 P NMR, 1 H NMR, ESI-MS, and FT-IR. The purity was determined by a potentiometric titration method, and the results indicate that the purity can exceed 96%.

  4. Comparison between bulk and thin foil ion irradiation of ultra high purity Fe

    Energy Technology Data Exchange (ETDEWEB)

    Prokhodtseva, A., E-mail: anna.prokhodtseva@psi.ch [Ecole Polytechnique Fédérale de Lausanne (EPFL), Centre de Recherches en Physique des Plasmas, Association Euratom-Confédération Suisse, 5232 Villigen PSI (Switzerland); Décamps, B. [Centre de Spectrométrie Nucléaire et de Spectrométrie de Masse (CSNSM), CNRS-IN2P3-Univ. Paris-Sud 11, UMR 8609, Bât. 108, 91405 Orsay (France); Schäublin, R. [Ecole Polytechnique Fédérale de Lausanne (EPFL), Centre de Recherches en Physique des Plasmas, Association Euratom-Confédération Suisse, 5232 Villigen PSI (Switzerland)

    2013-11-15

    Accumulation of radiation damage in ultra high purity iron under self ion irradiation without and with simultaneous He implantation was investigated in bulk and thin foil form to assess, on the one hand, the effect of free surfaces and, on the other hand, the influence of He. Specimens were irradiated at room temperature to a dose of 0.8 dpa and ∼900 appm He content. We found in thin foils after irradiation with single beam a majority of a{sub 0} 〈1 0 0〉 type loops, while in the presence of He it is the ½ a{sub 0} 〈1 1 1〉 type loops that prevail. In single beam irradiated bulk samples most of the loops are of ½ a{sub 0} 〈1 1 1〉 type. In both bulk and thin foils density of defects visible in transmission electron microscope is considerably higher when He is implanted with prevailing ½ a{sub 0} 〈1 1 1〉 dislocation loops, indicating that He stabilizes them.

  5. Spectral Purity Enhancement via Polyphase Multipath Circuits

    NARCIS (Netherlands)

    Mensink, E.; Klumperink, Eric A.M.; Nauta, Bram

    2004-01-01

    The central question of this paper is: can we enhance the spectral purity of nonlinear circuits by using polyphase multipath circuits? The basic idea behind polyphase multipath circuits is to split the nonlinear circuits into two or more paths and exploit phase differences between these paths to

  6. Fabrication of novel cryomill for synthesis of high purity metallic nanoparticles

    Science.gov (United States)

    Kumar, Nirmal; Biswas, Krishanu

    2015-08-01

    The successful preparation of free standing metal nanoparticles with high purity in bulk quantity is the pre-requisite for any potential application. This is possible by using ball milling at cryogenic temperature. However, the most of ball mills available in the market do not allow preparing high purity metal nanoparticles by this route. In addition, it is not possible to carry out in situ measurements of process parameters as well as diagnostic of the process. In the present investigation, we present a detailed study on the fabrication of a cryomill, which is capable of avoiding contaminations in the product. It also provides in situ measurements and diagnostic of the low temperature milling process. Online monitoring of the milling temperature and observation of ball motion are the important aspects in the newly designed mill. The nanoparticles prepared using this fabricated mill have been found to be free standing and also free from contaminations.

  7. High-purity Cu nanocrystal synthesis by a dynamic decomposition method

    Science.gov (United States)

    Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

    2014-12-01

    Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

  8. Voltage-controlled colour-tunable microcavity OLEDs with enhanced colour purity

    International Nuclear Information System (INIS)

    Choy, Wallace C H; Niu, J H; Li, W L; Chui, P C

    2008-01-01

    The emission spectrum of single-unit voltage-controlled colour-tunable organic light emitting devices (OLEDs) has been theoretically and experimentally studied. Our results show that by introducing the microcavity structure, the colour purity of not only the destination colour but also the colour-tunable route can be enhanced, while colour purity is still an issue in typical single-unit voltage-controlled colour-tunable OLEDs. With the consideration of the periodical cycling of resonant wavelength and absorption loss of the metal electrodes, the appropriate change in the thickness of the microcavity structure has been utilized to achieve voltage-controlled red-to-green and red-to-blue colour-tunable OLEDs without adding dyes or other organic materials to the OLEDs

  9. Enhanced color purity of blue OLEDs based on well-design structure

    Science.gov (United States)

    Du, Qianqian; Wang, Wenjun; Li, Shuhong; Wang, Qingru; Xia, Shuzhen; Zhang, Bingyuan; Wang, Minghong; Fan, Quli

    2016-09-01

    We have fabricated blue organic light-emitting devices (OLEDs) with higher color purity and stability by optimizing the structure of the Glass/ITO/NPB(50 nm)/ BCzVBi (30 nm)/ TPBi (x nm)/Alq3(20 nm)/LiF/Al. The results show that the introducing of hole blocking layer(HBL) TPBi greatly can improve not only the color purity but the color stability, which owe to its higher the Highest Occupied Molecular Orbital (HOMO) energy levels of 6.2 eV. We expect our work will be useful to optimizing the blue OLEDs structure to enhancing the color property.

  10. Synthesis of high-purity Li{sub 8}ZrO{sub 6} powder by solid state reaction under hydrogen atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Shin-mura, Kiyoto; Otani, Yu; Ogawa, Seiya [Course of Mechanical Engineering, Graduate School of Engineering, Tokai University, 4-1-1 Kitakaname, Hiratsuka, Kanagawa 259-1292 (Japan); Niwa, Eiki; Hashimoto, Takuya [Department of Physics, College of Humanities and Sciences, Nihon University, 3-8-1 Sakurajousui, Setagaya-ku, Tokyo 156-8550 (Japan); Hoshino, Tsuyoshi [Breeding Functional Materials Development Group, Department of Blanket Systems Research, Rokkasho Fusion Institute, Sector of Fusion Research and Development, Japan Atomic Energy Agency, 2-166 Obuchi, Omotedate, Rokkasho-mura, Kamikita-gun, Aomori 039-3212 (Japan); Sasaki, Kazuya, E-mail: k_sasaki@tokai-u.ac.jp [Course of Mechanical Engineering, Graduate School of Engineering, Tokai University, 4-1-1 Kitakaname, Hiratsuka, Kanagawa 259-1292 (Japan); Department of Prime Mover Engineering, School of Engineering, Tokai University, 4-1-1 Kitakaname, Hiratsuka, Kanagawa 259-1292 (Japan)

    2016-11-01

    Highlights: • A fine pure Li{sub 8}ZrO{sub 6} powder was synthesized by using Li{sub 2}CO{sub 3} and ZrO{sub 2} via a solid state reaction. • Influences on the purity of product powder, lattice defect, and crystal orientation were revealed. • The suitable synthesis conditions of the fine and high purity Li{sub 8}ZrO{sub 6} powder were found. • The reaction process of the synthesis of Li{sub 8}ZrO{sub 6} was estimated. - Abstract: Li{sub 8}ZrO{sub 6} contains a large amount of Li and has a significant potential as a tritium breeder. However, few syntheses of fine-grain, high-purity Li{sub 8}ZrO{sub 6} powder have been reported. In this study, a high-purity powder of Li{sub 8}ZrO{sub 6} was synthesized by solid state reaction under hydrogen atmosphere combined with an effective lithium source and a suitable initial Li:Zr molar ratio. Mixed powders of Li{sub 2}CO{sub 3} and ZrO{sub 2} were fired at around 630 °C in H{sub 2} for several hours and several firing cycles. The low firing temperature inhibited the vaporization of Li during the heating, so that excessive amounts of Li were not needed for the synthesis, and the Li:Zr ratio in the starting material was 10:1 (mol:mol). In this synthesis, Li{sub 2}O was generated via the decomposition of Li{sub 2}CO{sub 3} during firing in H{sub 2}, and reacted with ZrO{sub 2} to form Li{sub 6}Zr{sub 2}O{sub 7}, which reacted with itself to form Li{sub 8}ZrO{sub 6}.

  11. Synthesis and structural characterization of bulk Sb2Te3 single crystal

    Science.gov (United States)

    Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

    2018-05-01

    We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

  12. Novel catalytic route to bulk production of high purity carbon nanotube

    International Nuclear Information System (INIS)

    Dasgupta, Kinshuk; Venugopalan, Ramani; Dey, G. K.; Sathiyamoorthy, D.

    2008-01-01

    Carbon nanotubes have been synthesized by catalytic chemical vapour deposition of acetylene diluted with argon using three different catalysts, namely, nickel formate, cobalt formate and ferrocene. The synthesis was carried out at 700 deg. C in a quartz reactor for 30 minutes. Thermal analysis was carried out in order to determine the yield of the nanotube. It was found that the deposit contains 86% nanotube, with nickel-based catalyst, which was the maximum. The yield of nanotube was 71 times that of the nickel loading. The TEM images reveal helical type of nanotubes with iron catalyst while cobalt and nickel catalysts yielded straight nanotubes. This technique can be explored for the bulk production of carbon nanotube in an economic way

  13. Microwave-Hydrothermal Synthesis and Characterization of High-Purity Nb Doped BaTiO3 Nanocrystals

    Directory of Open Access Journals (Sweden)

    A. Khanfekr

    2014-01-01

    Full Text Available The synthesis of Nb doped BaTiO3 has been investigated under Microwave-Hydrothermal (MH conditions in the temperature of 150°C for only 2 h using C16H36O4Ti, BaH2O2.8H2O and NbCl5 as Ba, Ti and  Nb sources, respectively.  Typical experiments performed on MH processing have not yet reported for Nb doped BaTiO3.  In the MH process, the formation of high purity nano tetragonal Nb-BaTiO3 was strongly enhanced. New hydrothermal method was used instead of the previous solid state reaction for the BaTiO3±Nb2O3 system. The new method uses high pressure to create nano dimension particles in a lower time and temperature. In case of the phase evolution studies, the XRD pattern measurements and Raman spectroscopy were performed. TEM and FE-SEM images were taken for the detailed analysis of the particle size, surface and morphology.  Synthesis of Nb doped BaTiO3 with the Microwave-hydrothermal provides an advantage of fast crystallization and reduced crystal size when compared to existing methods.

  14. A combined arc-melting and tilt-casting furnace for the manufacture of high-purity bulk metallic glass materials.

    Science.gov (United States)

    Soinila, E; Pihlajamäki, T; Bossuyt, S; Hänninen, H

    2011-07-01

    An arc-melting furnace which includes a tilt-casting facility was designed and built, for the purpose of producing bulk metallic glass specimens. Tilt-casting was chosen because reportedly, in combination with high-purity processing, it produces the best fatigue endurance in Zr-based bulk metallic glasses. Incorporating the alloying and casting facilities in a single piece of equipment reduces the amount of laboratory space and capital investment needed. Eliminating the sample transfer step from the production process also saves time and reduces sample contamination. This is important because the glass forming ability in many alloy systems, such as Zr-based glass-forming alloys, deteriorates rapidly with increasing oxygen content of the specimen. The challenge was to create a versatile instrument, in which high purity conditions can be maintained throughout the process, even when melting alloys with high affinity for oxygen. Therefore, the design provides a high-vacuum chamber to be filled with a low-oxygen inert atmosphere, and takes special care to keep the system hermetically sealed throughout the process. In particular, movements of the arc-melting electrode and sample manipulator arm are accommodated by deformable metal bellows, rather than sliding O-ring seals, and the whole furnace is tilted for tilt-casting. This performance of the furnace is demonstrated by alloying and casting Zr(55)Cu(30)Al(10)Ni(5) directly into rods up to ø 10 mm which are verified to be amorphous by x-ray diffraction and differential scanning calorimetry, and to exhibit locally ductile fracture at liquid nitrogen temperature.

  15. Large-scale synthesis of high-purity well-aligned carbon nanotubes using pyrolysis of iron(II) phthalocyanine and acetylene

    Science.gov (United States)

    Liu, B. C.; Lee, T. J.; Lee, S. H.; Park, C. Y.; Lee, C. J.

    2003-08-01

    Well-aligned carbon nanotubes (CNTs) with high purity have been produced by pyrolysis of iron(II) phthalocyanine and acetylene at 800 °C. The synthesized CNTs have a length of 75 μm and diameters ranging from 20 to 60 nm. The CNTs have a bamboo-like structure and exhibit good crystallinity of graphite sheets. The growth rate of the CNTs was rapidly increased with adding C 2H 2. Our results demonstrate that the proposed growth method is suitable to large-scale synthesis of high-purity well-aligned CNTs on various substrates.

  16. On-surface synthesis on a bulk insulator surface

    Science.gov (United States)

    Richter, Antje; Floris, Andrea; Bechstein, Ralf; Kantorovich, Lev; Kühnle, Angelika

    2018-04-01

    On-surface synthesis has rapidly emerged as a most promising approach to prepare functional molecular structures directly on a support surface. Compared to solution synthesis, performing chemical reactions on a surface offers several exciting new options: due to the absence of a solvent, reactions can be envisioned that are otherwise not feasible due to the insolubility of the reaction product. Perhaps even more important, the confinement to a two-dimensional surface might enable reaction pathways that are not accessible otherwise. Consequently, on-surface synthesis has attracted great attention in the last decade, with an impressive number of classical reactions transferred to a surface as well as new reactions demonstrated that have no classical analogue. So far, the majority of the work has been carried out on conducting surfaces. However, when aiming for electronic decoupling of the resulting structures, e.g. for the use in future molecular electronic devices, non-conducting surfaces are highly desired. Here, we review the current status of on-surface reactions demonstrated on the (10.4) surface of the bulk insulator calcite. Besides thermally induced C-C coupling of halogen-substituted aryls, photochemically induced [2  +  2] cycloaddition has been proven possible on this surface. Moreover, experimental evidence exists for coupling of terminal alkynes as well as diacetylene polymerization. While imaging of the resulting structures with dynamic atomic force microscopy provides a direct means of reaction verification, the detailed reaction pathway often remains unclear. Especially in cases where the presence of metal atoms is known to catalyze the corresponding solution chemistry reaction (e.g. in the case of the Ullmann reaction), disclosing the precise reaction pathway is of importance to understand and generalize on-surface reactivity on a bulk insulator surface. To this end, density-functional theory calculations have proven to provide atomic

  17. New insights on the synthesis and electronic transport in bulk polycrystalline Pr-doped SrTiO3−δ

    International Nuclear Information System (INIS)

    Dehkordi, Arash Mehdizadeh; Bhattacharya, Sriparna; Darroudi, Taghi; Alshareef, Husam N.; Tritt, Terry M.

    2015-01-01

    Recently, we have reported a significant enhancement in the electronic and thermoelectric properties of bulk polycrystalline SrTiO 3 ceramics via praseodymium doping. This improvement was originated from the simultaneous enhancement in the thermoelectric power factor and reduction in thermal conductivity, which was contributed to the non-uniform distribution of Pr dopants. In order to further understand the underlying mechanism, we herein investigate the role of praseodymium doping source (Pr 2 O 3 versus Pr 6 O 11 ) on the synthesis and electronic transport in Pr-doped SrTiO 3 ceramics. It was observed that the high-temperature electronic transport properties are independent of the choice of praseodymium doping source for samples prepared following our synthesis strategy. Theoretical calculations were also performed in order to estimate the maximum achievable power factor and the corresponding optimal carrier concentration. The result suggests the possibility of further improvement of the power factor. This study should shed some light on the superior electronic transport in bulk polycrystalline Pr-doped SrTiO 3 ceramics and provide new insight on further improvement of the thermoelectric power factor

  18. New insights on the synthesis and electronic transport in bulk polycrystalline Pr-doped SrTiO3−δ

    KAUST Repository

    Dehkordi, Arash Mehdizadeh

    2015-02-07

    Recently, we have reported a significant enhancement in the electronic and thermoelectric properties of bulk polycrystalline SrTiO3 ceramics via praseodymium doping. This improvement was originated from the simultaneous enhancement in the thermoelectric power factor and reduction in thermal conductivity, which was contributed to the non-uniform distribution of Pr dopants. In order to further understand the underlying mechanism, we herein investigate the role of praseodymium doping source (Pr2O3 versus Pr6O11) on the synthesis and electronic transport in Pr-doped SrTiO3 ceramics. It was observed that the high-temperature electronic transport properties are independent of the choice of praseodymium doping source for samples prepared following our synthesis strategy. Theoretical calculations were also performed in order to estimate the maximum achievable power factor and the corresponding optimal carrier concentration. The result suggests the possibility of further improvement of the power factor. This study should shed some light on the superior electronic transport in bulk polycrystalline Pr-doped SrTiO3 ceramics and provide new insight on further improvement of the thermoelectric power factor.

  19. Preparation of high-purity Pr{sup 3+} doped Ge–As–Se–In–I glasses for active mid-infrared optics

    Energy Technology Data Exchange (ETDEWEB)

    Karaksina, E.V.; Shiryaev, V.S., E-mail: shiryaev@ihps.nnov.ru; Kotereva, T.V.; Velmuzhov, A.P.; Ketkova, L.A.; Snopatin, G.E.

    2016-09-15

    The multi-stage method for the synthesis of high-purity Ge–As–Se–In–I glasses doped with Pr{sup 3+} ions is developed. It is based on the chemical distillation purification of glass-forming melt and the chemical transport reactions for purification and vacuum loading of indium. The level of purity of glasses, synthesized by this method, is higher in comparison with the traditional direct melting method for glass synthesis. The high-purity Pr{sup 3+}-doped Ge–As–Se–In and Pr{sup 3+}-doped Ge–As–Se–In–I glass samples are prepared; the optical, thermal and luminescent properties are investigated. The purest host glass samples, obtained by the multi-stage purification techniques, contain a low concentration of limiting impurities: hydrogen − ≤0.05 ppm (wt) and oxygen − ≤0.1 ppm (wt), that is, at present, the best result for multi-component chalcogenide glasses for mid-IR active fibers. The samples of Pr{sup 3+}-doped Ge–As–Se–In glass fibers have the minimum optical losses of 0.58 dB/m at the wavelength of 2.72 μm and exhibit an intense broadband luminescence in the spectral range of 3.5–5.5 μm, with a maximum shifted to longer wavelengths as compared with the bulk samples.

  20. Synthesis and thermoelectric properties of fine-grained FeVSb system half-Heusler compound polycrystals with high phase purity

    International Nuclear Information System (INIS)

    Zou Minmin; Li Jingfeng; Guo Peijun; Kita, Takuji

    2010-01-01

    Nearly single-phased FeVSb half-Heusler compound thermoelectric materials with fine grains of diameter 100-200 nm were prepared from their elemental powders by combining mechanical alloying (MA) and spark plasma sintering. The resultant bulk samples showed a relatively low room-temperature electrical resistivity on the order of 10 μΩm, and a moderate negative Seebeck coefficient with a maximum value of -175 μV K -1 at 300 0 C. It was found that proper excessive addition of V relative to the stoichiometric composition (FeVSb) during MA enhanced the phase purity and hence the power factor of the spark plasma sintered samples, resulting in a large power factor value of 2480 μW m -1 K -2 when the elemental powders were mixed with the composition FeV 1.15 Sb. Its thermal conductivity was significantly reduced mainly due to refined grain sizes, resulting in a high dimensionless figure of merit ZT of 0.31 at a low-to-mid temperature (300 0 C) as for undoped half-Heusler compounds.

  1. Syntheses of therapeutically active labelled molecules for metabolic and pharmacokinetic studies. Synthesis, preservation and radiochemical purity problems

    International Nuclear Information System (INIS)

    Pichat, L.

    1977-01-01

    Molecules labelled with radioactive isotopes are without question an essential tool for metabolic and pharmacokinetic studies. Carbon 14 is often preferred to tritium since it allows better observation of the fate of carbonated structures. The fact that 14 CO 2 alone is used as basic material is the distinguishing feature of syntheses with isotopic carbon. In many cases the synthesis schemes of labelled drugs diverge considerably or entirely from those normally adopted for the unlabelled product. It is usually necessary to work on micro-quantities in order to maintain high specific activities, which implies the use of special synthesis techniques and of chromatographic separation and purification methods. Radiochemical purity tests are carried out by thin layer, column and gas phase chromatography, purity and identity checks by mass spectrometry and by 13 C and proton RMN. Labelled products are radiolysed by interaction of excited species with the molecules of the compound, a phenomenon much faster with tritiated than with 14 C-labelled molecules. The radiolysis rates may be reduced by molecule dilution. For ethical reasons it is not convenient to use 14 C molecules in human experiments, but molecular labelled with stable isotopes ( 13 C, 15 N, D) can serve instead [fr

  2. ROOM TEMPERATURE BULK AND TEMPLATE-FREE SYNTHESIS OF LEUCOEMARLDINE POLYANILINE NANOFIBERS

    Science.gov (United States)

    An extremely simple single-step method is described for the bulk synthesis of nanofibers of the electronic polymer polyaniline in fully reduced state (leucoemarldine form) without using any reducing agents, surfactants, and/or large amounts of insoluble templates. Chemical oxida...

  3. Synthesis and morphological examination of high-purity Ca(OH)2 nanoparticles suitable to consolidate porous surfaces

    Science.gov (United States)

    Madrid, Juan Antonio; Lanzón, Marcos

    2017-12-01

    Adequate synthetic methods to obtain pure Ca(OH)2 nanoparticles are scarcely documented in the literature. This paper presents a complete methodology to obtain highly-pure Ca(OH)2 nanoparticles that are appropriate for strengthening heritage materials. The precipitation synthesis was operated in controlled atmosphere to avoid carbonation by atmospheric CO2. A complete purification method was developed to eliminate the sodium chloride generated in the reaction. Several analytical techniques, such as electrical conductivity, pH, ion chromatography, X-ray diffraction (XRD) and thermogravimetric analysis coupled to mass spectrometry (TGA-MS) were used to analyse both the aqueous medium and solid phase. The amount of material obtained in the synthesis (yield) was quantified throughout the purification procedure. The influence of temperature on the nanoparticles' size and stability was studied by transmission electron microscopy (HRTEM) and sedimentation tests (light scattering). It was found that the synthesis yielded high-purity nanoparticles, whose morphological features were greatly affected by the reaction temperature.

  4. The rapid synthesis of high purity [{sup 18}F]butyrophenone neuroleptics from nitro precursors for PET study

    Energy Technology Data Exchange (ETDEWEB)

    Hashizume, Kazunari; Hashimoto, Naoto; Kato, Hiroo; Cork, D G; Miyake, Yoshihiro [National Cardiovascular Center, Suita, Osaka (Japan)

    1995-04-01

    We have completed rapid syntheses of [{sup 18}F]butyrophenone neuroleptics ([{sup 18}F]haloperidol and [{sup 18}F]spiperone) from their nitro precursors in high radiochemical yields (up to 21%) by combining a one-step nitro-fluoro exchange reaction and a novel high performance liquid chromatography (HPLC) separation method. The synthesis time was ca. 95 min and both the radiochemical and chemical purities of the labeled products were over 99%. (author).

  5. Cavitational synthesis of nanostructured inorganic materials for enhanced heterogeneous catalysis

    Science.gov (United States)

    Krausz, Ivo Michael

    The synthesis of nanostructured inorganic materials by hydrodynamic cavitation processing was investigated. The goal of this work was to develop a general synthesis technique for nanostructured materials with a control over crystallite size in the 1--20 nm range. Materials with crystallite sizes in this range have shown enhanced catalytic activity compared to materials with larger crystallite sizes. Several supported and unsupported inorganic materials were studied to understand the effects of cavitation on crystallite size. Cavitation processing of calcium fluoride resulted in more spherical particles, attached to one another by melted necks. This work produced the first evidence of shock wave heating of nanostructured materials by hydrodynamic cavitation processing. Hydrodynamic cavitation synthesis of various catalytic support materials indicated that their phase composition and purity could be controlled by adjustment of the processing parameters. Zirconia/alumina supports synthesized using hydro-dynamic cavitation and calcined to 1368 K retained a high purity cubic zirconia phase, whereas classically prepared samples showed a phase transformation to monoclinic zirconia. Similarly, the synthesis of alumina resulted in materials with varying Bohmite and Bayerite contents as a function of the process parameters. High temperature calcination resulted in stable alumina supports with varying amounts of delta-, and theta-alumina. Synthesis studies of palladium and silver showed modest variations in crystallite size as a function of cavitation process parameters. Calcination resulted in larger grain materials, indicating a disappearance of intergrain boundaries. Based on these results, a new synthesis method was studied involving controlled agglomeration of small silver crystallites by hydrodynamic cavitation processing, followed by deposition on alumina. The optimal pH, concentration, and processing time for controlling the silver crystallite size in the cavitation

  6. Abridged acid-base wet-milling synthesis of high purity hydroyapatite

    Directory of Open Access Journals (Sweden)

    Sandi Carolina Ruiz-Mendoza

    2008-06-01

    Full Text Available There is a plethora of routes to produce hydroxyapatite(HA and in general calcium phosphates(CP but production usually leads to a mixture of several phases. Besides ionic contamination, most of these methods are cumbersome, restricted to small volumes of product and require a lot of thermal energy. The acid-base route eliminates foreign ions or additives and its only byproduct is water. Heterogeneous reaction drawback is that solid reactants do not easily come in contact with each other and therefore addition and stirring times become very lengthy and still the product is a mixture. The synthesis started from calcium hydroxide and phosphoric acid (PA. Ball milling was used to favor kinetics and stoichiometry. Six sets of PA addition, paddle stirring and ball milling times were used. Products were evaluated by X ray diffraction (XRD, Fourier Transform Infrared (FTIR, scanning electron microscopy (SEM, X ray fluorescence (XRF and Ca/P ratio. Chemical analysis for calcium proceeded through oxalate precipitate and phosphorus by the phosphomolibdate technique. A set of conditions yielding high purity HA was established.

  7. Synthesis of high purity tungsten nanoparticles from tungsten heavy alloy scrap by selective precipitation and reduction route

    International Nuclear Information System (INIS)

    Kamal, S.S. Kalyan; Sahoo, P.K.; Vimala, J.; Shanker, B.; Ghosal, P.; Durai, L.

    2016-01-01

    In this paper we report synthesis of tungsten nanoparticles of high purity >99.7 wt% from heavy alloy scrap using a novel chemical route of selective precipitation and reduction. The effect of Poly(vinylpyrrolidone) polymer on controlling the particle size is established through FTIR spectra and corroborated with TEM images, wherein the average size decreased form 210 to 45 nm with increasing PVP content from zero to 2 g under different experimental conditions. This process is economical as raw material is a scrap and the efficiency of the reaction is >95%. - Highlights: • Tungsten nanoparticles were synthesized from tungsten heavy alloy scrap. • A novel chemical route of precipitation and reduction with Poly(vinylpyrrolidone) polymer as stabilizer is reported. • The average size decreased form 210 to 45 nm with increasing PVP content from zero to 2 g. • High pure tungsten nanoparticles of >99.7% purity could be synthesized using this route. • Efficiency of the reaction is >95%.

  8. Synthesis of electro-active manganese oxide thin films by plasma enhanced chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Merritt, Anna R. [Energetics Research Division, Naval Air Warfare Center Weapons Division, China Lake, CA 93555 (United States); Rajagopalan, Ramakrishnan [Department of Engineering, The Pennsylvania State University, Dubois, PA 15801 (United States); Materials Research Institute, The Pennsylvania State University, University Park, PA 16802 (United States); Carter, Joshua D. [Energetics Research Division, Naval Air Warfare Center Weapons Division, China Lake, CA 93555 (United States)

    2014-04-01

    The good stability, cyclability and high specific capacitance of manganese oxide (MnO{sub x}) has recently promoted a growing interest in utilizing MnO{sub x} in asymmetric supercapacitor electrodes. Several literature reports have indicated that thin film geometries of MnO{sub x} provide specific capacitances that are much higher than bulk MnO{sub x} powders. Plasma enhanced chemical vapor deposition (PECVD) is a versatile technique for the production of metal oxide thin films with high purity and controllable thickness. In this work, MnO{sub x} thin films deposited by PECVD from a methylcyclopentadienyl manganese tricarbonyl precursor are presented and the effect of processing conditions on the quality of MnO{sub x} films is described. The film purity and oxidation state of the MnO{sub x} films were studied by Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. Preliminary electrochemical testing of MnO{sub x} films deposited on carbon fiber electrodes in aqueous electrolytes indicates that the PECVD synthesized films are electrochemically active. - Highlights: • Plasma enhanced chemical vapor deposition of manganese oxide thin films. • Higher plasma power and chamber pressure increase deposition rate. • Manganese oxide thin films are electrochemically active. • Best electrochemical performance observed for pure film with low stress • Lower capacitance observed at higher scan rates despite thin film geometry.

  9. Synthesis of Fe-based amorphous composite coatings with low purity materials by laser cladding

    Energy Technology Data Exchange (ETDEWEB)

    Zhu Qingjun [School of Materials Science and Engineering, Shandong University, Jinan 250061 (China)]. E-mail: sduzhu@yahoo.com.cn; Qu Shiyao [School of Materials Science and Engineering, Shandong University, Jinan 250061 (China); Wang Xinhong [School of Materials Science and Engineering, Shandong University, Jinan 250061 (China); Zou Zengda [School of Materials Science and Engineering, Shandong University, Jinan 250061 (China)

    2007-06-30

    Amorphous composite coatings Fe{sub 38}Ni{sub 30-X}Si{sub 16}B{sub 14}V{sub 2}M {sub X} (X = 0, 1, 2) (M contains Al, Ti, Mo, and C) were prepared with low purity of raw materials by laser cladding. X-ray diffraction and transmission electron microscopy results show that the coating have an amorphous structure with a few crystalline phase on it. The amorphous phase is the primary phase. The glass forming ability as well as the microhardness of the Fe-based alloy made from low purity raw materials can be much enhanced by adding small amount of multi-components. However, the elements addition has its optimal quantity. When X is equal to 1, the microstructure of the coating contains 97.93% amorphous phase and 2.07% crystalline phase on it. As a result, the microhardness of the coating reaches maximum. With further increasing of the additions, the amorphous phase in the coating lessens instead of augment and the crystalline phase begins to accumulate, which result in the decrease of the microhardness.

  10. Synthesis of bulk nanocrystalline Pb-Sn-Te alloy under high pressure

    International Nuclear Information System (INIS)

    Zhu, P W; Chen, L X; Jia, X; Ma, H A; Ren, G Z; Guo, W L; Liu, H J; Zou, G T

    2002-01-01

    Pb-Sn-Te bulk nanocrystalline (NC) materials are prepared successfully by quenching melts under high pressure. The mean particle size is about 100 nm and the crystal structure is NaCl type. The mechanism of formation of the bulk NC alloy is explained: there is an increasing of the nucleation rate and a decrease in the growth rate of nuclei with increase of pressure during the solidification processes. The thermoelectric properties of Pb-Sn-Te bulk NC alloy are enhanced. This method is promising for producing thermoelectric materials with improved high-energy conversion efficiency

  11. Emergent Low-Symmetry Phases and Large Property Enhancements in Ferroelectric KNbO 3 Bulk Crystals

    Energy Technology Data Exchange (ETDEWEB)

    Lummen, Tom T. A. [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 USA; Leung, J. [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 USA; Kumar, Amit [School of Mathematics and Physics, Queen' s University Belfast, University Road, Belfast BT71NN Northern Ireland UK; Wu, X. [Department of Physics, University of Texas at Austin, Austin TX 78712 USA; Ren, Y. [Department of Physics, University of Texas at Austin, Austin TX 78712 USA; VanLeeuwen, Brian K. [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 USA; Haislmaier, Ryan C. [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 USA; Holt, Martin [Center for Nanoscale Materials, Argonne National Laboratory, Argonne IL 60439 USA; Lai, Keji [Department of Physics, University of Texas at Austin, Austin TX 78712 USA; Kalinin, Sergei V. [Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge TN 37831 USA; Gopalan, Venkatraman [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 USA

    2017-06-19

    The design of new or enhanced functionality in materials is traditionally viewed as requiring the discovery of new chemical compositions through synthesis. Large property enhancements may however also be hidden within already well-known materials, when their structural symmetry is deviated from equilibrium through a small local strain or field. Here, the discovery of enhanced material properties associated with a new metastable phase of monoclinic symmetry within bulk KNbO3 is reported. This phase is found to coexist with the nominal orthorhombic phase at room temperature, and is both induced by and stabilized with local strains generated by a network of ferroelectric domain walls. While the local microstructural shear strain involved is only approximate to 0.017%, the concurrent symmetry reduction results in an optical second harmonic generation response that is over 550% higher at room temperature. Moreover, the meandering walls of the low-symmetry domains also exhibit enhanced electrical conductivity on the order of 1 S m(-1). This discovery reveals a potential new route to local engineering of significant property enhancements and conductivity through symmetry lowering in ferroelectric crystals.

  12. Synthesis of high purity monoglycerides from crude glycerol and palm stearin

    Directory of Open Access Journals (Sweden)

    Pakamas Chetpattananondh

    2008-07-01

    Full Text Available The optimum conditions for the glycerolysis of palm stearin and crude glycerol derived from biodiesel process werefound to be a reaction temperature of 200oC with a molar ratio of crude glycerol to palm stearin of 2.5:1, and a reaction timeof 20 minutes. The yield and purity of monoglycerides obtained under these conditions was satisfactory as compared withthe glycerolysis of pure glycerol. To increase the purity of monoglycerides a two-step process, removal of residual glyceroland crystallization, was proposed instead of either vacuum or molecular distillation. Residual glycerol was removed byadding hydrochloric acid followed by washing with hot water. Optimum conditions for crystallization were achieved byusing isooctane as a solvent and a turbine impeller speed of 200 rpm at a crystallization temperature of 35oC. A purity notexceeding 99 percent of monoglycerides was obtained with monopalmitin as the major product.

  13. Method of high purity silane preparation

    Science.gov (United States)

    Tsuo, Y. Simon; Belov, Eugene P.; Gerlivanov, Vadim G.; Zadde, Vitali V.; Kleschevnikova, Solomonida I.; Korneev, Nikolai N.; Lebedev, Eugene N.; Pinov, Akhsarbek B.; Ryabenko, Eugene A.; Strebkov, Dmitry S.; Chernyshev, Eugene A.

    2000-01-01

    A process for the preparation of high purity silane, suitable for forming thin layer silicon structures in various semiconductor devices and high purity poly- and single crystal silicon for a variety of applications, is provided. Synthesis of high-purity silane starts with a temperature assisted reaction of metallurgical silicon with alcohol in the presence of a catalyst. Alcoxysilanes formed in the silicon-alcohol reaction are separated from other products and purified. Simultaneous reduction and oxidation of alcoxysilanes produces gaseous silane and liquid secondary products, including, active part of a catalyst, tetra-alcoxysilanes, and impurity compounds having silicon-hydrogen bonds. Silane is purified by an impurity adsorption technique. Unreacted alcohol is extracted and returned to the reaction with silicon. Concentrated mixture of alcoxysilanes undergoes simultaneous oxidation and reduction in the presence of a catalyst at the temperature -20.degree. C. to +40.degree. C. during 1 to 50 hours. Tetra-alcoxysilane extracted from liquid products of simultaneous oxidation and reduction reaction is directed to a complete hydrolysis. Complete hydrolysis of tetra-alcoxysilane results in formation of industrial silica sol and alcohol. Alcohol is dehydrated by tetra-alcoxysilane and returned to the reaction with silicon.

  14. Crystallinity and flux pinning properties of MgB2 bulks

    International Nuclear Information System (INIS)

    Yamamoto, A.; Shimoyama, J.; Ueda, S.; Katsura, Y.; Iwayama, I.; Horii, S.; Kishio, K.

    2006-01-01

    The relationship between flux pinning properties and crystallinity of MgB 2 bulks was systematically studied. Improved flux pinning properties under high fields were observed for samples with low crystallinity. Increased impurity scattering due to strain and defects in lattice corresponding to the degraded crystallinity was considered to enhance flux pinning strength at grain boundaries. Low-temperature synthesis and carbon substitution were confirmed to be effective for degrading crystallinity of MgB 2 bulks, resulting in high critical current properties under high fields

  15. Transformation of bulk alloys to oxide nanowires

    Science.gov (United States)

    Lei, Danni; Benson, Jim; Magasinski, Alexandre; Berdichevsky, Gene; Yushin, Gleb

    2017-01-01

    One dimensional (1D) nanostructures offer prospects for enhancing the electrical, thermal, and mechanical properties of a broad range of functional materials and composites, but their synthesis methods are typically elaborate and expensive. We demonstrate a direct transformation of bulk materials into nanowires under ambient conditions without the use of catalysts or any external stimuli. The nanowires form via minimization of strain energy at the boundary of a chemical reaction front. We show the transformation of multimicrometer-sized particles of aluminum or magnesium alloys into alkoxide nanowires of tunable dimensions, which are converted into oxide nanowires upon heating in air. Fabricated separators based on aluminum oxide nanowires enhanced the safety and rate capabilities of lithium-ion batteries. The reported approach allows ultralow-cost scalable synthesis of 1D materials and membranes.

  16. Enhanced bulk heterojunction devices prepared by thermal and solvent vapor annealing processes

    Science.gov (United States)

    Forrest, Stephen R.; Thompson, Mark E.; Wei, Guodan; Wang, Siyi

    2017-09-19

    A method of preparing a bulk heterojunction organic photovoltaic cell through combinations of thermal and solvent vapor annealing are described. Bulk heterojunction films may prepared by known methods such as spin coating, and then exposed to one or more vaporized solvents and thermally annealed in an effort to enhance the crystalline nature of the photoactive materials.

  17. Influence factor on automated synthesis yield of 3'-deoxy-3'-[18F] fluorothymidine

    International Nuclear Information System (INIS)

    Zhang Jinming; Tian Jiahe; Liu Changbin; Liu Jian; Luo Zhigang

    2009-01-01

    3'-deoxy-3'-[ 18 F] fluorothymidine ( 18 F-FLT) was prepared from N-BOC precursor to improve the synthesis yield, chemical purity and radiochemical purity of 18 F-FLT by home-made automated synthesis module. The results showed that residual water in synthesis system and the amount of precursor could affect the synthesis yield dramatically. The more the amount of precursor, the higher the synthesis yield of N-BOC. The residual water can decrease the synthesis yield. In the presence of excess base, the precursor was consumed by elimination before substitution was completed. The precursor to base was optimal in 1 to 1. The balance of semi-preparatiove HPLC Column can affect purified the final 18 F-FLT product. The chemical purity of 18 F-FLT could be decreased with 8% EtOH as mobile phase in semi-preparatiove HPLC. The high chemical purity, radiochemical purity and synthesis yield could be obtained by optimized the parameter of synthesis with home-made automated synthesis module. (authors)

  18. Flame spray synthesis under a non-oxidizing atmosphere: Preparation of metallic bismuth nanoparticles and nanocrystalline bulk bismuth metal

    Energy Technology Data Exchange (ETDEWEB)

    Grass, Robert N.; Stark, Wendelin J. [Institute for Chemical and Bioengineering, ETH Zuerich (Switzerland)], E-mail: wendelin.stark@chem.ethz.ch

    2006-10-15

    Metallic bismuth nanoparticles of over 98% purity were prepared by a modified flame spray synthesis method in an inert atmosphere by oxygen-deficient combustion of a bismuth-carboxylate based precursor. The samples were characterized by X-ray diffraction, thermal analysis and scanning electron microscopy confirming the formation of pure, crystalline metallic bismuth nanoparticles. Compression of the as-prepared powder resulted in highly dense, nanocrystalline pills with strong electrical conductivity and bright metallic gloss.

  19. Measurement of oxide-layer thickness of internal granules in high-purity aluminium

    International Nuclear Information System (INIS)

    Takacs, S.; Ditroi, F.; Mahunka, I.

    1989-01-01

    Charged-particle activation analysis was used for the determination of bulk oxygen concentration in aluminium. High-purity aluminium samples and mixtures containing different amounts of alumina were irradiated by 13 MeV 3 He particles. The aim of the investigation was to determine the oxide-layer thickness on the surface of internal aluminium granules. The measurement was carried out by determining the bulk oxygen concentration in the samples, and calculating the oxide-layer thickness, by using model conditions about the microstructure of the aluminium samples. (author) 5 refs

  20. Strengthening Purity: Moral Purity as a Mediator of Direct and Extended Cross-Group Friendships on Sexual Prejudice.

    Science.gov (United States)

    Vezzali, Loris; Brambilla, Marco; Giovannini, Dino; Paolo Colucci, Francesco

    2017-01-01

    The present research investigated whether enhanced perceptions of moral purity drive the effects of intergroup cross-group friendships on the intentions to interact with homosexuals. High-school students (N = 639) reported their direct and extended cross-group friendships with homosexuals as well as their beliefs regarding the moral character of the sexual minority. Participants further reported their desire to interact with homosexuals in the future. Results showed that both face-to-face encounters and extended contact with homosexuals increased their perceived moral purity, which in turn fostered more positive behavioral intentions. Results further revealed the specific role of moral purity in this sense, as differential perceptions along other moral domains (autonomy and community) had no mediation effects on behavioral tendencies toward homosexuals. The importance of these findings for improving intergroup relations is discussed, together with the importance of integrating research on intergroup contact and morality.

  1. Scalable preparation of high purity rutin fatty acid esters following enzymatic synthesis

    DEFF Research Database (Denmark)

    Lue, Bena-Marie; Guo, Zheng; Xu, Xuebing

    2010-01-01

    Investigations into expanded uses of modified flavonoids are often limited by the availability of these high purity compounds. As such, a simple, effective and relatively fast method for isolation of gram quantities of both long and medium chain fatty acid esters of rutin following scaled......-up biosynthesis reactions was established. Acylation reactions of rutin and palmitic or lauric acids were efficient in systems containing dried acetone and molecular sieves, yielding from 70–77% bioconversion after 96 h. Thereafter, high purity isolates (>97%) were easily obtained in significant quantities...

  2. The Simple, Effective Synthesis of Highly Dispersed Pd/C and CoPd/C Heterogeneous Catalysts via Charge-Enhanced Dry Impregnation

    Directory of Open Access Journals (Sweden)

    Lawrence D’Souza

    2016-05-01

    Full Text Available Pd/C and CoPd/C heterogeneous catalysts have been synthesized by adopting Charge Enhanced Dry Impregnation (CEDI. The particles size distribution, their high metal surface-to-bulk ratios, and synthesis feasibility are unmatchable to any known noble metal bimetallic heterogeneous catalyst preparation techniques. Next generation Fuel Cells and Fischer-Tropsch catalytic processes economy will be benefited from the proposed methodology.

  3. Large-Scale Surfactant-Free Synthesis of p-Type SnTe Nanoparticles for Thermoelectric Applications

    Directory of Open Access Journals (Sweden)

    Guang Han

    2017-02-01

    Full Text Available A facile one-pot aqueous solution method has been developed for the fast and straightforward synthesis of SnTe nanoparticles in more than ten gram quantities per batch. The synthesis involves boiling an alkaline Na2SnO2 solution and a NaHTe solution for short time scales, in which the NaOH concentration and reaction duration play vital roles in controlling the phase purity and particle size, respectively. Spark plasma sintering of the SnTe nanoparticles produces nanostructured compacts that have a comparable thermoelectric performance to bulk counterparts synthesised by more time- and energy-intensive methods. This approach, combining an energy-efficient, surfactant-free solution synthesis with spark plasma sintering, provides a simple, rapid, and inexpensive route to p-type SnTe nanostructured materials.

  4. Combinatorial processing libraries for bulk BiFeO3-PbTiO3 piezoelectric ceramics

    International Nuclear Information System (INIS)

    Hu, W.; Tan, X.; Rajan, K.

    2010-01-01

    A high throughput approach for generating combinatorial libraries with varying processing conditions for bulk ceramics has been developed. This approach utilized the linear temperature gradient in a tube furnace to screen a whole temperature range for optimized preparation. With this approach, the processing of 0.98[0.6BiFeO 3 -0.4PbTiO 3 ]-0.02Pb(Mg 1/3 Nb 2/3 )O 3 ceramic powders and pellets for high-temperature piezoelectric applications was demonstrated to identify the best synthesis conditions for phase purity. The dielectric property measurement on the as-processed solid solution ceramics confirmed the high Curie temperature and the improved loss tangent with the Pb(Mg 1/3 Nb 2/3 )O 3 doping. (orig.)

  5. Preparation of high-purity Pr(3+) doped Ge–Ga–Sb–Se glasses with intensive middle infrared luminescence

    Energy Technology Data Exchange (ETDEWEB)

    Karaksina, E.V.; Shiryaev, V.S., E-mail: shiryaev@ihps.nnov.ru; Kotereva, T.V.; Churbanov, M.F.

    2016-02-15

    Glass materials with high emission characteristics and low content of limiting impurities are required for creation of devices for middle infrared (mid-IR) fiber optics. The paper presents the results of preparation of high-purity Pr{sup 3+}-doped Ga{sub x}Ge{sub y}Sb{sub z}Se{sub 1−(x+y+z)} (x=3÷4, y=20÷26, z=5÷11) glasses. The multi-stage technique for synthesis of these glasses is developed. It is based on chemical distillation purification of glass components and the transport reaction for purification of gallium. Transmitting, as well as thermal and luminescent properties of glasses are investigated. The content of limiting impurities of oxygen, carbon and hydrogen in the glass samples was ≤0.2 ppm wt. The 1300–3000 ppm wt Pr{sup 3+}-doped Ga–Ge–Sb–Se bulk glasses exhibit an intensive photoluminescence in the spectral range of 3.5–5.5 μm.

  6. Enhancement of magnetic coupling between permanent magnets and bulk superconductors through iron embedding

    International Nuclear Information System (INIS)

    Seki, H.; Kurabayashi, H.; Suzuki, A.; Ikeda, M.; Akiyama, S.; Murakami, M.

    2009-01-01

    Magnetic torque can be transferred without contact through the coupling of permanent magnets (PM) and bulk superconductors (BSC). For this purpose, permanent magnets should have multiple pole configuration like NSNS. The magnitude of the transferable torque depends on the field strength and the gap between PM and BSC. It was found that the torque decays quickly with the gap. In order to enhance the strength of transferable magnetic torque, we prepared bulk Y-Ba-Cu-O superconductors for which Fe bars are embedded. Holes about 1 mm in diameter were mechanically drilled into bulk Y-Ba-Cu-O, and Fe bars about 0.9 mm in diameter were inserted followed by impregnation of Bi-Pb-Sn alloys with low melting points. The composite of Y-Ba-Cu-O and Fe bars attract magnetic fields generated from permanent magnet before cooling, and thereby magnetic coupling will be improved. We have found that the magnetic torque force can be greatly enhanced through iron embedding.

  7. Aspects of 6-[18F]fluoro-L-DOPA preparation: precursor synthesis, preparative HPLC purification and determination of radiochemical purity

    International Nuclear Information System (INIS)

    Fuechtner, F.; Angelberger, P.; Kvaternik, H.; Hammerschmidt, F.; Simovc, B. Peric; Steinbach, J.

    2002-01-01

    A modified method for the synthesis of the intermediate product N-Boc-3,4-di(Boc-O)-6-iodo-L-phenylalanine ethyl ester of the [ 18 F]FDOPA precursor preparation was developed. With the application of bis-(trifluoroacetoxy)-iodobenzene for the iodination step with elemental iodine the yield of the intermediate can be increased from 12% to 50-60%. By replacing silica-gel-based RP HPLC column by a polymer-based column for semi-preparative purification of [ 18 F]FDOPA from the reaction mixture the radiochemical purity of the final product can be increased up to >99%. For the determination of the radiochemical impurity [ 18 F]fluoride a HPLC method using a column with polymer-based RP material was introduced

  8. Simultaneous synthesis of single-walled carbon nanotubes and graphene in a magnetically-enhanced arc plasma.

    Science.gov (United States)

    Li, Jian; Shashurin, Alexey; Kundrapu, Madhusudhan; Keidar, Michael

    2012-02-02

    Carbon nanostructures such as single-walled carbon nanotubes (SWCNT) and graphene attract a deluge of interest of scholars nowadays due to their very promising application for molecular sensors, field effect transistor and super thin and flexible electronic devices(1-4). Anodic arc discharge supported by the erosion of the anode material is one of the most practical and efficient methods, which can provide specific non-equilibrium processes and a high influx of carbon material to the developing structures at relatively higher temperature, and consequently the as-synthesized products have few structural defects and better crystallinity. To further improve the controllability and flexibility of the synthesis of carbon nanostructures in arc discharge, magnetic fields can be applied during the synthesis process according to the strong magnetic responses of arc plasmas. It was demonstrated that the magnetically-enhanced arc discharge can increase the average length of SWCNT (5), narrow the diameter distribution of metallic catalyst particles and carbon nanotubes (6), and change the ratio of metallic and semiconducting carbon nanotubes (7), as well as lead to graphene synthesis (8). Furthermore, it is worthwhile to remark that when we introduce a non-uniform magnetic field with the component normal to the current in arc, the Lorentz force along the J×B direction can generate the plasmas jet and make effective delivery of carbon ion particles and heat flux to samples. As a result, large-scale graphene flakes and high-purity single-walled carbon nanotubes were simultaneously generated by such new magnetically-enhanced anodic arc method. Arc imaging, scanning electron microscope (SEM), transmission electron microscope (TEM) and Raman spectroscopy were employed to analyze the characterization of carbon nanostructures. These findings indicate a wide spectrum of opportunities to manipulate with the properties of nanostructures produced in plasmas by means of controlling the

  9. High-purity Cu nanocrystal synthesis by a dynamic decomposition method

    OpenAIRE

    Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

    2014-01-01

    Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential sca...

  10. Fire Synthesis

    Indian Academy of Sciences (India)

    industrial floor is the gradual replacement of conventional metal or plastic materials with ... is a simpler method that can be adopted for the bulk production of high purity alumina and .... Nitrogen is considered to have zero valency. For example:.

  11. Development of superconductor bulk for superconductor bearing

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Chan Joong; Jun, Byung Hyuk; Park, Soon Dong (and others)

    2008-08-15

    Current carrying capacity is one of the most important issues in the consideration of superconductor bulk materials for engineering applications. There are numerous applications of Y-Ba-Cu-O (YBCO) bulk superconductors e.g. magnetic levitation train, flywheel energy storage system, levitation transportation, lunar telescope, centrifugal device, magnetic shielding materials, bulk magnets etc. Accordingly, to obtain YBCO materials in the form of large, single crystals without weak-link problem is necessary. A top seeded melt growth (TSMG) process was used to fabricate single crystal YBCO bulk superconductors. The seeded and infiltration growth (IG) technique was also very promising method for the synthesis of large, single-grain YBCO bulk superconductors with good superconducting properties. 5 wt.% Ag doped Y211 green compacts were sintered at 900 .deg. C {approx} 1200 .deg.C and then a single crystal YBCO was fabricated by an infiltration method. A refinement and uniform distribution of the Y211 particles in the Y123 matrix were achieved by sintering the Ag-doped samples. This enhancement of the critical current density was ascribable to a fine dispersion of the Y211 particles, a low porosity and the presence of Ag particles. In addition, we have designed and manufactured large YBCO single domain with levitation force of 10-13 kg/cm{sup 2} using TSMG processing technique.

  12. Synthesis of polyaryl rigid-core carbosilane dendrimers for supported organic synthesis

    NARCIS (Netherlands)

    Wander, M.; Hausoul, P.J.C.; Sliedregt, L.A.J.M.; van Steen, B.J.; van Koten, G.; Klein Gebbink, R.J.M.

    2009-01-01

    Carbosilane dendrimers can be used as soluble supports for organic synthesis, since their structure allows separation of excess reagents from the supported products, eventually yielding products of high purity and in high yield, as in solid-phase organic synthesis (SPOS). In previous studies often

  13. Photochemical Synthesis of Silver Nanodecahedrons and Related Nanostructures for Plasmonic Field Enhancement Applications

    Science.gov (United States)

    Lu, Haifei

    Noble-metal nanocrystals have received considerable attention in recent years for their size and shape dependent localized surface Plasmon resonances (LSPR). Various applications based on colloidal nanoparticles, such as surface enhanced Raman scattering (SERS), surface enhanced fluorescence (SEF), plasmonic sensing, photothermal therapy etc., have been broadly explored in the field of biomedicine, because of their extremely large optical scattering and absorption cross sections, as well as giant electric field enhancement on their surface. However, despite its high chemical stability, gold exhibits quite large losses and electric field enhancement is comparatively weaker than silver. Silver nanoparticles synthesized by the traditional technique only cover an LSPR ranged from 420~500 nm. On the other hand, the range of 500~660 nm, which is covered by several easily available commercial laser lines, very limited colloidal silver nanostructures with controllable size and shape have been reported, and realization of tuning the resonance to longer wavelengths is very important for the practical applications. In this thesis, a systematic study on photochemical synthesis of silver nanodecahedrons (NDs) and related nanostructures, and their plasmonic field enhancements are presented. First, the roles of chemicals and the light source during the formation of silver nanoparticles have been studied. We have also developed a preparation route for the production size-controlled silver nanodecahedrons (LSPR range 420 ~ 660 nm) in high purity. Indeed our experiments indicate that both the chemicals and the light sources can affect the shape and purity of final products. Adjusting the molar ratio between sodium citrate and silver nitrate can help to control the crystal structure following rapid reduction from sodium borohydride. Light from a blue LED (465 nm) can efficiently transform the polyvinylpyrrolidone stabilized small silver nanoparticles into silver NDs through photo

  14. Synthesis of Bulk Superconducting Magnesium Diboride

    Directory of Open Access Journals (Sweden)

    Margie Olbinado

    2002-06-01

    Full Text Available Bulk polycrystalline superconducting magnesium diboride, MgB2, samples were successfully prepared via a one-step sintering program at 750°C, in pre Argon with a pressure of 1atm. Both electrical resistivity and magnetic susceptibility measurements confirmed the superconductivity of the material at 39K, with a transition width of 5K. The polycrystalline nature, granular morphology, and composition of the sintered bulk material were confirmed using X-ray diffractometry (XRD, scanning electron microscopy (SEM, and energy dispersive X-ray analysis (EDX.

  15. Deuterium permeation and diffusion in high-purity beryllium

    International Nuclear Information System (INIS)

    Abramov, E.; Riehm, M.P.; Thompson, D.A.; Smeltzer, W.W.

    1990-01-01

    The permeation rate of deuterium through high-purity beryllium membranes was measured using the gas-driven permeation technique. The time-dependent and the steady-state deuterium flux data were analyzed and the effective diffusivities of the samples were determined. Using multilayer permeation theory the effects of surface oxide were eliminated and the diffusion coefficients of the bulk beryllium determined. The diffusion parameters obtained for the extra-grade beryllium samples (99.8%) are D 0 =6.7x10 -9 m 2 /s and E D =28.4 kJ/mol. For the high-grade beryllium samples (99%) the parameters are D 0 =8.0x10 -9 m 2 /s and E D =35.1 kJ/mol. (orig.)

  16. Continuous microwave flow synthesis of mesoporous hydroxyapatite

    International Nuclear Information System (INIS)

    Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O.; Hussain, Rafaqat

    2015-01-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca 2+ ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA

  17. Continuous microwave flow synthesis of mesoporous hydroxyapatite

    Energy Technology Data Exchange (ETDEWEB)

    Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini [Department of Chemistry, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Lintang, Hendrik O. [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Hussain, Rafaqat, E-mail: rafaqat@kimia.fs.utm.my [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia)

    2015-11-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca{sup 2+} ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA.

  18. Disgust and the moralization of purity.

    Science.gov (United States)

    Horberg, E J; Oveis, Christopher; Keltner, Dacher; Cohen, Adam B

    2009-12-01

    Guided by appraisal-based models of the influence of emotion upon judgment, we propose that disgust moralizes--that is, amplifies the moral significance of--protecting the purity of the body and soul. Three studies documented that state and trait disgust, but not other negative emotions, moralize the purity moral domain but not the moral domains of justice or harm/care. In Study 1, integral feelings of disgust, but not integral anger, predicted stronger moral condemnation of behaviors violating purity. In Study 2, experimentally induced disgust, compared with induced sadness, increased condemnation of behaviors violating purity and increased approval of behaviors upholding purity. In Study 3, trait disgust, but not trait anger or trait fear, predicted stronger condemnation of purity violations and greater approval of behaviors upholding purity. We found that, confirming the domain specificity of the disgust-purity association, disgust was unrelated to moral judgments about justice (Studies 1 and 2) or harm/care (Study 3). Finally, across studies, individuals of lower socioeconomic status (SES) were more likely than individuals of higher SES to moralize purity but not justice or harm/care.

  19. Sorption-enhanced water gas shift reaction for high-purity hydrogen production: Application of a Na-Mg double salt-based sorbent and the divided section packing concept

    International Nuclear Information System (INIS)

    Lee, Chan Hyun; Lee, Ki Bong

    2017-01-01

    Highlights: •Na-Mg double salt-based sorbent was used for high-temperature CO 2 sorption. •Divided section packing concept was applied to the SE-WGS reaction. •High-purity H 2 was produced from the SE-WGS reaction with divided section packing. •High-purity H 2 productivity could be further enhanced by modifying packing method. -- Abstract: Hydrogen is considered a promising environmentally benign energy carrier because it has high energy density and produces no pollutants when it is converted into other types of energy. The sorption-enhanced water gas shift (SE-WGS) reaction, where the catalytic WGS reaction and byproduct CO 2 removal are carried out simultaneously in a single reactor, has received considerable attention as a novel method for high-purity hydrogen production. Since the high-purity hydrogen productivity of the SE-WGS reaction is largely dependent on the performance of the CO 2 sorbent, the development of sorbents having high CO 2 sorption capacity is crucial. Recently, a Na-Mg double salt-based sorbent has been considered for high-temperature CO 2 capture since it has been reported to have a high sorption capacity and fast sorption kinetics. In this study, the SE-WGS reaction was experimentally demonstrated using a commercial catalyst and a Na-Mg double salt-based sorbent. However, the SE-WGS reaction with a one-body hybrid solid, a physical admixture of catalyst and sorbent, showed poor reactivity and reduced CO 2 sorption uptake. As a result, a divided section packing concept was suggested as a solution. In the divided section packing method, the degree of mixing for the catalyst and sorbent in a column can be controlled by the number of sections. High-purity hydrogen (<10 ppm CO) was produced directly from the SE-WGS reaction with divided section packing, and the hydrogen productivity was further improved when the reactor column was divided into more sections and packed with more sorbent.

  20. Suppression of bulk conductivity in InAs/GaSb broken gap composite quantum wells

    Energy Technology Data Exchange (ETDEWEB)

    Charpentier, Christophe; Fält, Stefan; Reichl, Christian; Nichele, Fabrizio; Nath Pal, Atindra; Pietsch, Patrick; Ihn, Thomas; Ensslin, Klaus; Wegscheider, Werner [Laboratory for Solid State Physics, ETH Zürich, 8093 Zürich (Switzerland)

    2013-09-09

    The two-dimensional topological insulator state in InAs/GaSb quantum wells manifests itself by topologically protected helical edge channel transport relying on an insulating bulk. This work investigates a way of suppressing bulk conductivity by using gallium source materials of different degrees of impurity concentrations. While highest-purity gallium is accompanied by clear conduction through the sample bulk, intentional impurity incorporation leads to a bulk resistance over 1 MΩ, independent of applied magnetic fields. In addition, ultra high electron mobilities for GaAs/AlGaAs structures fabricated in a molecular beam epitaxy system used for the growth of Sb-based samples are reported.

  1. Deuterium permeation and diffusion in high purity beryllium

    International Nuclear Information System (INIS)

    Abramov, E.

    1990-05-01

    The permeation rate of deuterium through high-purity beryllium membranes was measured using the gas-driven permeation technique. The time-dependent and the steady-state deuterium flux data were analyzed and the effective diffusivities of the samples were determined. A multilayer permeation theory was used in order to eliminate the surface oxide effects and the diffusion coefficients of the bulk beryllium were determined. The diffusion parameters obtained for the extra-grade beryllium samples (99.8%) are D 0 = 6.7 x 10 -9 [m 2 /s] and E D = 28.4 [KJ/mol]; and for the high-grade beryllium samples (99%) the parameters are D 0 = 8.0 x 10 -9 [m 2 /s] and E D = 35.1 [KJ/mol

  2. Enantioselective synthesis of 6-[18F] fluoro-L-DOPA

    International Nuclear Information System (INIS)

    Zhang Lan; Tang Ganghua; Zhou Wei; Li Junling; Yin Duanzhi; Wang Yongxian; Tang Xiaolan; Huang Zuhan

    2002-01-01

    Trimethylammonium veratraldehyde triflate was synthesized and used as a precurser for the synthesis of 6-[ 18 F] Fluoro-L-DOPA by using the chiral phase-transfer catalyst, O-Allyl-N-(9)-anthracenylcinchonidinium bromide which was also synthesized in this study. Based on these, 6-[ 18 F] Fluoro-L-DOPA was prepared with acceptable radiochemical yield (10 ± 3)% in short synthesis time (80 min), with high radiochemical purity, specific activity and chemical purity

  3. Feasibility of introducing ferromagnetic materials to onboard bulk high-Tc superconductors to enhance the performance of present maglev systems

    International Nuclear Information System (INIS)

    Deng, Zigang; Wang, Jiasu; Zheng, Jun; Zhang, Ya; Wang, Suyu

    2013-01-01

    Highlights: ► Ferromagnetic materials guide the flux distribution of the PMG to bulk positions. ► With ferromagnetic materials, guidance performance can be enhanced greatly. ► A new HTS Maglev system with onboard ferromagnetic materials is designed. ► The design can meet large guidance force requirements for practical applications. -- Abstract: Performance improvement is a long-term research task for the promotion of practical application of promising high-temperature superconducting (HTS) magnetic levitation (maglev) vehicle technologies. We studied the feasibility to enhance the performance of present HTS Maglev systems by introducing ferromagnetic materials to onboard bulk superconductors. The principle here is to make use of the high magnetic permeability of ferromagnetic materials to alter the flux distribution of the permanent magnet guideway for the enhancement of magnetic field density at the position of the bulk superconductors. Ferromagnetic iron plates were added to the upper surface of bulk superconductors and their geometric and positioning effects on the maglev performance were investigated experimentally. Results show that the guidance performance (stability) was enhanced greatly for a particular setup when compared to the present maglev system which is helpful in the application where large guidance forces are needed such as maglev tracks with high degrees of curves

  4. An Innovative Electrolysis Approach for the Synthesis of Metal Matrix Bulk Nanocomposites: A Case Study on Copper-Niobium System

    Science.gov (United States)

    Shokrvash, Hussein; Rad, Rahim Yazdani; Massoudi, Abouzar

    2018-04-01

    Design and synthesis of a prototype Cu-Nb nanocomposite are presented. Oxygen-free Cu-Nb nanocomposites were prepared using an electrolysis facility with special emphasis on the cathodic deoxidation of Cu and nanometric Nb2O5 blends in a molten NaCl-CaCl2 electrolyte. The as-prepared nanocomposites were characterized by X-ray diffraction and energy-dispersive X-ray spectroscopy. The elemental analysis of the Cu matrix and Nb phase revealed the high solubility of Nb in the Cu structure (0.85 at. pct) and Cu in the Nb structure (10.59 at. pct) over short synthesis times (4-5 hours). Furthermore, precise analysis using field emission scanning electron microscopy and transmission electron microscopy confirmed the unique structure and nanocomposite morphology of the Cu-Nb nanocomposite. The successful synthesis of Cu-Nb nanocomposites offers a new conceptual and empirical outlook on the generation of bulk nanostructures of immiscible bimetals using electro-synthesis.

  5. Full Automatic synthesis of [18F]FMISO

    International Nuclear Information System (INIS)

    Seung Jun Oh; Se Hun Kang; Jin-Sook Ryu; Dae Hyuk Moon

    2004-01-01

    [ 18 F]FMISO is a radiopharmaceutical for hypoxia imaging. Although it was developed in 1986, there has been no report about automatic synthesis. In this experiment, we established the full automatic synthesis of [ 18 F]FMISO and evaluate the stability according to ICH guideline. Method: We used GE MicroLab MX for automatic synthesis. Sequence program was modified to control of the module as follows: [ 18 F]Fluoride drying→[ 18 F]fluorination→trapping of reaction mixture on C18 cartridge→purification-elution of reaction mixture→hydrolysis and HPLC purification. We used disposable cassette for each synthesis and discard it after synthesis. To find optimal synthesis condition, we tested 90 120 degree C as reaction temperature, 5 15 mg of 1-(2-nitro-1-imidazolyl) -2-O-tetrahtdropyranyl-3-O-toluenesulfonyl-propanediol as precursor and 5 15 min as [ 18 F]fluorination time. HPLC purification condition was EtOH:H20 = 5:95, 5ml/min with Alltech Econosil column. To check the stability of production, we performed 30 times of run. We checked the radiochemical stability until 6 hours at 25 degree C and 40% humidity condition. We also performed the stability test at 50 70 degree C with 60-80% humidity condition or under UV light for 6 hours after synthesis for acceleration test, Results: The optimal [ 18 F] fluorination condition was 10mg of precursor and 15 min incubation at 110 degree C. Hydrolysis was performed at 105 degree C for 5 min. After HPLC purification, radiochemical yields and purity were 45±2.8 and 98±1.2%, respectively. Total synthesis time was 60±5.2 min. [ 18 F]FMISO was stable until 6 hours after production with 97±2.4% of radiochemical purity. [ 18 F]FMISO was also stable in acceleration test and photochemical test with 97±2.4 and 97±2.8% of radiochemical purity, respectively. Conclusion: We established the full automatic synthesis method of [ 18 F]FMISO with reproducible high production yield. [18F]FMISO synthesized by this method was stable

  6. Feasibility of introducing ferromagnetic materials to onboard bulk high-Tc superconductors to enhance the performance of present maglev systems

    Science.gov (United States)

    Deng, Zigang; Wang, Jiasu; Zheng, Jun; Zhang, Ya; Wang, Suyu

    2013-02-01

    Performance improvement is a long-term research task for the promotion of practical application of promising high-temperature superconducting (HTS) magnetic levitation (maglev) vehicle technologies. We studied the feasibility to enhance the performance of present HTS Maglev systems by introducing ferromagnetic materials to onboard bulk superconductors. The principle here is to make use of the high magnetic permeability of ferromagnetic materials to alter the flux distribution of the permanent magnet guideway for the enhancement of magnetic field density at the position of the bulk superconductors. Ferromagnetic iron plates were added to the upper surface of bulk superconductors and their geometric and positioning effects on the maglev performance were investigated experimentally. Results show that the guidance performance (stability) was enhanced greatly for a particular setup when compared to the present maglev system which is helpful in the application where large guidance forces are needed such as maglev tracks with high degrees of curves.

  7. The synthesis of nanostructured, phase pure catalysts by hydrodynamic cavitation

    Energy Technology Data Exchange (ETDEWEB)

    Moser, W.R.; Sunstrom, J.E.; Marshik-Geurts, B.J. [Worcester Polytechnic Institute, Worcester, MA (United States)

    1995-12-01

    A new process for the synthesis of advanced catalytic materials based on performing the synthesis under hydrodynamic cavitation conditions has been discovered. This continuous process for catalyst synthesis resulted in the formation of both supported and unsupported catalysts. The advantage of the process over classical methods of synthesis is that it permits the formation of a wide variety of nanostructured catalysts in exceptionally high phase purities. The synthesis of platinum and palladium catalysts supported on alumina and other supports resulted in high dispersions of the noble metals. The synthesis of alpha, beta- and gamma-bismuth molybdates resulted in catalysts having superior phase purities as compared to several other classical methods of synthesis. The beta-bismuth molybdate was synthesized directly onto Cabosil. These studies showed that the particle size of the active component could be varied from a few manometers to much larger grains. The process enabled the synthesis of other complex metal oxides like perovskites as pure phases. The process uses a commercially available Microfluidizer.

  8. Corrosion of high purity Fe-Cr-Ni alloys in 13 N boiling nitric acid

    International Nuclear Information System (INIS)

    Ohta, Joji; Mayuzumi, Masami; Kusanagi, Hideo; Takaku, Hiroshi

    1998-01-01

    Corrosion in boiling nitric acid was investigated for high purity Fe-18%Cr-12%Ni alloys and type 304L stainless steels (SS). Owing to very low impurity concentration, the solution treated high purity alloys show almost no intergranular corrosion while the type 304L SS show severe intergranular corrosion. Both in the high purity alloys and type 304L SS, aging treatments ranging from 873 K to 1073 K for 1 h enhance intergranular corrosion. During the aging treatments, impurities should be segregated to the grain boundaries. The corrosion behaviors were discussed from a standpoint of impurity segregation to grain boundaries. This study is of importance for purex reprocessing of spent fuels

  9. Bulk and nanocrystalline electron doped Gd0.15Ca0.85MnO3: Synthesis and magnetic characterization

    Science.gov (United States)

    Dhal, Lakshman; Chattarpal; Nirmala, R.; Santhosh, P. N.; Kumary, T. Geetha; Nigam, A. K.

    2014-09-01

    Polycrystalline Gd0.15Ca0.85MnO3 sample was prepared by solid state reaction method and nanocrystalline samples of different grain sizes of the same were prepared by sol-gel method. Phase purity and composition were verified by room temperature X-ray diffraction and SEM-EDAX analysis. Magnetization data of bulk Gd0.15Ca0.85MnO3 in 5 kOe field shows a peak at 119 K (TN) suggesting an antiferromagnetic transition. Nanocrystalline Gd0.15Ca0.85MnO3 sample ( 54 nm size) also shows a cusp at 107 K and a broad thermal hysteresis between field cooled cooling (FCC) and field cooled warming (FCW) data around this temperature. This thermal hysteresis suggests possible crystal structural transition. Field variation of magnetization of bulk Gd0.15Ca0.85MnO3 at 5 K shows a tendency to saturate, but yields a magnetic moment value of only 1.12 μB/f.u. in 70 kOe. The value of magnetization of nanocrystalline sample at 5 K in 70 kOe field is slightly larger and is 1.38 μB/f.u. which is probably due to the surface moments of the nanoparticle samples. Both the samples show Curie-Weiss-like behaviour in their paramagnetic state.

