940 resultados para Purification and Characterization


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Solid-state Ln(2-MeO-BP) compounds, where Ln stands for trivalent Eu to Lu and Y(III) and 2-MeO-BP (which is 2-methoxybenzylidenepyruvate) have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffraction, infrared spectroscopy and other methods of analysis were used to characterize and to study these compounds. on the base of the obtained results an Ln(2MeO-BP)(3)center dot H2O general formula can be established.

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A methodology of identification and characterization of coherent structures mostly known as clusters is applied to hydrodynamic results of numerical simulation generated for the riser of a circulating fluidized bed. The numerical simulation is performed using the MICEFLOW code, which includes the two-fluids IIT's hydrodynamic model B. The methodology for cluster characterization that is used is based in the determination of four characteristics, related to average life time, average volumetric fraction of solid, existing time fraction and frequency of occurrence. The identification of clusters is performed by applying a criterion related to the time average value of the volumetric solid fraction. A qualitative rather than quantitative analysis is performed mainly owing to the unavailability of operational data used in the considered experiments. Concerning qualitative analysis, the simulation results are in good agreement with literature. Some quantitative comparisons between predictions and experiment were also presented to emphasize the capability of the modeling procedure regarding the analysis of macroscopic scale coherent structures. (c) 2007 Elsevier B.V. All rights reserved.

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The [Ru(NH3)5(H2O)]2+ and trans-[Ru(NH3)4SO2(H2O)]2+ complexes ions were immobilized on poly(4-vinylpyridine) (4-PVP) through reactions in aqueous solutions. The stability of the imobilized complexes was checked in aqueous solution in the pH 2.0-8.0 range. The number of pyridinic nitrogens in the polymer 4-PVP is 2.80±0.05 mmol/g according to nitrogen elemental analysis. Potentiometric titration experiments showed that the accessible nitrogen, in aqueous medium, was 0.94±0.02 mmol/g with a p Ka value of 7.4±0.2. In addition, ruthenium and sulfate analysis has demonstrated that about 15% of the accessible nitrogen sites are able to coordinate to the metal centers. The characterization of the immobilized complexes was made through diffuse electronic and infrared spectroscopies and differential pulse and cyclic voltammetries. © 1993 Plenum Publishing Corporation.

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Synthesis and crystallographic data are reported for the double rubidium-scandium chromate RbSc(CrO4)2. The parameters of the orthorhombic cell are a = 14.836(2) A ̊; b = 5.627(1) A ̊ and c = 8.835(4) A ̊, Z = 4. The compound is closely related to the lamellar double chromates with other alkali metal cations, iron, lanthanides and yttrium offering the advantage of obtaining inorganic materials for electronics. © 1995.

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The preparation of spherical Y2O2S and Y2O2S:Eu particles using a solid-gas reaction of monodispersed precursors with elemental sulfur vapor under an argon atmosphere has been investigated. The precursors, undoped and doped yttrium basic carbonates, are synthesized by aging a stock solution containing the respective cation chloride and urea at 82-84 °C. Y2O2S and Y2O2S:Eu were characterized in terms of their composition, crystallinity and morphology by chemical analysis, X-ray powder diffraction (XRD), IR spectroscopy, and scanning electron microscopy (SEM). The Eu-doped oxysulfide was also characterized by atomic absorption spectrophotometry and luminescence spectroscopy. The spherical morphology of oxysulfide products and of basic carbonate precursors suggests a topotatic inter-relationship between both compounds.

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A polymeric precursor solution was employed in preparing SrBi2Nb2O9 (SBN) powder and thin films dip coated onto Si(100) substrate. XRD results show that the SBN perovskite phase forms at temperatures as low as 600°C through an intermediate fluorite phase. This fluorite phase is observed for samples heat-treated at temperatures of 400 and 500°C. After heat treatment at temperatures ranging from 300 to 800°C, thin films were shown to be crack free. Grazing incident angle XRD characterization shows the occurrence of the fluorite intermediate phase for films also. The thickness of films, measured by MEV, was in the order of 80-100 nm.

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The fac-[RuCl3(NO)(dppm)] (1) and cis-[RuCl2(dppm)2] (2) complexes were obtained with co-crystallization in the solid state from the reaction of RuCl3(NO) with the diphosphine in dichloromethane. mer-[RuCl3(NO)(dppb)] (3) was obtained from [RuCl3(dppb)(H2O)] by bubbling NO for 30 min in the same solvent. The crystal and molecular structures of these three compounds have been determined from X-ray studies. © Elsevier Science Ltd.

