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Theory of solid-state thermal decomposition reactions

Scientific stagnation or chemical catastrophe? An alternative approach appraised and advocated

Journal of Thermal Analysis and Calorimetry
Author: Andrew K. Galwey

Introduction It should, by now, be obvious to researchers interested in Thermal Decompositions of Solids that the theoretical foundations of this subject are (at best) of doubtful validity or (at worst) nonexistent. The

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Melting and thermal decompositions of solids

An appraisal of mechanistic interpretations of thermal processes in crystals

Journal of Thermal Analysis and Calorimetry
Author: Andrew K. Galwey

. Anal. Cal. , accepted. 5 Galwey , AK Brown , ME et al. 1999 Thermal Decomposition of Ionic Solids Elsevier Amsterdam . 6

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Abstract  

Trifluoromethoxy functionalized copper(II) Schiff base complexes N,N′-bis(5-trifluoromethoxysalicylaldehyde)cyclohexanediiminatodiaquacopper(II) and N,N′-bis(5-trifluoromethoxysalicylaldehyde)phenylenediiminatocopper(II) were synthesized and characterized. Thermal decompositions of the synthesized complexes were studied by thermogravimetry in order to evaluate their thermal stability and thermal decomposition pathways. Three similar decomposition steps occurred for the two copper complexes. Mass losses and evolved gasses were characterized by TG/DTA-MS. Kinetic parameters were calculated and the results showed that the values obtained are comparable.

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decompose, while at higher temperatures, the peroxyester fragments break down [ 5 ]. N 2 is released in the first stage and CO 2 in the second (Scheme 2 ). Scheme 2 Thermal decomposition pathways of azo

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Abstract  

Thermal decomposition of magnesium salts of organic acids used in medicine (Mg acetate, Mg valproate, Mg lactate, Mg citrate, Mg hydrogen aspartate, Zn hydrogen aspartate) was analyzed by thermoanalytical, calorimetrical, and computational methods. Thermoanalytical studies were performed with aid of a derivatograph. 50-, 100-, and 200-mg samples were heated in a static air atmosphere at a heating rate of 3, 5, 10, and 15 °C min−1 up to the final temperature of 700–900 °C. By differential thermal analysis (DTA), thermogravimetry (TG), and derivative thermogravimetry (DTG) methods, it has been established that thermal decomposition of the salts under study occurs via two stages. The first stage (dehydratation) was distinctly marked on the thermoanalytical curves. Calorimetrical studies were carried out by using of a heat-flux Mettler Toledo differential scanning calorimetry (DSC) system. Ten milligram samples of compounds under study were heated in the temperature range from 20 to 400 °C at a heating rate of 10 and 20 °C min−1 under an air stream. The studies showed that the values of transitions heats and enthalpies of dehydration for investigated salts varied with the increasing of heating rate. For chemometric evaluation of thermoanalytical results, the principal component analysis (PCA) was applied. This method revealed that points on PC1 versus PC2 diagrams corresponding to the compounds of similar chemical constitution are localized in the similar ranges of the first two PC’s values. This proves that thermal decomposition reflects similarity in the structure of magnesium salts of organic acids.

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Abstract  

Orthorhombic structural perovskite NdCrO3 nanocrystals with size of 60 nm were prepared by microemulsion method, and characterized by XRD, TEM, HRTEM, SEM, EDS and BET. The catalytic effect of the NdCrO3 for thermal decomposition of ammonium perchlorate (AP) was investigated by DSC and TG-MS. The results revealed that the NdCrO3 nanoparticles had effective catalysis on the thermal decomposition of AP. Adding 2% of NdCrO3 nanoparticles to AP decreased the temperature of thermal decomposition by 87° and increased the heat of decomposition from 590 to 1073 J g−1. Gaseous products of thermal decomposition of AP were NH3, H2O, O2, HCl, N2O, NO, NO2 and Cl2. The mechanism of catalytic action was based on the presence of superoxide ion O2 on the surface of NdCrO3, and the difference of thermal decomposition of AP with 2% of NdCrO3 and pure AP was mainly caused by the different extent of oxidation of ammonium.

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Journal of Thermal Analysis and Calorimetry
Authors: Seied Mahdi Pourmortazavi, Mehdi Rahimi-Nasrabadi, Iraj Kohsari, and Seiedeh Somayyeh Hajimirsadeghi

]. Thermal analysis techniques such as differential scanning calorimetry (DSC) and thermogravimetry-differential thermal analysis (TG/DTA) are powerful systems for acquiring thermal decomposition and kinetic data on energetic materials [ 11 ]. Until

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Abstract  

The ammonium manganese phosphate monohydrate (NH4MnPO4 · H2O) was found to decompose in three steps in the sequence of: deammination, dehydration and polycondensation. At the end of each step, the consecutive one started before the previous step was finished. The thermal final product was found to be Mn2P2O7 according to the characterization by X-ray powder diffraction (XRD) and Fourier transform infrared spectroscopy. Vibrational frequencies of breaking bonds in three stages were estimated from the isokinetic parameters and found to agree with the observed FTIR spectra. The kinetics of thermal decomposition of this compound under non-isothermal conditions was studied by Kissinger method. The calculated activation energies Ea are 110.77, 180.77 and 201.95 kJ mol−1 for the deammination, dehydration and polycondensation steps, respectively. Thermodynamic parameters for this compound were calculated through the kinetic parameters for the first time.

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Abstract  

Thermal decomposition of natural pyrite (cubic, FeS2) has been investigated using X-ray diffraction and57Fe Mössbauer spectroscopy. X-ray diffraction analysis of pyrite ore from different sources showed the presence of associated minerals, such as quartz, szomolnokite, stilbite or stellerite, micas and hematite. Hematite, maghemite and pyrrhotite were detected as thermal decomposition products of natural pyrite. The phase composition of the thermal decomposition products depends on the temperature, time of heating and starting size of pyrite crystals. Hematite is the end product of the thermal decomposition of natural pyrite.

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Thermal decomposition of liebigite

A high resolution thermogravimetric and hot-stage Raman spectroscopic study

Journal of Thermal Analysis and Calorimetry
Authors: R. L. Frost, M. L. Weier, and W. Martens

A combination of high resolution thermogravimetric analysis coupled to a gas evolution mass spectrometer has been used to study the thermal decomposition of liebigite. Water is lost in two steps at 44 and 302°C. Two mass loss steps are observed for carbon dioxide evolution at 456 and 686°C. The product of the thermal decomposition was found to be a mixture of CaUO4 and Ca3UO6. The thermal decomposition of liebigite was followed by hot-stage Raman spectroscopy. Two Raman bands are observed in the 50°C spectrum at 3504 and 3318 cm-1 and shift to higher wavenumbers upon thermal treatment; no intensity remains in the bands above 300°C. Three bands assigned to the υ 1 symmetric stretching modes of the (CO3)2- units are observed at 1094, 1087 and 1075 cm-1 in agreement with three structurally distinct (CO3)2- units. At 100°C, two bands are found at 1089 and 1078 cm-1. Thermogravimetric analysis is undertaken as dynamic experiment with a constant heating rate whereas the hot-stage Raman spectroscopic experiment occurs as a staged experiment. Hot stage Raman spectroscopy supports the changes in molecular structure of liebigite during the proposed stages of thermal decomposition as observed in the TG-MS experiment.

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