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Abstract
Thermal reactions of polyethylene with coal were studied. Coal used exhibited an endothermal effect in the temperature range of 425-495C with a flat maximum (about 460C). In contrast, polyethylene alone was decomposed in the temperature range of 420-540C (mainly of 485-540C) with the significant DSC maximum at 510C. In the presence of coal this maximum shifted to lower temperature (483C), therefore, coal promoted the decomposition of polyethylene. As decomposition of polyethylene yields alkenes and alkadienes, the thermal reaction of polyethylene with coal under low temperature conditions can be described as two-stage process in which the first stage includes the decomposition of polyethylene giving unsaturated hydrocarbons and the second stage adsorption and hydrogenation of these products (mainly by coal hydrogen) on the inner surfaces of semicoke and coal.
Abstract
The temperature calibration of a TA Instruments 3200-2920 DSC has been performed on cooling using the isotropic → nematic, isotropic → cholesteric and other liquid crystal → liquid crystal transitions of thermally stable, high purity liquid crystals. The thermal stability of these liquid crystals has been verified by measuring the temperature of the mentioned transitions during cyclic heating and cooling experiments. Correspondence has been established between the real and indicated temperature during cooling for all combinations of heating and cooling rates of practical interest: correction values were determined to the indicated temperature in order to obtain the real temperature on cooling. These correction values were calculated as the average from the temperatures of four or five different liquid crystal transitions for each heating-cooling rate combination. The accuracy of the temperature calibration on cooling is ca. 0.2‡C for heating and cooling rates up to 20‡C min−1.
In the range from −50° to +130°C, the temperature dependence of the heat capacity for different kinds of gelatins with water contents of from 2 to 95% was studied by the DSC method. It was shown that, in all studied cases, metastable collagen-like structures are formed in gels or crystalline gelatins, with thermodynamic parameters depending on the formation conditions. The characteristic properties of the glass transitions in amorphous gelatins and crystalline gelatins with different melting heats and different contents of the ordered phase were established. Special attention is paid to the structural properties of free and bound water. The dependence of the glass transition temperatureT g on the bound water content was shown to be of general applicability for many denatured biopolymers. Free water in gelatins, in distinction to the bound water, does not act as a plasticizer, but forms a rigid matrix inhibiting the glass transition.
DSC analysis of human fat tissue in steroid induced osteonecrosis
A preliminary study
Abstract
Osteonecrosis (ON) of the femoral frequently occurs after steroid medication. One of the final pathways leading to steroid induced ON is thought to be pathologic fat metabolism. The pathobiological mechanism underlying the induction of fat metabolism outslides by steroids leading to ON has not been fully elucidated. The purpose of this study was to examine the intraoperative obtained gluteal fat tissue from ON patients with histology, gas chromatography (GC) and differential scanning calorimetry (DSC) and to compare them with otherwise healthy patient’s samples. The histological sections showed no significant differences compared with the control group. GC revealed that fraction of saturated fatty acids decreased in ON samples from mean values of controls of 24% to 21, the polyunsaturated fraction from 20 to 14%. The monounsaturated acids showed an increase from mean rate of 52% of the controls to 65% of steroid treated samples. DSC curves correlate with chromatographic analysis of the tissue fatty acids (Steroid treated, heating between 0–100°C: T m=5.7°C, ΔH= −15.8J/g−1; heating between −20–100°C: Tm= −9.96 and 5.85°C, ΔH= −59.17 and −16.2 J g−1. Non-necrotic, heating between 0–100°C: two separable transition with Tm=5.7 and 9.9°C, total ΔH= −20.8 J g−1; heating between −20–100°C: Tm= −10.9 and 4.95°C, total ΔH= −75.8 J g−1.) Our preliminary findings are rather tendentious. Further investigations are needed with higher sample rate and under other anamnestic circumstances too.
Gas reactions, catalyzed by solid catalysts, can be measured by DSC. In the experimental set-up an open sample pan with catalyst (powder or pellet) is placed on the sample side of the DSC sensor. The reactive gas mixture flows through the cell and reacts on the catalyst surface. The heat effect, caused by this reaction, results into a DSC signal.
DSC investigations have been performed for a series of compounds Ba2YCu3Oy with the oxygen content varying in the rangey=6.0...6.9 by means of various heat treatments at 800–1200 K followed by quenching, or through the chemical extraction of oxygen by placing the sample in dihydrogen at 470–490 K. The sample preserving a constant oxygen content during heating in nitrogen exhibited exothermal effects between 450 and 850 K. It has been shown that the ΔH vs. y function reaches maximum aty ≈ 6.5. Kinetic measurements have shown that the diffusive mobility of oxygen atoms in the lattice is responsible for these effects, viz. the Arrhenius and cooperative processes of reorganization in the non-equilibrium oxygen subsystem of the bulk.
Abstract
Water molecules in hydrogels were classified into three categories according to phase transition behavior; non-freezing, freezing bound and free water. Melting, crystallization, and glass transition of water in hydrogels reflected the state of the water interacting with polysaccharides. Freezing bound water formed metastable ice by slow cooling and formed amorphous ice by quenching. From the isothermal crystallization measurement, nucleation rate and crystal growth rate were obtained. The crystal growth rate of freezing bound water was about ten times slower than that of free water. The DSC characterization of water in hydrogels was summarized.
Abstract
The dehydrated lactose forms αH and αS were investigated by time- and temperature-resolved X-ray powder diffractometry and differential scanning calorimetry. We found different X-ray structures for these two forms, which is probably related to the different dehydration processes. The rapidly dehydrated form αH obviously has the same X-ray structure as the starting material α-lactose monohydrate, although the crystallinity is reduced. A thermally induced transition of the αH-form into the αS-form was observed. This transition should allow one to “switch” between the physicochemical properties of the excipient, which may be important for applications in pharmaceutical and food industries.
Abstract
A new method for determining the degree of conversion of gelation (αgel) and gel time (t gel) at gel point using a single technology, DSC, is discussed in this work. Four kinds of thermoset resins are evaluated. It is found that the mutation points of reduced reaction rate (V r ) vs. reaction conversion (α) curves, corresponding with the changes of reaction mechanism, represents the gelation of the reaction. The α at the mutation point is defined as αgel. From isothermal DSC curves, the point at αgel is defined ast gel. Traditional techniques (ASTM D3532 and DSC method) are also used to determine αgel andt gel in order to demonstrate this new method. We have found that the results obtained from this new method are very consistent with the results obtained from traditional methods.
Abstract
In this research, differential scanning calorimetry (DSC) was used to determine the combustion behavior and kinetic analysis of raw and cleaned coal samples of different size fractions. DSC curves of the three coal samples (Soma, Tuncbilek and Afsin Elbistan) showed two reaction regions. The first reaction region was due to moisture loss (endothermic) and observed in the temperature range of ambient to 150C. The second region was the exothermic region due to the combustion and observed in the temperature range of 150 to 600C. Kinetic parameters of the samples were determined using Roger and Morris kinetic model and the results are discussed.