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- Author or Editor: A. Souza x
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Abstract
Xerogels were prepared from zirconium, barium, aluminum, lanthanum and lithium acetates, corresponding to a Li containing ZBLA composition. The study of their thermal properties (DSC, TG/DTG, FT-IR) showed that they might be used as chemically stable precursors in the preparation of fluoride glasses. Hydrofluoric acid in solution was chosen as a mild fluorinating agent. This newly proposed technique of fluorinating allowed to obtain high quality ZBLALi glass which presents the advantage of higher thermal stability and homogeneity in comparison with the glass obtained using individual commercial fluorides.
Abstract
Chemical composition of oils and fats used in the biodiesel synthesis can influence in processing and storage conditions, due to the presence of unsaturated fatty acids. An important point is the study of the biodiesel thermal stability to evaluate its quality using thermal analysis methods. In this study the thermal stabilities of the poultry fat and of their ethyl (BEF) and methyl (BMF) biodiesels were determined with the use of thermogravimetry (TG/DTG), differential thermal analysis (DTA) and differential scanning calorimetry (DSC), in different atmospheres. The TG/DTG curves of the poultry fat in synthetic air presented three decomposition steps while only one step was observed in nitrogen (N2) atmosphere. The DSC results indicated four exothermic enthalpic transitions in synthetic air and an endothermic transitions in N2 atmosphere attributed to the combustion process and to the volatilization and/or decomposition of the fatty acids, respectively. For both biodiesels the TG/DTG curves in air indicated two mass loss steps. In the DSC curves four exothermic transitions were observed in synthetic air besides an endothermic one in N2 atmosphere.
Abstract
The vegetal species Pimenta dioica Lindl, popularly known as Jamaican pepper, is a 6–15 m tall tree, which belongs to the Mirtaceae family. Its fruits have an essential oil of great economic value in the international market, due to its high level of eugenol (its major compound), which is largely used in chemical and pharmaceutical industries. In this work, the extraction of the essential oil from the fruits of Pimenta dioica Lindl was carried out by the hydrodistillation method, using a modified Clevenger system. It was observed that the volume of the extracted oil reaches a maximum at 4 h, with a yield of 2.7% (m/m). The essential oil was characterized by physico-chemical analyses, such as density, refraction index, ethanol solubility, color, and appearance, besides UV–vis and infrared spectroscopy and gas chromatography/mass spectrometry. Thus, eugenol was confirmed as the major component of the essential oil of Pimenta dioica Lindl (77%). The technique of differential scanning calorimetry (DSC) was used for the determination of boiling point of the sample of essential oil from the fruits of Pimenta dioica (L.).
Abstract
Poly(3-hydroxybutyrate), PHB has been structurally modified through reaction with maleic anhydride, MA. Transesterification reaction was carried out fixing the PHB and MA and besides time and temperature the concentration of the triethylamine (used as catalyst) was changed. Glass transition, melting and crystallization temperature obtained from DSC curves and thermal degradation temperatures obtained from TG traces were used to evaluate the influence of the reaction conditions on the modification of PHB according to factorial design. On the base of the results the optimum conditions are to perform the PHB modification reaction with MA reaction at 110C for 1 h with 5% v/v triethylamine.
Abstract
Cis-norbixin isomer obtained by hydrolysis of cis-bixin and isolated by solvent extraction from annatto seeds. The thermal decomposition data of the cis-norbixin samples were analyzed by thermogravimetric analysis at different heating rates in the 25–900C temperature range. DSC curves showed that thermal decomposition reactions for cis-norbixin occurred in the solid phase. The kinetic parameters, such as activation energy and pre-exponential factor were determined using integral and approximate methods: Coats–Redfern, Madhusudanan, Horowitz–Metzger and Van Krevelen. F1 mechanism describes well the first stage of the thermal decomposition.
Solid state reactions in the platinum–mercury system
Thermogravimetry and differential scanning calorimetry
Abstract
Thermogravimetry, Differential Scanning Calorimetry and other analytical techniques (Energy Dispersive X-ray Analysis; Scanning Electron Microscopy; Mapping Surface; X-ray Diffraction; Inductively Coupled Plasma Atomic Emission Spectroscopy and Cold Vapor Generation Atomic Absorption Spectroscopy) have been used to study the reaction of mercury with platinum foils. The results suggest that, when heated, the electrodeposited Hg film reacts with Pt to form intermetallic compounds each having a different stability, indicated by at least three mass loss steps. Intermetallic compounds such as PtHg4, PtHg and PtHg2 were characterized by XRD. These intermetallic compounds were the main products formed on the surface of the samples after partial removal of bulk mercury via thermal desorption. The Pt(Hg) solid solution formation caused great surface instability, attributed to the atomic size factor between Hg and Pt, facilitating the acid solution’s attack to the surface.
Abstract
Thermogravimetry (TG), cyclic voltammetry (CV) and other analytical techniques were used to study the reactions of mercury with Pt–30% Ir alloy. The results allowed to suggest that an electrodeposited mercury film interacts with the substrate and when subjected to heat or electrochemical removal at least four mass loss steps or five peaks appeared during the mercury desorption process. The first two steps were attributed to Hg(0) removal probably from the bulk and from the adsorbed monolayer which wets the electrode surface. These two processes are responsible for peaks D and F in the cyclic voltammograms. The last two peaks (G, H) in CV were ascribed to the intermetallic compound decomposition. In TG curves, the last two steps were attributed to the PtHg4 (third step), and PtHg2 decomposition followed by Hg removal from the subsurface. The PtHg2 was formed by an eutectoide reaction: PtHg→PtHg2+Hg(Pt–Ir). The Hg diffused to the subsurface was not detectable by cyclic voltammetry.
Abstract
The degradation kinetics of polycarbonate with flame retardant additive was investigated by means of thermogravimetric analysis. The samples were heated from 30 to 900C in nitrogen atmosphere, with three different heating rates: 5, 10 and 20C min–1. The Vyazovkin model-free kinetics method was applied to calculate the activation energy (E a) of the degradation process as a function of conversion and temperature. The results indicated that the polycarbonate without flame retardant additive starts to loose mass slightly over 380C and the polycarbonate with flame retardant additive, slightly over 390C (with heating rate of 5C min–1). The activation energy for flame retardant polycarbonate and normal polycarbonate were 190 and 165 kJ mol–1, respectively.
Abstract
In this work, the influence of attapulgite concentration on the nucleating efficiency of isotactic polypropylene (iPP) and on the kinetics of non-isothermal crystallization were ascertained.The study was conducted by DSC. The nucleating efficiency was determined according to the procedure described by Fillon and the kinetics of non-isothermal crystallization was determined using Ozawa's method using cooling rates of 2, 5 and 10C min−1.Our results indicate that both the relative crystallinity and the crystallization temperature increase with filler content and that a maximum occurs at 2% mass/mass filler content. Both parameters decrease with increasing cooling rates. The Ozawa's exponent tended to increase with temperature and filler content.