  10. Synthesis of high purity rutile nanoparticles from medium-grade Egyptian natural ilmenite

    Directory of Open Access Journals (Sweden)

    Mohamed G. Shahien

    2015-09-01

    Full Text Available The Egyptian magmatic ilmenite is classified as a medium-grade ore. The present work is an attempt to produce a high-quality TiO2 that can be used in several industries from this medium-grade raw material using the mechanical activation, carbothermic reduction, hydrochloric acid leaching and calcination. A mixture from the ilmenite (FeTiO3 and activated carbon was milled for 30 h. This mixture was annealed at 1200 °C for one hour and the product was leached by hydrochloric acid and calcined at 600 °C for two hours. The role of the ball milling was to grind the raw ilmenite to obtain the nano size, and the carbothermic reduction was to reduce all the Fe-Ti phases to a mixture from Fe metal and TiO2. Leaching procedure was carried out to remove all the Fe metal and obtain a high-grade TiO2. After leaching and calcination of the milled and annealed mixture of FeTiO3/C under the optimal conditions, TiO2 nanoparticles with a size of 10–100 nm and purity more than 95% were obtained. The qualifications of the synthesized high purity rutile nanoparticles from the Egyptian natural ilmenite match the conditions of many industrial applications.

  11. Fabrication high-purity Fe nanochains with near theoretical limit value of saturation magnetization of bulk Fe

    Energy Technology Data Exchange (ETDEWEB)

    Bian, Erkang [Henan University, Key Laboratory for Special Functional Materials of Ministry of Education (China); Xu, Yanling [Henan University, The Audit Department (China); Lou, Shiyun, E-mail: lousy@henu.edu.cn [Henan University, Key Laboratory for Special Functional Materials of Ministry of Education (China); Fu, Yunlong, E-mail: yunlongfu@dns.sxnu.edu.cn [Shanxi Normal University, School of Chemistry and Material Science (China); Zhou, Shaomin, E-mail: smzhou@henu.edu.cn [Henan University, Key Laboratory for Special Functional Materials of Ministry of Education (China)

    2016-11-15

    High-yield purity chain-like one-dimensional nanostructures consisting of single crystal Fe nanoparticles have been produced by using solution dispersion approach. Room temperature magnetic measurement shows that the as-fabricated Fe nanochains are ferromagnetic with a high saturation magnetization (203 emu/g) whereas the nanoparticles are single magnetic domains, which indicate that the as-synthesized products have superparamagnetism behavior with the saturation magnetization of about 28 emu/g. Maybe this results from the directional alignment of the nanoparticles. The excellent characteristic may have led to the potential applications in spin filtering, high density magnetic recording, and nanosensors.

  12. Enhancement of surface magnetism due to bulk bond dilution

    International Nuclear Information System (INIS)

    Tsallis, C.; Sarmento, E.F.; Albuquerque, E.L. de

    1985-01-01

    Within a renormalization group scheme, the phase diagram of a semi-infinite simple cubic Ising ferromagnet is discussed, with arbitrary surface and bulk coupling constants, and including possible dilution of the bulk bonds. It is obtained that dilution makes easier the appearance of surface magnetism in the absence of bulk magnetism. (Author) [pt

  13. Feasibility of introducing ferromagnetic materials to onboard bulk high-T{sub c} superconductors to enhance the performance of present maglev systems

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Zigang, E-mail: zgdeng@gmail.com [Applied Superconductivity Laboratory (ASCLab), Southwest Jiaotong University (SWJTU), Chengdu, Sichuan 610031 (China); State Key Laboratory of Traction Power (TPL), Southwest Jiaotong University (SWJTU), Chengdu, Sichuan 610031 (China); Wang, Jiasu [Applied Superconductivity Laboratory (ASCLab), Southwest Jiaotong University (SWJTU), Chengdu, Sichuan 610031 (China); Zheng, Jun; Zhang, Ya [Applied Superconductivity Laboratory (ASCLab), Southwest Jiaotong University (SWJTU), Chengdu, Sichuan 610031 (China); State Key Laboratory of Traction Power (TPL), Southwest Jiaotong University (SWJTU), Chengdu, Sichuan 610031 (China); Wang, Suyu [Applied Superconductivity Laboratory (ASCLab), Southwest Jiaotong University (SWJTU), Chengdu, Sichuan 610031 (China)

    2013-02-14

    Highlights: ► Ferromagnetic materials guide the flux distribution of the PMG to bulk positions. ► With ferromagnetic materials, guidance performance can be enhanced greatly. ► A new HTS Maglev system with onboard ferromagnetic materials is designed. ► The design can meet large guidance force requirements for practical applications. -- Abstract: Performance improvement is a long-term research task for the promotion of practical application of promising high-temperature superconducting (HTS) magnetic levitation (maglev) vehicle technologies. We studied the feasibility to enhance the performance of present HTS Maglev systems by introducing ferromagnetic materials to onboard bulk superconductors. The principle here is to make use of the high magnetic permeability of ferromagnetic materials to alter the flux distribution of the permanent magnet guideway for the enhancement of magnetic field density at the position of the bulk superconductors. Ferromagnetic iron plates were added to the upper surface of bulk superconductors and their geometric and positioning effects on the maglev performance were investigated experimentally. Results show that the guidance performance (stability) was enhanced greatly for a particular setup when compared to the present maglev system which is helpful in the application where large guidance forces are needed such as maglev tracks with high degrees of curves.

  14. Purity and crystallinity of microwave synthesized antimony sulfide microrods

    Energy Technology Data Exchange (ETDEWEB)

    Martínez-Alonso, Claudia, E-mail: claudiamartinezalonso30@gmail.com [Facultad de Química, Universidad Autónoma de Querétaro, Querétaro, Querétaro, 76010 (Mexico); Olivos-Peralta, Eliot U. [Instituto de Energías Renovables, Universidad NacionalAutónoma de México, Temixco, Morelos, 62580 (Mexico); Sotelo-Lerma, Mérida [Universidad de Sonora, Hermosillo, Sonora, 83000 (Mexico); Sato-Berrú, Roberto Y. [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, MéxicoD.F., 04510 (Mexico); Mayén-Hernández, S.A. [Facultad de Química, Universidad Autónoma de Querétaro, Querétaro, Querétaro, 76010 (Mexico); Hu, Hailin, E-mail: hzh@ier.unam.mx [Instituto de Energías Renovables, Universidad NacionalAutónoma de México, Temixco, Morelos, 62580 (Mexico)

    2017-01-15

    Antimony sulfide (Sb{sub 2}S{sub 3}) is a promising semiconductor material for solar cell applications. In this work, microrods of Sb{sub 2}S{sub 3} were synthesized by microwave heating with different sulfur sources, solvents, temperature, heating rate, power, and solution concentration. It was found that 90% of stoichiometric Sb{sub 2}S{sub 3} can be obtained with thiourea (TU) or thioacetamide (TA) as sulfur sources and that their optical band gap values were within the range of 1.59–1.60 eV. The most crystalline Sb{sub 2}S{sub 3} were obtained by using TU. The morphology of the Sb{sub 2}S{sub 3} with TU the individual rods were exhibited, whereas rods bundles appeared in TA-based products. The solvents were ethylene glycol (EG) and dimethylformamide (DMF). EG generates more heat than DMF during the microwave synthesis. As a result, the Sb{sub 2}S{sub 3} obtained with EG contained a larger percentage of oxygen and smaller crystal sizes compared to those from DMF. On the other hand, the length and diameter of Sb{sub 2}S{sub 3} microrods can be increased by applying higher heating power although the crystal size did not change at all. In summary, pure and highly crystalline Sb{sub 2}S{sub 3} microrods of 6–10 μm long and 330–850 nm in diameter can be obtained by the microwave method with a careful selection of chemical and thermodynamic parameters of the synthesis. - Highlights: • Purity up to 90% of crystalline Sb{sub 2}S{sub 3} nanorods can be obtained by microwave heating. • The combination of solvent and sulfide type affects crystallinity & purity of Sb2S3. • The high pressure generated in microwave heating helps to form Sb{sub 2}S{sub 3} nanorods.

  15. Purity and crystallinity of microwave synthesized antimony sulfide microrods

    International Nuclear Information System (INIS)

    Martínez-Alonso, Claudia; Olivos-Peralta, Eliot U.; Sotelo-Lerma, Mérida; Sato-Berrú, Roberto Y.; Mayén-Hernández, S.A.; Hu, Hailin

    2017-01-01

    Antimony sulfide (Sb_2S_3) is a promising semiconductor material for solar cell applications. In this work, microrods of Sb_2S_3 were synthesized by microwave heating with different sulfur sources, solvents, temperature, heating rate, power, and solution concentration. It was found that 90% of stoichiometric Sb_2S_3 can be obtained with thiourea (TU) or thioacetamide (TA) as sulfur sources and that their optical band gap values were within the range of 1.59–1.60 eV. The most crystalline Sb_2S_3 were obtained by using TU. The morphology of the Sb_2S_3 with TU the individual rods were exhibited, whereas rods bundles appeared in TA-based products. The solvents were ethylene glycol (EG) and dimethylformamide (DMF). EG generates more heat than DMF during the microwave synthesis. As a result, the Sb_2S_3 obtained with EG contained a larger percentage of oxygen and smaller crystal sizes compared to those from DMF. On the other hand, the length and diameter of Sb_2S_3 microrods can be increased by applying higher heating power although the crystal size did not change at all. In summary, pure and highly crystalline Sb_2S_3 microrods of 6–10 μm long and 330–850 nm in diameter can be obtained by the microwave method with a careful selection of chemical and thermodynamic parameters of the synthesis. - Highlights: • Purity up to 90% of crystalline Sb_2S_3 nanorods can be obtained by microwave heating. • The combination of solvent and sulfide type affects crystallinity & purity of Sb2S3. • The high pressure generated in microwave heating helps to form Sb_2S_3 nanorods.

  16. Texturing for bulk α-Fe/Nd2Fe14B nanocomposites with enhanced magnetic properties

    International Nuclear Information System (INIS)

    Lou, L.; Hou, F.C.; Wang, Y.N.; Cheng, Y.; Li, H.L.; Li, W.; Guo, D.F.; Li, X.H.; Zhang, X.Y.

    2014-01-01

    In the present study, the texturing of bulk α-Fe/Nd 2 Fe 14 B nanocomposites produced from Nd-lean amorphous Nd x Fe 92.5−x Cu 1.5 B 6 (x=9 to 11.5 at%) via a hot deformation under a uniaxial stress of ∼350 MPa at 973 K has been studied. An enhanced (00l) texture of the hard phase is observed with increasing Nd content, which results in an increase in the magnetic anisotropy of the nanocomposite magnets. As a result, both the coercivity and the remanence of the magnets increase simultaneously with increasing Nd content from x=9–11.5 at%, yielding a significant enhancement of the maximum energy product from (BH) max =13.2 to 17.5 MGOe in the direction parallel to stress axis. - Highlights: • Textured bulk α-Fe/Nd 2 Fe 14 B nanocomposites have been produced from Nd-lean alloys. • Nd content has an effect on the texturing of α-Fe/Nd 2 Fe 14 B nanocomposite magnets. • An enhanced (00l) texture of hard phase is observed with increasing Nd content. • Both the coercivity and remanence increase simultaneously with Nd content

  17. Thermal conductivity of high purity vanadium

    International Nuclear Information System (INIS)

    Jung, W.D.

    1975-01-01

    The thermal conductivity, Seebeck coefficient, and electrical resistivity of four high-purity vanadium samples were measured over the temperature range 5 to 300 0 K. The highest purity sample had a resistance ratio (rho 273 /rho 4 . 2 ) of 1524. The highest purity sample had a thermal conductivity maximum of 920 W/mK at 9 0 K and had a thermal conductivity of 35 W/mK at room temperature. At low temperatures, the thermal resistivity was limited by the scattering of electrons by impurities and phonons. The thermal resistivity of vanadium departed from Matthiessen's rule at low temperatures. The electrical resistivity and Seebeck coefficient of high purity vanadium showed no anomalous behavior above 130 0 K. The intrinsic electrical resistivity at low temperatures was due primarily to interband scattering of electrons. The Seebeck coefficient was positive from 10 to 240 0 K and had a maximum which was dependent upon sample purity

  18. Fabrication of Bi2223 bulks with high critical current properties sintered in Ag tubes

    Energy Technology Data Exchange (ETDEWEB)

    Takeda, Yasuaki, E-mail: ytakeda@g.ecc.u-tokyo.ac.jp [Department of Applied Chemistry, University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan); Shimoyama, Jun-ichi; Motoki, Takanori [Department of Physics and Mathematics, Aoyama Gakuin University, 5-10-1 Fuchinobe, Chuo-ku, Sagamihara, Kanagawa 252-5258 (Japan); Kishio, Kohji [Department of Applied Chemistry, University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan); Nakashima, Takayoshi; Kagiyama, Tomohiro; Kobayashi, Shin-ichi; Hayashi, Kazuhiko [Sumitomo Electric Industries, Ltd. 1-1-3 Shimaya, Konohana-ku, Osaka 554-0024 (Japan)

    2017-03-15

    Highlights: • Fabrication conditions of Bi2223 bulks was reconsidered in terms of high J{sub c}. • Pressure of uniaxial pressing and heat treatment conditions were investigated. • The best sample showed higher J{sub c} than that of practically used Bi2223 bulks. - Abstract: Randomly grain oriented Bi2223 sintered bulks are one of the representative superconducting materials having weak-link problem due to very short coherence length particularly along the c-axis, resulting in poor intergrain J{sub c} properties. In our previous studies, sintering and/or post-annealing under moderately reducing atmospheres were found to be effective for improving grain coupling in Bi2223 sintered bulks. Further optimizations of the synthesis process for Bi2223 sintered bulks were attempted in the present study to enhance their intergrain J{sub c}. Effects of applied pressure of uniaxial pressing and sintering conditions on microstructure and superconducting properties have been systematically investigated. The best sample showed intergrain J{sub c} of 2.0 kA cm{sup −2} at 77 K and 8.2 kA cm{sup −2} at 20 K, while its relative density was low ∼65%. These values are quite high as for a randomly oriented sintered bulk of cuprate superconductors.

  19. High Purity Hydrogen Production with In-Situ Carbon Dioxide and Sulfur Capture in a Single Stage Reactor

    Energy Technology Data Exchange (ETDEWEB)

    Nihar Phalak; Shwetha Ramkumar; Daniel Connell; Zhenchao Sun; Fu-Chen Yu; Niranjani Deshpande; Robert Statnick; Liang-Shih Fan

    2011-07-31

    Enhancement in the production of high purity hydrogen (H{sub 2}) from fuel gas, obtained from coal gasification, is limited by thermodynamics of the water gas shift (WGS) reaction. However, this constraint can be overcome by conducting the WGS in the presence of a CO{sub 2}-acceptor. The continuous removal of CO{sub 2} from the reaction mixture helps to drive the equilibrium-limited WGS reaction forward. Since calcium oxide (CaO) exhibits high CO{sub 2} capture capacity as compared to other sorbents, it is an ideal candidate for such a technique. The Calcium Looping Process (CLP) developed at The Ohio State University (OSU) utilizes the above concept to enable high purity H{sub 2} production from synthesis gas (syngas) derived from coal gasification. The CLP integrates the WGS reaction with insitu CO{sub 2}, sulfur and halide removal at high temperatures while eliminating the need for a WGS catalyst, thus reducing the overall footprint of the hydrogen production process. The CLP comprises three reactors - the carbonator, where the thermodynamic constraint of the WGS reaction is overcome by the constant removal of CO{sub 2} product and high purity H{sub 2} is produced with contaminant removal; the calciner, where the calcium sorbent is regenerated and a sequestration-ready CO{sub 2} stream is produced; and the hydrator, where the calcined sorbent is reactivated to improve its recyclability. As a part of this project, the CLP was extensively investigated by performing experiments at lab-, bench- and subpilot-scale setups. A comprehensive techno-economic analysis was also conducted to determine the feasibility of the CLP at commercial scale. This report provides a detailed account of all the results obtained during the project period.

  20. Thermal Plasma Synthesis of Crystalline Gallium Nitride Nanopowder from Gallium Nitrate Hydrate and Melamine

    Directory of Open Access Journals (Sweden)

    Tae-Hee Kim

    2016-02-01

    Full Text Available Gallium nitride (GaN nanopowder used as a blue fluorescent material was synthesized by using a direct current (DC non-transferred arc plasma. Gallium nitrate hydrate (Ga(NO33∙xH2O was used as a raw material and NH3 gas was used as a nitridation source. Additionally, melamine (C3H6N6 powder was injected into the plasma flame to prevent the oxidation of gallium to gallium oxide (Ga2O3. Argon thermal plasma was applied to synthesize GaN nanopowder. The synthesized GaN nanopowder by thermal plasma has low crystallinity and purity. It was improved to relatively high crystallinity and purity by annealing. The crystallinity is enhanced by the thermal treatment and the purity was increased by the elimination of residual C3H6N6. The combined process of thermal plasma and annealing was appropriate for synthesizing crystalline GaN nanopowder. The annealing process after the plasma synthesis of GaN nanopowder eliminated residual contamination and enhanced the crystallinity of GaN nanopowder. As a result, crystalline GaN nanopowder which has an average particle size of 30 nm was synthesized by the combination of thermal plasma treatment and annealing.

  1. Neurotensin enhances estradiol induced DNA synthesis in immature rat uterus

    Energy Technology Data Exchange (ETDEWEB)

    Mistry, A.; Vijayan, E.

    1985-05-27

    Systemic administration of Neurotensin, a tridecapeptide, in immature rats treated with estradiol benzoate significantly enhances uterine DNA synthesis as reflected by the incorporation of /sup 3/H-thymidine. The peptide may have a direct action on the uterus. Substance P, a related peptide, had no effect on uterine DNA synthesis. 18 references, 4 tables.

  2. Synthesis of graphene using gamma radiations

    Indian Academy of Sciences (India)

    Considering the advantages of radiolytic synthesis such as the absence of toxic chemical as a reducing agent, uniform distribution of reducing agent and high purity of product, the synthesis of graphene (rGO) from graphene oxide (GO) by the gamma irradiation technique using a relatively low dose rate of 0.24 kGy h−1 has ...

  3. Enhanced infrared magneto-optical response of the nonmagnetic semiconductor BiTeI driven by bulk Rashba splitting

    Energy Technology Data Exchange (ETDEWEB)

    Demko, L.; Tokura, Y. [Multiferroics Project, ERATO, JST, c/o Department of Applied Physics, University of Tokyo (Japan); Schober, G.A.H. [Institute for Theoretical Physics, University of Heidelberg (Germany); Kocsis, V.; Kezsmarki, I. [Department of Physics, Budapest University of Technology and Economics and Condensed Matter Research Group of the Hungarian Academy of Sciences (Hungary); Bahramy, M.S.; Murakawa, H. [CMRG and CERG, RIKEN ASI (Japan); Lee, J.S.; Arita, R.; Nagaosa, N. [Department of Applied Physics, University of Tokyo (Japan)

    2013-07-01

    We study the magneto-optical (MO) response of the polar semiconducting BiTeI with giant bulk Rashba spin splitting at various carrier densities. Despite being nonmagnetic, the material is found to yield a huge MO activity in the infrared region under moderate magnetic fields (up to 3 T). Our first-principles calculations show that the enhanced MO response of BiTeI comes mainly from the intraband transitions between the Rashba-split bulk conduction bands. These transitions connecting electronic states with opposite spin directions become active due to the presence of strong spin-orbit interaction and give rise to distinct features in the MO spectra with a systematic doping dependence. We predict an even more pronounced enhancement in the low-energy MO response and dc Hall effect near the crossing (Dirac) point of the conduction bands.

  4. Synthesis and Characterization of the in Situ Bulk Polymerization of PMMA Containing Graphene Sheets Using Microwave Irradiation

    Directory of Open Access Journals (Sweden)

    Mohammad A. Aldosari

    2013-03-01

    Full Text Available Polymethylmethacrylate–graphene (PMMA/RGO nanocomposites were prepared via in situ bulk polymerization using two different preparation techniques. In the first approach, a mixture of graphite oxide (GO and methylmethacrylate monomers (MMA were polymerized using a bulk polymerization method with a free radical initiator. After the addition of the reducing agent hydrazine hydrate (HH, the product was reduced via microwave irradiation (MWI to obtain R-(GO-PMMA composites. In the second approach, a mixture of graphite sheets (RGO and MMA monomers were polymerized using a bulk polymerization method with a free radical initiator to obtain RGO-(PMMA composites. The composites were characterized by FTIR, 1H-NMR and Raman spectroscopy and XRD, SEM, TEM, TGA and DSC. The results indicate that the composite obtained using the first approach, which involved MWI, had a better morphology and dispersion with enhanced thermal stability compared with the composites prepared without MWI.

  5. Influence of solvents on the changes in structure, purity, and in vitro characteristics of green-synthesized ZnO nanoparticles from Costus igneus

    Science.gov (United States)

    Nandhini, G.; Suriyaprabha, R.; Maria Sheela Pauline, W.; Rajendran, V.; Aicher, Wilhelm Karl; Awitor, Oscar Komla

    2018-05-01

    The present study is intended to produce high-purity zinc oxide nanoparticles from the leaves of Costus igneus and zinc acetate precursor via sustainable methods by the tribulation with three different solvents (hot water, methanol, and acetone) for the extraction of plant compounds. While examining the physico-chemical characteristics of ZnO nanoparticles incurred by the catalysis of plant bioactive compounds extracted from different solvents, the hot water extract-based green synthesis process yields higher purity (99.89%) and smaller particle size (94 nm) than other solvents. The optimization of the solvents used for the green synthesis of nanoparticles renders key identification in appropriate extraction of bioactive compounds suitable for the nucleation/production of nanoparticles in addition to annealing temperature. The impregnable usage of ZnO nanoparticles in clinical applications is further confirmed based on the treatment of particles (1-10 mg ml-1) against Gram-positive (S. aureus and S. epidermis) and Gram-negative bacteria (E. coli and K. pneumoniae) with respect to their growth inhibition. An in-force growth inhibition against particular S. aureus and S. epidermis imparted by the low concentration of ZnO nanoparticles signifies the utilization and consumption of green-synthesized high-purity nanoparticles for therapeutic and cosmetic applications.

  6. High-Purity Semiconducting Single-Walled Carbon Nanotubes: A Key Enabling Material in Emerging Electronics.

    Science.gov (United States)

    Lefebvre, Jacques; Ding, Jianfu; Li, Zhao; Finnie, Paul; Lopinski, Gregory; Malenfant, Patrick R L

    2017-10-17

    Semiconducting single-walled carbon nanotubes (sc-SWCNTs) are emerging as a promising material for high-performance, high-density devices as well as low-cost, large-area macroelectronics produced via additive manufacturing methods such as roll-to-roll printing. Proof-of-concept demonstrations have indicated the potential of sc-SWCNTs for digital electronics, radiofrequency circuits, radiation hard memory, improved sensors, and flexible, stretchable, conformable electronics. Advances toward commercial applications bring numerous opportunities in SWCNT materials development and characterization as well as fabrication processes and printing technologies. Commercialization in electronics will require large quantities of sc-SWCNTs, and the challenge for materials science is the development of scalable synthesis, purification, and enrichment methods. While a few synthesis routes have shown promising results in making near-monochiral SWCNTs, gram quantities are available only for small-diameter sc-SWCNTs, which underperform in transistors. Most synthesis routes yield mixtures of SWCNTs, typically 30% metallic and 70% semiconducting, necessitating the extraction of sc-SWCNTs from their metallic counterparts in high purity using scalable postsynthetic methods. Numerous routes to obtain high-purity sc-SWCNTs from raw soot have been developed, including density-gradient ultracentrifugation, chromatography, aqueous two-phase extraction, and selective DNA or polymer wrapping. By these methods (termed sorting or enrichment), >99% sc-SWCNT content can be achieved. Currently, all of these approaches have drawbacks and limitations with respect to electronics applications, such as excessive dilution, expensive consumables, and high ionic impurity content. Excess amount of dispersant is a common challenge that hinders direct inclusion of sc-SWCNTs into electronic devices. At present, conjugated polymer extraction may represent the most practical route to sc-SWCNTs. By the use of

  7. Evaluation of an automated double-synthesis module: efficiency and reliability of subsequent radiosyntheses of FHBG and FLT

    International Nuclear Information System (INIS)

    Niedermoser, Sabrina; Pape, Manuela; Gildehaus, Franz Josef; Wängler, Carmen; Hartenbach, Markus; Schirrmacher, Ralf; Bartenstein, Peter; Wängler, Björn

    2012-01-01

    We optimized the synthesis methods for 3′-deoxy-3′-[ 18 F]fluorothymidine ([ 18 F]FLT) and 9-(4-[ 18 F]fluoro-3-[hydroxymethyl]butyl)guanine) ([ 18 F]FHBG) and automated them on an Explora General Nucleophilic double-synthesis module. Furthermore, the synthesis efficiency and reliability and the formation of cross-contaminations of the products when preparing two consecutive batches were evaluated. Whereas the preinstalled FLT synthesis conditions required substantial modification in reaction and neutralization conditions to achieve radiochemical yields of up to 60% within 70±10 min including high-performance liquid chromatography purification, the synthesis of FHBG had to be implemented to the module to obtain competitive radiochemical yields of up to 40% in an overall synthesis time of 60±10 min. The radiochemical purities obtained were ≥99% and ≥96% for the synthesis of [ 18 F]FLT and [ 18 F]FHBG, respectively. No significant changes in yield or purity could be observed between both batch productions. We found that the yields and purities also did not change when performing FLT after FHBG syntheses and vice versa. Hence, we developed a synthesis setup that offers the opportunity to perform two subsequent syntheses of either [ 18 F]FLT, [ 18 F]FHBG or [ 18 F]FLT after [ 18 F]FHBG without decrease in radiochemical yields and purities. Also, no cross-contaminations were observed, which can be attributed to the use of separate product delivery tubes, purification columns and an automated intermediate cleaning program. These results open up the possibility of producing consecutively either two equal 18 F-fluorinated tracers or two different ones in high yields on the same synthesis module.

  8. Synthesis de 1-dotriacotanol

    International Nuclear Information System (INIS)

    Hernandez, L.; Gonzalez, J.C.

    1996-01-01

    In order to prepare isotopic labeled long chain aliphatic primary alcohol's, the synthesis overall yielding and chemical purity of 1-dotriacotanol were 41% and 98%, respectively. This procedure is very useful for carbon-14 and tritium labeling at Beta position of saturated fatty alcohol's

  9. Recovery of high-purity metallic Pd from Pd(II)-sorbed biosorbents by incineration.

    Science.gov (United States)

    Won, Sung Wook; Lim, Areum; Yun, Yeoung-Sang

    2013-06-01

    This work reports a direct way to recover metallic palladium with high purity from Pd(II)-sorbed polyethylenimine-modified Corynebacterium glutamicum biosorbent using a combined method of biosorption and incineration. This study is focused on the incineration part which affects the purity of recovered Pd. The incineration temperature and the amount of Pd loaded on the biosorbent were considered as major factors in the incineration process, and their effects were examined. The results showed that both factors significantly affected the enhancement of the recovery efficiency and purity of the recovered Pd. SEM-EDX and XRD analyses were used to confirm that Pd phase existed in the ash. As a result, the recovered Pd was changed from PdO to zero-valent Pd as the incineration temperature was increased from 600 to 900°C. Almost 100% pure metallic Pd was recovered with recovery efficiency above 99.0% under the conditions of 900°C and 136.9 mg/g. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. Facile synthesis of upconversion nanoparticles with high purity using lanthanide oleate compounds

    Science.gov (United States)

    Kang, Ning; Ai, Chao-Chao; Zhou, Ya-Ming; Wang, Zuo; Ren, Lei

    2018-02-01

    A novel strategy for preparing highly pure NaYF4-based upconversion nanoparticles (UCNPs) was developed using lanthanide oleate compounds [Ln(OA)3] as the precursor, denoted as the Ln-OA preparation method. Compared to the conventional solvothermal method for synthesizing UCNPs using lanthanide chloride compounds (LnCl3) as the precursor (denoted as the Ln-Cl method), the Ln-OA strategy exhibited the merits of high purity, reduced purification process and a uniform size in preparing core and core-shell UCNPs excited by a 980 or 808 nm near infrared (NIR) laser. This work sheds new insight on the preparation of UCNPs and promotes their application in biomedical fields.

  11. Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

    Science.gov (United States)

    Nanjundaswamy, K. S.; Standlee, D.; Kelly, C. O.; Whiteley, R. V., Jr.

    1997-01-01

    A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

  12. Cuprous Oxide Scale up: Gram Production via Bulk Synthesis using Classic Solvents at Low Temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Hall, A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Han, T. Y. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2015-05-07

    Cuprous oxide is a p-type semiconducting material that has been highly researched for its interesting properties. Many small-scale syntheses have exhibited excellent control over size and morphology. As the demand for cuprous oxide grows, the synthesis method need to evolve to facilitate large-scale production. This paper supplies a facile bulk synthesis method for Cu₂O on average, 1-liter reaction volume can produce 1 gram of particles. In order to study the shape and size control mechanisms on such a scale, the reaction volume was diminished to 250 mL producing on average 0.3 grams of nanoparticles per batch. Well-shaped nanoparticles have been synthesized using an aqueous solution of CuCl₂, NaOH, SDS surfactant, and NH₂OH-HCl at mild temperatures. The time allotted between the addition of NaOH and NH₂OH-HCl was determined to be critical for Cu(OH)2 production, an important precursor to the final produce The effects of stirring rates on a large scale was also analyzed during reagent addition and post reagent addition. A morphological change from rhombic dodecahedra to spheres occurred as the stirring speed was increased. The effects of NH₂OH-HCl concentration were also studied to control the etching effects of the final product.

  13. Compact Layers of Hybrid Halide Perovskites Fabricated via the Aerosol Deposition Process-Uncoupling Material Synthesis and Layer Formation.

    Science.gov (United States)

    Panzer, Fabian; Hanft, Dominik; Gujar, Tanaji P; Kahle, Frank-Julian; Thelakkat, Mukundan; Köhler, Anna; Moos, Ralf

    2016-04-08

    We present the successful fabrication of CH₃NH₃PbI₃ perovskite layers by the aerosol deposition method (ADM). The layers show high structural purity and compactness, thus making them suitable for application in perovskite-based optoelectronic devices. By using the aerosol deposition method we are able to decouple material synthesis from layer processing. Our results therefore allow for enhanced and easy control over the fabrication of perovskite-based devices, further paving the way for their commercialization.

  14. Synthesis of indium nanoparticles at ambient temperature; simultaneous phase transfer and ripening

    Energy Technology Data Exchange (ETDEWEB)

    Aghazadeh Meshgi, Mohammad; Kriechbaum, Manfred [Graz University of Technology, Institute of Inorganic Chemistry (Austria); Biswas, Subhajit; Holmes, Justin D., E-mail: j.holmes@ucc.ie [University College Cork, Materials Chemistry and Analysis Group, Department of Chemistry and the Tyndall National Institute (Ireland); Marschner, Christoph, E-mail: christoph.marschner@tugraz.at [Graz University of Technology, Institute of Inorganic Chemistry (Austria)

    2016-12-15

    The synthesis of size-monodispersed indium nanoparticles via an innovative simultaneous phase transfer and ripening method is reported. The formation of nanoparticles occurs in a one-step process instead of well-known two-step phase transfer approaches. The synthesis involves the reduction of InCl{sub 3} with LiBH{sub 4} at ambient temperature and although the reduction occurs at room temperature, fine indium nanoparticles, with a mean diameter of 6.4 ± 0.4 nm, were obtained directly in non-polar n-dodecane. The direct synthesis of indium nanoparticles in n-dodecane facilitates their fast formation and enhances their size-monodispersity. In addition, the nanoparticles were highly stable for more than 2 months. The nanoparticles were characterised by dynamic light scattering (DLS), small angle X-ray scattering (SAXS), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) and Fourier transform infrared (FT-IR) spectroscopy to determine their morphology, structure and phase purity.

  15. Establishing comparability and compatibility in the purity assessment of high purity zinc as demonstrated by the CCQM-P149 intercomparison

    Science.gov (United States)

    Vogl, Jochen; Kipphardt, Heinrich; Richter, Silke; Bremser, Wolfram; del Rocío Arvizu Torres, María; Manzano, Judith Velina Lara; Buzoianu, Mirella; Hill, Sarah; Petrov, Panayot; Goenaga-Infante, Heidi; Sargent, Mike; Fisicaro, Paola; Labarraque, Guillaume; Zhou, Tao; Turk, Gregory C.; Winchester, Michael; Miura, Tsutomu; Methven, Brad; Sturgeon, Ralph; Jährling, Reinhard; Rienitz, Olaf; Mariassy, Michal; Hankova, Zuzana; Sobina, Egor; Ivanovich Krylov, Anatoly; Anatolievich Kustikov, Yuri; Vladimirovich Smirnov, Vadim

    2018-04-01

    For the first time, an international comparison was conducted on the determination of the purity of a high purity element. Participants were free to choose any analytical approach appropriate for their institute’s applications and services. The material tested was a high purity zinc, which had earlier been assessed for homogeneity and previously used in CCQM-K72 for the determination of six defined metallic impurities. Either a direct metal assay of the Zn mass fraction was undertaken by EDTA titrimetry, or an indirect approach was used wherein all impurities, or at least the major ones, were determined and their sum subtracted from ideal purity of 100%, or 1 kg kg-1. Impurity assessment techniques included glow discharge mass spectrometry, inductively coupled plasma mass spectrometry and carrier gas hot extraction/combustion analysis. Up to 91 elemental impurities covering metals, non-metals and semi-metals/metalloids were quantified. Due to the lack of internal experience or experimental capabilities, some participants contracted external laboratories for specific analytical tasks, mainly for the analysis of non-metals. The reported purity, expressed as zinc mass fraction in the high purity zinc material, showed excellent agreement for all participants, with a relative standard deviation of 0.011%. The calculated reference value, w(Zn)  =  0.999 873 kg kg-1, was assigned an asymmetric combined uncertainty of  +0.000 025 kg kg-1 and  -0.000 028 kg kg-1. Comparability amongst participating metrology institutes is thus demonstrated for the purity determination of high purity metals which have no particular difficulties with their decomposition/dissolution process when solution-based analytical methods are used, or which do not have specific difficulties when direct analysis approaches are used. Nevertheless, further development is required in terms of uncertainty assessment, quantification of non-metals and the determination of purity

  16. Analysis of the Purity of Cetrimide by Titrations

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov; Rasmussen, Claus/Dallerup; Nielsen, Hans/Boye

    2006-01-01

    . Titration by perchloric acid showed a 99.69 ± 0.05 % purity of cetrimide and titration by silver nitrate showed a 99.85% ± 0.05 % purity while the traditional assay method predicted a purity of only 97.1 ± 0.4. It was found that the discrepancy could be identified as differences in selectivity during...

  17. Bulk Nanostructured FCC Steels With Enhanced Radiation Tolerance

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xinghang; Hartwig, K. Ted; Allen, Todd; Yang, Yong

    2012-10-27

    The objective of this project is to increase radiation tolerance in austenitic steels through optimization of grain size and grain boundary (GB) characteristics. The focus will be on nanocrystalline austenitic Fe-Cr-Ni alloys with an fcc crystal structure. The long-term goal is to design and develop bulk nanostructured austenitic steels with enhanced void swelling resistance and substantial ductility, and to enhance their creep resistance at elevated temperatures via GB engineering. The combination of grain refinement and grain boundary engineering approaches allows us to tailor the material strength, ductility, and resistance to swelling by 1) changing the sink strength for point defects, 2) by increasing the nucleation barriers for bubble formation at GBs, and 3) by changing the precipitate distributions at boundaries. Compared to ferritic/martensitic steels, austenitic stainless steels (SS) possess good creep and fatigue resistance at elevated temperatures, and better toughness at low temperature. However, a major disadvantage of austenitic SS is that they are vulnerable to significant void swelling in nuclear reactors, especially at the temperatures and doses anticipated in the Advanced Burner Reactor. The lack of resistance to void swelling in austenitic alloys led to the switch to ferritic/martensitic steels as the preferred material for the fast reactor cladding application. Recently a type of austenitic stainless steel, HT-UPS, was developed at ORNL, and is expected to show enhanced void swelling resistance through the trapping of point defects at nanometersized carbides. Reducing the grain size and increasing the fraction of low energy grain boundaries should reduce the available radiation-produced point defects (due to the increased sink area of the grain boundaries), should make bubble nucleation at the boundaries less likely (by reducing the fraction of high-energy boundaries), and improve the strength and ductility under radiation by producing a higher

  18. Metallic oxide nano-clusters synthesis by ion implantation in high purity Fe10Cr alloy

    International Nuclear Information System (INIS)

    Zheng, Ce

    2015-01-01

    ODS (Oxide Dispersed Strengthened) steels, which are reinforced with metal dispersions of nano-oxides (based on Y, Ti and O elements), are promising materials for future nuclear reactors. The detailed understanding of the mechanisms involved in the precipitation of these nano-oxides would improve manufacturing and mechanical properties of these ODS steels, with a strong economic impact for their industrialization. To experimentally study these mechanisms, an analytical approach by ion implantation is used, to control various parameters of synthesis of these precipitates as the temperature and concentration. This study demonstrated the feasibility of this method and concerned the behaviour of alloys models (based on aluminium oxide) under thermal annealing. High purity Fe-10Cr alloys were implanted with Al and O ions at room temperature. Transmission electron microscopy observations showed that the nano-oxides appear in the Fe-10Cr matrix upon ion implantation at room temperature without subsequent annealing. The mobility of implanted elements is caused by the defects created during ion implantation, allowing the nucleation of these nanoparticles, of a few nm in diameter. These nanoparticles are composed of aluminium and oxygen, and also chromium. The high-resolution experiments show that their crystallographic structure is that of a non-equilibrium compound of aluminium oxide (cubic γ-Al 2 O 3 type). The heat treatment performed after implantation induces the growth of the nano-sized oxides, and a phase change that tends to balance to the equilibrium structure (hexagonal α-Al 2 O 3 type). These results on model alloys are fully applicable to industrial materials: indeed ion implantation reproduces the conditions of milling and heat treatments are at equivalent temperatures to those of thermo-mechanical treatments. A mechanism involving the precipitation of nano-oxide dispersed in ODS alloys is proposed in this manuscript based on the obtained experimental results

  19. Effect of zirconium purity on the glass-forming-ability and notch toughness of Cu{sub 43}Zr{sub 43}Al{sub 7}Be{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Andersen, Laura M. [Department of NanoEngineering, University of California, San Diego, 9500 Gilman Drive, La Jolla, CA (United States); Hofmann, Douglas C. [Materials Development and Manufacturing Technology Group, NASA Jet Propulsion Laboratory/California Institute of Technology, MS 18-105, 4800 Oak Grove Dr. Pasadena, CA 91109 (United States); Vecchio, Kenneth S., E-mail: kvecchio@ucsd.edu [Department of NanoEngineering, University of California, San Diego, 9500 Gilman Drive, La Jolla, CA (United States)

    2016-09-30

    The effect of substituting standard grade zirconium lump (99.8% excluding up to 4% hafnium) for high purity zirconium crystal bar (99.5%) in a Cu{sub 43}Zr{sub 43}Al{sub 7}Be{sub 7} bulk metallic glass (BMG) is examined. The final hafnium content in the BMG specimens was found to range from 0 to 0.44 at%. Introducing low purity zirconium significantly decreased the glass-forming-ability and reduced the notch toughness of the BMG. In contrast, when adding high purity hafnium to Cu{sub 43}Zr{sub 43}Al{sub 7}Be{sub 7} made with high purity zirconium, no significant change in the glass-forming-ability or toughness was observed. This suggests that the introduction of low purity zirconium in BMGs creates a more complex response than a simple addition of hafnium. It is likely that other impurities in the material, such as oxygen, play a role in the complex crystallization kinetics and change in mechanical properties. The notch toughness was measured through four-point-bend tests, which showed a decrease in notch toughness from an average of ~53 MPa m{sup 1/2} for the high purity samples to an average of ~29 MPa m{sup 1/2} with full substitution of low purity zirconium. A similar decrease in glass-forming-ability and toughness is observed in commercially synthesized high purity Cu{sub 43}Zr{sub 43}Al{sub 7}Be{sub 7}. The large scale commercial process is expected to introduced some unintentional impurities, which decrease the properties of the BMG in the same way as the lower purity elements. Lastly, Weibull statistics are used to provide an analysis of variability in toughness for both ingots synthesized in a small laboratory arc-melter and those synthesized commercially.

  20. Corrosion behavior of high purity Fe-Cr-Ni alloys in trans-passive condition

    International Nuclear Information System (INIS)

    Mayuzumi, Masami; Ohta, Jyoji; Kako, Kenji

    1998-01-01

    The corrosion behavior of high-purity (99.99%) Fe-Cr-Ni alloys was investigated in 13 N nitric acid with/without Ce 4+ ions to clarify the effect of impurities on the trans-passive corrosion of stainless steel. The following results were obtained. (1) Almost no intergranular corrosion was observed in the high-purity alloys, although the corrosion rate of the matrix region was nearly the same as that of a commercial stainless steel with the same Cr and Ni content. (2) Due to the improved intergranular corrosion resistance, the effect of the purification became significant in the corrosion condition with the grain-separation being predominant. (3) The high-purity alloys showed higher susceptivility to intergranular corrosion with aging treatment between 873 K and 1073 K. Although the sulfuric acid/copper sulfate test suggested the formation of Cr-depleted zones, a grain boundary micro-analysis using a FETEM with an EDX did not reveal any change in Cr content or impurity segregain along the grain boundaries. The mechanism of corrosion enhancement resulting from the aging treatment remains nuclear. (author)

  1. Compact Layers of Hybrid Halide Perovskites Fabricated via the Aerosol Deposition Process—Uncoupling Material Synthesis and Layer Formation

    Directory of Open Access Journals (Sweden)

    Fabian Panzer

    2016-04-01

    Full Text Available We present the successful fabrication of CH3NH3PbI3 perovskite layers by the aerosol deposition method (ADM. The layers show high structural purity and compactness, thus making them suitable for application in perovskite-based optoelectronic devices. By using the aerosol deposition method we are able to decouple material synthesis from layer processing. Our results therefore allow for enhanced and easy control over the fabrication of perovskite-based devices, further paving the way for their commercialization.

  2. Synthesis and quality control of [18F] fluorothymidine

    International Nuclear Information System (INIS)

    Nascimento, Leonardo Tafas C.; Silva, Juliana B.; Silveira, Marina B.; Santos, Priscilla F.; Faria, Tiago

    2013-01-01

    The Positron Emission Tomography (PET) is a technique that allows early diagnosis of various diseases by detecting metabolic changes of cells, in addition to being a noninvasive technique. The most widely used radiopharmaceutical for PET imaging is [ 18 F] Fludesoxiglucose ( 18 FDG), which is a marker of glucose metabolism and has high sensitivity and specificity for diagnosis and staging of various cancers. However, some carcinomas do not have high glucose consumption, besides 18 FDG possess high urinary excretion rate interfering with the detection of tumors in pelvis and high uptake in brain and in inflammation, reducing the contrast tumor / background. The radiotracer 3'-fluoro-L-3'-deoxythymidine ( 18 FLT) is an analogue of thymidine used as an alternative to 18 FDG for detecting tumors with high proliferation rate. The aim of this work was to develop [ 18 F] Fluorothymidine synthesis and quality control at the Radiopharmaceuticals Research and Production Facility of CDTN/CNEN. The synthesis was adapted from that used to 18 FDG, based on the methodologies described in related papers. Radiochemical purity and impurities levels were determined by HPLC, RTLC and GC techniques. Total synthesis time was 35 minutes and the radiochemical yield in the end of bombardment (EOB) was 7%, with a radiochemical purity of about 93%. Radionuclidic identity and purity, pH, residual solvents, radiochemical and chemical purity were evaluated according to analytical methods described on the literature and on the United States Pharmacopeia (USP 32). Residual levels of Stavudine, Thymine and Thymidine were found and are under toxicological investigation in order to establish a maximum amount allowed in the final product. (author)

  3. Release characteristics of tritium from high-purity lithium oxide

    International Nuclear Information System (INIS)

    O'Kula, K.R.; Vogelsang, W.F.

    1985-01-01

    Rates of tritium release from neutronirradiated lithium oxide were determined from isothermal release experiments. High-purity, monocrystalline lithium oxide was purged ex-reactor with helium and helium-hydrogen gas streams. Overall release was found to be controlled by solid-phase diffusion, and was predominantly in the form of condensible species. The result of an independent concentration profile analysis at 923 K was in agreement with the gas release diffusion coefficient. Sweeping the Li 2 O with hydrogen-containing gas was found to enhance tritium removal during the early stage of each run

  4. Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jilin [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Gu, Yunle [School of Material Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Li, Zili [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Wang, Weimin, E-mail: wangwm@hotmail.com [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Fu, Zhengyi [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)

    2013-06-01

    Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH{sub 4} played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B{sub 2}O{sub 3} and KBH{sub 4} as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH{sub 4} played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed.

  5. Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

    International Nuclear Information System (INIS)

    Wang, Jilin; Gu, Yunle; Li, Zili; Wang, Weimin; Fu, Zhengyi

    2013-01-01

    Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH 4 played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B 2 O 3 and KBH 4 as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH 4 played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed

  6. Evaluation of purity with its uncertainty value in high purity lead stick by conventional and electro-gravimetric methods.

    Science.gov (United States)

    Singh, Nahar; Singh, Niranjan; Tripathy, S Swarupa; Soni, Daya; Singh, Khem; Gupta, Prabhat K

    2013-06-26

    A conventional gravimetry and electro-gravimetry study has been carried out for the precise and accurate purity determination of lead (Pb) in high purity lead stick and for preparation of reference standard. Reference materials are standards containing a known amount of an analyte and provide a reference value to determine unknown concentrations or to calibrate analytical instruments. A stock solution of approximate 2 kg has been prepared after dissolving approximate 2 g of Pb stick in 5% ultra pure nitric acid. From the stock solution five replicates of approximate 50 g have been taken for determination of purity by each method. The Pb has been determined as PbSO4 by conventional gravimetry, as PbO2 by electro gravimetry. The percentage purity of the metallic Pb was calculated accordingly from PbSO4 and PbO2. On the basis of experimental observations it has been concluded that by conventional gravimetry and electro-gravimetry the purity of Pb was found to be 99.98 ± 0.24 and 99.97 ± 0.27 g/100 g and on the basis of Pb purity the concentration of reference standard solutions were found to be 1000.88 ± 2.44 and 1000.81 ± 2.68 mg kg-1 respectively with 95% confidence level (k = 2). The uncertainty evaluation has also been carried out in Pb determination following EURACHEM/GUM guidelines. The final analytical results quantifying uncertainty fulfills this requirement and gives a measure of the confidence level of the concerned laboratory. Gravimetry is the most reliable technique in comparison to titremetry and instrumental method and the results of gravimetry are directly traceable to SI unit. Gravimetric analysis, if methods are followed carefully, provides for exceedingly precise analysis. In classical gravimetry the major uncertainties are due to repeatability but in electro-gravimetry several other factors also affect the final results.

  7. Production of high purity granular metals: cadmium, zinc, lead

    Directory of Open Access Journals (Sweden)

    Shcherban A. P.

    2017-04-01

    Full Text Available Cadmium, zinc and lead are constituent components of many semiconductor compounds. The obtained high purity distillates and ingots are large-size elements, which is not always convenient to use, and thus require additional grinding, which does not always allow maintaining the purity of the original materials. For the growth of semiconductor and scintillation single crystals it is advisable to use "friable" granular high-purity distillates, which can be processed without the risk of contamination. For example, the European low-background experiment LUCIFER required more than 20 kg of high-purity granulated zinc, which was agreed to be supplied by NSC KIPT. This task was then extended to cadmium and lead. Motivated by these tasks, the authors of this paper propose complex processes of deep refining of cadmium, zinc and lead by vacuum distillation. A device producing granules has been developed. The process of granulation of high-purity metals is explored. The purity of produced granules for cadmium and zinc is >99,9999, and >99,9995% for lead granules. To prevent oxidation of metal granules during exposition to air, chemical methods of surface passivation were used. Organic solvent based on dimethylformamide used as a coolant improves the resistance of granules to atmospheric corrosion during the granulation of high purity Cd, Zn and Pb.

  8. Preparation and characterization of rare-earth bulks with controllable nanostructures

    International Nuclear Information System (INIS)

    Song Xiaoyan; Zhang Jiuxing; Li Erdong; Lu Nianduan; Yin Fuxing

    2006-01-01

    The preparation and characterization of pure rare-earth-metal bulks with controllable nanostructures are reported in this paper. A novel 'oxygen-free' in situ synthesis technique that combines inert-gas condensation with spark plasma sintering (SPS) technology is proposed. Taking into account the special mechanisms of SPS consolidation and the scale effects of nanoparticles, we introduced practical procedures for preparing rare-earth bulks of amorphous, mixed amorphous and nanocrystals, and nanocrystalline microstructures, respectively. Compared with the conventional polycrystalline bulk, these nanostructured bulks exhibit substantially improved physical and mechanical properties. This technique enables comprehensive studies on the microstructures and properties of a large variety of nanostructured metallic materials that are highly reactive in the air

  9. Effects of sintering conditions on critical current properties and microstructures of MgB2 bulks

    International Nuclear Information System (INIS)

    Yamamoto, Akiyasu; Shimoyama, Jun-ichi; Ueda, Shinya; Katsura, Yukari; Iwayama, Isao; Horii, Shigeru; Kishio, Kohji

    2005-01-01

    The effects of heating conditions on critical current properties and microstructures of undoped MgB 2 bulks were systematically studied. Strong correlation was observed between J c and microstructures. The network structure with an excellent inter-grain connectivity of MgB 2 grains contributed to high-J c under low magnetic fields, and small grain size of MgB 2 enhanced the grain boundary flux pinning. Long time heating at low temperatures below the melting point of magnesium was discovered to be most effective for synthesis of MgB 2 bulks having strongly connected MgB 2 network structure with small grains. The sample heated at 550 deg. C for 1200 h recorded a high-J c of 4.02 x 10 5 A cm -2 at 20 K in self-field, while high-temperature and long time heating brought a significant grain growth which resulted in low J c

  10. Microwave-assisted solid-phase peptide synthesis of the 60-110 domain of human pleiotrophin on 2-chlorotrityl resin.

    Science.gov (United States)

    Friligou, Irene; Papadimitriou, Evangelia; Gatos, Dimitrios; Matsoukas, John; Tselios, Theodore

    2011-05-01

    A fast and efficient microwave-assisted solid phase peptide synthesis (MW-SPPS) of a 51mer peptide, the main heparin-binding site (60-110) of human pleiotrophin (hPTN), using 2-chlorotrityl chloride resin (CLTR-Cl) following the 9-fluorenylmethyloxycarbonyl/tert-butyl (Fmoc/tBu) methodology and with the standard N,N'-diisopropylcarbodiimide/1-hydroxybenzotriazole (DIC/HOBt) coupling reagents, is described. An MW-SPPS protocol was for the first time successfully applied to the acid labile CLTR-Cl for the faster synthesis of long peptides (51mer peptide) and with an enhanced purity in comparison to conventional SPPS protocols. The synthesis of such long peptides is not trivial and it is generally achieved by recombinant techniques. The desired linear peptide was obtained in only 30 h of total processing time and in 51% crude yield, in which 60% was the purified product obtained with 99.4% purity. The synthesized peptide was purified by reversed phase high performance liquid chromatography (RP-HPLC) and identified by electrospray ionization mass spectrometry (ESI-MS). Then, the regioselective formation of the two disulfide bridges of hPTN 60-110 was successfully achieved by a two-step procedure, involving an oxidative folding step in dimethylsulfoxide (DMSO) to form the Cys(77)-Cys(109) bond, followed by iodine oxidation to form the Cys(67)-Cys(99) bond.

  11. Automated radiochemical synthesis and biodistribution of [11C]l-α-acetylmethadol ([11C]LAAM)

    International Nuclear Information System (INIS)

    Sai, Kiran Kumar Solingapuram; Fan, Jinda; Tu, Zhude; Zerkel, Patrick; Mach, Robert H.; Kharasch, Evan D.

    2014-01-01

    Long-acting opioid agonists methadone and l-α-acetylmethadol (LAAM) prevent withdrawal in opioid-dependent persons. Attempts to synthesize [ 11 C]-methadone for PET evaluation of brain disposition were unsuccessful. Owing, however, to structural and pharmacologic similarities, we aimed to develop [ 11 C]LAAM as a PET ligand to probe the brain exposure of long-lasting opioids in humans. This manuscript describes [ 11 C]LAAM synthesis and its biodistribution in mice. The radiochemical synthetic strategy afforded high radiochemical yield, purity and specific activity, thereby making the synthesis adaptable to automated modules. - Highlights: • Radiochemical synthesis of opioid [ 11 C]l-α-acetylmethadol (LAAM) described for the first time. • High radiochemical yield, purity and specific activity. • Easily reproducible and adaptable synthesis to any C-11 automated modules. • [ 11 C]LAAM utility as a PET radiopharmaceutical for assessing brain penetration

  12. Bulk and nanocrystalline electron doped Gd{sub 0.15}Ca{sub 0.85}MnO{sub 3}: Synthesis and magnetic characterization

    Energy Technology Data Exchange (ETDEWEB)

    Dhal, Lakshman; Chattarpal [Department of Physics, Indian Institute of Technology Madras, Chennai 600 036 (India); Nirmala, R., E-mail: nirmala@iitm.ac.in [Department of Physics, Indian Institute of Technology Madras, Chennai 600 036 (India); Santhosh, P.N. [Department of Physics, Indian Institute of Technology Madras, Chennai 600 036 (India); Kumary, T. Geetha [CMPD, Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102 (India); Nigam, A.K. [Tata Institute of Fundamental Research, Mumbai 400 005 (India)

    2014-09-01

    Polycrystalline Gd{sub 0.15}Ca{sub 0.85}MnO{sub 3} sample was prepared by solid state reaction method and nanocrystalline samples of different grain sizes of the same were prepared by sol–gel method. Phase purity and composition were verified by room temperature X-ray diffraction and SEM-EDAX analysis. Magnetization data of bulk Gd{sub 0.15}Ca{sub 0.85}MnO{sub 3} in 5 kOe field shows a peak at ∼119 K (T{sub N}) suggesting an antiferromagnetic transition. Nanocrystalline Gd{sub 0.15}Ca{sub 0.85}MnO{sub 3} sample (∼54 nm size) also shows a cusp at ∼107 K and a broad thermal hysteresis between field cooled cooling (FCC) and field cooled warming (FCW) data around this temperature. This thermal hysteresis suggests possible crystal structural transition. Field variation of magnetization of bulk Gd{sub 0.15}Ca{sub 0.85}MnO{sub 3} at 5 K shows a tendency to saturate, but yields a magnetic moment value of only ∼1.12 μ{sub B}/f.u. in 70 kOe. The value of magnetization of nanocrystalline sample at 5 K in 70 kOe field is slightly larger and is ∼1.38 μ{sub B}/f.u. which is probably due to the surface moments of the nanoparticle samples. Both the samples show Curie–Weiss-like behaviour in their paramagnetic state.

  13. Automated synthesis of ["1"8F](2S,4R)-4-fluoroglutamine on a GE TRACERlab™ FX-N Pro module

    International Nuclear Information System (INIS)

    Zhang, Xiang; Basuli, Falguni; Shi, Zhen-Dan; Xu, Biying; Blackman, Burchelle; Choyke, Peter L.; Swenson, Rolf E.

    2016-01-01

    Glutamine (Gln) and its analogues may serve as imaging agents for tumor diagnosis using positron emission tomography (PET), especially for tumors with negative ["1"8F]FDG scan. We report the first automated synthesis of ["1"8F](2S,4R)-4-fluoroglutamine (["1"8F]FGln) on a GE TRACERlab™ FX-N Pro module. ["1"8F]FGln was obtained in 80±3 min with a radiochemical yield of 21±3% (n=5, uncorrected). The radiochemical purity was >98%, and optical purity 90±5%. The synthesis is highly reproducible with good chemical purity, radiochemical yield, and is suitable for translation to cGMP production. - Highlights: • The radiosynthesis of ["1"8F]fluoroglutamine was optimized with improved yield and purity. • Fully automated synthesis was established on a GE TRACERlab™ FX-N Pro module. • Radiochemical yield of 21±3% (uncorrected, n=5) was obtained with good reproducibility. • The automation could be easily adapted to cGMP production for routine clinical use.

  14. Synthesis and characterization of straight and stacked-sheet AlN nanowires with high purity

    International Nuclear Information System (INIS)

    Lei, M.; Yang, H.; Li, P.G.; Tang, W.H.

    2008-01-01

    Large-scale AlN nanowires with hexagonal crystal structure were synthesized by the direct nitridation method at high temperatures. The experimental results indicate that these single-crystalline AlN nanowires have high purity and consist of straight and stacked-sheet nanowires. It is found that straight AlN nanowire grows along [1, 1, -2, 0] direction, whereas the stacked-sheet nanowire with hexagonal cross section is along [0 0 0 1] direction. It is thought that vapor-solid (VS) mechanism should be responsible for the growth of AlN nanowires

  15. Synthesis and quality control of [{sup 18}F] fluorothymidine

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, Leonardo Tafas C.; Silva, Juliana B.; Silveira, Marina B.; Santos, Priscilla F.; Faria, Tiago, E-mail: ltcn@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2013-07-01

    The Positron Emission Tomography (PET) is a technique that allows early diagnosis of various diseases by detecting metabolic changes of cells, in addition to being a noninvasive technique. The most widely used radiopharmaceutical for PET imaging is [{sup 18}F] Fludesoxiglucose ({sup 18}FDG), which is a marker of glucose metabolism and has high sensitivity and specificity for diagnosis and staging of various cancers. However, some carcinomas do not have high glucose consumption, besides {sup 18}FDG possess high urinary excretion rate interfering with the detection of tumors in pelvis and high uptake in brain and in inflammation, reducing the contrast tumor / background. The radiotracer 3'-fluoro-L-3'-deoxythymidine ({sup 18}FLT) is an analogue of thymidine used as an alternative to {sup 18}FDG for detecting tumors with high proliferation rate. The aim of this work was to develop [{sup 18}F] Fluorothymidine synthesis and quality control at the Radiopharmaceuticals Research and Production Facility of CDTN/CNEN. The synthesis was adapted from that used to {sup 18}FDG, based on the methodologies described in related papers. Radiochemical purity and impurities levels were determined by HPLC, RTLC and GC techniques. Total synthesis time was 35 minutes and the radiochemical yield in the end of bombardment (EOB) was 7%, with a radiochemical purity of about 93%. Radionuclidic identity and purity, pH, residual solvents, radiochemical and chemical purity were evaluated according to analytical methods described on the literature and on the United States Pharmacopeia (USP 32). Residual levels of Stavudine, Thymine and Thymidine were found and are under toxicological investigation in order to establish a maximum amount allowed in the final product. (author)

  16. Enhancement of RNA synthesis by promoter duplication in tombusviruses

    International Nuclear Information System (INIS)

    Panavas, T.; Panaviene, Z.; Pogany, J.; Nagy, P.D.

    2003-01-01

    Replication of tombusviruses, small plus-strand RNA viruses of plants, is regulated by cis-acting elements present in the viral RNA. The role of cis-acting elements can be studied in vitro by using a partially purified RNA-dependent RNA polymerase (RdRp) preparation obtained from tombusvirus-infected plants , Virology 276, 279- 288). Here, we demonstrate that the minus-strand RNA of tombusviruses contains, in addition to the 3'-terminal minimal plus-strand initiation promoter, a second cis-acting element, termed the promoter proximal enhancer (PPE). The PPE element enhanced RNA synthesis by almost threefold from the adjacent minimal promoter in the in vitro assay. The sequence of the PPE element is 70% similar to the minimal promoter, suggesting that sequence duplication of the minimal promoter may have been the mechanism leading to the generation of the PPE. Consistent with this proposal, replacement of the PPE element with the minimal promoter, which resulted in a perfectly duplicated promoter region, preserved its enhancer-like function. In contrast, mutagenesis of the PPE element or its replacement with an artificial G/C-rich sequence abolished its stimulative effect on initiation of RNA synthesis in vitro. In vivo experiments are also consistent with the role of the PPE element in enhancement of tombusvirus replication. Sequence comparison of several tombusviruses and related carmoviruses further supports the finding that duplication of minimal promoter sequences may have been an important mechanism during the evolution of cis-acting elements in tombusviruses and related RNA viruses

  17. 10 CFR 36.63 - Pool water purity.

    Science.gov (United States)

    2010-01-01

    ... 10 Energy 1 2010-01-01 2010-01-01 false Pool water purity. 36.63 Section 36.63 Energy NUCLEAR... § 36.63 Pool water purity. (a) Pool water purification system must be run sufficiently to maintain the conductivity of the pool water below 20 microsiemens per centimeter under normal circumstances. If pool water...

  18. In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

    Science.gov (United States)

    Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

    2006-12-01

    We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 3. Bulk samples with 98.5(2)% purity were prepared using low-temperature reduction methods. The preparative methods limited the crystallinity of this new phase to approximately 225(50) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

  19. Engineering high power induction plasma unit at BARC for mass synthesis of refractory nano-ceramics

    International Nuclear Information System (INIS)

    Ghorui, S.; Sahasrabudhe, S.N.; Dhamale, G.; Das, A.K.

    2013-01-01

    Atmospheric pressure RF thermal plasma sources are gaining increasing importance for production of high purity novel nano-materials in different high-end technological applications. Inherent electrode-less features of the discharge together with the large volume and high energy density of the produced plasma ensures contamination free process environment and mass production ability. Reported herewith is the development of an indigenous induction plasma system for mass synthesis of nanopowders of refractory ceramic materials. The system has been tested for continuous synthesis of Al 2 O 3 nano-powder at a rate of more than 600 gm per hour and checked for its viability for bulk production of nano-particles of other refractory ceramics like Yttrium oxide and Neodymium Oxide. From collected evidences, the process of formation of the nano-particles is identified as the evaporation and subsequent homogeneous nucleation. Major features observed for alumina are complete conversion into highly spherical nano-sized particles, small particle sizes, very narrow size distribution, highly crystallite nature and mixed phases depending on the zone of collection. For alumina, the particles are found to exhibit a uni-modal distribution with peak near 15 nm

  20. Epitaxially Grown Layered MFI–Bulk MFI Hybrid Zeolitic Materials

    KAUST Repository

    Kim, Wun-gwi

    2012-11-27

    The synthesis of hybrid zeolitic materials with complex micropore-mesopore structures and morphologies is an expanding area of recent interest for a number of applications. Here we report a new type of hybrid zeolite material, composed of a layered zeolite material grown epitaxially on the surface of a bulk zeolite material. Specifically, layered (2-D) MFI sheets were grown on the surface of bulk MFI crystals of different sizes (300 nm and 10 μm), thereby resulting in a hybrid material containing a unique morphology of interconnected micropores (∼0.55 nm) and mesopores (∼3 nm). The structure and morphology of this material, referred to as a "bulk MFI-layered MFI" (BMLM) material, was elucidated by a combination of XRD, TEM, HRTEM, SEM, TGA, and N2 physisorption techniques. It is conclusively shown that epitaxial growth of the 2-D layered MFI sheets occurs in at least two principal crystallographic directions of the bulk MFI crystal and possibly in the third direction as well. The BMLM material combines the properties of bulk MFI (micropore network and mechanical support) and 2-D layered MFI (large surface roughness, external surface area, and mesoporosity). As an example of the uses of the BMLM material, it was incorporated into a polyimide and fabricated into a composite membrane with enhanced permeability for CO2 and good CO2/CH4 selectivity for gas separations. SEM-EDX imaging and composition analysis showed that the polyimide and the BMLM interpenetrate into each other, thereby forming a well-adhered polymer/particle microstructure, in contrast with the defective interfacial microstructure obtained using bare MFI particles. Analysis of the gas permeation data with the modified Maxwell model also allows the estimation of the effective volume of the BMLM particles, as well as the CO2 and CH4 gas permeabilities of the interpenetrated layer at the BMLM/polyimide interface. © 2012 American Chemical Society.

  1. Bulk synthesis of monodisperse magnetic FeNi3 nanopowders by flow levitation method.

    Science.gov (United States)

    Chen, Shanjun; Chen, Yan; Kang, Xiaoli; Li, Song; Tian, Yonghong; Wu, Weidong; Tang, Yongjian

    2013-10-01

    In this work, a novel bulk synthesis method for monodisperse FeNi3 nanoparticles was developed by flow levitation method (FL). The Fe and Ni vapours ascending from the high temperature levitated droplet was condensed by cryogenic Ar gas under atmospheric pressure. X-ray diffraction was used to identify and characterize the crystal phase of prepared powders exhibiting a FeNi3 phase. The morphology and size of nanopowders were observed by transmission electron microscopy (TEM). The chemical composition of the nanoparticles was determined with energy dispersive spectrometer (EDS). The results indicated that the FeNi3 permalloy powders are nearly spherical-shaped with diameter about 50-200 nm. Measurement of the magnetic property of nanopowders by a superconducting quantum interference device (SQUID, Quantum Design MPMS-7) showed a symmetric hysteresis loop of ferromagnetic behavior with coercivity of 220 Oe and saturation magnetization of 107.17 emu/g, at 293 K. At 5 K, the obtained saturation magnetization of the sample was 102.16 emu/g. The production rate of FeNi3 nanoparticles was estimated to be about 6 g/h. This method has great potential in mass production of FeNi3 nannoparticles.

  2. Synthesis of iodine-123 labelled analogues of imidazenil and ethyl-imidazenil for studying benzodiazepine receptors using SPECT

    International Nuclear Information System (INIS)

    Katsifis, A.; Mattner, F.; Dikic, B.; Najdovski, L.; Kassiou, M.

    1996-01-01

    The [ 123 I]iodinated analogues of the benzodiazepine receptor partial agonist imidazenil and N-ethyl imidazenil have been synthesised for the study of the central benzodiazepine receptor using SPECT. [ 123 I]Iodomidazenil and [ 123 I]N-ethyliodoimidazenil were prepared by nucleophilic bromine-iodine exchange in acetic acid at 150 o . The products were purified by semi-preparative reverse-phase HPLC with average radiochemical yields of 80% in a total synthesis time of 80 minutes. The specific activity was determined to be greater than 2500 Ci/mmol. The radiochemical and chemical purity assessed by radio-TLC and HPLC were found to be 98%. Alternatively, iododestannylation reactions via the trimethyltin precursors with Na[ 123 I] in the presence of Chloramine-T or peracetic acid resulted in yields of only 20-25% with the bulk of activity being lost as volatile methyl [ 123 I]iodide. (author)

  3. Properties of structural steels melted out of high-purity charge

    International Nuclear Information System (INIS)

    Marchenko, V.N.; Sergeeva, T.K.; Kondakova, N.K.; Morozov, V.P.; Madorskij, L.L.

    1993-01-01

    A comparative evaluation has been made of impurities, mechanical properties and hydrogen embirittlement parameters for steels type 40Kh and 40KhS produced by electrometallurgical method with the use of direct reduced charge (DR-steels) and melted in an open-hearth furnace. Investigation results have shown that 40Kh and 40KhS Dr-steels have more coarse austenitic grains and experience more complete transformation of martensite into ferritic-pearlitic mixture on tempering. Threshold stresses increase 2.5 times due to purity enhancement at the expense of application of direct reduced charge

  4. Helium gas purity monitor based on low frequency acoustic resonance

    Science.gov (United States)

    Kasthurirengan, S.; Jacob, S.; Karunanithi, R.; Karthikeyan, A.

    1996-05-01

    Monitoring gas purity is an important aspect of gas recovery stations where air is usually one of the major impurities. Purity monitors of Katherometric type are commercially available for this purpose. Alternatively, we discuss here a helium gas purity monitor based on acoustic resonance of a cavity at audio frequencies. It measures the purity by monitoring the resonant frequency of a cylindrical cavity filled with the gas under test and excited by conventional telephone transducers fixed at the ends. The use of the latter simplifies the design considerably. The paper discusses the details of the resonant cavity and the electronic circuit along with temperature compensation. The unit has been calibrated with helium gas of known purities. The unit has a response time of the order of 10 minutes and measures the gas purity to an accuracy of 0.02%. The unit has been installed in our helium recovery system and is found to perform satisfactorily.

  5. Batch extractive distillation for high purity methanol

    International Nuclear Information System (INIS)

    Zhang Weijiang; Ma Sisi

    2006-01-01

    In this paper, the application in chemical industry and microelectronic industry, market status and the present situation of production of high purity methanol at home and abroad were introduced firstly. Purification of industrial methanol for high purity methanol is feasible in china. Batch extractive distillation is the best separation technique for purification of industrial methanol. Dimethyl sulfoxide was better as an extractant. (authors)

  6. Cryogenic milling for the fabrication of high J{sub c} MgB{sub 2} bulk superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Kim, D. N.; Kang, M. O.; Park, H. W. [Korea University of Technology and Education, Cheonan (Korea, Republic of); Jun, B. H.; Kim, C. J. [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2017-06-15

    Cryogenic milling which is a combined process of low-temperature treatment and mechanical milling was applied to fabricate high critical current density (J{sub c}) MgB{sub 2} bulk superconductors. Liquid nitrogen was used as a coolant, and no solvent or lubricant was used. Spherical Mg (6-12 μm, 99.9 % purity) and plate-like B powder (⁓ 1 μm, 97 % purity) were milled simultaneously for various time periods (0, 2, 4, 6 h) at a rotating speed of 500 rpm using ZrO{sub 2} balls. The (Mg{sup +2B}) powders milled were pressed into pellets and heat-treated at 700°C for 1 h in flowing argon. The use of cryomilled powders as raw materials promoted the formation reaction of superconducting MgB{sub 2}, reduced the grain size of MgB{sub 2}, and suppressed the formation of impurity MgO. The superconducting critical temperature (T{sub c}) of MgB{sub 2} was not influenced as the milling time (t) increased up to 6 h. Meanwhile, the critical current density (J{sub c}) of MgB{sub 2} increased significantly when t increased to 4 h. When t increased further to 6 h, however, Jc decreased. The J{sub c} enhancement of MgB{sub 2} by cryogenic milling is attributed to the formation of the fine grain MgB{sub 2} and a suppression of the MgO formation.