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The preparation and characterization of transparent glass-ceramics in the composition of 30Li2O:5ZrO2:xBaO:(100-x) SiO2 with x = 0, 5, 10, 15, and 20 mol% are described. Glasses were melted in a platinum crucible at 1100°C for 2 h and then heat-treated at 900°C for 3 h. The characterizations were performed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman and infrared spectroscopy, and scanning electron microscopy (SEM). The experimental results indicate that there was a structural change in the glass-ceramics as the BaO concentration in the mixture increased. In the XRD patterns of samples without heat treatment, only the halo was observed. After heat treatment, the appearance of the materials was verified by X-ray diffraction peaks. The reorganization of the amorphous solid was confirmed by Raman and IR spectroscopy along with XPS and SEM, with a more homogeneous phase formation being observed.

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Pure BBN powders and with addition of 1 and 2 wt% in excess of bismuth were obtained by Pechini Method. The powders calcined at 300°C/4h were analyzed by TG/DTA to study the temperature of organic matter decomposition. A systematic study of calcination temperature and time to the formation of the BBN phase was performed and the phase formation was accompanied by XRD. The calcined powders at 800°C during 2h were analyzed by infrared spectroscopy and by BET. The powders were isostaticaly pressed and sintered at temperatures ranging from 900°C to 1000°C. The ceramics were characterized by XRD to control the crystalline phase and by SEM to analyze the microstructure.

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The purpose of this work is to obtain spherical particles yttrium iron garnet (YIG) by coprecipitation technique. The spherical particles were obtained from either nitrate or chloride salt solutions by controlling the precipitation medium. Different agents of dispersion such as PVP and ammonium iron sulfate were used to optimize the shape and size of YIG. Samples were characterized by X-ray diffraction, scanning electron microscopy and vibrating sample magnetometry. The results show that the samples phase transition takes place at 850°C (orthorhombic phase) and at 1200°C (cubic phase). Spherical shape particles, with diameter of around 0.5 μm, present magnetization values close to the bulk value (26 emu g -1). © 2001 Elsevier Science B.V. All rights reserved.

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Arachis pintoi is an alternative to forage production in the tropics. Its germplasm comprises more than 150 accessions, that could be used to improve it. Our objective was the isolation and characterization of microsatellite loci in A. pintoi to be used to molecular evaluation of this germplasm and of A. repens (section Caulorrhizae). Seven loci were analyzed using five accessions of A. repens and 20 accessions of A. pintoi. The high variation found makes clear the high potential of this marker in genetic studies in these species. The developed markers showed total transferability to A. repens.

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Studies on firefly (Lampyridae) luciferases have focused on nearctic species of Photinus and Photuris and Euroasiatic species of Lampyris, Luciola, Hotaria, and Pyrocoelia. Despite accounting for the greatest diversity of fireflies in the world, no molecular studies have been carried out on the highly diverse genera from the neotropical region. Here we report the luciferase cDNA cloning for the larva of the Brazilian firefly Cratomorphus distinctus. The cDNA has 1978 bp and codes for a 547-residue-long polypeptide. Noteworthy, sequence comparison as well as functional properties show the highest degree of similarity with Lampyris noctiluca (93%) and Pyrocoelia spp. (91%) luciferases, suggesting a close phylogenetic relationship despite the geographical distance separating these species. The bioluminescence emission spectrum peaks at 550 nm and, as expected, is sensitive to pH, shifting to 605 nm at pH 6. The kinetic properties of the recombinant luciferase were similar to those of other firefly luciferases. © 2004 Elsevier Inc. All rights reserved.

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Poly(o-methylaniline) (poly-o-toluidine, PTOL) was synthesized by chemical oxidation of o-toluidine with ammonium peroxydisulfate in an aqueous 1.0 mol L -1 HCl solution. The progress of polymerization was followed by measuring the open-circuit potential (OCP) of a Pt electrode immersed in the reaction medium with the polymerization time. The chemical synthesis of PTOL was carried out at different monomer:oxidant (M:O) molar ratios (4:1, 2:1, 1.5:1, 1:1, and 0.66:1), and the products obtained were characterized by infrared spectroscopy, gel permeation chromatography, and X-ray diffraction. The molecular weight and percentage of crystallinity of PTOL are higher for samples synthesized in an excess of the monomer, i.e. at higher M:O ratios. However, the yield of PTOL prepared at higher M:O ratios is considerably low, in particular at a 4:1 M:O ratio, which is the M:O ratio most commonly used in the literature to synthesize polyaniline and its derivatives.