954 resultados para Chemical Characterization
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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A novel porous silica matrix has been prepared from Pyrex glass, using hydrothermal treatment under saturated-steam condition. This process makes it possible to obtain, in one step, a silica support formed of a homogeneously distributed and interconnected macropore microstructure. The new matrix contains silanol groups that can be used in reactions of surface modification to provide a hybrid material and a selective macrofiltration membrane, and also it can improve chemical inertness. The porous matrix is noncrystalline as obtained and, after thermal treatment at temperatures higher than 950degreesC, exhibits an X-ray pattern characteristic of alpha-cristobalite and low volume contraction. The present samples were characterized by scanning electron microscopy, mercury intrusion porosimetry, nitrogen adsorption-desorption isotherms, infrared spectroscopy, X-ray powder diffractometry, atomic absorption, and high-resolution solid-state nuclear magnetic resonance. The results present a new way of producing a macroporous silica matrix.
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A phase diagram of the pseudo-ternary Aerosol OT (AOT) + n-butanol/n-heptane/water system, at a mass ratio of AOT/n-butanol = 2, is presented. Conductivity measurements showed that within the vast one-phase microemulsion region observed, the structural transition from water-in-oil to oil-in-water microemulsion occurs continuously without phase separation. This pseudo-ternary system was applied to the synthesis of carbon-supported Pt 70Fe30 nanoparticles, and it was found that nanoparticles prepared in microemulsions containing n-butanol have more Fe than those prepared in ternary microemulsions of AOT/n-heptane/water under similar conditions. It was verified that introducing n-butanol as a cosurfactant into the AOT/n-heptane/water system lead to complete reduction of the Fe ions that allowed obtaining alloyed PtFe nanoparticles with the desired composition, without the need of preparing functionalized surfactants and/or the use of inert atmosphere. © 2007 American Chemical Society.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Solid-state M-2-MeO-BP compounds, where M represents bivalent Mn, Fe, Co, Ni, Cu, Zn and 2-MeO-BP is 2-methoxybenzylidenepyruvate have been synthesized. Simultaneous thermogravinietry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal stability and thermal decomposition of these compounds. The results led to information about the composition, dehydration, crystallinity and thermal decomposition of the isolated compounds.
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Biomodification of existing hard tissue structures, specifically tooth dentin, is an innovative approach proposed to improve the biomechanical and biochemical properties of tissue for potential preventive or reparative therapies. The objectives of the study were to systematically characterize dentin matrices biomodified by proanthocyanidin-rich grape seed extract (GSE) and glutaraldehyde (GD). Changes to the biochemistry and biomechanical properties were assessed by several assays to investigate the degree of interaction, biodegradation rates, proteoglycan interaction, and effect of collagen fibril orientation and environmental conditions on the tensile properties. The highest degree of agent–dentin interaction was observed with GSE, which exhibited the highest denaturation temperature, regardless of the agent concentration. Biodegradation rates decreased remarkably following biomodification of dentin matrices after 24 h collagenase digestion. A significant decrease in the proteoglycan content of GSE-treated samples was observed using a micro-assay for glycosaminoglycans and histological electron microscopy, while no changes were observed for GD and the control. The tensile strength properties of GD-biomodified dentin matrices were affected by dentin tubule orientation, most likely due to the orientation of the collagen fibrils. Higher and/or increased stability of the tensile properties of GD- and GSE-treated samples were observed following exposure to collagenase and 8 months water storage. Biomodification of dentin matrices using chemical agents not only affects the collagen biochemistry, but also involves interaction with proteoglycans. Tissue biomodifiers interact differently with dentin matrices and may provide the tissue with enhanced preventive and restorative/reparative abilities.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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The high electronegativity and small size of the fluorine atom and the high stability of C-F bonds impart interesting properties and applications to fluorine containing polymers. The unique properties of fluoropolymers include high thermal stability, improved chemical resistance, low surface energies, low coefficients of friction, and low dielectric constants. Applications of fluorinated polymers include use as noncorrosive materials, polymer processing aids, chemically resistant and antifouling coatings, as well as interlayer dielectrics. Fluorine-containing polymers can be directly synthesized via polymerization of fluorine-containing monomers or by post-polymerization modification. The latter method can be used to attach fluorinated species, such as perfluoroalkyl groups, onto conventional polymer chains, thereby imparting properties of fluorine-containing polymers into conventional polymers and widening their range of potential applications.
