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  • Author or Editor: S. K. Mehta x
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The transformation of gibbsite have been studied under hydrothermal influence. Results of the X-ray diffraction analysis of the samples heated at different temperatures from 170°C to 265°C are also discussed in detail. The percentage of the boehmite phase formed, due to the transformation of the gibbsite, have been determined by comparing the intensity of the most strongest reflection of the boehmite phase with a fully transformed sample. The activation energy value calculated form X-ray diffractograms is almost comparable with the value calculated from main DTA endotherm of gibbsite.

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Abstract

Thermal behavior of various synthesized transition metal surfactant complexes of the type [M(CH3COO)4]2−[C12H25NH3 +]2 where M: Cu(II), Ni(II), Co(II) has been investigated using Thermogravimetric Analysis (TGA). It was found that pyrolytic decomposition occurs with melting in metal complexes, and that metal oxides remain as final products. The activation energy order obtained, E Cu > E Ni > E Co, could be explained on the basis of size of transition metal ion and metal ligand bond strength. In the course of our investigation on the decomposition of complexes, we carried out a comparative study of different measurement and calculation procedures for the thermal decomposition. A critical examination was made of the kinetic parameters of non-isothermal thermoanalytic rate measurement by means of several methods such as Coats–Redfern (CR), Horowitz–Metzger (HM), van Krevelen (vK), Madhusudanan–Krishnan–Ninan (MKN), and Wanjun–Yuwen–Hen–Cunxin (WYHC). The most appropriate method among these was determined for each decomposition step according to the least-squares linear regression. It was found that the results obtained using CR method differ considerably from HM method, as the former method involves a lot of approximations and is not much reliable. The application of thermoanalytic techniques to the investigation of rate processes has also been discussed.

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Summary  

The present paper reports the Differential Scanning Calorimetric (DSC) study of some Ag doped Se-Te chalcogenide glasses. DSC runs were taken at different heating rates. Well-defined endothermic and exothermic peaks were obtained at glass transition and crystallization temperatures. The variation of glass transition temperature T gwith Ag concentration has been studied. It has been found that T gdecreases with increase in Ag concentration. The heating rate dependence of T gis used to evaluate the activation energy of glass transition (DE t). The value ofDE thas been found to increase with increase in Ag concentration followed by nearly constant value at higher concentrations of Ag.

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Clay from the Nagrotta area of Jammu (J & K State, India) was calcined at various temperatures. The products were analysed by X-ray diffraction. The mode of loss of hydroxyl group from the structure with respect to temperature is discussed. The results were supplemented by differential thermal analysis. The calcined products were subjected to lime reactivity tests and the data obtained were correlated with those of the above study to investigate the pozzolanic activity at various temperatures.

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A novel, simple, robust, and rapid reversed-phased high-performance liquid chromatographic method has been developed for the separation and quantitative determination of the related substances of ezetimibe and simvastatin in combined dosage forms. Successful separation of the drug from the process-related impurities and degradation products formed under stress conditions was achieved on Inertsil ODS-3V (150 × 4.6 mm, 5.0 μm) column. The gradient liquid chromatography (LC) method employs solution A and solution B as mobile phase. The solution A contains 0.1% orthophosphoric acid solution in water, and solution B contains 0.1% orthophosphoric acid solution in acetonitrile. Flow rate was monitored at 2.0 mL/min, and the ultraviolet (UV) detection, at 238 nm. In forced degradation studies, the effect of acid, base, oxidation, UV light, and temperature was investigated, showing that good resolution between the peaks corresponds to process-related impurities and degradation products from both analyte. The performance of the method was validated according to the present International Conference on Harmonization (ICH) guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, ruggedness, and robustness. To the best of our knowledge, a rapid LC method, which separates all the impurities of ezetimibe and simvastatin in combined dosage forms, disclosed in this investigation was not published elsewhere.

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