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Human exposure to perchlorate is commonplace because it is a contaminant of drinking water, certain foods, and breast milk. The U.S. Environmental Protection Agency (EPA) conducted a perchlorate risk...Full Text Available

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... adsorption aqueous solutions astatine complexes astatine ions enthalpy organic

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Here we demonstrate that the as-prepared MCM-41 mesoporous silica material, which is synthesized using cetyltrimethylammonium bromide as a cationic surfactant exhibits very high capacity for perchlorate uptake from solutions. Thus we discover a new function for the as-synthesized mesoporous materials containing cationic surfactants. These materials are shown to have better capacity than the currently used activated carbon, which is preloaded with cationic surfactant. As-synthesized MCM-41 has a higher removal of perchlorate with 0.378???0.038?meq/g than the surfactant modified activated carbon sample, which removed 0.304???0.005?meq/g i.e., MCM-41 has a 24 % higher capacity than the surfactant modified activated carbon sample for perchlorate uptake because of higher surfactant content and ...

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The method of augmented plane wave (APW) is used to obtain the band structure of the SmS compound in the semiconductor and metal phases. The noncentral part of the Coulomb electron-electron interaction is taken into account in the first order perturbation theory. In this case the radial part of the wave APW-function is taken as a zero approximation function. A multiplet structure of the excited configuration f"5d, which provides a good description of the X-ray photoelectron spectrum and optical spectrum epsilon_2(#omega#), is obtained. The configuration fd is calculated for the interpretation of the optical absorption spectrum of the samarium monosulfide metal phase. (author).

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A series of #alpha#-sialon (#alpha#') compositions containing mixed stabilising cations were prepared, by introducing additional CaO to a basic Sm #alpha#-sialon compositions. The thermal stability of these Sm-Ca-containing #alpha#-sialon phases was investigated using XRD, SEM and EDXS techniques. It was found that the addition of calcium into the Sm #alpha#-sialon systems greatly improved the stability of the #alpha#-sialon phases. Calcium was found to be incorporated into the #alpha#-sialon structure, coexistent with the samarium, and partitioning of the calcium and samarium was observed between the #alpha#' phase and grain boundary phases. This indicates a technique which may be used to improve the thermal stability of the #alpha#' phase while maintaining good refractory phases at the sialon grain boundaries.

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Samarium cobaltite ceramic perovskites, with and without platinum particles dispersion, are possible candidates as electrode for electrochemical conversion of hydrocarbon and for intermediate temperature solid oxide fuel cells (ITSOFC). In this work, samarium cobaltites were synthesized by the combustion method using cobalt, and samarium nitrates as cation precursors and urea as fuel. For containing-platinum compositions Pt (II) acetyl acetonate was also employed as precursor. The effect of Sr on the phase formation and its electrical behavior is also studied. Specific surface area (BET), SEM-EDX, TEM and XRD analysis are used to characterize the powders obtained. Powders were pressed into pellets and sintered in air in the temperature range of 1200 -1400 C. Electrical impedance spectroscopy studies (EIS) are performed on sintered samples. The as-prepared powders showed an amorphous structure and by TEM a very small ...

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Fluorocarbon polymers are used to enhance thermal stability and electrostatic protection of composite propellant compositions. A precipitation technique has been developed to coat ammonium perchlorate (AP) using a copolymer of hexafluoropropylene and vinylidene fluoride (HFP-VF) with the help of solvent-counter solvent method. The coated AP has been used to prepare propellant compositions in different ratio based on hydroxyl terminated polybutadiene (HTPB), aluminium powder along with uncoated AP and studied for viscosity build-up and visco-elastic behaviour as well as mechanical, ballistic, thermal and sensitivity properties keeping 86% solid loading. The data on viscosity build-up indicate that as the percentage of viton coated AP increases end of mix viscosity and viscosity build-up inc...

