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Abstract  

Positron annihilation lifetime spectra and ionic conductivity have been measured for poly(etherurethane)-LiClO4 as a function of temperature. The effects of Li salt on glas transition free volume and ionic conductivity have been discussed. A correlation between fractional free volume and ionic conductivity was first experimentally confirmed by using the free volume theory.

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Thermodynamic investigation of several natural polyols (II)

Heat capacities and thermodynamic properties of sorbitol

Journal of Thermal Analysis and Calorimetry
Authors: B. Tong, Z. Tan, Q. Shi, Y. Li, and S. Wang

Abstract  

The low-temperature heat capacity C p,m of sorbitol was precisely measured in the temperature range from 80 to 390 K by means of a small sample automated adiabatic calorimeter. A solid-liquid phase transition was found at T=369.157 K from the experimental C p-T curve. The dependence of heat capacity on the temperature was fitted to the following polynomial equations with least square method. In the temperature range of 80 to 355 K, C p,m/J K−1 mol−1=170.17+157.75x+128.03x 2-146.44x 3-335.66x 4+177.71x 5+306.15x 6, x= [(T/K)−217.5]/137.5. In the temperature range of 375 to 390 K, C p,m/J K−1 mol−1=518.13+3.2819x, x=[(T/K)-382.5]/7.5. The molar enthalpy and entropy of this transition were determined to be 30.35±0.15 kJ mol−1 and 82.22±0.41 J K−1 mol−1 respectively. The thermodynamic functions [H T-H 298.15] and [S T-S 298.15], were derived from the heat capacity data in the temperature range of 80 to 390 K with an interval of 5 K. DSC and TG measurements were performed to study the thermostability of the compound. The results were in agreement with those obtained from heat capacity measurements.

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Abstract  

In the present study, the characteric-structure relationship of epoxidized soybean oils (ESO) with various degrees of epoxidation has been investigated. FTIR analysis was used to identify the relative extent of epoxidation of the samples during the epoxidation reaction. The viscosities of ESO were much higher than that of the raw oil, viscosity increased with degree of epoxidation. The viscous-flow activation energy of ESO was determined to be higher than that of the raw oil (20.72 to 77.93% higher). Thermogravimetry analysis (TG) of ESO was used to investigate the thermodynamic behavior of the samples. With increasing degree of epoxidation, the thermal stability of the samples initially decreased, then increased at the final reacting stage. Differential scanning calorimeter (DSC) indicated that the melting point of ESO was higher than that of soybean oil. Gel permeation chromatography (GPC) indicated the molecular mass of the samples increased initially, then decreased, with an increase in the extent of epoxidation.

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The use of polypropylene materials in industry for food packaging is increasing. The presence of additives in the polymer matrix enables the modification or improvement of the properties and performance of the polymer, but these additives are potential risk for human health. In this context, an efficient analytical method for the quantitative determination of three antioxidants (2,6-di-tert-butyl-4-methylphenol (BHT), dibutylhydroxyphenylpropionic acid stearyl ester (Irganox 1076), and tns-(2.4-di-tert-butyl)-phosphite (Irgafos 168)) and five ultraviolet stabilizers (2-(2′-hydroxy-5′-methylphenyl) (UV-P), (2′-hydroxy-3′-tert-5′-methylphenyl)-5-chloroben zotriazole (UV-326), 2-(2′-hydroxy-3′,5′-di-tert-butylphenyl)-5-chlorobenzotriazole (UV-327), 2-(2H-benzotriazol- 2-yl)-4-(1,1,3,3-tetramethylbutyl)phenol(UV-329), and 2-hydroxy-4(octyloxy) benzophenone (UV-531)) in polypropylene food packaging and food simulants by high-performance liquid chromatography (HPLC) has been developed. Parameters affecting the efficiency in the process such as extraction and chromatographic condition were studied in order to determine operating conditions. The analytical method showed good linearity, presenting correlation coefficients (R ≥ 0.9977) for all additives. The limits of detection and quantification were between 0.03 and 0.30 μg mL−1 and between 0.10 and 1.00 μg mL−1 for eight analytes, respectively. Average spiked recoveries in blank polypropylene packaging and food simulants were in the range of 80.4–99.5% and 75.2–106.7%, with relative standard deviations in the range of 0.9–9.1% and 0.2–9.8%. Dissolving the polypropylene food packaging with toluene and precipitating by methanol was demonstrated more effective than ultrasonic extract with acetonitrile or dichloromethane for extracting the additives. The method was successfully applied to commercial polypropylene packaging determination, Irgafos 168 and UV-P were frequently found in six commercial polypropylene films, and the content ranged from 166.47 ± 5.11 to 845.27 ± 29.31 μg g−1 and 2.10 ± 0.29 to 19.23 ± 1.26 μg g−1, respectively.