  7. Approaches to the accurate characterization of high purity metal fluorides and fluoride glasses

    Science.gov (United States)

    Beary, E. S.; Paulsen, P. J.; Rains, T. C.; Ewing, K. J.; Jaganathan, J.; Aggarwal, I.

    1990-11-01

    The analytical challenges posed by the measurement of trace contaminants in high purity metal fluorides require that innovative chemical preparation procedures be used to enhance existing instrumental techniques. The instrumental techniques used to analyze these difficult matrices must be sensitive enough to detect extremely low levels of trace impurities, and the background interferences derived from the matrix (metal fluoride or glass) must be minimized. A survey of analytical techniques that have the necessary characteristics to analyze these materials will be given. In addition, means of controlling the chemical blank will be presented. Mass and atomic spectrometric techniques will be discussed, specifically graphite furnace atomic absorption spectrometry (GFAAS) and inductively coupled plasma-mass spectrometry (ICP-MS). Analytical procedures using GFAAS and ICP-MS have been developed to determine sub ppb (part per billion) levels of contaminants in high purity fluoride materials.

  8. Uncertainty estimates of purity measurements based on current information: toward a "live validation" of purity methods.

    Science.gov (United States)

    Apostol, Izydor; Kelner, Drew; Jiang, Xinzhao Grace; Huang, Gang; Wypych, Jette; Zhang, Xin; Gastwirt, Jessica; Chen, Kenneth; Fodor, Szilan; Hapuarachchi, Suminda; Meriage, Dave; Ye, Frank; Poppe, Leszek; Szpankowski, Wojciech

    2012-12-01

    To predict precision and other performance characteristics of chromatographic purity methods, which represent the most widely used form of analysis in the biopharmaceutical industry. We have conducted a comprehensive survey of purity methods, and show that all performance characteristics fall within narrow measurement ranges. This observation was used to develop a model called Uncertainty Based on Current Information (UBCI), which expresses these performance characteristics as a function of the signal and noise levels, hardware specifications, and software settings. We applied the UCBI model to assess the uncertainty of purity measurements, and compared the results to those from conventional qualification. We demonstrated that the UBCI model is suitable to dynamically assess method performance characteristics, based on information extracted from individual chromatograms. The model provides an opportunity for streamlining qualification and validation studies by implementing a "live validation" of test results utilizing UBCI as a concurrent assessment of measurement uncertainty. Therefore, UBCI can potentially mitigate the challenges associated with laborious conventional method validation and facilitates the introduction of more advanced analytical technologies during the method lifecycle.

  9. The synthesis of [14C] C I pigment violet 19

    International Nuclear Information System (INIS)

    Filer, C.N.; Kelly, T.P.

    1990-01-01

    For the custom synthesis of radiolabeled compounds in the authors laboratory, aside from spectroscopic examination, their identity and radiochemical purity is routinely corroborated by demonstration of cochromatography with an authentic cold standard. In the synthesis of [ 14 C] red pigment 1 for the Cosmetic Toiletry and Fragrance Association, its insolubility precluded this. The preparation as well as characterization of 1 is described

  10. Bulk viscosity of spin-one color superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Sa' d, Basil A.

    2009-08-27

    The bulk viscosity of several quark matter phases is calculated. It is found that the effect of color superconductivity is not trivial, it may suppress, or enhance the bulk viscosity depending on the critical temperature and the temperature at which the bulk viscosity is calculated. Also, is it found that the effect of neutrino-emitting Urca processes cannot be neglected in the consideration of the bulk viscosity of strange quark matter. The results for the bulk viscosity of strange quark matter are used to calculate the r-mode instability window of quark stars with several possible phases. It is shown that each possible phase has a different structure for the r-mode instability window. (orig.)

  11. Bulk viscosity of spin-one color superconductors

    International Nuclear Information System (INIS)

    Sa'd, Basil A.

    2009-01-01

    The bulk viscosity of several quark matter phases is calculated. It is found that the effect of color superconductivity is not trivial, it may suppress, or enhance the bulk viscosity depending on the critical temperature and the temperature at which the bulk viscosity is calculated. Also, is it found that the effect of neutrino-emitting Urca processes cannot be neglected in the consideration of the bulk viscosity of strange quark matter. The results for the bulk viscosity of strange quark matter are used to calculate the r-mode instability window of quark stars with several possible phases. It is shown that each possible phase has a different structure for the r-mode instability window. (orig.)

  12. Tuning structural motifs and alloying of bulk immiscible Mo-Cu bimetallic nanoparticles by gas-phase synthesis

    Science.gov (United States)

    Krishnan, Gopi; Verheijen, Marcel A.; Ten Brink, Gert H.; Palasantzas, George; Kooi, Bart J.

    2013-05-01

    Nowadays bimetallic nanoparticles (NPs) have emerged as key materials for important modern applications in nanoplasmonics, catalysis, biodiagnostics, and nanomagnetics. Consequently the control of bimetallic structural motifs with specific shapes provides increasing functionality and selectivity for related applications. However, producing bimetallic NPs with well controlled structural motifs still remains a formidable challenge. Hence, we present here a general methodology for gas phase synthesis of bimetallic NPs with distinctively different structural motifs ranging at a single particle level from a fully mixed alloy to core-shell, to onion (multi-shell), and finally to a Janus/dumbbell, with the same overall particle composition. These concepts are illustrated for Mo-Cu NPs, where the precise control of the bimetallic NPs with various degrees of chemical ordering, including different shapes from spherical to cube, is achieved by tailoring the energy and thermal environment that the NPs experience during their production. The initial state of NP growth, either in the liquid or in the solid state phase, has important implications for the different structural motifs and shapes of synthesized NPs. Finally we demonstrate that we are able to tune the alloying regime, for the otherwise bulk immiscible Mo-Cu, by achieving an increase of the critical size, below which alloying occurs, closely up to an order of magnitude. It is discovered that the critical size of the NP alloy is not only affected by controlled tuning of the alloying temperature but also by the particle shape.Nowadays bimetallic nanoparticles (NPs) have emerged as key materials for important modern applications in nanoplasmonics, catalysis, biodiagnostics, and nanomagnetics. Consequently the control of bimetallic structural motifs with specific shapes provides increasing functionality and selectivity for related applications. However, producing bimetallic NPs with well controlled structural motifs still

  13. High-purity germanium crystal growing

    International Nuclear Information System (INIS)

    Hansen, W.L.; Haller, E.E.

    1982-10-01

    The germanium crystals used for the fabrication of nuclear radiation detectors are required to have a purity and crystalline perfection which is unsurpassed by any other solid material. These crystals should not have a net electrically active impurity concentration greater than 10 10 cm - 3 and be essentially free of charge trapping defects. Such perfect crystals of germanium can be grown only because of the highly favorable chemical and physical properties of this element. However, ten years of laboratory scale and commercial experience has still not made the production of such crystals routine. The origin and control of many impurities and electrically active defect complexes is now fairly well understood but regular production is often interrupted for long periods due to the difficulty of achieving the required high purity or to charge trapping in detectors made from crystals seemingly grown under the required conditions. The compromises involved in the selection of zone refining and crystal grower parts and ambients is discussed and the difficulty in controlling the purity of key elements in the process is emphasized. The consequences of growing in a hydrogen ambient are discussed in detail and it is shown how complexes of neutral defects produce electrically active centers

  14. Purity of antidotal oxime HI-6 DMS as an active pharmaceutical ingredient for auto-injectors and infusions.

    Science.gov (United States)

    Bogan, Reinhard; Koller, Marianne; Klaubert, Bernd

    2012-01-01

    As reactivators of inhibited acetylcholinesterase, oximes are essential antidotes in poisoning by organophosphorus compounds. Due to its superior efficacy in cases of soman, cyclosarin, and sarin poisoning, the oxime HI-6 represents a promising option for an active pharmaceutical ingredient (API) in the further development of antidote therapy for nerve agent poisoning. Developmental lots of HI-6 DMS (dimethanesulfonate) provided by different manufacturers were examined with respect to their content and purity with a view to their future use as an API. There are distinct differences in the HI-6 content from three manufacturers. With respect to purity, gradual differences arise with the known synthetic by-products as well as with unknown accompanying compounds. It became apparent that in the case of a modified synthesis using protective groups, the proportion of some synthesis by-products decreases considerably. With one exception, they are thus below the reporting threshold for API in accordance with pertinent regulatory guidelines. In HI-6, an unknown impurity always occurs, whose percentage necessitates identification due to regulations. This unknown impurity, which has not been described so far, could be identified as an isomer. These findings supply data required for the description of pharmaceutical quality in accordance with module 3 of a Common Technical Document (CTD). They thus contribute to the marketing authorization of this substance as an API for auto-injectors and infusions. Copyright © 2012 John Wiley & Sons, Ltd.

  15. Radiochemical purity of Mo and Tc solution obtained after irradiation and dissolution of Mo-100-enriched and ultra-high-purity natural Mo disks

    Energy Technology Data Exchange (ETDEWEB)

    Tkac, Peter [Argonne National Lab. (ANL), Argonne, IL (United States); Gromov, Roman [Argonne National Lab. (ANL), Argonne, IL (United States); Chemerisov, Sergey D. [Argonne National Lab. (ANL), Argonne, IL (United States); Rotsch, David A. [Argonne National Lab. (ANL), Argonne, IL (United States); Vandegrift, George F. [Argonne National Lab. (ANL), Argonne, IL (United States)

    2016-09-01

    Four irradiations of ultra-high-purity natural Mo targets and one irradiation using 97.4% Mo-100-enriched material were performed. The purpose of these irradiations was to determine whether the presence of Sn stabilizer in the H2O2 used for the dissolution of sintered Mo disks can affect the radiochemical purity of the final K2MoO4 in 5M KOH solution. Results from radiochemical purity tests performed using thin-layer paper chromatography show that even 2– 3× excess of Sn-stabilized H2O2 typically used for dissolution of sintered Mo disks did not affect the radiochemical purity of the final product.

  16. Synthesis and magnetic properties of bulk transparent PMMA/Fe-oxide nanocomposites

    Science.gov (United States)

    Li, Shanghua; Qin, Jian; Fornara, Andrea; Toprak, Muhammet; Muhammed, Mamoun; Kim, Do Kyung

    2009-05-01

    PMMA/Fe-oxide nanocomposites are fabricated by a chemical method. Monodispersed Fe-oxide nanoparticles are well dispersed in the PMMA matrix by in situ polymerization, resulting in a bulk transparent polymeric nanocomposite. The magnetic behavior of the PMMA/Fe-oxide nanocomposites is investigated. The transparent PMMA/Fe-oxide nanocomposite has potentially interesting magneto-optic applications without compromising the advantages of a lightweight, noncorrosive polymeric material with very high transparency even for bulk samples.

  17. Synthesis and magnetic properties of bulk transparent PMMA/Fe-oxide nanocomposites

    International Nuclear Information System (INIS)

    Li Shanghua; Qin Jian; Fornara, Andrea; Toprak, Muhammet; Muhammed, Mamoun; Kim, Do Kyung

    2009-01-01

    PMMA/Fe-oxide nanocomposites are fabricated by a chemical method. Monodispersed Fe-oxide nanoparticles are well dispersed in the PMMA matrix by in situ polymerization, resulting in a bulk transparent polymeric nanocomposite. The magnetic behavior of the PMMA/Fe-oxide nanocomposites is investigated. The transparent PMMA/Fe-oxide nanocomposite has potentially interesting magneto-optic applications without compromising the advantages of a lightweight, noncorrosive polymeric material with very high transparency even for bulk samples.

  18. Mixed Domains Enhance Charge Generation and Extraction in Bulk-Heterojunction Solar Cells with Small-Molecule Donors

    KAUST Repository

    Alqahtani, Obaid; Babics, Maxime; Gorenflot, Julien; Savikhin, Victoria; Ferron, Thomas; Balawi, Ahmed H.; Paulke, Andreas; Kan, Zhipeng; Pope, Michael; Clulow, Andrew J.; Wolf, Jannic Sebastian; Burn, Paul L.; Gentle, Ian R.; Neher, Dieter; Toney, Michael F.; Laquai, Fré dé ric; Beaujuge, Pierre; Collins, Brian A.

    2018-01-01

    The interplay between nanomorphology and efficiency of polymer-fullerene bulk-heterojunction (BHJ) solar cells has been the subject of intense research, but the generality of these concepts for small-molecule (SM) BHJs remains unclear. Here, the relation between performance; charge generation, recombination, and extraction dynamics; and nanomorphology achievable with two SM donors benzo[1,2-b:4,5-b]dithiophene-pyrido[3,4-b]-pyrazine BDT(PPTh), namely SM1 and SM2, differing by their side-chains, are examined as a function of solution additive composition. The results show that the additive 1,8-diiodooctane acts as a plasticizer in the blends, increases domain size, and promotes ordering/crystallinity. Surprisingly, the system with high domain purity (SM1) exhibits both poor exciton harvesting and severe charge trapping, alleviated only slightly with increased crystallinity. In contrast, the system consisting of mixed domains and lower crystallinity (SM2) shows both excellent exciton harvesting and low charge recombination losses. Importantly, the onset of large, pure crystallites in the latter (SM2) system reduces efficiency, pointing to possible differences in the ideal morphologies for SM-based BHJ solar cells compared with polymer-fullerene devices. In polymer-based systems, tie chains between pure polymer crystals establish a continuous charge transport network, whereas SM-based active layers may in some cases require mixed domains that enable both aggregation and charge percolation to the electrodes.

  19. Mixed Domains Enhance Charge Generation and Extraction in Bulk-Heterojunction Solar Cells with Small-Molecule Donors

    KAUST Repository

    Alqahtani, Obaid

    2018-03-25

    The interplay between nanomorphology and efficiency of polymer-fullerene bulk-heterojunction (BHJ) solar cells has been the subject of intense research, but the generality of these concepts for small-molecule (SM) BHJs remains unclear. Here, the relation between performance; charge generation, recombination, and extraction dynamics; and nanomorphology achievable with two SM donors benzo[1,2-b:4,5-b]dithiophene-pyrido[3,4-b]-pyrazine BDT(PPTh), namely SM1 and SM2, differing by their side-chains, are examined as a function of solution additive composition. The results show that the additive 1,8-diiodooctane acts as a plasticizer in the blends, increases domain size, and promotes ordering/crystallinity. Surprisingly, the system with high domain purity (SM1) exhibits both poor exciton harvesting and severe charge trapping, alleviated only slightly with increased crystallinity. In contrast, the system consisting of mixed domains and lower crystallinity (SM2) shows both excellent exciton harvesting and low charge recombination losses. Importantly, the onset of large, pure crystallites in the latter (SM2) system reduces efficiency, pointing to possible differences in the ideal morphologies for SM-based BHJ solar cells compared with polymer-fullerene devices. In polymer-based systems, tie chains between pure polymer crystals establish a continuous charge transport network, whereas SM-based active layers may in some cases require mixed domains that enable both aggregation and charge percolation to the electrodes.

  20. Enhancing transparency in reporting the synthesis of qualitative research: ENTREQ

    Science.gov (United States)

    2012-01-01

    Background The syntheses of multiple qualitative studies can pull together data across different contexts, generate new theoretical or conceptual models, identify research gaps, and provide evidence for the development, implementation and evaluation of health interventions. This study aims to develop a framework for reporting the synthesis of qualitative health research. Methods We conducted a comprehensive search for guidance and reviews relevant to the synthesis of qualitative research, methodology papers, and published syntheses of qualitative health research in MEDLINE, Embase, CINAHL and relevant organisational websites to May 2011. Initial items were generated inductively from guides to synthesizing qualitative health research. The preliminary checklist was piloted against forty published syntheses of qualitative research, purposively selected to capture a range of year of publication, methods and methodologies, and health topics. We removed items that were duplicated, impractical to assess, and rephrased items for clarity. Results The Enhancing transparency in reporting the synthesis of qualitative research (ENTREQ) statement consists of 21 items grouped into five main domains: introduction, methods and methodology, literature search and selection, appraisal, and synthesis of findings. Conclusions The ENTREQ statement can help researchers to report the stages most commonly associated with the synthesis of qualitative health research: searching and selecting qualitative research, quality appraisal, and methods for synthesising qualitative findings. The synthesis of qualitative research is an expanding and evolving methodological area and we would value feedback from all stakeholders for the continued development and extension of the ENTREQ statement. PMID:23185978

  1. Determination of continuous variable entanglement by purity measurements.

    Science.gov (United States)

    Adesso, Gerardo; Serafini, Alessio; Illuminati, Fabrizio

    2004-02-27

    We classify the entanglement of two-mode Gaussian states according to their degree of total and partial mixedness. We derive exact bounds that determine maximally and minimally entangled states for fixed global and marginal purities. This characterization allows for an experimentally reliable estimate of continuous variable entanglement based on measurements of purity.

  2. Steam purity in PWRs

    International Nuclear Information System (INIS)

    Hopkinson, J.; Passell, T.

    1982-01-01

    Reports that 2 EPRI studies of PWRs prove that impure steam triggers decay of turbine metals. Reveals that EPRI is attempting to improve steam monitoring and analysis, which are key steps on the way to deciding the most cost-effective degree of steam purity, and to upgrade demineralizing systems, which can then reliably maintain that degree of purity. Points out that 90% of all cracks in turbine disks have occurred at the dry-to-wet transition zone, dubbed the Wilson line. Explains that because even very clean water contains traces of chemical impurities with concentrations in the parts-per-billion range, Crystal River-3's secondary loop was designed with even more purification capability; a deaerator to remove oxygen and prevent oxidation of system metals, and full-flow resin beds to demineralize 100% of the secondary-loop water from the condenser. Concludes that focusing attention on steam and water chemistry can ward off cracking and sludge problems caused by corrosion

  3. High-Purity Glasses Based on Arsenic Chalcogenides

    Science.gov (United States)

    2001-06-01

    Chemical interaction of chalcogenides and some impurities (CS 2, TeO2 ) with the quartz glass at high temperature leads to the thin layers formation...UNCLASSIFIED Defense Technical Information Center Compilation Part Notice ADPO1 1523 TITLE: High-Purity Glasses Based on Arsenic Chalcogenides...Materials Vol. 3, No. 2, June 2001, p. 341 - 349 HIGH-PURITY GLASSES BASED ON ARSENIC CHALCOGENIDES M. F. Churbanov, I. V. Scripachev, G. E. Snopatin, V. S

  4. Metabolic approaches to enhance transdermal drug delivery. 1. Effect of lipid synthesis inhibitors.

    Science.gov (United States)

    Tsai, J C; Guy, R H; Thornfeldt, C R; Gao, W N; Feingold, K R; Elias, P M

    1996-06-01

    The intercellular domains of the stratum corneum, which contain a mixture of cholesterol, free fatty acids, and ceramides, mediate both the epidermal permeability barrier and the transdermal delivery of both lipophilic and hydrophilic molecules. Prior studies have shown that each of the three key lipid classes is required for normal barrier function. For example, selective inhibition of either cholesterol, fatty acid, or ceramide synthesis in the epidermis delays barrier recovery rates after barrier perturbation of hairless mouse skin in vivo. In this study, we investigated the potential of certain inhibitors of lipid synthesis to enhance the transdermal delivery of lidocaine or caffeine as a result of their capacity to perturb barrier homeostasis. After acetone disruption of the barrier, the extent of lidocaine delivery and the degree of altered barrier function paralleled each other. Moreover, the further alteration in barrier function produced by either the fatty acid synthesis inhibitor 5-(tetradecyloxy)-2-furancarboxylic acid (TOFA), the cholesterol synthesis inhibitor fluvastatin (FLU), or cholesterol sulfate (CS) resulted in a further increase in lidocaine absorption. Furthermore, coapplications of TOFA and CS together caused an additive increase in lidocaine uptake. Finally, a comparable increase in drug delivery occurred when the barrier was disrupted initially with DMSO instead of acetone; coapplications of TOFA and FLU together again delayed barrier recovery and increased drug delivery by about 8-fold vs delivery from a standard enhancing vehicle. Whereas these metabolic inhibitors also variably increased the octanol/water partitioning of the drugs studied (perhaps via complexion or pH alterations), physicochemical effects of the inhibitors alone did not alter drug uptake in intact skin; i.e., passive mechanisms alone cannot account for the net increase in drug delivery. Our results show that modulations of epidermal lipid biosynthesis, following

  5. An Improved, Highly Efficient Method for the Synthesis of Bisphenols

    Directory of Open Access Journals (Sweden)

    L. S. Patil

    2011-01-01

    Full Text Available An efficient synthesis of bisphenols is described by condensation of substituted phenols with corresponding cyclic ketones in presence of cetyltrimethylammonium chloride and 3-mercaptopropionic acid as a catalyst in extremely high purity and yields.

  6. Bulk Synthesis and Characterization of Ti3Al Nanoparticles by Flow-Levitation Method

    Directory of Open Access Journals (Sweden)

    Shanjun Chen

    2013-01-01

    Full Text Available A novel bulk synthesis method for preparing high pure Ti3Al nanoparticles was developed by flow-levitation method (FL. The Ti and Al vapours ascending from the high temperature levitated droplet were condensed by cryogenic Ar gas under atmospheric pressure. The morphology, crystalline structure, and chemical composition of Ti3Al nanoparticles were, respectively, investigated by transmission electron microscopy, X-ray diffraction, and inductively coupled plasma atomic emission spectrometry. The results indicated that the Ti3Al powders are nearly spherical-shaped, and the particle size ranges from several nanometers to 100 nm in diameter. Measurements of the d-spacing from X-ray (XRD and electron diffraction studies confirmed that the Ti3Al nanoparticles have a hexagonal structure. A thin oxidation coating of 2-3 nm in thickness was formed around the particles after exposure to air. Based on the XPS measurements, the surface coating of the Ti3Al nanoparticles is a mixture of Al2O3 and TiO2. The production rate of Ti3Al nanoparticles was estimated to be about 3 g/h. This method has a great potential in mass production of Ti3Al nanoparticles.

  7. Enhanced magnetodielectric and multiferroic properties of Er-doped bismuth ferrite nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Mukherjee, A.; Banerjee, M. [Department of Physics, National Institute of Technology, Durgapur 713209 (India); Basu, S., E-mail: soumen.basu@phy.nitdgp.ac.in [Department of Physics, National Institute of Technology, Durgapur 713209 (India); Mukadam, M.D.; Yusuf, S.M. [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Pal, M. [CSIR-Central Glass & Ceramic Research Institute, Kolkata 700032 (India)

    2015-07-15

    An enhancement in multiferroic properties has been achieved for chemically prepared BFO nanoparticles by doping with erbium (Er). XRD along with electron microscopy study reveals the phase purity and nanocrystalline nature of BFO. Enhancement of both the magnetic moment and resistivity is observed by virtue of Er doping. The observed enhanced magnetic moment is considered to be associated with smaller crystallite whereas increase of resistivity may be attributed to a decrease of oxygen vacancies. Doping also display an improvement of leakage behaviour and dielectric constant in nanocrystalline BFO, reflected in well-developed P-E loop. In addition, large enhancement in magnetodielectric coefficient is observed because of Er doping. Therefore, the results provide interesting approaches to improve the multiferroic properties of BFO, which has great implication towards its applications. - Highlights: • Synthesis of pure Er-doped BFO nanoparticles by chemical route. • Large increase in magnetic moment and resistivity due to Er doping. • Er doping produce well developed P-E loop and enhance polarization. • Drastic increase in dielectric constant as well as magnetodielectric coefficient observes because of Er doping.

  8. Synthesis of (R)-(+)-3H-etomidate

    International Nuclear Information System (INIS)

    Janssen, C.G.M.; Thijssen, J.B.A.; Verluyten, W.L.M.; Heykants, J.J.P.

    1987-01-01

    Etomidate, (R)-(+)-ethyl-1-(1-phenylethyl)-1H-imidazole-5-carboxylate, is a short-acting hypnotic. A new synthesis, featuring optical resolution on a non-radioactive precursor and introduction of the tritium label by reductive dehalogenation, is described. The title compound was obtained at a specific activity of 3.77 Ci/mmol and a 99.9% HPLC purity. (author)

  9. Zero- and two-dimensional hybrid carbon phosphors for high colorimetric purity white light-emission.

    Science.gov (United States)

    Ding, Yamei; Chang, Qing; Xiu, Fei; Chen, Yingying; Liu, Zhengdong; Ban, Chaoyi; Cheng, Shuai; Liu, Juqing; Huang, Wei

    2018-03-01

    Carbon nanomaterials are promising phosphors for white light emission. A facile single-step synthesis method has been developed to prepare zero- and two-dimensional hybrid carbon phosphors for the first time. Zero-dimensional carbon dots (C-dots) emit bright blue luminescence under 365 nm UV light and two-dimensional nanoplates improve the dispersity and film forming ability of C-dots. As a proof-of-concept application, the as-prepared hybrid carbon phosphors emit bright white luminescence in the solid state, and the phosphor-coated blue LEDs exhibit high colorimetric purity white light-emission with a color coordinate of (0.3308, 0.3312), potentially enabling the successful application of white emitting phosphors in the LED field.

  10. Synthesis and labeling 5'-O-(4-4'-dimetoxytrityl) -2,3-anhidrothymidine for preparation of radiopharmaceutical [18F]FLT

    International Nuclear Information System (INIS)

    Purwoko; Maskur; Chaeruman; Sugiarto, Yono

    2013-01-01

    It is has been known that the compound of 3'-deoxy-3,-( 18 F] Fluorothymidine or ( 18 F] FLT is a thymidine derivative radiopharmaceutical used for cancer detection based on DNA metabolism. Synthesis and labeling of 5'-0-(4,4 '-dimetoxytrityl) -2,3' anhidrothymidine precursor for preparation of the radiopharmaceutical [ 18 F]FL T was carried out. The precursor was synthesized in similar manner and procedure literature and it have been obtained a crystalline product with total yield of 32,4 %. The chemical purity of the product which determined by HPLC was found to be more than 95%. Characterization of the product was done by observing the results of the LC / MS and 1 H-NMR test, the resulted data were found to be very closed to those reported in the literature. Labeling of the precursor was done by nucleophilic fluorination reactions using 18 Fluoride at 160 °C for 15 minutes with kryptofix 2.2.2 catalyst followed hydrolysis using HCI at 100 °C for 10 minutes and then neutralized with NaOH. Purification [ 18 F]FLT was performed by single cartridge Alumina-N as a substitute HPLC methods. The results have been obtained a label compound [ 18 F]FLT with high purity as a bulk for preparation of the radiopharmaceutical [ 18 F]FLT. The label compound of [ 18 F]FLT undergone a quality test which included a clarity, pH and a radiochemical purity. The results of quality control on four batches of [ 18 F]FLT showed that these products were colorless clear solution with pH between 6.0-7.5, and radiochemical purity 97.93 ± 1,48% and showed that the label compounds have been obtained [ 18 F]FLT-free particles form a clear solution with a pH between 6,0 - 7,5, radiochemical purity of 97.93 ± 1,48 %, radiochemical yields 8.18 ± 1.54% (decay uncorrected) and processing time 73 ± 4 minutes. (author)

  11. Synthesis of an allergy inducing tetrasaccharide "4P-X".

    Science.gov (United States)

    Moriya, Takashi; Nagahata, Naoki; Odaka, Rei; Nakamura, Hirohide; Yoshikawa, Jun; Kurashima, Katsumi; Saito, Tadao

    2017-02-01

    4P-X (β-D-galactopyranosyl-(1 → 4)-β-D-galactopyranosyl-(1 → 6)-[β-D-galactopyranosyl-(1 → 4)]-β-D-glucopyranose) is included in galacto-oligosaccharides (GOSs) produced by β-galactosidase derived from Bacillus circulans. 4P-X has been known to induce particularly strong allergies. High purity 4P-X is essential for use as a standard to quantify the amount of 4P-X in GOSs; however, the isolation of high purity 4P-X has never been reported. In this study, we achieved the synthesis of 4P-X by a combination of organic and enzymatic chemical syntheses in a short time. This is the first report of isolated, high purity 4P-X. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Preparation of High Purity CdTe for Nuclear Detector: Electrical and Nuclear Characterization

    Science.gov (United States)

    Zaiour, A.; Ayoub, M.; Hamié, A.; Fawaz, A.; Hage-ali, M.

    High purity crystal with controllable electrical properties, however, control of the electrical properties of CdTe has not yet been fully achieved. Using the refined Cd and Te as starting materials, extremely high-purity CdTe single crystals were prepared by the traditional vertical THM. The nature of the defects involved in the transitions was studied by analyzing the position of the energy levels by TSC method. The resolution of 4.2 keV (FWHM) confirms the high quality and stability of the detectors: TSC spectrum was in coherence with detectors spectrum with a horizontal plate between 0.2 and 0.6 eV. The enhancement in resolution of detectors with a full width at half- maximum (less than 0.31 meV), lead to confirm that the combination of vacuum distillation and zone refining was very effective to obtain more purified CdTe single crystals for photovoltaic or nuclear detectors with better physical properties.

  13. Preparation of high-purity cerium nitrate

    International Nuclear Information System (INIS)

    Avila, Daniela Moraes; Silva Queiroz, Carlos Alberto da; Santos Mucillo, Eliana Navarro dos

    1995-01-01

    The preparation of high-purity cerium nitrate has been carried out Cerium oxide has been prepared by fractioned precipitation and ionic exchange techniques, using a concentrate with approximately 85% of cerium oxide from NUCLEMON as raw material. Five sequential ion-exchange columns with a retention capacity of 170 g each have been used. The ethylenediamine-tetraacetic acid (EDTA) was used as eluent. The cerium content has been determined by gravimetry and iodometry techniques. The resulting cerium oxide has a purity > 99%. This material was transformed in cerium nitrate to be used as precursor for the preparation of Zirconia-ceria ceramics by the coprecipitation technique. (author)

  14. Bulk synthesis of nanocrystalline urania powders by citrate gel-combustion method

    International Nuclear Information System (INIS)

    Sanjay Kumar, D.; Ananthasivan, K.; Venkata Krishnan, R.; Amirthapandian, S.; Dasgupta, Arup

    2016-01-01

    Bulk quantities (60 g) of nanocrystalline (nc) free flowing urania powders with crystallite size ranging from 38 to 252 nm have been synthesized for the first time by the citrate gel combustion method. A systematic study of the influence of the fuel (citric acid) to oxidant (nitrate) ratio (R) on the characteristics of the urania powders has been carried out for the first time. Mixture with an “R” value of 0.25 exhibited a vigorous auto-ignition reaction. This reaction was investigated with Differential Scanning Calorimetry (DSC) and in-situ thermogravimetry coupled with differential thermal analysis and mass spectrometry (TG-DTA-MS). The bulk density, specific surface area, X-ray crystallite size, residual carbon and size distribution of particles of this powder were unique. Microscopic and microstructural investigation of selected samples revealed the presence of nanocrystals with irregular exfoliated morphology; their Electron Energy Loss Spectra testified the covalency of the U–O bond. - Highlights: • Bulk quantities of nanocrystalline urania were prepared for the first time using citrate gel combustion method. • Volume combustion was observed in mixtures with fuel to nitrate ratio (R) 0.25. • The value of R was found to significantly influence the characteristics of the final product. • Typical exfoliated microstructure and nanopores were observed. • Established correlation between particle size distribution and bulk density, X-ray crystallite size and lattice strain. • Relationship between fuel to nitrate (R) mole ratio and physical characteristics of powders were also established.

  15. Synthesis of specific labelled [methyl-14C]sarin

    International Nuclear Information System (INIS)

    Sin-Ren, A.C.; Riggio, G.; Hopff, W.H.; Waser, P.G.

    1988-01-01

    The synthesis of [methyl- 14 C]sarin ([ 14 C]methylphosphono-fluoridic acid 1-methylethyl ester) was accomplished by another approach as for nonlabelled sarin in a tele-conducted reaction vessel. The purity was estimated by IR, GC, and GC-MS and the stability in different media was examined. (author)

  16. Green Tea Polyphenol Epigallocatechin-3-Gallate Enhance Glycogen Synthesis and Inhibit Lipogenesis in Hepatocytes

    Directory of Open Access Journals (Sweden)

    Jane J. Y. Kim

    2013-01-01

    Full Text Available The beneficial effects of green tea polyphenols (GTP against metabolic syndrome and type 2 diabetes by suppressing appetite and nutrient absorption have been well reported. However the direct effects and mechanisms of GTP on glucose and lipid metabolism remain to be elucidated. Since the liver is an important organ involved in glucose and lipid metabolism, we examined the effects and mechanisms of GTP on glycogen synthesis and lipogenesis in HepG2 cells. Concentrations of GTP containing 68% naturally occurring (−-epigallocatechin-3-gallate (EGCG were incubated in HepG2 cells with high glucose (30 mM under 100 nM of insulin stimulation for 24 h. GTP enhanced glycogen synthesis in a dose-dependent manner. 10 μM of EGCG significantly increased glycogen synthesis by 2fold (P<0.05 compared with insulin alone. Western blotting revealed that phosphorylation of Ser9 glycogen synthase kinase 3β and Ser641 glycogen synthase was significantly increased in GTP-treated HepG2 cells compared with nontreated cells. 10 μM of EGCG also significantly inhibited lipogenesis (P<0.01. We further demonstrated that this mechanism involves enhanced expression of phosphorylated AMP-activated protein kinase α and acetyl-CoA carboxylase in HepG2 cells. Our results showed that GTP is capable of enhancing insulin-mediated glucose and lipid metabolism by regulating enzymes involved in glycogen synthesis and lipogenesis.

  17. Plasmon enhanced power conversion efficiency in inverted bulk heterojunction organic solar cell

    Science.gov (United States)

    Mohan, Minu; Ramkumar, S.; Namboothiry, Manoj A. G.

    2017-08-01

    P3HT:PCBM is one of the most studied polymer-fullerene system. However the reported power conversion efficiency (PCE) values falls within the range of 4% to 5%. The thin film architecture in OPVs exhibits low PCE compared to inorganic photovoltaic cells. This is mainly due to the low exciton diffusion length that limits the active layer thickness which in turn reduces the absorption of incident light. Several strategies are adapted in order to increase the absorption in the active layer without increasing the film thickness. Inclusion of metal nanoparticles into the polymer layer of bulk heterojunction (BHJ) solar cells is one of the promising methods. Incorporation of metal nanostructures increases the absorption of organic materials due to the high electromagnetic field strength in the vicinity of the excited surface plasmons. In this work, we used 60 nm Au plasmonic structures to improve the efficiency of organic solar cell. The prepared metal nano structures were characterized through scanning electron microscopy (SEM), and UV-Visible spectroscopy techniques. These prepared metallic nanoparticles can be incorporated either into the electron transport layer (ETL) or into the active P3HT:PC71BM layer. The effect of incorporation of plasmonic gold (Au) nanoparticle in the inverted bulk heterojunction organic photovoltaic cells (OPVs) of P3HT:PC71BM fabricated in ambient air condition is in progress. Initial studies shows an 8.5% enhancement in the PCE with the incorporation of Au nanoparticles under AM1.5G light of intensity 1 Sun.

  18. Simple Synthesis and Enhanced Performance of Graphene Oxide-Gold Composites

    Directory of Open Access Journals (Sweden)

    Min Song

    2012-01-01

    Full Text Available Graphene oxide-gold composites were prepared by one-step reaction in aqueous solution, where the gold nanoparticles were deposited on the graphene oxide during their synthesis process. Transmission electron morphology, X-ray diffraction, Roman spectra, and UV-Vis absorption spectra were used to characterize the obtained composites. Furthermore, based on the BET analysis results, it was found that the surface area of the composite film was obviously enhanced compared with the synthesized graphene oxide. Electrochemical measurements indicated that the modification of the composites on electrode could efficiently enhance the voltammetric response, suggesting the potential application for making electrochemical sensors.

  19. Effect of phosphorus on hot ductility of high purity iron

    International Nuclear Information System (INIS)

    Abiko, K.; Liu, C.M.; Ichikawa, M..; Suenaga, H.; Tanino, M.

    1995-01-01

    Tensile tests on high purity Fe-P alloys with 0, 0.05 and 0.1 mass%P were carried out at temperatures between 300 K and 1073 K to clarify the intrinsic effect of phosphorus on the mechanical properties of iron at elevated temperatures. Microstructures of as-quenched, interrupted and ruptured specimens were observed. Experimental results show that the addition of phosphorus causes a remarkable increase in proof stress of high purity iron at 300 K, but the increase in proof stress by phosphorus decreases with increasing test temperature. The strengthening effect of phosphorus reduces to zero at 1073 K. High purity iron and Fe-P alloys rupture at almost 100% reduction in area at the whole test temperatures. However, Fe-P alloys show much larger elongation at test temperatures above 773 K than high purity iron. The increased elongation of high purity iron by addition of phosphorus was shown to be related to the effect of phosphorus on dynamic recovery and recrystallization of iron as its intrinsic effect. (orig.)

  20. Compositional engineering of acceptors for highly efficient bulk heterojunction hybrid organic solar cells.

    Science.gov (United States)

    Amber Yousaf, S; Ikram, M; Ali, S

    2018-10-01

    The wet chemical synthesis of chromium oxide (Cr 2 O 3 ) nanoparticles (NPs) and its application in active layer of inverted bulk heterojunction organic solar cells is documented in this research. Chromium oxide NPs of 10-30 nm size range having a band gap of 2.9 eV were successfully synthesized. These NPs were used in inverted organic solar cells in amalgamation with P3HT:PCBM and PTB7:PCBM polymers. The fabricated hybrid devices improves PCE significantly for P3HT:PCBM and PTB7:PCBM systems. The photophysical energy levels, optoelectrical properties and microscopic images have been systematically studied for the fabricated devices. The introduction of Cr 2 O 3 nanoparticles (NPs) enhances light harvesting and tunes energy levels into improved electrical parameters. A clear red shift and improved absorption have been observed for ternary blended devices compared to that observed with controlled organic solar cells. Apparently, when the amount of NPs in the binary polymer blend exceeds the required optimum level, there is a breakdown of the bulk heterojunction leading to lowering of the optical and electrical performance of the devices. Copyright © 2018 Elsevier Inc. All rights reserved.

  1. Inhibition of nitric oxide synthesis enhances leukocyte rolling and adhesion in human microvasculature

    Directory of Open Access Journals (Sweden)

    Hossain Mokarram

    2012-07-01

    Full Text Available Abstract Background Nitric oxide (NO is a multifunctional signaling molecule that regulates important cellular events in inflammation including leukocyte recruitment. Previous studies have shown that pharmacological inhibition of NO synthesis induces leukocyte recruitment in various in vitro and animal models. However, it is not known whether NO modulation has similar effects on leukocyte-endothelial cell interactions within the human microvasculature. The present study explored the effect of systemic L-NAME treatment on leukocyte recruitment in the SCID-hu mouse model. Methods Human skin xenografts were transplanted in SCID mice to study human leukocyte dynamics in human vasculature. Early events of human leukocyte recruitment in human vasculature were studied using intravital microscopy. NO synthesis was pharmacologically inhibited using NG-nitro-L-arginine methyl ester (L-NAME. Immunohistochemical analysis was performed to elucidate E-selectin expression in human xenograft skin. Human neutrophil-endothelial cell interactions were also studied in an in vitro flow chamber assay system. P- and E-selectin expression on cultured human umbilical vein endothelial cells (HUVECs was measured using ELISA. Platelet-activating factor (PAF synthesis was detected using a TLC-based assay. Results L-NAME treatment significantly enhanced the rolling and adhesion of human leukocytes to the human vasculature. Functional blocking of P- and E-selectins significantly inhibited rolling but not adhesion induced by inhibition of NO synthesis. Systemic L-NAME treatment enhanced E-selectin expression in human xenograft skin. L-NAME treatment significantly enhanced P- and E-selectin expression on HUVECs. L-NAME treatment did not significantly modify neutrophil rolling or adhesion to HUVECs indicating that L-NAME−induced subtle P- and E-selectin expression was insufficient to elicit dynamic neutrophil-HUVEC interactions in vitro. Moreover, synthesis of endothelial

  2. Bulk tungsten with uniformly dispersed La2O3 nanoparticles sintered from co-precipitated La2O3/W nanoparticles

    International Nuclear Information System (INIS)

    Xia, Min; Yan, Qingzhi; Xu, Lei; Guo, Hongyan; Zhu, Lingxu; Ge, Changchun

    2013-01-01

    Graphical abstract: La 2 O 3 doped La 2 O 3 /W nanoparticles with high-purity and uniform diameters have been fabricated by a co-precipitation process. The as-prepared nanoparticles demonstrate the potential of this method for fabricating uniformly structured bulk tungsten materials. -- Abstract: We report the preparation of 1 wt% La 2 O 3 doped La 2 O 3 /W nanoparticles by a co-precipitation process, using ammonium metatungstate (AMT) and lanthanum nitrate as raw materials. The as-synthesized nanoparticles were characterized by X-ray diffraction, Filed-emission scanning electron microscopy, Transmission electron microscopy (TEM), energy dispersive spectroscopy. Our results reveal that the as-synthesized particles possess uniform diameters of about 70 nm, and are of high purity. The TEM and the corresponding fast Fourier transform images demonstrated that La 2 O 3 precipitates were homogeneously doped into the nano-sized tungsten particles. When the as-synthesized nanoparticles were sintered by spark plasma sintering, the electron backscatter diffraction images of the bulk material reveal that La 2 O 3 nanoparticles were homogenously distributed in both the tungsten grains and the grain boundaries, and the sample exhibit a narrow micro-hardness distribution

  3. Thermal and electrical conductivities of high purity tantalum

    International Nuclear Information System (INIS)

    Archer, S.L.

    1978-01-01

    The electrical resistivity and thermal conductivity of three high purity tantalum samples have been measured as functions of temperature over a temperature range of 5K to 65K. Sample purities ranged up to a resistivity ratio of 1714. The highest purity sample had a residual resistivity of .76 x 10 -10 OMEGA-m. The intrinsic resistivity varied as T 3 . 9 from 10K to 31K. The thermal conductivity of the purest sample had a maximum of 840 W/mK at 9.8K. The intrinsic thermal resistivity varied as T 2 . 4 from 10K to 35K. At low temperatures electrons were scattered primarily by impurities and by phonons with both interband and intraband transitions observed. The electrical and thermal resistivity is departed from Matthiessen's rule at low temperatures

  4. Fabrication of high quality anodic aluminum oxide (AAO) on low purity aluminum—A comparative study with the AAO produced on high purity aluminum

    International Nuclear Information System (INIS)

    Michalska-Domańska, Marta; Norek, Małgorzata; Stępniowski, Wojciech J.; Budner, Bogusław

    2013-01-01

    Highlights: • Nanoporous alumina was fabricated by anodization in sulfuric acid solution with glycol. • The AAO manufacturing on low- and high-purity Al was compared. • The pores size was ranging between 30 and 50 nm. • No difference in the quality of the AAO fabricated on both Al types was observed. • The current vs. anodization time curves were recorded. -- Abstract: In this work the quality, arrangement, composition, and regularity of nanoporous AAO formed on the low-purity (AA1050) and high-purity aluminum during two-step anodization in a mixture of sulfuric acid solution (0.3 M), water and glycol (3:2, v/v), at various voltages (15, 20, 25, 30, 35 V) and at temperature of −1 °C, are investigated. The electrochemical conditions have allowed to obtain pores with the size ranging from 30 to 50 nm, which are much larger than those usually obtained by anodization in a pure sulfuric acid solution (<20 nm). The mechanism of the AAO growth is discussed. It was found that with the increase of applied anodizing voltage a number of incorporated sulfate ions in the aluminum oxide matrix increases, which was connected with the appearance of an unusual area in the current vs. time curves. On the surface of anodizing low- and high-purity aluminum, the formation of hillocks was observed, which was associated with the sulfate ions incorporation. The sulfate ions are replacing the oxygen atom/atoms in the AAO amorphous crystal structure and, consequently, the AAO template swells, the oxide cracks and uplifts causing the formation of hillocks. The same mechanism occurs for both low- and high-purity aluminum. Nanoporous AAO characterized by a very high regularity, not registered previously for low purity aluminum, was obtained. Furthermore, no significant difference in the regularity ratio between the AAO obtained on low- and high-purity aluminum, was observed. The electrochemical conditions applied in this study can be, thus, used for the fabrication of high quality

  5. Radioactive preparations. Determination of radiochemical purity by thin-layer chromatography

    International Nuclear Information System (INIS)

    1986-01-01

    The standard sets the data which must be attached to every sample, and the equipment, chemicals and auxiliary substances used in the determination of radiochemical purity of substances by chromatography. Described are preparation of the sample, the procedure of sample deposition, the development, drying and detection of the radioactive preparation. The qualitative and quantitative assessment of the radiochromatogram is described as are the calculation of radiochemical purity and the determination of the reproducibility of measurement of radiochemical purity of radioactive preparations. (E.S.)

  6. Synthesis of L-[35S] homocysteine thiolactone hydrochloride

    International Nuclear Information System (INIS)

    Hamacher, K.

    1989-01-01

    L-[ 35 S]Homocysteine thiolactone has been synthesized by demethylation of L-[ 35 S]Methionine with sodium in liquid ammonia and subsequent lactonisation in acid solution. The radiochemical yield of the carrier added synthesis was in the range of 45 to 50% with a radiochemical purity higher than 96%. (author)

  7. Synthesis of 14C-dehydrocorydaline chloride

    International Nuclear Information System (INIS)

    Zhang Rui; Wang Ding

    1988-01-01

    A method for synthesis of 14 C-dehydrocorydaline chloride is described. In the presence of sodium hydroxide, acetonylpalmatine is reacted with 14 C-methyl iodide in sealed glass ampoule to give 14 C-13-methylpalmatine iodide which is then converted to chloride. The radiochemical purity of 14 C-dehydrocorydaline determined by TLC is over 98% and the labelling efficiency is 54%

  8. Purity of Gaussian states: Measurement schemes and time evolution in noisy channels

    International Nuclear Information System (INIS)

    Paris, Matteo G.A.; Illuminati, Fabrizio; Serafini, Alessio; De Siena, Silvio

    2003-01-01

    We present a systematic study of the purity for Gaussian states of single-mode continuous variable systems. We prove the connection of purity to observable quantities for these states, and show that the joint measurement of two conjugate quadratures is necessary and sufficient to determine the purity at any time. The statistical reliability and the range of applicability of the proposed measurement scheme are tested by means of Monte Carlo simulated experiments. We then consider the dynamics of purity in noisy channels. We derive an evolution equation for the purity of general Gaussian states both in thermal and in squeezed thermal baths. We show that purity is maximized at any given time for an initial coherent state evolving in a thermal bath, or for an initial squeezed state evolving in a squeezed thermal bath whose asymptotic squeezing is orthogonal to that of the input state

  9. Automated synthesis with HPLC purification of 18F-FMISO as specific molecular imaging probe of tumor hypoxia

    International Nuclear Information System (INIS)

    Wang Mingwei; Zhang Yingjian; Zhang Yongping

    2012-01-01

    An improved automated synthesis of 1-H-1-(3-[ 18 F] fluoro-2-hydroxypropyl)-2-nitro-imidazole ( 18 F-FMISO), a specific molecular imaging probe of tumor hypoxia, was developed using an upgraded Explora GN module integrated with Explora LC for HPLC purification in this study. The radiochemical synthesis of 18 F-FMISO was started with precursor 1-( 2'-nitro-1'-imidazolyl)-2-O-tetrahydropyranyl-3-O-tosyl-propanediol (NITTP) and included nucleophilic [ 18 F] radio-fluorination at 120℃ for 5 min and hydrolysis at 130℃ for 8 min. The automated synthesis of 18 F-FMISO, presenting fast, reliable and multi-run features, could be completed with the total synthesis time of less than 65 min and radiochemical yield of 25%∼35% (without decay correction). The quality control of 18 F-FMISO was identical with the radiopharmaceutical requirements, especially the radiochemical purity of greater than 99% and high chemical purity and specific activity own to HPLC purification. (authors)

  10. Thermodynamic-Controlled Gas Phase Process for the Synthesis of Nickel Nanoparticles of Adjustable Size and Morphology

    International Nuclear Information System (INIS)

    Kauffeldt, Elena; Kauffeldt, Thomas

    2006-01-01

    Gas phase processes are a successful route for the synthesis of nano materials. Nickel particles are used in applications ranging from catalysis to nano electronics and energy storage. The application field defines the required particle size, morphology, crystallinity and purity. Nickel tetracarbonyl is the most promising precursor for the synthesis of high purity nickel particles. Due to the toxicity of this precursor and to obtain an optimal process control we developed a two-step flow type process. Nickel carbonyl and nickel particles are synthesized in a sequence of reactions. The particles are formed in a hot wall reactor at temperatures below 400 deg. C in different gas compositions. Varying the process conditions enables the adjustment of the particle size in a range from 3 to 140 nm. The controllable crystalline habits are polycrystalline, single crystals or multiple twinned particles (MTP). Spectroscopic investigations show an excellent purity. We report about the process and first investigations of the properties of the synthesized nickel nanomaterial

  11. Nearly Blinking-Free, High-Purity Single-Photon Emission by Colloidal InP/ZnSe Quantum Dots.

    Science.gov (United States)

    Chandrasekaran, Vigneshwaran; Tessier, Mickaël D; Dupont, Dorian; Geiregat, Pieter; Hens, Zeger; Brainis, Edouard

    2017-10-11

    Colloidal core/shell InP/ZnSe quantum dots (QDs), recently produced using an improved synthesis method, have a great potential in life-science applications as well as in integrated quantum photonics and quantum information processing as single-photon emitters. Single-particle spectroscopy of 10 nm QDs with 3.2 nm cores reveals strong photon antibunching attributed to fast (70 ps) Auger recombination of multiple excitons. The QDs exhibit very good photostability under strong optical excitation. We demonstrate that the antibunching is preserved when the QDs are excited above the saturation intensity of the fundamental-exciton transition. This result paves the way toward their usage as high-purity on-demand single-photon emitters at room temperature. Unconventionally, despite the strong Auger blockade mechanism, InP/ZnSe QDs also display very little luminescence intermittency ("blinking"), with a simple on/off blinking pattern. The analysis of single-particle luminescence statistics places these InP/ZnSe QDs in the class of nearly blinking-free QDs, with emission stability comparable to state-of-the-art thick-shell and alloyed-interface CdSe/CdS, but with improved single-photon purity.

  12. 7 CFR 201.51b - Purity procedures for coated seed.

    Science.gov (United States)

    2010-01-01

    ... ACT FEDERAL SEED ACT REGULATIONS Purity Analysis in the Administration of the Act § 201.51b Purity...). Use of fine mesh sieves is recommended for this procedure, and stirring or shaking the coated units...

  13. The Liquid Argon Purity Demonstrator

    Energy Technology Data Exchange (ETDEWEB)

    Adamowski, M.; Carls, B.; Dvorak, E.; Hahn, A.; Jaskierny, W.; Johnson, C.; Jostlein, H.; Kendziora, C.; Lockwitz, S.; Pahlka, B.; Plunkett, R.; Pordes, S.; Rebel, B.; Schmitt, R.; Stancari, M.; Tope, T.; Voirin, E.; Yang, T.

    2014-07-01

    The Liquid Argon Purity Demonstrator was an R&D test stand designed to determine if electron drift lifetimes adequate for large neutrino detectors could be achieved without first evacuating the cryostat. We describe here the cryogenic system, its operations, and the apparatus used to determine the contaminant levels in the argon and to measure the electron drift lifetime. The liquid purity obtained by this system was facilitated by a gaseous argon purge. Additionally, gaseous impurities from the ullage were prevented from entering the liquid at the gas-liquid interface by condensing the gas and filtering the resulting liquid before returning to the cryostat. The measured electron drift lifetime in this test was greater than 6 ms, sustained over several periods of many weeks. Measurements of the temperature profile in the argon, to assess convective flow and boiling, were also made and are compared to simulation.

  14. Purity and adulterant analysis of crack seizures in Brazil.

    Science.gov (United States)

    Fukushima, André R; Carvalho, Virginia M; Carvalho, Débora G; Diaz, Ernesto; Bustillos, Jose Oscar William Vega; Spinosa, Helenice de S; Chasin, Alice A M

    2014-10-01

    Cocaine represents a serious problem to society. Smoked cocaine is very addictive and it is frequently associated with violence and health issues. Knowledge of the purity and adulterants present in seized cocaine, as well as variations in drug characteristics are useful to identify drug source and estimate health impact. No data are available regarding smoked cocaine composition in most countries, and the smoked form is increasing in the Brazilian market. The purpose of the present study is to contribute to the current knowledge on the status of crack cocaine seized samples on the illicit market by the police of São Paulo. Thus, 404 samples obtained from street seizures conducted by the police were examined. The specimens were macroscopically characterized by color, form, odor, purity, and adulterant type, as well as smoke composition. Samples were screened for cocaine using modified Scott test and thin-layer chromatographic (TLC) technique. Analyses of purity and adulterants were performed with gas chromatography equipped with flame ionization detector (GC-FID). Additionally, smoke composition was analyzed by GC-mass spectrometry (MS), after samples burning. Samples showed different colors and forms, the majority of which is yellow (74.0%) or white (20.0%). Samples free of adulterants represented 76.3% of the total. Mean purity of the analyzed drug was 71.3%. Crack cocaine presented no correlations between macroscopic characteristics and purity. Smoke analysis showed compounds found also in the degradation of diesel and gasoline. Therefore, the drug marketed as crack cocaine in São Paulo has similar characteristics to coca paste. High purity can represent a greater risk of dependency and smoke compounds are possibly worsening drug health impact. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

  15. Purity Evaluation of Single-Walled Carbon Nanotubes Using Thermogravimetric Analysis

    International Nuclear Information System (INIS)

    Goak, Jeung Choon; Kim, Tae Yang; Jung, Jongwan; Seo, Young-Soo; Lee, Naesung; Sok, Junghyun

    2013-01-01

    This study evaluated the purity of single-walled carbon nanotubes (SWCNTs) in the arc-synthesized SWCNT samples by using thermogravimetric analysis (TGA). The as-produced SWCNT samples were heat-treated in air for 20 h at 275-475°C and characterized by scanning and transmission electron microscopes and TGA to establish oxidation temperature ranges of SWCNTs and carbonaceous impurities comprising the samples. Based on these oxidation temperature ranges, derivative thermogravimetric curves were deconvoluted, and differentiated peaks were assigned to SWCNTs and carbonaceous impurities. The compositions and the SWCNT purities of the samples were obtained simply by calculating the areal ratios under the deconvoluted curves. TGA studies on purity evaluation and thermal stabilities of SWCNTs and carbonaceous impurities are likely to provide us with a simple route of thermal oxidation purification to acquire high-purity SWCNT samples.

  16. Correlation between product purity and process parameters for the synthesis of Cu2ZnSnS4 nanoparticles using microwave irradiation

    Science.gov (United States)

    Ahmad, R.; Nicholson, K. S.; Nawaz, Q.; Peukert, W.; Distaso, M.

    2017-07-01

    Kesterites (CZT(S,Se)4) emerged as a favourable photovoltaic material, leading to solar cell efficiencies as high as 12.7%. The development of sustainable roll-to-roll printing processes that make use of Cu2ZnSnS4 (CZTS) nanoparticle inks requires the proper design of synthetic approaches and the understanding of the relation between process parameters and product purity. In the current paper, we developed this relationship by calculating a specific energy factor. A microwave-assisted synthetic method that operates at atmospheric pressure and makes use of eco-friendly solvents is established. Four solvents, i.e. ethylene glycol (EG), diethylene glycol (di-EG), triethylene glycol (tri-EG) and tetraethylene glycol (tet-EG) are compared and the temperature during the reaction is assessed by two different methods. In particular, two by-products have been identified, i.e. Cu2 - x S and a hexagonal phase. We show that the variation of reaction parameters such as power irradiation, type of solvent and precursor concentration influences the nanoparticles' sizes (from 12 to 6 nm) and also the temperature-time profile of reaction which, in turn, can be related to phase purity of CZTS nanoparticles. The results suggest that the product purity scales with the specific energy factor providing a useful tool to a rational design of high-quality CZTS nanoparticles.

  17. Combinatorial synthesis of oxazol-thiazole bis-heterocyclic compounds.

    Science.gov (United States)

    Murru, Siva; Nefzi, Adel

    2014-01-13

    A combinatorial library of novel oxazol-thiazole bis-heterocycles was synthesized in good to excellent overall yields with high purity using a solution and solid-phase parallel synthesis approach. Oxazole amino acids, prepared from serine methyl ester and amino acids via coupling and cyclodehydration, were treated with Fmoc-NCS and α-haloketones for the parallel synthesis of diverse bis-heterocycles. Fmoc-isothiocyanate is used as a traceless reagent for thiazole formation. Oxazole diversity can be achieved by using variety of amino acids, whereas thiazole diversity is produced with various haloketones.

  18. Iodine Absorption Cells Purity Testing

    Directory of Open Access Journals (Sweden)

    Jan Hrabina

    2017-01-01

    Full Text Available This article deals with the evaluation of the chemical purity of iodine-filled absorption cells and the optical frequency references used for the frequency locking of laser standards. We summarize the recent trends and progress in absorption cell technology and we focus on methods for iodine cell purity testing. We compare two independent experimental systems based on the laser-induced fluorescence method, showing an improvement of measurement uncertainty by introducing a compensation system reducing unwanted influences. We show the advantages of this technique, which is relatively simple and does not require extensive hardware equipment. As an alternative to the traditionally used methods we propose an approach of hyperfine transitions’ spectral linewidth measurement. The key characteristic of this method is demonstrated on a set of testing iodine cells. The relationship between laser-induced fluorescence and transition linewidth methods will be presented as well as a summary of the advantages and disadvantages of the proposed technique (in comparison with traditional measurement approaches.

  19. Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

    International Nuclear Information System (INIS)

    Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

    2011-01-01

    The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO 2 ) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO 2 ). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO 2 /TiO 2 ) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO 2 -Degussa P25 catalyst is detected.

  20. Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

    Science.gov (United States)

    Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

    2011-11-01

    The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO2) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO2). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO2/TiO2) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO2-Degussa P25 catalyst is detected.

  1. Semi-automatic synthesis and biological evaluation of 18F-FCH as an oncologic PET tracer

    International Nuclear Information System (INIS)

    Wu Zhanhong; Wang Shizhen; Zhou Qian; Fu Zhe; Qiu Feichan; Huo Li

    2005-01-01

    18 F-fluromethylcholine ( 18 F-FCH) as a PET tracer is synthesized. The semi-automatic synthesis assembly of 18 F-FCH is modified from CPCU(CTI). The radiochemical purity is measured by analytical HPLC. The radiochemical yield and the radiochemical purity of 18 F-FCH are 15% and >99%, respectively. The total radiosynthesis time is 55 min after EOB. The labeled product exhibited low toxicity. The biodistribution in normal mice and the toxicity are studied. PET imaging with 18 F-FCH is performed on tumor xenograft murine model. The semi-automatic synthesis assembly is promising to be used for routine clinic radiopharmaceutical preparation and preliminary study has shown the usefulness of 18 F-FCH as an oncologic PET tracer. (authors)

  2. Superconducting radio-frequency cavities made from medium and low-purity niobium ingots

    Science.gov (United States)

    Ciovati, Gianluigi; Dhakal, Pashupati; Myneni, Ganapati R.

    2016-06-01

    Superconducting radio-frequency cavities made of ingot niobium with residual resistivity ratio (RRR) greater than 250 have proven to have similar or better performance than fine-grain Nb cavities of the same purity, after standard processing. The high purity requirement contributes to the high cost of the material. As superconducting accelerators operating in continuous-wave typically require cavities to operate at moderate accelerating gradients, using lower purity material could be advantageous not only to reduce cost but also to achieve higher Q 0-values. In this contribution we present the results from cryogenic RF tests of 1.3-1.5 GHz single-cell cavities made of ingot Nb of medium (RRR = 100-150) and low (RRR = 60) purity from different suppliers. Cavities made of medium-purity ingots routinely achieved peak surface magnetic field values greater than 70 mT with an average Q 0-value of 2 × 1010 at 2 K after standard processing treatments. The performances of cavities made of low-purity ingots were affected by significant pitting of the surface after chemical etching.

  3. The influence of micropore size on the mechanical properties of bulk hydroxyapatite and hydroxyapatite scaffolds.

    Science.gov (United States)

    Cordell, Jacqueline M; Vogl, Michelle L; Wagoner Johnson, Amy J

    2009-10-01

    While recognized as a promising bone substitute material, hydroxyapatite (HA) has had limited use in clinical settings because of its inherent brittle behavior. It is well established that macropores ( approximately 100 microm) in a HA implant, or scaffold, are required for bone ingrowth, but recent research has shown that ingrowth is enhanced when scaffolds also contain microporosity. HA is sensitive to synthesis and processing parameters and therefore characterization for specific applications is necessary for transition to the clinic. To that end, the mechanical behavior of bulk microporous HA and HA scaffolds with multi-scale porosity (macropores between rods in the range of 250-350 microm and micropores within the rods with average size of either 5.96 microm or 16.2 microm) was investigated in order to determine how strength and reliability were affected by micropore size (5.96 microm versus 16.2 microm). For the bulk microporous HA, strength increased with decreasing micropore size in both bending (19 MPa to 22 MPa) and compression (71 MPa to 110 MPa). To determine strength reliability, the Weibull moduli for the bulk microporous HA were determined. The Weibull moduli for bending increased (became more reliable) with decreasing pore size (7 to 10) while the Weibull moduli for compression decreased (became less reliable) with decreasing pore size (9 to 6). Furthermore, the elastic properties of the bulk microporous HA (elastic modulus of 30 GPa) and the compressive strengths of the HA scaffolds with multi-scale porosity (8 MPa) did not vary with pore size. The mechanisms responsible for the trends observed were discussed.

  4. Light Enhanced Hydrofluoric Acid Passivation: A Sensitive Technique for Detecting Bulk Silicon Defects

    Science.gov (United States)

    Grant, Nicholas E.

    2016-01-01

    A procedure to measure the bulk lifetime (>100 µsec) of silicon wafers by temporarily attaining a very high level of surface passivation when immersing the wafers in hydrofluoric acid (HF) is presented. By this procedure three critical steps are required to attain the bulk lifetime. Firstly, prior to immersing silicon wafers into HF, they are chemically cleaned and subsequently etched in 25% tetramethylammonium hydroxide. Secondly, the chemically treated wafers are then placed into a large plastic container filled with a mixture of HF and hydrochloric acid, and then centered over an inductive coil for photoconductance (PC) measurements. Thirdly, to inhibit surface recombination and measure the bulk lifetime, the wafers are illuminated at 0.2 suns for 1 min using a halogen lamp, the illumination is switched off, and a PC measurement is immediately taken. By this procedure, the characteristics of bulk silicon defects can be accurately determined. Furthermore, it is anticipated that a sensitive RT surface passivation technique will be imperative for examining bulk silicon defects when their concentration is low (<1012 cm-3). PMID:26779939

  5. Relationship between critical current properties and microstructure in cylindrical RE123 melt-solidified bulks

    International Nuclear Information System (INIS)

    Nakashima, T.; Shimoyama, J.; Honzumi, M.; Tazaki, Y.; Horii, S.; Kishio, K.

    2005-01-01

    We report the synthesis of cylindrical melt-solidified bulks in REBa 2 Cu 3 O y (RE = Sm, Gd, Dy, Ho, Y and Er), and their critical current properties and microstructures of the a- and the c-growth regions. It was found from the microstructure analysis that the volume fractions of RE211 particles in the c-growth region were always lower than those in the a-growth region. Moreover, those in the c-growth region were increased with distance from the seed crystal. Interestingly, the second peak effects in J c -B curves were prominently enhanced for the c-growth region. J c values at zero field for the c-growth region through the appropriate oxygen post-annealing reached approximately 95 kA cm -2 for RE = Ho, Dy and Y

  6. Microwave heating in solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Pedersen, Søren Ljungberg; Shelton, Anne Pernille Tofteng; Malik, Leila

    2012-01-01

    synthesis, precise microwave irradiation to heat the reaction mixture during coupling and N(a)-deprotection has become increasingly popular. It has often provided dramatic reductions in synthesis times, accompanied by an increase in the crude peptide purity. Microwave heating has been proven especially...... relevant for sequences which might form ß-sheet type structures and for sterically difficult couplings. The beneficial effect of microwave heating appears so far to be due to the precise nature of this type of heating, rather than a peptide-specific microwave effect. However, microwave heating...... in microwave heating for peptide synthesis, with a focus on systematic studies and general protocols, as well as important applications. The assembly of ß-peptides, peptoids and pseudopeptides are also evaluated in this critical review (254 references)....

  7. A Co-Opted DEAD-Box RNA helicase enhances tombusvirus plus-strand synthesis.

    Directory of Open Access Journals (Sweden)

    Nikolay Kovalev

    2012-02-01

    Full Text Available Replication of plus-strand RNA viruses depends on recruited host factors that aid several critical steps during replication. In this paper, we show that an essential translation factor, Ded1p DEAD-box RNA helicase of yeast, directly affects replication of Tomato bushy stunt virus (TBSV. To separate the role of Ded1p in viral protein translation from its putative replication function, we utilized a cell-free TBSV replication assay and recombinant Ded1p. The in vitro data show that Ded1p plays a role in enhancing plus-strand synthesis by the viral replicase. We also find that Ded1p is a component of the tombusvirus replicase complex and Ded1p binds to the 3'-end of the viral minus-stranded RNA. The data obtained with wt and ATPase deficient Ded1p mutants support the model that Ded1p unwinds local structures at the 3'-end of the TBSV (-RNA, rendering the RNA compatible for initiation of (+-strand synthesis. Interestingly, we find that Ded1p and glyceraldehyde-3-phosphate dehydrogenase (GAPDH, which is another host factor for TBSV, play non-overlapping functions to enhance (+-strand synthesis. Altogether, the two host factors enhance TBSV replication synergistically by interacting with the viral (-RNA and the replication proteins. In addition, we have developed an in vitro assay for Flock house virus (FHV, a small RNA virus of insects, that also demonstrated positive effect on FHV replicase activity by the added Ded1p helicase. Thus, two small RNA viruses, which do not code for their own helicases, seems to recruit a host RNA helicase to aid their replication in infected cells.

  8. Entanglement and purity of two-mode Gaussian states in noisy channels

    International Nuclear Information System (INIS)

    Serafini, Alessio; Illuminati, Fabrizio; De Siena, Silvio; Paris, Matteo G.A.

    2004-01-01

    We study the evolution of purity, entanglement, and total correlations of general two-mode continuous variable Gaussian states in arbitrary uncorrelated Gaussian environments. The time evolution of purity, von Neumann entropy, logarithmic negativity, and mutual information is analyzed for a wide range of initial conditions. In general, we find that a local squeezing of the bath leads to a faster degradation of purity and entanglement, while it can help to preserve the mutual information between the modes

  9. Robotic synthesis of [carbon-11]methionine

    International Nuclear Information System (INIS)

    Korsakov, M.V.; Kisselev, M.Y.; Solovyov, D.; Horti, A.G.; Vasilev, A.; Nilsson, L.E.; Ulin, J.

    1992-01-01

    [ 11 C]Methionine was prepared in a fully automated robotic synthesis, using the SCANDITRONIX robotic system starting from [ 11 C]I and homocysteine thiolactone. The product was purified using solid phase extraction on anionic exchange cartridges. The decay corrected yield was 60% based on CH 3 I and 16 min synthesis time. The radiochemical purity was 98-99% and the chemical impurities were: homocysteine 0.05-0.07 mg/ml, homocystine 0.005 mg/ml, 'cold' methionine 0.03-0.05 mg/ml, and homocysteine thiolactone 0.0008-0.002 mg/ml. The total procedure takes 30 min from EOB. (author) 6 figs., 3 tabs

  10. Modelling of bulk superconductor magnetization

    International Nuclear Information System (INIS)

    Ainslie, M D; Fujishiro, H

    2015-01-01

    This paper presents a topical review of the current state of the art in modelling the magnetization of bulk superconductors, including both (RE)BCO (where RE = rare earth or Y) and MgB 2 materials. Such modelling is a powerful tool to understand the physical mechanisms of their magnetization, to assist in interpretation of experimental results, and to predict the performance of practical bulk superconductor-based devices, which is particularly important as many superconducting applications head towards the commercialization stage of their development in the coming years. In addition to the analytical and numerical techniques currently used by researchers for modelling such materials, the commonly used practical techniques to magnetize bulk superconductors are summarized with a particular focus on pulsed field magnetization (PFM), which is promising as a compact, mobile and relatively inexpensive magnetizing technique. A number of numerical models developed to analyse the issues related to PFM and optimise the technique are described in detail, including understanding the dynamics of the magnetic flux penetration and the influence of material inhomogeneities, thermal properties, pulse duration, magnitude and shape, and the shape of the magnetization coil(s). The effect of externally applied magnetic fields in different configurations on the attenuation of the trapped field is also discussed. A number of novel and hybrid bulk superconductor structures are described, including improved thermal conductivity structures and ferromagnet–superconductor structures, which have been designed to overcome some of the issues related to bulk superconductors and their magnetization and enhance the intrinsic properties of bulk superconductors acting as trapped field magnets. Finally, the use of hollow bulk cylinders/tubes for shielding is analysed. (topical review)

  11. Superconducting radio-frequency cavities made from medium and low-purity niobium ingots

    International Nuclear Information System (INIS)

    Ciovati, Gianluigi; Dhakal, Pashupati; Myneni, Ganapati R

    2016-01-01

    Superconducting radio-frequency cavities made of ingot niobium with residual resistivity ratio (RRR) greater than 250 have proven to have similar or better performance than fine-grain Nb cavities of the same purity, after standard processing. The high purity requirement contributes to the high cost of the material. As superconducting accelerators operating in continuous-wave typically require cavities to operate at moderate accelerating gradients, using lower purity material could be advantageous not only to reduce cost but also to achieve higher Q 0 -values. In this contribution we present the results from cryogenic RF tests of 1.3–1.5 GHz single-cell cavities made of ingot Nb of medium (RRR = 100–150) and low (RRR = 60) purity from different suppliers. Cavities made of medium-purity ingots routinely achieved peak surface magnetic field values greater than 70 mT with an average Q 0 -value of 2 × 10 10 at 2 K after standard processing treatments. The performances of cavities made of low-purity ingots were affected by significant pitting of the surface after chemical etching. (paper)

  12. An automated synthesis-purification-sample-management platform for the accelerated generation of pharmaceutical candidates.

