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- Author or Editor: A. Souza x
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Abstract
The synthesis and the characterization of Al2O3-based nanocrystalline inorganic pigments are reported. The pigments were synthesized by the polymeric precursor (Pechini method) using Cr2O3 as chromophore. XRD results only evidenced the corundum phase. The average particle size was about 34 nm. The samples were also characterized by differential scanning calorimetry (DSC) and thermogravimetry (TG), and CIE-L*a*b* calorimetry. The pigments obtained in this work presented different colors, ranging from green to rose.
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
Sunflower biodiesel
Use of P-DSC in the evaluation of antioxidant efficiency
Abstract
The higher is the degree of unsaturation in ester chain of a biodiesel, the smaller is its oxidation stability. Sunflower biodiesel obtained by the ethyl route possesses a high amount of unsaturated fatty acids, mainly oleic acid (C18:1) and linoleic acid (C18:2), thus being more prone to the oxidation process. In Brazil, with the purpose of meeting the specifications of the Brazilian National Agency of Petroleum, Natural Gas and Biofuels (ANP), antioxidant additives, from synthetic and natural origins, have been added to the biofuel. Antioxidants are an alternative to prevent the oxidative deterioration of the fatty acid derivatives, as they are substances able to reduce the oxidation rate. In this study, the oxidative stability of sunflower biodiesel, obtained by the ethyl route and additivated with different concentrations of the antioxidants butylated hydroxytoluene (BHT) and t-butylhydroquinone (TBHQ), was evaluated by means of Pressure differential scanning calorimetry (P-DSC) and the Accelerated oxidative stability test (Rancimat, Method EN 14112). The results obtained by the two techniques showed the same oxidation tendency. Thus, P-DSC can be used as an alternative to determine the oxidative stability of biodiesel. The antioxidant TBHQ, added to biodiesel at the concentrations of 2000 and 2500 mg kg−1, raised the oxidation induction time to a value higher than 6 h, the limit established by the Resolution ANP number 7/2008, thus being the best alternative among the studied antioxidants.
Abstract
Biodiesel oxidation is a complex process widely influenced by the chemical composition of the biofuel and storage conditions. Several oxidation products can be formed from these processes, depending on type and amount of the unsaturated fatty acid esters. In this work, fatty acid methyl and ethyl esters were obtained by base-catalyzed transesterification of soybean oil and physicochemically characterized according to standards from ASTM, EN, and ABNT. The thermal and oxidative stabilities of biodiesel samples were investigated during the storage process by pressure differential scanning calorimetry (PDSC) and by viscosity measurements. Absolute viscosities of biodiesels after accelerated aging were also determined. The viscosity increased as the aging temperature and time were raised. The results showed that oxidation induction can occur during storage, decreasing the biodiesel stability. PDSC analysis showed that during storage under climate simulation the values of high-pressure oxidative induction times (HPOIT) were reduced for both FAEE and FAME.
Abstract
Isothermal decomposition kinetic of three lanthanide mixed complexes with the general formula of Ln(thd)3phen (where Ln=Nd3+, Sm3+ or Er3+, thd=2,2,6,6-tetramethyl-3,5-heptanodione and phen=1,10-phenanthroline) has been studied in this work. The powders were characterized by their melting point, elemental analysis, FTIR spectroscopy and thermogravimetry. The isothermal TG curves have been recorded under the same conditions at 265–285, 265–285 and 250–270°C for Nd(thd)3phen, Sm(thd)3phen and Er(thd)3phen, respectively. The kinetic parameters, i.e. activation energy, reaction order and frequency factor were obtained through the technique of lineal regression using the relation g(α)=kt+g 0. The analysis was done at decomposed fractions between 0.10–0.90. The values of activation energy were: 114.10, 114.24 and 115.04 kJ mol–1 for the Nd(thd)3phen, Sm(thd)3phen and Er(thd)3phen complexes, respectively. The kinetic models that best described the isothermal decomposition reaction the complexes were R1 and R2. The values of activation energy suggests the following decreasing order of stability: Nd(thd)3phen<Sm(thd)3phen<Er(thd)3phen.
Lanthanide Lanthanide nitrate complexes with 2-azacyclononanone
Thermal and kinetic studies
Abstract
Thermal behavior of rare earth nitrate complexes with 2-azacyclononanone (AZA) with Ln(NO3)3·3(AZA) composition (where Ln=Gd, Er and Ho) was analyzed in kinetic point of view. Kinetic parameters were calculated from thermogravimetric data. All obtained results were similar. The first decomposition step was representative to the loss of ligand and the residue was essentially Ln2O3. Furthermore, a reaction path was proposed for the thermal decomposition of the Ln(NO3)3·3(AZA).
Abstract
Chemical and thermal analyses of golden and brown flaxseeds were carried out for raw and toasted seeds aiming at evaluating their nutritional and thermo-oxidative properties. Moisture, lipids, protein, soluble carbohydrates, and ash contents were quantified. Concerning lipids and proteins, in average, no meaningful differences were observed for the two varieties, being also equivalent to the literature data. The golden variety had a lower amount of fibers and a higher amount of soluble carbohydrates than the brown variety. The techniques of thermogravimetry and differential scanning calorimetry were applied for elucidating the thermal degradation process of the seeds. The toasted gold and brown seeds were more stable to thermal decomposition than the raw seeds, under oxidative conditions. Golden seeds seem to be more susceptible to oxidation than brown seeds, under toasting conditions. Finally, no meaningful advantages were observed for the golden seeds in comparison to the brown ones.
Abstract
Hydrotalcite was synthesised by co-precipitation method, calcined and characterized by XRD, BET, IR and TG/DTA/DTG analyses and tested as solid base catalyst in the transesterification of soybean oil with methanol, achieving a methyl ester content of 99.5%. The thermal decomposition of hydrotalcite calcined occurred in four mass loss steps at 28, 105, 203 and 400 °C. The hydrotalcite was recovered and through a simple evaluation by TG/DTA/DTG techniques it was found that at 500 °C is the temperature, where the organic matter should be eliminated from the catalyst. This study shows the importance of thermal analysis in the evaluation of the recovery temperature of hydrotalcite.
Abstract
SrSnO3 was synthesized by the polymeric precursor method with elimination of carbon in oxygen atmosphere at 250 °C for 24 h. The powder precursors were characterized by TG/DTA and high temperature X-ray diffraction (HTXRD). After calcination at 500, 600 and 700 °C for 2 h, samples were evaluated by X-ray diffraction (XRD), infrared spectroscopy (IR) and Rietveld refinement of the XRD patterns for samples calcined at 900, 1,000 and 1,100 °C. During thermal treatment of the powder precursor ester combustion was followed by carbonate decomposition and perovskite crystallization. No phase transition was observed as usually presented in literature for SrSnO3 that had only a rearrangement of SnO6 polyhedra.
