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Abstract  

The k 0 parametric neutron activation analysis has been applied since 1995 in the Radiochemical Sector/CDTN, Belo Horizonte, Brazil. Several certified reference materials were studied with the aim of analysing biological samples. This work is related to an IAEA co-ordinated research project whose goal is to make a survey of the exposures to metals related to occupational diseases. It has been conducted by CDTN and government departments of health. The hair samples as bioindicators were donated by galvanising factory workers in Belo Horizonte. This city and surrounding area are important industrial centres and that industry is responsible for the majority of patients who look for medical assistance because of metal contamination. The Al, Co, Cu, Cr, La, Mn, Sb and V concentrations determined in the workers' samples suggest endogenous contamination.

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Biodiesels from beef tallow/soybean oil/babassu oil blends

Correlation between fluid dynamic properties and TMDSC data

Journal of Thermal Analysis and Calorimetry
Authors: G. A. A. Teixeira, A. S. Maia, I. M. G. Santos, A. L. Souza, A. G. Souza, and N. Queiroz

Abstract

Cloud point (CP), cold filter plugging point (CFPP), and pour point (PP) of biodiesel samples obtained from blends containing different amounts of beef tallow, babassu oil, and soybean oil were investigated by the corresponding conventional techniques and by temperature modulated differential scanning calorimetry (TMDSC). The CP and CFPP values correlate well with the crystallization temperature (T onset) obtained from the TMDSC curves, being the highest for the biodiesel sample containing the highest amount of methyl stearate. A correspondence between PP and the peak temperature was also noticed, pointing out that pouring ceases after the crystallization of the heavier fatty acid ester. Among the samples of biodiesel, Bio-3 (highest amount of babassu oil) and Bio-4 (highest amount of soybean oil) showed better cold-flow properties, or in other words, lower values of CP, CFPP, and PP. Independently of the composition, the cold-flow properties of all biodiesel samples meet the requirements from the Brazilian National Agency of Petroleum, Natural Gas, and Biofuels (ANP).

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Journal of Thermal Analysis and Calorimetry
Authors: E. F. S. M. Ramalho, I. M. G. Santos, A. S. Maia, A. L. Souza, and A. G. Souza

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.

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Journal of Thermal Analysis and Calorimetry
Authors: E. F. S. M. Ramalho, A. R. Albuquerque, A. L. Souza, A. K. Barro, A. S. Maia, I. M. G. Santos, and A. G. Souza

Abstract

The poultry fat methylic (BMF) and ethylic (BEF) biodiesels were synthesized through transesterification by homogeneous basic catalysis. The chromatographic analyses showed the palmitic, stearic, oleic, and linoleic esters as majority components. Owing to its considerable amount of polyunsaturated fat acids, poultry fat usually leads to a biodiesel with low oxidative stability. In this study, the oxidation of their ethylic and methylic biodiesels was evaluated by Rancimat, PDSC, and PetroOxy. The OSI (Rancimat) was of 0.47 and 0.40 h for the ethylic and methylic biodiesel, respectively. In PDSC, both fuels presented an OT of about 120–123 °C. PetroOxy analysis indicated an OxyStab of 11 min for BEF and higher than 11 min for BMF. There was no correspondence among the oxidative stabilities of the employed techniques [OT(BEF) ≈ OT(BMF), OSI(BEF) > OSI(BMF), and OxyStab(BEF) < OxyStab(BMF)]. The discussion of these results was based on the indicator measured by each technique: enthalpic events are observed by PDSC; conductivity of volatile secondary oxidation products is measured by Rancimat; reduction of the oxygen pressure is determined by PetroOxy. This discussion showed that these different indicators do not reflect the same stage of the oxidative process as energy is release at the beginning of the propagation step, oxygen pressure decreases during the propagation step, and oxidation products are formed during the termination step.

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Journal of Thermal Analysis and Calorimetry
Authors: F. T. G. Vieira, A. L. M. Oliveira, D. S. Melo, S. J. G. Lima, E. Longo, A. S. Maia, A. G. Souza, and I. M. G. Santos

Abstract

Alkaline earth stannates have recently become important materials in ceramic technology due to its application as humidity sensor. In this work, alkaline earth stannates doped with Fe3+ were synthesized by the polymeric precursor method, with calcination at 300 °C/7 h and between 400 and 1100 °C/4 h. The powder precursors were characterized by TG/DTA after partial elimination of carbon. Characterization after the second calcination step was done by X-ray diffraction, infrared spectroscopy, and UV–vis spectroscopy. Results confirmed the formation of the SrSnO3:Fe with orthorhombic perovskite structure, besides SrCO3 as secondary phase. Crystallization occurred at 600 °C, being much lower than the crystallization temperature of perovskites synthesized by solid state reaction. The analysis of TG curves indicated that the phase crystallization was preceded by two thermal decomposition steps. Carbonate elimination occurred at two different temperatures, around 800 °C and above 1000 °C.