    Science.gov (United States)

    Sutherland, J David; Tu, Noah P; Nemcek, Thomas A; Searle, Philip A; Hochlowski, Jill E; Djuric, Stevan W; Pan, Jeffrey Y

    2014-04-01

    A flexible and integrated flow-chemistry-synthesis-purification compound-generation and sample-management platform has been developed to accelerate the production of small-molecule organic-compound drug candidates in pharmaceutical research. Central to the integrated system is a Mitsubishi robot, which hands off samples throughout the process to the next station, including synthesis and purification, sample dispensing for purity and quantification analysis, dry-down, and aliquot generation.

  13. Analytical monitoring of systems for the production of high-purity, desalinated water

    International Nuclear Information System (INIS)

    Kunert, I.

    1988-01-01

    The purity requirements to be met by high-purity water currently push the most sensitive analytical methods to their utmost limits of sensitivity. The required degree of purity of the water at present can only be achieved by application of membrane processes, and pre-purification of the feedwater to a quality corresponding to that of the raw water source. The contribution in hand discusses the analytical monitoring of the raw water treatment plant, the water treatment prior to the treatment by reverse osmosis, monitoring and control of the modules for reverse osmosis, and the monitoring of high-purity water production for the microelectronics industry. (orig./RB) [de

  14. Synthesis of bulk quantity BN nanotubes with uniform morphology

    International Nuclear Information System (INIS)

    Wen, G.; Zhang, T.; Huang, X.X.; Zhong, B.; Zhang, X.D.; Yu, H.M.

    2010-01-01

    Bulk quantity hexagonal BN nanotubes (h-BNNTs) with uniform morphology were synthesized via an improved ball-milling and annealing method. The sample was characterized by X-ray photoelectron spectrometry, electron energy loss spectroscopy, X-ray diffraction, scanning electron microscopy, conventional transmission electron microscopy (TEM) and high-resolution TEM. The results show that the fabricated BNNTs have a uniform diameter ranging from 80 to 100 nm and a length of about 50-60 μm.

  15. Lutetium-177 DOTATATE Production with an Automated Radiopharmaceutical Synthesis System.

    Science.gov (United States)

    Aslani, Alireza; Snowdon, Graeme M; Bailey, Dale L; Schembri, Geoffrey P; Bailey, Elizabeth A; Pavlakis, Nick; Roach, Paul J

    2015-01-01

    Peptide Receptor Radionuclide Therapy (PRRT) with yttrium-90 ((90)Y) and lutetium-177 ((177)Lu)-labelled SST analogues are now therapy option for patients who have failed to respond to conventional medical therapy. In-house production with automated PRRT synthesis systems have clear advantages over manual methods resulting in increasing use in hospital-based radiopharmacies. We report on our one year experience with an automated radiopharmaceutical synthesis system. All syntheses were carried out using the Eckert & Ziegler Eurotope's Modular-Lab Pharm Tracer® automated synthesis system. All materials and methods used were followed as instructed by the manufacturer of the system (Eckert & Ziegler Eurotope, Berlin, Germany). Sterile, GMP-certified, no-carrier added (NCA) (177)Lu was used with GMP-certified peptide. An audit trail was also produced and saved by the system. The quality of the final product was assessed after each synthesis by ITLC-SG and HPLC methods. A total of 17 [(177)Lu]-DOTATATE syntheses were performed between August 2013 and December 2014. The amount of radioactive [(177)Lu]-DOTATATE produced by each synthesis varied between 10-40 GBq and was dependant on the number of patients being treated on a given day. Thirteen individuals received a total of 37 individual treatment administrations in this period. There were no issues and failures with the system or the synthesis cassettes. The average radiochemical purity as determined by ITLC was above 99% (99.8 ± 0.05%) and the average radiochemical purity as determined by HPLC technique was above 97% (97.3 ± 1.5%) for this period. The automated synthesis of [(177)Lu]-DOTATATE using Eckert & Ziegler Eurotope's Modular-Lab Pharm Tracer® system is a robust, convenient and high yield approach to the radiolabelling of DOTATATE peptide benefiting from the use of NCA (177)Lu and almost negligible radiation exposure of the operators.

  16. Purity and surface roughness of vacuum deposited aluminium films

    Energy Technology Data Exchange (ETDEWEB)

    Dhere, N G; Arsenio, T P [Instituto Militar de Engenharia, Rio de Janeiro (Brazil); Patnaik, B K [Pontificia Universidade Catolica do Rio de Janeiro (Brazil). Instituto de Fisica; Assuncao, F C.R.; de Souza, A M [Pontificia Universidade Catolica do Rio de Janeiro (Brazil). Departamento de Ciencia dos Materiais e Metalurgia

    1975-04-01

    The authors studied the purity, surface roughness and grain size of vacuum-deposited aluminium films, using an intermetallic crucible and a continuous feed of pure aluminium wire. The grain size and roughness were studied by electron difraction, X-ray diffraction and the scanning electron microscope. Purity was determined by X-ray fluorescence produced by proton bombardment in the Van de Graaff accelerator and by X-ray and optical emission spectrometry.

  17. Synthesis, characterization and photocatalysis enhancement of Eu2O3-ZnO mixed oxide nanoparticles

    Science.gov (United States)

    Mohamed, W. S.; Abu-Dief, Ahmed M.

    2018-05-01

    Pure ZnO nanoparticles (NPs) and mixed Eu2O3 and ZnO NPs with different Eu2O3 ratios (5%, 10%, and 15%) were synthesized by a precipitation method under optimum conditions. The synthesized samples were characterized by means of X-ray diffraction, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy, transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, and UV-vis diffuse reflectance spectroscopy. The as-synthesized ZnO NPs exhibit high phase purity and a highly crystalline wurtzite ZnO structure. The mixed Eu2O3 and ZnO NPs exhibit a Eu2O3 zinc blend phase in addition to the wurtzite phase of pure ZnO, confirming the high purity and good crystallinity of the as-synthesized samples. The high-purity formation of ZnO and Eu2O3 phases was confirmed by FTIR and Raman spectra. Microstructural analysis by SEM and TEM confirmed the sphere-like morphology with different particle sizes (29-40 nm) of the as-synthesized samples. The photocatalytic activities of pure ZnO NPs and mixed Eu2O3 and ZnO NPs for the degradation of methylene blue were evaluated under ultraviolet (UV) irradiation. The results show that Eu2O3 plays an important role in the enhancement of the photocatalytic properties of ZnO NPs. We found that mixed 5% Eu2O3 and ZnO NPs exhibit the highest photocatalytic activity (degradation efficiency of 96.5% after 180 min of UV irradiation) as compared with pure ZnO NPs (degradation efficiency of 80.3% after 180 min of UV irradiation). The increased photocatalytic activity of the optimum mixed Eu2O3 and ZnO NPs is due to the high crystallinity, high surface area with small particle size, and narrow energy gap.

  18. Leucine pulses enhance skeletal muscle protein synthesis during continuous feeding in neonatal pigs

    Science.gov (United States)

    Infants unable to maintain oral feeding can be nourished by orogastric tube. We have shown that orogastric continuous feeding restricts muscle protein synthesis compared with intermittent bolus feeding in neonatal pigs. To determine whether leucine leu infusion can be used to enhance protein synthes...

  19. High-purity aluminium creep under high hydrostatic pressure

    International Nuclear Information System (INIS)

    Zajtsev, V.I.; Lyafer, E.I.; Tokij, V.V.

    1977-01-01

    The effect of the hydrostatic pressure on the rate of steady-state creep of high-purity aluminium was investigated. It is shown that the hydrostatic pressure inhibits the creep. The activation volume of the creep is independent of the direction in the range of (4.7-6.2) kg/mm 2 and of the pressure in the range of (1-7.8000) atm. It is concluded that self-diffusion does not control the creep of high-purity aluminium at room temperature in the investigated stress and pressure range

  20. High-Purity Hybrid Organolead Halide Perovskite Nanoparticles Obtained by Pulsed-Laser Irradiation in Liquid

    KAUST Repository

    Amendola, Vincenzo

    2016-11-17

    Nanoparticles of hybrid organic-inorganic perovskites have attracted a great deal of attention due to their variety of optoelectronic properties, their low cost, and their easier integration into devices with complex geometry, compared with microcrystalline, thin-film, or bulk metal halides. Here we present a novel one-step synthesis of organolead bromide perovskite nanocrystals based on pulsed-laser irradiation in a liquid environment (PLIL). Starting from a bulk CHNHPbBr crystal, our PLIL procedure does not involve the use of high-boiling-point polar solvents or templating agents, and runs at room temperature. The resulting nanoparticles are characterized by high crystallinity and are completely free of any microscopic product or organic coating layer. We also demonstrate the straightforward inclusion of laser-generated perovskite nanocrystals in a polymeric matrix to form a nanocomposite with single- and two-photon luminescence properties.

  1. Sub-band gap photo-enhanced secondary electron emission from high-purity single-crystal chemical-vapor-deposited diamond

    International Nuclear Information System (INIS)

    Yater, J. E.; Shaw, J. L.; Pate, B. B.; Feygelson, T. I.

    2016-01-01

    Secondary-electron-emission (SEE) current measured from high-purity, single-crystal (100) chemical-vapor-deposited diamond is found to increase when sub-band gap (3.06 eV) photons are incident on the hydrogenated surface. Although the light does not produce photoemission directly, the SEE current increases by more than a factor of 2 before saturating with increasing laser power. In energy distribution curves (EDCs), the emission peak shows a corresponding increase in intensity with increasing laser power. However, the emission-onset energy in the EDCs remains constant, indicating that the bands are pinned at the surface. On the other hand, changes are observed on the high-energy side of the distribution as the laser power increases, with a well-defined shoulder becoming more pronounced. From an analysis of this feature in the EDCs, it is deduced that upward band bending is present in the near-surface region during the SEE measurements and this band bending suppresses the SEE yield. However, sub-band gap photon illumination reduces the band bending and thereby increases the SEE current. Because the bands are pinned at the surface, we conclude that the changes in the band levels occur below the surface in the electron transport region. Sample heating produces similar effects as observed with sub-band gap photon illumination, namely, an increase in SEE current and a reduction in band bending. However, the upward band bending is not fully removed by either increasing laser power or temperature, and a minimum band bending of ∼0.8 eV is established in both cases. The sub-band gap photo-excitation mechanism is under further investigation, although it appears likely at present that defect or gap states play a role in the photo-enhanced SEE process. In the meantime, the study demonstrates the ability of visible light to modify the electronic properties of diamond and enhance the emission capabilities, which may have potential impact for diamond-based vacuum electron

  2. Growth of high purity semiconductor epitaxial layers by liquid phase ...

    Indian Academy of Sciences (India)

    Unknown

    semiconductor materials in high purity form by liquid phase epitaxy (LPE) technique. Various possible sources of impurities in such ... reference to the growth of GaAs layers. The technique of growing very high purity layers ... the inner walls of the gas lines and (e) the containers for storing, handling and cleaning of the mate-.

  3. Purity and Defect Characterization of Single-Wall Carbon Nanotubes Using Raman Spectroscopy

    Directory of Open Access Journals (Sweden)

    Yasumitsu Miyata

    2011-01-01

    Full Text Available We investigated the purity and defects of single-wall carbon nanotubes (SWCNTs produced by various synthetic methods including chemical vapor deposition, arc discharge, and laser ablation. The SWCNT samples were characterized using scanning electron microscopy (SEM, thermogravimetric analysis (TGA, and Raman spectroscopy. Quantitative analysis of SEM images suggested that the G-band Raman intensity serves as an index for the purity. By contrast, the intensity ratio of G-band to D-band (G/D ratio reflects both the purity and the defect density of SWCNTs. The combination of G-band intensity and G/D ratio is useful for a quick, nondestructive evaluation of the purity and defect density of a SWCNT sample.

  4. High purity in steels as a criterion for materials development

    International Nuclear Information System (INIS)

    Jacobi, H.

    1995-01-01

    This summarizing report discusses the materials and application prospects for higher purity in steels, which will make possible further advances in materials behaviour and workability. Improvements in purity and homogeneity permit in particular more rational production of thin foils and wire, one-piece shaping of complicated bodywork components and the drawing, wall-ironing and flanging of two-piece beverage cans. Welded designs in plant and mechanical engineering can be fabricated with less effort and less weight. Difficult component geometries and shaping processes can be more easily mastered. Steels with optimized fracture toughness can be exposed to more extreme loads at even lower temperatures: applications worthy of mention include offshore engineering and large-diameter linepipes for use in arctic regions and at great underwater depths. Liquefied-gas transport vessels can be made more resistant to brittle rupture. The bending fatigue strength and service-life of valve-spring and rolling-bearing steels can be significantly increased. High-purity surfaces on piston rods and cylinders guarantee reliability in hydraulic systems, and high-purity calendering rolls permit defect-free embossing of paper surfaces. (orig.)

  5. Activation analysis of high purity metals and application to study on physical properties

    International Nuclear Information System (INIS)

    Ueda, Yoshitake; Hashimoto, Eiji; Matsushita, Rokuji.

    1994-01-01

    In order to determine the true characteristics of matters, the utmost reduction of impurities is indispensable. By the heightening of the purity of aluminum, that of 99.9999% purity has been obtained, but efforts have been exerted to further heighten the purity. For the purpose, it is important to know the behavior of trace impurities during refining, and the quantitative research by neutron activation analysis for various impurities has been carried out. The research on the electron condition of trace impurity atoms in refined aluminum is also important. The band refining of high purity aluminum is explained. By repeating the refining 10 times, the sample of RRR exceeding 30000 was obtained. The impurities contributing to the resistivity are Sc, Ti, V and Cr. Based on the results, the heightening of aluminum purity was attempted by devising the new procedure. As for the electric properties of solute elements in high purity metals, those of transition elements and rare earth elements in aluminum are reported. As the result of measuring the remaining resistance, the sample having the RRR exceeding 45000 after the correction for size effect was done has been obtained. At present, the efforts toward further high purity are continued. (K.I.)

  6. Low-cost high purity production

    Science.gov (United States)

    Kapur, V. K.

    1978-01-01

    Economical process produces high-purity silicon crystals suitable for use in solar cells. Reaction is strongly exothermic and can be initiated at relatively low temperature, making it potentially suitable for development into low-cost commercial process. Important advantages include exothermic character and comparatively low process temperatures. These could lead to significant savings in equipment and energy costs.

  7. On the purity assessment of solid sodium borohydride

    Science.gov (United States)

    Botasini, Santiago; Méndez, Eduardo

    2012-01-01

    Since sodium borohydride has become extensively used as chemical hydrogen storage material in fuel cells, many techniques have been proposed to assess the purity of this substance. However, all of them are developed in aqueous media, where the reagent is unstable. In addition, its hygroscopic nature was difficults in any attempt to make precise quantifications. The present work compares three different methods, namely, voltammetric, titrimetric, and Fourier transformed infrared spectroscopy (FTIR) in order to assess the purity of sodium borohydride, using an expired and a new sodium borohydride samples as references. Our results show that only the FTIR measurements provide a simple and semi-quantitative means to assess the purity of sodium borohydride due to the fact that it is the only one that measures the sample in the solid state. A comparison between the experimental data and theoretical calculation reveals the identification of the absorption bands at 1437 cm-1 of sodium metaborate and 2291 cm-1 of sodium borohydride which represent a good fingerprint for the qualitative assessment of the sample quality.

  8. High mechanical Q-factor measurements on silicon bulk material

    Energy Technology Data Exchange (ETDEWEB)

    Schwarz, Christian; Nawrodt, Ronny; Heinert, Daniel; Schroeter, Anja; Neubert, Ralf; Thuerk, Matthias; Vodel, Wolfgang; Seidel, Paul [Institut fuer Festkoerperphysik, Helmholtzweg 5, D-07743 Jena (Germany); Tuennermann, Andreas [Institut fuer Angewandte Physik, Albert-Einstein-Strasse 15, D-07745 Jena (Germany)

    2008-07-01

    The direct observation of gravitational waves is one of the biggest challenges in science. Current detectors are limited by different kinds of noise. One of the fundamental noise sources is thermal noise arising from the optical components. One of the most promising attempts to reduce the thermal noise contribution in future detectors will be the use of high Q-factor materials at cryogenic temperatures. Silicon seems to be the most interesting material due to its excellent optical and thermal properties. We present high Q-factor measurements on bulk samples of high purity silicon in a temperature range from 5 to 300 K. The sample dimensions vary between 76.2 mm x 12..75 mm. The Q-factor exceeds 4.10{sup 8} at 6 K. The influence of the crystal orientation, doping and the sample preparation on the Q-factor is discussed.

  9. Perspectives of data-driven LPV modeling of high-purity distillation columns

    NARCIS (Netherlands)

    Bachnas, A.A.; Toth, R.; Mesbah, A.; Ludlage, J.H.A.

    2013-01-01

    Abstract—This paper investigates data-driven, Linear- Parameter-Varying (LPV) modeling of a high-purity distillation column. Two LPV modeling approaches are studied: a local approach, corresponding to the interpolation of Linear Time- Invariant (LTI) models identified at steady-state purity levels,

  10. Growth of Bulk Wide Bandgap Semiconductor Crystals and Their Potential Applications

    Science.gov (United States)

    Chen, Kuo-Tong; Shi, Detang; Morgan, S. H.; Collins, W. Eugene; Burger, Arnold

    1997-01-01

    Developments in bulk crystal growth research for electro-optical devices in the Center for Photonic Materials and Devices since its establishment have been reviewed. Purification processes and single crystal growth systems employing physical vapor transport and Bridgman methods were assembled and used to produce high purity and superior quality wide bandgap materials such as heavy metal halides and II-VI compound semiconductors. Comprehensive material characterization techniques have been employed to reveal the optical, electrical and thermodynamic properties of crystals, and the results were used to establish improved material processing procedures. Postgrowth treatments such as passivation, oxidation, chemical etching and metal contacting during the X-ray and gamma-ray device fabrication process have also been investigated and low noise threshold with improved energy resolution has been achieved.

  11. Template-free synthesis of sub-micrometric cobalt fibers with controlled shape and structure. Characterization and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Lakhdar, Allagui [Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Borges, Joao P. [i3N/CENIMAT, Department of Materials Science, Faculty of Science and Technology, Universidade NOVA de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Ben Haj Amara, Abdesslam [Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Dakhlaoui-Omrani, Amel, E-mail: dakhlaoui_amel@yahoo.fr [Department of Chemistry, Faculty of Sciences and Arts-Khulais, University of Jeddah, Khulais, P. O. Box 355, Postal Code 21921 (Saudi Arabia); Laboratoire de Physico-Chimie des Matériaux Minéraux et leurs Applications, Centre National des Recherches en Sciences des Matériaux, Technopôle de Bordj Cedria, BP 73, 8027 Soliman (Tunisia)

    2017-03-01

    Sub-micrometric Co fibers were prepared via a modified polyol process at 90 °C under an external magnetic field of about 550 Oe, using ethelyne glycol as solvent and hydrazine as reducing agent. The structure, the size and the morphology of the as-elaborated products were highly controlled through properly monitoring the synthesis parameters (amount of NaOH added, the amount of the reducing agent, precursor’ concentration and precursors mixing protocol). The XRD characterization confirmed the formation of pure cobalt powders with either hexagonal compact (hcp) or face-centered-cubic (fcc) structure depending on the concentration of the metal precursor and sodium hydroxide. The scanning electron microscopy observations of the powders shows sub-micrometric fibers with about 0.4–0.6 µm in diameter and a length that could reach 15 µm. Fibers prepared at high reducing ratio were constituted of flower-like spheres that coalesce in the direction of the applied magnetic field. For their high contact surface, these fibers offer new opportunities for catalysis applications. The hysteresis loop measurements show an enhancement of the Hc of the as-obtained fibers compared to their bulk counterparts and permit to confirm the relationship between the structure and the magnetic properties of the materials. - Highlights: • Template free synthesis of cobalt sub-micrometric fibers. • High control of the structure the structure, the size and the morphology of the products through properly monitoring the synthesis parameters. • cobalt sub-micrometric fibers with enhanced magnetic properties compared to bulk cobalt.

  12. Determination of radiochemical purity using gas chromatography

    International Nuclear Information System (INIS)

    1975-01-01

    The concepts of chromatography, gas chromatography, activity, radiochemical impurity are defined; the procedure of the application of gas chromatography for detecting radiochemical purity of substances is standardized. (E.F.)

  13. Synthesis and characterization of hydroxyapatite crystals: a review study on the analytical methods

    NARCIS (Netherlands)

    Koutsopoulos, S.

    2002-01-01

    For the synthesis of hydroxyapatite crystals from aqueous solutions three preparation methods were employed. From the experimental processes and the characterization of the crystals it was concluded that aging and precipitation kinetics are critical for the purity of the product and its

  14. Characterization of the crystalline quality of β-SiC formed by ion beam synthesis

    International Nuclear Information System (INIS)

    Intarasiri, S.; Hallen, A.; Kamwanna, T.; Yu, L.D.; Possnert, G.; Singkarat, S.

    2006-01-01

    The ion beam synthesis (IBS) technique is applied to form crystalline silicon carbide (SiC) for future optoelectronics applications. Carbon ions at 80 and 40 keV were implanted into (1 0 0) high-purity p-type silicon wafers at room temperature and 400 deg. C, respectively, to doses in excess of 10 17 ions/cm 2 . Subsequent thermal annealing of the implanted samples was performed in a vacuum furnace at temperatures of 800, 900 and 1000 deg. C, respectively. Elastic recoil detection analysis was used to investigate depth distributions of the implanted ions and infrared transmittance (IR) measurement was used to characterize formation of SiC in the implanted Si substrate. Complementary to IR, Raman scattering measurements were also carried out. Levels of the residual damage distribution of the samples annealed at different temperatures were compared with that of the as-implanted one by Rutherford backscattering spectrometry (RBS) in the channeling mode. The results show that C-ion implantation at the elevated temperature, followed by high-temperature annealing, enhances the synthesis of crystalline SiC

  15. A Generalizable Top-Down Nanostructuring Method of Bulk Oxides: Sequential Oxygen-Nitrogen Exchange Reaction.

    Science.gov (United States)

    Lee, Lanlee; Kang, Byungwuk; Han, Suyoung; Kim, Hee-Eun; Lee, Moo Dong; Bang, Jin Ho

    2018-05-27

    A thermal reaction route that induces grain fracture instead of grain growth is devised and developed as a top-down approach to prepare nanostructured oxides from bulk solids. This novel synthesis approach, referred to as the sequential oxygen-nitrogen exchange (SONE) reaction, exploits the reversible anion exchange between oxygen and nitrogen in oxides that is driven by a simple two-step thermal treatment in ammonia and air. Internal stress developed by significant structural rearrangement via the formation of (oxy)nitride and the creation of oxygen vacancies and their subsequent combination into nanopores transforms bulk solid oxides into nanostructured oxides. The SONE reaction can be applicable to most transition metal oxides, and when utilized in a lithium-ion battery, the produced nanostructured materials are superior to their bulk counterparts and even comparable to those produced by conventional bottom-up approaches. Given its simplicity and scalability, this synthesis method could open a new avenue to the development of high-performance nanostructured electrode materials that can meet the industrial demand of cost-effectiveness for mass production. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Bulk viscosity of molecular fluids

    Science.gov (United States)

    Jaeger, Frederike; Matar, Omar K.; Müller, Erich A.

    2018-05-01

    The bulk viscosity of molecular models of gases and liquids is determined by molecular simulations as a combination of a dilute gas contribution, arising due to the relaxation of internal degrees of freedom, and a configurational contribution, due to the presence of intermolecular interactions. The dilute gas contribution is evaluated using experimental data for the relaxation times of vibrational and rotational degrees of freedom. The configurational part is calculated using Green-Kubo relations for the fluctuations of the pressure tensor obtained from equilibrium microcanonical molecular dynamics simulations. As a benchmark, the Lennard-Jones fluid is studied. Both atomistic and coarse-grained force fields for water, CO2, and n-decane are considered and tested for their accuracy, and where possible, compared to experimental data. The dilute gas contribution to the bulk viscosity is seen to be significant only in the cases when intramolecular relaxation times are in the μs range, and for low vibrational wave numbers (<1000 cm-1); This explains the abnormally high values of bulk viscosity reported for CO2. In all other cases studied, the dilute gas contribution is negligible and the configurational contribution dominates the overall behavior. In particular, the configurational term is responsible for the enhancement of the bulk viscosity near the critical point.

  17. Stoichiometry and phase purity control of radio frequency magnetron sputter deposited Ba0.45Sr0.55TiO3 thin films for tunable devices

    Science.gov (United States)

    Alema, Fikadu; Reinholz, Aaron; Pokhodnya, Konstantin

    2013-11-01

    The systematic study of the oxygen partial pressure (OPP) and total chamber gas pressure (TGP) effects on the stoichiometry and crystal structure of rf sputtered Ba0.45Sr0.55TiO3 (BST) films and their phase purity allowed identifying close to optimal sputtering parameters for BST single phase polycrystalline film. The film with a Ba/Sr ratio equal to that of the source target and (Ba + Sr)/Ti ratio close to unity demonstrated the enhanced permittivity value of 553 and tunability of 69%. It was confirmed that the increase of TGP enables better match of the film and target stoichiometry. However, using O2/Ar ratio as a parameter should be utilized cautiously since exceeding a threshold OPP (2 mTorr in our case) may facilitate secondary phase formation. Relatively large dielectric losses were observed in both films sputtered at high (30 mTorr) and low (5 mTor) TGPs. The presence of oxygen vacancies was identified as a probable cause of losses, which is indirectly confirmed by the deviation of the film lattice constant from that of the bulk target.

  18. Solid-phase synthesis of an apoptosis-inducing tetrapeptide mimicking the Smac protein

    DEFF Research Database (Denmark)

    Le Quement, Sebastian Thordal; Ishøy, Mette; Petersen, Mette Terp

    2011-01-01

    An approach for the solid-phase synthesis of apoptosis-inducing Smac peptidomimetics is presented. Using a Rink linker strategy, tetrapeptides mimicking the N-4-terminal residue of the Smac protein [(N-Me)AVPF sequence] were synthesized on PEGA resin in excellent purities and yields. Following two...

  19. Synthesis and application of a new fluorous-tagged ammonia equivalent

    DEFF Research Database (Denmark)

    Nielsen, Simon Dalsgaard; Smith, Garrick; Begtrup, Mikael

    2010-01-01

    A novel fluorous-tagged ammonia equivalent has been developed. It is based on a nitrogen-oxygen bond, which can be cleaved in a traceless manner by a molybdenum complex or samarium diiodide. The application in the synthesis of ureas, amides, sulfonamides, and carbamates is described. The scope of...... of the fluorous N--O linker is exemplified by the synthesis of itopride, a drug used for the treatment of functional dyspepsia. Itopride was synthesized with the aid of fluorous purification methods and the product was isolated in good overall yield, with high purity....

  20. Animal Sex: Purity Education and the Naturalization of the Abstinence Agenda

    Science.gov (United States)

    Sethna, Christabelle

    2010-01-01

    An early-twentieth-century movement for social purity in England, Canada and the United States aimed to eradicate prostitution, the double standard of sexual morals and their dreaded corollary, the venereal diseases. Social purists suggested that "purity education" for children was the best pedagogical prophylaxis against such…

  1. Comparative analysis of oxidative synthesis of N-alkyl, N,N-dialkyl and N-cykloalkyl-O-isobutyl thioncarbamate

    Directory of Open Access Journals (Sweden)

    Sovrlić Milica Ž.

    2011-01-01

    Full Text Available A optimized synthesis of N-alkyl, N,N-dialkyl- and N-cycloalkyl-O-isobutyl thioncarbamates by aminolysis of sodium isobutylxanthogenic acid (NaiBXAc and primary, secondary and cycloalkyl amines was developed at laboratory scale and applied at semi-industrial level. Studies on dependence of N-n-propyl-O-isopropylthiocarbamate yield and purity with respect to reaction parameters: reaction time and molar ratio of n-propylamine and NaiBXAc, were performed. In such way, optimal reaction conditions for synthesis of N-alkyl, N,N-dialkyl- and N-cycloalkyl-O-isobutyl thioncarbamates, by aminolysis of NaiBXAc, were established. Also, comparative results of thioncarbamates synthesis starting from potassium isobutyl xanthate (KiBX and corresponding amines in presence of different oxidants: hydrogen peroxide, sodium hypochlorite and new oxidative agent potassium peroxodisulfate were evaluated. Synthesized compounds have been fully characterized by FTIR, 1H and 13C NMR and MS data, elemental analysis and purity have been determined by gas chromatographic method (GC. According to our knowledge, ten synthesized thioncarbamates are for the first time characterized. Synthesized compounds could be used as selective reagents for flotation of copper and zinc ores. The presented methods offer several benefits, namely, high product yields and purity, simple operation, mild reaction conditions without use of hazardous organic solvents, while some of them could be implemented on industrial scale production.

  2. Effect of Zr Purity and Oxygen Content on the Structure and Mechanical Properties of Melt-Spun and Suction-Cast Cu46Zr42Al7Y5 Alloy

    Directory of Open Access Journals (Sweden)

    Kozieł T.

    2016-06-01

    Full Text Available The effect of oxygen content in zirconium on the structure and mechanical properties of the Cu46Zr42Al7Y5 alloy, in the form of melt-spun ribbons and suction-cast rods, was investigated. Two types of Zr, rod and crystal bar of different nominal purities and oxygen contents, were used to synthesize the alloy by arc melting. Rapidly solidified ribbons were produced by melt spinning and their amorphous structures were confirmed by X-ray diffractometry (XRD and differential scanning calorimetry (DSC. Bulk samples in the form of rods were cast using a special water-cooled suction casting unit attached to the arc melting system. XRD and DSC studies proved the amorphous structure of the bulk alloy synthesized from low-oxygen Zr and partial crystallization of the same alloy for high-oxygen Zr. In both bulk samples, uniformly distributed crystalline particles were identified as yttrium oxides. Higher mean compressive strength of amorphous alloy was observed. The hardness of amorphous phase was close to 500 HV1 in both bulk alloys, while the hardness of crystalline dendritic areas, observed in the alloy synthesized from high oxygen Zr, was lower by about 50 HV1.

  3. Synthesis of Spongy-Like Mesoporous Hydroxyapatite from Raw Waste Eggshells for Enhanced Dissolution of Ibuprofen Loaded via Supercritical CO2

    Directory of Open Access Journals (Sweden)

    Abdul-Rauf Ibrahim

    2015-04-01

    Full Text Available The use of cheaper and recyclable biomaterials (like eggshells to synthesize high purity hydroxyapatite (HAp with better properties (small particle size, large surface area and pore volume for applications (in environmental remediation, bone augmentation and replacement, and drug delivery systems is vital since high-purity synthetic calcium sources are expensive. In this work, pure and mesoporous HAp nanopowder with large pore volume (1.4 cm3/g and surface area (284.1 m2/g was produced from raw eggshells at room temperature using a simple two-step procedure. The control of precursor droplets could stabilize the pH value of the reaction solution, because of the size of the needle (of the syringe pump used for precursor additions leading to production of HAp with high surface area and pore size. The as-produced HAp revealed high ibuprofen (as a model drug loading (1.38 g/g HAp, enhanced dissolution and controllable release of the drug via solute-saturated supercritical carbon dioxide.

  4. Synthesis of Spongy-Like Mesoporous Hydroxyapatite from Raw Waste Eggshells for Enhanced Dissolution of Ibuprofen Loaded via Supercritical CO2

    Science.gov (United States)

    Ibrahim, Abdul-Rauf; Li, Xiangyun; Zhou, Yulan; Huang, Yan; Chen, Wenwen; Wang, Hongtao; Li, Jun

    2015-01-01

    The use of cheaper and recyclable biomaterials (like eggshells) to synthesize high purity hydroxyapatite (HAp) with better properties (small particle size, large surface area and pore volume) for applications (in environmental remediation, bone augmentation and replacement, and drug delivery systems) is vital since high-purity synthetic calcium sources are expensive. In this work, pure and mesoporous HAp nanopowder with large pore volume (1.4 cm3/g) and surface area (284.1 m2/g) was produced from raw eggshells at room temperature using a simple two-step procedure. The control of precursor droplets could stabilize the pH value of the reaction solution, because of the size of the needle (of the syringe pump used for precursor additions) leading to production of HAp with high surface area and pore size. The as-produced HAp revealed high ibuprofen (as a model drug) loading (1.38 g/g HAp), enhanced dissolution and controllable release of the drug via solute-saturated supercritical carbon dioxide. PMID:25860950

  5. Bulk Restoration for SDN-Based Transport Network

    Directory of Open Access Journals (Sweden)

    Yang Zhao

    2016-01-01

    Full Text Available We propose a bulk restoration scheme for software defined networking- (SDN- based transport network. To enhance the network survivability and improve the throughput, we allow disrupted flows to be recovered synchronously in dynamic order. In addition backup paths are scheduled globally by applying the principles of load balance. We model the bulk restoration problem using a mixed integer linear programming (MILP formulation. Then, a heuristic algorithm is devised. The proposed algorithm is verified by simulation and the results are analyzed comparing with sequential restoration schemes.

  6. Glutamic Acid as Enhancer of Protein Synthesis Kinetics in Hepatocytes from Old Rats.

    Science.gov (United States)

    Brodsky, V Y; Malchenko, L A; Butorina, N N; Lazarev Konchenko, D S; Zvezdina, N D; Dubovaya, T K

    2017-08-01

    Dense cultures of hepatocytes from old rats (~2 years old, body weight 530-610 g) are different from similar cultures of hepatocytes from young rats by the low amplitude of protein synthesis rhythm. Addition of glutamic acid (0.2, 0.4, or 0.6 mg/ml) into the culture medium with hepatocytes of old rats resulted in increase in the oscillation amplitudes of the protein synthesis rhythm to the level of young rats. A similar action of glutamic acid on the protein synthesis kinetics was observed in vivo after feeding old rats with glutamic acid. Inhibition of metabotropic receptors of glutamic acid with α-methyl-4-carboxyphenylglycine (0.01 mg/ml) abolished the effect of glutamic acid. The amplitude of oscillation of the protein synthesis rhythm in a cell population characterizes synchronization of individual oscillations caused by direct cell-cell communications. Hence, glutamic acid, acting as a receptor-dependent transmitter, enhanced direct cell-cell communications of hepatocytes that were decreased with aging. As differentiated from other known membrane signaling factors (gangliosides, norepinephrine, serotonin, dopamine), glutamic acid can penetrate into the brain and thus influence the communications and protein synthesis kinetics that are disturbed with aging not only in hepatocytes, but also in neurons.

  7. Disgust sensitivity is primarily associated with purity-based moral judgments.

    Science.gov (United States)

    Wagemans, Fieke M A; Brandt, Mark J; Zeelenberg, Marcel

    2018-03-01

    Individual differences in disgust sensitivity are associated with a range of judgments and attitudes related to the moral domain. Some perspectives suggest that the association between disgust sensitivity and moral judgments will be equally strong across all moral domains (i.e., purity, authority, loyalty, care, fairness, and liberty). Other perspectives predict that disgust sensitivity is primarily associated with judgments of specific moral domains (e.g., primarily purity). However, no study has systematically tested if disgust sensitivity is associated with moral judgments of the purity domain specifically, more generally to moral judgments of the binding moral domains, or to moral judgments of all of the moral domains equally. Across 5 studies (total N = 1,104), we find consistent evidence for the notion that disgust sensitivity relates more strongly to moral condemnation of purity-based transgressions (meta-analytic r = .40) than to moral condemnation of transgressions of any of the other domains (range meta-analytic rs: .07-.27). Our findings are in line with predictions from Moral Foundations Theory, which predicts that personality characteristics like disgust sensitivity make people more sensitive to a certain set of moral issues. (PsycINFO Database Record (c) 2018 APA, all rights reserved).

  8. Monitoring the Microbial Purity of the Treated Water and Dialysate

    Directory of Open Access Journals (Sweden)

    Canaud Bernard

    2001-01-01

    Full Text Available Dialysate purity has become a major concern in recent years since it has been proven that contamination of dialysate is able to induce the production of proinflammatory cytokines, putatively implicated in the development of dialysis related pathology. In order to reduce this risk, it is advised to use ultrapure dialysate as a new standard of dialysate purity. Ultrapure dialysate preparation may be easily achieved with modern water treatment technologies. The reliable production of ultrapure dialysate requires several prerequisites: use of ultrapure water, use of clean electrolytic concentrates, implementation of ultrafilters in the dialysate pathway to ensure cold sterilization of the fresh dialysate. The regular supply with such high-grade purity dialysate relies on predefined microbiological monitoring of the chain using adequate and sensitive methods, and hygienic handling including frequent disinfection to reduce the level of contamination and to prevent biofilm formation. Reliability of this process requires compliance with a very strict quality assurance process. In this paper, we summarized the principles of the dialysate purity monitoring and the criteria used for surveillance in order to establish good antimicrobial practices in dialysis.

  9. Estrogen Enhances Matrix Synthesis in Nucleus Pulposus Cell through the Estrogen Receptor β-p38 MAPK Pathway

    Directory of Open Access Journals (Sweden)

    Pei Li

    2016-11-01

    Full Text Available Background/Aims: Matrix homeostasis within the disc nucleus pulposus (NP tissue is important for disc function. Increasing evidence indicates that sex hormone can influence the severity of disc degeneration. This study was aimed to study the role of 17β-estradiol (E2 in NP matrix synthesis and its underlying mechanism. Methods: Rat NP cells were cultured with (10-5, 10-7 and 10-9 M or without (control E2 for48 hours. The estrogen receptor (ER-β antagonist PHTPP and ERβ agonist ERB 041 were used to investigate the role mediated by ERβ. The p38 MAPK inhibitor SB203580 was used to investigate the role of p38 MAPK signaling pathway. Gene and protein expression of SOX9, aggrecan and collagen II, glycosaminoglycan (GAG content, and immunostaining assay for aggrecan and collagen II were analyzed to evaluate matrix production in rat NP cells. Results: E2 enhanced NP matrix synthesis in a concentration-dependent manner regarding gene and proetin expression of SOX9, aggrecan and collagen II, protein deposition of aggrecan and collagen II, and GAG content. Moreover, activation of p38 MAPK signaling pathway was increased with elevating E2 concentration. Further analysis indicated that ERB 041 and PHTPP could respectively enhance and suppress effects of E2 on matrix synthesis in NP cells, as well as activation of p38 MAPK pathway. Additionally, inhibition of p38 MAPK signaling pathway significantly abolished the effects of E2 on matrix synthesis. Conclusion: E2 can enhance matrix synthesis of NP cells and the ERβ/p38 MAPK pathway is involved in this regulatory process.

  10. The role of the chemical composition of monetite on the synthesis and properties of α-tricalcium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Duncan, Jo, E-mail: jo.duncan@abdn.ac.uk [Department of Chemistry, University of Aberdeen, Meston Walk, Aberdeen AB24 3UE (United Kingdom); MacDonald, James F., E-mail: J.F.MacDonald@warwick.ac.uk [Department of Physics, University of Warwick, Gibbet Hill Road, Coventry CV4 7AL (United Kingdom); Hanna, John V., E-mail: J.V.Hanna@warwick.ac.uk [Department of Physics, University of Warwick, Gibbet Hill Road, Coventry CV4 7AL (United Kingdom); Shirosaki, Yuki, E-mail: yukis@cc.okayama-u.ac.jp [Graduate School of Natural Science and Technology, Okayama University, 3-1-1 Tsushima, Kita-ku, Okayama 700-8530 (Japan); Hayakawa, Satoshi, E-mail: satoshi@cc.okayama-u.ac.jp [Graduate School of Natural Science and Technology, Okayama University, 3-1-1 Tsushima, Kita-ku, Okayama 700-8530 (Japan); Osaka, Akiyoshi, E-mail: a-osaka@cc.okayama-u.ac.jp [Graduate School of Natural Science and Technology, Okayama University, 3-1-1 Tsushima, Kita-ku, Okayama 700-8530 (Japan); Skakle, Janet M.S., E-mail: j.skakle@abdn.ac.uk [Department of Chemistry, University of Aberdeen, Meston Walk, Aberdeen AB24 3UE (United Kingdom); Gibson, Iain R., E-mail: i.r.gibson@abdn.ac.uk [Department of Chemistry, University of Aberdeen, Meston Walk, Aberdeen AB24 3UE (United Kingdom); School of Medical Sciences, Institute of Medical Sciences, University of Aberdeen, Foresterhill, Aberdeen AB25 2ZD (United Kingdom)

    2014-01-01

    There has been a resurgence of interest in alpha-tricalcium phosphate (α-TCP), with use in cements, polymer composites and in bi- and tri-phasic calcium phosphate bone grafts. The simplest and most established method for preparing α-TCP is the solid state reaction of monetite (CaHPO{sub 4}) and calcium carbonate at high temperatures, followed by quenching. In this study, the effect of the chemical composition of reagents used in the synthesis of α-TCP on the local structure of the final product is reported and findings previously reported pertaining to the phase composition and stability are also corroborated. Chemical impurities in the monetite reagents were identified and could be correlated to the calcium phosphate products formed; magnesium impurities favoured the formation of β-TCP, whereas single phase α-TCP was favoured when magnesium levels were low. Monetite synthesised in-house exhibited a high level of chemical purity; when this source was used to produce an α-TCP sample, the α-polymorph could be obtained by both quenching and by cooling to room temperature in the furnace at rates between 1 and 10 °C/min, thereby simplifying the synthesis process. It was only when impurities were minimised that the 12 phosphorus environments in the α-TCP structure could be resolved by {sup 31}P nuclear magnetic resonance; samples containing chemical impurity showed differing degrees of line-broadening. Reagent purity should therefore be considered a priority when synthesising/characterising the α-polymorph of TCP. - Highlights: • Most commercial sources of monetite contain impurities that affect synthesis of phase pure α-TCP. • Ratio of α:β-TCP polymorphs formed by solid state reaction is dependent on reactant chemical purity. • If reagents in α-TCP synthesis are chemically pure, quenching is not required to obtain α-polymorph. • 12 unique P sites in α-TCP were only fully realised by {sup 31}P NMR when chemically pure reagents are used.

  11. Enhanced bulk conductivity and bipolar transport in mixtures of MoOx and organic hole transport materials

    International Nuclear Information System (INIS)

    Tian, Baolin; Ban, Dayan; Aziz, Hany

    2013-01-01

    We study the conductivity of thin films of molybdenum oxide (MoO x ) mixed with an organic hole transport material, such as N,N′-bis(naphthalen-1-yl)-N,N′-bis (phenyl)benzidine or 4′,4″-tri(N-carbazolyl)triphenylamine, in lateral test devices. Contrary to previous reports, the conductivity of the mixture is found to exceed that of neat MoO x , exhibiting ∼ 5 orders of magnitude higher conductivity in comparison to the neat films. Studies also show that the mixing enhances both hole and electron transport. The higher conductivity may be attributed to a higher concentration of “free” carriers in the mixture, as a result of the formation of a charge transfer complex between the MoO x and the hole transport material. The findings shed light on the potential of hybrid composites of inorganic and organic materials in realizing enhanced conductivity. - Highlights: • We investigate the conductivity of mixtures of MoO x and hole transport material (HTM). • Materials are studied in lateral devices instead of conventional vertical devices. • Mixing MoO x with HTM brings > 5 orders of magnitude increase in bulk conductivity. • The mixture of MoO x and HTM enhances both hole and electron transport

  12. Gallium‐68 DOTATATE Production with Automated PET Radiopharmaceutical Synthesis System: A Three Year Experience

    Directory of Open Access Journals (Sweden)

    Alireza Aslani

    2014-10-01

    Full Text Available Objective(s: Gallium‐68 (Ga‐68 is an ideal research and hospital‐based PET radioisotope. Currently, the main form of Ga‐68 radiopharmaceutical that is being synthesised in‐house is Ga‐68 conjugated with DOTA based derivatives. The development of automated synthesis systems has increased the reliability, reproducibility and safety of radiopharmaceutical productions. Here we report on our three year, 500 syntheses experience with an automated system for Ga‐68 DOTATATE. Methods: The automated synthesis system we use is divided into three parts of a servomotor modules, b single use sterile synthesis cassettes and, c a computerized system that runs the modules. An audit trail is produced by the system as a requirement for GMP production. The required reagents and chemicals are made in‐. The Germanium breakthrough is determined on a weekly basis. Production yields for each synthesis are calculated to monitor the performance and efficiency of the synthesis. The quality of the final product is assessed after each synthesis by ITLC‐SG and HPLC methods. Results: A total of 500 Ga‐68 DOTATATE syntheses (>800 patient doses were performed between March 2011 and February 2014. The average generator yield was 81.3±0.2% for 2011, 76.7±0.4% for 2012 and 75.0±0.3% for 2013. Ga‐68 DOTATATE yields for 2011, 2012, and 2013 were 81.8±0.4%, 82.2±0.4% and 87.9±0.4%, respectively. These exceed the manufacturer’s expected value of approximately 70%. Germanium breakthrough averaged 8.6×10‐6% of total activity which is well below the recommended level of 0.001%. The average ITLC‐measured radiochemical purity was above 98.5% and the average HPLC‐measured radiochemical purity was above 99.5%. Although there were some system failures during synthesis, there were only eight occasions where the patient scans needed to be rescheduled. Conclusion: In our experience the automated synthesis system performs reliably with a relatively low incident

  13. Zeolite and wollastonite synthesis from rice hull ash

    International Nuclear Information System (INIS)

    Fernandes, Alberto de Andrade

    2006-01-01

    Rice hull ash (RHA) is a industry scrap rich in amorphous silica. A simple and low-energy cost method for the extraction of this silica was researched. A low level of impurity and high reactivity material was produced, which is appropriate for the synthesis of zeolites and wollastonite (CaSiO 3 ). The synthetic zeolites has not similar structures in nature, and they have been more and more valued in the market due to their purity and efficiency in specific applications like ion exchange, molecular sieve and catalysis areas. High purity wollastonite has many applications in manufacturing and agriculture. The mineral wollastonite can be formed in nature in different ways; it is generally accepted two forming processes, both encompassing limestone metamorphism (heat and pressure). In this work, a new process for the synthesis of zeolites and wollastonite from RHA colloidal silica was developed. Moreover, the process is aimed at lower energy costs, fewer stages and fewer reactants consume. In this work, zeolite A used in detergent and zeolite ZSM-5, employed in the petrochemical industry due to its high selectivity in catalytic reactions and its high thermo and acid stability, were synthesized. The first step of the wollastonite synthesis was studied, with the purpose of obtaining calcium hydrosilicate. Eleven different hydrosilicates occur in the system Ca(OH) 2 -SiO 2 -H 2 O, in the second step it was annealed to form the wollastonite phase. (author)

  14. Recovery of high-purity hydrogen from COG

    Energy Technology Data Exchange (ETDEWEB)

    Tsukiyama, Y

    1982-01-01

    A general account of the latest trends in the recovery of high-purity hydrogen from coke oven gas (COG), the article being based on both Japanese and overseas literature: 1) Deep-freeze separation: impurities are liquefied and removed. This method make use of the fact that hydrogen is hard to liquefy. 2) The PSA method: high-purity hydrogen is recovered by the adsorption of other constituents at high pressures. This technique makes use of the fact that the adsorption capacity of an adsorbent varies with the partial pressure of the substances being adsorbed. 3) Membrane separation: a permeation separation method that uses a functional polymer separation membrane, and that depends on the fact that hydrogen has a low molecular weight in comparison with the other constituents. (19 refs.) (In Japanese)

  15. Continuous microwave flow synthesis of mesoporous hydroxyapatite.

    Science.gov (United States)

    Akram, Muhammad; Alshemary, Ammar Z; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O; Hussain, Rafaqat

    2015-11-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Effect of reducing agents on low-temperature synthesis of nanostructured LiFePO4

    Science.gov (United States)

    Kulka, Andrzej; Walczak, Katarzyna; Zając, Wojciech; Molenda, Janina

    2017-09-01

    Simple co-precipitation synthesis procedure yielding nanometric LiFePO4 with enhanced electrochemical properties without any post-synthesis heat treatment is presented. XRD, SEM and TEM analysis of the obtained powders revealed platelet crystallites and well crystalized bulk structure. Effective way of decreasing amount of Fe3+ containing phases by addition of reducing agents (KI, (NH4)2S2O3, glucose and the atmosphere of 5%H2-95%Ar) during low-temperature (107 °C) synthesis is described. The traditional analytical chemistry methods or the Mӧssbauer spectroscopy methods revealed that utilization of selected reducing agents diminished Fe3+ concentration from 25 to 12 at%. The constructed cells with optimized LiFePO4 as a cathode material showed superior electrochemical performances, including high reversible capacity up to 162 mAh/g at C/10 current discharge rate, flat voltage plateau with a value close to 3.45 V vs. Li0/+.

  17. Improvement in fuel utilization in pressurized heavy water reactors due to increased heavy water purity

    International Nuclear Information System (INIS)

    Balakrishnan, M.R.

    1991-01-01

    This paper reports that in a pressurized heavy water reactor (PHWR), the reactivity of the reactor and, consequently, the discharge burnup of the fuel depend on the isotopic purity of the heavy water used in the reactor. The optimal purity of heavy water used in PHWRs, in turn, depends on the cost of fabricated uranium fuel and on the incremental cost incurred in improving the heavy water purity. The physics and economics aspects of the desirability of increasing the heavy water purity in PHWRs in India were first examined in 1978. With the cost data available at that time, it was found that improving the heavy water purity from 99.80% to 99.95% was economically attractive. The same problem is reinvestigated with current cost data. Even now, there is sufficient incentive to improve the isotopic purity of heavy water used in PHWRs. Admittedly, the economic advantage that can be derived depends on the cost of the fabricated fuel. Nevertheless, irrespective of the economics, there is also a fairly substantial saving in natural uranium. That the increase in the heavy water purity is to be maintained only in the low-pressure moderator system, and not in the high-pressure coolant system, makes the option of achieving higher fuel burnup with higher heavy water purity feasible

  18. Bulk synthesis of nanocrystalline urania powders by citrate gel-combustion method

    Science.gov (United States)

    Sanjay Kumar, D.; Ananthasivan, K.; Venkata Krishnan, R.; Amirthapandian, S.; Dasgupta, Arup

    2016-01-01

    Bulk quantities (60 g) of nanocrystalline (nc) free flowing urania powders with crystallite size ranging from 38 to 252 nm have been synthesized for the first time by the citrate gel combustion method. A systematic study of the influence of the fuel (citric acid) to oxidant (nitrate) ratio (R) on the characteristics of the urania powders has been carried out for the first time. Mixture with an "R" value of 0.25 exhibited a vigorous auto-ignition reaction. This reaction was investigated with Differential Scanning Calorimetry (DSC) and in-situ thermogravimetry coupled with differential thermal analysis and mass spectrometry (TG-DTA-MS). The bulk density, specific surface area, X-ray crystallite size, residual carbon and size distribution of particles of this powder were unique. Microscopic and microstructural investigation of selected samples revealed the presence of nanocrystals with irregular exfoliated morphology; their Electron Energy Loss Spectra testified the covalency of the U-O bond.

  19. Field percolation and high current density in 80/20 DyBa2Cu3O7-x/Dy2BaCuO5 bulk magnetically textured composite ceramics

    International Nuclear Information System (INIS)

    Cloots, R.; Liege Univ.; Dang, A.; Vanderbemden, P.; Vanderschueren, A.; Vanderschueren, H.W.; Bougrine, H.; Liege Univ.; Rulmont, A.; Ausloos, M.

    1996-01-01

    We measured the AC susceptibility of magnetically textured (123) 80%/211(20%) DyBaCuO composite in a special set-up in order to enhance the intergrain contribution. The synthesis process led to very clean weak links at grain boundaries. At the percolation threshold bulk shielding paths were such that the intergrain critical current density J C was above 10 5 A/cm 2 . The field dependence of J C was understood through an analytical form indicating a distribution of currents similar to the law of clusters at fracture/percolation thresholds. (orig.)

  20. Large enhancements of thermopower and carrier mobility in quantum dot engineered bulk semiconductors.

    Science.gov (United States)

    Liu, Yuanfeng; Sahoo, Pranati; Makongo, Julien P A; Zhou, Xiaoyuan; Kim, Sung-Joo; Chi, Hang; Uher, Ctirad; Pan, Xiaoqing; Poudeu, Pierre F P

    2013-05-22

    The thermopower (S) and electrical conductivity (σ) in conventional semiconductors are coupled adversely through the carriers' density (n) making it difficult to achieve meaningful simultaneous improvements in both electronic properties through doping and/or substitutional chemistry. Here, we demonstrate the effectiveness of coherently embedded full-Heusler (FH) quantum dots (QDs) in tailoring the density, mobility, and effective mass of charge carriers in the n-type Ti(0.1)Zr(0.9)NiSn half-Heusler matrix. We propose that the embedded FH QD forms a potential barrier at the interface with the matrix due to the offset of their conduction band minima. This potential barrier discriminates existing charge carriers from the conduction band of the matrix with respect to their relative energy leading to simultaneous large enhancements of the thermopower (up to 200%) and carrier mobility (up to 43%) of the resulting Ti(0.1)Zr(0.9)Ni(1+x)Sn nanocomposites. The improvement in S with increasing mole fraction of the FH-QDs arises from a drastic reduction (up to 250%) in the effective carrier density coupled with an increase in the carrier's effective mass (m*), whereas the surprising enhancement in the mobility (μ) is attributed to an increase in the carrier's relaxation time (τ). This strategy to manipulate the transport behavior of existing ensembles of charge carriers within a bulk semiconductor using QDs is very promising and could pave the way to a new generation of high figure of merit thermoelectric materials.

  1. On the chemical synthesis route to bulk-scale skutterudite materials

    DEFF Research Database (Denmark)

    Tafti, Mohsen Y.; Saleemi, Mohsin; Han, Li

    2016-01-01

    In this article an alternative high yield route for the synthesis of CoSb3-based unfilled skutterudites is presented. Using low-melting temperature salts of the constituents, melting and mixing them homogeneously in a hydrophobic liquid with postprocessing of the powders we achieve a more intimat......, compaction of the powders with SPS technique provided a safe route to maintaining the nanopowder size and achieving low thermal conductivity (3 W/mK). The proposed method can easily be scaled up and adopted by the industry.......In this article an alternative high yield route for the synthesis of CoSb3-based unfilled skutterudites is presented. Using low-melting temperature salts of the constituents, melting and mixing them homogeneously in a hydrophobic liquid with postprocessing of the powders we achieve a more...

  2. Synthesis and characterization of bulk and coatings of hydroxyapatite using methanol precursor

    International Nuclear Information System (INIS)

    Khongwar, Jasper K.; Kannan, K.R.; Buvaneswari, G.

    2008-01-01

    Hydroxyapatite, an important bioceramic was synthesized in the bulk form and developed as a coating by a sol-gel route using alcoholic precursor. The bioactive coating was developed on bio-inert α-alumina and yttria stabilized zirconia substrates. The apatite phase began to form after the heat treatment of the precursor at 500 deg. C for 10 min. The complete crystallization of the apatite was obtained at 800 deg. C heat treatment for 10 min. The phase composition of the bulk and the coatings was identified by FT-IR spectroscopic and powder X-ray diffraction (XRD) techniques. Surface morphology was determined by scanning electron microscopy. The study indicates different surface textures for the powder and for the coatings on α-alumina and yttria stabilized zirconia substrates

  3. Statistical distribution of the local purity in a large quantum system

    International Nuclear Information System (INIS)

    De Pasquale, A; Pascazio, S; Facchi, P; Giovannetti, V; Parisi, G; Scardicchio, A

    2012-01-01

    The local purity of large many-body quantum systems can be studied by following a statistical mechanical approach based on a random matrix model. Restricting the analysis to the case of global pure states, this method proved to be successful, and a full characterization of the statistical properties of the local purity was obtained by computing the partition function of the problem. Here we generalize these techniques to the case of global mixed states. In this context, by uniformly sampling the phase space of states with assigned global mixedness, we determine the exact expression of the first two moments of the local purity and a general expression for the moments of higher order. This generalizes previous results obtained for globally pure configurations. Furthermore, through the introduction of a partition function for a suitable canonical ensemble, we compute the approximate expression of the first moment of the marginal purity in the high-temperature regime. In the process, we establish a formal connection with the theory of quantum twirling maps that provides an alternative, possibly fruitful, way of performing the calculation. (paper)

  4. Opuntia ficus indica peel derived pectin mediated hydroxyapatite nanoparticles: Synthesis, spectral characterization, biological and antimicrobial activities

    Science.gov (United States)

    Gopi, D.; Kanimozhi, K.; Kavitha, L.

    2015-04-01

    In the present study, we have adapted a facile and efficient green route for the synthesis of HAP nanoparticles using pectin as a template which was extracted from the peel of prickly pear (Opuntia ficus indica) fruits. The concentration of pectin plays a major role in the behavior of crystallinity, purity, morphology as well as biological property of the as-synthesized HAP nanoparticles. The extracted pectin and the as-synthesized nanoparticles were characterized by various analytical techniques. The in vitro apatite formation on the surface of the as-synthesized nanoparticles in simulated body fluid (SBF) for various days showed an enhanced bioactivity. Also, the antimicrobial activity was investigated using various microorganisms. All the results revealed the formation of pure, low crystalline and discrete granular like HAP nanoparticles of size around 25 nm with enhanced biological and antimicrobial activities. Hence the as-synthesized nanoparticles can act as a better bone regenerating material in the field of biomedicine.

  5. Opuntia ficus indica peel derived pectin mediated hydroxyapatite nanoparticles: synthesis, spectral characterization, biological and antimicrobial activities.

    Science.gov (United States)

    Gopi, D; Kanimozhi, K; Kavitha, L

    2015-04-15

    In the present study, we have adapted a facile and efficient green route for the synthesis of HAP nanoparticles using pectin as a template which was extracted from the peel of prickly pear (Opuntia ficus indica) fruits. The concentration of pectin plays a major role in the behavior of crystallinity, purity, morphology as well as biological property of the as-synthesized HAP nanoparticles. The extracted pectin and the as-synthesized nanoparticles were characterized by various analytical techniques. The in vitro apatite formation on the surface of the as-synthesized nanoparticles in simulated body fluid (SBF) for various days showed an enhanced bioactivity. Also, the antimicrobial activity was investigated using various microorganisms. All the results revealed the formation of pure, low crystalline and discrete granular like HAP nanoparticles of size around 25 nm with enhanced biological and antimicrobial activities. Hence the as-synthesized nanoparticles can act as a better bone regenerating material in the field of biomedicine. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Synthesis, characterization and electrocatalytic properties of delafossite CuGaO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, Jahangeer [Department of Chemistry, University of Texas Rio Grande Valley, 1201 West University Drive, Edinburg, TX 78539 (United States); Department of Chemistry, College of Science, King Saud University, Riyadh 11451 (Saudi Arabia); Mao, Yuanbing, E-mail: yuanbing.mao@utrgv.edu [Department of Chemistry, University of Texas Rio Grande Valley, 1201 West University Drive, Edinburg, TX 78539 (United States)

    2016-10-15

    Delafossite CuGaO{sub 2} has been employed as photocatalysts for solar cells, but their electrocatalytic properties have not been extensively studied, especially no comparison among samples made by different synthesis routes. Herein, we first reported the successful synthesis of delafossite CuGaO{sub 2} particles with three different morphologies, i.e. nanocrystalline hexagons, sub-micron sized plates and micron–sized particles by a modified hydrothermal method at 190 °C for 60 h [1–3], a sono-chemical method followed by firing at 850 °C for 48 h, and a solid state route at 1150 °C, respectively. Morphology, composition and phase purity of the synthesized samples was confirmed by powder X-ray diffraction and Raman spectroscopic studies, and then their electrocatalytic performance as active and cost effective electrode materials to the oxygen and hydrogen evolution reactions in 0.5 M KOH electrolyte versus Ag/AgCl was investigated and compared under the same conditions for the first time. The nanocrystalline CuGaO{sub 2} hexagons show enhanced electrocatalytic activity than the counterpart sub-micron sized plates and micron-sized particles. - Graphical abstract: Representative delafossite CuGaO2 samples with sub-micron sized plate and nanocrystalline hexagon morphologies accompanying with chronoamperometric voltammograms for oxygen evolution reaction and hydrogen evolution reaction in 0.5 M KOH electrolyte after purged with N{sub 2} gas. - Highlights: • Delafossite CuGaO{sub 2} with three morphologies has been synthesized. • Phase purity of the synthesized samples was confirmed. • Comparison on their electrocatalytic properties was made for the first time. • Their use as electrodes for oxygen and hydrogen evolution reactions was evaluated. • Nanocrystalline CuGaO{sub 2} hexagons show highest electrocatalytic activity.

  7. Confined recrystallization of high-purity aluminium during accumulative roll bonding of aluminium laminates

    International Nuclear Information System (INIS)

    Chekhonin, Paul; Beausir, Benoît; Scharnweber, Juliane; Oertel, Carl-Georg; Hausöl, Tina; Höppel, Heinz Werner; Brokmeier, Heinz-Günter; Skrotzki, Werner

    2012-01-01

    Aluminium laminates consisting of high-purity aluminium and commercially pure aluminium have been produced by accumulative roll bonding (ARB) at ambient temperature for up to 10 cycles. To study the microstructure and texture development of the high-purity aluminium layers with regard to the shrinking layer thickness during ARB, microstructure and texture investigations were carried out by electron backscatter diffraction and neutron and X-ray diffraction, respectively. While the commercially pure aluminium layers develop an ultrafine-grained microstructure, partial discontinuous recrystallization occurs in the high-purity layers. The texture of the high-purity layers mainly consists of Cube and “Tilted Cube” (tilted with respect to the transverse direction) components. The experimental results are discussed with respect to confined recrystallization in the ARB aluminium laminates.

  8. Room temperature synthesis of porous SiO2 thin films by plasma enhanced chemical vapor deposition

    OpenAIRE

    Barranco Quero, Ángel; Cotrino Bautista, José; Yubero Valencia, Francisco; Espinós, J. P.; Rodríguez González-Elipe, Agustín

    2004-01-01

    Synthesis of porous SiO2 thin films in room temperature was carried out using plasma enhanced chemical vapor deposition (CVD) in an electron cyclotron resonance microwave reactor with a downstream configuration.The gas adsorption properties and the type of porosity of the SiO2 thin films were assessed by adsorption isotherms of toluene at room temperature.The method could also permit the tailoring synthesis of thin films when both composition and porosity can be simultaneously and independent...

  9. The Research about Preparation of High Purity Hexachlorodisilane

    Science.gov (United States)

    Wan, Ye; Zhao, Xiong; Yan, Dazhou; Zhao, Yu; Guo, Shuhu; Wang, Lei; Yang, Dian

    2017-12-01

    This article demonstrated a technology for producing high purity hexachlorodisilane what is one raw material of Semiconductor industry, which using the method of combination adsorption with rectification, whose material was from polysilicon residues of polysilicon company. This technology could remove most high boiling points chloro-silicane impurities and metal impurities effectively. The purity of Si2Cl6 produced by this technology can be up to 99.9%, the content of metal impurities can be low at 4ppb, which can meet the requirement of industy using completely. The technology extends the routes of Si2Cl6 in localization, having the advantages of simple process, continuous operation, and large capacity and so on.

  10. High-pressure torsion of aluminum with ultrahigh purity (99.9999%) and occurrence of inverse Hall-Petch relationship

    Energy Technology Data Exchange (ETDEWEB)

    Ito, Yuki [Department of Materials Science and Engineering, Kyushu University, Fukuoka 819-0395 (Japan); Edalati, Kaveh, E-mail: Kaveh.edalati@zaiko6.zaiko.kyushu-u.ac.jp [Department of Materials Science and Engineering, Kyushu University, Fukuoka 819-0395 (Japan); WPI, International Institute for Carbon-Neutral Energy Research (WPI-I2CNER), Kyushu University, Fukuoka 819-0395 (Japan); Horita, Zenji [Department of Materials Science and Engineering, Kyushu University, Fukuoka 819-0395 (Japan); WPI, International Institute for Carbon-Neutral Energy Research (WPI-I2CNER), Kyushu University, Fukuoka 819-0395 (Japan)

    2017-01-02

    Severe plastic deformation through the high-pressure torsion (HPT) method was applied to pure aluminum with a wide range of purity levels such as 99% (A1100), 99.5% (A1050), 99.99% (4NAl), 99.999% (5NAl) and 99.9999% (6NAl). The hardness of 6NAl decreased with straining and saturated to a level below the hardness level of the annealed sample. This softening behavior, which was similar to the behavior of metals with low melting temperatures such as indium, tin, lead and zinc, was not observed in 5NAl or less pure Al. It was found that the grain-size dependence of hardness became less significant with increasing the purity level, while the HPT-processed 6NAl followed an inverse Hall-Petch relationship. In 6NAl with large grain sizes, dislocations accumulated in the grains in the form of dislocation cells and enhanced the hardness, but when the grain size was small, the dislocations moved fast and disappeared in high-angle grain boundaries.

  11. Potential utility of eGFP-expressing NOG mice (NOG-EGFP as a high purity cancer sampling system

    Directory of Open Access Journals (Sweden)

    Shima Kentaro

    2012-06-01

    Full Text Available Abstract Purpose It is still technically difficult to collect high purity cancer cells from tumor tissues, which contain noncancerous cells. We hypothesized that xenograft models of NOG mice expressing enhanced green fluorescent protein (eGFP, referred to as NOG-EGFP mice, may be useful for obtaining such high purity cancer cells for detailed molecular and cellular analyses. Methods Pancreato-biliary cancer cell lines were implanted subcutaneously to compare the tumorigenicity between NOG-EGFP mice and nonobese diabetic/severe combined immunodeficiency (NOD/SCID mice. To obtain high purity cancer cells, the subcutaneous tumors were harvested from the mice and enzymatically dissociated into single-cell suspensions. Then, the cells were sorted by fluorescence-activated cell sorting (FACS for separation of the host cells and the cancer cells. Thereafter, the contamination rate of host cells in collected cancer cells was quantified by using FACS analysis. The viability of cancer cells after FACS sorting was evaluated by cell culture and subsequent subcutaneous reimplantation in NOG-EGFP mice. Results The tumorigenicity of NOG-EGFP mice was significantly better than that of NOD/SCID mice in all of the analyzed cell lines (p  Conclusions This method provides a novel cancer sampling system for molecular and cellular analysis with high accuracy and should contribute to the development of personalized medicine.

  12. A High-Purity Alumina for Use in Studies of Shock Loaded Samples

    Science.gov (United States)

    Lacina, David; Neel, Christopher

    2017-06-01

    We report the results of plate impact experiments on a potential new ``standard'' material, Coorstek Plasmapure-UC (99.9% purity) polycrystalline alumina, for use in non-conduction, impact environment, shock loading studies. This work was motivated by a desire to find a 99.9% purity alumina to replace the now unavailable Coors Vistal (99.9%) alumina, as it was hoped the Hugoniot elastic limit (HEL) of the new standard would match the 9-11 GPa value of Vistal. Shock response data, including the HEL, Hugoniot particle velocities, Hugoniot shock velocities, stress vs volume, and release wave speeds, was obtained up to 14 GPa. This data will be compared with Hugoniot curve data for other high purity alumina to contrast differences in the shock response, and is intended to be useful in impedance matching calculations. We will show that the HEL of Plasmapure-UC alumina is 5.5 GPa and speculate on causes for this lower than expected value. We will also explore why the elastic-plastic response for Plasmapure-UC alumina differs from what has been observed from other high purity alumina. The final result of this work is to recommend a well-characterized, lower purity alumina (Coorstek AD-995) as a potential new ``standard'' material.

  13. High-temperature mechanical properties of high-purity 70 mass% Cr-Fe alloy

    Energy Technology Data Exchange (ETDEWEB)

    Asahina, M.; Harima, N.; Takaki, S.; Abiko, K. [Tohoku Univ., Sendai (Japan). Inst. for Materials Research

    2002-01-16

    An ingot of high-purity 70 mass% Cr-Fe alloy was prepared by high-frequency induction melting in a high-purity argon atmosphere using a cold copper crucible. Its tensile properties such as hot-ductility and tensile strength were measured, and compared with the results for a high-purity 50 mass% Cr-Fe alloy, a high-purity 60 mass% Cr-Fe alloy and a Ni-based super-alloy. The formation of {sigma}-phase was also examined. The purity of a 70Cr-Fe alloy (70 mass% Cr-Fe alloy) ingot is more than 99.98 mass% and the total amount of gaseous impurities (C, N, O, S, H) in the 70Cr-Fe alloy is 69.9 mass ppm. The strength of the 70Cr-Fe alloy is higher than those of the 60Cr-Fe alloy and the 50Cr-Fe alloy at the temperatures between 293 and 1573 K, without decrease in ductility with increasing Cr content. The 70Cr-Fe alloy also possesses excellent high-temperature ductility. The {sigma}-phase was not observed after aging of 3.6 Ms at 873 K. Consequently, the 70Cr-Fe alloy is an excellent alloy as the base of super heat-resistant alloys. (orig.)

