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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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Thermal and kinetic study of statins

Simvastatin and lovastatin

Journal of Thermal Analysis and Calorimetry
Authors: M. Souza, Marta Conceição, M. Silva, L. Soledade, and A. Souza

Abstract  

Statins are a group of lipoproteins that are used in medicine to treat the high cholesterol level. The effectiveness of statins in reducing the cholesterol level is significant and in long time scale the reduction of the cholesterol level helps to avoid the incidence of degenerative diseases. Simvastatin and lovastatin are belonging to the ‘statins’ family, one of the pharmacologic groups used in the control of dislipidemy. The objective of this work is the thermal stability and kinetic study of the active forms of simvastatin and lovastatin. Thermal data indicated that lovastatin and simvastatin are stable up to 190 and 170°C in air and up to 205 and 203°C in nitrogen, respectively. For melting temperatures DSC curves showed good correlation with the literature data. Comparing the activation energies of the statins at heating rate of 10°C min–1, lovastatin is more stable than simvastatin under the applied experimental conditions.

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Abstract  

The thermal behaviour of chitosan was studied by means of thermogravimetry, mass spectrometry and infrared spectrometry. Kinetic parameters were obtained by advanced kinetic evaluation (differential isoconversional analysis) from DSC curves, in non-isothermal conditions, at several heating rates, between 5 and 30°C min−1. The results showed that the decomposition of chitosan does not follow a single mechanism because both the activation energy and the pre-exponential factor are not constant during the course of the reaction. A comparison with the results obtained by applying different conventional calculating methods is also shown.

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

Abstract  

Thermoanalytical, kinetic and rheological parameters of commercial edible oils were evaluated. The thermal decomposition of the oils occurred in three steps, due to polyunsaturated, monounsaturated and saturated fatty acids decomposition, respectively. According to the temperature of the beginning of the decomposition, the following stability order was observed: corn (A)>corn>sunflower (A)>rice>soybean>rapeseed (A)>olive>rapeseed>sunflower (A - artificial antioxidants). Kinetic parameters were obtained using Coats-Redfern and Madhusudanan methods and presented good correlation. According to the activation energy of the first thermal decomposition event, obtained of Coats-Redfern' method, the following stability order is proposed: sunflower>corn>rice>soybean>rapeseed>olive. In relation to rheological properties, a Newtonian behavior was observed and no degradation occurred in the temperature range studied.

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Abstract  

The kinetic and thermodynamic study of synthetic lubricant oils was accomplished in this work, using isothermal and non-isothermal thermogravimetry based on mass loss as a function of time and temperature. The thermodynamic and kinetic behavior of the synthetic lubricant oils depends on atmosphere and heating rates used in TG analysis. The kinetic and thermodynamic results were satisfactory, presenting good correlation.

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Abstract  

The world production of tyre waste amounts to 5106 ton year–1, 2106 tons of which are produced in Europe, but the final destination of nearly 65–70% of them is the landfill, despite the high added value materials lost and the consequent environmental impact. Treatments alternative to landfilling take into account reconstruction and reuse of the tyres or the matter and/or energy recovery by means of thermal treatment processes (incineration, gasification and pyrolysis). Among these, pyrolysis seems to be a promising and realistic alternative to attain the conversion of tyre waste into valuable and reusable products. Present work relates to experimental tests and results obtained for the study of tyre waste pyrolysis, conducted by means of thermo-gravimetric analysis (TG) of the material and the simultaneous determination, through Fourier transform infrared (FTIR) and mass spectrometry (MS), of the decomposition products. The analysis of the volatile fraction allows to isolate, within the thermograms, the evolution of products referable to specific tyre components and therefore it suggests the application of a multi-component decomposition model. The kinetic model consequently developed agrees fairly well with the experimental data.

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Nitration of acetyl guaiacol, one typical aromatic nitration, is highly exothermic and extremely fast. Better control and high efficiency can be achieved in the microreactor due to its enhanced mixing and heat transfer rates. In this study, nitration of acetyl guaiacol was carried out in a microreactor using nitric acid—acetic acid as nitrating agent. The nitration kinetics was first investigated, and a kinetic model was established and revealed good prediction of experimental results at higher temperatures. Effects of molar ratio of nitric acid—acetyl guaiacol, residence time, temperature, and nitric acid concentration on the reaction were studied in detail. Under optimized condition, 90.7% yield of desired product, 5-nitroguaiacol, was achieved with 40% of nitric acid concentration, nitric acid—acetyl guaiacol molar ratio of 2.6, reaction temperature of 120 °C, and residence time of 2 min. Compared to traditional batch reactor, microreactor showed the advantages of higher yield and selectivity, much shorter reaction time, and less use of nitric acid.

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Summary  

The effect of the concentration of benzyl dimethyl amine as a catalyst on the cure reaction of bisphenol-F based epoxy resin(BPF)/nadic methyl ahydride(NMA) system was studied by differential scanning calorimetery using an isothermal approach over the temperature range 115-145C. Kinetic parameters of the curing reaction including the reaction order, activation energy and kinetic rate constants were investigated. The results were dependent on the cure temperature and catalyst concentration and proceeded through an autocatalytic kinetic mechanism. The curing kinetic constants and the cure activation energies were obtained by the Arrhenius kinetic model. The suggested kinetic model with a diffusion term was successfully used to describe and predict the cure kinetic of BPF resin compositions as a function of the catalyst content and temperature.

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Abstract  

The kinetic characteristic of thermal decomposition of the Emulsion Explosive Base Containing Fe and Mn elements (EEBCFM) which was used to prepare nano-MnFe2O4 particles via detonation method was investigated by means of non-isothermal DSC and TG methods at various heating rates of 2.5, 5 and 7.5°C min−1respectively under the atmosphere of dynamic air from room temperature to 400°C. The results indicated that the EEBCFM was sensitive to temperature, especially to heating rate and could decompose at the temperature up to 60°C. The maximum speed of decomposition (dα/dT)m at the heating rate of 5 and 7.5°C min−1 was more than 10 times of that at 2.5°C min−1 and nearly 10 times of that of the second-category coal mine permitted commercial emulsion explosive (SCPCEE). The plenty of metal ions could seriously reduce the thermal stability of emulsion explosive, and the decomposition reaction in the conversion degree range of 0.0∼0.6 was most probably controlled by nucleation and growth mechanism and the mechanism function could be described with Avrami-Erofeev equation with n=2. When the fractional extent of reaction α>0.6, the combustion of oil phase primarily controlled the decomposition reaction.

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