829 resultados para SOLID-STATE NMR SPECTROSCOPY


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A method for the attachment of 2-mercaptothiazoline (MTZ) to modified silica gel has been developed. In the first step, a new silylant agent was synthesized, named SiMTZ, by the reaction between MTZ molecule and chloropropyltrimethoxysilane (SiCl). SiMTZ and tetraethylortosilicate were co-condensed in the presence of n-dodecylamine, a neutral surfactant template, to produce a modified ordered hexagonal mesoporous silica named HMTZ. The modified material contained 0.89 +/- 0.03 mmol of 2-mercaptothiazoline per gram of silica. FT-IR, FT-Raman, Si-29- and C-13-NMR spectra were in agreement with the proposed structure of the modified mesoporous silica in the solid state. HMTZ material has been used for divalent mercury adsorption from aqueous solution at 298 I K. The series of adsorption isotherms were adjusted to a modified Langmuir equation. The maximum number of moles of mercury adsorbed gave 2.34 +/- 0.09 mmol/g of material. The same interaction was followed by calorimetric titration on an isoperibol calorimeter. The HMTZ presented a high capacity for the removal of the contaminant mercury from water. The Delta H and Delta G values for the interaction were determined to be -56.34 +/- 1.07 and -2.14 +/- 0.11 kJ mol(-1). This interaction process was accompanied by a decrease of entropy value (- 182 J mol(-1) K-1). Thus, the interaction between mercury and HMTZ resulted in a spontaneous thermodynamic system with a high favorable exothermic enthalpic effect. (c) 2007 Elsevier B.V. All rights reserved.

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The polycrystalline sample of Nd3/2Bi3/2Fe5O12 was prepared by a high- temperature solid-state reaction technique. Preliminary X-ray structural analysis exhibits the formation of a single-phase tetragonal structure at room temperature. Microstructural analysis by scanning electron microscopy shows that the sintered sample has well defined grains. These grains are distributed uniformly throughout the surface of the sample. Detailed studies of dielectric response at various frequencies and temperatures exhibit a dielectric anomaly at 400 A degrees C. The electrical properties (impedance, modulus and conductivity) of the material were studied using a complex impedance spectroscopy technique. These studies reveal a significant contribution of grain and grain boundary effects in the material. The frequency dependent plots of modulus and the impedance loss show that the conductivity relaxation is of non-Debye type. Studies of electrical conductivity with temperature demonstrate that the compound exhibits Arrhenius-type of electrical conductivity. Study of ac conductivity with frequency suggests that the material obeys Jonscher's universal power law.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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In this work were synthesized the materials called vanadyl phosphate, hydrogen vanadyl phosphate and vanadyl phosphate doped by transition metals with the aim in adsorption the following compounds: ammonia, hydrogen sulfide and nitrogen oxide. To characterize the starting compounds was used DRX, FTIR, FRX and TG analysis. After the characterization of substrates, proceeded de adsorption of NH3 and H2S gases in reactor, passing the gases with continuous flow for 30 min and room temperature. Gravimetric data indicate that the matrices of higher performance in adsorption of ammonia was those doped by aluminum and manganese, obtaining results of 216,77 mgNH3/g and 200,40 mgNH3/g of matrix, respectively. The matrice of higher performance in adsorption of hydrogen sulfide was that doped by manganese, obtaining results of 86,94 mgH2S/g of matrix. The synthesis of substrates VOPO4.2H2O and MnVOPO4.2H2O with nitrogen oxide was made in solution, aiming the final products VOPO4.G.nH2O and MnVOPO4.G.nH2O (G = NO and n = number of water molecules). The thermo analytical behavior and the infrared spectroscopy are indicative of formation of VOPO4.2,5NO.3H2O compound. Results of scanning electron microscopy (SEM) and Energy dispersive spectroscopy (EDS) of materials vanadyl phosphate and vanadyl phosphate modified after reaction in solid state or in solution with the gases show morphology changes in substrates, beyond the formation of orthorhombic sulfur crystals over their respective hosts when these adsorb hydrogen sulfide