  14. Synthesis and application of a new fluorous-tagged ammonia equivalent.

    Science.gov (United States)

    Nielsen, Simon D; Smith, Garrick; Begtrup, Mikael; Kristensen, Jesper L

    2010-04-19

    A novel fluorous-tagged ammonia equivalent has been developed. It is based on a nitrogen-oxygen bond, which can be cleaved in a traceless manner by a molybdenum complex or samarium diiodide. The application in the synthesis of ureas, amides, sulfonamides, and carbamates is described. The scope of the fluorous N-O linker is exemplified by the synthesis of itopride, a drug used for the treatment of functional dyspepsia. Itopride was synthesized with the aid of fluorous purification methods and the product was isolated in good overall yield, with high purity. Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Enhancement of plasticity of Fe-based bulk metallic glass by Ni substitution for Fe

    Energy Technology Data Exchange (ETDEWEB)

    Guo, S.F. [State Key Laboratory of Material Processing and Die and Mould Technology, Huazhong University of Science and Technology, 430074 Wuhan (China); State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083 (China); Li, N.; Zhang, C. [State Key Laboratory of Material Processing and Die and Mould Technology, Huazhong University of Science and Technology, 430074 Wuhan (China); Liu, L., E-mail: sfguo2005@163.co [State Key Laboratory of Material Processing and Die and Mould Technology, Huazhong University of Science and Technology, 430074 Wuhan (China)

    2010-08-15

    Bulk metallic glasses (BMGs) (Fe{sub 1-x}Ni{sub x}){sub 71}Mo{sub 5}P{sub 12}C{sub 10}B{sub 2} (x = 0, 0.1 and 0.2) with a diameter of 3 mm were synthesized by copper mold casting. The effect of Ni substitution for Fe on the structure, thermal and mechanical properties has been studied by X-ray diffraction (XRD), differential scanning calorimetry (DSC) and compressive testing. It was found that the substitution of Ni for Fe enhances the glass forming ability, and improves the plasticity of Fe{sub 71}Mo{sub 5}P{sub 12}C{sub 10}B{sub 2} BMG as indicated by the increase in the plastic strain from 3.1% (x = 0) to 5.2% (x = 0.2). The improvement of the plasticity is discussed in term of the reduction of glass transition temperature and the supercooled liquid region due to the substitution of Ni for Fe.

  16. Growth and characterization of high-purity SiC single crystals

    Science.gov (United States)

    Augustine, G.; Balakrishna, V.; Brandt, C. D.

    2000-04-01

    High-purity SiC single crystals with diameter up to 50 mm have been grown by the physical vapor transport method. Finite element analysis was used for thermal modeling of the crystal growth cavity in order to reduce stress in the grown crystal. Crystals are grown in high-purity growth ambient using purified graphite furniture and high-purity SiC sublimation sources. Undoped crystals up to 50 mm in diameter with micropipe density less than 100 cm -2 have been grown using this method. These undoped crystals exhibit resistivities in the 10 3 Ω cm range and are p-type due to the presence of residual acceptor impurities, mainly boron. Semi-insulating SiC material is obtained by doping the crystal with vanadium. Vanadium has a deep donor level located near the middle of the band gap, which compensates the residual acceptor resulting in semi-insulating behavior.

  17. Method of determination of radiochemical purity of gallium-67 citrate injection

    International Nuclear Information System (INIS)

    Wang Quanji

    1985-01-01

    A simple method is used to compare the effect of five developing agents on the radiochemical purity of neutral products of 67 GaCit and on Rsub(f) values. Two preferable developing agents are recommended as suitable for the identification of 67 GaCit injection in its production. The effect of six pH values of different developing agents on radiochemical purity, Rsub(f) and chromatogram are compared for the neutral products. The results of the experiments show that the ascending paper chromatography with 1:2:4 pyridine/ethanol/water and 85:15 methanol/water is preferable for the determination of the radiochemical purity of 67 GaCit. The other developing agents also can be used if there are not any impurities except gallium radioisotopes

  18. Tuning for optimal performance in angle control, uniformity, and energy purity

    International Nuclear Information System (INIS)

    Liebert, Reuel B.; Olson, Joseph C.; Arevalo, Edwin A.; Downey, Daniel F.

    2005-01-01

    Advances in reducing the sizes of device structures and line widths place increasing demands on the accuracy of dopant placement and the control of dopant motion during activation anneals. Serial process high current ion implantation systems seek to produce beams in which the angles are controlled to high precision avoiding the angles introduced by conical structures used for holding wafers on spinning discs in batch systems. However, ion optical corrections and control of incident beam angle, dose uniformity, high throughput and energy purity often present apparently contradictory requirements in machine design. Data is presented to illustrate that tuning procedures can be used to simultaneously optimize angle purity in both x and y planes as well as control energy purity and dose uniformity

  19. Production of high purity radiothallium

    International Nuclear Information System (INIS)

    Lebowitz, E.; Greene, M.W.

    1976-01-01

    The method of producing high-purity thallium-201 for use as a myocardial scanning agent comprises the steps of irradiating a thallium target with protons to give the reaction 203 Tl(p,3n) 201 Pb, separating in ion exchange columns the lead from the thallium isotopes, permitting the lead to decay, and then purifying the thallium solution and converting the thallium present to thallous form in which it can be used

  20. [Research on determination of chemical purity of andrographolide by coulometric titration method].

    Science.gov (United States)

    Yang, Ning; Yang, Dezhi; Xu, Lishen; Lv, Yang

    2010-04-01

    The determination of chemical purity of andrographolide by coulometric titration method is studied in this paper. The coulometric titration was carried out in a mixture composed of 4 mol x L(-1) hydrochloric acid and 1 mol x L(-1) potassium bromide solution and 1 mol x L(-1) potassium nitrate solution (1:1). Bromine is electrogenerated at the anode and reacts with the andrographolide. The number of electrons involved in the eleatrode reaction is 2. Purity of andrographolide is 99.76% compared with 99.77% utilizing area normalization method by HPLC. The RSD are 0.33% and 0.02% respectively. The results from two methods are consistent, so the determination of chemical purity of andrographolide by coulometric titration method is scientific and feasible. The method is rapid, simple, convenient, sensitive and accurate. The reference material is not essential in the method. The method is suitable for determination of chemical purity of andrographolide.

  1. Human tonsillar IgE biosynthesis in vitro. I. Enhancement of IgE and IgG synthesis in the presence of pokeweed mitogen by T-cell irradiation

    International Nuclear Information System (INIS)

    Ohta, K.; Manzara, T.; Harbeck, R.J.; Kirkpatrick, C.H.

    1982-01-01

    A study of the events regulating human IgE biosynthesis in vitro was undertaken with tonsillar lymphocytes. IgG synthesis was also studied to evaluate the specificity of our observations. T-cell irradiation significantly enhanced synthesis of IgE by pokeweed mitogen (PWM)-stimulated B cells from 12 of 18 donors and IgG in all 18 donors. This enhancement was the result of de novo immunoglobulin synthesis, since the amount of IgE and IgG spontaneously released from lysed and lysed-and-cultured mononuclear cells was significantly less than that detected in the cell cultures, and the augmentation was completely ablated by the treatment of the cells with cycloheximide or mitomycin C. Enhancement was also dependent on the presence of PWM; T-cell irradiation did not enhance IgE synthesis in unstimulated cultures. Moreover, this enhancement was also observed in the co-cultures of B cells and allogeneic irradiated T cells. These observations suggest that radiosensitive T cells exert a suppressive activity that contributes to regulation of human IgE and IgG synthesis and that the suppressor function as well as the helper function can overcome allogeneic disparities

  2. Development of high purity niobium material for superconducting cavities

    International Nuclear Information System (INIS)

    Umezawa, Hiroaki; Takeuchi, Koichi; Sakita, Kohei; Suzuki, Takafusa; Saito, Kenji; Noguchi, Shuichi.

    1993-01-01

    For the superconducting niobium cavities, issues of thermal quench and field emission have to be solved to achieve a high field gradient (>25MV/m) for TESLA (TeV Energy Superconducting Linear Accelerator). In order to overcome the quench, upgrading of thermal conductivity of niobium material at the low temperature is very important. On the reduction of the field emission not only dust particles but also defect, impurity and inhomogeneity should be considered. Therefore development of high purity niobium material is very important to solve these issues. This paper describes the our latest R and D for high purity niobium material. (author)

  3. Defect structure of ultrafine MgB2 nanoparticles

    International Nuclear Information System (INIS)

    Bateni, Ali; Somer, Mehmet; Repp, Sergej; Erdem, Emre; Thomann, Ralf; Acar, Selçuk

    2014-01-01

    Defect structure of MgB 2 bulk and ultrafine particles, synthesized by solid state reaction route, have been investigated mainly by the aid of X-band electron paramagnetic resonance spectrometer. Two different amorphous Boron (B) precursors were used for the synthesis of MgB 2 , namely, boron 95 (purity 95%–97%, <1.5 μm) and nanoboron (purity >98.5%, <250 nm), which revealed bulk and nanosized MgB 2 , respectively. Scanning and transmission electron microscopy analysis demonstrate uniform and ultrafine morphology for nanosized MgB 2 in comparison with bulk MgB 2 . Powder X-ray diffraction data show that the concentration of the by-product MgO is significantly reduced when nanoboron is employed as precursor. It is observed that a significant average particle size reduction for MgB 2 can be achieved only by using B particles of micron or nano size. The origin and the role of defect centers were also investigated and the results proved that at nanoscale MgB 2 material contains Mg vacancies. Such vacancies influence the connectivity and the conductivity properties which are crucial for the superconductivity applications

  4. Disorder-induced transition from grain boundary to bulk dominated ionic diffusion in pyrochlores

    International Nuclear Information System (INIS)

    Perriot, Romain; Dholabhai, Pratik P.; Uberuaga, Blas P.

    2017-01-01

    In this paper, we use molecular dynamics simulations to investigate the role of grain boundaries (GBs) on ionic diffusion in pyrochlores, as a function of the GB type, chemistry of the compound, and level of cation disorder. We observe that the presence of GBs promotes oxygen transport in ordered and low-disordered systems, as the GBs are found to have a higher concentration of mobile carriers with higher mobilities than in the bulk. Thus, in ordered samples, the ionic diffusion is 2D, localized along the grain boundary. When cation disorder is introduced, bulk carriers begin to contribute to the overall diffusion, while the GB contribution is only slightly enhanced. In highly disordered samples, the diffusive behavior at the GBs is bulk-like, and the two contributions (bulk vs. GB) can no longer be distinguished. There is thus a transition from 2D/GB dominated oxygen diffusivity to 3D/bulk dominated diffusivity versus disorder in pyrochlores. Finally, these results provide new insights into the possibility of using internal interfaces to enhance ionic conductivity in nanostructured complex oxides.

  5. Bulk and track etching of PET studied by spectrophotometer

    International Nuclear Information System (INIS)

    Zhu, Z.Y.; Duan, J.L.; Maekawa, Y.; Koshikawa, H.; Yoshida, M.

    2004-01-01

    UV-VIS spectra of poly(ethylene terephthalate) (PET) solutions formed by etching PET in NaOH solution were analyzed with respect to the etching time. A linear relationship between absorptions centered at 4.45 and 5.11 eV with weight loss of PET in NaOH solution was established. The relation was applied to study the influence of UV light illumination on bulk etching of PET and to evaluate pore size of etched-through tracks. It is found that bulk etching of PET can be greatly enhanced by UV illumination in air in the wavelength range around 313 nm. A surface area of about 350 nm in thickness shows a 23 times increase in bulk-etching rate after illuminated for 6 h. The phenomenon is attributed to the oxygen-assisted photo-degradation through generating of new photo-unstable species. The enhancement in bulk etching was immediately reduced as the etching proceeds below the surface with an exponential decay constant of about 1.5 μm -1 . Etching of Xe ion irradiated PET films gives extra etching products with similar chemical structure as revealed by spectrophotometer measurements. Quantitative analysis of etching products from latent tracks implies that pores of about 14.6 nm in radius are formed after etching in 0.74 N NaOH at 40 deg. C for 35 min, which is in agreement with the conductometric measurement

  6. Sol-gel synthesis of hydroxyapatite

    International Nuclear Information System (INIS)

    Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P.

    2010-01-01

    Hydroxyapatite (HAp) has been established as the calcium phosphate based compound with most applications in the biological field. Among the numerous techniques for synthesis of HAp, the sol-gel processing route affords great control over purity and formed phases using low processing temperatures. In addition, the sol-gel approach offers an option for homogeneous HAp coating on metal substrates, as well as the ability to generate nanocrystalline powders. In this work, the sol-gel synthesis of HAp was investigated employing triethyl phosphate and calcium nitrate tetrahydrate as phosphorous and calcium precursors, respectively. The aging effect on phase composition and powder morphology of the final product was studied in terms of temperature and aging time. The powders were studied by using X-ray diffraction, Fourier transform infrared spectroscopy, particle size distribution by laser diffraction and scanning electron microscopy. (author)

  7. Distribution of oxides in a Zr-Cu-Ni-Al-Nb-Si bulk metallic glass

    Energy Technology Data Exchange (ETDEWEB)

    Heinrich, Jochen; Busch, Ralf [Chair of Metallic Materials, Saarland University, PO Box 151150, 66041 Saarbruecken (Germany); Mueller, Frank; Huefner, Stefan [Chair of Experimental Physics, Saarland University, PO Box 151150, 66041 Saarbruecken (Germany)

    2010-07-01

    The course of oxide presence with distance from the sample surface and bonding partner was studied for the bulk metallic glass with the nominal composition Zr{sub 57.9}Cu{sub 15.4}Ni{sub 12.7}Al{sub 10.2}Nb{sub 2.8}Si{sub 1} (at%) by X-ray photoelectron spectroscopy (XPS). Investigated specimens are taken from vacuum quench-cast rods subjected to oxidation at room temperature and atmosphere. Binding energies were determined in various depths using ion beam ablation of up to 100 nanometers. XPS spectra confirm oxidation primarily of the pure zirconium and aluminum constituents, all other peaks correspond to metallic bonds. While the surface area shows a passivating zirconia layer a few nanometers thick, oxygen is bonded predominantly with aluminum inside the bulk. Since the concentration of oxygen is a crucial factor in the crystallization behavior of bulk metallic glass forming liquids on basis of oxygen affine metals, so far only high purity materials were thought to be suitable. The findings in this study, however, are promising for alloys with industrial grade elements with sufficient glass forming ability. Comparisons of the alloy with differing oxygen content support the conclusion that aluminum acts as an appropriate scavenger for both adsorbed and large amounts of intrinsic oxygen in zirconium based amorphous metals.

  8. ROOM TEMPERATURE BULK SYNTHESIS OF SILVER NANOCABLES WRAPPED WITH POLYPYRROLE

    Science.gov (United States)

    Wet chemical synthesis of silver cables wrapped with polypyrrole is reported in aqueous media without use of any surfactant/capping agent and/or template. The method employs direct polymerization of pyrrole of an aqueous solution with AgNO3 as an oxidizing agent. The four probe c...

  9. Preparation of high purity nickel film from industrial effluent by the distribution of charge over microelectrodes using newly designed free electrolytic diffusion approach

    International Nuclear Information System (INIS)

    Ahmed, Sheikh Asrar; Qadir, Muhammad Abdul; Zafar, Muhammad Nadeem; Hussain, Ishtiaq; Tufail, Shahid; Rashid, Saima; Shah, Hamid Ali

    2008-01-01

    The present work deals with the development of a newly designed free electrolytic diffusion approach (the distribution of charge over microelectrodes) for the purification of metals and was successfully applied for the purification of nickel from the industrial effluent containing high proportion of nickel. Atomic absorption spectrophotometer (AAS) analyzed the purified nickel deposited on working microelectrodes. The results obtained show that the purity of nickel was enhanced from 95% to 99.9% with traces of copper etc. It was concluded that distribution of charge over the microcathodes at a rate of 50 cycles per second (cps) shows better results for the production of high purity (HP) nickel as compared to 25 cycles per second (cps)

  10. Preparation of high purity nickel film from industrial effluent by the distribution of charge over microelectrodes using newly designed free electrolytic diffusion approach

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, Sheikh Asrar; Qadir, Muhammad Abdul [Institute of Chemistry, University of the Punjab, Lahore, 54590 (Pakistan); Zafar, Muhammad Nadeem [Institute of Chemistry, University of the Punjab, Lahore, 54590 (Pakistan)], E-mail: znadeempk@yahoo.com; Hussain, Ishtiaq [Institute of Chemistry, University of the Punjab, Lahore, 54590 (Pakistan); Tufail, Shahid [PCSIR Laboratories Complex, Feroz pur Road, Lahore (Pakistan); Rashid, Saima; Shah, Hamid Ali [Institute of Chemistry, University of the Punjab, Lahore, 54590 (Pakistan)

    2008-09-15

    The present work deals with the development of a newly designed free electrolytic diffusion approach (the distribution of charge over microelectrodes) for the purification of metals and was successfully applied for the purification of nickel from the industrial effluent containing high proportion of nickel. Atomic absorption spectrophotometer (AAS) analyzed the purified nickel deposited on working microelectrodes. The results obtained show that the purity of nickel was enhanced from 95% to 99.9% with traces of copper etc. It was concluded that distribution of charge over the microcathodes at a rate of 50 cycles per second (cps) shows better results for the production of high purity (HP) nickel as compared to 25 cycles per second (cps)

  11. Synthesis of deuterium-labelled viloxazine. [Antidepressant

    Energy Technology Data Exchange (ETDEWEB)

    Mamada, Kumiko; Furuta, Takashi; Kasuya, Yasuji

    1988-06-01

    The synthesis of deuterium-labelled viloxazine with high isotopic purity is described. The synthetic procedures employ alkylation of 2-(benzyloxy)phenol with (/sup 2/H/sub 5/)ethyl iodide for the introduction of deuterium. Catalytic removal of the benzyl group of the deuterated product followed by reaction with epichlorohydrin afforded 1,2-epoxy-3-(2'-pentadeuteroethoxy-phenoxy)propane. Addition of 2-aminoethyl hydrogen sulphate to the epoxide and subsequent ring formation into a morpholine derivative produced the desired (/sup 2/H/sub 5/)viloxazine.

  12. Enhanced photoelectrochemical water splitting performance using morphology-controlled BiVO4 with W doping

    Directory of Open Access Journals (Sweden)

    Xin Zhao

    2017-12-01

    Full Text Available Nanostructures exhibit numerous merits to improve the efficiency in solar-to-energy conversion. These include shortened carrier collection pathways, an increased volume ratio between depletion layer and bulk, enhanced light capture due to multiple light scattering in nanostructures, and a high surface area for photochemical conversion reactions. In this study, we describe the synthesis of morphology-controlled W-doped BiVO4 by simply tuning the solvent ratio in precursor solutions. Planar and porous W-doped BiVO4 thin films were prepared and compared. The porous film, which exhibits increased surface area and enhanced light absorption, has displayed enhanced charge separation and interfacial charge injection. Our quantitative analysis showed an enhancement of about 50% of the photoelectrochemical performance for the porous structure compared to the planar structure. This enhancement is attributed to improved light absorption (13% increase, charge separation (14% increase, and interfacial charge injection (20% increase.

  13. Epitaxial growth of high purity cubic InN films on MgO substrates using HfN buffer layers by pulsed laser deposition

    International Nuclear Information System (INIS)

    Ohba, R.; Ohta, J.; Shimomoto, K.; Fujii, T.; Okamoto, K.; Aoyama, A.; Nakano, T.; Kobayashi, A.; Fujioka, H.; Oshima, M.

    2009-01-01

    Cubic InN films have been grown on MgO substrates with HfN buffer layers by pulsed laser deposition (PLD). It has been found that the use of HfN (100) buffer layers allows us to grow cubic InN (100) films with an in-plane epitaxial relationship of [001] InN //[001] HfN //[001] MgO . X-ray diffraction and electron back-scattered diffraction measurements have revealed that the phase purity of the cubic InN films was as high as 99%, which can be attributed to the use of HfN buffer layers and the enhanced surface migration of the film precursors by the use of PLD. - Graphical abstract: Cubic InN films have been grown on MgO substrates with HfN buffer layers by pulsed laser deposition (PLD). It has been revealed that the phase purity of the cubic InN films was as high as 99 %, which can be attributed to the use of HfN buffer layers and the enhanced surface migration of the film precursors by the use of PLD.

  14. High-Throughput Synthesis and Characterization of Eu Doped Ba xSr2- xSiO4 Thin Film Phosphors.

    Science.gov (United States)

    Frost, Sara; Guérin, Samuel; Hayden, Brian E; Soulié, Jean-Philippe; Vian, Chris

    2018-06-20

    High-throughput techniques have been employed for the synthesis and characterization of thin film phosphors of Eu-doped Ba x Sr 2- x SiO 4 . Direct synthesis from evaporation of the constituent elements under a flux of atomic oxygen on a sapphire substrate at 850 °C was used to directly produce thin film libraries (415 nm thickness) of the crystalline orthosilicate phase with the desired compositional variation (0.24 > x > 1.86). The orthosilicate phase could be synthesized as a pure, or predominantly pure, phase. Annealing the as synthesized library in a reducing atmosphere resulted in the reduction of the Eu while retaining the orthosilicate phase, and resulted in a materials thin film library where fluorescence excited by blue light (450 nm) was observable by the naked eye. Parallel screening of the fluorescence from the combinatorial libraries of Eu doped Ba x Sr 2- x SiO 4 has been implemented by imaging the fluorescent radiation over the library using a monochrome digital camera using a series of color filters. Informatics tools have been developed to allow the 1931 CIE color coordinates and the relative quantum efficiencies of the materials library to be rapidly assessed and mapped against composition, crystal structure and phase purity. The range of compositions gave values of CIE x between 0.17 and 0.52 and CIE y between 0.48 and 0.69 with relative efficiencies in the range 2.0 × 10 -4 -7.6 × 10 -4 . Good agreement was obtained between the thin film phosphors and the fluorescence characteristics of a number of corresponding bulk phosphor powders. The thermal quenching of fluorescence in the thin film libraries was also measured in the temperature range 25-130 °C: The phase purity of the thin film was found to significantly influence both the relative quantum efficiency and the thermal quenching of the fluorescence.

  15. Purity-activity relationships of natural products: the case of anti-TB active ursolic acid.

    Science.gov (United States)

    Jaki, Birgit U; Franzblau, Scott G; Chadwick, Lucas R; Lankin, David C; Zhang, Fangqiu; Wang, Yuehong; Pauli, Guido F

    2008-10-01

    The present study explores the variability of biological responses from the perspective of sample purity and introduces the concept of purity-activity relationships (PARs) in natural product research. The abundant plant triterpene ursolic acid (1) was selected as an exemplary natural product due to the overwhelming number yet inconsistent nature of its approximate 120 reported biological activities, which include anti-TB potential. Nine different samples of ursolic acid with purity certifications were obtained, and their purity was independently assessed by means of quantitative 1H NMR (qHNMR). Biological evaluation consisted of determining MICs against two strains of virulent Mycobacterium tuberculosis and IC50 values in Vero cells. Ab initio structure elucidation provided unequivocal structural confirmation and included an extensive 1H NMR spin system analysis, determination of nearly all J couplings and the complete NOE pattern, and led to the revision of earlier reports. As a net result, a sigmoid PAR profile of 1 was obtained, demonstrating the inverse correlation of purity and anti-TB bioactivity. The results imply that synergistic effects of 1 and its varying impurities are the likely cause of previously reported antimycobacterial potential. Generating PARs is a powerful extension of the routinely performed quantitative correlation of structure and activity ([Q]SAR). Advanced by the use of primary analytical methods such as qHNMR, PARs enable the elucidation of cases like 1 when increasing purity voids biological activity. This underlines the potential of PARs as a tool in drug discovery and synergy research and accentuates the need to routinely combine biological testing with purity assessment.

  16. Differential behaviour of combustion and gasification fly ash from Puertollano Power Plants (Spain) for the synthesis of zeolites and silica extraction

    International Nuclear Information System (INIS)

    Font, O.; Moreno, N.; Diez, S.; Querol, X.; Lopez-Soler, A.; Coca, P.; Garcia Pena, F.

    2009-01-01

    Coal gasification (IGCC) and pulverised coal combustion (PCC) fly ashes (FAs), obtained from two power plants fed with the carboniferous bituminous coal from Puertollano (Spain), were characterised and used as raw materials for zeolite synthesis by direct conversion (DC) and by alkaline fusion (Fu), and SiO 2 extraction (Si-Ex) at laboratory scale. The Puertollano FAs are characterised by a high SiO 2 content (59%) with respect to EU coal FAs. High zeolite synthesis yields were obtained from both FAs by using conventional alkaline activation. However, the Si extraction yields were very different. The results of the zeolite synthesis from the Si-bearing extracts from both FAs demonstrated that high purity zeolites with high cation exchange capacity (CEC, between 4.3 and 5.3 meq/g) can be produced. The solid residue arising from Si-Ex is also a relatively high NaP1 zeolite product (CEC 2.4-2.7 meq/g) equivalent to the DC products. The zeolitic materials synthesised from both FAs by Fu showed an intermediate (between the high purity zeolites and the DC products) zeolite content with CEC values from 3.4 to 3.7 meq/g. Low leachable metal contents were obtained from high purity A and X zeolites and zeolite material synthesised by Fu for PCC FA.

  17. Enhanced Mechanical Properties of MgZnCa Bulk Metallic Glass Composites with Ti-Particle Dispersion

    Directory of Open Access Journals (Sweden)

    Pei Chun Wong

    2016-05-01

    Full Text Available Rod samples of Mg60Zn35Ca5 bulk metallic glass composites (BMGCs dispersed with Ti particles have been successfully fabricated via injection casting. The glass forming ability (GFA and the mechanical properties of these Mg-based BMGCs have been systematically investigated as a function of the volume fraction (Vf of Ti particles. The results showed that the compressive ductility increased with Vf. The mechanical performance of these BMGCs, with up to 5.4% compressive failure strain and 1187 MPa fracture strength at room temperature, can be obtained for the Mg-based BMGCs with 50 vol % Ti particles, suggesting that these dispersed Ti particles can absorb the energy of the crack propagations and can induce branches of the primary shear band into multiple secondary shear bands. It follows that further propagation of the shear band is blocked, enhancing the overall plasticity.

  18. Characterisation of two AGATA asymmetric high purity germanium capsules

    International Nuclear Information System (INIS)

    Colosimo, S.J.; Moon, S.; Boston, A.J.; Boston, H.C.; Cresswell, J.R.; Harkness-Brennan, L.; Judson, D.S.; Lazarus, I.H.; Nolan, P.J.; Simpson, J.; Unsworth, C.

    2015-01-01

    The AGATA spectrometer is an array of highly segmented high purity germanium detectors. The spectrometer uses pulse shape analysis in order to track Compton scattered γ-rays to increase the efficiency of nuclear spectroscopy studies. The characterisation of two high purity germanium detector capsules for AGATA of the same A-type has been performed at the University of Liverpool. This work will examine the uniformity of performance of the two capsules, including a comparison of the resolution and efficiency as well as a study of charge collection. The performance of the capsules shows good agreement, which is essential for the efficient operation of the γ-ray tracking array

  19. Characterisation of two AGATA asymmetric high purity germanium capsules

    Energy Technology Data Exchange (ETDEWEB)

    Colosimo, S.J., E-mail: sjc@ns.ph.liv.ac.uk [Department of Physics, Oliver Lodge Laboratory, University of Liverpool, Liverpool L69 7ZE (United Kingdom); Moon, S.; Boston, A.J.; Boston, H.C.; Cresswell, J.R.; Harkness-Brennan, L.; Judson, D.S. [Department of Physics, Oliver Lodge Laboratory, University of Liverpool, Liverpool L69 7ZE (United Kingdom); Lazarus, I.H. [STFC Daresbury, Daresbury, Warrington WA4 4AD (United Kingdom); Nolan, P.J. [Department of Physics, Oliver Lodge Laboratory, University of Liverpool, Liverpool L69 7ZE (United Kingdom); Simpson, J. [STFC Daresbury, Daresbury, Warrington WA4 4AD (United Kingdom); Unsworth, C. [Department of Physics, Oliver Lodge Laboratory, University of Liverpool, Liverpool L69 7ZE (United Kingdom)

    2015-02-11

    The AGATA spectrometer is an array of highly segmented high purity germanium detectors. The spectrometer uses pulse shape analysis in order to track Compton scattered γ-rays to increase the efficiency of nuclear spectroscopy studies. The characterisation of two high purity germanium detector capsules for AGATA of the same A-type has been performed at the University of Liverpool. This work will examine the uniformity of performance of the two capsules, including a comparison of the resolution and efficiency as well as a study of charge collection. The performance of the capsules shows good agreement, which is essential for the efficient operation of the γ-ray tracking array.

  20. The dependence of Pi2 waveforms on periodic velocity enhancements within bursty bulk flows

    Directory of Open Access Journals (Sweden)

    K. R. Murphy

    2011-03-01

    Full Text Available Pi2s are a category of Ultra Low Frequency (ULF waves associated with the onset of magnetic substorms. Recent work has suggested that the deceleration of bulk plasma flows in the central plasmasheet, known as bursty bulk flows (BBFs, are able to directly-drive Pi2 oscillations. Some of these studies have further shown evidence that there is a one-to-one correlation between Pi2 magnetic waveforms observed on the ground and periodic peaks in flow velocity within the BBF, known as flow bursts. Utilising a favourable conjunction between the Geotail spacecraft and the Canadian Array for Real-time Investigations of Magnetic Activity (CARISMA magnetometer array on 31 May 1998, we examine the causality of the link between BBF flow bursts and Pi2 waveforms. Using a series of analytical tests in both the time and frequency domains, we find that while the Pi2 and BBF waveforms are very similar, the ground response for this event occurs prior to the observed flow enhancements in the magnetotail. We conclude that during this specific case study the temporal variations of the flow bursts within the BBF are not directly-driving the observed ground-based Pi2 waveforms, despite the fact that a visual inspection of both time-series might initially suggest that there is a causal relationship. We postulate that rather than there being a direct causal relation, the similar waveforms observed in both Pi2s and BBFs may result from temporal variations in a common source for both the BBFs and the Pi2s, such as magnetic reconnection in the tail, this source modulating both the Pi2 and BBF at the same frequency.

  1. Fused salt processing of impure plutonium dioxide to high-purity plutonium metal

    International Nuclear Information System (INIS)

    Mullins, L.J.; Christensen, D.C.; Babcock, B.R.

    1982-01-01

    A process for converting impure plutonium dioxide (approx. 96% pure) to high-purity plutonium metal (>99.9%) was developed. The process consists of reducing the oxide to an impure plutonium metal intermediate with calcium metal in molten calcium chloride. The impure intermediate metal is cast into an anode and electrorefined to produce high-purity plutonium metal. The oxide reduction step is being done now on a 0.6-kg scale with the resulting yield being >99.5%. The electrorefining is being done on a 4.0-kg scale with the resulting yield being 80 to 85%. The purity of the product, which averages 99.98%, is essentially insensitive to the purity of the feed metal. The yield, however, is directly dependent on the chemical composition of the feed. To date, approximately 250 kg of impure oxide has been converted to pure metal by this processing sequence. The availability of impure plutonium dioxide, together with the need for pure plutonium metal, makes this sequence a valuable plutonium processing tool

  2. Effect of Aluminum Purity on the Pore Formation of Porous Anodic Alumina

    International Nuclear Information System (INIS)

    Kim, Byeol; Lee, Jin Seok

    2014-01-01

    Anodic alumina oxide (AAO), a self-ordered hexagonal array, has various applications in nanofabrication such as the fabrication of nanotemplates and other nanostructures. In order to obtain highly ordered porous alumina membranes, a two-step anodization or prepatterning of aluminum are mainly conducted with straight electric field. Electric field is the main driving force for pore growth during anodization. However, impurities in aluminum can disturb the direction of the electric field. To confirm this, we anodized two different aluminum foil samples with high purity (99.999%) and relatively low purity (99.8%), and compared the differences in the surface morphologies of the respective aluminum oxide membranes produced in different electric fields. Branched pores observed in porous alumina surface which was anodized in low-purity aluminum and the size; dimensions of the pores were found to be usually smaller than those obtained from high-purity aluminum. Moreover, anodization at high voltage proceeds to a significant level of conversion because of the high speed of the directional electric field. Consequently, anodic alumina membrane of a specific morphology, i. e., meshed pore, was produced

  3. Effect of Aluminum Purity on the Pore Formation of Porous Anodic Alumina

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Byeol; Lee, Jin Seok [Sookmyung Women' s Univ., Seoul (Korea, Republic of)

    2014-02-15

    Anodic alumina oxide (AAO), a self-ordered hexagonal array, has various applications in nanofabrication such as the fabrication of nanotemplates and other nanostructures. In order to obtain highly ordered porous alumina membranes, a two-step anodization or prepatterning of aluminum are mainly conducted with straight electric field. Electric field is the main driving force for pore growth during anodization. However, impurities in aluminum can disturb the direction of the electric field. To confirm this, we anodized two different aluminum foil samples with high purity (99.999%) and relatively low purity (99.8%), and compared the differences in the surface morphologies of the respective aluminum oxide membranes produced in different electric fields. Branched pores observed in porous alumina surface which was anodized in low-purity aluminum and the size; dimensions of the pores were found to be usually smaller than those obtained from high-purity aluminum. Moreover, anodization at high voltage proceeds to a significant level of conversion because of the high speed of the directional electric field. Consequently, anodic alumina membrane of a specific morphology, i. e., meshed pore, was produced.

  4. Materials processing and machine applications of bulk HTS

    Science.gov (United States)

    Miki, M.; Felder, B.; Tsuzuki, K.; Xu, Y.; Deng, Z.; Izumi, M.; Hayakawa, H.; Morita, M.; Teshima, H.

    2010-12-01

    We report a refrigeration system for rotating machines associated with the enhancement of the trapped magnetic flux of bulk high-temperature superconductor (HTS) field poles. A novel cryogenic system was designed and fabricated. It is composed of a low-loss rotary joint connecting the rotor and a closed-cycle thermosiphon under a GM cryocooler using a refrigerant. Condensed neon gas was adopted as a suitable cryogen for the operation of HTS rotating machines with field poles composed of RE-Ba-Cu-O family materials, where RE is a rare-earth metal. Regarding the materials processing of the bulks HTS, thanks to the addition of magnetic particles to GdBa2Cu3O7 - d (Gd123) bulk superconductors an increase of more than 20% in the trapped magnetic flux density was achieved at liquid nitrogen temperature. Field-pole Gd123 bulks up to 46 mm in diameter were synthesized with the addition of Fe-B alloy magnetic particles and assembled into the synchronous machine rotor to be tested. Successful cooling of the magnetized rotor field poles down to 35 K and low-output-power rotating operation was achieved up to 720 rpm in the test machine with eight field-pole bulks. The present results show a substantial basis for making a prototype system of rotating machinery of applied HTS bulks.

  5. Materials processing and machine applications of bulk HTS

    Energy Technology Data Exchange (ETDEWEB)

    Miki, M; Felder, B; Tsuzuki, K; Xu, Y; Deng, Z; Izumi, M [Department of Marine Electronics and Mechanical Engineering, Tokyo University of Marine Science and Technology, 2-1-6, Etchu-jima, Koto-ku, Tokyo 135-8533 (Japan); Hayakawa, H [Kitano Seiki Co. Ltd, 7-17-3, Chuo, Ohta-ku, Tokyo 143-0024 (Japan); Morita, M; Teshima, H, E-mail: d082025@kaiyodai.ac.j [Nippon Steel Co. Ltd, 20-1, Shintomi, Huttsu-shi, Chiba 293-8511 (Japan)

    2010-12-15

    We report a refrigeration system for rotating machines associated with the enhancement of the trapped magnetic flux of bulk high-temperature superconductor (HTS) field poles. A novel cryogenic system was designed and fabricated. It is composed of a low-loss rotary joint connecting the rotor and a closed-cycle thermosiphon under a GM cryocooler using a refrigerant. Condensed neon gas was adopted as a suitable cryogen for the operation of HTS rotating machines with field poles composed of RE-Ba-Cu-O family materials, where RE is a rare-earth metal. Regarding the materials processing of the bulks HTS, thanks to the addition of magnetic particles to GdBa{sub 2}Cu{sub 3}O{sub 7-d} (Gd123) bulk superconductors an increase of more than 20% in the trapped magnetic flux density was achieved at liquid nitrogen temperature. Field-pole Gd123 bulks up to 46 mm in diameter were synthesized with the addition of Fe-B alloy magnetic particles and assembled into the synchronous machine rotor to be tested. Successful cooling of the magnetized rotor field poles down to 35 K and low-output-power rotating operation was achieved up to 720 rpm in the test machine with eight field-pole bulks. The present results show a substantial basis for making a prototype system of rotating machinery of applied HTS bulks.

  6. Hydrogen adsorption-mediated synthesis of concave Pt nanocubes and their enhanced electrocatalytic activity

    Science.gov (United States)

    Lu, Bang-An; Du, Jia-Huan; Sheng, Tian; Tian, Na; Xiao, Jing; Liu, Li; Xu, Bin-Bin; Zhou, Zhi-You; Sun, Shi-Gang

    2016-06-01

    Concave nanocubes are enclosed by high-index facets and have negative curvature; they are expected to have enhanced reactivity, as compared to nanocubes with flat surfaces. Herein, we propose and demonstrate a new strategy for the synthesis of concave Pt nanocubes with {hk0} high-index facets, by using a hydrogen adsorption-mediated electrochemical square-wave potential method. It was found that Pt atoms prefer to deposit on edge sites rather than terrace sites on Pt surfaces with intensive hydrogen adsorption, resulting in the formation of concave structures. The as-prepared concave Pt nanocubes exhibit enhanced catalytic activity and stability towards oxidation of ethanol and formic acid in acidic solutions, compared to commercial Pt/C catalysts.Concave nanocubes are enclosed by high-index facets and have negative curvature; they are expected to have enhanced reactivity, as compared to nanocubes with flat surfaces. Herein, we propose and demonstrate a new strategy for the synthesis of concave Pt nanocubes with {hk0} high-index facets, by using a hydrogen adsorption-mediated electrochemical square-wave potential method. It was found that Pt atoms prefer to deposit on edge sites rather than terrace sites on Pt surfaces with intensive hydrogen adsorption, resulting in the formation of concave structures. The as-prepared concave Pt nanocubes exhibit enhanced catalytic activity and stability towards oxidation of ethanol and formic acid in acidic solutions, compared to commercial Pt/C catalysts. Electronic supplementary information (ESI) available: Details of DFT calculation, SEM images of concave Pt nanocubes, mass activity and stability characterization of the catalysts. See DOI: 10.1039/c6nr02349e

  7. Surface passivation of high purity granular metals: zinc, cadmium, lead

    Directory of Open Access Journals (Sweden)

    Pirozhenko L. A.

    2017-10-01

    Full Text Available For the high purity metals (99.9999%, such as zinc, cadmium, and lead, which are widely used as initial components in growing semiconductor and scintillation crystals (CdTe, CdZnTe, ZnSe, (Cd, Zn, Pb WO4, (Cd, Zn, Pb MoO4 et al., it is very important to ensure reliable protection of the surface from oxidation and adsorption of impurities from the atmosphere. The specific features of surface passivation of high purity cadmium, lead and zinc are not sufficiently studied and require specific methodologies for further studies. The use of organic solutions in the schemes of chemical passivation of the investigated metals avoids hydrolysis of the obtained protective films. The use of organic solvents with pure cation and anion composition as the washing liquid prevents chemisorption of ions present in the conventionally used distilled water. This keeps the original purity of the granular metals. Novel compositions of etchants and etching scheme providing simultaneous polishing and passivation of high purity granular Zn, Cd and Pb are developed. Chemical passivation allows storing metals in the normal atmospheric conditions for more than half a year for Zn and Cd and up to 30 days for Pb without changing the state of the surface. The use of the glycerol-DMF solution in the processes for obtaining Pb granules provides self-passivation of metal surfaces and eliminates the additional chemical processing while maintaining the quality of corrosion protection.

  8. Efficient automated synthesis of 2-(5-["1"8F]fluoropentyl)-2-methylmalonic acid (["1"8F]ML-10) on a commercial available ["1"8F]FDG synthesis module

    International Nuclear Information System (INIS)

    Liu, Shaoyu; Nie, Dahong; Jiang, Shende; Tang, Ganghua

    2017-01-01

    ["1"8F]ML-10 (2-(5-["1"8F]fluoro-pentyl)-2-methylmalonic acid) is a small molecule positron emission tomography (PET) probe for apoptosis imaging. Automated synthesis of ["1"8F]ML-10 was developed by using two different purification methods through a direct saponification procedure on a modified commercial ["1"8F]Fluoro-2-Deoxyglucose (["1"8F]FDG) synthesizer. C18 purification method 1: The final ["1"8F]ML-10 solution containing ethanol was obtained with radiochemical yields of 60±5% (n=5) at the end of bombardment (EOB) and radiochemical purity of 98% in 35 min. Al_2O_3 and SCX purification method 2: To avoid possible side effects of a conventional ethanol-containing formulation, an new ethanol-free solution of ["1"8F]ML-10 was also developed, the radiochemical yields was 50±5% (n=5, EOB) within 45 min and the radiochemical purity was 98%. - Highlights: • The production of ["1"8F]ML-10 was optimized by using a straightforward saponification procedure. • Automated synthesis was performed on a commonly FDG synthesis module. • An ethanol-containing ["1"8F]ML-10 formulation was obtained with high radiochemical yield in a shorter time. • An ethanol-free formulation method of ["1"8F]ML-10 was also developed.

  9. Investigation on luminescence enhancement and decay characteristics of long afterglow nanophosphors for dark-vision display applications

    Energy Technology Data Exchange (ETDEWEB)

    Swati, G.; Chawla, S.; Mishra, S.; Rajesh, B.; Vijayan, N.; Sivaiah, B.; Dhar, A.; Haranath, D., E-mail: haranath@nplindia.org

    2015-04-01

    Graphical abstract: - Highlights: • Synthesis and structural characterization has been performed on long afterglow SrAl{sub 2}O{sub 4}:Eu{sup 2+}, Dy{sup 3+} nanophosphor having afterglow time of ∼12 h. • Studied the effect of various fuels used for synthesis of nanophosphors on the decay and luminescence characteristics. Interestingly, afterglow times varied significantly with different fuels used for the synthesis of the nanophosphor. • Excitation by different illuminants has profound influence on the luminescence intensity and afterglow times of the synthesized nanophosphor. • Such studies could be guidelines for appropriate usage of nanophosphor under different lighting environment. - Abstract: Long afterglow SrAl{sub 2}O{sub 4}:Eu{sup 2+},Dy{sup 3+} nanophosphors were synthesized via a facile but effectual auto-combustion technique followed by post-annealing treatment at elevated temperatures. The influence of various fuels during synthesis and thereafter improvement in the luminescence decay characteristics under various illuminant irradiations of long afterglow nanophosphors have been reported. Extensive studies on structural, morphological and luminescent properties of the as-synthesized afterglow nanophosphors have been presented. Powder X-ray diffraction studies confirm the presence of high-purity, single-phase monoclinic nanophosphors. HRTEM investigations confirm the formation of nanophosphors of particle size less than 50 nm. Photoluminescence emission is attributed to the characteristic d–f transition (4f{sup 6}5d{sup 1}→4f{sup 7}) of Eu{sup 2+} ions and was positioned at 512 nm. As-synthesized nanophosphors exhibit considerable confinement effects resulting into blue shift in emission maxima as compared to their bulk counterparts. The mechanism underlined for long afterglow has been discussed using trapping–detrapping model. The nanophosphor being multifunctional finds many interesting applications including dark-vision display

  10. [Synthesis and Characterization of a Sugar Based Electrolyte for Thin-film Polymer Batteries

    Science.gov (United States)

    1998-01-01

    The work performed during the current renewal period, March 1,1998 focused primarily on the synthesis and characterization of a sugar based electrolyte for thin-film polymer batteries. The initial phase of the project involved developing a suitable sugar to use as the monomer in the polymeric electrolyte synthesis. The monomer has been synthesized and characterized completely. Overall the yield of this material is high and it can be produced in relatively large quantity easily and in high purity. The scheme used for the preparation of the monomer is outlined along with pertinent yields.

  11. Enhanced unscheduled DNA synthesis in UV-irradiated human skin explants treated with T4N5 liposomes

    International Nuclear Information System (INIS)

    Yarosh, D.B.; Kibitel, J.T.; Green, L.A.; Spinowitz, A.

    1991-01-01

    Epidermal keratinocytes cultured from explants of skin cancer patients, including biopsies from xeroderma pigmentosum patients, were ultraviolet light-irradiated and DNA repair synthesis was measured. Repair capacity was much lower in xeroderma pigmentosum patients than in normal patients. The extent of DNA repair replication did not decline with the age of the normal patient. Treatment with T4N5 liposomes containing a DNA repair enzyme enhanced repair synthesis in both normal and xeroderma pigmentosum keratinocytes in an irradiation- and liposome-dose dependent manner. These results provide no evidence that aging people or skin cancer patients are predisposed to cutaneous malignancy by a DNA repair deficiency, but do demonstrate that T4N5 liposomes enhance DNA repair in the keratinocytes of the susceptible xeroderma pigmentosum and skin cancer population

  12. Solventless synthesis of ruthenium nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    García-Peña, Nidia G. [Departmento de Tecnociencias, Universidad Nacional Autónoma de México, Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Cd. Universitaria A.P. 70-186, C.P. 04510 Coyoacán, México D.F. (Mexico); Redón, Rocío, E-mail: rredon@unam.mx [Departmento de Tecnociencias, Universidad Nacional Autónoma de México, Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Cd. Universitaria A.P. 70-186, C.P. 04510 Coyoacán, México D.F. (Mexico); Herrera-Gomez, Alberto [Estudios Avanzados del Instituto Politécnico Nacional, Campus Juriquilla, Querétaro (Mexico); Fernández-Osorio, Ana Leticia [FES-Cuautitlán, Universidad Nacional Autónoma de México, Edo. de Mexico (Mexico); Bravo-Sanchez, Mariela; Gomez-Sosa, Gustavo [Estudios Avanzados del Instituto Politécnico Nacional, Campus Juriquilla, Querétaro (Mexico)

    2015-06-15

    Graphical abstract: - Highlights: • Successful synthesis of Ru nanoparticles by a cheap, fast and solventless approach was achieved. • The zero-valent state as well as the by-product/impurity free of the mechanochemical obtained Ru nanoparticles was proven by XPS, TEM and XRD. • Compared to two other synthesis strategies, the above-mentioned synthesis was more suitable to obtain smaller particles with fewer impurities in shorter time. - Abstract: This paper presents a novel solventless method for the synthesis of zero-valent ruthenium nanoparticles Ru(0). The proposed method, although not entirely new in the nanomaterials world, was used for the first time to synthesize zero-valent ruthenium nanoparticles. This new approach has proved to be an environmentally friendly, clean, cheap, fast, and reproducible technique which employs low amounts of solvent. It was optimized through varying amounts of reducing salt on a determined quantity of precursor and measuring the effect of this variation on the average particle size obtained. The resulting products were fully characterized by powder XRD, TEM, HR-TEM, and XPS studies, all of which corroborated the purity of the nanoparticles achieved. In order to verify the advantages of our method over other techniques, we compared our nanoparticles with two common colloidal-synthesized ruthenium nanoparticles.

  13. Influence of the polymer architecture on morphology and device properties of polymer bulk heterojunction photovoltaic cells

    NARCIS (Netherlands)

    Koetse, M.M.; Sweelssen, J.; Franse, T.; Veenstra, S.C.; Kroon, J.M.; Yang, X.N.; Alexeev, A.A.; Loos, J.; Schubert, U.S.; Schoo, H.F.M.; Kafafi, Z.H.; Lane, P.A.

    2004-01-01

    Polymer bulk hetero junction solar cells were made from poly(2-methoxy-5-(3,7-dimethyloctyloxy)-1,4-phenylene-vinylene) (MDMO-PPV) as donor and poly(cyanoetherphenylenevinylene) (PCNEPV) derivatives as acceptor material. In this paper we start out with discussing the synthesis of the materials.

  14. Water-based synthesis of hydrophobic ionic liquids for high-energy electrochemical devices

    International Nuclear Information System (INIS)

    Montanino, Maria; Alessandrini, Fabrizio; Passerini, Stefano; Appetecchi, Giovanni Battista

    2013-01-01

    Highlights: ► Water-based synthesis of ionic liquids with high yield. ► Full recycling of reagents. ► High purity pyrrolidinium-based ionic liquids with exceptional electrochemical stability window. ► Lithium plating from pyrrolidinium-based ionic liquids. -- Abstract: In this work is described an innovative synthesis route for hydrophobic ionic liquids (ILs) composed of N-methyl-N-alkylpyrrolidinium (or piperidinium) or imidazolium or tetralkylammonium cations and (perfluoroalkylsulfonyl)imide, ((C n F 2n+1 SO 2 )(C m F 2m+1 SO 2 )N − ), anions. This synthesis does not require the use of any environmental unfriendly solvent such as acetone, acetonitrile or halogen-containing compounds, which is not welcome in industrial applications. Only water is used as the process solvent throughout the entire process. In addition, the commonly used iodine-containing reagents were replaced by the cheaper, more chemically stable and less toxic bromine-containing compounds. A particular care was devoted to the development of the purification route, which is especially important for ILs to be used in high-energy electrochemical devices such as high voltage supercapacitors and lithium batteries. The effect of the reaction temperature, the time and the stoichiometry in the various steps of the synthesis have been investigated in detail. This novel procedure allowed obtaining ultrapure (>99.9 wt.%), clear, colourless, inodorous ILs with an overall yield above 92 wt.% and moisture content below 1 ppm. NMR measurements were run to confirm the chemical structure whereas elemental analysis and electrochemical tests were performed to check the purity of the synthesized ILs

  15. Development and Validation of a Stability-Indicating RP-HPLC Method for Rapid Determination of Doxycycline in Pharmaceutical Bulk and Dosage Forms

    Directory of Open Access Journals (Sweden)

    Shabnam Pourmoslemi, Soroush Mirfakhraee, Saeid Yaripour, Ali Mohammadi

    2016-06-01

    Full Text Available Background: A rapid stability-indicating RP-HPLC method for analysis of doxycycline in the presence of its degradation products was developed and validated. Methods: Forced degradation studies were carried out on bulk samples and capsule dosage forms of doxycycline using acid, base, H2O2, heat, and UV light as described by ICH for stress conditions to demonstrate the stability-indicating power of the method. Separations were performed on a Perfectsil® Target ODS column (3-5µm, 125 mm×4 mm, using a mobile phase consisting of methanol-50 mM ammonium acetate buffer (containing 0.1% v/v trifluoroacetic acid and 0.1% v/v triethylamine, pH 2.5 (50:50 v/v at room temperature. The flow rate was 0.8 mL/min. Results: The method linearity was investigated in the range of 25–500 µg/mL (r > 0.9999. The LOD and LOQ were 5 and 25 µg/mL, respectively. The method selectivity was evaluated by peak purity test using a diode array detector. There was no interference among detection of doxycycline and its stressed degradation products. Total peak purity numbers were in the range of 0.94-0.99, indicating the homogeneity of DOX peaks. Conclusion: These data show the stability-indicating nature of the method for quality control of doxycycline in bulk samples and capsule dosage forms.

  16. Differential scanning calorimetry method for purity determination: A case study on polycyclic aromatic hydrocarbons and chloramphenicol

    International Nuclear Information System (INIS)

    Kestens, V.; Zeleny, R.; Auclair, G.; Held, A.; Roebben, G.; Linsinger, T.P.J.

    2011-01-01

    Highlights: → Purity assessment of polycyclic aromatic hydrocarbons and chloramphenicol by DSC. → DSC results compared with traditional purity methods. → Different methods give different results, multiple method approach recommended. → DSC sensitive to impurities that have similar structures as main component. - Abstract: In this study the validity and suitability of differential scanning calorimetry (DSC) to determine the purity of selected polycyclic aromatic hydrocarbons and chloramphenicol has been investigated. The study materials were two candidate certified reference materials (CRMs), 6-methylchrysene and benzo[a]pyrene, and two different batches of commercially available highly pure chloramphenicol. The DSC results were compared with those obtained by other methods, namely gas and liquid chromatography with mass spectrometric detection, liquid chromatography with diode array detection, and quantitative nuclear magnetic resonance. The purity results obtained by these different analytical methods confirm the well-known challenges of comparing results of different method-defined measurands. In comparison with other methods, DSC has a much narrower working range. This limits the applicability of DSC as purity determination method, for instance during the assignment of the purity value of a CRM. Nevertheless, this study showed that DSC can be a powerful technique to detect impurities that are structurally very similar to the main purity component. From this point of view, and because of its good repeatability, DSC can be considered as a valuable technique to investigate the homogeneity and stability of candidate purity CRMs.

  17. Synthesis of deuterium-labeled felbamate from diethyl phenylmalonate

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Y.M.; Kucharczyk, N.; Sofia, R.D.

    1986-07-01

    A synthesis of the antiepileptic drug, felbamate-d/sub 4/ (2-phenyl-1,3-propanediol-1,1,3,3-d/sub 4/ dicarbamate), starting from diethyl phenylmalonic acid ester and lithium aluminum deuteride was developed. The procedure has three steps from the starting material to felbamate-d/sub 4/ via the intermediate, 2-phenyl-1,3-propanediol-1,1,3,3-d/sub 4/. The final overall yield was 44%. The isotope purity was 99.2%.

  18. Curcumin: Synthesis optimization and in silico interaction with cyclin dependent kinase.

    Science.gov (United States)

    Ahmed, Mahmood; Abdul Qadir, Muhammad; Imtiaz Shafiq, Muhammad; Muddassar, Muhammad; Hameed, Abdul; Nadeem Arshad, Muhammad; Asiri, Abdullah M

    2017-09-01

    Curcumin is a natural product with enormous biological potential. In this study, curcumin synthesis was revisited using different reaction solvents, a catalyst (n-butylamine) and a water scavenger [(n-BuO)3B], to develop the optimal procedure for its rapid acquisition. During synthesis, solvent choice was found to be an important parameter for better curcumin yield and high purity. In a typical reaction, acetyl acetone was treated with boron trioxide, followed by condensation with vanillin in the presence of tri-n-butyl borate as water scavenger and n-butylamine as catalyst at 80 °C in ethyl acetate to afford curcumin. Moreover, curcumin was also extracted from turmeric powder and spectroscopic properties such as IR, MS, 1H NMR and 13C NMR with synthetic curcumin were established to identify any impurity. The purity of synthetic and extracted curcumin was also checked by TLC and HPLC-DAD. To computationally assess its therapeutic potential against cyclin dependent kinases (CDKs), curcumin was docked in different isoforms of CDKs. It was observed that it did not dock at the active sites of CDK2 and CDK6. However, it could enter into weak interactions with CDK4 protein.

  19. Definition of the generalized criterion of estimation of ecological purity of textile products

    International Nuclear Information System (INIS)

    Gintibidze, N.; Valishvili, T.

    2009-01-01

    One of actual problems is the estimation of hygienic and ecological properties of fabrics on the basis of the data on the properties of initial fiber. In the present article, the definition of generalized criterion of the estimation of ecological purity of textile products is discussed. The estimation is based on the International Standard EKO-TEX-100, regulating the contents of inorganic and organic compounds in textile production. The determination of all listed substances is made according to appropriate techniques for each parameter. The quantity of substances is determined and compared with norms. The judgement about ecological purity is made by separate parameters. There is no uniform parameter which could estimate the degree of ecological purity of textile products. For calculating the generalized criterion of estimation of ecological purity of textile products, it is offered to estimate each criterion by the points corresponding to each factor. The textile product is recognized as ecologically pure (environment friendly) if the total estimate is more than 1. (author)

  20. Magnesium silicide production and silane synthesis on its basis

    International Nuclear Information System (INIS)

    Taurbaev, T.I.; Mukashev, F.A.; Manakov, S.M.; Francev, U.V.; Kalblanbekov, B.M.; Akhter, P.; Abbas, M.; Hussain, A.

    2003-01-01

    We had developed an alternative method of production of magnesium silicide with use of ferroalloys of silicon. Magnesium silicide is raw material for silane synthesis. The essence of the method consist of sintering FS -75 (ferrosilicium with 75 % of silicon and 25 % of iron, made by ferroalloy factories) with metal magnesium at temperature of 650 deg. C. The X-ray analysis has shown formation of magnesium silicide. That is further used for synthesis of silane. The output of silane is 60 % in respect of the contents of silicon. After removing the water vapors the mass-spectrometer analysis has estimated the purity of silane as 99.95 % with no detection of phosphine and diborane. (author)

  1. Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

    KAUST Repository

    Mehdizadeh Dehkordi, Arash; Bhattacharya, Sriparna; Darroudi, Taghi; Zeng, Xiaoyu; Alshareef, Husam N.; Tritt, Terry M.

    2015-01-01

    We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

  2. Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

    KAUST Repository

    Mehdizadeh Dehkordi, Arash

    2015-08-15

    We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

  3. [Purity Detection Model Update of Maize Seeds Based on Active Learning].

    Science.gov (United States)

    Tang, Jin-ya; Huang, Min; Zhu, Qi-bing

    2015-08-01

    Seed purity reflects the degree of seed varieties in typical consistent characteristics, so it is great important to improve the reliability and accuracy of seed purity detection to guarantee the quality of seeds. Hyperspectral imaging can reflect the internal and external characteristics of seeds at the same time, which has been widely used in nondestructive detection of agricultural products. The essence of nondestructive detection of agricultural products using hyperspectral imaging technique is to establish the mathematical model between the spectral information and the quality of agricultural products. Since the spectral information is easily affected by the sample growth environment, the stability and generalization of model would weaken when the test samples harvested from different origin and year. Active learning algorithm was investigated to add representative samples to expand the sample space for the original model, so as to implement the rapid update of the model's ability. Random selection (RS) and Kennard-Stone algorithm (KS) were performed to compare the model update effect with active learning algorithm. The experimental results indicated that in the division of different proportion of sample set (1:1, 3:1, 4:1), the updated purity detection model for maize seeds from 2010 year which was added 40 samples selected by active learning algorithm from 2011 year increased the prediction accuracy for 2011 new samples from 47%, 33.75%, 49% to 98.89%, 98.33%, 98.33%. For the updated purity detection model of 2011 year, its prediction accuracy for 2010 new samples increased by 50.83%, 54.58%, 53.75% to 94.57%, 94.02%, 94.57% after adding 56 new samples from 2010 year. Meanwhile the effect of model updated by active learning algorithm was better than that of RS and KS. Therefore, the update for purity detection model of maize seeds is feasible by active learning algorithm.

  4. Two Step Synthesis of a Non-symmetric Acetylcholinesterase Reactivator

    Directory of Open Access Journals (Sweden)

    Vit Koleckar

    2007-08-01

    Full Text Available The newly developed and very promising acetylcholinesterase reactivator (E-1- (2-hydroxyiminomethylpyridinium-4-(4-hydroxyiminomethylpyridinium-but-2-ene dibromide was prepared using two different pathways via a two-step synthesis involving the appropriate (E-1-(4-bromobut-2-enyl-2- or 4-hydroxyiminomethyl-pyridinium bromides. Afterwards, purities and yields of the desired product prepared by both routes were compared. Finally, its potency to reactivate several nerve agent-inhibited acetylcholinesterases was tested.

  5. Synthesis of [14α, 15α-3H]-norgestrel

    International Nuclear Information System (INIS)

    Wagner, H.

    1988-01-01

    The preparation of the well-known gestogen norgestrel in a tritium labelled form is described. Starting material was 18-methyl-3-methoxy-estra-1,3,5(10),8,14-pentaen-17β-o1 acetate. In a four step synthesis 17α-ethinyl-17β-hydroxy-18-methyl-[14α,15α- 3 H]-estr-4-en-3-one was obtained with a specific activity of 52 Ci/mmol and a radiochemical purity > 99%. (author)

  6. An efficient and economical way to enhance the performance of present HTS Maglev systems by utilizing the anisotropy property of bulk superconductors

    International Nuclear Information System (INIS)

    Deng Zigang; Wang Jiasu; Zheng Jun; Zhang Ya; Wang Suyu

    2013-01-01

    We report a simple, efficient and economical way to enhance the levitation or guidance performance of present high-temperature superconducting (HTS) Maglev systems by exploring the anisotropic properties of the critical current density in the a–b plane and along the c-axis of bulk superconductors. In the method, the bulk laying mode with different c-axis directions is designed to match with the magnetic field configuration of the applied permanent magnet guideway (PMG). Experimental results indicate that more than a factor of two improvement in the levitation force or guidance force is achieved when changing the laying mode of bulk superconductors from the traditional fashion of keeping the c-axis vertical to the PMG surface to the studied one of keeping the c-axis parallel to the PMG surface, at the maximum horizontal and vertical magnetic field positions of the PMG, respectively. These phenomena resulted from the physical nature of the generated levitation force and guidance force (electromagnetic forces) and the fact that there are different critical current densities in the a–b plane and along the c axis. Based on the experimental results, new HTS Maglev systems can be designed to meet the requirements of practical heavy-load or curved-route applications. (paper)

  7. An efficient and economical way to enhance the performance of present HTS Maglev systems by utilizing the anisotropy property of bulk superconductors

    Science.gov (United States)

    Deng, Zigang; Wang, Jiasu; Zheng, Jun; Zhang, Ya; Wang, Suyu

    2013-02-01

    We report a simple, efficient and economical way to enhance the levitation or guidance performance of present high-temperature superconducting (HTS) Maglev systems by exploring the anisotropic properties of the critical current density in the a-b plane and along the c-axis of bulk superconductors. In the method, the bulk laying mode with different c-axis directions is designed to match with the magnetic field configuration of the applied permanent magnet guideway (PMG). Experimental results indicate that more than a factor of two improvement in the levitation force or guidance force is achieved when changing the laying mode of bulk superconductors from the traditional fashion of keeping the c-axis vertical to the PMG surface to the studied one of keeping the c-axis parallel to the PMG surface, at the maximum horizontal and vertical magnetic field positions of the PMG, respectively. These phenomena resulted from the physical nature of the generated levitation force and guidance force (electromagnetic forces) and the fact that there are different critical current densities in the a-b plane and along the c axis. Based on the experimental results, new HTS Maglev systems can be designed to meet the requirements of practical heavy-load or curved-route applications.

  8. 2-Methyltetrahydrofuran and cyclopentyl methyl ether for green solid-phase peptide synthesis.

    Science.gov (United States)

    Jad, Yahya E; Acosta, Gerardo A; Khattab, Sherine N; de la Torre, Beatriz G; Govender, Thavendran; Kruger, Hendrik G; El-Faham, Ayman; Albericio, Fernando

    2016-02-01

    2-MeTHF and CPME were evaluated as greener alternatives for the most employed solvents in peptide synthesis. The ability of these solvents to dissolve amino acid derivatives and a range of coupling reagents were evaluated as well as the swelling of polystyrene and polyethylene glycol resins. In addition, racemization and coupling efficiencies were also determined. We concluded that the use of 2-MeTHF with combination of DIC/OxymaPure gave the lowest racemization level during stepwise synthesis of Z-Phg-Pro-NH2 and the highest purity during SPPS of Aib-enkephalin pentapeptide (H-Tyr-Aib-Aib-Phe-Leu-NH2).

  9. Study of absorption and IR-emission of Er3+, Dy3+, Tm3+ doped high-purity tellurite glasses

    Science.gov (United States)

    Motorin, S. E.; Dorofeev, V. V.; Galagan, B. I.; Sverchkov, S. E.; Koltashev, V. V.; Denker, B. I.

    2018-04-01

    A study of high-purity TeO2-ZnO based tellurite glasses doped with Er3+, Dy3+ or Tm3+ that could be used as laser media in the 2-3 μm spectral range is presented. The glasses are prepared by melting the oxides mixture inside a silica glass reactor in an atmosphere of purified oxygen. The low level of hydroxyl groups absorption allowed to measure correctly the luminescence decay characteristics of the dopants. The rare-earth ions absorption bands, the luminescence spectra and kinetic characteristics of emission from the levels 4I11/2, 4I13/2 of Er3+, 6H13/2 of Dy3+ and 3H4, 3H5, 3F4 of Tm3+ ions are investigated. The results confirm the high potential of tellurite glasses as an active media for bulk, planar waveguide and fiber lasers.

  10. The Feasibility of Bulk Crystallization as an Industrial Purification and Production Technique for Proteins

    Science.gov (United States)

    Judge, Russell A.; Forsythe, Elizabeth L.; Johns, Michael R.; Pusey, Marc L.; White, Edward T.

    1998-01-01

    Bulk crystallization in stirred vessels is used industrially for the recovery and purification of many inorganic and organic materials. Although much has been written on the crystallization of proteins for X-ray diffraction analysis, very little has been reported on the application of bulk crystallization in stirred vessels. In this study, a 1-liter, seeded, stirred, batch crystallizer was used with ovalbumin as a model protein to test the feasibility of this crystallization method as a recovery and purification process for proteins. Results were obtained for ovalbumin solubility, nucleation thresholds, crystal breakage and crystal growth kinetics in bulk solution under a range of operating conditions of pH and ammonium sulphate concentration (Judge et al., 1996). Experiments were also performed to determine the degree of purification that can be achieved by the crystallization of ovalbumin from a mixture of proteins. The effect of the presence of these proteins upon the ovalbumin crystal growth kinetics was also investigated (Judge et al., 1995). All of these aspects are essential for the design of bulk crystallization processes which have not previously been reported for proteins. Results from a second study that investigated the effect of structurally different proteins on the solubility, crystal growth rates and crystal purity of chicken egg white lysozyme are also presented (Judge et al., 1997). In this case face growth rates were measured using lysozyme purified by liquid chromatography and the effect of the addition of specific protein impurities were observed on the (110) and (101) crystal faces. In these two studies the results are presented to show the feasibility and purifying ability of crystallization as a production process for proteins.

  11. Ultrarapid Multimode Microwave Synthesis of Nano/Submicron β-SiC

    Directory of Open Access Journals (Sweden)

    Min Zhao

    2018-02-01

    Full Text Available This paper presents the design, development and realization of a fast and novel process for the synthesis of 3C silicon carbide (β-SiC nanorods and submicron powder. Using SiO2 (or Si and activated carbon (AC, this process allows β-SiC to be synthesized with almost 100% purity in timeframes of seconds or minutes using multimode microwave rotary tube reactors under open-air conditions. The synthesis temperature used was 1460 ± 50 °C for Si + AC and 1660 ± 50 °C for SiO2 + AC. The shortest β-SiC synthesis time achieved was about 20 s for Si + AC and 100 s for SiO2 + AC. This novel synthesis method allows for scaled-up flow processes in the rapid industrial-scale production of β-SiC, having advantages of time/energy saving and carbon dioxide emission reduction over comparable modern processes.

  12. A microscale synthesis of a promising radiolabelled antitumor drug: cis-1,1-cyclobutanedicarboxylato (2R)-2-methyl-1,4-butanediamine platinum(II), NK121

    International Nuclear Information System (INIS)

    Suwa, Masato; Kogawa, Osamu; Hashimoto, Yutaka

    1992-01-01

    A promising antitumor drug, cis-1,1-cyclobutane-dicarboxylato (2R)-2-methyl-1,4-butanediamine platinum (II), NK121, was synthesized from radionuclides of platinum such as 193m Pt, 195m Pt and 191 Pt which were produced by neutron irradiation of enriched 192 Pt. The overall yield was 38.6% in a synthesis time of 10 hours. The radioactivities present in 8.39 mg of NK121 were 115.3 μCi as 193m Pt, 29.9 μCi as 197 Pt, 22.0 μCi as 195m Pt, and 4.8 μCi as 191 Pt at the end of synthesis. The specific activity of the NK121 was 13.7 μCi ( 193m Pt)/mg NK121 at the end of synthesis. The radiochemical purity of NK121 was typically 99%. HPLC analyses confirmed that NK121 was in an adequate chemical purity and suitable for animal experimentation. (author)

  13. A microscale synthesis of a promising radiolabelled antitumor drug: cis-1,1-cyclobutanedicarboxylato (2R)-2-methyl-1,4-butanediamine platinum(II), NK121

    Energy Technology Data Exchange (ETDEWEB)

    Suwa, Masato; Kogawa, Osamu; Hashimoto, Yutaka (Nippon Kayaku Co. Ltd., Tokyo (Japan). Research Labs. of Pharmaceuticals Group); Nowatari, Hiroyoshi (Nippon Kayaku Co. Ltd., Takasaki, Gumma (Japan). Takasaki Research Labs.); Murase, Yuko; Homma, Yoshio (Kyoritsu Coll. of Pharmacy, Tokyo (Japan))

    1992-05-01

    A promising antitumor drug, cis-1,1-cyclobutane-dicarboxylato (2R)-2-methyl-1,4-butanediamine platinum (II), NK121, was synthesized from radionuclides of platinum such as {sup 193m}Pt, {sup 195m}Pt and {sup 191}Pt which were produced by neutron irradiation of enriched {sup 192}Pt. The overall yield was 38.6% in a synthesis time of 10 hours. The radioactivities present in 8.39 mg of NK121 were 115.3 {mu}Ci as {sup 193m}Pt, 29.9 {mu}Ci as {sup 197}Pt, 22.0 {mu}Ci as {sup 195m}Pt, and 4.8 {mu}Ci as {sup 191}Pt at the end of synthesis. The specific activity of the NK121 was 13.7 {mu}Ci ({sup 193m}Pt)/mg NK121 at the end of synthesis. The radiochemical purity of NK121 was typically 99%. HPLC analyses confirmed that NK121 was in an adequate chemical purity and suitable for animal experimentation. (author).

  14. 104 evaluation of microbiological purity of some brands of ...

    African Journals Online (AJOL)

    DR. AMINU

    Keywords: Microbiological purity, tetracycline, contaminants, bacterial load, fungal load, microbiological ... Just like food substances, pharmaceutical products .... Malaysia. Chlortetracycline a. Mar. 2005. Mar. 2008. Ghana b. Aug. 2005. Aug.

  15. Synthesis of formamidinium lead iodide perovskite bulk single crystal and its optical properties

    Science.gov (United States)

    Zheng, Hongge; Duan, Junjie; Dai, Jun

    2017-07-01

    Formamidinium lead iodide (FAPbI3) is a promising hybrid perovskite material for optoelectronic devices. We synthesized bulk single crystal FAPbI3 by a rapid solution crystallization method. X-ray diffraction (XRD) was performed to characterize the crystal structure. Temperature-dependent photoluminescence (PL) spectra of the bulk single crystal FAPbI3 were measured from 10 to 300 K to explain PL recombination mechanism. It shows that near band edge emission blueshifts with the temperature increasing from 10 to 120 K and from 140 K to room temperature, a sudden emission band redshift demonstrates near 140 K because of the phase transition from orthorhombic phase to cubic phase. From the temperature-dependent PL spectra, the temperature coefficients of the bandgap and thermal activation energies of FAPbI3 perovskite are fitted.

