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Journal of Thermal Analysis and Calorimetry
Authors: J. Santos, M. Conceiçăo, M. Trindade, A. Araújo, V. Fernandes, and A. Souza

Abstract  

The lanthanidic complexes of general formula Ln(C11H19O2)3 were synthesized and characterized by elementary analysis, infrared absorption espectroscopy, thermogravimetry (TG) and differential scanning calorimetry (DSC). The reaction of thermal decomposition of complexes has been studied by non-isothermal and isothermal TG. The thermal decomposition reaction of complexes began in the solid phase for Tb(thd)3, Tm(thd)3 and Yb(thd)3 and in the liquid phase for Er(thd)3 and Lu(thd)3, as it was observed by TG/DTG/DSC superimposed curves. The kinetic model that best adjusted the experimental isothermal thermogravimetric data was the R1 model. Through the Ozawa method it was possible to find coherent results in the kinetic parameters and according to the activation energy the following stability order was obtained: Tb(thd)3>Lu(thd)3>Yb(thd)3>Tm(thd)3>Er(thd)3

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Abstract  

Curves obtained by controlled rate TG of polyimide film in air are quite different from those obtained by conventional constant rate heating TG. A two step mass loss was observed during the constant rate heating TG, while mass loss proceeded as a single step process in the controlled rate TG. To elucidate the cause for this difference, kinetic analysis was made, and it was found that the reaction mechanism in a lower temperature range is different from those in a higher temperature range. The lower temperature decomposition is a single step process, and the higher temperature decomposition is a two-step process. The reason for the difference is that only the low temperature single step process is observed in the controlled rate TG, while both reactions are observed in the constant heating rate TG along with the temperature increase. This speculation was confirmed by isothermal TG. These facts show us another usefulness of controlled rate TG. To analyze the three types of TG data together, the Friedman—Ozawa method was used, and it is demonstrated to be the most appropriate and reliable.

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a single process separately with the others, so that we can also analyzed equivalent isothermal curves similarly. References 1. Ozawa , T Non-stoichiometry of YBa

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Journal of Thermal Analysis and Calorimetry
Authors: Marta Conceição, V. Fernandes Jr, A. Bezerra, M. Silva, Iêda Santos, F. Silva, and A. Souza

Abstract  

Diesel oil has an important role in the field of urban traffic as well as in the transportation of products. However, the amount of the non-renewable sources is continuously decreasing. This fact and the environmental requirements brought the necessity to search for other, renewable sources. This paper aimed the dynamic kinetic calculation of thermal decomposition of castor oil, methanol biodiesel and ethanol biodiesel using Coats–Redfern, Madhusudanan and Ozawa methods. On the base of the thermogravimetric curves the following thermal stability order could be established: castor oil>ethanol biodiesel>methanol biodiesel. Kinetic data presented coherent results. Methanol biodiesel presented lower activation energy than ethanol biodiesel, suggesting that methanol biodiesel has a better quality for combustion.

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Abstract  

The crystallisation behaviour of in situ polymerised cyclic butylene terephthalates (pCBT) and poly(butylene terephthalate)s (PBT) were studied by differential scanning calorimetry (DSC) both under isothermal and non-isothermal conditions. The crystallisation was analysed by adopting the Avrami, Ozawa and Kissinger methods for the isothermal and non-isothermal crystallisations, respectively. An Avrami exponent n between 2 and 3 was found for the pCBTs whereas the exponent ranged between 3 and 4 for the PBTs. The Ozawa exponent m varied for all materials between 2 and 3. Differences in the crystallisation kinetics were also reflected in the related activation energy data.

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Abstract  

Data on the thermal stability of organic materials such as diaminofurazan (DAF) and diaminoglyoxime (DAG) was required in order to obtain safety information for handling, storage and use. These compounds have been shown to be a useful intermediate for the preparation of energetic compounds. In the present study, the thermal stability of the DAF and DAG was determined by differential scanning calorimetery (DSC) and simultaneous thermogravimetery-differential thermal analysis (TG-DTA) techniques. The results of TG analysis revealed that the main thermal degradation for the DAF and DAG occurs in the temperature ranges of 230–275°C and 180–230°C, respectively. On the other hand, the TG-DTA analysis of compounds indicates that DAF melts (at about 182°C) before it decomposes. However, the thermal decomposition of the DAG started simultaneously with its melting. The influence of the heating rate (5, 10, 15 and 20°C min−1) on the DSC behaviour of the compounds 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 E698 and Ozawa. Based on the values of activation energy obtained by ASTM and Ozawa methods, the following order in the thermal stability was noticed: DAF>DAG.

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Abstract  

In this paper, the thermal behaviours of N-{bis[benzyl(methyl) amino]phosphoryl}-2,2-dichloroacetamide (BMA) and N-{bis[dibenzylamino]phosphoryl}-2,2-dichloroacetamide (DBA) were studied by thermogravimetery (TG) and differential scanning calorimetery (DSC) techniques under the non-isothermal conditions. The results showed that BMA melts about 120 °C before it decomposes. BMA decomposition occurs in three continuous steps, in the 170–400 °C temperature range. Each thermal degradation stage for BMA results an exothermic peak in the DSC curve. On the other hand, applying TG-DSC techniques indicates that DBA melts about 175 °C before it decomposes. This compound decomposes in the temperature range of 200–600 °C in three steps. Activation energy and pre-exponential factor for each compound were found by means of Kissinger method and were verified by Ozawa–Flynn–Wall method. Activation energy obtained by Kissinger method for the first stage of BMA and DBA decompositions are 151.8 (±2.0) KJ mol−1 and 138.7 (±2.6) KJ mol−1, respectively. Finally, the thermodynamic parameters (ΔG #, ΔH # and ΔS #) for first step decomposition of DBA and BMA were determined.

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Summary  

Isothermal and non-isothermal kinetics of three dimensional growth processes from nuclei pre-existing on surface of infinite plate specimen have been derived. Some useful and interesting relations have been found, and methods for kinetic analysis of experimental data are proposed.

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