997 resultados para X-ray powder diffractometry


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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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

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Solid-state compounds of general formula LnL3.nH2O, in wich Ln represents lanthanum, lanthanides and yttrium, L is ketoprofen, and n = 0,5 (Pr, Sm, Tb), 1 (La, Eu, Dy, Ho, Er, Tm, Lu) e 1,5 (Ce, Nd, Gd, Yb, Y) were synthesized. Simultaneous thermogravimetry-differential analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and EDTA complexometry were employed to characterize these compounds. The TG-DTA and DSC curves provided information concerning the thermal behaviour and thermal decomposition of synthesized compounds. The experimental and theoretical infrared spectroscopic data suggested that ketoprofen acts as a bidentate ligand towards trivalent lanthanides and yttrium (III)

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Solid state Ln-4-Me-BP compounds, where Ln stands for heavier trivalent lanthanides (gadolinium to lutetium) and yttrium(III) and 4-Me-BP is 4-methylbenzylidenepyruvate (CH3-C6H4-CH=CH-COCOO-), have been synthesized. Elemental analysis, complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA), have been used to characterise and to study the thermal behaviour of these compounds. The results provided information concerning the stoichiometry, crystallinity, ligand's denticity, thermal stability and thermal decomposition. © 2002 Elsevier Science B.V. All rights reserved.

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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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Solid-state LnL(3) compounds, where L is 2-metboxybenzoate and Ln is light trivalent lanthanides, have been synthesized. Thermogravimetry (TG), differential scanning calorimetty (DSC), X-ray powder diffractometry, infrared spectroscopy and elementary analysis were used to characterize and to study the thermal behaviour of these compounds. The results led to information on the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds. on heating these complexes decompose in three (Ce, Pr) or five (La, Nd, Sm) steps with the formation of the respective oxide: CeO2, Pr6O11 and Ln(2)O(3) (Ln=La, Nd, Sm) as final residues. The theoretical and experimental spectroscopic study suggests predominantly the ionic bond between the ligand and metallic center.

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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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Starch is one of the most important sources of reserve of carbohydrate in plants and the main source in the human diet due to its abundance in the nature. There no other food ingredient that can be compared with starch in terms of sheer versatility of application in the food industry. Unprocessed native starches are structurally too weak and functionally too restricted for application in today’s advanced food and industrial technologies. The main objective of this study was to compare the thermal behavior of native cassava starch and those treated with hydrogen peroxide, as well as those treated with hydrogen peroxide and ferrous sulfate. The cassava starch was extracted from cassava roots (Manihot esculenta, Crantz) and treated by standardized hydrogen peroxide (H2 O2 ) solutions at 1, 2 and 3% (with or without FeSO4 ). Investigated by using they are thermoanalytical techniques: thermogravimetry - TG, differential thermal analysis – DTA and differential scanning calorimetry - DSC, as well as optical microscopy and X-ray powder diffractometry. The results showed the steps of thermal decomposition, changes in temperatures and in gelatinization enthalpy and small changes in crystallinity of the granules.

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A robust, direct, rapid and non-destructive X-ray diffraction crystallography method to detect the polyprenylated benzophenones 7-epi-clusianone (1) and guttiferone A (2) in extracts from Garcinia brasiliensis is presented. Powder samples of benzophenones 1 and 2, dried hexane extracts from G. brasiliensis seeds and fruit`s pericarp, and the dried ethanolic extract from G. brasiliensis seeds were unambiguously characterized by powder X-ray diffractometry. The calculated X-ray diffraction peaks from crystal structures of analytes 1 and 2, previously determined by single-crystal X-ray diffraction technique, were overlaid to those of the experimental powder diffractograms, providing a practical identification of these compounds in the analyzed material and confirming the pure contents of the powder samples. Using the X-ray diffraction crystallography method, the studied polyprenylated benzophenones were selectively and simultaneously detected in the extracts which were mounted directly on sample holder. In addition, reference materials of the analytes were not required for analyses since the crystal structures of the compounds are known. High performance liquid chromatography analyses also were comparatively carried out to quantify the analytes in the same plant extracts showing to be in agreement with X-ray diffraction crystallography method. (C) 2010 Elsevier B.V. All rights reserved.