  16. “Flash” Solvent-free Synthesis of Triazoles Using a Supported Catalyst

    Directory of Open Access Journals (Sweden)

    Ibtissem Jlalia

    2009-01-01

    Full Text Available A solvent-free synthesis of 1,4-disubstituted-1,2,3-triazoles using neat azides and alkynes and a copper(I polymer supported catalyst (Amberlyst® A21•CuI is presented herein. As it provides the products in high yields and purities within minutes, this method thus being characterized as a "flash" synthesis, and was exemplified through the synthesis of a 24-compound library on a small scale.

  17. LASER APPLICATIONS AND OTHER TOPICS IN QUANTUM ELECTRONICS: Synthesis of bulk SiO2 : MxOy materials in a steady-state laser plume

    Science.gov (United States)

    Lebedev, V. F.

    1997-01-01

    An analysis was made of the conditions of existence of a two-component steady-state laser plume in atmospheric air. Such a plume is used in single-stage synthesis of bulk molten materials belonging to the SiO2 : MxOy system. Targets of the SiO2 : M type (metal foil and a silica glass rod) and doping elements with boiling points below and above the boiling point of silica glass are discussed. The regimes and efficiency of steady-state transfer of the dopants are considered. The efficiency of transfer of metal oxides during growth of samples with the aid of a cw CO2 laser is reported to be ~0.05, 0.4, and 0.75g min-1 kW-1 when the mass dopant concentration is ~8%, 20%, and 60% for the oxides of Ti, Cu, and Ni, respectively.

  18. Ion-exchange preparation of high-purity vanadium acid from industrial liquors

    International Nuclear Information System (INIS)

    Sajdakhmedov, U.A.; Arslanov, Sh.S.; Vulikh, A.I.

    1994-01-01

    The results of investigations on production of special-purity vanadium acid and vanadium oxide directly from process solutions (technical grade liquors) using ionites are presented. Potentiality of thorough purification of vanadium(5) oxide, when producing vanadium acid on the KU-2 cationite with subsequent purification on anionite, is shown. On the basis of the results obtained a principle flowsheet of ion-exchange production of high-purity vanadium(5) oxide from industrial liquors has been developed. 2 refs.; 1 fig.; 4 tabs

  19. Monitoring xenon purity in the LUX detector with a mass spectrometry system

    Science.gov (United States)

    Balajthy, Jon; LUX Experiment Collaboration

    2015-04-01

    The LUX dark matter search experiment is a 350 kg two-phase liquid/gas xenon time projection chamber located at the 4850 ft level of the Sanford Underground Research Facility in Lead, SD. To monitor for radioactive impurities such as krypton and impurities which limit charge yield such as oxygen, LUX uses a xenon sampling system consisting of a mass spectrometer and a liquid nitrogen cold trap. The cold trap separates the gaseous impurities from a small sample of xenon and allows them to pass to the mass spectrometer for analysis. We report here on results from the LUX xenon sampling program. We also report on methods to enhance the sensitivity of the cold trap technique in preparation for the next-generation LUX-ZEPLIN experiment which will have even more stringent purity requirements.

  20. Automated process flowsheet synthesis for membrane processes using genetic algorithm: role of crossover operators

    KAUST Repository

    Shafiee, Alireza

    2016-06-25

    In optimization-based process flowsheet synthesis, optimization methods, including genetic algorithms (GA), are used as advantageous tools to select a high performance flowsheet by ‘screening’ large numbers of possible flowsheets. In this study, we expand the role of GA to include flowsheet generation through proposing a modified Greedysub tour crossover operator. Performance of the proposed crossover operator is compared with four other commonly used operators. The proposed GA optimizationbased process synthesis method is applied to generate the optimum process flowsheet for a multicomponent membrane-based CO2 capture process. Within defined constraints and using the random-point crossover, CO2 purity of 0.827 (equivalent to 0.986 on dry basis) is achieved which results in improvement (3.4%) over the simplest crossover operator applied. In addition, the least variability in the converged flowsheet and CO2 purity is observed for random-point crossover operator, which approximately implies closeness of the solution to the global optimum, and hence the consistency of the algorithm. The proposed crossover operator is found to improve the convergence speed of the algorithm by 77.6%.

  1. Eco-friendly Synthesis of Organics and Nanomaterials ...

    Science.gov (United States)

    The presentation summarizes our recent activity in chemical synthesis involving benign alternatives, such as the use of supported reagents, and greener reaction medium in aqueous or solvent-free conditions.1 The synthesis of heterocyclic compounds, coupling reactions, and a variety of name reactions2 are the primary beneficiaries as exemplified by the synthesis of N-aryl azacycloalkanes, isoindoles, and dihydropyrazoles, 1,3,4-oxadiazoles, 1,3,4-thiadiazoles, 1,3-dioxanes, pyrazoles, catalyzed by basic water or polystyrene sulfonic acid (PSSA) in conjunction with microwave (MW) irradiation.2 Vitamins B1, B2, C, and tea and wine polyphenols which function both as reducing and capping agents, provide extremely simple, one-pot, green synthetic methods to bulk quantities of nanomaterials in water.3a Shape-controlled synthesis of noble nanostructures via MW-assisted spontaneous reduction of noble metal salts using sugars will be presented.3b A general method has been developed for the cross-linking reaction of poly (vinyl alcohol) (PVA) with metallic systems; bimetallic systems,3c and SWNT, MWNT, and C-60.3d The strategy is extended to the formation of biodegradable carboxymethylcellulose (CMC) composite films with noble nanometals;3e such metal decoration and alignment of carbon nanotubes in CMC is possible using MW approach3f which also enables the shape-controlled bulk synthesis of Ag and Fe nanorods in poly (ethylene glycol).3g MW hydrothermal process delivers m

  2. Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

    International Nuclear Information System (INIS)

    Teixeira, G.F.; Gasparotto, G.; Santos, N.A.; Zaghete, M.A.; Varela, J.A.; Longo, E.

    2009-01-01

    Full text: Lead Zirconate Titanate (PZT) is a ceramic witch has great interest because of their ferroelectric, piezoelectric, and other electrical properties. In this work Pb(ZrxTi1-x)O3 powders were synthesized by microwave hydrothermal synthesis (M-H) at 180°C without excess lead content. This method allows obtaining particles whit nanometer size, good stoichiometric controls, high purity and crystalline degree at low temperatures and short times of synthesis. Powders were synthesized with molar concentration of 0.15 mol.L -1 during different times: 30 min, 2, 4, 6 and 8 h. After that the powders were characterized by X-ray diffraction (XRD), Field Emission Gun (FEG) and photoluminescence (PL). Through analysis it is observed that the crystalline phase of PZT is obtained from 2 hours of synthesis and this same time also presents more intense PL emission. (author)

  3. Gallic Acid Grafted Chitosan Has Enhanced Oxidative Stability in Bulk Oils.

    Science.gov (United States)

    Gim, Seo Yeong; Hong, Seungmi; Kim, Mi-Ja; Lee, JaeHwan

    2017-07-01

    Gallic acid (GA) was grafted in chitosan and the effects of GA grafted chitosan (GA-g-CS) on the oxidative stability in bulk oil was tested at 60 and 140 °C. To text oxidative stability in oils, headspace oxygen content, conjugated dienoic acid (CDA) value, p-anisidine value (p-AV), and acid value were determined. Chitosan itself did not show antioxidative or prooxidative effects in oils at 60 °C. However, GA-g-CS and GA acted as antioxidants at 60 °C. At 140 °C heating with moisture supplied condition, different results were observed. GA-g-CS acted as antioxidants based on the results of CDA and p-AV. However, chitosan showed the highest oxidative stability based on results of acid value and brown color formation at 140 °C. This could be due to reduction of moisture content by chitosan. GA was continuously released from GA-g-CS in bulk oil. This might have provided extra antioxidant activities to oils. © 2017 Institute of Food Technologists®.

  4. Pressure-assisted sintering of high purity barium titanate

    NARCIS (Netherlands)

    van den Cruijsem, S.; Varst, van der P.G.T.; With, de G.; Bortzmeyer, D.; Boussuge, M.; Chartier, Th.; Hausonne, J.M.; Mocellin, A.; Rousset, A.; Thevenot, F.

    1997-01-01

    The dielectric behaviour of High Purity Barium titanate (HPB) ceramics is strongly dependent on the grain size and porosity. For applications, control of grain size and porosity is required. Pressure-assisted sintering techniques at relatively low temperatures meet these requirements. In this study,

  5. High-Energy Laser Interaction with Gases, Droplets, and Bulk Liquids.

    Science.gov (United States)

    Jarzembski, Maurice Anthony

    Breakdown threshold intensities (I_ {rm TH}) were measured as functions of wavelengths and pressure for air, He, Ar, and Xe using a Nd:YAG pulsed laser. Multiphoton absorption dominates in the UV and cascade collision ionization dominates in the IR; however, both can be affected by other electron gain and loss processes. Presence of droplets lowers breakdown of gases due to field enhancements. Breakdown is initiated either in the droplet material or in the gas. At lambda = 0.532mum for a 50 μm dia. water droplet in He, Ar, and air for p pressure. For droplet -in-Xe, at p pressure. For droplet-in-Xe, at p 140 Torr, breakdown occurs outside the droplet and is dependent on gas pressure. Pressure dependence of breakdown was observed for 120mum dia. water droplets in Ar at p > 400 Torr. The required intensity for breakdown of droplet depends on I_{ rm TH} of bulk liquid and the effective field enhancement created by the droplet. The I _{rm TH} of droplet-in-air provides an upper limit to the propagation of a high energy laser beam in the atmosphere containing particles. By geometrical optics approach, a significant field enhancement located at the critical ring region, encircling the axis of the sphere in the forward direction at angle theta_{c}, was discovered where nonlinear processes can occur. This was confirmed experimentally and by Mie theory. Field enhancements calculated at the critical ring for water droplets of different sizes agree well with measurements. For a droplet of given size and real refractive index, the effective field enhancement and the volume over which it occurs are two important factors governing the occurrence of breakdown in droplets for both off resonance and on resonance conditions. Measurements of wavelength dependence of breakdown showed that in the UV, I_{rm TH} for droplets and bulk liquids were comparable and lower by few orders of magnitude from that of air. Transmittance and reflectance of bulk liquids in the UV change with

  6. Event timing in high purity germanium coaxial detectors

    International Nuclear Information System (INIS)

    El-Ibiary, M.Y.

    1979-08-01

    The timing of gamma ray radiation in systems using high purity coaxial germanium detectors is analyzed and compared to that of systems using Ge(Li) detectors. The analysis takes into account the effect of the residual impurities on the electric field distribution, and hence on the rate of rise of the electrical pulses delivered to the timing module. Conditions under which the electric field distribution could lead to an improvement in timing performance, are identified. The results of the analysis confirm the experimental results published elsewhere and when compared with those for Ge(Li) detectors, which usually operate under conditions of charge carrier velocity saturation, confirm that high purity germanium detectors need not have inferior timing characteristics. A chart is given to provide a quantitative basis on which the trade off between the radius of the detector and its time resolution may be made

  7. Temperature dependence of luminescence for different surface flaws in high purity silica glass

    International Nuclear Information System (INIS)

    Fournier, J.; Grua, P.; Neauport, J.; Fargin, E.; Jubera, V.; Talaga, D.; Del Guerzo, A.; Raffy, G.; Jouannigot, S.

    2013-01-01

    In situ temperature dependence of the Photoluminescence under 325 nm irradiation is used to investigate defect populations existing in different surface flaws in high purity fused silica. Five photoluminescence bands peaking at 1.9, 2.1, 2.3, 2.63 and 3.11 eV have been detected in the spectral area ranging from 1.6 up to 3.6 eV. The Gaussian deconvolution of spectra allows dividing the five luminescence bands in two categories. The former corresponds to bands showing a significant intensity enhancement while temperature decreases; the latter corresponds to bands remaining insensitive to the temperature evolution. Such a behavior brings new information on defects involved in laser damage mechanism at 351 nm in nanosecond regime. (authors)

  8. Synthesis of carbon nanofibers by catalytic CVD of chlorobenzene over bulk nickel alloy

    Science.gov (United States)

    Kenzhin, Roman M.; Bauman, Yuri I.; Volodin, Alexander M.; Mishakov, Ilya V.; Vedyagin, Aleksey A.

    2018-01-01

    Catalytic chemical vapor deposition (CCVD) of chlorobenzene over bulk nickel alloy (nichrome) was studied. The bulk Ni-containing samples being exposed to a contact with aggressive reaction medium undergo self-disintegration followed by growth of carbon nanofibers. This process, also known as a metal dusting, requires the simultaneous presence of chlorine and hydrogen sources in the reaction mixture. Molecule of chlorobenzene complies with these requirements. The experiments on CCVD were performed in a flow-through reactor system. The initial stages of nickel disintegration process were investigated in a closed system under Autogenic Pressure at Elevated Temperature (RAPET) conditions. Scanning and transmission electron microscopies and ferromagnetic resonance spectroscopy were applied to examine the samples after their interaction with chlorobenzene. Introduction of additional hydrogen into the flow-through system was shown to affect the morphology of grown carbon nanofibers.

  9. Optical fiber design with orbital angular momentum light purity higher than 99.9.

    Science.gov (United States)

    Zhang, Zhishen; Gan, Jiulin; Heng, Xiaobo; Wu, Yuqing; Li, Qingyu; Qian, Qi; Chen, Dongdan; Yang, Zhongmin

    2015-11-16

    The purity of the synthesized orbital-angular-momentum (OAM) light in the fiber is inversely proportional to channel crosstalk level in the OAM optical fiber communication system. Here the relationship between the fiber structure and the purity is firstly demonstrated in theory. The graded-index optical fiber is proposed and designed for the OAM light propagation with the purity higher than 99.9%. 16 fiber modes (10 OAM modes) have been supported by a specific designed graded-index optical fiber with dispersion less than 35 ps/(km∙nm). Such fiber design has suppressed the intrinsic crosstalk to be lower than -30 dB, and can be potentially used for the long distance OAM optical communication system.

  10. Synthesis of seven deuteromethyl-caffeine analogues observation of deuterium isotope effects on CMR analysis

    Energy Technology Data Exchange (ETDEWEB)

    Falconnet, J.B.; Brazier, J.L.; Desage, M.

    1986-03-01

    The synthesis of all 7 N-trideuteromethyl isotopomers of caffeine by reaction of trideuteromethyl iodide (C/sup 2/H/sub 3/I) with the appropriate xanthine molecules is described. The use of proton, deuterium and carbon-13-NMR as a first step in purity assessment revealed /sup 13/C-NMR deuterium isotope effects on the resonance of perdeuteromethyl carbons.

  11. Study of various synthesis techniques of nanomaterials

    Science.gov (United States)

    Patil, Madhuri; Sharma, Deepika; Dive, Avinash; Mahajan, Sandeep; Sharma, Ramphal

    2018-05-01

    Development of synthesis techniques of realizing nano-materials over a range of sizes, shapes, and chemical compositions is an important aspect of nanotechnology. The remarkable size dependent physical & chemical properties of particles have fascinated and inspired research activity in this direction. This paper describes some aspects on synthesis and characterization of particles of metals, metal alloys, and oxides, either in the form of thin films or bulk shapes. A brief discussion on processing of thin-films is also described.

  12. Yonsei Evolutionary Population Synthesis (YEPS). II. Spectro-photometric Evolution of Helium-enhanced Stellar Populations

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Chul; Yoon, Suk-Jin; Lee, Young-Wook, E-mail: chulchung@yonsei.ac.kr, E-mail: sjyoon0691@yonsei.ac.kr [Center for Galaxy Evolution Research, Yonsei University, Seoul 03722 (Korea, Republic of)

    2017-06-20

    The discovery of multiple stellar populations in Milky Way globular clusters (GCs) has stimulated various follow-up studies on helium-enhanced stellar populations. Here we present the evolutionary population synthesis models for the spectro-photometric evolution of simple stellar populations (SSPs) with varying initial helium abundance ( Y {sub ini}). We show that Y {sub ini} brings about dramatic changes in spectro-photometric properties of SSPs. Like the normal-helium SSPs, the integrated spectro-photometric evolution of helium-enhanced SSPs is also dependent on metallicity and age for a given Y {sub ini}. We discuss the implications and prospects for the helium-enhanced populations in relation to the second-generation populations found in the Milky Way GCs. All of the models are available at http://web.yonsei.ac.kr/cosmic/data/YEPS.htm.

  13. Yonsei Evolutionary Population Synthesis (YEPS). II. Spectro-photometric Evolution of Helium-enhanced Stellar Populations

    International Nuclear Information System (INIS)

    Chung, Chul; Yoon, Suk-Jin; Lee, Young-Wook

    2017-01-01

    The discovery of multiple stellar populations in Milky Way globular clusters (GCs) has stimulated various follow-up studies on helium-enhanced stellar populations. Here we present the evolutionary population synthesis models for the spectro-photometric evolution of simple stellar populations (SSPs) with varying initial helium abundance ( Y ini ). We show that Y ini brings about dramatic changes in spectro-photometric properties of SSPs. Like the normal-helium SSPs, the integrated spectro-photometric evolution of helium-enhanced SSPs is also dependent on metallicity and age for a given Y ini . We discuss the implications and prospects for the helium-enhanced populations in relation to the second-generation populations found in the Milky Way GCs. All of the models are available at http://web.yonsei.ac.kr/cosmic/data/YEPS.htm.

  14. A facile and rapid automated synthesis of 3'-deoxy-3'-[18F]fluorothymidine

    International Nuclear Information System (INIS)

    Tang Ganghua; Tang Xiaolan; Wen Fuhua; Wang Mingfang; Li Baoyuan

    2010-01-01

    Aim: To develop a simplified and fully automated synthesis procedure of 3'-deoxy-3'-[ 18 F]fluorothymidine ([ 18 F]FLT) using PET-MF-2V-IT-I synthesis module. Methods: Synthesis of [ 18 F]FLT was performed using PET-MF-2V-IT-I synthesis module by one-pot two-step reaction procedure, including nucleophilic fluorination of 3-N-t-butoxycarbonyl-1-[5'-O-(4,4'-dimethoxy triphenylmethyl)-2'-deoxy-3'-O-(4-nitrobenzenesulfonyl) -β-D-threopentofuranosyl]thymine (15 mg) as the precursor molecule with [ 18 F]fluoride, and subsequent hydrolysis of the protecting group with 1.0 M HCl at the same reaction vessel and purification with SEP PAK cartridges instead of the HPLC system. Results: The automated synthesis of [ 18 F]FLT with SEP PAK purification gave corrected radiochemical yield of 23.2±2.6% (n=6, uncorrected yield: 16-22%) and radiochemical purity of >97% within the total synthesis time of 35 min. Conclusion: The fully one-pot automated synthesis procedure with SEP PAK purification can be applied to the fully automated synthesis of [ 18 F]FLT using commercial [ 18 F]FDG synthesis module.

  15. Recent advances in synthesis of bacterial rare sugar building blocks and their applications.

    Science.gov (United States)

    Emmadi, Madhu; Kulkarni, Suvarn S

    2014-07-01

    Covering: 1964 to 2013. Bacteria have unusual glycans on their surfaces which distinguish them from the host cells. These unique structures offer avenues for targeting bacteria with specific therapeutics and vaccine. However, these rare sugars are not accessible in acceptable purity and amounts by isolation from natural sources. Thus, procurement of orthogonally protected rare sugar building blocks through efficient chemical synthesis is regarded as a crucial step towards the development of glycoconjugate vaccines. This Highlight focuses on recent advances in the synthesis of the bacterial deoxy amino hexopyranoside building blocks and their application in constructing various biologically important bacterial O-glycans.

  16. Weak ferromagnetic component on the bulk ZnFe{sub 2}O{sub 4} compound

    Energy Technology Data Exchange (ETDEWEB)

    Jesus, C.B.R. [Departamento de Física, Campus prof. Aluísio de Campos, UFS, 49100-000 São Cristóvão, SE (Brazil); Mendonça, E.C. [Departamento de Física, Campus prof. Alberto Carvalho, UFS, 49500-000 Itabaiana, SE (Brazil); Silva, L.S. [Departamento de Física, Campus prof. Aluísio de Campos, UFS, 49100-000 São Cristóvão, SE (Brazil); Folly, W.S.D.; Meneses, C.T. [Departamento de Física, Campus prof. Alberto Carvalho, UFS, 49500-000 Itabaiana, SE (Brazil); Duque, J.G.S., E-mail: gerivaldoduque@gmail.com [Departamento de Física, Campus prof. Alberto Carvalho, UFS, 49500-000 Itabaiana, SE (Brazil)

    2014-01-15

    Magnetization data on the bulk ZnFe{sub 2}O{sub 4} antiferromagnetic compound (T{sub N}≈10 K) obtained via solid state reaction at different synthesis temperatures show one weak ferromagnetic component at room temperature. We have related it with the cationic disorder effect present on spinel structure of our bulk samples which comes from the magnetic interaction between iron ions sit on both octahedral and tetrahedral sites. The magnetization measurements show to all samples a clear peak around 10 K consistent with the antiferromagnetic phase transition. On the other hand, after extracted the paramagnetic component, the hysteresis loops measured at room temperature display one weak ferromagnetic component. Once the T-dependence of magnetization does not fit to a Curie–Weiss law to temperatures well above the magnetic transition we have used a combination of the Curie–Weiss law (paramagnetic spins) and a typical temperature dependence of M{sub 0}, M{sub 0}(T)=M{sub 0}(0)[1−(T/T{sub C}){sup 2}]{sup 0.5} (ordered ferromagnetic spins). We note an increase of the M{sub 0}(0) as function of the synthesis temperature. This reinforce our supposition of a cationic disorder effect driving the system to present two kinds of magnetic interactions between iron ions on A and B sites. - Highlights: • Study of the cationic disorder at bulk ZnFe{sub 2}O{sub 4} compound. • Structural and magnetization characterization. • The observation of two magnetic phases.

  17. Optimization, formulation, and characterization of multiflavonoids-loaded flavanosome by bulk or sequential technique.

    Science.gov (United States)

    Karthivashan, Govindarajan; Masarudin, Mas Jaffri; Kura, Aminu Umar; Abas, Faridah; Fakurazi, Sharida

    2016-01-01

    This study involves adaptation of bulk or sequential technique to load multiple flavonoids in a single phytosome, which can be termed as "flavonosome". Three widely established and therapeutically valuable flavonoids, such as quercetin (Q), kaempferol (K), and apigenin (A), were quantified in the ethyl acetate fraction of Moringa oleifera leaves extract and were commercially obtained and incorporated in a single flavonosome (QKA-phosphatidylcholine) through four different methods of synthesis - bulk (M1) and serialized (M2) co-sonication and bulk (M3) and sequential (M4) co-loading. The study also established an optimal formulation method based on screening the synthesized flavonosomes with respect to their size, charge, polydispersity index, morphology, drug-carrier interaction, antioxidant potential through in vitro 1,1-diphenyl-2-picrylhydrazyl kinetics, and cytotoxicity evaluation against human hepatoma cell line (HepaRG). Furthermore, entrapment and loading efficiency of flavonoids in the optimal flavonosome have been identified. Among the four synthesis methods, sequential loading technique has been optimized as the best method for the synthesis of QKA-phosphatidylcholine flavonosome, which revealed an average diameter of 375.93±33.61 nm, with a zeta potential of -39.07±3.55 mV, and the entrapment efficiency was >98% for all the flavonoids, whereas the drug-loading capacity of Q, K, and A was 31.63%±0.17%, 34.51%±2.07%, and 31.79%±0.01%, respectively. The in vitro 1,1-diphenyl-2-picrylhydrazyl kinetics of the flavonoids indirectly depicts the release kinetic behavior of the flavonoids from the carrier. The QKA-loaded flavonosome had no indication of toxicity toward human hepatoma cell line as shown by the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide result, wherein even at the higher concentration of 200 µg/mL, the flavonosomes exert >85% of cell viability. These results suggest that sequential loading technique may be a promising

  18. A short synthesis and its application to the preparation of radio labelled leukotriene inhibitor Sch 37224

    International Nuclear Information System (INIS)

    Duelfer, T.; Gala, D.

    1991-01-01

    A new, short synthesis of 1-(1,2-dihydro-4-hydroxyl-1-phenyl-2-oxo-1,8-naphthyridin-3-yl)-pyrrolidinium hydroxide, inner salt, 1, was achieved by condensing methyl 2-phenylamino-3-pyridine carboxylate 2 with ethyl 1-pyrrolidine acetate 4. This gave highly pure product in 60% yield. This synthesis was applied to the preparation of 14 C labelled 1. Radiolabelled 1 was synthesized from u-[ 14 C]-aniline in three steps at 97% radiochemical purity and 27.3% radiochemical yield. (author)

  19. Determination of nanoparticle surface coatings and nanoparticle purity using microscale thermogravimetric analysis.

    Science.gov (United States)

    Mansfield, Elisabeth; Tyner, Katherine M; Poling, Christopher M; Blacklock, Jenifer L

    2014-02-04

    The use of nanoparticles in some applications (i.e., nanomedical, nanofiltration, or nanoelectronic) requires small samples with well-known purities and composition. In addition, when nanoparticles are introduced into complex environments (e.g., biological fluids), the particles may become coated with matter, such as proteins or lipid layers. Many of today's analytical techniques are not able to address small-scale samples of nanoparticles to determine purity and the presence of surface coatings. Through the use of an elevated-temperature quartz crystal microbalance (QCM) method we call microscale thermogravimetric analysis, or μ-TGA, the nanoparticle purity, as well as the presence of any surface coatings of nanomaterials, can be measured. Microscale thermogravimetric analysis is used to determine the presence and amount of surface-bound ligand coverage on gold nanoparticles and confirm the presence of a poly(ethylene glycol) coating on SiO2 nanoparticles. Results are compared to traditional analytical techniques to demonstrate reproducibility and validity of μ-TGA for determining the presence of nanoparticle surface coatings. Carbon nanotube samples are also analyzed and compared to conventional TGA. The results demonstrate μ-TGA is a valid method for quantitative determination of the coatings on nanoparticles, and in some cases, can provide purity and compositional data of the nanoparticles themselves.

  20. Nano-particulate Aluminium Nitride/Al: An Efficient and Versatile Heterogeneous Catalyst for the Synthesis of Biginelli Scaffolds

    Science.gov (United States)

    Tekale, S. U.; Tekale, A. B.; Kanhe, N. S.; Bhoraskar, S. V.; Pawar, R. P.

    2011-12-01

    Nano-particulate aluminium nitride/Al (7:1) is reported as a new heterogeneous solid acid catalyst for the synthesis of 3, 4-dihydroxypyrimidi-2-(1H)-ones and their sulphur analogues using the Biginelli reaction. This method involves short reaction time, easy separation, high yields and purity of products.

  1. Evaluation of measurement uncertainty for purity of a monoterpenic acid by small-scale coulometry

    Science.gov (United States)

    Norte, L. C.; de Carvalho, E. M.; Tappin, M. R. R.; Borges, P. P.

    2018-03-01

    Purity of the perylic acid (HPe) which is a monoterpenic acid from natural product (NP) with anti-inflammatory and anticancer properties was analyzed by small-scale coulometry (SSC), due to the low availability of HPe on the pharmaceutic market and its high cost. This work aims to present the evaluation of the measurements uncertainty from the purity of HPe by using SSC. Coulometric mean of purity obtained from 5 replicates resulted in 94.23% ± 0.88% (k = 2.06, for an approximately 95% confidence level). These studies aim in the future to develop the production of certified reference materials from NPs.

  2. Spectroscopic Determination of Trace Contaminants in High Purity Oxygen

    Science.gov (United States)

    Hornung, Steven D.

    2011-01-01

    Oxygen used for extravehicular activities (EVA) must be free of contaminants because a difference in a few tenths of a percent of argon or nitrogen content can mean significant reduction in available EVA time. These inert gases build up in the extravehicular mobility unit because they are not metabolized or scrubbed from the atmosphere. Measurement of oxygen purity above 99.5% is problematic, and currently only complex instruments such as gas chromatographs or mass spectrometers are used for these determinations. Because liquid oxygen boil-off from the space shuttle will no longer be available to supply oxygen for EVA use, other concepts are being developed to produce and validate high purity oxygen from cabin air aboard the International Space Station. A prototype optical emission technique capable of detecting argon and nitrogen below 0.1% in oxygen was developed at White Sands Test Facility. This instrument uses a glow discharge in reduced pressure gas to produce atomic emission from the species present. Because the atomic emission lines from oxygen, nitrogen, and argon are discrete and in many cases well-separated, trace amounts of argon and nitrogen can be detected in the ultraviolet and visible spectrum. This is a straightforward, direct measurement of the target contaminants and may lend itself to a device capable of on-orbit verification of oxygen purity. System design and optimized measurement parameters are presented.

  3. Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis.

    Science.gov (United States)

    Dias, Jorge T; Svedberg, Gustav; Nystrand, Mats; Andersson-Svahn, Helene; Gantelius, Jesper

    2018-03-07

    The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity and convenient colorimetric readout. However, high densities of nanoparticles are typically needed for detection. The available synthesis-based enhancement protocols are either limited to gold and silver nanoparticles or rely on precise enzymatic control and optimization. Here, we present a protocol to enhance the colorimetric readout of gold, silver, silica, and iron oxide nanoprobes. It was observed that the colorimetric signal can be improved by up to a 10000-fold factor. The basis for such signal enhancement strategies is the chemical reduction of Au 3+ to Au 0 . There are several chemical reactions that enable the reduction of Au 3+ to Au 0 . In the protocol, Good's buffers and H2O2 are used and it is possible to favor the deposition of Au 0 onto the surface of existing nanoprobes, in detriment of the formation of new gold nanoparticles. The protocol consists of the incubation of the microarray with a solution consisting of chloroauric acid and H2O2 in 2-(N-morpholino)ethanesulfonic acid pH 6 buffer following the nanoprobe-based detection assay. The enhancement solution can be applied to paper and glass-based sensors. Moreover, it can be used in commercially available immunoassays as demonstrated by the application of the method to a commercial allergen microarray. The signal development requires less than 5 min of incubation with the enhancement solution and the readout can be assessed by naked eye or low-end image acquisition devices such as a table-top scanner or a digital camera.

  4. High purity materials as targets for radioisotope production: Needs ...

    Indian Academy of Sciences (India)

    Unknown

    lity of high purity target materials, natural or enriched, are crucial for any successful radioisotope pro- gramme. Selection ... and blockages detection in buried pipelines are rendered ..... from reputed international suppliers with analysis report.

  5. Synthesis of nanocrystalline Y2O3 in a specially designed atmospheric pressure radio frequency thermal plasma reactor

    International Nuclear Information System (INIS)

    Dhamale, G. D.; Mathe, V. L.; Bhoraskar, S. V.; Sahasrabudhe, S. N.; Ghorui, S.

    2015-01-01

    Synthesis of yttrium oxide nanoparticles in a specially designed radio frequency thermal plasma reactor is reported. Good crystallinity, narrow size distribution, low defect state concentration, high purity, good production rate, single-step synthesis, and simultaneous formation of nanocrystalline monoclinic and cubic phases are some of the interesting features observed. Synthesized particles are characterized through X-ray diffraction, transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, thermo-luminescence (TL), and Brunauer–Emmett–Teller surface area analysis. Polymorphism of the nanocrystalline yttria is addressed in detail. Synthesis mechanism is explored through in-situ emission spectroscopy. Post-synthesis environmental effects and possible methods to eliminate the undesired phases are probed. Defect states are investigated through the study of TL spectra

  6. Improved synthesis and application of [(11) C]benzyl iodide in positron emission tomography radiotracer production.

    Science.gov (United States)

    Pekošak, Aleksandra; Filp, Ulrike; Rotteveel, Lonneke; Poot, Alex J; Windhorst, Albert D

    2015-06-30

    Positron emission tomography has increased the demand for new carbon-11 radiolabeled tracers and building blocks. A promising radiolabeling synthon is [(11) C]benzyl iodide ([(11) C]BnI), because the benzyl group is a widely present functionality in biologically active compounds. Unfortunately, synthesis of [(11) C]BnI has received little attention, resulting in limited application. Therefore, we investigated the synthesis in order to significantly improve, automate, and apply it for labeling of the dopamine D2 antagonist [(11) C]clebopride as a proof of concept. [(11) C]BnI was synthesized from [(11) C]CO2 via a Grignard reaction and purified prior the reaction with desbenzyl clebopride. According to a one-pot procedure, [(11) C]BnI was synthesized in 11 min from [(11) C]CO2 with high yield, purity, and specific activity, 52 ± 3% (end of the cyclotron bombardment), 95 ± 3%, and 123 ± 17 GBq/µmol (end of the synthesis), respectively. Changes in the [(11) C]BnI synthesis are reduced amounts of reagents, a lower temperature in the Grignard reaction, and the introduction of a solid-phase intermediate purification. [(11) C]Clebopride was synthesized within 28 min from [(11) C]CO2 in an isolated decay-corrected yield of 11 ± 3% (end of the cyclotron bombardment) with a purity of >98% and specific activity (SA) of 54 ± 4 GBq/µmol (n = 3) at the end of the synthesis. Conversion of [(11) C]BnI to product was 82 ± 11%. The reliable synthesis of [(11) C]BnI allows the broad application of this synthon in positron emission tomography radiopharmaceutical development. Copyright © 2015 John Wiley & Sons, Ltd.

  7. Effects of bulk charged impurities on the bulk and surface transport in three-dimensional topological insulators

    Energy Technology Data Exchange (ETDEWEB)

    Skinner, B.; Chen, T.; Shklovskii, B. I., E-mail: shklovsk@physics.spa.umn.edu [University of Minnesota, Fine Theoretical Physics Institute (United States)

    2013-09-15

    In the three-dimensional topological insulator (TI), the physics of doped semiconductors exists literally side-by-side with the physics of ultrarelativistic Dirac fermions. This unusual pairing creates a novel playground for studying the interplay between disorder and electronic transport. In this mini-review, we focus on the disorder caused by the three-dimensionally distributed charged impurities that are ubiquitous in TIs, and we outline the effects it has on both the bulk and surface transport in TIs. We present self-consistent theories for Coulomb screening both in the bulk and at the surface, discuss the magnitude of the disorder potential in each case, and present results for the conductivity. In the bulk, where the band gap leads to thermally activated transport, we show how disorder leads to a smaller-than-expected activation energy that gives way to variable-range hopping at low temperatures. We confirm this enhanced conductivity with numerical simulations that also allow us to explore different degrees of impurity compensation. For the surface, where the TI has gapless Dirac modes, we present a theory of disorder and screening of deep impurities, and we calculate the corresponding zero-temperature conductivity. We also comment on the growth of the disorder potential in passing from the surface of the TI into the bulk. Finally, we discuss how the presence of a gap at the Dirac point, introduced by some source of time-reversal symmetry breaking, affects the disorder potential at the surface and the mid-gap density of states.

  8. Effects of bulk charged impurities on the bulk and surface transport in three-dimensional topological insulators

    International Nuclear Information System (INIS)

    Skinner, B.; Chen, T.; Shklovskii, B. I.

    2013-01-01

    In the three-dimensional topological insulator (TI), the physics of doped semiconductors exists literally side-by-side with the physics of ultrarelativistic Dirac fermions. This unusual pairing creates a novel playground for studying the interplay between disorder and electronic transport. In this mini-review, we focus on the disorder caused by the three-dimensionally distributed charged impurities that are ubiquitous in TIs, and we outline the effects it has on both the bulk and surface transport in TIs. We present self-consistent theories for Coulomb screening both in the bulk and at the surface, discuss the magnitude of the disorder potential in each case, and present results for the conductivity. In the bulk, where the band gap leads to thermally activated transport, we show how disorder leads to a smaller-than-expected activation energy that gives way to variable-range hopping at low temperatures. We confirm this enhanced conductivity with numerical simulations that also allow us to explore different degrees of impurity compensation. For the surface, where the TI has gapless Dirac modes, we present a theory of disorder and screening of deep impurities, and we calculate the corresponding zero-temperature conductivity. We also comment on the growth of the disorder potential in passing from the surface of the TI into the bulk. Finally, we discuss how the presence of a gap at the Dirac point, introduced by some source of time-reversal symmetry breaking, affects the disorder potential at the surface and the mid-gap density of states

  9. Valproate induced hepatic steatosis by enhanced fatty acid uptake and triglyceride synthesis

    International Nuclear Information System (INIS)

    Bai, Xupeng; Hong, Weipeng; Cai, Peiheng; Chen, Yibei; Xu, Chuncao; Cao, Di; Yu, Weibang; Zhao, Zhongxiang; Huang, Min; Jin, Jing

    2017-01-01

    Steatosis is the characteristic type of VPA-induced hepatotoxicity and may result in life-threatening hepatic lesion. Approximately 61% of patients treated with VPA have been diagnosed with hepatic steatosis through ultrasound examination. However, the mechanisms underlying VPA-induced intracellular fat accumulation are not yet fully understood. Here we demonstrated the involvement of fatty acid uptake and lipogenesis in VPA-induced hepatic steatosis in vitro and in vivo by using quantitative real-time PCR (qRT-PCR) analysis, western blotting analysis, fatty acid uptake assays, Nile Red staining assays, and Oil Red O staining assays. Specifically, we found that the expression of cluster of differentiation 36 (CD36), an important fatty acid transport, and diacylglycerol acyltransferase 2 (DGAT2) were significantly up-regulated in HepG2 cells and livers of C57B/6J mice after treatment with VPA. Furthermore, VPA treatment remarkably enhanced the efficiency of fatty acid uptake mediated by CD36, while this effect was abolished by the interference with CD36-specific siRNA. Also, VPA treatment significantly increased DGAT2 expression as a result of the inhibition of mitogen-activated protein kinase kinase (MEK) – extracellular regulated kinase (ERK) pathway; however, DGAT2 knockdown significantly alleviated VPA-induced intracellular lipid accumulation. Additionally, we also found that sterol regulatory element binding protein-1c (SREBP-1c)-mediated fatty acid synthesis may be not involved in VPA-induced hepatic steatosis. Overall, VPA-triggered over-regulation of CD36 and DGAT2 could be helpful for a better understanding of the mechanisms underlying VPA-induced hepatic steatosis and may offer novel therapeutic strategies to combat VPA-induced hepatotoxicity. - Highlights: • VPA induced hepatic steatosis and modulated genes associated with lipid metabolism. • CD36-mediated fatty acid uptake contributed to VPA-induced lipid accumulation. • PA increased the hepatic

  10. Valproate induced hepatic steatosis by enhanced fatty acid uptake and triglyceride synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Bai, Xupeng; Hong, Weipeng; Cai, Peiheng; Chen, Yibei; Xu, Chuncao [School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou (China); Cao, Di [School of Chinese Materia Medica, Guangzhou University of Chinese Medicine, Guangzhou (China); Yu, Weibang [School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou (China); Zhao, Zhongxiang [School of Chinese Materia Medica, Guangzhou University of Chinese Medicine, Guangzhou (China); Huang, Min [School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou (China); Jin, Jing, E-mail: jinjing@mail.sysu.edu.cn [School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou (China)

    2017-06-01

    Steatosis is the characteristic type of VPA-induced hepatotoxicity and may result in life-threatening hepatic lesion. Approximately 61% of patients treated with VPA have been diagnosed with hepatic steatosis through ultrasound examination. However, the mechanisms underlying VPA-induced intracellular fat accumulation are not yet fully understood. Here we demonstrated the involvement of fatty acid uptake and lipogenesis in VPA-induced hepatic steatosis in vitro and in vivo by using quantitative real-time PCR (qRT-PCR) analysis, western blotting analysis, fatty acid uptake assays, Nile Red staining assays, and Oil Red O staining assays. Specifically, we found that the expression of cluster of differentiation 36 (CD36), an important fatty acid transport, and diacylglycerol acyltransferase 2 (DGAT2) were significantly up-regulated in HepG2 cells and livers of C57B/6J mice after treatment with VPA. Furthermore, VPA treatment remarkably enhanced the efficiency of fatty acid uptake mediated by CD36, while this effect was abolished by the interference with CD36-specific siRNA. Also, VPA treatment significantly increased DGAT2 expression as a result of the inhibition of mitogen-activated protein kinase kinase (MEK) – extracellular regulated kinase (ERK) pathway; however, DGAT2 knockdown significantly alleviated VPA-induced intracellular lipid accumulation. Additionally, we also found that sterol regulatory element binding protein-1c (SREBP-1c)-mediated fatty acid synthesis may be not involved in VPA-induced hepatic steatosis. Overall, VPA-triggered over-regulation of CD36 and DGAT2 could be helpful for a better understanding of the mechanisms underlying VPA-induced hepatic steatosis and may offer novel therapeutic strategies to combat VPA-induced hepatotoxicity. - Highlights: • VPA induced hepatic steatosis and modulated genes associated with lipid metabolism. • CD36-mediated fatty acid uptake contributed to VPA-induced lipid accumulation. • PA increased the hepatic

  11. Synergetic scattering of SiO2 and Ag nanoparticles for light-trapping enhancement in organic bulk heterojunction

    Science.gov (United States)

    Yang, Huan; Ding, Qiuyu; Li, Ben Q.; Jiang, Xinbing; Zhang, Manman

    2018-02-01

    Though noble metal nanoparticles have been explored to enhance the performance of the organic solar cell, effect of dielectric nanoparticles, and coupled effect of dielectric and metal nanoparticles, have rarely been reported, if at all, on organic solar cell. This work reports an experimental study on synergetic scattering of SiO2 and Ag nanoparticles in a bulk organic heterojunction for the broadband light absorption enhancement. The wavelength scale SiO2 particles were arranged as a monolayer on the surface of the solar cell to guide incident light into the active layer and prolong the effective optical length of the entered energy. This is achieved by the excitation of whispering gallery modes in SiO2 nanoparticles and by leaky mode radiation. When small size Ag particles were incorporated into the transport layer of the solar cell, synergetic scattering of SiO2 and Ag nanoparticles is formed by coupling of the whispering gallery mode of closely arranged SiO2 particles atop and collaborative localized surface plasma resonance scattering of Ag nanoparticles dispersed in the transport layer. As a result, the performance of the organic solar cell is greatly enhanced and the short-circuit current density has an improvement of 42.47%. Therefore, the organic solar cell incorporated with SiO2 and Ag particles presents a meaningful strategy to achieve high energy-harvesting performance. [Figure not available: see fulltext.

  12. BULK AND TEMPLATE-FREE SYNTHESIS OF SILVER NANOWIRES USING CAFFEINE AT ROOM TEMPERATURE

    Science.gov (United States)

    A simple eco-friendly one-pot method is described to synthesize bulk quantities of nanowires of silver (Ag) using caffeine without the need of reducing agent, surfactants, and/or large amounts of insoluble templates. Chemical reduction of silver salts with caffeine dramatically c...

  13. Synthesis and Characterization of High Aluminum Zeolite X from Technical Grade Materials

    Directory of Open Access Journals (Sweden)

    Seyed Kamal Masoudian

    2013-06-01

    Full Text Available Zeolites are widely used as ion exchangers, adsorbents, separation materials and catalyst due to their well-tailored and highly-reproducible structures; therefore, the synthesis of zeolite from low grade resources can be interested. In the present work, high aluminum zeolite X was prepared from mixing technical grade sodium aluminate and sodium silicate solutions at temperatures between 70°C and 100°C. The synthesized zeolite X was characterized by SEM and X-ray methods according to ASTM standard procedures. The results showed that aging of the synthesis medium at the room temperature considerably increased the selectivity of zeolite X formation. On the other hand, high temperature of reaction mixture during crystallization formed zeolite A in the product; therefore, it decreased the purity of zeolite X. In addition, it was found that increasing H2O/Na2O and decreasing Na2O/SiO2 molar ratios in the reaction mixture resulted product with higher purity. © 2013 BCREC UNDIP. All rights reservedReceived: 7th January 2013; Revised: 7th April 2013; Accepted: 19th April 2013[How to Cite: Masoudian, S. K., Sadighi, S., Abbasi, A. (2013. Synthesis and Characterization of High Alu-minum Zeolite X from Technical Grade Materials. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1: 54-60. (doi:10.9767/bcrec.8.1.4321.54-60][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.1.4321.54-60] | View in  |

  14. Zone refining high-purity germanium

    International Nuclear Information System (INIS)

    Hubbard, G.S.; Haller, E.E.; Hansen, W.L.

    1977-10-01

    The effects of various parameters on germanium purification by zone refining have been examined. These parameters include the germanium container and container coatings, ambient gas and other operating conditions. Four methods of refining are presented which reproducibly yield 3.5 kg germanium ingots from which high purity (vertical barN/sub A/ - N/sub D/vertical bar less than or equal to2 x 10 10 cm -3 ) single crystals can be grown. A qualitative model involving binary and ternary complexes of Si, O, B, and Al is shown to account for the behavior of impurities at these low concentrations

  15. Preserving high-purity 233U

    International Nuclear Information System (INIS)

    Krichinsky, Alan; Giaquinto, Joe; Canaan, Doug

    2016-01-01

    The MARC X Conference hosted a workshop for the scientific community to communicate needs for high-purity 233 U and its by-products in order to preserve critical items otherwise slated for downblending and disposal. Currently, only small portions of the U.S. holdings of separated 233 U are being preserved. However, many additional kilograms of 233 U (>97 % pure) still are destined to be disposed, and it is unlikely that this material will ever be replaced due to a lack of operating production capability. Summaries of information conveyed at the workshop and feedback obtained from the scientific community are presented herein. (author)

  16. Towards the synthesis of hydroxyapatite/protein scaffolds with controlled porosities: bulk and interfacial shear rheology of a hydroxyapatite suspension with protein additives.

    Science.gov (United States)

    Maas, Michael; Bodnar, Pedro Marcus; Hess, Ulrike; Treccani, Laura; Rezwan, Kurosch

    2013-10-01

    The synthesis of porous hydroxyapatite scaffolds is essential for biomedical applications such as bone tissue engineering and replacement. One way to induce macroporosity, which is needed to support bone in-growth, is to use protein additives as foaming agents. Another reason to use protein additives is the potential to introduce a specific biofunctionality to the synthesized scaffolds. In this work, we study the rheological properties of a hydroxyapatite suspension system with additions of the proteins bovine serum albumin (BSA), lysozyme (LSZ) and fibrinogen (FIB). Both the rheology of the bulk phase as well as the interfacial shear rheology are studied. The bulk rheological data provides important information on the setting behavior of the thixotropic suspension, which we find to be faster with the addition of FIB and LSZ and much slower with BSA. Foam bubble stabilization mechanisms can be rationalized via interfacial shear rheology and we show that it depends on the growth of interfacial films at the suspension/air interface. These interfacial films support the stabilization of bubbles within the ceramic matrix and thereby introduce macropores. Due to the weak interaction of the protein molecules with the hydroxyapatite particles of the suspension, we find that BSA forms the most stable interfacial films, followed by FIB. LSZ strongly interacts with the hydroxyapatite particles and thus only forms thin films with very low elastic moduli. In summary, our study provides fundamental rheological insights which are essential for tailoring hydroxyapatite/protein suspensions in order to synthesize scaffolds with controlled porosities. Copyright © 2013 Elsevier Inc. All rights reserved.

  17. Low temperature synthesis & characterization of lead-free BCZT ceramics using molten salt method

    Science.gov (United States)

    Jai Shree, K.; Chandrakala, E.; Das, Dibakar

    2018-04-01

    Piezoelectric properties are greatly influenced by the synthesis route, microstructure, stoichiometry of the chemical composition, purity of the starting materials. In this study, molten salt method was used to prepare lead-free BCZT ceramics. Molten salt method is one of the simplestmethods to prepare chemically-purified, single phase powders in high yield often at lower temperatures and shorten reaction time. Calcination of the molten salt synthesized powders resulted in asingle-phase perovskite structure at 1000 °C which is ˜ 350 °C less than the conventional solid-sate reaction method. With increasing calcination temperature the average template size was increased (˜ 0.5-2 µm). Formation of well dispersive templates improves the sinterability at lower temperatures. Lead-free BCZT ceramics sintered at 1500 °C for 2 h resulted in homogenous and highly dense microstructure with ˜92% of the theoretical density and a grain size of ˜ 35 µm. This highly dense microstructure could enhance the piezoelectric properties of the system.

  18. Synthesis of selective extractor for minor actinide elements

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jong Seung [Konyang University, Nonsan (Korea); Cho, Moon Hwan [Kangwon National University, Chunchon (Korea)

    1998-04-01

    To selectively co-separate the lanthanide and actinide elements (MA) such as Am or Cm ion from radioactive waste, synthesis of diamide derivatives has been accomplished. In addition, picoline amide derivatives were also synthesized for selectively separate the minor actinide elements from lanthanide elements. The content of research has don are as follows: (1) synthesis of diamide as co-extractant (2) introduction of n-tetradecyl to increase the lipophilicity (3) Picolyl chloride, intermediate of the final product, was synthesized by improved method rather than reported method. (4) The length of alkyl side chain was adjusted to increase the lipophilicity of free ligand and its derivatives able to selectively separate the actinide metal from lanthanide metal ions was successfully synthesized and determined their purity by analytical instruments. (author). 12 refs., 28 figs.

  19. Biodiesel production using heterogeneous catalysts including wood ash and the importance of enhancing byproduct glycerol purity

    International Nuclear Information System (INIS)

    Uprety, Bijaya K.; Chaiwong, Wittavat; Ewelike, Chinomnso; Rakshit, Sudip K.

    2016-01-01

    Highlights: • Comparison of biodiesel production using homogeneous and heterogeneous catalysts. • Comparative study of CaO and CaO supported on alumina for biodiesel production. • Tradeoff between biodiesel conversion rate and purity. • Ash from birch bark and wood pellet industry explored as a potential catalyst. - Abstract: Transesterification of vegetable oils or animal fats with methanol in the presence of catalysts produces fatty acid methyl esters (FAME) and glycerol as a co-product. This study was focused on a comparative study of the transesterification of refined, bleached and deodorized palm oil (RBD palm oil) using a heterogeneous catalysts CaO with and without γ-alumina (γ-Al_2O_3) as a support. The results were also compared to that using sodium hydroxide (NaOH), which is a homogenous catalyst. Parameters like the amount of catalyst, the molar ratio of methanol to oil, reaction time and reaction temperature that affect methyl ester and glycerol formation were analyzed and the optimum conditions were determined. The FAME and glycerol content (96.75% and 92.73% respectively) obtained using CaO were lower in purity compared to that using CaO/Al_2O_3 (97.66% and 96.36% respectively). In the second phase of our work, wood ash from two different sources (birch bark & flyash from a biomass based power plant), which were calcined at 800 °C were studied for their potential use as a cheap renewable alternative heterogeneous catalyst. Both the wood ash samples were found to have good potential for use in such production process, but needs to be optimized further to obtain biodiesel which meets fuel biodiesel specifications. Both CaO and CaO supported on alumina produces FAME to levels that meet the fuel specifications required for blending with diesel. However, the latter produces a purer form of byproduct glycerol that can be easily converted to value added products, without the need for purification. On this basis the supported catalyst is

  20. Synthesis of racemic, R- and S-[1-11C]-β-hydroxybutyric acid

    International Nuclear Information System (INIS)

    Thorell, J.-O.; Stone-Elander, S.; Karolinska Hospital and Inst., Stockholm; Koenig, W.A.; Halldin, C.; Widen, L.

    1991-01-01

    Racemic, R- and S-β-hydroxybutyric acid were labelled with 11 C in the carboxylic position by a two-step stereospecific synthesis starting with carrier-added [ 11 C]cyanide and R/S, R- or S-propylene oxide. Hydrolysis of the intermediate nitrile with hydrochloric acid gave racemic [1- 11 C]-β-hydroxybutyric acid and R- or S-[1- 11 C]-β-hydroxybutyric acid with an enantiomeric excess of 87-97%. The total synthesis time (including HPLC purification) was 45-50 min from end of trapping. The isolated decay-corrected radiochemical yield was 20-30% based on [ 11 C]cyanide. The radiochemical purity of the products was > 99%]. (author)

  1. A new method for synthesis of As-Te chalcogenide films

    Science.gov (United States)

    Mochalov, Leonid; Nezhdanov, Aleksey; Usanov, Dmitry; Markelov, Aleksey; Trushin, Vladimir; Chidichimo, Giuseppe; De Filpo, Giovanni; Gogova, Daniela; Mashin, Aleksandr

    2017-11-01

    A novel Plasma Enhanced Chemical Vapor Deposition method for synthesis of amorphous AsxTe100-x (31 ≤ x ≤ 49) films is demonstrated. The innovative process has been developed in a non-equilibrium low-temperature argon plasma under reduced pressure, employing for the first time volatile As and Te as precursors. Utilization of inorganic precursors, in contrast to the typically used in CVD metal-organic precursors, has given us the chance to achieve ≿halcogenide As-Te films of very high quality and purity. Phase and structural evolution of the As-Te system, based on equilibrium coexistence of two phases (AsTe and As2Te3) has been studied. The dependence of structure and optical bandgap of the chalcogenide materials on their composition was established. The newly developed process is cost-effective and enables deposition of As-Te films with a thickness ranging from 10 nm to 10 μm, the latter is highly desireable for one-mode planar waveguides applications and in other components of integral optics.

  2. Preparation of 16α[18F] fluoro-17β-fluoroestradiol on domestic synthesis module

    International Nuclear Information System (INIS)

    Sun Chuanjin; Zhu Hong; Fang Keyuan

    2012-01-01

    To investigate the synthesis method of 16α-[ 18 F] fluoro-17β-fluoroestradiol on domestic synthesizing module, the automated synthesis was carried out through the reaction of 3-O-(methoxymethyl) -16,17-O-sulfuryl-16-epiestriol (MMSE, 1 mg) as precursor with 18 F- at 105 ℃ for 15 min in sealed system on domestic synthesizer, then 0.8 mL 1 mol/L HC1 dissolved in 7.2 mL acetonetrile was added in three parts to the reaction vessel for hydrolysis and hydrolysis reaction was performed at 105 ℃ for 6 min. The final reaction solution was purified by HPLC to give 18 F-FES. Preparation of 18 F-FES on domestic synthesis module was in the uncorrected synthesis yield of 8.2% (corrected synthesis yield 12.8%). Total synthesis time was about 70 min and radiochemical purity was higher than 98%. The product had good stability at room temperature. 18 F-FES injection can be prepared on domes- tic synthesis module and the quality can meet the requirements of radiopharmaceuticals for clinical use, (authors)

  3. Analysis technique of impurity in high purity deuterium by cryogenic gas-chromatography

    International Nuclear Information System (INIS)

    Zhou Junbo; Gao Liping

    2007-01-01

    A veracious and applicable quantitative analysis method of O 2 , N 2 and H 2 , HD in high purity deuterium by the chromatogram columniation filled with 5A molecular sieve and alumina was researched and constituted at natural temperature and 77 K, respectively. Minimum detecting limit of the present method is (150-200) x 10 -6 for H 2 and HD, and it can meet the need of quantitative analysis of the impurity during high purity deuterium preparation. (authors)

  4. Ehrenfest dynamics is purity non-preserving: A necessary ingredient for decoherence

    International Nuclear Information System (INIS)

    Alonso, J. L.; Clemente-Gallardo, J.; Cuchí, J. C.

    2012-01-01

    We discuss the evolution of purity in mixed quantum/classical approaches to electronic nonadiabatic dynamics in the context of the Ehrenfest model. As it is impossible to exactly determine initial conditions for a realistic system, we choose to work in the statistical Ehrenfest formalism that we introduced in Alonso et al. [J. Phys. A: Math. Theor. 44, 396004 (2011)]. From it, we develop a new framework to determine exactly the change in the purity of the quantum subsystem along with the evolution of a statistical Ehrenfest system. In a simple case, we verify how and to which extent Ehrenfest statistical dynamics makes a system with more than one classical trajectory, and an initial quantum pure state become a quantum mixed one. We prove this numerically showing how the evolution of purity depends on time, on the dimension of the quantum state space D, and on the number of classical trajectories N of the initial distribution. The results in this work open new perspectives for studying decoherence with Ehrenfest dynamics.

  5. Photoinduced Bulk Polarization and Its Effects on Photovoltaic Actions in Perovskite Solar Cells.

    Science.gov (United States)

    Wu, Ting; Collins, Liam; Zhang, Jia; Lin, Pei-Ying; Ahmadi, Mahshid; Jesse, Stephen; Hu, Bin

    2017-11-28

    This article reports an experimental demonstration of photoinduced bulk polarization in hysteresis-free methylammonium (MA) lead-halide perovskite solar cells [ITO/PEDOT:PSS/perovskite/PCBM/PEI/Ag]. An anomalous capacitance-voltage (CV) signal is observed as a broad "shoulder" in the depletion region from -0.5 to +0.5 V under photoexcitation based on CV measurements where a dc bias is gradually scanned to continuously drift mobile ions in order to detect local polarization under a low alternating bias (50 mV, 5 kHz). Essentially, gradually scanning the dc bias and applying a low alternating bias can separately generate continuously drifting ions and a bulk CV signal from local polarization under photoexcitation. Particularly, when the device efficiency is improved from 12.41% to 18.19% upon chlorine incorporation, this anomalous CV signal can be enhanced by a factor of 3. This anomalous CV signal can be assigned as the signature of photoinduced bulk polarization by distinguishing from surface polarization associated with interfacial charge accumulation. Meanwhile, replacing easy-rotational MA + with difficult-rotational formamidinium (FA + ) cations largely minimizes such anomalous CV signal, suggesting that photoinduced bulk polarization relies on the orientational freedom of dipolar organic cations. Furthermore, a Kelvin probe force microscopy study shows that chlorine incorporation can suppress the density of charged defects and thus enhances photoinduced bulk polarization due to the reduced screening effect from charged defects. A bias-dependent photoluminescence study indicates that increasing bulk polarization can suppress carrier recombination by decreasing charge capture probability through the Coulombic screening effect. Clearly, our studies provide an insightful understanding of photoinduced bulk polarization and its effects on photovoltaic actions in perovskite solar cells.

  6. Synthesis, characterization and catalytic application of silica supported tin oxide nanoparticles for synthesis of 2,4,5-tri and 1,2,4,5-tetrasubstituted imidazoles under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Ashok V. Borhade

    2017-02-01

    Full Text Available Highly efficient and eco-friendly, one pot synthesis of 1,2,4,5-tetra substituted imidazoles and 2,4,5-trisubstituted imidazoles was reported under solvent free conditions using nanocrystalline silica supported tin oxide (SiO2:SnO2 as a catalyst with excellent yield. The present methodology offers several advantages such as mild reaction conditions, short reaction time, good yield, high purity of product, recyclable catalyst without a noticeable decrease in catalytic activity and can be used for large scale synthesis. The synthesized SiO2:SnO2 nanocrystalline catalyst was characterized by XRD, BET surface area and TEM techniques.

  7. Synthesis and characterization of Taurine

    Directory of Open Access Journals (Sweden)

    B Bayarmaa

    2014-10-01

    Full Text Available Have been obtained 2-aminoethanesulfonic acid (taurine from ethanolamine, sulfuric acid and sodium sulfite during the synthesis in laboratory condition. The process involves two steps of reactions, the first was esterification of ethanolamine with sulfuric acid to produce the intermediate product of 2-aminoethyl ester which than was extended to the second step by sulfonation with sodium sulfite to produce 2-aminoethanesulfonic acid. Resulting product was analyzed using 1H-NMR, IR, FAB-MS analysis and examined purity characterizations of the synthesized products. DOI: http://dx.doi.org/10.5564/mjc.v14i0.200 Mongolian Journal of Chemistry 14 (40, 2013, p57-60

  8. Research progress in the electrochemical synthesis of ferrate(VI)

    International Nuclear Information System (INIS)

    Macova, Zuzana; Bouzek, Karel; Hives, Jan; Sharma, Virender K.; Terryn, Raymond J.; Baum, J. Clayton

    2009-01-01

    There is renewed interest in the +6 oxidation state of iron, ferrate (VI) (Fe VI O 4 2- ), because of its potential as a benign oxidant for organic synthesis, as a chemical in developing cleaner ('greener') technology for remediation processes, and as an alternative for environment-friendly battery cathodes. This interest has led many researchers to focus their attention on the synthesis of ferrate(VI). Of the three synthesis methods, electrochemical, wet chemical and thermal, electrochemical synthesis has received the most attention due to its ease and the high purity of the product. Moreover, electrochemical processes use an electron as a so-called clean chemical, thus avoiding the use of any harmful chemicals to oxidize iron to the +6 oxidation state. This paper reviews the development of electrochemical methods to synthesize ferrate(VI). The approaches chosen by different laboratories to overcome some of the difficulties associated with the electrochemical synthesis of ferrate(VI) are summarized. Special attention is paid to parameters such as temperature, anolyte, and anode material composition. Spectroscopic work to understand the mechanism of ferrate(VI) synthesis is included. Recent advances in two new approaches, the use of an inert electrode and molten hydroxide salts, in the synthesis of ferrate(VI) are also reviewed. Progress made in the commercialization of ferrate(VI) continuous production is briefly discussed as well

  9. Preparation of 18F-FDG by basic hydrolysis on '1-pot' FDG synthesis module

    International Nuclear Information System (INIS)

    Li Qiming; Jin Rongbing; Fan Xijiang

    2007-01-01

    '1-pot' equipment is an automatic synthesis module of producing 18 F-FDG by acid hydrolysis process. Simple changes in the chemistry, plumbing, and programming of CPCU enable two back-to-back '1-pot' systems in a unit. The preparation of precursor of 18 F-FDG is the same with origin. The results of experiments showed that by basic hydrolysis procedure, the synthesis time is shorten from 45-50 min to 30-35 min, uncorrected synthesis yield can be increased from 45%-50% to 60%-65%, and the preparing procedure is stable. The quality of 18 F-FDG meets the requirements under USP fludeoxyglucose 18 F injection, radiochemical purity is more than 99% especially by HPLC. With '1-pot' FDG synthesis module Chemical Processing Control Unit (CPCU), 18 F-FDG can be prepared by basic hydrolysis process. (authors)

  10. High-pressure-assisted synthesis of high-volume ZnGeP2 polycrystalline

    Science.gov (United States)

    Huang, Changbao; Wu, Haixin; Xiao, Ruichun; Chen, Shijing; Ma, Jiaren

    2018-06-01

    The pnictide and chalcogenide semiconductors are promising materials for the applications in the field of photoelectric. High-purity and high-volume polycrystalline required in the real-world applications is hard to be synthesized due to the high vapor pressure of phosphorus and sulfur components at high temperature. A new high-pressure-resisted method was used to investigate the synthesis of the nonlinear-optical semiconductor ZnGeP2. The high-purity ZnGeP2 polycrystalline material of approximately 500 g was synthesized in one run, which enables the preparation of nominally stoichiometric material. Since increasing internal pressure resistance of quartz crucible and reducing the reaction space, the high-pressure-resisted method can be used to rapidly synthesize other pnictide and chalcogenide semiconductors and control the components ratio.

  11. The synthesis of a tritium, carbon-14, and stable isotope-labeled cathepsin C inhibitors.

    Science.gov (United States)

    Allen, Paul; Bragg, Ryan A; Caffrey, Moya; Ericsson, Cecilia; Hickey, Michael J; Kingston, Lee P; Elmore, Charles S

    2017-02-01

    As part of a medicinal chemistry program aimed at developing a highly potent and selective cathepsin C inhibitor, tritium, carbon-14, and stable isotope-labeled materials were required. The synthesis of tritium-labeled methanesulfonate 5 was achieved via catalytic tritiolysis of a chloro precursor, albeit at a low radiochemical purity of 67%. Tritium-labeled AZD5248 was prepared via a 3-stage synthesis, utilizing amide-directed hydrogen isotope exchange. Carbon-14 and stable isotope-labeled AZD5248 were successfully prepared through modifications of the medicinal chemistry synthetic route, enabling the use of available labeled intermediates. Copyright © 2016 John Wiley & Sons, Ltd.

  12. Acetylsalicylic acid: Incoming 150 years of the first synthesis

    Directory of Open Access Journals (Sweden)

    Mijin Dušan Ž.

    2002-01-01

    Full Text Available Acetylsalicylic acid is one of the most fascinating and versatile drugs known to medicine, as well as one of the oldest. Acetylsalicylic acid is a drug which is safe, with analgetic, antirheumatic, anti-inflammatory antiplatelet and antithrombotic action. It may be applied not only in clinical practice, but also as prevention. The first known use of an acetylsalicylic acid-like preparation can be traced to ancient Greece. In 1853 Charles Gerhardt published the first synthesis of acetylsalicylic acid. Felix Hoffmann, a chemist for Friedrich Bayer, a German dye company obtained a patent on acetylsalicylic acid some 40 years later. Bayer coined the name Aspirin for the new product. The 20 in century was the century in which many researchers in many companies tried to improve the synthesis of acetylsalicylic acid not only in terms of yield but also purity. This paper describes the history, use, mechanism of action, synthesis and production as well as the purification and stability of acetylsalicylic acid.

  13. Synthesis of sub-millimeter calcite from aqueous solution

    Science.gov (United States)

    Reimi, M. A.; Morrison, J. M.; Burns, P. C.

    2011-12-01

    A novel aqueous synthesis that leads to the formation of calcite (CaCO3) crystals, up to 500μm in diameter, will be used to facilitate the study of contaminant transport in aqueous environmental systems. Existing processes tend to be complicated and often yield nanometer-sized or amorphous CaCO3. The synthesis method presented here, which involves slow mixing of concentrated solutions of CaCl2 ¬and (NH4)2CO3, produces single crystals of rhombohedral calcite in 2 to 4 days. Variations on the experimental method, including changes in pH and solution concentration, were explored to optimize the synthesis. Scanning Electron Microscope images show the differences in size and purity observed when the crystals are grown at pH values ranging from 2 to 6. The crystals grown from solutions of pH 2 were large (up to 500 micrometers in diameter) with minimal polycrystalline calcium carbonate, while crystals grown from solutions with pH values beyond 4 were smaller (up to 100 micrometers in diameter) with significant polycrystalline calcium carbonate. The synthesis method, materials characterization, and use in future actinide contaminant studies will be discussed.

  14. The analytical of radiochemical purity of tumor receptor imaging agent 99Tcm-octreotide

    International Nuclear Information System (INIS)

    Wang Xufu; Zuo Shuyao; Shao Wenbo; Wang Guoming; Sun Jianwen; Zhang Qin

    2003-01-01

    The radiochemical purity of tumor receptor imaging agent 99 Tc m -octreotide is measured by High Pressure Liquid Chromatography (HPLC) and two systems of chromatography combining method of silver stain. The results show that the radiochemical purity of 98 Tc m -octreotide measured by both methods are effective and correct. It can separate 99 Tc m -octreotide from other radioactive compositions correctly and effectively

  15. Evaluation of radiochemical purities of some radiopharmaceuticals in Shiraz Namazi teaching hospital

    Directory of Open Access Journals (Sweden)

    Hossein Sadeghpour

    2015-03-01

    Full Text Available Many radiopharmaceuticals, as a special group of drugs, are eventually prepared at the nuclear medicine departments of the hospitals. Therefore, their quality control procedures such as sterility tests, radionuclide, radiochemical and chemical purity should be carried out in the hospitals. In this study, radiochemical purity for more than 300 preparations of three different radiopharmaceutical formulations from commercial kits were tested using instant thin layer chromatography. The formulations 99mTc-DTPA, 99mTc-MDP and 99mTc-MIBI were obtained from Pars Isotope Co. Several paper chromatographic systems including standard and factory recommended thin layer chromatography systems were used in this study. In addition different equipments for detection of radioactivity in paper chromatography like gamma camera and dose calibrator were used. The results showed that the most observed impurities were hydrolyzed reduced technetium (HR-Tc. There were no significant differences between calculated 99mTc-MIBI radiochemical purities when the radioactive detection device was gamma camera instead of dose calibrator. In case of 99mTc-DTPA and 99mTc-MDP, there were significant differences in detection of HR-Tc. On the contrary, no significant differences in free pertechnetate were observed when package insert procedures for quality control were used instead of those recommended in the references. Finally, we observed that the package insert procedures for quality control can offer higher radiochemical purities.

  16. Nanocrystalline Ni-Co Alloy Synthesis by High Speed Electrodeposition

    OpenAIRE

    Idris, Jamaliah; Christian, Chukwuekezie; Gaius, Eyu

    2013-01-01

    Electrodeposition of nanocrystals is economically and technologically viable production path for the synthesis of pure metals and alloys both in coatings and bulk form. The study presents nanocrystalline Ni-Co alloy synthesis by high speed electrodeposition. Nanocrystalline Ni-Co alloys coatings were prepared by direct current (DC) and deposited directly on steel and aluminum substrates without any pretreatment, using high speed electrodeposition method. The influence of the electrolysis par...

  17. Synthesis of nanometer-sized fayalite and magnesium-iron(II) mixture olivines

    Energy Technology Data Exchange (ETDEWEB)

    Qafoku, Odeta; Ilton, Eugene S.; Bowden, Mark E.; Kovarik, Libor; Zhang, Xin; Kukkadapu, Ravi K.; Engelhard, Mark H.; Thompson, Christopher J.; Schaef, Herbert T.; McGrail, Bernard Peter; Rosso, Kevin M.; Loring, John S.

    2018-04-01

    Olivines are divalent orthosilicates with important geologic, biological, and industrial significance and are typically comprised of mixtures of Mg2+ and Fe2+ ranging from forsterite (Mg2SiO4) to fayalite (Fe2SiO4). Investigating the role of Fe(II) in olivine reactivity requires the ability to synthesize olivines that are nanometer-sized, have different percentages of Mg2+ and Fe2+, and have good bulk and surface purity. This article demonstrates a new method for synthesizing nanosized fayalite and Mg-Fe mixture olivines. First, carbonaceous precursors are generated from sucrose, PVA, colloidal silica, Mg2+, and Fe3+. Second, these precursors are calcined in air to burn carbon and create mixtures of Fe(III)-oxides, forsterite, and SiO2. Finally, calcination in reducing CO-CO2 gas buffer leads to Fe(II)-rich olivines. XRD, Mössbauer, and IR analyses verify good bulk purity and composition. XPS indicates that surface iron is in its reduced Fe(II) form, and surface Si is consistent with olivine. SEM shows particle sizes predominately between 50 and 450 nm, and BET surface areas are 2.8-4.2 m2/g. STEM HAADF analysis demonstrates even distributions of Mg and Fe among the available M1 and M2 sites of the olivine crystals. These nanosized Fe(II)-rich olivines are suitable for laboratory studies with in situ probes that require mineral samples with high reactivity at short timescales.