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Silicon carbide (SiC) is considered a suitable candidate for high-power, high-frequency devices due to its wide bandgap, high breakdown field, and high electron mobility. It also has the unique ability to synthesize graphene on its surface by subliming Si during an annealing stage. The deposition of SiC is most often carried out using chemical vapor deposition (CVD) techniques, but little research has been explored with respect to the sputtering of SiC. Investigations of the thin film depositions of SiC from pulse sputtering a hollow cathode SiC target are presented. Although there are many different polytypes of SiC, techniques are discussed that were used to identify the film polytype on both 4H-SiC substrates and Si substrates. Results are presented about the ability to incorporate Ge into the growing SiC films for the purpose of creating a possible heterojunction device with pure SiC. Efforts to synthesize graphene on these films are introduced and reasons for the inability to create it are discussed. Analysis mainly includes crystallographic and morphological studies about the deposited films and their quality using x-ray diffraction (XRD), reflection high energy electron diffraction (RHEED), transmission electron microscopy (TEM), scanning electron microscopy (SEM), atomic force microscopy (AFM), Auger electron spectroscopy (AES) and Raman spectroscopy. Optical and electrical properties are also discussed via ellipsometric modeling and resistivity measurements. The general interpretation of these analytical experiments indicates that the films are not single crystal. However, the majority of the films, which proved to be the 3C-SiC polytype, were grown in a highly ordered and highly textured manner on both (111) and (110) Si substrates.
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As the area of nanotechnology continues to grow, the development of new nanomaterials with interesting physical and electronic properties and improved characterization techniques are several areas of research that will be remain vital for continued improvement of devices and the understanding in nanoscale phenomenon. In this dissertation, the chemical vapor deposition synthesis of rare earth (RE) compounds is described in detail. In general, the procedure involves the vaporization of a REClx (RE = Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho) in the presence of hydride phase precursors such as decaborane and ammonia at high temperatures and low pressures. The vapor-liquid-solid mechanism was used in combination with the chemical vapor deposition process to synthesize single crystalline rare earth hexaboride nanostructures. The crystallographic orientation of as-synthesized rare earth hexaboride nanostructures and gadolinium nitride thin films was controlled by judicious choice of specific growth substrates and modeled by analyzing x-ray diffraction powder patterns and crystallographic models. The rare earth hexaboride nanostructures were then implemented into two existing technologies to enhance their characterization capabilities. First, the rare earth hexaboride nanowires were used as a test material for the development of a TEM based local electrode atom probe tomography (LEAP) technique. This technique provided some of the first quantitative compositional information of the rare earth hexaboride systems. Second, due to the rigidity and excellent conductivity of the rare earth hexaborides, nanostructures were grown onto tungsten wires for the development of robust, oxidation resistant nanomanipulator electronic probes for semiconductor device failure analysis.
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Wet impregnation of pre-synthesized surfactant-stabilized aqueous rhodium (0) colloidal suspension on silica was employed in order to prepare supported Rh-0 nanoparticles of well-defined composition, morphology and size. A magnetic core-shell support of silica (Fe(3)O4@SiO2) was used to increase the handling properties of the obtained nanoheterogeneous catalyst. The nanocomposite catalyst Fe3O4@SiO2-Rh-0 NPs was highly active in the solventless hydrogenation of model olefins and aromatic substrates under mild conditions with turnover frequencies up to 143,000 h(-1). The catalyst was characterized by various transmission electron microscopy techniques showing well-dispersed rhodium nanoparticles (similar to 3 nm) mainly located at the periphery of the silica coating. The heterogeneous magnetite-supported nanocatalyst was investigated in the hydrogenation of cyclohexene and compared to the previous surfactant-stabilized aqueous Rh-0 colloidal suspension and various silica-supported Rh-0 nanoparticles. Finally, the composite catalyst could be reused in several runs after magnetic separation. (C) 2011 Elsevier B. V. All rights reserved.
