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The mechanism of the dehydration and condensation reaction taking place during calcination of Co1/2Ca1/2(H2PO4)2.2H2O has been followed by means of thermal analyses at non-isothermal (dynamic) and at quasi-isothermal-isobaric conditions. Isothermal calcination of starting binary dihydrogenphosphate was carried out in electric oven at various temperatures. The reaction intermediates and products obtained were analyzed by instrumental analytical methods and extraction experiments with solutions of inorganic compounds and with organic reagents. Effect of water vapour pressure has been followed on course, rate and yield of the condensation reactions and of the formation of main considered product-binary cyclo-tetraphosphate (tetrametaphosphate)c-CoCaP4O12.

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Selenium nuclides are available from thermal neutron induced nuclear fission of 235U at the gas-jet facility at the Swiss spallation neutron source (SINQ) at Paul Scherrer Institute, Switzerland. The formation of stable selenium compounds, their transport yields using the gas-jet system and their relative thermal decomposition temperature were investigated under oxidizing and reducing conditions in the target chamber. Using O2, H2, CO, and propene as additional gases, the selenium isotopes are suggested to form H2SeO3, H2Se, COSe, and C3H6Se, respectively, with overall 84Se yields of 1.5%, 4.7%, 6.3%, and 21.9%, respectively. Adsorption enthalpy, vapour pressure, solubility and acidity data for these species were collected from the literature or estimated from other known thermochemical properties. Carrier free bromine isotopes (84Br, 86Br) in the form of HOBr were obtained by thermally decomposing H2SeO3 and retaining elemental Se under oxygen rich conditions on quartz at 400 K.

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Enthalpies and entropies of sublimation for N-acetylglycine amide (NAGA), N-acetyl-L-alanine amide (L-NAAA), and N-acetyl-D-leucine amide (D-NALA) were determined from the dependence of their vapour pressures on temperature, as measured by the torsion-effusion method.

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The use of modulated temperature differential scanning calorimetry (TMDSC) and differential scanning calorimetry (DSC) in the measurement of the glass transition temperature (T g) in polymer-water systems presents several important problems. These include the presence of water evaporation endotherms, partial water evaporation during scanning, changes in pan integrity due to vapour pressure developing in the pan headspace during analysis, and possible interaction between water and polymer at high temperatures. As a result, in most of the cases, only apparent T g values can be obtained. In this study, TMDSC and DSC were used to determinate the thermal behaviour of methylmethacrylate copolymer-water systems. The samples were previously equilibrated at different relative humidities (RH) from 0 to 97% RH. Three different pan arrangements were used. In addition, thermogravimetric analysis (TG) was carried out to determine the initial amount of water in the sample. None of the pan arrangements was entirely suitable for the study of these systems. When sealed pans were used, the plastification effect of water was observed. Some evidence of degradation was also observed in which water and methylmethacrylate appeared to play roles.

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A thermobalance for studies of the high-temperature sulfidation of metals and alloys is described. This apparatus permits the determination of mass changes in the sulfidized sample as functions of temperature and sulfur vapour pressure with an accuracy of 10−6 g. Besides heterogeneous kinetics measurements, it has been shown that the chemical diffusion coefficients and deviations from stoichiometry of metal sulfides can also be studied as functions of temperature and sulfur pressure by means of equilibration measurements.

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A new tin dithiocarbamate containing sulphur bridges, di-μ-sulphidobis [bis(N,N-diethyldithiocarbamato)tin(IV)], has been isolated from the thermal decomposition of tetrakis(N,N-diethyldithiocarbamato)tin(IV). A dimeric structure is proposed on the basis of results from mass spectrometry, infrared spectroscopy, thermal analysis and vapour pressure osmometry.

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A miniaturized effusion cell adapted to a Sorption LKB microcalorimeter has been designed, built and tested. Vaporization is performed isothermally into a vacuum through a small orifice permitting a vapour pressure very close to the equilibrium values. The cell has been tested by measuring the enthalpies of vaporization at 298.15 K of reference liquid compounds (water, benzene, propanol-1, propanol-2) with a reproducibility better than 1%. Enthalpies of vaporization of butanol-1 and deuterated water have also been determined.

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Fluorophenyl derivatives of elements II-VI groups

Phase transitions thermodynamics and growing films by CVD

Journal of Thermal Analysis and Calorimetry
Authors: L. Zelenina, T. Chusova, Yu. Stenin, and V. Bakovets

Abstract  

The enthalpies and temperatures of melting of RSi(CH3)3, R4Si, R3P, R3As, R3Sb, R3Bi, R2Te and R2Hg (R=C6F5) were obtained by scanning calorimetry measurements. The pressure of the saturated and unsaturated vapors of RSi(CH3)3, R2Si(CH3)2, R4Si, R3Ga, R3P, R3As, R3Sb, R3Bi, R2Te and R2Hg has been measured by the static method with a membrane-gauge manometer. It was established that all investigated substances proceeded to vapor as monomers. Equations approximating the dependences of saturated vapor pressures on temperature and the enthalpies and entropies of vaporization were obtained. Grafite films with silicon intercalated up to 25 at.% were grown by CVD using R4Si as a precursor. These films showed semiconductor properties in the temperature interval 80–300 K.

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The results of this study indicate that in terms of efficiency, the Packard 2250Ca liquid scintillation spectrometer is sensitive to the scintillation cocktail employed for241Pu analysis, particularly when the burst counting circuit is enabled. Cocktails exhibiting low t-SIE values should be avoided since quenching has a critical influence on such a low energy emitter. This effect would be independent of burst circuitry use. Cocktails which include naphthalene type derivatives such as the alkylnaphthalene solvent employed in Optiphase HiSafe 3 and Ultima Gold should be avoided since the broad pulse shapes produced are incompatible with the burst counting circuit which distinguishes background events from true events by means of pulse shape/duration analysis. Efficiency is also sensitive to the concentration of bis-MSB employed in conjunction with the primary fluor. Enhancements in efficiency are observed with appropriate concentrations. These results are in line with previous work with14C and are postulated as being a consequence of sharpening prompt pulse widths or suppression of afterpulsing. It is recommended that Instafluor should be used to maximize response, or a cocktail such as butyl-PBD/bis-MSB in pseudocumene at rates of 6 and 1.5 mg ml–1, respectively, where a lower vapor pressure solvent is particularly required.

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Abstract  

Uranium dendrites which were deposited at a solid cathode of an electrorefiner contained a certain amount of salts. These salts should be removed for the recovery of pure metal using a cathode processor. In the uranium deposits from the electrorefining process, there are actinide chlorides and rare earth chlorides in addition to uranium chloride in the LiCl–KCl eutectic salt. The evaporation behaviors of the actinides and rare earth chlorides in the salts should be investigated for the removal of salts in the deposits. Experiments on the salt evaporation of rare earth chlorides in a LiCl–KCl eutectic salt were carried out. Though the vapor pressures of the rare earth chlorides were lower than those of the LiCl and KCl, the rare earth chlorides were co-evaporized with the LiCl–KCl eutectic salt. The Hertz–Langmuir relation was applied for this evaporation, and also the evaporation rates of the salt were obtained. The co-evaporation of the rare earth chlorides and LiCl–KCl eutectic were also discussed.

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