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Summary By applying an advanced isoconversional method to DSC data one can evaluate a dependence of the effective activation energy (the temperature coefficient of the growth rate) on the relative extent of melt crystallization. The conversion dependence can further be converted into a temperature dependence and parameterized in terms of the Hoffman-Lauritzen equation. For poly(ethylene terephthalate) (PET) we observe a transition from regime I to II. Poly(ethylene oxide) (PEO) crystallization appears to begin in regime II and then undergoes 2 consecutive changes that however cannot be clearly interpreted as regime III. The K g and sse parameters obtained for regime I and II (PET) and regime II (PEO) are consistent with the respective parameters reported for isothermal crystallization.

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Abstract  

The kinetics of the thermal decomposition of ammonium perchlorate at temperatures between 215 and 260°C is studied, in this work, by measuring the sample mass loss as a function of time applying the isothermal thermogravimetric method. From the maximum decomposition rate – temperature dependence two different decomposition stages, corresponding to two different structural phases of ammonium perchlorate, are identified. For the first region (215–235°C), corresponding to the orthorhombic phase, the mean value of the activation energy of 146.3 kJ mol–1, and the pre-exponential factor of 3.43⋅1014 min–1 are obtained, whereas for the second region (240–260°C), corresponding to the cubic phase, the mean value of the activation energy of153.3 kJ mol–1, and the pre-exponential factor of 4.11⋅1014 min–1 are obtained.

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The thermal degradation and thermal stability of rice husk flour (RHF) filled polypropylene (PP) and high-density polyethylene (HDPE) composites in a nitrogen atmosphere were studied using thermogravimetric analysis. The thermal stability of pure PP and HDPE was found to be higher than that of wood flour (WF) and RHF. As the content of RHF increased, the thermal stability of the composites decreased and the ash content increased. The activation energy of the RHF filled PP composites increased slowly in the initial stage until α=0.3 (30% of thermal degradation region) and thereafter remained almost constant, whereas that of the RHF filled HDPE composites decreased at between 30 and 40 mass% of RHF content. The activation energy of the composites was found to depend on the dispersion and interfacial adhesion of RHF in the PP and HDPE matrix polymers.

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Abstract  

The thermal decomposition of salbutamol (β2 — selective adrenoreceptor) was studied using differential scanning calorimetry (DSC) and thermogravimetry/derivative thermogravimetry (TG/DTG). It was observed that the commercial sample showed a different thermal profile than the standard sample caused by the presence of excipients. These compounds increase the thermal stability of the drug. Moreover, higher activation energy was calculated for the pharmaceutical sample, which was estimated by isothermal and non-isothermal methods for the first stage of the thermal decomposition process. For isothermal experiments the average values were E act=130 kJ mol−1 (for standard sample) and E act=252 kJ mol−1 (for pharmaceutical sample) in a dynamic nitrogen atmosphere (50 mL min−1). For non-isothermal method, activation energy was obtained from the plot of log heating rates vs. 1/T in dynamic air atmosphere (50 mL min−1). The calculated values were E act=134 kJ mol−1 (for standard sample) and E act=139 kJ mol−1 (for pharmaceutical sample).

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The thermal properties of four heteropoly complexes α-K3H3[SiW11Ni(H2O)O39]·11.5H2O (I), α-K3H2[SiW11Fe(H2O)O39]·9H2O (II), α-[(C4H9)4N]3.5H1.5[SiW11Fe(H2O)O39]·4.5H2O (III) and α-[(C4H9)4N]3.5H2.5[SiW11Cu(H2O)O39]·6H2O (IV) were studied by means of TG, DTA and DSC. The activation energy and reaction order of the thermal decomposition reaction of these complexes have been calculated.

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Abstract  

A theoretical approach has been used to show that, except for certain types of reaction mechanism, the ease with which it is possible to distinguish the form of the reaction mechanism by the reduced-time plot method depends particularly on the rate of transfer of heat into the sample. The original reduced-time plots [1] were calculated from model equatioons which assume that the sample is, from the outset, at a fixed temperature and remains under isothermal conditions throughout the reaction. The variations produced in the appearance of reduced-time plots when the sample is programmed to rise to a given fixed temperature through various temperature schedules have been investigated. It is shown that even relatively rapid temperature rises can produce distortion of the reduced-time plots for various reaction equations. If the reaction mechanism is known, however, fairly accurate values of the activation energy for the reaction can be determined, even when the furnace used has relatively poor heat-transfer characteristics.

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Thermal analysis increasingly being used to obtain kinetic data relating to sample decomposition. This work involves a comparative study of several methods used to analyse DSC and TG/DTG data obtained on the oxidation of Beypazari lignite. A general computer program was developed and the methods are compared with regard to their accuracy and the ease of interpretation of the kinetics of thermal decomposition. For this study, the ratio method was regarded as the preferred method, because it permits the estimation of reaction order, activation energy and Arrhenius constant simultaneously from a single experiment.

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Abstract  

This research was aimed to investigate the combustion and kinetics of oil shale samples (Mengen and Himmetoğlu) by differential scanning calorimetry (DSC). Experiments were performed in air atmosphere up to 600�C at five different heating rates. The DSC curves clearly demonstrate distinct reaction regions in the oil shale samples studied. Reaction intervals, peak and burn-out temperatures of the oil shale samples are also determined. Arrhenius kinetic method was used to analyze the DSC data and it was observed that the activation energies of the samples are varied in the range of 22.4–127.3 kJ mol−1 depending on the oil shale type and heating rate.

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The thermal behavior of four unusual lignocellulose fibers — namely Caroa, Curaua, Piassava and Sponge gourd — is described. Caroa and Curaua fibers showed a more homogeneous thermal degradation, with a single peak dominating in the DTG curve. Piassava and Sponge gourd showed two separated peaks, revealing the more pronounced amounts of hemicellulose present at these fibers. All four fibers are, however, thermally stable up to temperatures of around 200°C. The activation energies for the thermal degradation of the fibers were similar, except for the Caroa fiber. The lower activation energy associated to this fiber was attributed to its higher hemicellulose to cellulose ratio.

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Journal of Thermal Analysis and Calorimetry
Authors: Jinn-Shing Lee, Chung-King Hsu, Li-Kuo Lin, Chih-Long Chang, Shich Borjinn, and Chin-Wang Huang

Abstract  

Vitreous solder glasses, such as Mansol #40 and FEG-2002, are commercialized solder glasses, which are compression sealing glasses that can be used to solder materials with expansions between 55-68⊙10-7C-1, such as Al2O3. In order to understand and tailor the thermal behaviour of solder glasses, cylindrical-like glasses were first carefully ground with a stainless steel mortar and pestle. Initially, no exothermic or endothermic data were obtained from the DTA/DSC curves except those relating to melting. However, exothermic peaks appeared after the glass samples were re-melted. In this work, kinetic parameters such as the activation energy, and the morphology of the devitrification mechanisms for two kinds of solder glasses were also investigated, using non-isothermal DTA techniques. The activation energies ranged from 220 to 235 kJ mol-1 and the devitrification mechanism parameters were close to 1. This indicates that the devitrification mechanisms of the two kinds of solder glasses involve surface nuclei.

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