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, Chrissafis K , Lalia-Kantouri M . Luminescence and thermal behavior by simultaneous TG/DTG-DTA coupled with MS of neutral copper(I) complexes with heterocyclic thiones . J Therm Anal Calorim. 2010 . doi: 10.1007/s10973

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. Advanced inorganic chemistry . 5 New York : Wiley ; 1988 . 14. Skoczylas , ML , Mikuli , E , Szklarzewicz , J , Hetmańczyk , J . Thermal behaviour, phase transition and molecular

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Abstract  

New complexes of 2-benzoyl-pyridil-isonicotinoylhydrazone (L) with Cu(II), Co(II), Ni(II) and Mn(II), having formula of type [ML2] SO4·xH2O (M = Cu2+, Co2+, Ni2+, x = 2 and M = Mn2+, x = 3), have been synthesised and characterised. All complexes were characterised on the basis of elemental analyses, IR spectroscopy, UV–VIS–NIR, EPR, as well as thermal analysis and determination of molar conductivity and magnetic moments. The thermal behaviour of complexes was studied using thermogravimetry (TG), differential thermal analysis (DTA) and differential scanning calorimetry (DSC). The structure of L hydrazone was established by X-ray study on single crystal. The ligand works as tridentate NNO, being coordinated through the azomethine nitrogen, the pyridine nitrogen and carbonylic oxygen. Heats of decomposition, ΔH, associated with the exothermal effects were also determined.

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Abstract  

The inorganic ion-exchanger α-zirconium phosphate was synthesized by the sol-gel method and its properties relating to the exchange of Cd2+ and the intercalation of CdS particles were studied. The Cd2+-exchange process is a fast process and the material obtained exhibits an increased interlayer distance d with respect to its precursor (9.56 vs. 7.56 ). The resulting Cd-containing material was exposed to aH2S gas flow to give CdS particles in the exchanger. The zirconium phosphate containing CdS particles still possesses a layered structure, with a pattern almost identical to that of the initial ion-exchanger precursor. Moreover, the material may exchange further Cd2+ and hence lead to a higher CdS particle content. The thermal behavior of this ion-exchangers containing Cd2+ or CdS particles was studied.

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Abstract  

Chromium doped spinels LiCrYMn2−YO4 (0.2≤Y≤0.8) has been synthesized by the sucrose-aided combustion procedure. The thermal behaviour, phase homogeneity and structural characteristics of the samples were studied by thermal analysis, coupled mass spectrometry, and room-and high-temperature X-ray diffraction methods. It was found that the ‘as prepared’ samples contained residual organic impurities undetectable for X-ray diffraction, that burn out completely at 400°C. Samples treated between 400 and 750°C are single phase spinels, whose crystallites size increase from 10 to 50 nm on increasing the temperature. Cr-doping enhances the thermal stability of the spinels, which augments on increasing the Cr content Y. The enhanced thermal stability of the spinels has been accounted for based on the high excess stabilization energy of Cr3+ in octahedral ligand field.

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Abstract  

The binary system Li2CO3–BaCO3 was studied by means of differential thermal analysis (DTA), thermogravimetry (TG) and X-ray phase analysis. The composition of carbonate and CO2 partial pressure influence on the thermal behavior of carbonate were examined. It was shown that lithium carbonate does not form the substitutional solid solution with barium carbonate, however the possible formation of diluted interstitial solid solutions is discussed. Above the melting temperature the mass loss is observed on TG curves. This loss is the result of both decomposition of lithium carbonate and evaporation of lithium in Li2CO3–BaCO3 system. Increase of CO2 concentration in surrounding gas atmosphere leads to slower decomposition of lithium carbonate and to increase the melting point.

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Abstract  

The effect of heating rate on the thermal behavior of ammonium nitrate (AN) and on the kinetic parameters of decomposition of AN and its blends with limestone and dolomite was studied on the basis of commercial fertilizer-grade AN and several Estonian limestone and dolomite samples. Experiments were carried out under dynamic heating conditions up to 900 °C at heating rates of 2, 5, 10 and 20 °C min−1 in a stream of dry air using Setaram Labsys 2000 equipment. For calculation of kinetic parameters, the TG data were processed by differential isoconversional method of Friedman. The variation of the value of activation energy E along the reaction progress α showed a complex character of decomposition of AN—interaction of AN with limestone and dolomite additives with the formation of nitrates as well as decomposition of these nitrates at higher temperatures.

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From the thermal decomposition curves of riboflavin at various heating rates in static air atmosphere, the stages of thermal decomposition of this compound were established. The following kinetic parameters were calculated for the first decomposition stage of this process: activation energy (E a), reaction order (n), preexponential factor (A) and reaction rate constant (k). A mechanism of the changes is proposed.

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Thermal behavior of drugs

Investigation on decomposition kinetic of naproxen and celecoxib

Journal of Thermal Analysis and Calorimetry
Author: M. Sovizi

Abstract  

Data on the thermal stability of drugs was required to obtain information for handling, storage, shelf life and usage. In this study, the thermal stability of two nonsteroidal anti-inflammatory drugs (NSAIDs) was determined by differential scanning calorimetry (DSC) and simultaneous thermogravimetery/differential thermal analysis (TG/DTA) techniques. The results of TG analysis revealed that the main thermal degradation for the naproxen and celecoxib occurs in the temperature ranges of 196–300 and 245–359 °C, respectively. The TG/DTA analysis of compounds indicates that naproxen melts (at about 158.1 °C) before it decomposes. However, the thermal decomposition of the celecoxib started about 185 °C after its melting. The influence of the heating rate (5, 10, 15, and 20 °C min−1) on the DSC behavior of the both drug samples was verified. The results showed that, as the heating rate was increased, decomposition temperatures of the compounds were increased. Also, the kinetic parameters such as activation energy and frequency factor for the compounds were obtained from the DSC data by non-isothermal methods proposed by ASTM E696 and Ozawa. Based on the values of activation energy obtained by various methods, the following order for the thermal stability was noticed: naproxen > celecoxib. Finally, the values of ΔS #, ΔH #, and ΔG # of their decomposition reaction were calculated.

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