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In this paper, Co/CeO2 catalysts, with different cobalt contents were prepared by the polymeric precursor method and were evaluated for the steam reforming of ethanol. The catalysts were characterized by N-2 physisorption (BET method), X-ray diffraction (XRD), UV-visible diffuse reflectance, temperature programmed reduction analysis (TPR) and field emission scanning electron microscopy (FEG-SEM). It was observed that the catalytic behavior could be influenced by the experimental conditions and the nature of the catalyst employed. Physical-chemical characterizations revealed that the cobalt content of the catalyst influences the metal-support interaction which results in distinct catalyst performances. The catalyst with the highest cobalt content showed the best performance among the catalysts tested, exhibiting complete ethanol conversion, hydrogen selectivity close to 66% and good stability at a reaction temperature of 600 degrees C. (c) 2012 Elsevier B.V. All rights reserved.
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The performance of an anaerobic sequencing-batch biofilm reactor (ASBBR-laboratory scale- 14L) containing biomass immobilized on coal was evaluated for the removal of elevated concentrations of sulfate (between 200 and 3,000 mg SO4-2.L-1) from industrial wastewater effluents. The ASBBR was shown to be efficient for removal of organic material (between 90% and 45%) and sulfate (between 95% and 85%). The microbiota adhering to the support medium was analyzed by amplified ribosomal DNA restriction analysis (ARDRA). The ARDRA profiles for the Bacteria and Archaea domains proved to be sensitive for the determination of microbial diversity and were consistent with the physical-chemical monitoring analysis of the reactor. At 3,000 mg SO4-2.L-1, there was a reduction in the microbial diversity of both domains and also in the removal efficiencies of organic material and sulfate.
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Males, queens and workers of stingless bees show differences in external morphology, behaviour and roles within a colony. In addition, each individual has a cuticular chemical signature responsible for mutual communication that is essential for maintaining the integrity of the colony. In this paper we characterize the cuticular hydrocarbon composition of newly emerged diploid and haploid males, workers and virgin queens of Melipona quadrifasciata by gas chromatography-mass spectrometry (GC/MS) analysis. This is the first time that the cuticular profile of diploid males in a species of stingless bee has been characterized. We found differences in the cuticular hydrocarbon composition among males, workers and virgin queens, recording both qualitative and quantitative differences among individuals of different phenotypes. However, no compound was found exclusively in diploid males. The cuticular chemical profiles of haploid and diploid males were very similar to those of workers. Moreover, the cuticular lipids of males and workers were significantly different from those of queens. Tricosane, pentacosene-2 and 7-methyl-heptacosane were the compounds responsible for this significant separation. This result correlates with the behavioural and morphological differences among these phenotypes.
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Sugarcane bagasse cellulose was subjected to the extremely low acid (ELA) hydrolysis in 0.07% H2SO4 at 190, 210 and 225 degrees C for various times. The cellulose residues from this process were characterized by TGA, XRD, GPC, FIR and SEM. A kinetic study of thermal decomposition of the residues was also carried out, using the ASTM and Kissinger methods. The thermal studies revealed that residues of cellulose hydrolyzed at 190, 210 and 225 degrees C for 80,40 and 8 min have initial decomposition temperature and activation energy for the main decomposition step similar to those of Avicel PH-101. XRD studies confirmed this finding by showing that these cellulose residues are similar to Avicel in crystallinity index and crystallite size in relation to the 110 and 200 planes. FTIR spectra revealed no significant changes in the cellulose chemical structure and analysis of SEM micrographs demonstrated that the particle size of the cellulose residues hydrolyzed at 190 and 210 degrees C were similar to that of Avicel. (C) 2011 Elsevier B.V. All rights reserved.