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Abstract
Thermogravimetric data were used to calculate the kinetics of isothermal degradation of layered tetratitanate intercalated with n-alkyldiamines H2N(CH2)nNH2 (n=2, 3, 4, 6 or 8). The hydrous matrix showed two mass loss steps from the thermogravimetric curve, corresponding to the release of physisorbed and lattice water molecules. For the intercalated matrices a third mass loss was observed due to the release of organic moiety. From these values, the amine intercalated matrices can be ordered in the following sequence of thermal stability; C4>C2>C3≅C6>C8. Kinetic studies were carried out to the release of lattice water molecules. The kinetic model that best adjusted the experimental isothermal TG data was the diffusion mechanism controlling process.
Abstract
Thermogravimetric data and the kinetic interpretation of the curves of mass loss for ferrocene, ferrocenecarboxylic and ferrocenedicarboxylic acids and a series of ferrocene-containing polyamides are presented. The results indicate that the degradation process occurred with more than one stage of thermal degradation. The apparent activation energy values and the FTIR spectra of the degradation products suggest that the degradation mechanism occurred by either scission of weak links or by random scission of the chain. Apparently, the N-vicinal methylene group was the primary site of attack of oxygen on the polymer chain.
Thermal and kinetic study of statins
Simvastatin and lovastatin
Abstract
Statins are a group of lipoproteins that are used in medicine to treat the high cholesterol level. The effectiveness of statins in reducing the cholesterol level is significant and in long time scale the reduction of the cholesterol level helps to avoid the incidence of degenerative diseases. Simvastatin and lovastatin are belonging to the ‘statins’ family, one of the pharmacologic groups used in the control of dislipidemy. The objective of this work is the thermal stability and kinetic study of the active forms of simvastatin and lovastatin. Thermal data indicated that lovastatin and simvastatin are stable up to 190 and 170°C in air and up to 205 and 203°C in nitrogen, respectively. For melting temperatures DSC curves showed good correlation with the literature data. Comparing the activation energies of the statins at heating rate of 10°C min–1, lovastatin is more stable than simvastatin under the applied experimental conditions.
Abstract
Pt/WOx–ZrO2 bifunctional catalysts were synthesized using impregnation and polymeric precursor methods. After the synthesis process the samples were calcined at 600, 700 and 800C and characterized by X-ray diffraction, nitrogen adsorption and temperature programmed reduction study by thermogravimetry. DTG-TPR profiles showed between three and five reduction events at different temperatures attributed to platinum reduction and to different stages of tungsten species reduction. A comparative study of the synthesis method influence on the DTG-TPR curves was accomplished.
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.
Seismic coda Qattenuation (Q c) in the frequency range from 6 to 20 Hz of two distinct Scoda windows (early and later portions) are compared to analyse the effects of both coda windows on crustal seismic attenuation estimates around Samambaia fault (João CâmaraNortheastern Brazil). Q cvalues associated with the later portion are systematically higher than those related to the early portion. These values follow a frequency (f) function given by Q c(f) = Q 0 f , where Q 0= 11739 and= 1.000.06. In general, Q 0estimate is less sensitive to site effects and stabler than that obtained from the early portion of S coda waves, while its corresponding frequency dependence is similar to that obtained from the early portion of S coda waves. It suggests thatparameter does not depend on coda window's location along the seismic signal. A comparative analysis of both Q 0andvalues with those found recently shows that there is no difference in using early or later portion of S coda waves in the stations located on Pre-Cambrian basement in the João Câmara area. This comparison also shows that the major variations in Q 0values were observed at seismic stations installed on sedimentary terrain. Differences in the seismic attenuation, in both sides of the Samambaia fault, were also observed in this study, and it is in agreement with the hypothesis that Samambaia fault is a kind of boundary between two seismic attenuation zones.
Comparative studies on some analytical methods
Thermal decomposition of powder milk
Abstract
This work present comparative results on powder milk storage quality, obtained from analytical methods. Protein content was determined conventional (Kjeldahl) and colorimetric with biuret reagent at 540 nm and integral quality by thermogravimetric and biological methods. A method was developed for the protein separation of powder milk. Powder milk was submitted to degradation processes at 45, 60 and 80°C for 20 days. The results indicated that protein content values were inconsistent if determinations by Kjeldahl and colorimetric methods and biological tests were compared. There is evidence of thermal decomposition of powder milk as detected by biological and thermogravimetric methods.
Abstract
The thermogravimetric procedures applied to quality control of foods attain the global analysis of quality of the product, through the determination of quality parameters and the thermal stability of products. The kinetic parameters such as order of reaction, apparent activation energy, pre-exponential factors and the thermal decomposition rate constant were determined for the samples of corn and its derivatives by applying isothermal thermogravimetry, utilizing the Arrhenius law. This method presented excellent results as verified with the coherence and data adjustment. The rate constant values showed the expected performance from the chemical point of view.
Abstract
In this work was studied the acid properties of a series of HZSM-12 zeolites with different Si/Al molar ratio. The samples of ZSM-12 were synthesized by the hydrothermal method starting from a gel with the following molar composition: 20MTEA:10Na2O:xAl2O3:100SiO2:200H2O, where: x=2, 1, 0.67 and 0.50, respectively. After the synthesis, the samples of ZSM-12 were ion-exchanged NH4Cl solution to obtain zeolite in the acid form (HZSM-12). The acid properties were evaluated by n-butylamine thermodesorption in a TG equipment at three different heating rates. The model-free kinetic model was applied in the TG integral curves to estimate the apparent activation energy (E a) of the n-butylamine desorption process. The results obtained showed that the HZSM-12 zeolite presents two kinds main of acid sites: one with E a in the range of 115-125 kJ mol-1 classified as weak and other kind with E a varying of 230-250 kJ mol-1 classified as strong.