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Abstract  

N,N-dimethylhydroxylamine (DMHA) is a novel salt-free reducing reagent used in the separation U from Pu and Np in the reprocessing of power spent fuel. This paper reports on the radiolysis of aqueous DMHA solution and its radiolytic liquid organics. Results show that the main organics in irradiated DMHA solution are N-methyl hydroxylamine, formaldehyde and formic acid. The analysis of DMHA and N-methyl hydroxylamine were performed by gas chromatography, and that of formaldehyde was performed by ultraviolet–visible spectrophotometry. The analysis of formic acid was performed by ion chromatography. For 0.1–0.5 mol L−1 DMHA irradiated to 5–25 kGy, the residual DMHA concentration is (0.07–0.47) mol L−1, the degradation rate of DMHA at 25 kGy is 10.1–30.1%. The concentrations of N-methylhydroxylamine, formaldehyde and formic acid are (8.25–19.36) × 10−3, (4.20–36.36) × 10−3 and (1.35–10.9) × 10−4 mol L−1, respectively. The residual DMHA concentration decreases with the increasing dose. The concentrations of N-methylhydroxylamine and formaldehyde increase with the dose and initial DMHA concentration, and that of formic acid increases with the dose, but the relationship between the concentration of formic acid and initial DMHA concentration is not obvious.

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Abstract  

The present paper based on experimental results contains discussions and suggestions on the possible use of fine-powder Al2O3 and SiO2 with their original content of microimpurities of up to 40 elements, as multielement standards for neutron activation analysis. For example, activation analysis of As, Au, Ba, Cr, Cs, Fe, Ga, K, Ni, Sb, Sc, Se, Sr, Ta, Th, Ti, U, W, Zn, Zr and the REE La, Ce, Nd, Sm, Eu, Tb, Tm, Yb contained in SiO2 powder off MERCK reagents showed their concentrations to be 0.1 to 5% of those in IAEA standard SL-1. In Al2O3 this level is even lower, approximately 10 times and more for the majority of the above-mentioned elements. As Al2O3 and SiO2 are good sorbents for the majority of elements, additional introduction of some elements may allow more methods of analysis. The homogeneity of Al2O3 and SiO2 samples both in the original state and after introduction of some elements was determined by neutron activation analysis, and the SD did not exceed 1% for an Al2O3 sample weight of 0.1 g, and 2% for SiO2.

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Abstract  

No-carrier-added48V at 37 Mbq (mCi) levels was produced at the JRC-Ispra cyclotron by (, n) reactions on a scandium target and used to label environmental and physiological levels of vanadium for metallobiochemical investigations. The radiochemical separation of48V from Sc is very simple and rapid and involves a single chromatographic step after fast dissolution of the bombarded target. The yield of the separation and the radioisotopic purity of the separated48V were nearly 100% A summary of the main results concerning different metabolic investigations on rats including absorption, retention, transfer of48V from mothers to newborns, binding with enzymes as well as uptake by cell culture system is reported.

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Abstract  

[Cd(NTO)4Cd(H2O)6]4H2O was prepared by mixing the aqueous solution of 3-nitro-1,2,4-triazol-5-one and cadmium carbonate in excess. The single crystal structure was determined by a four-circle X-ray diffractometer. The crystal is monoclinic, space group C2/c with crystal parameters of a=2.1229(3) nm, b=0.6261(8) nm, c=2.1165(3) nm, β=90.602(7), V=2.977(6) nm3, Z=4, Dc=2.055 gcm−3, μ=15.45 cm−1, F(000)=1824, λ(MoKα)=0.071073 nm. The final R is 0.0282. Based on the results of thermal analysis, the thermal decomposition mechanism of [Cd(NTO)4Cd(H2O)6]4H2O was derived. From measurements of the enthalpy of solution of [Cd(NTO)4Cd(H2O)6]4H2O in water at 298.15 K, the standard enthalpy of formation, lattice energy, lattice enthalpy and standard enthalpy of dehydration have been determined as -(1747.84.8), -2394, -2414 and 313.6 kJ mol−1 respectively.

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Abstract  

The effects of cisplatin and its trans isomer transplatin on the thermal denaturation of G-actin were studied with a Micro DSC-III differential scanning calorimeter. The denaturation enthalpy of G-actin was found to be 12 J g–1, and the denaturation temperature was 328 K. The thermal denaturation curve showed that increasing cisplatin concentration decreased the enthalpy change. However, after the ratio of cisplatin to G-actin attained 8:1 (mol:mol), the denaturation enthalpy no longer decreased. Transplatin decreased the enthalpy change more rapidly. In contrast with cisplatin, the denaturation peak at 328 K disappeared, and a strong exothermic peak appeared at 341 K when the ratio of transplatin to G-actin was 8:1 (mol:mol). The enthalpy change was 75 J g–1, which is far in excess of the range of weak interactions. This strong exothermic phenomenon probably reflects the agglutination of protein. The effects of cisplatin and transplatin on the number of the free thiol groups of G-actin are discussed.

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Abstract  

The heat capacities of trans-(R)-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropanecarboxylic acid in the temperature range from 78 to 389 K were measured with a precise automatic adiabatic calorimeter. The sample was prepared with the purity of 0.9874 mole fraction. A solid-liquid fusion phase transition was observed in the experimental temperature range. The melting point, T m, enthalpy and entropy of fusion, Δfus H m, Δfus S m, were determined to be 344.75±0.02 K, 13.75±0.07 kJ mol−1, 39.88±0.21 J K−1 mol−1, respectively. The thermodynamic functions of the sample, H (T)-H (298.15), S (T)-S (298.15) and G (T)-G (298.15), were reported with a temperature interval of 5 K. The thermal decomposition of the sample was studied by TG analysis, the thermal decomposition starts at ca. 421 K and terminates at ca. 535 K, the maximum decomposition rate was obtained at 525 K. The order of reaction, pre-exponential factor and activation energy, are n=0.14, A=1.15·108 min−1, E=66.27 kJ mol−1, respectively.

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