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Thermal analysis has been used to evaluate the stability, glass transition, and water retention of Nafion based polymer–ceramic electrolytes. These electrolytes are envisioned as promising replacement of Nafion in fuel cells operating above 100 °C. The polymeric matrix prepared by casting exhibits lower crystallinity than the extruded Nafion, a feature that affects the water absorption properties. The addition of titania-based nanotubes and nanoparticles to the polymer has enhanced the water retention at high temperatures (~130 °C) and the glass transition temperature, respectively. Such results are important for the design of composite electrolytes for the operation of fuel cells at high temperatures. [ABSTRACT FROM AUTHOR]

The aim of this study was to use DSC and X-ray diffraction measurements to determine the pore size and pore wall thickness of highly ordered SBA-15 materials. The DSC curves showed two endothermic events during the heating cycle. These events were due to the presence of water inside and outside of mesopores. The results of pore radius, wall thickness and pore volume measurements were in good agreement with the results obtained by nitrogen adsorption measurement, XRD and transmission electron microscopy. [ABSTRACT FROM AUTHOR]

A porous nickel–8 mol% yttria stabilized zirconia (Ni–8YSZ) composite, used as anode for solid oxide fuel cell, was obtained by reduction of NiO–8YSZ cermet. The first goal was the evaluation of the temperature effect of powder processing by thermogravimetry. In addition, the influence of porosity in the reduction kinetic of the sample sintered at 1450 °C was evaluated. The final porosity produced in NiO–8YSZ composite by pore former was 30.4 and 37.9 vol.%, respectively, for 10 and 15 mass% of corn starch. The sample with 15 mass% of corn starch promotes a reduction rate almost twice higher than sample with 10 mass% of corn starch. The porosity introduced by the reduction of NiO was 23 vol.%. [ABSTRACT FROM AUTHOR]

Differential Scanning Calorimetry (DSC), thermogravimetry/derivative thermogravimetry (TG/DTG) and infrared spectroscopy (IR) techniques were used to investigate the compatibility between prednicarbate and several excipients commonly used in semi solid pharmaceutical form. The thermoanalytical studies of 1:1 (m/m) drug/excipient physical mixtures showed that the beginning of the first thermal decomposition stage of the prednicarbate ( Tonset value) was decreased in the presence of stearyl alcohol and glyceryl stearate compared to the drug alone. For the binary mixture of drug/sodium pirrolidone carboxilate the first thermal decomposition stage was not changed, however the DTG peak temperature ( Tpeak DTG) decreased. The comparison of the IR spectra of the drug, the physical mixtures and of the thermally treated samples confirmed the thermal decomposition of prednicarbate. By the comparison of the thermal profiles of 1:1 prednicarbate:excipients mixtures (methylparaben, propylparaben, carbomer 940, acrylate crosspolymer, lactic acid, light liquid paraffin, isopropyl palmitate, myristyl lactate and cetyl alcohol) no interaction was observed. [ABSTRACT FROM AUTHOR]

The synthesis and thermal behavior of the new [Pd(fum)(bipy)] n·2 nH2O ( 1), [Pd(fum)(bpe)] n· nH2O ( 2) and [Pd(fum)(pz)] n·3 nH2O ( 3) {bipy = 4,4′-bipyridine, bpe = 1,2-bis(4-pyridyl)ethene and pz = pyrazine} fumarate complexes are described in this work as well their characterization by IR and 13C CPMAS NMR spectroscopies. TG curves showed that the compounds released organic ligands and lattice water molecules in the temperature range of 46–491 °C. In all the cases, metallic palladium was identified as the final residue. [ABSTRACT FROM AUTHOR]

The thermal decomposition of salbutamol (β2 — selective adrenoreceptor) was studied using differential scanning calorimetry (DSC) and thermogravimetry/derivative thermogravimetry (TG/DTG). It was observed that the commercial sample showed a different thermal profile than the standard sample caused by the presence of excipients. These compounds increase the thermal stability of the drug. Moreover, higher activation energy was calculated for the pharmaceutical sample, which was estimated by isothermal and non-isothermal methods for the first stage of the thermal decomposition process. For isothermal experiments the average values were Eact=130 kJ mol−1 (for standard sample) and Eact=252 kJ mol−1 (for pharmaceutical sample) in a dynamic nitrogen atmosphere (50 mL min−1). For non-isothermal method, activation energy was obtained from the plot of log heating rates vs. 1/ T in dynamic air atmosphere (50 mL min−1). The calculated values were Eact=134 kJ mol−1 (for standard sample) and Eact=139 kJ mol−1 (for pharmaceutical sample). [ABSTRACT FROM AUTHOR]

This paper demonstrates the application of thermal analysis in compatibility and stability studies between an ACE inhibitor (enalapril maleate) and excipients. The results have helped to elucidate the reason of a stability problem observed during the storage of enalapril maleate tablets. Incompatibility between enalapril maleate and colloidal silicon dioxide was detected. Besides, it was confirmed that the reaction between enalapril maleate and NaHCO3 increases the thermal stability of the drug. This study supports the importance of using thermoanalytical methods in the development of pharmaceuticals. [ABSTRACT FROM AUTHOR]