  18. High purity neodymium acetate from mixed rare earth carbonates

    International Nuclear Information System (INIS)

    Queiroz, Carlos A. da Silva; Rocha, Soraya M. Rizzo da; Vasconcellos, Mari E. de; Lobo, Raquel M.; Seneda, Jose A.; Pedreira, Walter dos R.

    2011-01-01

    A simple and economical chemical process for obtaining high purity neodymium acetate is discussed. The raw material in the form rare earth carbonate is produced industrially from the chemical treatment of Brazilian monazite. Ion exchange chromatography technique with a strong cationic resin, proper to water treatment, and without the use of retention ions was used for the fractionating of the rare earth elements (REE). In this way, it was possible to obtain 99.9% pure Nd 2 O 3 in yields greater than or equal 80%, with the elution of the REE using ammonium salt of ethylenediaminetetraacetic acid (EDTA) solution in pH controlled. The complex of EDTA-neodymium was transformed into neodymium oxide, which was subsequently dissolved in acetic acid to obtain the neodymium acetates. Molecular absorption spectrophotometry was used to monitor the neodymium content during the process and sector field inductively coupled plasma mass spectrometry was used to certify the purity of the neodymium acetates. The typical neodymium acetates obtained contain the followings contaminants in μg g -1 : Sc(5.1); Y (0.9); La (1.0); Ce (6.1); Pr (34,4); Sm (12.8); Eu (1.1); Gd (15.4); Tb (29.3); Dy (5.2), Ho(7.4); Er (14.6); Tm (0.3); Yb (2.5); Lu (1.0). The high purity neodymium acetates obtained from this procedure have been applied, replacing the imported product, in research and development area on rare earth catalysts. (author)

  19. Synthesis of [11C]PBR170, a novel imidazopyridine, for imaging the translocator protein with PET

    International Nuclear Information System (INIS)

    Bourdier, Thomas; Henderson, David; Fookes, Christopher J.R.; Lam, Peter; Mattner, Filomena; Fulham, Michael; Katsifis, Andrew

    2014-01-01

    The translocator protein (TSPO) ligand 2-(6,8-dichloro-2-(4-ethoxyphenyl)imidazo[1,2-a]pyridin-3-yl) –N-(2-fluoropyridin-3-yl)–N-methylacetamide (PBR170), is a novel imidazopyridineacetamide with high affinity (2.6 nm) and selectivity for the TSPO. The synthesis of [ 11 C]PBR170 was accomplished by N-methylation of the corresponding desmethyl precursor with [ 11 C]methyl iodide in the presence of sodium hydroxide in dimethylformamide. [ 11 C]PBR170 was produced in 30–45% radiochemical yield (decay-corrected, based on [ 11 C]methyl iodide) with a radiochemical purity >98% and a specific activity of 90–190 GBq/μmol after 35 min of synthesis time. - Highlights: • Radiosynthesis of a novel ligand PBR170 with carbon-11. • 30–45% radiochemical yield (decay-corrected, based on [ 11 C]methyl iodide). • Radiosynthesis and formulation achieved in 35 min. • High radiochemical purity (>98%) and specific activity (90–190 GBq/µmol). • High affinity and selectivity for the translocator protein (TSPO)

  20. Pulsed Field Waveforms for Magnetization of HTS Gd-Ba-Cu-O Bulk Magnets

    International Nuclear Information System (INIS)

    Ida, T; Matsuzaki, H; Morita, E; Sakashita, H; Harada, T; Ogata, H; Kimura, Y; Miki, M; Kitano, M; Izumi, M

    2006-01-01

    Progress in pulse magnetization technique for high-temperature superconductor bulks of melt-textured RE-Ba-Cu-O with large diameter is important for the realization of power applications. We studied the pulsed power source and pulsed field waveforms to enhance to improve the magnetization properties for Gd-Ba-Cu-O bulk. The risetime and duration of pulse waveform effectively varied distribution of magnetic flux

  1. Mesoporous CdS via Network of Self-Assembled Nanocrystals: Synthesis, Characterization and Enhanced Photoconducting Property.

    Science.gov (United States)

    Patra, Astam K; Banerjee, Biplab; Bhaumik, Asim

    2018-01-01

    Semiconduction nanoparticles are intensively studied due to their huge potential in optoelctronic applications. Here we report an efficient chemical route for hydrothermal synthesis of aggregated mesoporous cadmium sulfide (CdS) nanoparticles using supramolecular-assembly of ionic and water soluble sodium salicylate as the capping agent. The nanostructure, mesophase, optical property and photoconductivity of these mesoporous CdS materials have been characterized by using small and wide angle powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N2-sorption, Raman analysis, Fourier transformed infrared (FT-IR), UV-Visible DSR spectroscopy, and photoconductivity measurement. Wide angle XRD pattern and high resolution TEM image analysis suggested that the particle size of the materials is within 10 nm and the nanoparticles are in well-crystallized cubic phase. Mesoporous CdS nanoparticles showed drastically enhanced photoelectrochemical response under visible light irradiation on entrapping a photosensitizer (dye) molecule in the interparticle spaces. Efficient synthesis strategy and the enhanced photo response in the mesoporous CdS material could facilitate the designing of other porous semiconductor oxide/sulfide and their applications in photon-to-electron conversion processes.

  2. The Advanced Aluminum Nitride Synthesis Methods and Its Applications: Patent Review.

    Science.gov (United States)

    Shishkin, Roman A; Elagin, Andrey A; Mayorova, Ekaterina S; Beketov, Askold R

    2016-01-01

    High purity nanosized aluminum nitride synthesis is a current issue for both industry and science. However, there is no up-to-date review considering the major issues and the technical solutions for different methods. This review aims to investigate the advanced methods of aluminum nitride synthesis and its development tendencies. Also the aluminum nitride application patents and prospects for development of the branch have been considered. The patent search on "aluminum nitride synthesis" has been carried out. The research activity has been analyzed. Special attention has been paid to the patenting geography and the leading researchers in aluminum nitride synthesis. Aluminum nitride synthesis methods have been divided into 6 main groups, the most studied approaches are carbothermal reduction (88 patents) and direct nitridation (107 patents). The current issues for each group have been analyzed; the main trends are purification of the final product and nanopowder synthesis. The leading researchers in aluminum nitride synthesis have represented 5 countries, namely: Japan, China, Russia, South Korea and USA. The main aluminum nitride application spheres are electronics (59,1 percent of applications) and new materials manufacturing (30,9 percent). The review deals with the state of the art data in nanosized aluminum nitride synthesis, the major issues and the technical solutions for different synthesis methods. It gives a full understanding of the development tendencies and of the current leaders in the sphere.

  3. Sodium lauryl sulfate - a biocide for controlling acidity development in bulk commercially formed solid elemental sulfur

    Energy Technology Data Exchange (ETDEWEB)

    Hyne, J. B. [Calgary Univ., AB (Canada). Dept. of Biological Sciences

    1996-04-01

    Acidification of bulk elemental sulfur caused by Thiobacillus species which consume elemental sulfur by converting it into oxidized sulfur forms, was studied. Contributory factors, such as length of time in transit or in storage, warm temperatures, the presence of air and moisture, particle size and form of sulfur, and the presence of sources of carbon, nitrogen and phosphorus nutrients, were reviewed. Laboratory experiments with adding sodium lauryl sulfate (SLS), a known biocide, to sulfur inoculated with Thiobacillus, proved to be an efficient method for controlling acidity development. At the concentration required for effectiveness SLS did not interfere with purity specifications, had negligible effect on moisture, and appeared to be compatible with current dust suppression application practices. 2 tabs., 3 figs.

  4. Synthesis of N-[methyl-11C]hydromorphone by using multivariate strategies for optimization of radiochemical yields

    International Nuclear Information System (INIS)

    Rimland, Annika; Bergson, Goeran; Obenius, Ulf; Sjoeberg, Stefan; Langstroem, Bengt

    1987-01-01

    The synthesis of N-[methyl- 11 C]hydromorphone has been performed by using [ 11 C]methyl iodide and desmethyl hydromorphone in a mixture of dimethylsulphoxide and dimethylformamide as solvent. Optimization of the radiochemical yield by varying the reaction conditions was performed by using multivariate strategies. The labelled hydromorphone was obtained in 72% radiochemical yield in the alkylation reaction with [ 11 C]-methyl iodide, counted from the end of the [ 11 C]methyl iodide synthesis. N-[Methyl- 11 C]hydromorphone was obtained as a ready injectable pharmaceutical solution with a total synthesis time of 40 min and in a 10% total radiochemical yield, with a radiochemical purity > 99.5%, according to HPLC analysis. (author)

  5. Mesophase Formation Stabilizes High-purity Magic-sized Clusters

    KAUST Repository

    Nevers, Douglas R.; Williamson, Curtis B.; Savitzky, Benjamin H; Hadar, Ido; Banin, Uri; Kourkoutis, Lena F.; Hanrath, Tobias; Robinson, Richard D.

    2018-01-01

    Magic-sized clusters (MSCs) are renowned for their identical size and closed-shell stability that inhibit conventional nanoparticle (NP) growth processes. Though MSCs have been of increasing interest, understanding the reaction pathways toward their nucleation and stabilization is an outstanding issue. In this work, we demonstrate that high concentration synthesis (1000 mM) promotes a well-defined reaction pathway to form high-purity MSCs (>99.9%). The MSCs are resistant to typical growth and dissolution processes. Based on insights from in-situ X-ray scattering analysis, we attribute this stability to the accompanying production of a large, hexagonal organic-inorganic mesophase (>100 nm grain size) that arrests growth of the MSCs and prevents NP growth. At intermediate concentrations (500 mM), the MSC mesophase forms, but is unstable, resulting in NP growth at the expense of the assemblies. These results provide an alternate explanation for the high stability of MSCs. Whereas the conventional mantra has been that the stability of MSCs derives from the precise arrangement of the inorganic structures (i.e., closed-shell atomic packing), we demonstrate that anisotropic clusters can also be stabilized by self-forming fibrous mesophase assemblies. At lower concentration (<200 mM or >16 acid-to-metal), MSCs are further destabilized and NPs formation dominates that of MSCs. Overall, the high concentration approach intensifies and showcases inherent concentration-dependent surfactant phase behavior that is not accessible in conventional (i.e., dilute) conditions. This work provides not only a robust method to synthesize, stabilize, and study identical MSC products, but also uncovers an underappreciated stabilizing interaction between surfactants and clusters.

  6. Mesophase Formation Stabilizes High-purity Magic-sized Clusters

    KAUST Repository

    Nevers, Douglas R.

    2018-01-27

    Magic-sized clusters (MSCs) are renowned for their identical size and closed-shell stability that inhibit conventional nanoparticle (NP) growth processes. Though MSCs have been of increasing interest, understanding the reaction pathways toward their nucleation and stabilization is an outstanding issue. In this work, we demonstrate that high concentration synthesis (1000 mM) promotes a well-defined reaction pathway to form high-purity MSCs (>99.9%). The MSCs are resistant to typical growth and dissolution processes. Based on insights from in-situ X-ray scattering analysis, we attribute this stability to the accompanying production of a large, hexagonal organic-inorganic mesophase (>100 nm grain size) that arrests growth of the MSCs and prevents NP growth. At intermediate concentrations (500 mM), the MSC mesophase forms, but is unstable, resulting in NP growth at the expense of the assemblies. These results provide an alternate explanation for the high stability of MSCs. Whereas the conventional mantra has been that the stability of MSCs derives from the precise arrangement of the inorganic structures (i.e., closed-shell atomic packing), we demonstrate that anisotropic clusters can also be stabilized by self-forming fibrous mesophase assemblies. At lower concentration (<200 mM or >16 acid-to-metal), MSCs are further destabilized and NPs formation dominates that of MSCs. Overall, the high concentration approach intensifies and showcases inherent concentration-dependent surfactant phase behavior that is not accessible in conventional (i.e., dilute) conditions. This work provides not only a robust method to synthesize, stabilize, and study identical MSC products, but also uncovers an underappreciated stabilizing interaction between surfactants and clusters.

  7. Radiation Synthesis and Application of Absorbent Hydrogels to Enhance the Quality of Basadiesel

    International Nuclear Information System (INIS)

    Nguyen Duy Hang; Pham Thi Le Ha; Tran Thi Thuy; Le Hai; Nguyen Tan Man; Le Huu Tu; Nguyen Trong Hoanh Phong; Tran Thi Tam; Tran Thu Hong; Pham Thi Sam; Nguyen Tuong Li Lan

    2013-01-01

    Studying on the using ability of radiation synthesis hydrogels to enhance the quality of the biodiesel produced from Basa fish oil was implemented. Radiation synthesis of absorbent hydrogels and their application to removal of contaminants from biodiesel produced from fish oil were the major problems. The preparation of the super absorbent hydrogel obtained by radiation induced cross linking of polyacrylamide and polyacrylic was investigated and its application in removal of water, catalyst from the basadiesel emulsion is reported. The hydrogels were characterized in terms of gel content, swelling, character of water and mineral catalyst removal were studied. The effect of temperature, NaOH and KOH content of solution on the swelling degree of hydrogels was also determined. The results showed that the gel fraction of PAAm/PAAc hydrogel with PAAm/AAc (1/4) ratio and dose of 20 kGy was used to synthesized the Gel of A-311. Studies also made on the application of Gel A-311 during the refining process in Basadiesel industry. (author)

  8. Enhanced Synthesis of Alkyl Amino Acids in Miller's 1958 H2S Experiment

    Science.gov (United States)

    Parker, Eric T.; Cleaves, H. James; Callahan, Michael P.; Dworkin, James P.; Glavin, Daniel P.; Lazcano, Antonio; Bada, Jeffrey L.

    2011-01-01

    Stanley Miller's 1958 H2S-containing experiment, which included a simulated prebiotic atmosphere of methane (CH4), ammonia (NH3), carbon dioxide (CO2), and hydrogen sulfide (H2S) produced several alkyl amino acids, including the alpha-, beta-, and gamma-isomers of aminobutyric acid (ABA) in greater relative yields than had previously been reported from his spark discharge experiments. In the presence of H2S, aspariic and glutamic acids could yield alkyl amino acids via the formation of thioimide intermediates. Radical chemistry initiated by passing H2S through a spark discharge could have also enhanced alkyl amino acid synthesis by generating alkyl radicals that can help form the aldehyde and ketone precursors to these amino acids. We propose mechanisms that may have influenced the synthesis of certain amino acids in localized environments rich in H2S and lightning discharges, similar to conditions near volcanic systems on the early Earth, thus contributing to the prebiotic chemical inventory of the primordial Earth.

  9. JOYO coolant sodium and cover gas purity control database (MK-II core)

    International Nuclear Information System (INIS)

    Ito, Kazuhiro; Nemoto, Masaaki

    2000-03-01

    The experimental fast reactor 'JOYO' served as the MK-II irradiation bed core for testing fuel and material for FBR development for 15 years from 1982 to 1997. During the MK-II operation, impurities concentrations in the sodium and the argon gas were determined by 67 samples of primary sodium, 81 samples of secondary sodium, 75 samples of primary argon gas, 89 samples of secondary argon gas (the overflow tank) and 89 samples of secondary argon gas (the dump tank). The sodium and the argon gas purity control data were accumulated from in thirty-one duty operations, thirteen special test operations and eight annual inspections. These purity control results and related plant data were compiled into database, which were recorded on CD-ROM for user convenience. Purity control data include concentration of oxygen, carbon, hydrogen, nitrogen, chlorine, iron, nickel and chromium in sodium, concentration of oxygen, hydrogen, nitrogen, carbon dioxide, methane and helium in argon gas with the reactor condition. (author)

  10. Bulk damage and absorption in fused silica due to high-power laser applications

    Science.gov (United States)

    Nürnberg, F.; Kühn, B.; Langner, A.; Altwein, M.; Schötz, G.; Takke, R.; Thomas, S.; Vydra, J.

    2015-11-01

    Laser fusion projects are heading for IR optics with high broadband transmission, high shock and temperature resistance, long laser durability, and best purity. For this application, fused silica is an excellent choice. The energy density threshold on IR laser optics is mainly influenced by the purity and homogeneity of the fused silica. The absorption behavior regarding the hydroxyl content was studied for various synthetic fused silica grades. The main absorption influenced by OH vibrational excitation leads to different IR attenuations for OH-rich and low-OH fused silica. Industrial laser systems aim for the maximum energy extraction possible. Heraeus Quarzglas developed an Yb-doped fused silica fiber to support this growing market. But the performance of laser welding and cutting systems is fundamentally limited by beam quality and stability of focus. Since absorption in the optical components of optical systems has a detrimental effect on the laser focus shift, the beam energy loss and the resulting heating has to be minimized both in the bulk materials and at the coated surfaces. In collaboration with a laser research institute, an optical finisher and end users, photo thermal absorption measurements on coated samples of different fused silica grades were performed to investigate the influence of basic material properties on the absorption level. High purity, synthetic fused silica is as well the material of choice for optical components designed for DUV applications (wavelength range 160 nm - 260 nm). For higher light intensities, e.g. provided by Excimer lasers, UV photons may generate defect centers that effect the optical properties during usage, resulting in an aging of the optical components (UV radiation damage). Powerful Excimer lasers require optical materials that can withstand photon energy close to the band gap and the high intensity of the short pulse length. The UV transmission loss is restricted to the DUV wavelength range below 300 nm and

  11. Leucine stimulates protein synthesis in skeletal muscle of neonatal pigs by enhancing mTORC1 activation.

    Science.gov (United States)

    Suryawan, Agus; Jeyapalan, Asumthia S; Orellana, Renan A; Wilson, Fiona A; Nguyen, Hanh V; Davis, Teresa A

    2008-10-01

    Skeletal muscle in the neonate grows at a rapid rate due in part to an enhanced sensitivity to the postprandial rise in amino acids, particularly leucine. To elucidate the molecular mechanism by which leucine stimulates protein synthesis in neonatal muscle, overnight-fasted 7-day-old piglets were treated with rapamycin [an inhibitor of mammalian target of rapamycin (mTOR) complex (mTORC)1] for 1 h and then infused with leucine for 1 h. Fractional rates of protein synthesis and activation of signaling components that lead to mRNA translation were determined in skeletal muscle. Rapamycin completely blocked leucine-induced muscle protein synthesis. Rapamycin markedly reduced raptor-mTOR association, an indicator of mTORC1 activation. Rapamycin blocked the leucine-induced phosphorylation of mTOR, S6 kinase 1 (S6K1), and eukaryotic initiation factor (eIF)4E-binding protein-1 (4E-BP1) and formation of the eIF4E.eIF4G complex and increased eIF4E.4E-BP1 complex abundance. Rapamycin had no effect on the association of mTOR with rictor, a crucial component for mTORC2 activation, or G protein beta-subunit-like protein (GbetaL), a component of mTORC1 and mTORC2. Neither leucine nor rapamycin affected the phosphorylation of AMP-activated protein kinase (AMPK), PKB, or tuberous sclerosis complex (TSC)2, signaling components that reside upstream of mTOR. Eukaryotic elongation factor (eEF)2 phosphorylation was not affected by leucine or rapamycin, although current dogma indicates that eEF2 phosphorylation is mTOR dependent. Together, these in vivo data suggest that leucine stimulates muscle protein synthesis in neonates by enhancing mTORC1 activation and its downstream effectors.

  12. Enantioselective synthesis of no-carrier added (NCA) 6-[18F]Fluoro-L-Dopa

    International Nuclear Information System (INIS)

    Duanzhi Yin; Lan Zhang; Yongxian Wang; Ganghua Tang; First Military Medical Univ., Guangzhou; Xiaolan Tang

    2003-01-01

    6-[ 18 F]Fluoro-L-Dopa (6-FDOPA) is the analogue of L-Dopa, the biosynthesis precursor for dopamine. As a PET tracer, it was widely applied for the presynaptic dopamine function studies in human brain. The application of a chiral phase-transfer-catalyst (PTC) in enantioselective synthesis of N.C.A. 6-[ 18 F]Fluoro-L-Dopa has been developed recently. An improved procedure was described. The labeling precursor (6-Trimethylammoniumveratraldehyde Triflate) and PTC (O-Allyl-N-(9)-anthracenylcinchonidinium Bromide) were synthesized. A successful synthesis route was developed for the preparation of 6-[ 18 F]Fluoro-L-Dopa with high radiochemical yields (4-9%, decay uncorrected) and short synthesis time(80min). The radiochemical purity was over 99% and no D-isomer was detected by HPLC analysis using a chiral mobile phase. (author)

  13. Multifunctional silver nanoparticle-doped silica for solid-phase extraction and surface-enhanced Raman scattering detection

    Science.gov (United States)

    Markina, Natalia E.; Markin, Alexey V.; Zakharevich, Andrey M.; Gorin, Dmitry A.; Rusanova, Tatiana Yu.; Goryacheva, Irina Yu.

    2016-12-01

    Multifunctional silica gel with embedded silver nanoparticles (SiO2-AgNP) is proposed for application as sorbent for solid-phase extraction (SPE) and simultaneously as substrate for surface-enhanced Raman spectroscopy (SERS) due to their high sorption properties and ability to enhance Raman signal (SERS-active sorbents). SiO2-AgNP was synthesized via alkaline hydrolysis of tetraethyl orthosilicate with simultaneous reduction of silver ions to silver nanoparticles (AgNP) within the SiO2 bulk. Synthesis of AgNP directly to the SiO2 matrix enables to exclude any additional stabilizers for the nanoparticles that educes signal-to-noise ratio during SERS measurement. Apart from Raman spectroscopy, obtained sorbents were also characterized by scanning electron microscopy and UV-visible diffuse reflectance spectroscopy. The influence of AgNO3 concentration used during the SiO2-AgNP synthesis on its gelling time, color, diffuse reflectance spectra, and enhancement of Raman signal was investigated. A Raman enhancement factor of SiO2-AgNP with optimal composition was around 105. Finally, the sorbents were applied for SPE and subsequent SERS detection of model compounds (rhodamine 6G and folic acid). It was found that SPE enables to decrease detectable concentrations by two orders. Therefore, SPE combined with SERS has high potential for further analytical investigations.

  14. Multifunctional silver nanoparticle-doped silica for solid-phase extraction and surface-enhanced Raman scattering detection

    Energy Technology Data Exchange (ETDEWEB)

    Markina, Natalia E.; Markin, Alexey V., E-mail: av-markin@mail.ru; Zakharevich, Andrey M.; Gorin, Dmitry A.; Rusanova, Tatiana Yu.; Goryacheva, Irina Yu. [Saratov State University (Russian Federation)

    2016-12-15

    Multifunctional silica gel with embedded silver nanoparticles (SiO{sub 2}–AgNP) is proposed for application as sorbent for solid-phase extraction (SPE) and simultaneously as substrate for surface-enhanced Raman spectroscopy (SERS) due to their high sorption properties and ability to enhance Raman signal (SERS-active sorbents). SiO{sub 2}–AgNP was synthesized via alkaline hydrolysis of tetraethyl orthosilicate with simultaneous reduction of silver ions to silver nanoparticles (AgNP) within the SiO{sub 2} bulk. Synthesis of AgNP directly to the SiO{sub 2} matrix enables to exclude any additional stabilizers for the nanoparticles that educes signal-to-noise ratio during SERS measurement. Apart from Raman spectroscopy, obtained sorbents were also characterized by scanning electron microscopy and UV-visible diffuse reflectance spectroscopy. The influence of AgNO{sub 3} concentration used during the SiO{sub 2}–AgNP synthesis on its gelling time, color, diffuse reflectance spectra, and enhancement of Raman signal was investigated. A Raman enhancement factor of SiO{sub 2}–AgNP with optimal composition was around 10{sup 5}. Finally, the sorbents were applied for SPE and subsequent SERS detection of model compounds (rhodamine 6G and folic acid). It was found that SPE enables to decrease detectable concentrations by two orders. Therefore, SPE combined with SERS has high potential for further analytical investigations.

  15. Capillary electrophoresis-based assessment of nanobody affinity and purity

    NARCIS (Netherlands)

    Haselberg, Rob; Oliveira, Sabrina; van der Meel, Roy; Somsen, Govert W; de Jong, Gerhardus J

    2014-01-01

    Drug purity and affinity are essential attributes during development and production of therapeutic proteins. In this work, capillary electrophoresis (CE) was used to determine both the affinity and composition of the biotechnologically produced "nanobody" EGa1, the binding fragment of a

  16. Synthesis of γ-amino[4-11C]butyric acid (GABA)

    International Nuclear Information System (INIS)

    Antoni, G.; Laangstroem, B.

    1989-01-01

    A one-pot synthesis of no-carrier added γ-amino[4- 11 C]butyric acid (GABA) starting with hydrogen [ 11 C]cyanide prepared from [ 11 C]carbon dioxide, is presented. Hydrogen [ 11 C]cyanide was trapped in tetrahydrofuran/potassium hydroxide in the presence of the amino polyether Krytofix 2.2.2. A Michael addition with ethyl acrylate followed by a selective reduction and hydrolysis of the resulting amino ester gave [4- 11 C]GABA. The radiochemical purity of GABA was higher than 99% and the decay corrected radiochemical yield was 60-65% based on the amount of H[ 11 C]CN used. The total synthesis time including purification was around 40 min, counted from the start of the Michael addition reaction. (Author)

  17. Solid-Phase Synthesis of Smac Peptidomimetics Incorporating Triazoloprolines and Biarylalanines

    DEFF Research Database (Denmark)

    Le Quement, Sebastian T.; Ishoey, Mette; Petersen, Mette T.

    2011-01-01

    by deactivating proteolytic caspases. The Smac protein has an antagonistic effect on IAPs, thus providing structural clues for the synthesis of new pro-apoptotic compounds. Herein, we report a solid-phase approach for the synthesis of Smac-derived tetrapeptide libraries. On the basis of a common (N......-Me)AVPF sequence, peptides incorporating triazoloprolines and biarylalanines were synthesized by means of Cu(I)-catalyzed azide–alkyne cycloaddition and Pd-catalyzed Suzuki cross-coupling reactions. Solid-phase procedures were optimized to high efficiency, thus accessing all products in excellent crude purities...... and yields (both typically above 90%). The peptides were subjected to biological evaluation in a live/dead cellular assay which revealed that structural decorations on the AVPF sequence indeed are highly important for cytotoxicity toward HeLa cells....

  18. Synthesis of [119mSn]-mesoporphyrin IX dichloride

    International Nuclear Information System (INIS)

    Denissen, J.F.

    1990-01-01

    Tin mesoporphyrin IX dichloride (Sn-MPCl 2 ) is a heme oxygenase inhibitor of current clinical interest for the treatment of neonatal hyperbilirubinemia. The synthesis of [ 119m Sn]-MPCl 2 for drug metabolism and disposition studies is reported. [ 119m Sn]-MPCl 2 was prepared in 60% radiochemical yield by metalation of the porphyrin nucleus of mesoporphyrin IX dihydrochloride with tin(II)-119m acetate. The product had a specific activity of 43.4 mCi/mmol and a radiochemical purity of 99%, as determined by radio-HPLC analysis. (author)

  19. Titania doping effect on superconducting properties of MgB{sub 2} bulk samples

    Energy Technology Data Exchange (ETDEWEB)

    Serrano, G; Serquis, A [Institute Balseiro - Centra Atomico Bariloche and CONICET, (8400) S. C. de Bariloche, Rio Negro (Argentina); Bridoux, G, E-mail: serranog@ib.cnea.gov.a [Institute Balseiro - Centra Atomico Bariloche, (8400) S. C. de Bariloche, Rio Negro (Argentina)

    2009-05-01

    In this work we study the microstructural and superconducting properties of doped and undoped bulk MgB{sub 2} samples prepared by solid-state reaction, with 0 and 2.5 %at. nominal TiO{sub 2} nanotubes contents, annealed at different temperatures in the 750-900 deg. C range. We discuss the T{sub c}, J{sub c} and H{sub c2} performance and their correlation with the different synthesis parameters.

  20. Automated synthesis of n.c.a. [18F]FDOPA via nucleophilic aromatic substitution with [18F]fluoride

    International Nuclear Information System (INIS)

    Shen, B.; Ehrlichmann, W.; Uebele, M.; Machulla, H.-J.; Reischl, G.

    2009-01-01

    An improved, automated synthesis of [ 18 F]FDOPA including four synthetic steps (fluorination, reductive iodination, alkylation and hydrolysis) is reported with each step optimized individually. In a home-made automatic synthesizer, 9064±3076 MBq of [ 18 F]FDOPA were produced within 120 min from EOB (n=5). Radiochemical purity and enantiomeric excess were both ≥95%. Specific activity was ca. 50 GBq/μmol at EOS. This automatically operable synthesis is well suited for the multi-patient-dose routine production of n.c.a. [ 18 F]FDOPA.

  1. Purity of targets prepared on Cu substrates

    Science.gov (United States)

    Méens, A.; Rossini, I.; Sens, J. C.

    1993-09-01

    The purity of several elemental self-supporting targets usually prepared by evaporation onto soluble Cu substrates has been studied. The targets were analysed by Rutherford backscattering and instrumental neutron activation analysis. Because of the high percentage of Cu observed in some Si targets, further measurements, including transmission electron microscopy, have been performed on Si targets deposited by e-gun bombardment onto Cu and ion-beam sputtering onto betaine.

  2. Imaging Scanner Usage in Radiochemical Purity Test

    International Nuclear Information System (INIS)

    Norhafizah Othman; Yahaya Talib; Wan Hamirul Bahrin Wan Kamal

    2011-01-01

    Imaging Scanner model BIOSCAN AR-2000 has been used in the radiochemical purity test for the product of Mo-99/ Tc-99m generator. Result from this test was produced directly where the percentage of pertechnetate was calculated based on width peak area by thin layer chromatography. This paperwork will explain the function, procedure, calibration of the instrument and discussed the advantages compared to the previous method. (author)

  3. Bulk oil clauses

    International Nuclear Information System (INIS)

    Gough, N.

    1993-01-01

    The Institute Bulk Oil Clauses produced by the London market and the American SP-13c Clauses are examined in detail in this article. The duration and perils covered are discussed, and exclusions, adjustment clause 15 of the Institute Bulk Oil Clauses, Institute War Clauses (Cargo), and Institute Strikes Clauses (Bulk Oil) are outlined. (UK)

  4. The effective synthesis of Insoluble sulfur using electron beam

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Daejin; Yu, Kookhyun [Dongguk Univ., Seoul (Korea, Republic of)

    2013-07-01

    Vulcanization is process that formed crosslinking by Insoluble sulfur between linear structure of rubber polymer. Recently, Synthesis of Insoluble sulfur is used Thermal polymerization using about 250 {approx} 300 .deg. C and extraction process is used carbon disulfide(CS2) for separation between soluble sulfur and insoluble sulfur. But this process isn't environmental, economical and safety. This research was focus on developing of insoluble sulfur synthesis process using electron beam. This new process is using under the 140 .deg. C. Because of that, explosion risk is decrease, environmental and economical factor is increased. The sulfur can be melt by increase temperature or made solution using carbon disulfide. And electron beam is irradiated melting sulfur or sulfur solution. After irradiation, The high purity insoluble sulfur can be obtained by separation with carbon disulfide.

  5. Magnetic levitation force between a superconducting bulk magnet and a permanent magnet

    International Nuclear Information System (INIS)

    Wang, J J; He, C Y; Meng, L F; Li, C; Han, R S; Gao, Z X

    2003-01-01

    The current density J(ρ, z) in a disc-shaped superconducting bulk magnet and the magnetic levitation force F SBM z exerted on the superconducting bulk magnet by a cylindrical permanent magnet are calculated from first principles. The effect of the superconducting parameters of the superconducting bulk is taken into account by assuming the voltage-current law E = E c (J/J c ) n and the material law B = μ 0 H. The magnetic levitation force F SBM z is dominated by the remnant current density J' 2 (ρ, z), which is induced by switching off the applied magnetizing field. High critical current density and flux creep exponent may increase the magnetic levitation force F SBM z . Large volume and high aspect ratio of the superconducting bulk can further enhance the magnetic levitation force F SBM z

  6. Synthesis of tetraalkyl thiuram disulfides using different oxidants in recycling solvent mixture

    Directory of Open Access Journals (Sweden)

    Milosavljević Milutin M.

    2012-01-01

    Full Text Available A new optimized laboratory synthesis of tetraalkyl thiuram disulfides, starting from dialkyl amines and carbon disulfide in presence of three oxidants (hydrogen peroxide, potassium peroxodisulfate and sodium hypochlorite and appropriate reaction medium: two mixtures of isopropyl alcohol - water used in two consecutive syntheses, was presented in this work. First synthesis was performed in a recycled azeotropic mixture of isopropyl alcohol - water 87.7% - 12.3%, and second in a filtrate obtained after first synthesis, which was a mixture of isopropyl alcohol - water 70.4% - 29.6%. After the second synthesis and filtration, recycled azeotropic mixture isopropyl alcohol - water 87.7% - 12.3% was regenerated from the filtrate by rectification. Considering this, the technology for beneficial use of recycling isopropyl alcohol - water mixture as reaction medium for tetraalkyl thiuram disulfides synthesis was developed. Such concept contributes to extraordinary economical benefit of implemented optimal laboratory synthesis at semi-industrial level. High yields of tetraalkyl thiuram disulfides syntheses were obtained at both laboratory and semiindustrial level. Structure and purity of synthesized compounds were confirmed by elemental analysis, as well as FTIR, 1H and 13C NMR, and MS spectral data.

  7. Microwave-Enhanced Organic Syntheses for the Undergraduate Laboratory: Diels-Alder Cycloaddition, Wittig Reaction, and Williamson Ether Synthesis

    Science.gov (United States)

    Baar, Marsha R.; Falcone, Danielle; Gordon, Christopher

    2010-01-01

    Microwave heating enhanced the rate of three reactions typically performed in our undergraduate organic chemistry laboratory: a Diels-Alder cycloaddition, a Wittig salt formation, and a Williamson ether synthesis. Ninety-minute refluxes were shortened to 10 min using a laboratory-grade microwave oven. In addition, yields improved for the Wittig…

  8. Semi-automated microwave assisted solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Pedersen, Søren Ljungberg

    with microwaves for SPPS has gained in popularity as it for many syntheses has provided significant improvement in terms of speed, purity, and yields, maybe especially in the synthesis of long and "difficult" peptides. Thus, precise microwave heating has emerged as one new parameter for SPPS, in addition...... to coupling reagents, resins, solvents etc. We have previously reported on microwave heating to promote a range of solid-phase reactions in SPPS. Here we present a new, flexible semi-automated instrument for the application of precise microwave heating in solid-phase synthesis. It combines a slightly modified...... Biotage Initiator microwave instrument, which is available in many laboratories, with a modified semi-automated peptide synthesizer from MultiSynTech. A custom-made reaction vessel is placed permanently in the microwave oven, thus the reactor does not have to be moved between steps. Mixing is achieved...

  9. Fischer Indole Synthesis in the Gas Phase, the Solution Phase, and at the Electrospray Droplet Interface.

    Science.gov (United States)

    Bain, Ryan M; Ayrton, Stephen T; Cooks, R Graham

    2017-07-01

    Previous reports have shown that reactions occurring in the microdroplets formed during electrospray ionization can, under the right conditions, exhibit significantly greater rates than the corresponding bulk solution-phase reactions. The observed acceleration under electrospray ionization could result from a solution-phase, a gas-phase, or an interfacial reaction. This study shows that a gas-phase ion/molecule (or ion/ion) reaction is not responsible for the observed rate enhancement in the particular case of the Fischer indole synthesis. The results show that the accelerated reaction proceeds in the microdroplets, and evidence is provided that an interfacial process is involved. Graphical Abstract GRAPHICAL ABSTRACT TEXT HERE] -->.

  10. Hydrogen concentration and distribution in high-purity germanium crystals

    International Nuclear Information System (INIS)

    Hansen, W.L.; Haller, E.E.; Luke, P.N.

    1981-10-01

    High-purity germanium crystals used for making nuclear radiation detectors are usually grown in a hydrogen ambient from a melt contained in a high-purity silica crucible. The benefits and problems encountered in using a hydrogen ambient are reviewed. A hydrogen concentration of about 2 x 10 15 cm -3 has been determined by growing crystals in hydrogen spiked with tritium and counting the tritium β-decays in detectors made from these crystals. Annealing studies show that the hydrogen is strongly bound, either to defects or as H 2 with a dissociation energy > 3 eV. This is lowered to 1.8 eV when copper is present. Etching defects in dislocation-free crystals grown in hydrogen have been found by etch stripping to have a density of about 1 x 10 7 cm -3 and are estimated to contain 10 8 H atoms each

  11. Enhanced active aluminum content and thermal behaviour of nano-aluminum particles passivated during synthesis using thermal plasma route

    International Nuclear Information System (INIS)

    Mathe, Vikas L.; Varma, Vijay; Raut, Suyog; Nandi, Amiya Kumar; Pant, Arti; Prasanth, Hima; Pandey, R.K.; Bhoraskar, Sudha V.; Das, Asoka K.

    2016-01-01

    Graphical abstract: - Highlights: • Synthesis of nano crystalline Al (nAl) using DC thermal plasma reactor. • In situ passivation of nAl by palmitic acid and air. • Enhanced active aluminum content obtained for palmitic acid passivated nAl. • Palmitic acid passivated nAl are quite stable in humid atmospheres. - Abstract: Here, we report synthesis and in situ passivation of aluminum nanoparticles using thermal plasma reactor. Both air and palmitc acid passivation was carried out during the synthesis in the thermal plasma reactor. The passivated nanoparticles have been characterized for their structural and morphological properties using X-ray diffraction (XRD) and transmission electron microscopy (TEM) techniques. In order to understand nature of passivation vibrational spectroscopic analysis have been carried out. The enhancement in active aluminum content and shelf life for a palmitic acid passivated nano-aluminum particles in comparison to the air passivated samples and commercially available nano Al powder (ALEX) has been observed. Thermo-gravimetric analysis was used to estimate active aluminum content of all the samples under investigation. In addition cerimetric back titration method was also used to estimate AAC and the shelf life of passivated aluminum particles. Structural, microstructural and thermogravomateric analysis of four year aged passivated sample also depicts effectiveness of palmitic acid passivation.

  12. Enhanced active aluminum content and thermal behaviour of nano-aluminum particles passivated during synthesis using thermal plasma route

    Energy Technology Data Exchange (ETDEWEB)

    Mathe, Vikas L., E-mail: vlmathe@physics.unipune.ac.in [Department of Physics, Savitribai Phule Pune University, Pune 411007, Maharashtra (India); Varma, Vijay; Raut, Suyog [Department of Physics, Savitribai Phule Pune University, Pune 411007, Maharashtra (India); Nandi, Amiya Kumar; Pant, Arti; Prasanth, Hima; Pandey, R.K. [High Energy Materials Research Lab, Sutarwadi, Pune 411021, Maharashtra (India); Bhoraskar, Sudha V. [Department of Physics, Savitribai Phule Pune University, Pune 411007, Maharashtra (India); Das, Asoka K. [Utkal University, VaniVihar, Bhubaneswar, Odisha 751004 (India)

    2016-04-15

    Graphical abstract: - Highlights: • Synthesis of nano crystalline Al (nAl) using DC thermal plasma reactor. • In situ passivation of nAl by palmitic acid and air. • Enhanced active aluminum content obtained for palmitic acid passivated nAl. • Palmitic acid passivated nAl are quite stable in humid atmospheres. - Abstract: Here, we report synthesis and in situ passivation of aluminum nanoparticles using thermal plasma reactor. Both air and palmitc acid passivation was carried out during the synthesis in the thermal plasma reactor. The passivated nanoparticles have been characterized for their structural and morphological properties using X-ray diffraction (XRD) and transmission electron microscopy (TEM) techniques. In order to understand nature of passivation vibrational spectroscopic analysis have been carried out. The enhancement in active aluminum content and shelf life for a palmitic acid passivated nano-aluminum particles in comparison to the air passivated samples and commercially available nano Al powder (ALEX) has been observed. Thermo-gravimetric analysis was used to estimate active aluminum content of all the samples under investigation. In addition cerimetric back titration method was also used to estimate AAC and the shelf life of passivated aluminum particles. Structural, microstructural and thermogravomateric analysis of four year aged passivated sample also depicts effectiveness of palmitic acid passivation.

  13. Synthesis of uniform-sized zeolite from windshield waste

    International Nuclear Information System (INIS)

    Kim, Jae-Chan; Choi, Mingu; Song, Hee Jo; Park, Jung Eun; Yoon, Jin-Ho; Park, Kyung-Soo; Lee, Chan Gi; Kim, Dong-Wan

    2015-01-01

    We demonstrate the synthesis of A-type zeolite from mechanically milled windshield waste via acid treatment and a low-temperature hydrothermal method. As-received windshield cullet was crushed to a fine powder and impurities were removed by HNO 3 treatment. The resulting glass powder was used as the source material for the hydrothermal synthesis of A-type zeolite. Crystal structure, morphology, and elemental composition changes of the windshield waste were evaluated at each step of the process through scanning electron microscopy, X-ray diffraction, X-ray fluorescence spectrometry, etc. After a high-energy milling process, the glass had an average particle size of 520 nm; after acid treatment, its composition was over 94% silica. Zeolite was successfully synthesized in the A-type phase with a uniform cubic shape. - Highlights: • Environmental-friendly recycling of windshield waste for high valuable product of zeolite. • Synthesis of zeolite form windshield waste via a low-temperature hydrothermal process. • High-energy milling effect on the uniform cubic shape and high-purity A-type zeolite.

  14. Bulk-Fill Resin Composites

    DEFF Research Database (Denmark)

    Benetti, Ana Raquel; Havndrup-Pedersen, Cæcilie; Honoré, Daniel

    2015-01-01

    the restorative procedure. The aim of this study, therefore, was to compare the depth of cure, polymerization contraction, and gap formation in bulk-fill resin composites with those of a conventional resin composite. To achieve this, the depth of cure was assessed in accordance with the International Organization...... for Standardization 4049 standard, and the polymerization contraction was determined using the bonded-disc method. The gap formation was measured at the dentin margin of Class II cavities. Five bulk-fill resin composites were investigated: two high-viscosity (Tetric EvoCeram Bulk Fill, SonicFill) and three low......-viscosity (x-tra base, Venus Bulk Fill, SDR) materials. Compared with the conventional resin composite, the high-viscosity bulk-fill materials exhibited only a small increase (but significant for Tetric EvoCeram Bulk Fill) in depth of cure and polymerization contraction, whereas the low-viscosity bulk...

  15. Polarimetric purity and the concept of degree of polarization

    Science.gov (United States)

    Gil, José J.; Norrman, Andreas; Friberg, Ari T.; Setälä, Tero

    2018-02-01

    The concept of degree of polarization for electromagnetic waves, in its general three-dimensional version, is revisited in the light of the implications of the recent findings on the structure of polarimetric purity and of the existence of nonregular states of polarization [J. J. Gil et al., Phys Rev. A 95, 053856 (2017), 10.1103/PhysRevA.95.053856]. From the analysis of the characteristic decomposition of a polarization matrix R into an incoherent convex combination of (1) a pure state Rp, (2) a middle state Rm given by an equiprobable mixture of two eigenstates of R, and (3) a fully unpolarized state Ru -3 D, it is found that, in general, Rm exhibits nonzero circular and linear degrees of polarization. Therefore, the degrees of linear and circular polarization of R cannot always be assigned to the single totally polarized component Rp. It is shown that the parameter P3 D proposed formerly by Samson [J. C. Samson, Geophys. J. R. Astron. Soc. 34, 403 (1973), 10.1111/j.1365-246X.1973.tb02404.x] takes into account, in a proper and objective form, all the contributions to polarimetric purity, namely, the contributions to the linear and circular degrees of polarization of R as well as to the stability of the plane containing its polarization ellipse. Consequently, P3 D constitutes a natural representative of the degree of polarimetric purity. Some implications for the common convention for the concept of two-dimensional degree of polarization are also analyzed and discussed.

  16. Solid-phase synthesis and structural characterization of highly substituted hydroxyproline-based 2,5-diketopiperazines

    DEFF Research Database (Denmark)

    Bianco; Sonksen; Roepstorff

    2000-01-01

    . The synthesis procedures were conceived to enable a sequence of Hyp alkylation, Hyp N-acylation, cyclization, and amide bond alkylation. Up to three different centers of molecular diversity were introduced around the DKP scaffold. Highly functionalized bicyclic compounds were obtained in good yield and purity...... with multidimensional NMR experiments. The described reaction pathways can be applied to the identification of heterocyclic molecule inhibitors to diverse enzyme targets....

  17. Limits on uranium and thorium bulk content in GERDA Phase I detectors

    Science.gov (United States)

    GERDA Collaboration; Agostini, M.; Allardt, M.; Bakalyarov, A. M.; Balata, M.; Barabanov, I.; Baudis, L.; Bauer, C.; Becerici-Schmidt, N.; Bellotti, E.; Belogurov, S.; Belyaev, S. T.; Benato, G.; Bettini, A.; Bezrukov, L.; Bode, T.; Borowicz, D.; Brudanin, V.; Brugnera, R.; Caldwell, A.; Cattadori, C.; Chernogorov, A.; D'Andrea, V.; Demidova, E. V.; di Vacri, A.; Domula, A.; Doroshkevich, E.; Egorov, V.; Falkenstein, R.; Fedorova, O.; Freund, K.; Frodyma, N.; Gangapshev, A.; Garfagnini, A.; Grabmayr, P.; Gurentsov, V.; Gusev, K.; Hakemüller, J.; Hegai, A.; Heisel, M.; Hemmer, S.; Hofmann, W.; Hult, M.; Inzhechik, L. V.; Janicskó Csáthy, J.; Jochum, J.; Junker, M.; Kazalov, V.; Kihm, T.; Kirpichnikov, I. V.; Kirsch, A.; Kish, A.; Klimenko, A.; Kneißl, R.; Knöpfle, K. T.; Kochetov, O.; Kornoukhov, V. N.; Kuzminov, V. V.; Laubenstein, M.; Lazzaro, A.; Lebedev, V. I.; Lehnert, B.; Liao, H. Y.; Lindner, M.; Lippi, I.; Lubashevskiy, A.; Lubsandorzhiev, B.; Lutter, G.; Macolino, C.; Majorovits, B.; Maneschg, W.; Medinaceli, E.; Mingazheva, R.; Misiaszek, M.; Moseev, P.; Nemchenok, I.; Palioselitis, D.; Panas, K.; Pandola, L.; Pelczar, K.; Pullia, A.; Riboldi, S.; Rumyantseva, N.; Sada, C.; Salamida, F.; Salathe, M.; Schmitt, C.; Schneider, B.; Schönert, S.; Schreiner, J.; Schütz, A.-K.; Schulz, O.; Schwingenheuer, B.; Selivanenko, O.; Shevchik, E.; Shirchenko, M.; Simgen, H.; Smolnikov, A.; Stanco, L.; Stepaniuk, M.; Vanhoefer, L.; Vasenko, A. A.; Veresnikova, A.; von Sturm, K.; Wagner, V.; Walter, M.; Wegmann, A.; Wester, T.; Wiesinger, C.; Wojcik, M.; Yanovich, E.; Zhitnikov, I.; Zhukov, S. V.; Zinatulina, D.; Zuber, K.; Zuzel, G.

    2017-05-01

    Internal contaminations of 238U, 235U and 232Th in the bulk of high purity germanium detectors are potential backgrounds for experiments searching for neutrinoless double beta decay of 76Ge. The data from GERDA Phase I have been analyzed for alpha events from the decay chain of these contaminations by looking for full decay chains and for time correlations between successive decays in the same detector. No candidate events for a full chain have been found. Upper limits on the activities in the range of a few nBq/kg for 226Ra, 227Ac and 228Th, the long-lived daughter nuclides of 238U, 235U and 232Th, respectively, have been derived. With these upper limits a background index in the energy region of interest from 226Ra and 228Th contamination is estimated which satisfies the prerequisites of a future ton scale germanium double beta decay experiment.

  18. Transesterification Synthesis of Chloramphenicol Esters with the Lipase from Bacillus amyloliquefaciens

    Directory of Open Access Journals (Sweden)

    Fengying Dong

    2017-09-01

    Full Text Available This work presents a synthetic route to produce chloramphenicol esters by taking advantage the high enantio- and regio-selectivity of lipases. A series of chloramphenicol esters were synthesized using chloramphenicol, acyl donors of different carbon chain length and lipase LipBA (lipase cloned from Bacillus amyloliquefaciens. Among acyl donors with different carbon chain lengths, vinyl propionate was found to be the best. The influences of different organic solvents, reaction temperature, reaction time, enzyme loading and water content on the synthesis of the chloramphenicol esters were studied. The synthesis of chloramphenicol propionate (0.25 M with 4.0 g L−1 of LipBA loading gave a conversion of ~98% and a purity of ~99% within 8 h at 50 °C in 1,4-dioxane as solvent. The optimum mole ratio of vinyl propionate to chloramphenicol was increased to 5:1. This is the first report of B. amyloliquefaciens lipase being used in chloramphenicol ester synthesis and a detailed study of the synthesis of chloramphenicol propionate using this reaction. The high enzyme activity and selectivity make lipase LipBA an attractive catalyst for green chemical synthesis of molecules with complex structures.

  19. Fully automated synthesis of 11C-acetate as tumor PET tracer by simple modified solid-phase extraction purification

    International Nuclear Information System (INIS)

    Tang, Xiaolan; Tang, Ganghua; Nie, Dahong

    2013-01-01

    Introduction: Automated synthesis of 11 C-acetate ( 11 C-AC) as the most commonly used radioactive fatty acid tracer is performed by a simple, rapid, and modified solid-phase extraction (SPE) purification. Methods: Automated synthesis of 11 C-AC was implemented by carboxylation reaction of MeMgBr on a polyethylene Teflon loop ring with 11 C-CO 2 , followed by acidic hydrolysis with acid and SCX cartridge, and purification on SCX, AG11A8 and C18 SPE cartridges using a commercially available 11 C-tracer synthesizer. Quality control test and animals positron emission tomography (PET) imaging were also carried out. Results: A high and reproducible decay-uncorrected radiochemical yield of (41.0±4.6)% (n=10) was obtained from 11 C-CO 2 within the whole synthesis time about 8 min. The radiochemical purity of 11 C-AC was over 95% by high-performance liquid chromatography (HPLC) analysis. Quality control test and PET imaging showed that 11 C-AC injection produced by the simple SPE procedure was safe and efficient, and was in agreement with the current Chinese radiopharmaceutical quality control guidelines. Conclusion: The novel, simple, and rapid method is readily adapted to the fully automated synthesis of 11 C-AC on several existing commercial synthesis module. The method can be used routinely to produce 11 C-AC for preclinical and clinical studies with PET imaging. - Highlights: • A fully automated synthesis of 11 C-acetate by simple modified solid-phase extraction purification has been developed. • Typical non-decay-corrected yields were (41.0±4.6)% (n=10) • Radiochemical purity was determined by radio-HPLC analysis on a C18 column using the gradient program, instead of expensive organic acid column or anion column. • QC testing (RCP>99%)

  20. Synthesis of ultrafine alumina powders using egg white as complexing medium

    International Nuclear Information System (INIS)

    Salem, R.E.P.; Guilherme, K. A.; Chinelatto, A.S.A.; Chinelatto, A.L.

    2011-01-01

    Synthesis of alumina powders through chemical methods has been attracting much attention of researchers in the past few years, due to the ability to produce powders in nanometric scale with high degree of purity. In this work, there were synthesized alumina powders through a chemical route, using egg white as a complexing medium and aluminium nitrate as the source of Al 3+ cations. Egg white contains ovalbumin, a protein which acts effectively on the isolation of aluminium cations during the mixing process, enabling the formation of ultrafine alumina powders in a relatively economic and environmentally friendly way. The powders obtained by calcinations of the precursor resin were characterized by X-ray diffraction, specific surface area measurements, infrared spectroscopy and scanning electron microscopy. It was observed that the egg white, present at the reaction medium, allowed obtaining transition alumina powders, with high degree of purity. (author)

  1. Effects of surface and bulk transverse fields on critical behaviour of ferromagnetic films

    International Nuclear Information System (INIS)

    Saber, A.; Lo Russo, S.; Mattei, G.

    2002-02-01

    The influence of surface and bulk transverse fields on the critical behaviour of a ferromagnetic Ising film is studied using the effective field theory based on a single-site cluster method. Surface exchange enhancement is considered and a critical value is obtained. The dependence of the critical uniform transverse field on film thickness, phase diagrams in the fields, critical surface transverse field versus the bulk one, and exchange coupling ratio are presented. (author)

  2. Biotin enhances ATP synthesis in pancreatic islets of the rat, resulting in reinforcement of glucose-induced insulin secretion.

    Science.gov (United States)

    Sone, Hideyuki; Sasaki, Yuka; Komai, Michio; Toyomizu, Masaaki; Kagawa, Yasuo; Furukawa, Yuji

    2004-02-13

    Previous studies showed that biotin enhanced glucose-induced insulin secretion. Changes in the cytosolic ATP/ADP ratio in the pancreatic islets participate in the regulation of insulin secretion by glucose. In the present study we investigated whether biotin regulates the cytosolic ATP/ADP ratio in glucose-stimulated islets. When islets were stimulated with glucose plus biotin, the ATP/ADP ratio increased to approximately 160% of the ATP/ADP ratio in islets stimulated with glucose alone. The rate of glucose oxidation, assessed by CO(2) production, was also about 2-fold higher in islets treated with biotin. These increasing effects of biotin were proportional to the effects seen in insulin secretion. There are no previous reports of vitamins, such as biotin, directly affecting ATP synthesis. Our data indicate that biotin enhances ATP synthesis in islets following the increased rate of substrate oxidation in mitochondria and that, as a consequence of these events, glucose-induced insulin release is reinforced by biotin.

  3. Magnetic levitation force between a superconducting bulk magnet and a permanent magnet

    Energy Technology Data Exchange (ETDEWEB)

    Wang, J J; He, C Y; Meng, L F; Li, C; Han, R S; Gao, Z X [Department of Physics, Key Laboratory for Artificial Microstructure and Mesoscopic Physics, Peking University, Beijing 100871 (China)

    2003-04-01

    The current density J({rho}, z) in a disc-shaped superconducting bulk magnet and the magnetic levitation force F{sup SBM}{sub z} exerted on the superconducting bulk magnet by a cylindrical permanent magnet are calculated from first principles. The effect of the superconducting parameters of the superconducting bulk is taken into account by assuming the voltage-current law E = E{sub c}(J/J{sub c}){sup n} and the material law B = {mu}{sub 0}H. The magnetic levitation force F{sup SBM}{sub z} is dominated by the remnant current density J'{sub 2}({rho}, z), which is induced by switching off the applied magnetizing field. High critical current density and flux creep exponent may increase the magnetic levitation force F{sup SBM}{sub z}. Large volume and high aspect ratio of the superconducting bulk can further enhance the magnetic levitation force F{sup SBM}{sub z}.

  4. In situ scanning tunneling microscopy study of Ca-modified rutile TiO2(110 in bulk water

    Directory of Open Access Journals (Sweden)

    Giulia Serrano

    2015-02-01

    Full Text Available Despite the rising technological interest in the use of calcium-modified TiO2 surfaces in biomedical implants, the Ca/TiO2 interface has not been studied in an aqueous environment. This investigation is the first report on the use of in situ scanning tunneling microscopy (STM to study calcium-modified rutile TiO2(110 surfaces immersed in high purity water. The TiO2 surface was prepared under ultrahigh vacuum (UHV with repeated sputtering/annealing cycles. Low energy electron diffraction (LEED analysis shows a pattern typical for the surface segregation of calcium, which is present as an impurity on the TiO2 bulk. In situ STM images of the surface in bulk water exhibit one-dimensional rows of segregated calcium regularly aligned with the [001] crystal direction. The in situ-characterized morphology and structure of this Ca-modified TiO2 surface are discussed and compared with UHV-STM results from the literature. Prolonged immersion (two days in the liquid leads to degradation of the overlayer, resulting in a disordered surface. X-ray photoelectron spectroscopy, performed after immersion in water, confirms the presence of calcium.

  5. Enhanced Bulk-Edge Coulomb Coupling in Fractional Fabry-Perot Interferometers.

    Science.gov (United States)

    von Keyserlingk, C W; Simon, S H; Rosenow, Bernd

    2015-09-18

    Recent experiments use Fabry-Perot (FP) interferometry to claim that the ν=5/2 quantum Hall state exhibits non-Abelian topological order. We note that the experiments appear inconsistent with a model neglecting bulk-edge Coulomb coupling and Majorana tunneling, so we reexamine the theory of FP devices. Even a moderate Coulomb coupling may strongly affect some fractional plateaus, but very weakly affect others, allowing us to model the data over a wide range of plateaus. While experiments are consistent with the ν=5/2 state harboring Moore-Read topological order, they may have measured Coulomb effects rather than an "even-odd effect" due to non-Abelian braiding.

  6. Interface control: A modified rooting technique for enhancing field emission from multiwall carbon nanotube based bulk emitters

    Energy Technology Data Exchange (ETDEWEB)

    Lahiri, Indranil [Nanomaterials and Device Lab, Department of Mechanical and Materials Engineering, Florida International University, 10555 West Flagler Street, Miami, FL 33174 (United States); Choi, Wonbong, E-mail: choiw@fiu.edu [Nanomaterials and Device Lab, Department of Mechanical and Materials Engineering, Florida International University, 10555 West Flagler Street, Miami, FL 33174 (United States)

    2011-08-15

    The unique properties of carbon nanotubes (CNTs) have raised hopes that these materials might find wide application as cold cathodes in various electron sources. The excellent field emission properties shown by CNT-based field emitters has further stimulated this expectation. However, efficient performance of a practical field emitter, which comprises a large number of randomly or regularly oriented CNTs, is restricted primarily due to poor junctions formed between CNTs and substrates. This study is aimed at enhancing the junction performance by way of a modified 'rooting' technique-interface control. In this process, the interface between CNTs and substrate has been tailored with different metals in an attempt to improve the CNT-substrate junction performance. Multiwall carbon nanotubes (MWCNTs) were synthesized on different interface-controlled substrates, i.e. Cu, Al, W, Si and low-temperature co-fired ceramic. All the samples produced mat-type, randomly oriented MWCNT structures. Among the four different substrates studied, MWCNT-based field emitters on Cu substrate demonstrated the best field emission response, in terms of low turn-on field, high emission current, good field enhancement factor and excellent stability in long-term operation. Emitter structures and their field emission behavior were correlated and it was shown that interface control, as an advanced 'rooting' process, plays an important role in determining the emission response from a bulk field emitter.

  7. Interface control: A modified rooting technique for enhancing field emission from multiwall carbon nanotube based bulk emitters

    International Nuclear Information System (INIS)

    Lahiri, Indranil; Choi, Wonbong

    2011-01-01

    The unique properties of carbon nanotubes (CNTs) have raised hopes that these materials might find wide application as cold cathodes in various electron sources. The excellent field emission properties shown by CNT-based field emitters has further stimulated this expectation. However, efficient performance of a practical field emitter, which comprises a large number of randomly or regularly oriented CNTs, is restricted primarily due to poor junctions formed between CNTs and substrates. This study is aimed at enhancing the junction performance by way of a modified 'rooting' technique-interface control. In this process, the interface between CNTs and substrate has been tailored with different metals in an attempt to improve the CNT-substrate junction performance. Multiwall carbon nanotubes (MWCNTs) were synthesized on different interface-controlled substrates, i.e. Cu, Al, W, Si and low-temperature co-fired ceramic. All the samples produced mat-type, randomly oriented MWCNT structures. Among the four different substrates studied, MWCNT-based field emitters on Cu substrate demonstrated the best field emission response, in terms of low turn-on field, high emission current, good field enhancement factor and excellent stability in long-term operation. Emitter structures and their field emission behavior were correlated and it was shown that interface control, as an advanced 'rooting' process, plays an important role in determining the emission response from a bulk field emitter.

  8. Policosanol extraction from beeswax and improvement of the purity

    Directory of Open Access Journals (Sweden)

    Srisaipet Anakhaorn

    2017-01-01

    Full Text Available Policosanol is a mixture of high molecular weight aliphatic long chain alcohols (20-36 carbon atoms. It has been use in pharmaceutical composition and food supplements. This research aimed to isolate and improve the purity of policosanol extracted from beeswax. Triglycerides and other impurities were eliminated from beeswax by refluxing with hexane followed by isopropanol. The purified beeswax was hydrolyzed by refluxing with 1 M ethanolic NaOH for 2 hours. Purification of policosanol was performed by extracting the hydrolyzed product with acetone at 50-60 °C for 3 hours and it was stored at 4 °C for precipitation. The precipitate was refluxed with heptanes followed by washing with hot water. The heptanes layer was kept for policosanol precipitation at 4 °C. The purity of policosanol was confirmed by TLC and high performance liquid chromatography (HPLC. The yield of purified policosanol was 13.23-13.89 %.

  9. Electrophoresis for the analysis of heparin purity and quality.

    Science.gov (United States)

    Volpi, Nicola; Maccari, Francesca; Suwan, Jiraporn; Linhardt, Robert J

    2012-06-01

    The adulteration of raw heparin with oversulfated chondroitin sulfate (OSCS) in 2007-2008 produced a global crisis resulting in extensive revisions to the pharmacopeia monographs and prompting the FDA to recommend the development of additional methods for the analysis of heparin purity. As a consequence, a wide variety of innovative analytical approaches have been developed for the quality assurance and purity of unfractionated and low-molecular-weight heparins. This review discusses recent developments in electrophoresis techniques available for the sensitive separation, detection, and partial structural characterization of heparin contaminants. In particular, this review summarizes recent publications on heparin quality and related impurity analysis using electrophoretic separations such as capillary electrophoresis (CE) of intact polysaccharides and hexosamines derived from their acidic hydrolysis, and polyacrylamide gel electrophoresis (PAGE) for the separation of heparin samples without and in the presence of its relatively specific depolymerization process with nitrous acid treatment. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Synthesis and devitrification of high glass-forming ability bulk metallic glasses.

    OpenAIRE

    Huang, Hong.

    2007-01-01

    In this thesis, literature on the production, microstructures and properties of bulk metallic glasses (BMG) has been reviewed with particular reference to glass forming ability (GFA) and alloys of the Fe-Zr-B and Zr-based BMG systems. The experimental procedures used in the research are presented and the results for the amorphous Fe80Zr12B8 ribbon and the Zr57Ti5Al10Cu20Ni8, Zr57Nb5Al10Cu20Ni8, Zr53Nb2Al8Cu30Ni7 BMGs are given and discussed. Wedge-shaped ingots of the Zr-based BMGs were produ...

  11. Isolation of high purity americium metal via distillation

    Science.gov (United States)

    Squires, Leah N.; King, James A.; Fielding, Randall S.; Lessing, Paul

    2018-03-01

    Pure americium metal is a crucial component for the fabrication of transmutation fuels. Unfortunately, americium in pure metal form is not available; however, a number of mixed metals and mixed oxides that include americium are available. In this manuscript a method is described to obtain high purity americium metal from a mixture of americium and neptunium metals with lead impurity via distillation.

  12. Robotic production of 2-deoxy-2-[18F]fluoro-D-glucose: a routine method of synthesis using tetrabutylammonium [18F]fluoride

    International Nuclear Information System (INIS)

    Brodack, J.W.; Dence, C.S.; Kilbourn, M.R.; Welch, M.J.

    1988-01-01

    Using existing robotic hardware and software programs developed for the synthesis of several positron-emitting radiopharmaceuticals for PET imaging, the additional automated synthesis of 2-deoxy-2-[ 18 F]fluoro-D-glucose (2-[ 18 F]FDG) has been incorporated into our Zymate Laboratory Automation System. The robotic synthesis of 2-[ 18 F]FDG took less than one week to implement, including the organization of software subroutines and construction of an additional heating station. The end of synthesis yield (12-17%) and radiochemical purity (96-99%) for the robotic preparation of 2-[ 18 F]FDG is similar to that of the manual synthesis. This automated method uses anhydrous tetrabutylammonium [ 18 F]fluoride as the reactive fluoride source in the labeling step. The procedure is a modification of the synthesis reported by Hamacher et al. [Hamacher et al. (1986) J. Nucl. Med. 27, 235]. (author)

  13. Partial discharges and bulk dielectric field enhancement

    DEFF Research Database (Denmark)

    McAllister, Iain Wilson; Johansson, Torben

    2000-01-01

    A consequence of partial discharge activity within a gaseous void is the production of a field enhancement in the solid dielectric in the proximity of the void. This situation arises due to the charge created by the partial discharges accumulating at the void wall. The influence of the spatial...

  14. High-purity production of ultrathin boron nitride nanosheets via shock chilling and their enhanced mechanical performance and transparency in nanocomposite hydrogels

    Science.gov (United States)

    Sun, Zemin; Lin, Liu; Yuan, Mengwei; Li, Huifeng; Sun, Genban; Ma, Shulan; Yang, Xiaojing

    2018-05-01

    A simple, highly efficient, and eco-friendly method is prepared to divide bulk boron nitride (BN) into boron nitride nanosheets (BNNSs). Due to the anisotropy of the hexagonal BN expansion coefficient, bulk BN is exfoliated utilizing the rapid and tremendous change in temperature, the extreme gasification of water, and ice thermal expansion pressure under freeze drying. The thickness of most of the BNNSs was less than ∼3 nm with a yield of 12–16 wt%. The as-obtained BNNS/polyacrylamide (PAAm) composite hydrogels exhibited outstanding mechanical properties. The tensile strength is fives times the bulk of the BN/PAAm composite hydrogels and the elongations are more than nine-fold the bulk of the BN/PAAm composite hydrogels. The BNNS/PAAm nanocomposite hydrogels also exhibited excellent elastic recovery, and the hysteresis of the BNNS nanocomposite hydrogels was negligible even after 30 cycles with a maximum tensile strain (ε max) of 700%. This work provides new insight into the fabrication of BN/polymer nanocomposites utilizing the excellent mechanical properties and transparency of BN. The results confirm that a few layers of BNNSs can also efficiently and directly improve the mechanical properties of composite polymer due to its stronger surface free energy and better wettability.

  15. Bulk-fill resin-based composites: an in vitro assessment of their mechanical performance.

    Science.gov (United States)

    Ilie, N; Bucuta, S; Draenert, M

    2013-01-01

    The study aimed to assess the mechanical performance of seven bulk-fill RBCs (Venus Bulk Fill, Heraeus Kulzer; SureFil SDR flow, Dentsply Caulk; x-tra base and x-tra fil, VOCO; Filtek Bulk Fill, 3M ESPE; SonicFill, Kerr; Tetric EvoCeram Bulk Fill, Ivoclar Vivadent) by determining their flexural strength (σ), reliability (Weibull parameter, m), flexural modulus (Eflexural), indentation modulus (YHU), Vickers hardness (HV), and creep (Cr). The significant highest flexural strengths were measured for SonicFill, x-tra base, and x-tra fil, while x-tra base, SureFil SDR flow, and Venus Bulk Fill showed the best reliability. The differences among the materials became more evident in terms of Eflexural and YHU, with x-tra fil achieving the highest values, while Filtek Bulk Fill and Venus Bulk Fill achieved the lowest. The enlarged depth of cure in bulk-fill RBCs seems to have been realized by enhancing the materials' translucency through decreasing the filler amount and increasing the filler size. The manufacturer's recommendation to finish a bulk-fill RBC restoration by adding a capping layer made of regular RBCs is an imperative necessity, since the modulus of elasticity and hardness of certain materials (SureFil SDR flow, Venus Bulk Fill, and Filtek Bulk Fill) were considerably below the mean values measured in regular nanohybrid and microhybrid RBCs. The class of bulk-fill RBCs revealed similar flexural strength values as the class of nanohybrid and microhybrid RBCs, and significantly higher values when compared to flowable RBCs. The modulus of elasticity (Eflexural), the indentation modulus (YHU), and the Vickers hardness (HV) classify the bulk-fill RBCs as between the hybrid RBCs and the flowable RBCs; in terms of creep, bulk-fill and the flowable RBCs perform similarly, both showing a significantly lower creep resistance when compared to the nanohybrid and microhybrid RBCs.

  16. Synthesis of type A zeolite from calcinated kaolin

    International Nuclear Information System (INIS)

    Rodrigues, E.C.; Neves, R.F.; Souza, J.A.S.; Moraes, C.G.; Macedo, E.N.

    2011-01-01

    The mineral production has caused great concern in environmental and industrial scenario due to the effects caused to the environment. The industries of processing kaolin for paper are important economically for the state of Para, but produce huge quantities of tailings, which depend on large areas to be stocked. This material is rich in silico-aluminates can be recycled and used as raw material for other industries. The objective is to synthesize zeolite A at different temperatures of calcination and synthesis. The starting materials and synthesis of zeolite A have been identified and characterized through analysis of X-ray diffraction (DRX) and scanning electron microscopy (MEV). The synthesis process of zeolite A, using as source of silica and the aluminum metakaolin, which was calcined at temperatures of 700 ° C and 800 ° C for 2 hours of landing in a burning furnace type muffle. Observed in relation to the calcination of kaolin as the main phase, the metakaolin. This is just a removal of water from its structure, so we opted for the lower temperature, less energy consumption. The synthesis process of zeolite A, produced good results for the formation of zeolites type A, which were characterized with high purities. (author)

  17. Synthesis of Silver Nanoparticles from the Aqueous Extract of Leaves of Ocimum sanctum for Enhanced Antibacterial Activity

    Directory of Open Access Journals (Sweden)

    Charusheela Ramteke

    2013-01-01

    Full Text Available The field of nanotechnology is the most active area of research in modern materials science. Though there are many chemical as well as physical methods, green synthesis of nanomaterials is the most emerging method of synthesis. We report the synthesis of antibacterial silver nanoparticles (AgNPs using leaf broth of medicinal herb, Ocimum sanctum (Tulsi. The synthesized AgNPs have been characterized by UV-Vis spectroscopy, transmission electron microscopy (TEM, and X-ray diffractometry. The mean particle of synthesized NPs was found to be 18 nm, as confirmed by TEM. The qualitative assessment of reducing potential of leaf extract has also been carried out which indicated presence of significant amount of reducing entities. FTIR analysis revealed that the AgNPs were stabilized by eugenols, terpenes, and other aromatic compounds present in the extract. Such AgNPs stabilized by Tulsi leaf extract were found to have enhanced antimicrobial activity against well-known pathogenic strains, namely Staphylococcus aureus and E. coli.

