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Abstract  

The thermal degradation process of mineral base lubricating oils was studied in this work by means of thermal, spectroscopic and rheologic analysis. The lubricating oils were degraded at temperatures varying from 150 to 210C, and for degradation times from 1 to 48 h. After the degradation, the lubricating oils were characterized by X-ray fluorescence, IR and NMR spectroscopies, rheological properties and thermal analyses (TG/DSC). The spectroscopic analyses determined the oxidation reaction products. TG curves indicate that the thermal stability of lubricating oils is below 161C. TG curves in air present three mass loss stages, whereas in nitrogen there are only two mass loss steps. DSC analyses in air indicate two highly exothermic peaks related to hydrocarbon oxidation and combustion processes, while in nitrogen only two endothermic peaks were observed. The decrease in the degradation temperature led to a decrease of the lubricant viscosity.

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Journal of Thermal Analysis and Calorimetry
Authors: Nataly Santos, Marileide Tavares, R. Rosenhaim, F. Silva, V. Fernandes Jr, Iêda Santos, and A. Souza

Abstract  

The growing petroleum deficit requires the development of alternative fuel sources. Biodiesel is a good alternative, as it is a biodegradable and renewable product, which obeys the carbon cycle. In this work, the biodiesel from babassu was synthesized using the methanol route, and characterized by physico-chemical analyses in order to make able the investigated biodiesel to fulfill with its properties the requirements of Brazilian National Agency for Petroleum, Natural Gas and Biofuel (ANP). Besides gas chromatography, IR spectroscopy experiments and thermoanalytical measurements in air and in nitrogen were done to determine the main thermal decomposition processes and calorimetric events. The evaporation temperature of babassu biodiesel was similar in both atmospheres, started around 52 in air and around 60C in nitrogen.

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Abstract  

SnO2-based materials are used as sensors, catalysts and in electro–optical devices. This work aims to synthesize and characterize the SnO2/Sb2O3-based inorganic pigments, obtained by the polymeric precursor method, also known as Pechini method (based on the metallic citrate polymerization by means of ethylene glycol). The precursors were characterized by thermogravimetry (TG) and differential thermal analysis (DTA). After characterization, the precursors were heat-treated at different temperatures and characterized by X-ray diffraction. According to the TG/DTA curves basically two-step mass loss process was observed: the first one is related to the dehydration of the system; and the second one is representative to the combustion of the organic matter. Increase of the heat treatment temperature from 500 to 600C and 700C resulted higher crystallinity of the formed product.

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Journal of Thermal Analysis and Calorimetry
Authors: M. Dantas, Marta Conceição, V. Fernandes Jr, Nataly Santos, R. Rosenhaim, Aldalea Marques, Iêda Santos, and A. Souza

Abstract  

This work evaluates the thermal and kinetic behaviour of corn biodiesel obtained by the methanol and ethanol routes. As to the TG curves, in air three thermal decomposition steps are for the methanol biodiesel and two steps are for the ethanol biodiesel. These steps are related to the evaporization and/or combustion of the methyl and ethyl esters, respectively. The corn oil presented four thermal decomposition steps in air, and only one step in nitrogen. These steps were attributed to the evaporization and/or decomposition of triglycerides. The TG and DTA profiles of the biodiesel approach the mineral diesel oil ones.

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Journal of Thermal Analysis and Calorimetry
Authors: Márcia Silva, Mary Alves, S. Lima, L. Soledade, Elaine Paris, E. Longo, A. Souza, and Iêda Santos

Abstract  

Sr(Ti,Nd)O3 was synthesized in order to evaluate the influence of the amount of neodymium on the thermal and structural properties of SrTiO3. The synthesis was carried out using the polymeric precursor method. A small mass gain was observed for the SrTiO3 and SrTi0.98Nd0.02O3 samples accompanied by an exothermic peak in the DTA curves. Other steps at higher temperatures are assigned to the combustion of the organic material and carbonate. Elimination of defects by previous calcination of the precursors is responsible by the short and long range ordering of the perovskite. Cubic phase was obtained for undoped and doped SrTiO3.

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Journal of Thermal Analysis and Calorimetry
Authors: Marta Conceição, Manoel Dantas, Raul Rosenhaim, Valter Fernandes, Ieda Santos, and Antonio Souza

Abstract  

Oxidative stability is very important in the quality control of oils and biodiesel. Chemical characteristics, as acid, iodine and peroxide values, show the differences among samples and can be used by industries to evaluate the oxidation degree. In relation to advanced techniques, the use of PDSC to measure the oxidative induction time is very important. These measurements were used to evaluate the properties of castor oil after refining process and consequently the biodiesel characteristics. Oxidative induction time indicated that biodiesel samples were more stable than the refined oils. The biodiesel obtained from neutralized oil had a higher stability being probably related to the acid value.

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Journal of Thermal Analysis and Calorimetry
Authors: R. Candeia, J. Freitas, M. Souza, Marta Conceição, Iêda Santos, L. Soledade, and A. Souza

Abstract  

The most feasible alternative among fuels derived from biomass seems to be the biodiesel, having the required characteristics for a total or partial substitution of diesel oil. Therefore, the aim of this work is to evaluate the thermal and rheological behavior of the blends of diesel with the methanol biodiesel obtained from soybean oil, using B5, B15 and B25 blends. All thermogravimetric curves exhibited one overlapping mass loss step in the 35–280C temperature range at air atmosphere and one step between 37–265C in nitrogen. The rheological study showed a Newtonian behavior (n=1) for all blends.

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Abstract  

The present work investigates the influence of milling and calcination atmosphere on the thermal decomposition of SrTiO3 powder precursors. Both pure and neodymium-modified SrTiO3 samples were studied. Milling did not significantly influence numerical mass loss value, but reduced the number of decomposition steps, modifying the profiles of the TG and DTA curves. On the other hand, milling increases the amount of energy liberated by the system upon combustion of organic matter. It was also observed that the milling process, associated to the calcination in an oxygen atmosphere, considerably decreases the amount of organic matter and increases the final mass loss temperature.

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Abstract  

CaSnO3 was synthesized by the polymeric precursor method, using different precursor salts as (CH3COO)2CaH2O, Ca(NO3)24H2O, CaCl22H2O and CaCO3, leading to different results. Powder precursor was characterized using thermal analysis. Depending on the precursor different thermal behaviors were obtained. Results also indicate the formation of carbonates, confirmed by IR spectra. After calcination and characterization by XRD, the formation of perovskite as single phase was only identified when calcium acetate was used as precursor. For other precursors, tin oxide was observed as secondary phase.

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Journal of Thermal Analysis and Calorimetry
Authors: Érika Marinho, A. Souza, Danniely de Melo, Iêda Santos, Dulce Melo, and Walquíria da Silva

Abstract  

Because of their electrical, magnetic and catalytic properties rare earth and transition metal mixed oxides are important compounds. Lanthanum chromites have been extensively used as solid oxide fuel cell (SOFC) interconnect materials. In this work, lanthanum chromites partially substituted by alkaline earth metals were synthesized by the urea combustion process. TG and DSC techniques were used to evaluate the presence of the organic material in the powder after reaction on the hot plate. The powders were calcinated at 900C and characterized by XRD and SEM. The results show that the particles have nanometric dimensions and the perovskite structure was formed.

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