Rare earth picrate complexes with L-leucine (Leu) were synthesized and characterized. Elemental analysis (CHN), EDTA titrations and thermogravimetric data suggest a general formula RE(pic)32Leu⋅5H2O ( RE=La–Lu, Y and pic=picrate). IR spectra indicate the presence of water and suggest that L-leucine is coordinated to the central ion through the nitrogen of the aminogroup. The absorption spectrum of the solid Nd compound indicates that the metal-ligand bonds show a weak covalent character. Emission spectra and biexponential behavior of the luminescence decay of the Eu compound suggest the existence of polymeric species. Thermal analysis results indicate that all the compounds present a similar behavior, with five major thermal decomposition steps. The final products are rare earth oxides. A slow heating rate is necessary to observe all decomposition steps. [ABSTRACT FROM AUTHOR]

In the present work, the thermal decomposition of glimepiride (sulfonylurea hypoglycemic agent) was studied using differential scanning calorimetry (DSC) and thermogravimetry/derivative thermogravimetry (TG/DTG). Isothermal and non-isothermal methods were employed to determine kinetic data of decomposition process. The physical chemical properties and compatibilities of several commonly used pharmaceutical excipients (glycolate starch, microcrystalline cellulose, stearate, lactose and Plasdone®) with glimepiride were evaluated using thermoanalytical methods. The 1:1 physical mixtures of these excipients with glimepiride showed physical interaction of the drug with Mg stearate, lactose and Plasdone®. On the other hand, IR results did not evidence any chemical modifications. From isothermal experiments, activation energy ( E a) can be obtained from slope of ln t vs. 1/ T at a constant conversion level. The average value of this energy was 123 kJ mol–1. For non-isothermal method E a can be obtained from plot of logarithms of heating rates, as a function of inverse of temperature, resulting a value of 157 and 150 kJ mol–1, respectively, in air and N2 atmosphere, from the first stage of thermal decomposition. [ABSTRACT FROM AUTHOR]

Rare earth picrate (RE) complexes with L-lysine (Lys) were synthesized and characterized. Elemental analysis (CHN), EDTA titrations and thermogravimetry data suggest a general formula RE(pic)3·2Lys·2H2O, where RE=La-Lu (without Pm) and Y, pic=picrate). IR spectra suggest that Lys is coordinated to the central ion through the nitrogen of the α-amino group. Parameters obtained from the absorption spectrum of the Nd compound indicated that the metal-ligand bonds are essentially electrostatic. Emission spectrum and biexponential behavior of the luminescence decay of the Eu compound suggest the existence of polymeric species. Thermogravimetric/derivative thermogravimetric (TG/DTG) and differential scanning calorimetry (DSC) curves of all complexes are very similar, with five events. The final products are the corresponding rare earth oxides and their X-ray diffraction patterns are identical to the calcinated oxides. [ABSTRACT FROM AUTHOR]

The influence of experimental conditions on the kinetic parameters of solid-state reactions using thermogravimetry (TG) has been investigated for different materials. The evaluation of these thermal curves is used for the determination of the activation energy,Ea, the pre-exponential factor,A, and the function of the reaction extent,f(α) by the kinetic analysis for TGA (Shimadzu software) based on the Ozawa method. Factorial designs are excellent tools for determining the effects of a wide variety of factors on the results of complex processes. Here a 24factorial design was used to investigate the influence of four variables (sample mass, furnace environment, furnace atmosphere and sample container composition) on the estimation of kinetic parameters of the thermal decomposition of a zidovudine (AZT) pharmaceutical formulation. TG curves registered at five different heating rates showed that AZT has five stages of mass loss in the following temperature ranges: 25-130, 195-270, 270-350, 350-400 and 400-590°C. These events are characterized by the release of water molecules, thermal decomposition in three stages, followed by the elimination of carbonaceous materials. The average value obtained forEausing the TG curves in different experimental conditions was 119 kJ mol-1. The variability study of the influence of different experimental conditions of TG, using the factorial design, indicates with 95% probability that none of the analyzed effects were significant for the AZT sample. [ABSTRACT FROM AUTHOR]

Study of the decomposition kinetics is an important tool for the development of polymer recycling in industrial scale. In this work, parameters such as activation energy, frequency factor and reaction order, were measured under dynamic conditions. Flynn-Wall-Ozawa, Van Krevelen, Horowitz-Metzger, Coats-Redfern, Madhusudanan and Vyazovkin methods were used to determine the kinetic parameters. The analysis of the results obtained by the Coats-Redfern method shows that the thermal degradation process of LDPE and HDPE corresponds to a phase boundary controlled reaction (mechanism R2). This method shows that the reaction order values of LDPE and HDPE are about 0.7 and 0.6, respectively. [ABSTRACT FROM AUTHOR]

Thermal decomposition kinetics of solid rocket propellants based on hydroxyl-terminated polybutadiene-HTPB binder was studied by applying the Arrhenius and Flynn-Wall-Ozawa's methods. The thermal decomposition data of the propellant samples were analyzed by thermogravimetric analysis (TG/DTG) at different heating rates in the temperature range of 300-1200 K. TG curves showed that the thermal degradation occurred in three main stages regardless of the plasticizer (DOA) raw material, the partial HTPB/IPDI binder and the total ammonium perchlorate decompositions. The kinetic parameters Ea (activation energy) and A (pre-exponential factor) and the compensation parameter (Sp) were determined. The apparent activation energies obtained from different methods showed a very good agreement. [ABSTRACT FROM AUTHOR]