Análises térmicas e processo de sinterização da cerâmica KSr2Nb5O15 dopada com CuO

KSr2Nb5O15 is a ferroelectric material. The sintering process of the KSr2Nb5O15 ceramic doped with different amounts of CuO was investigated in this research. It was found that CuO is effective as promoter of the densification process of the KSN ceramic. The developed microstructures were different due to the amount of CuO and secondary phases were observed in the microstructures. However, the results of X - ray diffraction showed that only the tetragonal tungsten bronze (TTB) structure was identified in all the investigated ceramic systems. The thermal behavior of CuO and also of the CuO - KSN phase mixture was investigated by thermal analysis.

Caracterização da fusão peritética do cloreto de sódio di-hidratado por curvas de aquecimento

Binary mixture phase diagrams are normally obtained from thermal analysis involving freezing point curves. However, that approach is not always reliable and easy to follow to all kinds of mixtures in any proportion. In fact, even for a simple system, such as NaCl-H2O, this freezing methodology gives mixed results when one starts from a solid-solution system, due mostly to the formation of the NaCl.2H2O, which has an incongruent melting point, and the dependence of its solubility with the temperature. In this work we report a trustworthy, simple and cheap method involving heating curves to drawn the NaCl-H2O phase diagram.

Argilas como catalisadores verdes na esterificação do colesterol: caracterização espectroscópica e identificação de polimorfos por métodos de análise térmica. Uma proposta laboratorial interdisciplinar para o 1º ciclo universitário

A laboratory experiment that enables the professor to introduce the problematic of sustainable development in pharmaceutical chemistry to undergraduate students is proposed, using a simple synthetic procedure. Cholesteryl acetate is prepared by the esterification of cholesterol using Montmorillonite K10 as heterogeneous catalyst. Cholesterol and cholesteryl acetate are characterized by spectroscopic (¹H RMN, 13C RMN, FTIR) and thermal analysis techniques. The thermal methods are used to introduce the concepts of polymorphism and the nature of mesophases.

Processamento e caracterização de espumas vitrocerâmicas do sistema sncp (Sio2-Na2o-Cao-P2 O5)

Glass-ceramics foams prepared from glasses of the SiO2-Na2O-CaO-P2O5 by replication process were obtained and characterized in terms of their chemical and physical properties by X-ray fluorescence, X-ray diffraction, laser diffraction, thermal analysis, density, mechanical strength, microstructural and cytotoxic analysis. The results showed that it is possible to produce glass-ceramic foams by the replication method with optimized properties but cytotoxic analysis indicates that the glass-ceramic foams are not bioactive materials. Mechanical strength values varying from 0.5 to 1.0 MPa and from 0.8 to 2.3 MPa were reached for mean particle sizes of 10 and 6 µm, respectively.

Obtaining high purity silica from rice hulls

Many routes for extracting silica from rice hulls are based on direct calcining. These methods, though, often produce silica contaminated with inorganic impurities. This work presents the study of a strategy for obtaining silica from rice hulls with a purity level adequate for applications in electronics. The technique is based on two leaching steps, using respectively aqua regia and Piranha solutions, which extract the organic matrix and inorganic impurities. The material was characterized by Fourier-transform infrared spectroscopy (FTIR), powder x-ray diffraction (XRD), x-ray fluorescence (XRF), scanning electron microscopy (SEM), particle size analysis by laser diffraction (LPSA) and thermal analysis.

Análise térmica aplicada à caracterização da sinvastatina em formulações farmacêuticas

Thermogravimetry (TG) and differential scanning calorimetry (DSC) are used in pharmaceutical studies for drugs characterization, purity, formulations compatibility, polymorphism identification, stability evaluation, and thermal decomposition of drugs and pharmaceutical formulations. Simvastatin showed fusion at 138.5 ºC and thermal stability up to 248 ºC. Simvastatin was incompatible with preservative excipient butylhydroxyanisole (BHA) performing a process of crystal amorphization. The drug showed morphological polymorphism, where it has the same unit cell but with different crystal habits according to the recrystallization solvent.

Análise térmica aplicada a fármacos e formulações farmacêuticas na indústria farmacêutica

Several matters of the pharmaceutical demonstrate the great importance of thermal analysis application, especially TG and DSC for the pharmaceutical industry future, namely: characterization of the drugs with the thermal events definition, in studies of drug purity, in the polymorphs identification, in compatibility studies of solid dosage pharmaceutical formulations, in drugs and pharmaceutical formulations thermal stability, and in determination of shelf life for isothermal degradation kinetics by extrapolation using the Arrhenius equation. Thus, the test results obtained from thermal analysis are directly related to the quality of a pharmaceutical product, whether the stability or bioavailability of the pharmaceutical product.

Efeitos da história térmica nas propriedades do polímero pet: um experimento para ensino de análise térmica

Polyethilenetherephtalate (PET) is commonly used in manufacturing of beverage bottles representing a didactic appeal in thermal analysis education due to its presence in the student's day life. Additionally such polymer presents well defined thermal analytical curves and a well known thermal behavior. TGA curve is used to present the thermal stability. The thermal history effects in the thermal properties of a PET sample from a soft drink bottle are used to demonstrate the effect of different heating/cooling conditions on glass transition, melting, crystallization and crystalline degree using DSC curves.