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Apparent molar heat capacities for KI[sub 3](aq) were determined from flow-microcalorimetric measurements of KI(aq) solutions containing dissolved iodine. From these, the conventional partial molar heat capacity C[sub p,2][sup [infinity

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Uranium-aluminum alloys with a significant enrichment of uranium with "2"3"3U or "2"3"5U serve as nuclear fuels in research reactors. The quality assurance of this fuel requires, among other things, precise knowledge that all trace metal constituents that affect neutron economy, fuel integrity, and fuel fabrication process parameters are well within the specification limits. Trace metal characterization of "2"3"5U-Al alloy has been carried out by atomic spectrometry. The trace metal constituents of interest are grouped into common metals (silver, boron, calcium, cadmium, cobalt, chromium, copper, iron, magnesium, manganese, molybdenum, sodium, nickel, lead, silicon, tin, titanium, vanadium, tungsten, and zinc) and lanthanides (cerium, dysprosium, europium, gadolinium, holminium, lutetium, samarium, and terbium). The elements yttrium and zirconium are grouped with the latter in view of the chemical separation procedure used. The alloy samples are dissolved in 6 M ...

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Crystals of a new ternary samarium rhenium oxide, Sm{sub 3}ReO{sub 7} were obtained by subsolidus reaction of samariumsesquioxide and rheniumdioxide (ratio 1.5:1) in sealed Pt-10Rh-tubes at 1673 K. The structure was determined by single-crystal X-ray diffraction. Sm{sub 3}ReO{sub 7} crystallizes in the orthorohombic system with unit cell dimensions a = 10.736(5), b = 7.392(3), and c = 7.519(3) in space group Cmcm (No. 63) with Z = 4. The structure consists of ReO{sub 6} octahedra, distorted SmO{sub 6} octahedra, and SmO{sub 8} prisms that are interconnected to each other to form a three-dimensional network. Rhenium has the formal oxidation state of +5 but no metal-metal bond is observed in this compound. The observed magnetization in the temperature range 4 K < T < 52 K is explained by a Curie-Weiss law modified by a temperature independent Van Vleck paramagnetism of samarium (3+).

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In the MnIII complex of the title compound, [MnIII(C18H12N4O2)(H2O)2]ClO4, the MnIII atom is coordinated by four N atoms from the bpb2- [1,2-bis(pyridine-2-carboxamido)benzene] ligand located in the equatorial plane and two O atoms of water molecules at axial positions, yielding a distorted MnN4O2 octahedral coordination geometry. The bpb2- ligand is nearly planar, with a maximum deviation of 0.2311 (3) A from the mean plane. The MnIII complex cation and the perchlorate anion, both of which are located on twofold rotation axes, are connected by O-H...O and C-H...O hydrogen bonds into a three-dimensional supramolecular network structure.

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Crystallization points of aqueous solution of the systems M(ClO_4)_2-H_2O (M"2 = Mg"2"+, Ca"2"+, Sr"2"+, Ba"2"+), depending on the salt concentration, were identified by visual-polythermal method. Relying on model notions on the structure of the electrolyte solutions, specific features of strontium perchlorate solubility polytherm and concentration dependence of the relative dynamic viscosity of the salt aqueous solutions are discussed

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The Sputter coefficient of accelerated CO{sub 2} cluster ions hitting surfaces of various materials is investigated. For copper it varies proportional to the 2nd power of the energy between 155 and 260 keV. The rate of erosion for different target materials varies by two orders of magnitude from tungsten to PMMA. Diamond is eroded fairly quickly, while aluminum is eroded less than corundum (Al{sub 2}O{sub 3}). No simple correlation of the sputter coefficient on the bulk material properties is found. For copper the angular distribution of sputtered material is measured and found to be following roughly a cosine distribution. By using masks different microstructures have been produced in cobalt-samarium magnets, diamond and glass. (orig.)

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Very important performances in the practical use of solid propellants are combustion and physical properties. Among the present solid propellants, composite propellants used ammonium perchlorate (AP) as oxidizers are adopted widely now due to these excellent performances. Recently, a combination of ammonium nitrates (AN) as oxidizers and azido polymers as binders in expected as the propellants which control decrease of combustion properties and satisfy unsensitivity. However, in order to use these azido polymers/AN propellants in practice, further, it is necessary to improve the specific impulse and the burning rate. In this report, aiming to improve the combustion properties of BAMO/NMMO/AN propellants, the sensitivity and the combustion properties of propellants added high energetic plasticizers in binders, further, displaced a part of AN to cyclotetramethylenetetranitramine (HMX) and double based base-grain (BG) are described. 8 refs., 3 figs., 3 tabs.

