The study of mica–epoxy-based composite has a great role in high voltage machines industry. Beside electric properties, this composite should present compatible mechanical and chemical, in this case thermal characteristics to insulate properly the conductor strand, avoiding short-circuits, and leading electrical current with minimal losses. Improvement of the quality is possible through the knowledge of raw materials and system. This study aims to list a complete thermal characterization of mica composite, its components, epoxy resin, anhydride methylhexahydrophtalic, mica tape and zinc naphthenate, and thermoanalytical interactions between them. These data shows intrinsic properties of the system, which is so relevant to its great electrical and thermal performance. Thermal analysis allows the detailed study of curing process and thermal decomposition, predicting and suggesting mechanisms, beside future and possible optimization to the system. Composite system glass transition (Tg) was obtained through an important and very respected methodology, presenting the value of Tg = 138 ± 2 °C, finally characterizing the material.
Authors:Tamy Koreeda, Jivaldo Matos, and Camila S. Gonçalves
Cure kinetics study of epoxy resin composite, employed as stator bars insulation system, was evaluated through differential scanning calorimetry using the dynamic methodology, different heating rates. These experiments provided some important information about the system as activation energy (Ea = 65.4 kJ mol−1), glass transition (Tg) values on different curing stages including the final cured material information and, besides that, it enables the comparison of these data with new materials under development. The activation energy value allows the determination of different energy needs of the system under evaluation, specially temperature for the material cure, improving the possibility of comparison between different insulation systems in use in the high voltage insulation business. The composite conversion degree based on the cure enthalpy (ΔHcure) at different time of cure was also subject of analysis and from that it was possible to comprehend the cure pattern which allows the cure state prediction of further samples of this type of material and the more accurate evaluation of similar samples acquired directly from stator bars.
Authors:Hélio Salvio Neto and Jivaldo do Rosário Matos
In this work, TG/DTG and DSC techniques were used to the determination of thermal behavior of prednicarbate alone and associated with glyceryl stearate excipient (1:1 physical mixture). TG/DTG curves obtained for the binary mixture showed a reduction of approximately 37 °C to the thermal stability of drug (
). The disappearance of stretching band at 1280 cm−1 (νas C–O, carbonate group) and the presence of streching band with less intensity at 1750 cm−1 (νs C–O, ester group) in IR spectrum obtained to the binary mixture submitted at 220 °C, when compared with IR spectrum of drug submitted to the same temperature, confirmed the chemical interaction between these substances due to heating. Kinetics parameters of decomposition reaction of prednicarbate were obtained using isothermal (Arrhenius equation) and non-isothermal (Ozawa) methods. The reduction of approximately 45% of activation energy value (Ea) to the first step of thermal decomposition reaction of drug in the 1:1 (mass/mass) physical mixture was observed by both kinetics methods.
Authors:Elaine Moreschi, Jivaldo Matos, and Ligia Almeida-Muradian
Vitamin PP includes two vitamers, niacin and niacinamide which are essential for energy production. Vitamins are sensitive
and losses can occur during shelf life and heating processes. Thermal analysis can provide information about thermal behavior
of each vitamer relating them with time and/or temperature exposure. The vitamers thermal behavior were studied by TG/DTG
and DSC under air and nitrogen atmosphere and the results showed that niacin is more stable than the niacinamide and the decomposition
happens by volatilization at 238 °C while niacinamide melts at 129 °C and volatilize at 254 °C when there is the total mass
loss in the TG/DTG curves.
Authors:Caroline Miyazaki, Igor Medeiros, Jivaldo Matos, and Leonardo Rodrigues Filho
Dental composites can be improved by heat treatment, as a possible way to increase mechanical properties due to additional
cure (post-cure). Direct dental composites are essentially similar to the indirect ones, supposing they have the same indication.
Therefore, to establish a heat treatment protocol for direct composites, using as indirect (photoactivated by continuous and
pulse-delay techniques), a characterization (TG/DTG and DSC) is necessary to determine parameters, such as mass loss by thermal
decomposition, heat of reaction and glass transition temperature (Tg). By the results of this study, a heat treatment could be carried out above 160 °C (above Tg, and even higher than the endset exothermic event) and under 180 °C (temperature of significant initial mass loss).
Authors:Hélio Salvio Neto, Fábio Barros, Flávio de Sousa Carvalho, and Jivaldo Matos
In the present work, the thermal behavior of prednicarbate was studied using DSC and TG/DTG. The solid product remaining at
the first decomposition step of the drug was isolated by TG, in air and N2 atmospheres and was characterized using LC-MS/MS, NMR, and IR spectroscopy. It was found that the product at the first thermal
decomposition step of prednicarbate corresponds to the elimination of the carbonate group bonding to C17, and a consequent formation of double bond between C17 and C16. Structure elucidation of this degradation product by spectral data has been discussed in detail.
Authors:Rosely dos Reis Orsini, Elder Moscardini Filho, Lucildes Pita Mercuri, Jivaldo do Rosário Matos, and Fátima Maria Sequeira de Carvalho
The better use of agricultural residues is expected, when they are mostly disposed of improperly and it is often burned in the natural environment. This study of the thermal decomposition of residues was performed from the coffee crop for energy purposes and in this case was used thermal analysis techniques for such assessment. The TG/DTG and DSC curves showed that the thermal decomposition occurs in four consecutive events and it is predominantly exothermic. The first mass loss evidenced in TG/DTG curves has an endothermic peak in DSC curve, which it can be associated with the water liberation of the material. This first thermal event also can be related to the liberation of volatile compounds present in the sample, which is also corroborated by the endothermic peak. The other events of mass loss are related with the thermal decomposition of the material. This decomposition has an exothermic behavior, which is positively applied to the main aim of this scientific research: the coffee straw use like biomass energy font. The thermoanalytical techniques were satisfactory in the characterization of this material.
Authors:Gabriel de Araujo, Dalva de Faria, Márcio Zaim, Flávio de Souza Carvalho, Fabio de Andrade, and Jivaldo Matos
Tibolone polymorphic forms I (monoclinic) and II (triclinic) have been prepared by recrystallization from acetone and toluene,
respectively, and characterized by different techniques sensitive to changes in solid state, such as polarized light microscopy,
X-ray powder diffractometry, thermal analysis (TG/DTG/DSC), and vibrational spectroscopy (FTIR and Raman microscopy). The
nonisothermal decomposition kinetics of the obtained polymorphs were studied using thermogravimetry. The activation energies
were calculated through the Ozawa’s method for the first step of decomposition, the triclinic form showed a lower Ea (91 kJ mol−1) than the monoclinic one (95 kJ mol−1). Furthermore, Raman microscopy and DSC at low heating rates were used to identify and follow the thermal decomposition of
the triclinic form, showing the existence of three thermal events before the first mass loss.