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Abstract

Biodiesel can be obtained from various fatty acid sources. Each raw material has a different chemical composition that leads to different properties. Owing to these properties, the mixture of different proportions of raw materials can lead to biodiesels with best features in relation to physicochemical parameters such as viscosity, oxidative stability and flow properties, generating a fuel whose characteristics meet the requirements of the current legislation of the Brazilian National Agency of Petroleum, Natural Gas and Biofuels (ANP). The objective of this study was to determine the physicochemical properties of biodiesel samples produced from mixtures of beef tallow, babassu oil, and soybean oil. The thermo-oxidative stability was evaluated using thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC). The results showed that all samples were in accordance to the ANP specifications. The biodiesel obtained from a mixture containing 50% of babassu oil had lower values of pour point, cold filter plugging point, and freezing point. This biodiesel also showed a higher thermo-oxidative stability in synthetic air and in oxygen atmospheres.

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Journal of Thermal Analysis and Calorimetry
Authors: D. Melo, R. M. M. Marinho, F. T. G. Vieira, S. J. G. Lima, E. Longo, A. G. Souza, A. S. Maia, and I. M. G. Santos

Abstract

Perovskite type oxides have been intensively studied due to their interesting optical, electrical, and catalytic properties. Among perovskites the alkaline earth stannates stand out, being strontium stannates (SrSnO3) the most important material in ceramic technology among them due to their wide application as dielectric component. SrSnO3 has also been applied as stable capacitor and humidity sensor. In the present work, SrSnO3:Cu was synthesized by polymeric precursor method and heat treated at 700, 800, and 900 °C for 4 h. After that, the material was characterized by thermal analysis (TG/DTA), X-ray diffraction (XRD), infrared spectroscopy, and UV–vis spectroscopy. Results indicated three thermal decomposition steps and confirmed the presence of strontium carbonate and Cu2+ reduction to Cu+ at higher dopant amounts. XRD patterns indicated that the perovskite crystallization started at 700 °C with strontiatite (SrCO3) and cassiterite (SnO2) as intermediate phases, disappearing at higher temperatures. The amount of secondary phase was reduced with the increase in the Cu concentration.

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Journal of Thermal Analysis and Calorimetry
Authors: K. L. G. V. Araújo, P. S. Epaminondas, M. C. D. Silva, A. E. A. de Lima, R. Rosenhaim, A. S. Maia, L. E. B. Soledade, A. L. Souza, I. M. G. Santos, A. G. Souza, and N. Queiroz

Abstract

Physicochemical and thermal analyses were undertaken to evaluate the influence of the temperature on the oxidation of sea fish oil once its polyunsaturated fatty acids deteriorate rapidly. Fish oil displayed four decomposition steps in synthetic air atmosphere and only one step in nitrogen atmosphere. The first step started at 189 and 222 °C for oxidizing and inert atmospheres, respectively. An OIT value of 53 min was measured at 100 °C. After the degradation process the peroxide index and the iodine index reduced from 35.38 to 9.85 meq × 1000 g−1 and from 139.79 to 120.19 gI2 × 100 g−1, respectively. An increase of the free fatty acids amount from 0.07 to 0.17% was observed while viscosity increased from 57.2 to 58.0 cP. Absorption at 272 nm also increased. The thermogravimetric and spectroscopic techniques are reproducible and versatile being an option for characterization of edible oil oxidation.

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Biodiesel from soybean oil, castor oil and their blends

Oxidative stability by PDSC and rancimat

Journal of Thermal Analysis and Calorimetry
Authors: M. B. Dantas, A. R. Albuquerque, L. E. B. Soledade, N. Queiroz, A. S. Maia, I. M. G. Santos, A. L. Souza, E. H. S. Cavalcanti, A. K. Barro, and A. G. Souza

Abstract

Even not being described in the EN 14112 standard, PDSC has been used for the determination of the biodiesel oxidative stability, by OIT and OT measurements. In this study, biodiesel blends were obtained by mixing soybean (BES) and castor (BEM) ethyl esters and its induction periods were measured by Rancimat and PDSC. The blends (BSMX) showed intermediate values of OSI, OT, and OIT, compared with BES and BEM. Although, the molar fraction of the components varied linearly in BSMX, OSI, OT, and OIT values increased exponentially in relation to the castor biodiesel amount in the blends. Introduction of castor oil biodiesel increased the blend stability, so the BSM30 blend reached the OSI limit of 6 h. OSI, OIT, and OT showed a high-linear correlation, pointing out that PDSC can be used in the analysis of this kind of biodiesel, with a smaller sample and analysis time, as compared to Rancimat. The use of biodiesel blends was a good alternative in the correction of the oxidative stability of the final product without the need of antioxidant addition.

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