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Formation of the complex of the univalent astatine cation with nitrilotriacetic acid (AtL)[sup 2-] and its stability constant (lgK[sub 1]=8.97(4), 25degC, [mu]=0.1) have been found experimentally for the first time. The complex is stable in perchlorate solutions in presence of 5 . 10[sup -3] mol . l[sup -1] of the oxidizer Na[sub 2]S[sub 2]O[sub 8] in the interval 4[<=]pH[<=]8.5. The complex is supposed to be destroyed in weak alkaline solutions by reduction of astatine to astatide. The deprotonation constant of hypoastatic acid pK[sub dp]=5.23(9) was found to be lower than determined previously. The investigation was carried out by the method of ion electrophoresis in free electrolyte solutions. (orig.).

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An effective method of enhancing charge injection and electroluminescence efficiency of polymer-based light emitting diode is introduced. Spin-coated films of poly (N-vinylcarbazole) blended with electron-transport material (Bu-PBD), laser dye (Coumarin6), and the typical supporting electrolyte (tetraethylammonium perchlorate; TEAP) were examined and it was found that the injection current and luminance of the light emitting diode doped with TEAP were enhanced dramatically after heat-treatment at 80 deg. C and appropriate biasing in an external electric field of 1.5x10"8 V/m at this temperature. The thermally stimulated current (TSC) was also measured to investigate the relaxation process of ionic space charges in the films. The relaxation times of ionic polarization were found to be related to the cation size of the electrolyte. And the relaxation time becomes long enough by the use of TEAP doping.

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Relative densities and relative massic heat capacities have been measured for aqueous solutions of Y(ClO_4)_3, Yb(ClO_4)_3, Dy(ClO_4)_3, and Sm(ClO_4)_3 at T=(288.15,298.15,313.15, and 328.15) K and p=0.1 MPa. These measurements were made in the concentration range 0.01624#<=#m/(mol#centre dot#kg"-"1)#<=#0.41822 using a Sodev 02D Vibrating Tube Densimeter and a Picker Microflow Calorimeter, respectively. To counter the potential effects of hydrolysis, aqueous solutions of the investigated salts were acidified with perchloric acid. After correcting for the presence of the acid, the measured properties were used to calculate apparent molar volumes and apparent molar heat capacities for solutions of the perchlorate salts in water. The calculated apparent molar properties were modeled at each investigated temperature using Pitzer ion interaction equations to produce estimates of apparent molar volumes and heat capacities at infinite dilution. ...

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The crystal structure of the compound Sm_4Pd_4Si_3 was determined by the single-crystal method (KM-4 automatic diffractometer, Mo K#alpha# radiation). Sm_4Pd_4Si_3 has the monoclinic Nd_4Rh_4Ge_3 type structure: space group C2/c, mC44 (No. 15), a=20.693(6), b=5.584(1), c=7.699(2) A, #beta#=109.48(3) , V=838 A"3, Z=4, #mu#=36.23 mm"-"1, R_F=0.0537, R_W=0.0435 for 1652 unique reflections. The coordination numbers of samarium atoms are 17 and 18. For palladium and silicon atoms icosahedra and trigonal prisms with additional atoms are typical as coordination polyhedra. The structure of Sm_4Pd_4Si_3 is composed of fragments of the YPd_2Si and Y_3Rh_2Si_2 structure in a ratio 1:1. (orig.).

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The NiO-samaria doped ceria (SDC) composite powders were prepared by spray pyrolysis technique at temperatures between 400 and 1000 C. The variation of the particle structure was investigated by X-ray diffraction (XRD), X-ray absorption fine structure (XAFS), scanning electron microscope (SEM), and transmission electron microscope (TEM)-energy-dispersive X-ray spectroscopy (EDS). The thermal analysis of raw materials was also carried out. The following facts became clear in this study. Ceria and nickel have been already separated at 400 C. Samaria is amorphous phase below 600 C, and is dissolved in ceria at 600 C or higher. Samaria is distributed uniformly inside the particles before dissolving in ceria. The thermal decomposition temperatures of metal nitrate are: cerium < nickel < samarium. The results of these analyses were explained without contradiction. It was found that it is important to optimize the state of liquid drop before thermal ...