  18. Solvothermal synthesis and analysis of Bi1-xSbx nanoparticles

    International Nuclear Information System (INIS)

    Sumithra, S.; Misra, D.K.; Wei, C.; Gabrisch, H.; Poudeu, P.F.P.; Stokes, K.L.

    2011-01-01

    Bismuth-antimony alloy nanoparticles have been synthesized by a facile solvothermal method using N,N-dimethylformamide and ethylene glycol as solvent/reducing agent; BiCl 3 , SbCl 3 and Bi(NO 3 ) 3 as precursors; and citric acid as a surface modifier/stabilizing agent. The particle size and size distribution of Bi nanoparticles were analyzed as a function of the synthesis conditions: molar ratio of precursor to surfactant, precursor concentration and reducing agent. Synthesis of Sb and Bi 0.88 Sb 0.12 under similar conditions was also investigated. The phase purity of nanoparticles was confirmed from X-ray diffraction and thermogravimetry and the nanoparticle morphology was investigated by transmission electron microscopy. A case study of Bi nanoparticles with detailed analysis of the particle morphology and size distribution of the nanoparticles is reported.

  19. A New Route for High-Purity Organic Materials: High-Pressure-Ramp-Induced Ultrafast Polymerization of 2-(Hydroxyethyl)Methacrylate

    Science.gov (United States)

    Evlyukhin, E.; Museur, L.; Traore, M.; Perruchot, C.; Zerr, A.; Kanaev, A.

    2015-12-01

    The synthesis of highly biocompatible polymers is important for modern biotechnologies and medicine. Here, we report a unique process based on a two-step high-pressure ramp (HPR) for the ultrafast and efficient bulk polymerization of 2-(hydroxyethyl)methacrylate (HEMA) at room temperature without photo- and thermal activation or addition of initiator. The HEMA monomers are first activated during the compression step but their reactivity is hindered by the dense glass-like environment. The rapid polymerization occurs in only the second step upon decompression to the liquid state. The conversion yield was found to exceed 90% in the recovered samples. The gel permeation chromatography evidences the overriding role of HEMA2•• biradicals in the polymerization mechanism. The HPR process extends the application field of HP-induced polymerization, beyond the family of crystallized monomers considered up today. It is also an appealing alternative to typical photo- or thermal activation, allowing the efficient synthesis of highly pure organic materials.

  20. Enhancement in surface area and magnetization of CoFe2O4 nanoparticles for targeted drug delivery application

    Science.gov (United States)

    Kale, Swati B.; Somvanshi, Sandeep B.; Sarnaik, M. N.; More, S. D.; Shukla, S. J.; Jadhav, K. M.

    2018-05-01

    This paper reports facile synthesis, characterizations by X-ray diffraction and scanning electron microscopy and magnetic behaviour of cobalt ferrite nanoparticles. Cobalt ferrite nanoparticles were prepared by sol-gel auto combustion technique using glycine as a fuel. Phase purity and nanocrystalline nature of the prepared sample was confirmed through X-ray diffraction technique. No extra peak other than cubic spinel structure was observed in the XRD pattern. The crystallite size calculated by using Scherrer's formula is of the order of 21.6 nm indicating the nanocrystalline nature of the prepared cobalt ferrite sample. The surface morphological studies were carried out using scanning electron microscope (SEM). SEM image shows homogeneous, agglomerated particles with sponge-like form. The saturation magnetization, coercivity and remenance magnetization obtained by hysteresis curve clearly gives the evidence of excellent and enhanced magnetic behaviour.

  1. Synthesis of pure iron magnetic nanoparticles in large quantity

    International Nuclear Information System (INIS)

    Tiwary, C S; Kashyap, S; Chattopadhyay, K; Biswas, K

    2013-01-01

    Free nanoparticles of iron (Fe) and their colloids with high saturation magnetization are in demand for medical and microfluidic applications. However, the oxide layer that forms during processing has made such synthesis a formidable challenge. Lowering the synthesis temperature decreases rate of oxidation and hence provides a new way of producing pure metallic nanoparticles prone to oxidation in bulk amount (large quantity). In this paper we have proposed a methodology that is designed with the knowledge of thermodynamic imperatives of oxidation to obtain almost oxygen-free iron nanoparticles, with or without any organic capping by controlled milling at low temperatures in a specially designed high-energy ball mill with the possibility of bulk production. The particles can be ultrasonicated to produce colloids and can be bio-capped to produce transparent solution. The magnetic properties of these nanoparticles confirm their superiority for possible biomedical and other applications. (paper)

  2. Eu3+ doped yttrium oxide nano-luminophores from laser synthesis

    International Nuclear Information System (INIS)

    Ivanov, M.G.; Kynast, U.; Leznina, M.

    2016-01-01

    Nano-sized Y 2 O 3 :Eu phosphors were obtained from laser synthesis at a production rate of 25 g/h, the initial product consisting of purely monoclinic material, of primary particle sizes of 20–30 nm as could be shown by powder X-ray diffraction, TEM and BET. Despite a large amount of surface adsorbed water and O–H groups, and peculiarly, nitrous oxide species, as shown by mass spectrometer coupled thermoanalysis/thermogravimetry and FTIR, the luminescence efficiency still amounted to approximately 19% relative to bulk Y 2 O 3 :Eu. On thermal conversion at 900 °C, the transformation to cubic Y 2 O 3 :Eu, now yielding particles of approximately 60 nm appeared to be complete and had an efficiency of about 68%, however, an efficiency of 93%, approaching that of bulk Y 2 O 3 :Eu, was obtained on annealing at 1200 °C. Significantly, a rapid re-formation of carbonates takes place on the calcined samples also. - Highlights: • Nano-sized Y 2 O 3 :Eu phosphors were obtained from laser synthesis. • Luminescence efficiency of monoclinic phase 20 nm nanoparticles was about 19% relative to bulk Y 2 O 3 :Eu. • Purely cubic phase 92 nm particles demonstrated efficiency of 93% of bulk Y 2 O 3 :Eu.

  3. Management, nutrition, and lactation performance are related to bulk tank milk de novo fatty acid concentration on northeastern US dairy farms.

    Science.gov (United States)

    Woolpert, M E; Dann, H M; Cotanch, K W; Melilli, C; Chase, L E; Grant, R J; Barbano, D M

    2016-10-01

    This study investigated the relationship of management practices, dietary characteristics, milk composition, and lactation performance with de novo fatty acid (FA) concentration in bulk tank milk from commercial dairy farms with Holstein, Jersey, and mixed-breed cows. It was hypothesized that farms with higher de novo milk FA concentrations would more commonly use management and nutrition practices known to optimize ruminal conditions that enhance de novo synthesis of milk FA. Farms (n=44) located in Vermont and northeastern New York were selected based on a history of high de novo (HDN; 26.18±0.94g/100g of FA; mean ± standard deviation) or low de novo (LDN; 24.19±1.22g/100g of FA) FA in bulk tank milk. Management practices were assessed during one visit to each farm in March or April, 2014. Total mixed ration samples were collected and analyzed for chemical composition using near infrared spectroscopy. We found no differences in days in milk at the farm level. Yield of milk fat, true protein, and de novo FA per cow per day were higher for HDN versus LDN farms. The HDN farms had lower freestall stocking density (cows/stall) than LDN farms. Additionally, tiestall feeding frequency was higher for HDN than LDN farms. No differences between HDN and LDN farms were detected for dietary dry matter, crude protein, neutral detergent fiber, starch, or percentage of forage in the diet. However, dietary ether extract was lower for HDN than LDN farms. This research indicates that overcrowded freestalls, reduced feeding frequency, and greater dietary ether extract content are associated with lower de novo FA synthesis and reduced milk fat and true protein yields on commercial dairy farms. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  4. Peptide Synthesis Method and Solid Support for Use in the Method

    DEFF Research Database (Denmark)

    1994-01-01

    A method for the solid-phase synthesis of peptides or proteins in high yield and high purity uses a solid support consisting of a functionalized polystyrene-grafted polymer substrate, the grafted polystyrene chains being substantially non-cross-linked and having a chain molecular weight, not incl...... is immersed in a solution of optionally substituted styrene monomer in an alcohol such as methanol, the volume percentage of styrene in the solution preferably being about 30% v/v, and subjected to gamma irradiation....

  5. In vitro ischemia suppresses hypoxic induction of hypoxia-inducible factor-1α by inhibition of synthesis and not enhanced degradation.

    Science.gov (United States)

    Karuppagounder, Saravanan S; Basso, Manuela; Sleiman, Sama F; Ma, Thong C; Speer, Rachel E; Smirnova, Natalya A; Gazaryan, Irina G; Ratan, Rajiv R

    2013-08-01

    Hypoxia-inducible factor (HIF) mediates a broad, conserved adaptive response to hypoxia, and the HIF pathway is a potential therapeutic target in cerebral ischemia. This study investigated the mechanism by which in vitro ischemia (oxygen-glucose deprivation; OGD) affects canonical hypoxic HIF-1α stabilization. We validated the use of a reporter containing the oxygen-dependent degradation domain of HIF-1α fused to firefly luciferase (ODD-luc) to monitor quantitatively distinct biochemical events leading to hypoxic HIF-1α expression or stabilization in a human neuroblastoma cell line (SH-SY5Y). When OGD was imposed following a 2-hr hypoxic stabilization of ODD-luc, the levels of the reporter were reduced, consistent with prior models proposing that OGD enhances HIF prolylhydroxylase (PHD) activity. Surprisingly, PHD inhibitors and proteasome inhibitors do not stabilize ODD-luc in OGD. Furthermore, OGD does not affect the half-life of ODD-luc protein following hypoxia, suggesting that OGD abrogates hypoxic HIF-1α induction by reducing HIF-1α synthesis rather than by enhancing its degradation. We observed ATP depletion under OGD vs. hypoxia and propose that ATP depletion enhances translational suppression, overcoming the selective synthesis of HIF concurrent with global decreases in protein synthesis in hypoxia. Taken together, these findings biochemically characterize a practical reporter for monitoring HIF-1α levels and support a novel model for HIF regulation in an in vitro model of human ischemia. Copyright © 2013 Wiley Periodicals, Inc.

  6. Enhanced glass forming ability and refrigerant capacity of a Gd55Ni22Mn3Al20 bulk metallic glass

    International Nuclear Information System (INIS)

    Xia, L.; Chan, K.C.; Tang, M.B.

    2011-01-01

    Highlights: → A new Gd 55 Ni 22 Mn 3 Al 20 bulk metallic glass (BMG) was synthesized by minor Mn addition. → The BMG has enhanced glass forming ability and excellent refrigerant capacity (RC). → The RC of the BMG reaches a high value of 825 J kg -1 under a field of 3979 kA/m. → Its excellent RC is related to its large effective magnetic moment. - Abstract: In this work, a small amount of Mn was added to a Gd 55 Ni 25 Al 20 glass forming alloy, as a replacement for Ni, and a Gd 55 Ni 22 Mn 3 Al 20 bulk metallic glass (BMG) was obtained by suction casting. Its glass forming ability (GFA) was characterized by X-ray diffraction and differential scanning calorimetry, and its magnetic properties were measured using a magnetic property measurement system. It is found that the minor Mn addition can significantly improve both the GFA and the magnetocaloric effect (MCE) of the alloy. The refrigerant capacity (RC) of the BMG can reach a high value of 825 J kg -1 under a field of 3979 kA/m, which is about 29% larger than that of a Gd 55 Ni 25 Al 20 BMG. The effect of the minor Mn addition on the GFA and MCE of the BMG was investigated in the study.

  7. Plasma Synthesis of Nanoparticles for Nanocomposite Energy Applications

    Energy Technology Data Exchange (ETDEWEB)

    Peter C. Kong; Alex W. Kawczak

    2008-09-01

    The nanocomposite energy applications for plasma reactor produced nanoparticles are reviewed. Nanoparticles are commonly defined as particles less than 100 nm in diameter. Due to this small size, nanoparticles have a high surface-to-volume ratio. This increases the surface energy compared to the bulk material. The high surface-to-volume ratio and size effects (quantum effects) give nanoparticles distinctive chemical, electronic, optical, magnetic and mechanical properties from those of the bulk material. Nanoparticles synthesis can be grouped into 3 broad approaches. The first one is wet phase synthesis (sol-gel processing), the second is mechanical attrition, and the third is gas-phase synthesis (aerosol). The properties of the final product may differ significantly depending on the fabrication route. Currently, there are no economical large-scale production processes for nanoparticles. This hinders the widespread applications of nanomaterials in products. The Idaho National Laboratory (INL) is engaging in research and development of advanced modular hybrid plasma reactors for low cost production of nanoparticles that is predicted to accelerate application research and enable the formation of technology innovation alliances that will result in the commercial production of nanocomposites for alternative energy production devices such as fuel cells, photovoltaics and electrochemical double layer capacitors.

  8. High purity radioactive beams at the bevalac

    International Nuclear Information System (INIS)

    Alonso, J.R.; Chatterjee, A.; Tobias, C.A.

    1979-03-01

    Peripheral nuclear fragmentation reactions of primary Bevalac heavy ion beams are used to produce secondary beams of radioactive nuclei. The large cross section and small deflection of the projectile fragments lead to high production and delivery efficiency for these beams. Dispersive beam transport allows good separation and purification of the desired secondary beams. 11 C and 19 Ne beams of high purity and good intensity (almost 0.2% of the primary beam current) are presently being used for biomedical experiments

  9. An improved synthesis of pentacene: rapid access to a benchmark organic semiconductor.

    Science.gov (United States)

    Pramanik, Chandrani; Miller, Glen P

    2012-04-20

    Pentacene is an organic semiconductor used in a variety of thin-film organic electronic devices. Although at least six separate syntheses of pentacene are known (two from dihydropentacenes, two from 6,13-pentacenedione and two from 6,13-dihydro-6,13-dihydroxypentacene), none is ideal and several utilize elevated temperatures that may facilitate the oxidation of pentacene as it is produced. Here, we present a fast (-2 min of reaction time), simple, high-yielding (≥ 90%), low temperature synthesis of pentacene from readily available 6,13-dihydro-6,13-dihydroxypentacene. Further, we discuss the mechanism of this highly efficient reaction. With this improved synthesis, researchers gain rapid, affordable access to high purity pentacene in excellent yield and without the need for a time consuming sublimation.

  10. Facile synthesis and enhanced visible-light photocatalytic activity of micro/nanostructured Ag{sub 2}ZnGeO{sub 4} hollow spheres

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Jin [School of Resources and Environmental Engineering, Wuhan University of Technology, 122 Luoshi Road, Wuhan 430070 (China); The Key Laboratory of Rare Earth Functional Materials and Applications, Zhoukou Normal University, Zhoukou 466001 (China); Zhang, Gaoke, E-mail: gkzhang@whut.edu.cn [School of Resources and Environmental Engineering, Wuhan University of Technology, 122 Luoshi Road, Wuhan 430070 (China)

    2015-03-15

    Graphical abstract: - Highlights: • Micro/nanostructured Ag{sub 2}ZnGeO{sub 4} hollow spheres were synthesized by a facile method. • The formation mechanism for the Ag{sub 2}ZnGeO{sub 4} hollow spheres was investigated. • The catalyst exhibited an enhanced visible-light photocatalytic activity. • The reactive species in the photocatalytic process were studied. - Abstract: Micro/nanostructured Ag{sub 2}ZnGeO{sub 4} hollow spheres were successfully synthesized by a one-step and low-temperature route under ambient pressure. The micro/nanostructured Ag{sub 2}ZnGeO{sub 4} hollow spheres have a diameter of 1–2 μm and their shells are composed of numerous nanoparticles and nanorods. The growth process of the micro/nanostructured Ag{sub 2}ZnGeO{sub 4} hollow spheres was investigated in detail. The results indicated that the morphologies and composition of Ag{sub 2}ZnGeO{sub 4} samples were strongly dependent on the dose of the AgNO{sub 3} and reaction time. Excessive AgNO{sub 3} was favorable for the nucleation and growth rate of Ag{sub 2}ZnGeO{sub 4} crystals and the formation of pure Ag{sub 2}ZnGeO{sub 4}. Moreover, the formation mechanism of the micro/nanostructured Ag{sub 2}ZnGeO{sub 4} hollow spheres is related to the Ostwald ripening. Under the same conditions, the photocatalytic activity of micro/nanostructured Ag{sub 2}ZnGeO{sub 4} hollow spheres is about 1.7 times and 11 times higher than that of bulk Ag{sub 2}ZnGeO{sub 4} and Degussa P25, respectively. These interesting findings could provide new insight on the synthesis of micro/nanostructured ternary-metal oxides with enhanced photocatalytic activity.

  11. Ferromagnetic transitions of a spin-one Ising film in a surface and bulk transverse fields

    International Nuclear Information System (INIS)

    Saber, A.; Lo Russo, S.; Mattei, G.; Mattoni, A.

    2002-01-01

    Using the effective field theory method, we have calculated the Curie temperature of a spin-one Ising ferromagnetic film in a surface and bulk transverse fields. Numerical calculations give phase diagrams under various parameters. Surface exchange enhancement is considered. The dependence of the critical transverse field on film thickness, and phase diagrams in the fields, critical surface transverse field versus the bulk one are presented

  12. N-acetylcysteine stimulates protein synthesis in enterocytes independently of glutathione synthesis.

    Science.gov (United States)

    Yi, Dan; Hou, Yongqing; Wang, Lei; Long, Minhui; Hu, Shengdi; Mei, Huimin; Yan, Liqiong; Hu, Chien-An Andy; Wu, Guoyao

    2016-02-01

    Dietary supplementation with N-acetylcysteine (NAC) has been reported to improve intestinal health and treat gastrointestinal diseases. However, the underlying mechanisms are not fully understood. According to previous reports, NAC was thought to exert its effect through glutathione synthesis. This study tested the hypothesis that NAC enhances enterocyte growth and protein synthesis independently of cellular glutathione synthesis. Intestinal porcine epithelial cells were cultured for 3 days in Dulbecco's modified Eagle medium containing 0 or 100 μM NAC. To determine a possible role for GSH (the reduced form of glutathione) in mediating the effect of NAC on cell growth and protein synthesis, additional experiments were conducted using culture medium containing 100 μM GSH, 100 μM GSH ethyl ester (GSHee), diethylmaleate (a GSH-depletion agent; 10 μM), or a GSH-synthesis inhibitor (buthionine sulfoximine, BSO; 20 μM). NAC increased cell proliferation, GSH concentration, and protein synthesis, while inhibiting proteolysis. GSHee enhanced cell proliferation and GSH concentration without affecting protein synthesis but inhibited proteolysis. Conversely, BSO or diethylmaleate reduced cell proliferation and GSH concentration without affecting protein synthesis, while promoting protein degradation. At the signaling level, NAC augmented the protein abundance of total mTOR, phosphorylated mTOR, and phosphorylated 70S6 kinase as well as mRNA levels for mTOR and p70S6 kinase in IPEC-1 cells. Collectively, these results indicate that NAC upregulates expression of mTOR signaling proteins to stimulate protein synthesis in enterocytes independently of GSH generation. Our findings provide a hitherto unrecognized biochemical mechanism for beneficial effects of NAC in intestinal cells.

  13. Synthesis of few-layer graphene on a Ni substrate by using DC plasma enhanced chemical vapor deposition (PE-CVD)

    International Nuclear Information System (INIS)

    Kim, Jeong Hyuk; Castro, Edward Joseph; Hwang, Yong Gyoo; Lee, Choong Hun

    2011-01-01

    In this work, few-layer graphene (FLG) was successfully grown on polycrystalline Ni a large scale by using DC plasma enhanced chemical vapor deposition (DC PE-CVD), which may serve as an alternative route in large-scale graphene synthesis. The synthesis time had an effect on the quality of the graphene produced. The applied DC voltage, on the other hand, influenced the minimization of the defect densities in the graphene grown. We also present a method of producing a free-standing polymethyl methacrylate (PMMA)/graphene membrane on a FeCl 3(aq) solution, which could then be transferred to the desired substrate.

  14. Facile synthesis of uniform MWCNT@Si nanocomposites as high-performance anode materials for lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Yifan; Du, Ning, E-mail: dna1122@zju.edu.cn; Zhang, Hui; Yang, Deren

    2015-02-15

    Highlights: • A uniform SiO{sub 2} layer was deposited on multi-walled carbon nanotube. • Synthesis of uniform (MWCNT)@Si nanocomposites via the magnesiothermic reduction. • The MWCNT@Si nanocomposites show high reversible capacity and good cyclability. • Enhanced performance is attributed to porous nanostructure, introduction of MWCNTs. - Abstract: We demonstrate the synthesis of uniform multi-walled carbon nanotube (MWCNT)@Si nanocomposites via the magnesiothermic reduction of pre-synthesized MWCNT@SiO{sub 2} nanocables. At first, the acid vapor steaming is used to treat the surface, which can facilitate the uniform deposition of SiO{sub 2} layer via the TEOS hydrolysis. Then, the uniform MWCNT@Si nanocomposites are obtained on the basis of MWCNT@SiO{sub 2} nanocables via a simple magnesiothermic reduction. When used as an anode material for lithium-ion batteries, the as-synthesized MWCNT@Si nanocomposites show high reversible capacity and good cycling performance, which is better than bulk Si and bare MWCNTs. It is believed that the good electrochemical performance can be attributed to the novel porous nanostructure and the introduction of MWCNTs that can buffer the volume change, maintain the electrical conductive network, and enhance the electronic conductivity and lithium-ion transport.

  15. Radiation induced electrical degradation in crystalline Al2O3: a bulk effect

    International Nuclear Information System (INIS)

    Zong Xiangfu; Chen, Y.; Evans, B.D.; Gonzalez, R.; Sellers, C.H.

    1995-01-01

    Kesternich et al. and Jung et al. have recently raised serious questions as to whether past investigations of permanent radiation induced electrical degradation (RIED) of ceramics were actually monitoring bulk effects, as claimed. Their evidence to the contrary appears compelling. The present investigation provides evidence that bulk damage does exist and is in the form of dislocations. Discussions are focussed on some aspects of the controversy between evidence for RIED, as reported in the past, and evidence for radiation enhanced surface contaminations. ((orig.))

  16. Disgust sensitivity is primarily associated with purity-based moral judgments

    NARCIS (Netherlands)

    Wagemans, F.M.A.; Brandt, M.J.; Zeelenberg, M.

    2018-01-01

    Individual differences in disgust sensitivity are associated with a range of judgments and attitudes related to the moral domain. Some perspectives suggest that the association between disgust sensitivity and moral judgments will be equally strong across all moral domains (i.e., purity, authority,

  17. High purity zirconium obtainment through the iodine compounds transport method

    International Nuclear Information System (INIS)

    Bolcich, J.C.; Zuzek, E.; Dutrus, S.M.; Corso, H.L.

    1987-01-01

    This paper describes the experimental method and the equipment designed, constructed and actually applied for the high purity zirconium obtainment from a zirconium sponge of the nuclear type. The mechanism of purification is based on the impure metal attack with gaseous iodine (at 200 deg C) to obtain zirconium tetra iodine as main product which is then transformed into a pure zirconium base (at 1000-1300 deg C), precipitating the metallic zirconium and releasing the gaseous iodine. From the first experiences carried out, pure zirconium has been obtained from an initial filament of 0.5 mm of diameter as well as wires up to 2.5 mm of diameter. This work presents the results from the studies and analysis made to characterize the material obtained. Finally, the refining methods to which the zirconium produced may be submitted so as to optimize the final purity are discussed. (Author)

  18. Effect of relative nanohole position on colour purity of ultrathin plasmonic subtractive colour filters

    International Nuclear Information System (INIS)

    Sun, L B; Hu, X L; Zhang, D X; Zeng, Beibei; Wang, L S; Yang, S M; Tai, R Z; Fecht, H J; Jiang, J Z

    2015-01-01

    Plasmonic subtractive color filters through patterning periodic nanostructures on ultrathin Ag films deposited on a glass substrate, exhibiting good durability, simple fabrication, and flexible color tunability, have attracted considerable attention due to their tremendous potential applications. While previous studies have mainly focused on their extraordinary physical mechanisms, color purity, which is another key parameter for high quality imaging applications, has been much less investigated. In this work, we demonstrate that the relative position of nanoholes patterned on ultrathin Ag films can largely affect the color purity of plasmonic subtractive color filters. The calculated results agree reasonably well with the experimental data, revealing that the purity of subtractive colors can be improved by changing the nanohole arrays from square lattice to triangular lattice without reducing transmission at visible frequencies. In addition, underlying mechanisms are clarified by systematically analyzing the dominant valley in transmission spectra. (paper)

  19. Single Crystal Synthesis and STM Studies of High Temperature Superconductors

    Science.gov (United States)

    Barrientos, Alfonso

    1997-01-01

    This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

  20. The effect of foil purity on morphology of anodized nanoporous ZrO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Wierzbicka, Ewa; Syrek, Karolina [Department of Physical Chemistry & Electrochemistry, Faculty of Chemistry, Jagiellonian University in Krakow, Ingardena 3, 30-060 Krakow (Poland); Sulka, Grzegorz D., E-mail: sulka@chemia.uj.edu.pl [Department of Physical Chemistry & Electrochemistry, Faculty of Chemistry, Jagiellonian University in Krakow, Ingardena 3, 30-060 Krakow (Poland); Pisarek, Marcin; Janik-Czachor, Maria [Institute of Physical Chemistry, Polish Academy of Sciences, Kasprzaka 44/52, 01-224 Warsaw (Poland)

    2016-12-01

    Highlights: • Anodization of Zr with different purities in an aqueous electrolyte was studied. • The structural parameters of formed anodic oxides were compared. • Effect of Zr foil purity on the hexagonal arrangement of pores and cells in anodic ZrO{sub 2} was investigated. • Current efficiency and rate of anodic oxide formation were estimated. - Abstract: A two-step electrochemical formation of nanoporous zirconium oxide layers on different zirconium foils (purity 99.2% and 99.8%) was investigated. Anodizations were carried out at 20 V in an electrolyte composed of 1 M (NH{sub 4}){sub 2}SO{sub 4} and 0.15 M NH{sub 4}F. It was found that the thickness of grown oxide layer, and consequently, the rate of oxide formation depend slightly on the Zr substrate purity. The pore nucleation and anodization process occur easier in the presence of higher concentration of impurities. From top view SEM images, the structural parameters of oxide layers such as pore diameter, interpore distance, pore density, wall thickness and porosity of anodic oxide layers were estimated for both types of used substrates. On the other hand, cell size, intercell distance and cell density were evaluated from the bottom side of anodic oxide layers. A special emphasis was put on the qualitative analysis of hexagonal arrangement of nanopores and cells. The nanopore and cells arrangements in formed oxides were evaluated using various approaches based on Delaunay triangulations, angular distribution functions (ADFs) and pair distribution functions (PDFs). These results were supported by calculations of percentage of defective pores and cells for both types of used Zr substrates. The use of low purity Zr for anodizing does not affect drastically the morphology of formed nanoporous zirconia and offers a promising perspective to reduce production costs and increase availability of this material.

  1. Automated synthesis of the estrogen receptors imaging agent 18F-FES

    International Nuclear Information System (INIS)

    Guo Shen; Chen Guobao; Dai Hongfeng; Lin Meifu; Chen Wenxin

    2011-01-01

    Objective: 18 F-16α-17β-fluoroestradiol ( 18 F-FES), an estrogen receptors imaging agent, is synthesized with Tracerlab FX FN system. Methods: 18 F-FES is obtained by two steps reactions, including the nucleophilic displacement reaction of no-carrier-added 18 F-fluoride with 3-O-methoxymethyl-16, 17-O-sulfuryl-16-epiesteriol, then the intermediate is evaporated and hydrolyzed with HCI and finally gives 18 F-FES. Results: The synthesis of 18 F-FES can be completed in about 80 min.The radiochemical yield and radio-chemical purity are about 10% and 95% respectively. Conclusion: The procedure of synthesis is simple and automatical. 18 F-FES has an extremely low toxicity, which suggests that 18 F-FES may be a safe, a nd effective estrogen receptors imaging agent. (authors)

  2. The effect of bulk/surface defects ratio change on the photocatalysis of TiO2 nanosheet film

    Science.gov (United States)

    Wang, Fangfang; Ge, Wenna; Shen, Tong; Ye, Bangjiao; Fu, Zhengping; Lu, Yalin

    2017-07-01

    The photocatalysis behavior of TiO2 nanosheet array films was studied, in which the ratio of bulk/surface defects were adjusted by annealing at different temperature. Combining positron annihilation spectroscopy, EPR and XPS, we concluded that the bulk defects belonged to Ti3+ related vacancy defects. The results show that the separation efficiency of photogenerated electrons and holes could be significantly improved by optimizing the bulk/surface defects ratio of TiO2 nanosheet films, and in turn enhancing the photocatalysis behaviors.

  3. Large thermoelectric power factor in Pr-doped SrTiO3-δ ceramics via grain-boundary-induced mobility enhancement

    KAUST Repository

    Mehdizadeh Dehkordi, Arash

    2014-04-08

    We report a novel synthesis strategy to prepare high-performance bulk polycrystalline Pr-doped SrTiO3 ceramics. A large thermoelectric power factor of 1.3 W m-1 K-1 at 500 °C is achieved in these samples. In-depth investigations of the electronic transport and microstructure suggest that this significant improvement results from a substantial enhancement in carrier mobility originating from the formation of Pr-rich grain boundaries. This work provides new directions to higher performance oxide thermoelectrics as well as possibly other properties and applications of this broadly functional perovskite material. © 2014 American Chemical Society.

  4. Large thermoelectric power factor in Pr-doped SrTiO3-δ ceramics via grain-boundary-induced mobility enhancement

    KAUST Repository

    Mehdizadeh Dehkordi, Arash; Bhattacharya, Sriparna K.; Darroudi, Taghi; Graff, Jennifer W.; Schwingenschlö gl, Udo; Alshareef, Husam N.; Tritt, Terry M.

    2014-01-01

    We report a novel synthesis strategy to prepare high-performance bulk polycrystalline Pr-doped SrTiO3 ceramics. A large thermoelectric power factor of 1.3 W m-1 K-1 at 500 °C is achieved in these samples. In-depth investigations of the electronic transport and microstructure suggest that this significant improvement results from a substantial enhancement in carrier mobility originating from the formation of Pr-rich grain boundaries. This work provides new directions to higher performance oxide thermoelectrics as well as possibly other properties and applications of this broadly functional perovskite material. © 2014 American Chemical Society.

  5. Almost purity for overconvergent Witt vectors

    DEFF Research Database (Denmark)

    Davis, Christopher James; Kedlaya, Kiran

    2015-01-01

     . Here, we use almost purity to lift the finite étale extension of R[p−1]R[p−1] to a finite étale extension of rings of overconvergent Witt vectors. The point is that no hypothesis of p-adic completeness is needed; this result thus points towards potential global analogues of p  -adic Hodge theory....... As an illustration, we construct (φ,Γ)(φ,Γ)-modules associated with Artin Motives over QQ. The (φ,Γ)(φ,Γ)-modules we construct are defined over a base ring which seems well-suited to generalization to a more global setting; we plan to pursue such generalizations in later work....

  6. Electrochemical oxidation of 4-morpholinoaniline in aqueous solutions: Synthesis of a new trimer of 4-morpholinoaniline

    International Nuclear Information System (INIS)

    Esmaili, Roya; Nematollahi, Davood

    2011-01-01

    Research highlights: → Electrochemical study of 4-morpholinoaniline in various pHs. → Electrochemical trimerization of 4-morpholinoaniline in aqueous solution. → Green method for the synthesis of '4-morpholinoaniline-trimer'. → Potential-pH diagram for 4-morpholinoaniline. - Abstract: Electrochemical oxidation of 4-morpholinoaniline has been studied in various pHs using cyclic voltammetry and controlled-potential coulometry. The electrochemical trimerization of 4-morpholinoaniline is described and its mechanism has been studied in aqueous solution. This method provides a green, reagent-less, and environmentally friendly procedure with high atom economy, for the synthesis of '4-morpholinoaniline-trimer' using a carbon electrode in an undivided cell in good yield and purity.

  7. Convenient synthesis and application of versatile nucleic acid lipid membrane anchors in the assembly and fusion of liposomes

    DEFF Research Database (Denmark)

    Ries, Oliver; Löffler, Philipp M. G.; Vogel, Stefan

    2015-01-01

    or the construction of DNA origami structures. We herein present the synthesis and applications of versatile lipid membrane anchor building blocks suitable for solid phase oligonucleotide synthesis. These are readily synthesized in bulk in five to seven steps from commercially available precursors and can...

  8. Chemical purity using quantitative "1H-nuclear magnetic resonance: a hierarchical Bayesian approach for traceable calibrations

    International Nuclear Information System (INIS)

    Toman, Blaza; Nelson, Michael A.; Lippa, Katrice A.

    2016-01-01

    Chemical purity assessment using quantitative "1H-nuclear magnetic resonance spectroscopy is a method based on ratio references of mass and signal intensity of the analyte species to that of chemical standards of known purity. As such, it is an example of a calculation using a known measurement equation with multiple inputs. Though multiple samples are often analyzed during purity evaluations in order to assess measurement repeatability, the uncertainty evaluation must also account for contributions from inputs to the measurement equation. Furthermore, there may be other uncertainty components inherent in the experimental design, such as independent implementation of multiple calibration standards. As such, the uncertainty evaluation is not purely bottom up (based on the measurement equation) or top down (based on the experimental design), but inherently contains elements of both. This hybrid form of uncertainty analysis is readily implemented with Bayesian statistical analysis. In this article we describe this type of analysis in detail and illustrate it using data from an evaluation of chemical purity and its uncertainty for a folic acid material. (authors)

  9. High purity hydrogen production system by the PSA method

    Energy Technology Data Exchange (ETDEWEB)

    1986-01-01

    In a process developed by Nippon Steel, coke oven gas is compressed and purified of tarry matter, sulphur compounds and gum-formers by adsorption. It is then passed through a three-tower pressure-swing adsorption system to recover hydrogen whose purity can be selected in the range 99 to 99.999%. A composite adsorption agent is used.

  10. Characterization of a high-purity germanium detector for small-animal SPECT.

    Science.gov (United States)

    Johnson, Lindsay C; Campbell, Desmond L; Hull, Ethan L; Peterson, Todd E

    2011-09-21

    We present an initial evaluation of a mechanically cooled, high-purity germanium double-sided strip detector as a potential gamma camera for small-animal SPECT. It is 90 mm in diameter and 10 mm thick with two sets of 16 orthogonal strips that have a 4.5 mm width with a 5 mm pitch. We found an energy resolution of 0.96% at 140 keV, an intrinsic efficiency of 43.3% at 122 keV and a FWHM spatial resolution of approximately 1.5 mm. We demonstrated depth-of-interaction estimation capability through comparison of pinhole acquisitions with a point source on and off axes. Finally, a flood-corrected flood image exhibited a strip-level uniformity of less than 1%. This high-purity germanium offers many desirable properties for small-animal SPECT.

  11. p-Type semiconducting nickel oxide as an efficiency-enhancing anode interfacial layer in polymer bulk-heterojunction solar cells

    Science.gov (United States)

    Irwin, Michael D.; Buchholz, D. Bruce; Hains, Alexander W.; Chang, Robert P. H.; Marks, Tobin J.

    2008-01-01

    To minimize interfacial power losses, thin (5–80 nm) layers of NiO, a p-type oxide semiconductor, are inserted between the active organic layer, poly(3-hexylthiophene) (P3HT) + [6,6]-phenyl-C61 butyric acid methyl ester (PCBM), and the ITO (tin-doped indium oxide) anode of bulk-heterojunction ITO/P3HT:PCBM/LiF/Al solar cells. The interfacial NiO layer is deposited by pulsed laser deposition directly onto cleaned ITO, and the active layer is subsequently deposited by spin-coating. Insertion of the NiO layer affords cell power conversion efficiencies as high as 5.2% and enhances the fill factor to 69% and the open-circuit voltage (Voc) to 638 mV versus an ITO/P3HT:PCBM/LiF/Al control device. The value of such hole-transporting/electron-blocking interfacial layers is clearly demonstrated and should be applicable to other organic photovoltaics.

  12. Bulk Vitrification Performance Enhancement: Refractory Lining Protection Against Molten Salt Penetration

    Energy Technology Data Exchange (ETDEWEB)

    Hrma, Pavel R.; Bagaasen, Larry M.; Schweiger, Michael J.; Evans, Michael B.; Smith, Benjamin T.; Arrigoni, Benjamin M.; Kim, Dong-Sang; Rodriguez, Carmen P.; Yokuda, Satoru T.; Matyas, Josef; Buchmiller, William C.; Gallegos, Autumn B.; Fluegel, Alexander

    2007-08-06

    Bulk vitrification (BV) is a process that heats a feed material that consists of glass-forming solids and dried low-activity waste (LAW) in a disposable refractory-lined metal box using electrical power supplied through carbon electrodes. The feed is heated to the point that the LAW decomposes and combines with the solids to generate a vitreous waste form. This study supports the BV design and operations by exploring various methods aimed at reducing the quantities of soluble Tc in the castable refractory block portion of the refractory lining, which limits the effectiveness of the final waste form.

  13. Synthesis of 15N-labelled urea and methylenediurea

    International Nuclear Information System (INIS)

    Murray, T.P.; Jones, G.T.

    1985-01-01

    A new technique was developed for the large-scale synthesis of 15 N-labelled urea at low enrichment levels. The synthesis is based on nucleophilic displacement of the phenoxide ion from phenyl carbonate and uses anhydrous ammonia as the nucleophile. In previous reports a copper catalyst was used; however, in this study it was found that the copper resulted in product decomposition and tar formation, which makes product purification difficult. A novel set of reaction conditions was developed: no catalyst was used, and no product decomposition or tar formation occurred. The reaction product was easily purified, and consistently high yields of 15 N-labelled urea were obtained. 15 N-labelled methylenediurea was prepared by the dilute solution reaction of formalin with 15 N-labelled urea. The methodology developed for the reclamation of unreacted urea resulted in minimum loss of labelled urea. High performance liquid chromatography has been used to determine the chemical purity of both urea and methylenediurea. (author)

  14. Synthesis and Characterization of CdS/TiO2-Montmorillonite Nanocomposite with Enhanced Visible-Light Absorption

    OpenAIRE

    Feng-shan Zhou; Dai-mei Chen; Bao-lin Cui; Wei-heng Wang

    2014-01-01

    Sodium montmorillonite (MMT) was chosen as the carrier; a serial of CdS/TiO2-MMT nanocomposites with enhanced visible-light absorption ability was prepared by hydrothermal synthesis method combination with semiconductor compound modification method. The samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and ultraviolet visible (UV-Vis) spectroscopy; the results showed that TiO2 and CdS nanoparticles were loaded on the surface of montmorillonite unifo...

  15. Bulk Scale Formulation of Therapeutic Doses of Clinical Grade Ready-to-Use 177Lu-DOTA-TATE: The Intricate Radiochemistry Aspects.

    Science.gov (United States)

    Mathur, Anupam; Prashant, Vrinda; Sakhare, Navin; Chakraborty, Sudipta; Vimalnath, K V; Mohan, Repaka Krishna; Arjun, Chanda; Karkhanis, Barkha; Seshan, Ravi; Basu, Sandip; Korde, Aruna; Banerjee, Sharmila; Dash, Ashutosh; Sachdev, Satbir Singh

    2017-09-01

    177 Lu-DOTA-TATE is a clinically useful and promising therapeutic radiopharmaceutical for peptide receptor radionuclide therapy of neuroendocrine tumors (NETs) overexpressing somatostatin receptors. Currently, the radiopharmaceutical is prepared in-house at nuclear medicine centers, thereby restricting its use to limited centers only. In this article, the authors describe systematic studies toward bulk scale formulation of "ready-to-use" 177 Lu-DOTA-TATE using medium specific activity 177 Lu (740-1110 GBq/mg) at a centralized radiopharmacy facility. In an optimized protocol, 177 Lu-DOTA-TATE synthesis was carried out by direct heating of 177 LuCl 3 (Sp. act. 740-1110 GBq/mg) with DOTA-TATE peptide (1.5-3.0 equivalents) in ammonium acetate buffer (0.2 M) containing 2,5-dihydroxy benzoic acid (gentisic acid). Thereafter, the crude labeled product was purified using a Sep-Pak ® C18 column and diluted with acetate buffer-gentisic acid (1.5% w/v) solution to final radioactive concentration of 740 MBq/mL. This was further sterilized and dispensed as 7.4 GBq patient dose/vial with 2 days postformulation calibration. A peptide/metal ratio of 1.5-3.0 is essential for complexation wherein radiolabeling yields >90% are obtained minimizing free 177 Lu waste. For formulation of 7.4 GBq patient dose (2 days postproduction), even specific activity of about 555 GBq/mg was found to be adequate for the radiometal. The ready-to-use 740 MBq/mL 177 Lu-DOTA-TATE formulation with gentisic acid (1.5% w/v) is observed to be safe for human use for more than 1 week (radiochemical purity >98%) from the day of production when stored at -70°C. However, the target specificity may get affected beyond 2 days as the total peptide content for 7.4 GBq dose may exceed the critical peptide limit of 300 μg. Patient treatment carried with several batches of present formulation in diseased NET patients exhibited desired distribution at the tumor and its metastatic site. A ready

  16. Kit preparation of 153Sm-EDTMP and factors affecting radiochemical purity and stability

    International Nuclear Information System (INIS)

    Ferro-Flores, G.; Tendilla, J.I.; Lopez-Gomez, M.A.; Aguilar-Hernandez, F.; Gonzalez-Zavala, M.A.; Parades-Gutierrez, L.; Avila-Ramirez, E.

    1996-01-01

    A fast kit method was developed for the production of 153 Sm-EDTMP in two steps avoiding the use of nitric acid, evaporation and sterilization of the final solution by autoclave. Methods of analysis for the determination of chemical and radiochemical purity in the radiopharmaceutical solution were established. Factors affecting radiochemical purity and stability of the complex as the molar ratio of EDTMP/Sm, concentration of phosphate buffer and neutralization of EDTMP prior kit preparation were also analyzed. The use of this radiopharmaceutical in rabbits and patients showed selective skeletal uptake. (author). 5 refs., 4 figs., 3 tabs

  17. Preparation of high-purity zirconium dioxide from baddeleyite

    International Nuclear Information System (INIS)

    Voskobojnikov, N.B.; Skiba, G.S.

    1996-01-01

    Interaction of baddeleyite concentrate with calcium oxide and calcium chloride in the process of caking is studied. The influence of grain size on calcium zirconate formation is tested. Conditions for cake leaching by hydrochloric acid and zirconium(4) oxychloride purification from calcium and silicon compounds by recrystallization are reported. Zirconium dioxide corresponding to specifications (6-2 special purity) is obtained with a high (more than 90%) chemical yield. 9 refs., 1 tab

  18. Quantum and Classical Magnetoresistance in Ambipolar Topological Insulator Transistors with Gate-tunable Bulk and Surface Conduction

    Science.gov (United States)

    Tian, Jifa; Chang, Cuizu; Cao, Helin; He, Ke; Ma, Xucun; Xue, Qikun; Chen, Yong P.

    2014-01-01

    Weak antilocalization (WAL) and linear magnetoresistance (LMR) are two most commonly observed magnetoresistance (MR) phenomena in topological insulators (TIs) and often attributed to the Dirac topological surface states (TSS). However, ambiguities exist because these phenomena could also come from bulk states (often carrying significant conduction in many TIs) and are observable even in non-TI materials. Here, we demonstrate back-gated ambipolar TI field-effect transistors in (Bi0.04Sb0.96)2Te3 thin films grown by molecular beam epitaxy on SrTiO3(111), exhibiting a large carrier density tunability (by nearly 2 orders of magnitude) and a metal-insulator transition in the bulk (allowing switching off the bulk conduction). Tuning the Fermi level from bulk band to TSS strongly enhances both the WAL (increasing the number of quantum coherent channels from one to peak around two) and LMR (increasing its slope by up to 10 times). The SS-enhanced LMR is accompanied by a strongly nonlinear Hall effect, suggesting important roles of charge inhomogeneity (and a related classical LMR), although existing models of LMR cannot capture all aspects of our data. Our systematic gate and temperature dependent magnetotransport studies provide deeper insights into the nature of both MR phenomena and reveal differences between bulk and TSS transport in TI related materials. PMID:24810663

  19. Wet routes of high purity BaTiO3 nanopowders

    International Nuclear Information System (INIS)

    Wang Liqiu; Liu Liang; Xue Dongfeng; Kang Hongmin; Liu Changhou

    2007-01-01

    High purity BaTiO 3 nanopowders were prepared in wet routes through stearic acid gel (SAG) and acetic acid gel (AAG) techniques, respectively. BaTiO 3 samples were characterized by X-ray diffraction, transmission electron microscope, Fourier transform infrared spectrometry, X-ray fluorescence spectrometry, and thermal gravimetric analysis. The present results indicate that both methods have a similar reaction process during calcination, while BaTiO 3 crystallites were initially formed at 550 deg. C by SAG and 800 deg. C by AAG. Both methods could produce BaTiO 3 powders with a cubic perovskite structure, while they had different grain size distributions within 25-50 nm for SAG and 50-80 nm for AAG. BaTiO 3 samples prepared by SAG had a lower agglomeration than those by AAG. SAG has shown many distinctive advantages in the preparation of high purity BaTiO 3 nanopowders, without Ba and Ti losses and hazardous wastes

  20. Development of high purity large forgings for nuclear power plants

    International Nuclear Information System (INIS)

    Tanaka, Yasuhiko; Sato, Ikuo

    2011-01-01

    The recent increase in the size of energy plants has been supported by the development of manufacturing technology for high purity large forgings for the key components of the plant. To assure the reliability and performance of the large forgings, refining technology to make high purity steels, casting technology for gigantic ingots, forging technology to homogenize the material and consolidate porosity are essential, together with the required heat treatment and machining technologies. To meet these needs, the double degassing method to reduce impurities, multi-pouring methods to cast the gigantic ingots, vacuum carbon deoxidization, the warm forging process and related technologies have been developed and further improved. Furthermore, melting facilities including vacuum induction melting and electro slag re-melting furnaces have been installed. By using these technologies and equipment, large forgings have been manufactured and shipped to customers. These technologies have also been applied to the manufacture of austenitic steel vessel components of the fast breeder reactors and components for fusion experiments.

  1. Development of high purity large forgings for nuclear power plants

    Science.gov (United States)

    Tanaka, Yasuhiko; Sato, Ikuo

    2011-10-01

    The recent increase in the size of energy plants has been supported by the development of manufacturing technology for high purity large forgings for the key components of the plant. To assure the reliability and performance of the large forgings, refining technology to make high purity steels, casting technology for gigantic ingots, forging technology to homogenize the material and consolidate porosity are essential, together with the required heat treatment and machining technologies. To meet these needs, the double degassing method to reduce impurities, multi-pouring methods to cast the gigantic ingots, vacuum carbon deoxidization, the warm forging process and related technologies have been developed and further improved. Furthermore, melting facilities including vacuum induction melting and electro slag re-melting furnaces have been installed. By using these technologies and equipment, large forgings have been manufactured and shipped to customers. These technologies have also been applied to the manufacture of austenitic steel vessel components of the fast breeder reactors and components for fusion experiments.

  2. Gravimetric and volumetric determination of the purity of electrolytically refined silver and the produced silver nitrate

    Directory of Open Access Journals (Sweden)

    Ačanski Marijana M.

    2007-01-01

    Full Text Available Silver is, along with gold and the platinum-group metals, one of the so called precious metals. Because of its comparative scarcity, brilliant white color, malleability and resistance to atmospheric oxidation, silver has been used in the manufacture of coins and jewelry for a long time. Silver has the highest known electrical and thermal conductivity of all metals and is used in fabricating printed electrical circuits, and also as a coating for electronic conductors. It is also alloyed with other elements such as nickel or palladium for use in electrical contacts. The most useful silver salt is silver nitrate, a caustic chemical reagent, significant as an antiseptic and as a reagent in analytical chemistry. Pure silver nitrate is an intermediate in the industrial preparation of other silver salts, including the colloidal silver compounds used in medicine and the silver halides incorporated into photographic emulsions. Silver halides become increasingly insoluble in the series: AgCl, AgBr, AgI. All silver salts are sensitive to light and are used in photographic coatings on film and paper. The ZORKA-PHARMA company (Sabac, Serbia specializes in the production of pharmaceutical remedies and lab chemicals. One of its products is chemical silver nitrate (argentum-nitricum (l. Silver nitrate is generally produced by dissolving pure electrolytically refined silver in hot 48% nitric acid. Since the purity of silver nitrate, produced in 2002, was not in compliance with the p.a. level of purity, there was doubt that the electrolytically refined silver was pure. The aim of this research was the gravimetric and volumetric determination of the purity of electrolytically refined silver and silver nitrate, produced industrially and in a laboratory. The purity determination was carried out gravimetrically, by the sedimentation of silver(I ions in the form of insoluble silver salts: AgCl, AgBr and Agi, and volumetrically, according to Mohr and Volhardt. The

  3. Effects of Synthesis and Spark Plasma Sintering Conditions on the Thermoelectric Properties of Ca3Co4O9+δ

    DEFF Research Database (Denmark)

    Wu, NingYu; Holgate, Tim; Van Nong, Ngo

    2013-01-01

    Ca3Co4O9+δ samples were synthesized by solid-state (SS) and sol–gel (SG) reactions, followed by spark plasma sintering under different processing conditions. The synthesis process was optimized and the resulting materials characterized with respect to their microstructure, bulk density, and therm......Ca3Co4O9+δ samples were synthesized by solid-state (SS) and sol–gel (SG) reactions, followed by spark plasma sintering under different processing conditions. The synthesis process was optimized and the resulting materials characterized with respect to their microstructure, bulk density...

  4. One-step synthesis of zero-dimensional hollow nanoporous gold nanoparticles with enhanced methanol electrooxidation performance.

    Science.gov (United States)

    Pedireddy, Srikanth; Lee, Hiang Kwee; Tjiu, Weng Weei; Phang, In Yee; Tan, Hui Ru; Chua, Shu Quan; Troadec, Cedric; Ling, Xing Yi

    2014-09-17

    Nanoporous gold with networks of interconnected ligaments and highly porous structure holds stimulating technological implications in fuel cell catalysis. Current syntheses of nanoporous gold mainly revolve around de-alloying approaches that are generally limited by stringent and harsh multistep protocols. Here we develop a one-step solution phase synthesis of zero-dimensional hollow nanoporous gold nanoparticles with tunable particle size (150-1,000 nm) and ligament thickness (21-54 nm). With faster mass diffusivity, excellent specific electroactive surface area and large density of highly active surface sites, our zero-dimensional nanoporous gold nanoparticles exhibit ~1.4 times enhanced catalytic activity and improved tolerance towards carbonaceous species, demonstrating their superiority over conventional nanoporous gold sheets. Detailed mechanistic study also reveals the crucial heteroepitaxial growth of gold on the surface of silver chloride templates, implying that our synthetic protocol is generic and may be extended to the synthesis of other nanoporous metals via different templates.

  5. Enhancement of entanglement in the nonlinear optical coupler by homodyne-mediated feedback

    Energy Technology Data Exchange (ETDEWEB)

    Ke Shasha [Department of Physics, Huazhong Normal University, Wuhan 430079 (China); Cheng Guiping [Department of Physics, Huazhong Normal University, Wuhan 430079 (China); Zhang Lihui [Department of Physics, Jianghan University, Wuhan 430056 (China); Li, Gao-xiang [Department of Physics, Huazhong Normal University, Wuhan 430079 (China)

    2007-07-28

    The enhancement of the intracavity entanglement of a nonlinear coupler via homodyne-mediated quantum feedback is investigated. It is found that the feedback can effectively enhance the squeezing, entanglement and purity of a two-mode field in the nonlinear coupler by appropriately choosing the quadrature angle at which the quantum feedback is introduced.

  6. Templated green synthesis of plasmonic silver nanoparticles in onion epidermal cells suitable for surface-enhanced Raman and hyper-Raman scattering

    DEFF Research Database (Denmark)

    Palanco, Marta Espina; Mogensen, Klaus Bo; Guehlke, Marina

    2016-01-01

    We report fast and simple green synthesis of plasmonic silver nanoparticles in the epidermal cells of onions after incubation with AgNO3 solution. The biological environment supports the generation of silver nanostructures in two ways. The plant tissue delivers reducing chemicals for the initial...... for one-and two-photon-excited spectroscopy such as surface enhanced Raman scattering (SERS) and surface enhanced hyper-Raman scattering (SEHRS). Our studies demonstrate a templated green preparation of enhancing plasmonic nanoparticles and suggest a new route to deliver silver nanoparticles as basic...... building blocks of plasmonic nanosensors to plants by the uptake of solutions of metal salts....

  7. Synthesis and Characterization of Novel Quaternary Thioaluminogermanates

    KAUST Repository

    Al-Bloushi, Mohammed

    2013-05-01

    Metal chalcogenides form an important class of inorganic materials, which include several technologically important applications. The design of metal chlcogenides is of technological interest and has encouraged recent research into moderate temperature solid-state synthetic methods for the single crystal growth of new materials. The aim of this project is the investigation and development of synthetic methodology for the synthesis of novel metal chlcogenides. The new inorganic compounds of the type “M(AlS2)(GeS2)” (M = Na and K) are new metal-chalcogenides, synthesized by the classical solid state approach. The characterization of these compounds was carried out by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Single crystal and powder X-ray diffraction, solid state Nuclear Magnetic Resonance (NMR), Ultraviolet-visible (UV-VIS), Infrared (IR) and Raman spectroscopy. These theses study the synthesis of metal chalcogenides through the use of standard chemical techniques. The systematic studies demonstrate the effect of the reactants ratio and reaction temperature on the synthesis and growth of the single crystals. Metal chalcogenides have several potential applications in gas separation, ion exchange, environmental remediation, and energy storage. Especially, the ion exchange materials have found\\tpossible applications in waste-water treatment, water softening, metal separation, and production of high purity water.

  8. Grain Size and Phase Purity Characterization of U3Si2 Pellet Fuel

    Energy Technology Data Exchange (ETDEWEB)

    Hoggan, Rita E. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Tolman, Kevin R. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Cappia, Fabiola [Idaho National Lab. (INL), Idaho Falls, ID (United States); Wagner, Adrian R. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Harp, Jason M. [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2018-05-01

    Characterization of U3Si2 fresh fuel pellets is important for quality assurance and validation of the finished product. Grain size measurement methods, phase identification methods using scanning electron microscopes equipped with energy dispersive spectroscopy and x-ray diffraction, and phase quantification methods via image analysis have been developed and implemented on U3Si2 pellet samples. A wide variety of samples have been characterized including representative pellets from an initial irradiation experiment, and samples produced using optimized methods to enhance phase purity from an extended fabrication effort. The average grain size for initial pellets was between 16 and 18 µm. The typical average grain size for pellets from the extended fabrication was between 20 and 30 µm with some samples exhibiting irregular grain growth. Pellets from the latter half of extended fabrication had a bimodal grain size distribution consisting of coarsened grains (>80 µm) surrounded by the typical (20-30 µm) grain structure around the surface. Phases identified in initial uranium silicide pellets included: U3Si2 as the main phase composing about 80 vol. %, Si rich phases (USi and U5Si4) composing about 13 vol. %, and UO2 composing about 5 vol. %. Initial batches from the extended U3Si2 pellet fabrication had similar phases and phase quantities. The latter half of the extended fabrication pellet batches did not contain Si rich phases, and had between 1-5% UO2: achieving U3Si2 phase purity between 95 vol. % and 98 vol. % U3Si2. The amount of UO2 in sintered U3Si2 pellets is correlated to the length of time between U3Si2 powder fabrication and pellet formation. These measurements provide information necessary to optimize fabrication efforts and a baseline for future work on this fuel compound.

  9. Applied Hts Bulks and Wires to Rotating Machines for Marine Propulsion

    Science.gov (United States)

    Miki, M.; Felder, B.; Kimura, Y.; Tsuzuki, K.; Taguchi, R.; Shiliang, Y.; Xu, Y.; Ida, T.; Izumi, M.

    2010-04-01

    High-temperature superconductors allow a compact and efficient way to provide high-torque density to rotating machines with excellent operation. A field pole, providing flux density of more than 1.5 T around the armature, was initially designed for an axial-gap type with the flux parallel to the rotor axis. Melt-growth Gd-123 bulks as well as Bi-2223 wire windings have been successfully assembled on the rotor disk. No iron core was used, though being an auxiliary flux control found in most HTS motors. Both bulk and wire types have realized a practical motor operation within a limited output range. For bulks, a 15 kW, 720 rpm, synchronous motor was designed and tested in the group of TUMSAT, Kitano Seiki and University of Fukui. A bulk field pole was cooled down by liquid nitrogen and was magnetized in the motor. To enhance the output power to more than 30 kW, we developed a thermosyphon system using condensed neon. Another field pole with HTS wire for large-scale marine propulsion is also discussed on a 100 kW, 230 rpm tested machine. A closed-cycle condensed neon associated with thermal insulation is also reported.

  10. Surface-spin magnetism of antiferromagnetic NiO in nanoparticle and bulk morphology

    International Nuclear Information System (INIS)

    Jagodic, M; Jaglicic, Z; Jelen, A; Dolinsek, J; Lee, Jin Bae; Kim, Hae Jin; Kim, Young-Min

    2009-01-01

    The surface-spin magnetism of the antiferromagnetic (AFM) material NiO in nanoparticle and bulk morphology was investigated by magnetic measurements (temperature-dependent zero-field-cooled (zfc) and field-cooled (fc) dc susceptibility, ac susceptibility and zfc and fc hysteresis loops). We addressed the question of whether the multisublattice ordering of the uncompensated surface spins and the exchange bias (EB) effect are only present in the nanoparticles, originating from their high surface-to-volume ratio or if these surface phenomena are generally present in the AFM materials regardless of their bulky or nanoparticle morphology, but the effect is just too small to be detected experimentally in the bulk due to a very small surface magnetization. Performing experiments on the NiO nanoparticles of different sizes and bulk NiO grains, we show that coercivity enhancement and hysteresis loop shift in the fc experiments, considered to be the key experimental manifestations of multisublattice ordering and the EB effect, are true nanoscale phenomena only present in the nanoparticles and absent in the bulk.

  11. Creating high-purity angular-momentum-state Rydberg atoms by a pair of unipolar laser pulses

    Science.gov (United States)

    Xin, PeiPei; Cheng, Hong; Zhang, ShanShan; Wang, HanMu; Xu, ZiShan; Liu, HongPing

    2018-04-01

    We propose a method of producing high-purity angular-momentum-state Rydberg atoms by a pair of unipolar laser pulses. The first positive-polarity optical half-cycle pulse is used to prepare an excited-state wave packet while the second one is less intense, but with opposite polarity and time delayed, and is employed to drag back the escaping free electron and clip the shape of the bound Rydberg wave packet, selectively increasing or decreasing a fraction of the angular-momentum components. An intelligent choice of laser parameters such as phase and amplitude helps us to control the orbital-angular-momentum composition of an electron wave packet with more facility; thus, a specified angular-momentum state with high purity can be achieved. This scheme of producing high-purity angular-momentum-state Rydberg atoms has significant application in quantum-information processing.

  12. Purity of potassium iodide necessary for its use in phasers

    Energy Technology Data Exchange (ETDEWEB)

    Sood, B R [Punjabi Univ., Patiala (India). Dept. of Physics

    1981-08-16

    The purity requirements in KI crystals are discussed necessary to have longer lifetimes of phonons for its use in phasers. The main contribution to the phonon scattering at low temperatures arises from the scattering by natural isotopes (/sup 39/K, /sup 40/K, /sup 41/K, /sup 127/I).

  13. Improved methods to determine radionuclidic purity of F-18 compounds

    DEFF Research Database (Denmark)

    Jørgensen, Thomas; Micheelsen, Mille Ankerstjerne; Jensen, Mikael

    2012-01-01

    Current revisions of monographs for F-18 pharmaceuticals in the European Pharmacopoeia (Ph. Eur.) (Ph. Eur., 2011) call for a radionuclidic purity (RNP) of or better than 99.9%. However, the current method is not sufficient nor effective for testing this required RNP level. We present a theoretical...

  14. Nanopatterned Bulk Metallic Glass Biosensors.

    Science.gov (United States)

    Kinser, Emily R; Padmanabhan, Jagannath; Yu, Roy; Corona, Sydney L; Li, Jinyang; Vaddiraju, Sagar; Legassey, Allen; Loye, Ayomiposi; Balestrini, Jenna; Solly, Dawson A; Schroers, Jan; Taylor, André D; Papadimitrakopoulos, Fotios; Herzog, Raimund I; Kyriakides, Themis R

    2017-12-22

    Nanopatterning as a surface area enhancement method has the potential to increase signal and sensitivity of biosensors. Platinum-based bulk metallic glass (Pt-BMG) is a biocompatible material with electrical properties conducive for biosensor electrode applications, which can be processed in air at comparably low temperatures to produce nonrandom topography at the nanoscale. Work presented here employs nanopatterned Pt-BMG electrodes functionalized with glucose oxidase enzyme to explore the impact of nonrandom and highly reproducible nanoscale surface area enhancement on glucose biosensor performance. Electrochemical measurements including cyclic voltammetry (CV) and amperometric voltammetry (AV) were completed to compare the performance of 200 nm Pt-BMG electrodes vs Flat Pt-BMG control electrodes. Glucose dosing response was studied in a range of 2 mM to 10 mM. Effective current density dynamic range for the 200 nm Pt-BMG was 10-12 times greater than that of the Flat BMG control. Nanopatterned electrode sensitivity was measured to be 3.28 μA/cm 2 /mM, which was also an order of magnitude greater than the flat electrode. These results suggest that nonrandom nanotopography is a scalable and customizable engineering tool which can be integrated with Pt-BMGs to produce biocompatible biosensors with enhanced signal and sensitivity.

  15. The effect of bulk/surface defects ratio change on the photocatalysis of TiO_2 nanosheet film

    International Nuclear Information System (INIS)

    Wang, Fangfang; Ge, Wenna; Shen, Tong; Ye, Bangjiao; Fu, Zhengping; Lu, Yalin

    2017-01-01

    Highlights: • The defect behaviors of TiO_2 nanosheet array films were studied by positron annihilation spectroscopy. • Different bulk/surface defect ratios were realized by annealing at different temperature. • It was concluded that bulk defects are mainly Ti"3"+ vacancy defects. • The separation efficiency of photogenerated electrons and holes could be significantly improved by optimizing the bulk/surface defects ratio. - Abstract: The photocatalysis behavior of TiO_2 nanosheet array films was studied, in which the ratio of bulk/surface defects were adjusted by annealing at different temperature. Combining positron annihilation spectroscopy, EPR and XPS, we concluded that the bulk defects belonged to Ti"3"+ related vacancy defects. The results show that the separation efficiency of photogenerated electrons and holes could be significantly improved by optimizing the bulk/surface defects ratio of TiO_2 nanosheet films, and in turn enhancing the photocatalysis behaviors.

  16. An Improved Synthesis of Pentacene: Rapid Access to a Benchmark Organic Semiconductor

    Directory of Open Access Journals (Sweden)

    Glen P. Miller

    2012-04-01

    Full Text Available Pentacene is an organic semiconductor used in a variety of thin-film organic electronic devices. Although at least six separate syntheses of pentacene are known (two from dihydropentacenes, two from 6,13-pentacenedione and two from 6,13-dihydro-6,13-dihydroxypentacene, none is ideal and several utilize elevated temperatures that may facilitate the oxidation of pentacene as it is produced. Here, we present a fast (~2 min of reaction time, simple, high-yielding (≥90%, low temperature synthesis of pentacene from readily available 6,13-dihydro-6,13-dihydroxypentacene. Further, we discuss the mechanism of this highly efficient reaction. With this improved synthesis, researchers gain rapid, affordable access to high purity pentacene in excellent yield and without the need for a time consuming sublimation.

  17. Impact of precursor purity on optical properties and radiation detection of CsI:Tl scintillators

    Energy Technology Data Exchange (ETDEWEB)

    Saengkaew, Phannee; Cheewajaroen, Kulthawat; Yenchai, Chadet; Thong-aram, Decho [Chulalongkorn University, Department of Nuclear Engineering, Faculty of Engineering, Bangkok (Thailand); Sanorpim, Sakuntam [Chulalongkorn University, Department of Physics, Faculty of Science, Bangkok (Thailand); Jitpukdee, Manit [Kasetsart University, Department of Applied Radiation and Isotope, Faculty of Science, Bangkok (Thailand); Yordsri, Visittapong; Thanachayanont, Chanchana [Ministry of Science and Technology, National Metal and Materials Technology Center, National Science and Technology Development Agency, Pathumthani (Thailand); Nuntawong, Noppadon [Ministry of Science and Technology, National Electronic and Computer Technology Center, National Science and Technology Development Agency, Pathumthani (Thailand)

    2016-08-15

    Cesium iodide doped with thallium (CsI:Tl) crystals was grown to develop the gamma-ray detectors by using low-cost raw materials. Effect of impurities on optical properties and radiation detection performance was investigated. By a modified homemade Bridgman-Stockbarger technique, CsI:Tl samples were grown in two levels of CsI and TlI reactant materials, i.e., having as a very high purity of 99.999 % and a high purity of 99.9 %. XRD measurements indicate CsI:Tl crystals having a good quality with a dominant (110) plane. Having a cubic structure, a lattice constant of CsI crystals of 0.4574 nm and a crystallite size of 43.539 nm were obtained. From the lower-purity raw materials, calcite was found in an orange crystal with a lattice constant of 0.4560 nm and a crystallite size of 43.089 nm. By PL measurements, the optical properties of the CsI:Tl crystals were analyzed. ∝540-nm-wavelength PL peak was observed from the colorless high-purity crystal, and ∝600-nm-wavelength PL peak was observed from the orange crystal. The brighter PL emission was obtained from the orange crystals suggesting impurities. CsI:Tl surface morphology by SEM exhibited a smooth surface with some parallel crystal facets. For electrical properties of high-quality CsI:Tl crystals, the electrical resistances were 230 ± 16 MΩ in cross-sectional direction and 714 ± 136 MΩ in vertical direction with respect to more homogeneous crystal quality in cross-sectional direction than that in vertical direction. TEM measurement was applied to evaluate the microstructure of colorless CsI:Tl crystal with different patterns of a cubic structure. Both CsI:Tl crystals show good efficiencies and good resolutions. Maintaining the same electronic conditions and amplifications, the colorless CsI:Tl scintillators represented a higher detection efficiency at 122 keV of Co-57 of 78.4 % and the energy resolution of 23.3 % compared to the detection efficiency of 75.9 % and the energy resolution of 34.6 % of the

  18. The European Expression Of Interest For High Purity U-233 Materials

    Energy Technology Data Exchange (ETDEWEB)

    Giaquinto, Joseph M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Younkin, James R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-04-01

    The purpose of this letter report is to document the response for an Expression of Interest (EOI) sent to the European Safeguards and research and development (R&D) scientific communities for the distribution of small amounts of high purity 233U materials for use in safeguards, nonproliferation, and basic R&D in the nuclear disciplines. The intent for the EOI was to gauge the level of international interest for these materials from government and research institutions with programmatic missions in the nuclear security or nuclear R&D arena. The information contained herein is intended to provide information to assist key decision makers in DOE as to the ultimate disposition path for the high purity materials currently being recovered at Oak Ridge National Laboratory (ORNL) and only those items for which there is no United States (U.S.) sponsor identified.

  19. The synthesis of [4-3H]oxiracetam - a novel nootropic agent

    International Nuclear Information System (INIS)

    Crowe, A.M.; Lawrie, K.W.M.; Saunders, D.; Pfeiffer, U.

    1991-01-01

    The synthesis of [4- 3 H]oxiracetam from ethyl 2-(4-chloro-3-oxo-butyramido)acetate is described. Ethyl 2-(4-chloro-3-oxo-butyramido)-acetate was reduced with sodium borotritide at Amersham International plc to give ethyl 2-(4-chloro-[3- 3 H]-3-hydroxy-butyramido)acetate. This was elaborated, in four steps, to [4- 3 H]oxiracetam in 4.8% overall radiochemical yield, furnishing 5735 μCi, 212 MBq, 41.8 μg, of specific activity 21.7 Ci/mmol, 802.9 GBq/mmol, and radiochemical purity of greater than 98%. (author)

  20. Synthesis and 125I labeling of N-succinimidyl-3-(tri-n-butylstannyl)benzoate

    International Nuclear Information System (INIS)

    Liu Zhenfeng; Wang Yongxian; Zhou Wei; Wang Lihua; Xia Jiaoyun; Yin Duanzhi

    2005-01-01

    N-succinimidyl-3-(tri-n-butylstannyl)benzoate (ATE) and N-succinimidyl-3-iodo-benzoate (SIB) is synthesized. The structures of ATE and SIB are confirmed with 1 HNMR, MS and IR. The yields of ATE and SIB are 45.4% and 71.4%, respectively. ATE is labeled with 125 I. The labeling field is 93.0% and radiochemical purity is over 98.0%. The synthesis and the labeling of ATE have a important value for indirect label of radiopharmaceuticals. (authors)