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Cyclodextrin glycosyltransferase (CGTase) is an enzyme that produces cyclodextrins from starch by an intramolecular transglycosylation reaction. Cyclodextrins have been shown to have a number of applications in the food, cosmetic, pharmaceutical, and chemical industries. In the current study, the production of CGTase by Paenibacillus campinasensis strain H69-3 was examined in submerged and solid-state fermentations. P. campinasensis strain H69-3 was isolated from the soil, which grows at 45 C, and is a Gram-variable bacterium. Different substrate sources such as wheat bran, soybean bran, soybean extract, cassava solid residue, cassava starch, corn starch, and other combinations were used in the enzyme production. CGTase activity was highest in submerged fermentations with the greatest production observed at 48-72 h. The physical and chemical properties of CGTase were determined from the crude enzyme produced from submerged fermentations. The optimum temperature was found to be 70-75 degrees C, and the activity was stable at 55 degrees C for 1 h. The enzyme displayed two optimum pH values, 5.5 and 9.0 and was found to be stable between a pH of 4.5 and 11.0.

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Strontium zirconate (SrZrO3) powders have been synthesized by the polymeric precursor method after heat treatment at different temperatures for 2 h in oxygen atmosphere. The decomposition of precursor powder was followed by thermogravimetric analysis, X-ray diffraction (XRD) and Fourier transform Raman (FT-Raman). The UV-vis absorption spectroscopy measurements suggested the presence of intermediary energy levels in the band gap of structurally disordered powders. XRD, Rietveld refinement and FT-Raman revealed that the powders are free of secondary phases and crystallizes in the orthorhombic structure. (C) 2007 Elsevier Masson SAS. All rights reserved.

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The nonohmic electrical features of (Ca-1/4,Cu-3/4)TiO3 perovskite ceramics, which have very strong gigantic dielectric is believed originate from potential barriers at the grain boundaries. In the present study, we used the admittance and impedance spectroscopy technique to investigate (Ca-1/4,Cu-3/4)TiO3 perovskite ceramics with low nonohmic electrical properties. The study was conducted under two different conditions: on as-sintered ceramics and on ceramics thermally treated in an oxygen-rich atmosphere. The results confirm that thermal treatment in oxygen-rich atmospheres influence the nonohmic properties. Annealing at oxygen-rich atmospheres improve the nonohmic behavior and annealing at oxygen-poor atmospheres decrease the nonohmic properties, a behavior already reported for common metal oxide nonohmic devices and here firstly evidenced for the (Ca-1/4,Cu-3/4)TiO3 perovskite related materials. The results show that oxygen also influences the capacitance values at low frequencies, a behavior that is indicative of the Schottky-type nature of the potential barrier. (c) 2006 Elsevier Ltd. All rights reserved.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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The present paper describes the synthesis, characterization, structural refinement and optical absorption behavior of lead tungstate (PbWO(4)) powders obtained by the complex polymerization method heat treated at different temperatures for 2h in air atmosphere. PbWO(4) powders were characterized by X-ray diffraction (XRD), Rietveld refinement, Fourier transform Raman (FT-Raman) spectroscopy and ultraviolet visible (UV-vis) absorption spectroscopy measurements. XRD, Rietveld refinement and FT-Raman revealed that PbWO(4) powders are free of secondary phases and crystallizes in a tetragonal structure. The UV-vis absorption spectroscopy measurements suggest the presence of intermediary energy levels into the band gap of structurally disordered powders. (C) 2008 Elsevier B.V. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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The anodic behaviour of cast Ti-Mo alloys, having different Mo contents (6-20 wt.%), was investigated in acidic and neutral aerated aqueous solutions. All sample showed a valve-metal behaviour, owing to formation and thickening of barrier-type anodic oxides displaying interference colours Growth kinetics. of passive films is influenced by both anodizing electrolyte and composition of the starting alloy. This last parameter was found to change also the solid-state properties of the films, explored by photoelectrochemical and impedance spectroscopy experiments. Thicker films (U(f) = 8 V/MSE) grown on alloys richer in Mo showed more resistive character and a photocurrent sign inversion under negative bias, that revealed an insulating character, whereas corresponding films grown on alloys with lower Mo content, as well as thinner films, behaved as n-type semiconductors. Results are discussed in terms of formation of a mixed Ti-Mo oxide phase. (C) 2008 Elsevier Ltd. All rights reserved