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The formation of the melilite solid solution phase (M'), Sm_2Si_3_-_xAl_xO_3_+_xN_4_-_x, in an #alpha#-sialon sample of overall composition Sm_0_._6Si_9_._2_8Al_2_._6_9O_1_._3_6N_1_4_._7_6, was studied as a function of time in the temperature interval 1,375--1,525 C. The #alpha#-sialon ceramic contained only minor amounts of the 21R sialon polytype and some residual grain-boundary glass before heat treatment. In situ studies by high-temperature X-ray diffraction were combined with postsintering heat treatment followed by quenching. The M'-phase was found to be formed by two different mechanisms: either crystallization of the residual grain-boundary liquid or a direct decomposition of the #alpha#-sialon phase. The liquid crystallized during the first 10--15 min of heat treatment, yielding a rapid M'-phase formation, and further formation of M'-phase continued at a much slower rate, related to the decomposition of #alpha#-sialon.

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Schiff-base condensation of a equimolar proportion of diacetyl-monoxime monohydrazone and 1-methylimidazole-2-carboxaldehyde in methanol gives rise to the imidazole azine, 3-(1-methylimidazol-2-yl)methylenehydrazonobutan-2-one oxime(HL). Reaction of 1:1 stoichiometric proportion of HL with copper(II)perchlorate hexahydrate in methanol yields a dimeric oximato bridged copper compound, [Cu2L2(H2O)2](ClO4)2 (1). The compound is characterized by C, H and N analyses, FT-IR, ESI?MS, conductivity measurement, UV?Vis spectra and X-ray single crystal diffraction. The title compound (1) crystallizes in the monoclinic space group P21/c with a?=?6.8533 (8), b?=?18.413 (2), c?=?11.7399 (14) ?, ??=?93.685 (2)?, V?=?1478.4 (3) ?3 and Z?=?2. The geometry around each copper center is distorted square pyram...

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Lithium hexa-fluoro-phosphate LiPF{sub 6} is recommended for the replacement of the toxic LiAsF{sub 6} and the explosive perchlorates (like LiClO{sub 4}) in rechargeable lithium electrochemical generators. The aim of this work is to develop a new method of synthesis of this salt and to check its stability with respect to carbonated solvents: ethylene carbonate (EC), propylene carbonate (PC) and dimethyl-carbonate (DMC) in already optimized EC/DMC and PC/DMC binary mixtures. Two methods using HPF{sub 6} are proposed: the first one uses the direct neutralization of this commercial acid by LiOH in aqueous, alcoholic or acetonitrile environment, while in the second one LiPF{sub 6} is obtained from pyridinium hexa-fluoro-phosphate synthesized from HPF{sub 6} using a new and simple protocol. (J.S.) 24 refs.

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This work was made with the purpose to complete information about the hydrolysis constants of Europium (III) in high ion strength media. So it was determined at a ion forces media 4, 5 and 6 M of sodium perchlorate at 303 K. The method used was the potentiometric with the aid of the Super quad computer program. In high ion strength media, the measurements of p H do not correspond directly to negative logarithm of the concentration of hydrogen ions, by this it is necessary to calibrate the electrode in these conditions. The Europium was hydrolized at pC{sub H} values greater 6 in all cases. The potentiometric method used under the described experimental conditions is adequate to determine the hydrolysis constants of Europium (III). According to the results and diagrams of chemical species of Europium obtained we can conclude that the hydrolysis constants, differ by its distribution but not in its identity. (Author)

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The adsorption of glycolate anions at sputtered gold thin-film electrodes was studied in perchloric acid solutions by cyclic voltammetry experiments combined with in situ Surface Enhanced Raman Scattering (SERS) and Surface Enhanced Infrared Reflection Absorption Spectroscopy under attenuated total reflection conditions (ATR-SEIRAS). Theoretical harmonic vibrational frequencies and band intensities obtained from B3LYP/LANL2DZ,6-31+G(d) calculations for glycolate species adsorbed on Au clusters with (1 1 1) orientation were used to interpret the experimental spectra. Vibrational data confirm the bidentate bonding of glycolate anions through the oxygen atoms of the carboxylate group, in a bridge configuration with the OCO plane perpendicular to the metal surface. The DFT calculations show no significant effect of the total charge of the metal cluster-adsorbate adduct on the vibrational frequencies of adsorbed glycolate species. The infrared experimental study is ...