Preparation of association compound between rhodium(II) citrate and β-cyclodextrin

Inclusion compound of rhodium(II) citrate with β-cyclodextrin in a 1:1 molar ratio was prepared using freeze-drying method. X-ray diffactometry, thermal analysis (TG/DTG/DSC), infrared and ¹H-NMR with ¹H spin lattice relaxation (¹H T1) measurements and 13C techniques were used to characterize the system prepared. The results indicated the formation of inclusion or association compounds between rhodium(II) citrate and β-cyclodextrin.

Efeito da ativação mecânica de uma formulação de talco/caulim/alumina sobre o mecanismo e a cinética de formação de cordierita

In this study, the influence of mechanical activation by intensive ball milling of a stoichiometric mixture of talc, kaolin, and alumina on the mechanism and kinetics of cordierite (2MgO·2Al2O3·5SiO2) formation was evaluated. The raw materials were characterized by chemical analysis, X-ray diffraction (XRD), laser diffraction, and helium pycnometry. The kinetics and mechanism of cordierite formation were studied by XRD, differential thermal analysis, and dilatometry in order to describe the phase formation as a function of temperature (1000-1400 ºC), time of thermochemical treatment (0-4 h), and grinding time of the mixture (0-45 min). Finally, the optimal conditions of the thermochemical treatment that ensured the formation of cordierite were determined: milling time of 45 min and thermal treatment at 1280 ºC for 1 h.

Estudio de copolimerización injerto del acrilato de butilo sobre almidón empleando sistema iniciador redox

The mixture of synthetic and natural materials yields a material with improved physical-chemical properties. One way of obtaining this kind of material is through graft copolymerization. Some natural materials have been used in graft copolymerization with synthetic monomers. In this work, graft copolymerization of butyl acrylate (BA) onto starch using a redox initiator system was carried out. The graft yield was evaluated for different reaction conditions. The graft copolymer was characterized by infrared spectroscopy, thermal analysis and scanning electron microscopy (SEM).

Obtenção de nanocelulose da fibra de coco verde e incorporação em filmes biodegradáveis de amido plastificados com glicerol

Composites strengthened with nanocellulose have been developed with the aim of improving mechanical, barrier, and thermal properties of materials. This improvement is primarily due to the nanometric size and the high crystallinity of the incorporated cellulose. Cassava starch films plasticized with glycerol and incorporated with nanocellulose from coconut fibers were developed in this study. The effect of this incorporation was studied with respect to the water activity, solubility, mechanical properties, thermal analysis, and biodegradability. The study demonstrated that the film properties can be significantly altered through the incorporation of small concentrations of nanocellulose.

Poliuretanos obtenidos a partir de aceite de higuerilla modificado y poli-isocianatos de lisina: síntesis, propiedades mecánicas y térmicas y degradación in vitro

Biodegradable polyurethanes (PUR) were prepared from polyols derived from castor oil by transesterification of pentaerythritol-modified castor oil and lysine polyisocyanates (LDI and LTI). The polyurethanes obtained were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis (TGA), and dynamic mechanical thermal analysis (DMTA). The mechanical behavior of the polyurethanes was measured by Shore A hardness and tensile testing (stress-strain curves). The biodegradable nature of the material was determined by contact angle, water absorption tests, and in vitro degradation in PBS solution. This study aims to examine the effect of the structure and functionality of diisocyanate on the mechanical properties and in vitro degradation of the material. The results were compared with homologous materials obtained from isophorone diisocyanate (IPDI) used in previous works. The objective was to evaluate candidate materials that can be potentially used in tissue engineering.

DESENVOLVIMENTO DE MATERIAIS HÍBRIDOS MICRO-MESOPOROSOS DO TIPO ZSM-12/MCM-41

Micro-mesoporous hybrid materials of ZSM-12/MCM-41 type with different micro- and mesoporosity contributions were prepared by a procedure that uses the desilication of the zeolite in an alkaline medium, followed by recrystallization onto the mesostructure, where the zeolite is used as the silica source in the formation of mesoporous phase. The materials were characterized by X-ray diffraction, nitrogen adsorption-desorption at 77 K, scanning electron microscopy and thermal analysis. The results showed that the methodology utilized is efficient for obtaining hybrid materials of ZSM-12/MCM-41 type with optimized micro-and mesoporosity.

PARÂMETROS TERMODINÂMICOS DA CASCA DE LARANJA DESIDRATADA

The global energy scenario is currently a widely discussed topic, with growing concern about the future supplies. Thus, much attention has been dedicated to the utilization of biomass as an energy resource. In this respect, orange peel has become a material of great interest, especially to Brazil, which generates around 9.5 million tons of this waste per year. To this end, the authors studied the kinetics of the thermal processing of dried orange peel in inert and oxidizing atmosphere. The thermodynamic parameters were determined by the Ozawa-Flynn-Wall method for the global process observed during heating from the 25°C up to 800°C. The thermal analysis in air and nitrogen showed 3-2 stages of mass loss, respectively, with approximately 20% residual mass under a nitrogen atmosphere. The increase in the values of activation energy for the conversion points between 20% and 60% for thermal effects in air and nitrogen atmosphere was observed. The activation energy obtained in an oxidizing atmosphere was higher than that obtained under a nitrogen atmosphere. The fourier-transform infrared spectroscopy and X-ray diffraction analysis showed that the material has a high level of complexity with the presence of alkali and alkaline earth groups as well as phosphate, plus substances such as pectin, cellulose and lignin.