969 resultados para X-Ray Powder Diffraction
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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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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Atenolol is the most used drug in Brazil to hypertension treatment. Two crystal structures are known for this molecule: a racemic form (R,S)-atenolol and a pure form S-atenolol. The racemic form is found in commercial tablets. X-ray powder diffraction (XRD) is an adequate tool to study crystalline structures including drugs. Using the Rietveld Method with XRD data it is possible to quantify the crystalline structures existing in the raw material. Other methods like Le Bail and Pawley can be used to the profile fit and phases identification. For this work we analyzed three tablets of atenolol, two generics and the reference (materials were purchased from a drugstore at the city of Araraquara). These tablets were analyzed by Rietveld, Le Bail and Pawley methods. All tablets exhibited the racemic mixture API (R,S)-atenolol. Some crystalline excipients could be characterized: magnesium carbonate hydrate, lactose monohydrate and talc. The conclusion is that the three methods can be efficiently used to characterize the three atenolol tablets.
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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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The synthesis of calcium titanate, CaTiO3, was performed by mechanical activation and thermal treatment. Milling for up to 360 minutes in a planetary ball mill mechanically activated an equimolar mixture of CaCO 3 and TiO2 powders. A small amount of mechanically activated mixtures was pressed into briquettes and calcined at 850°C for two hours. The effect of mechanical activation on the solid-state reaction was studied using X-ray powder diffraction and differential thermal analysis. The change of morphology and size of powder particles due to milling, were determined by SEM, while BET analysis was used to determine the specific surface area of the powder. The sintering process was followed by a dilatometer during thermal treatment up to 1300°C. The main conclusion of the analysis of conducted investigations is that CaTiO3 ceramics can be obtained from an activated mixture at a much lower temperature than reported in the literature owing to acceleration of the chemical reaction and sintering.
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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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Crystallographic and microstructural properties of Ho(Ni,Co,Mn)O3± perovskite-type multiferroic material are reported. Samples were synthesized with a modified polymeric precursor method. The synchrotron X-ray powder diffraction (SXRPD) technique associated to Rietveld refinement method was used to perform structural characterization. The crystallographic structures, as well as microstructural properties, were studied to determine unit cell parameters and volume, angles and atomic positions, crystallite size and strain. X-ray energies below the absorption edges of the transition metals helped to determine the mean preferred atomic occupancy for the substituent atoms. Furthermore, analyzing the degree of distortion of the polyhedra centered at the transitions metal atoms led to understanding the structural model of the synthesized phase. X-ray photoelectron spectroscopy (XPS) was performed to evaluate the valence states of the elements, and the tolerance factor and oxygen content. The obtained results indicated a small decrease distortion in structure, close to the HoMnO3 basis compound. In addition, the substituent atoms showed the same distribution and, on average, preferentially occupied the center of the unit cell.
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Mejillonesite, ideally NaMg(2)(PO(3)OH)(PO(4))(OH)center dot H(5)O(2), is a new mineral approved by the CNMNC (IMA 2010-068). It occurs as isolated crystal aggregates in thin zones in fine-grained opal-zeolite aggregate on the north slope of Cerro Mejillones, Antofagasta, Chile. Closely associated minerals are bobierrite, opal, clinoptilolite-Na, clinoptilolite-K, and gypsum. Mejillonesite forms orthorhombic, prismatic, and elongated thick tabular crystals up to 6 mm long, usually intergrown in radiating aggregates. The dominant form is pinacoid {100}. Prisms {hk0}, {h0l}, and {0kl} are also observed. The crystals are colorless, their streak is white, and the luster is vitreous. The mineral is transparent. It is non-fluorescent under ultraviolet light. Mohs' hardness is 4, tenacity is brittle. Cleavage is perfect on {100}, good on {010} and {001}, and fracture is stepped. The measured density is 2.36(1) g/cm(3); the calculated density is 2.367 g/cm(3). Mejillonesite is biaxial (-), alpha= 1.507(2), beta= 1.531(2), gamma= 1.531(2), 2V(meas) = 15(10)degrees, 2V(calc) = 0 degrees (589 nm). Orientation is X= a, Z= elongation direction. The mineral is non-pleochroic. Dispersion is r> v, medium. The IR spectrum contains characteristic bands of the Zundel cation (H(5)O(2)(+), or H(+)center dot 2H(2)O) and the groups P-OH and OH(-). The chemical composition is (by EDS, H(2)O by the Alimarin method, wt%): Na(2)O 9.19, MgO 26.82, P(2)O(5) 46.87, H(2)O 19, total 101.88. The empirical formula, based on 11 oxygen atoms, is Na(0.93)Mg(2.08)(PO(3)OH)(1.00) (PO(4)) (OH)(0.86) .0.95H(5)O(2) The strongest eight X-ray powder-diffraction lines [d in angstrom(I)(hkl)] are: 8.095(100)(200), 6.846(9) (210), 6.470(8)(111), 3.317(5)(302), 2.959(5)(132), 2.706(12)(113), 2.157(19)(333), and 2.153(9) (622). The crystal structure was solved on a single crystal (R = 0.055) and gave the following data: orthorhombic, Pbca, a = 16.295(1), b = 13.009(2), c = 8.434(1) angstrom, V= 1787.9(4) angstrom(3), Z = 8. The crystal structure of mejillonesite is based on a sheet (parallel to the b-c plane) formed by two types of MgO(6) octahedra, isolated tetrahedra PO(4) and PO(3)OH whose apical vertices have different orientation with respect to the sheet. The sheets are connected by interlayer, 5-coordinated sodium ions, proton hydration complexes, and hydroxyl groups. The structure of mejillonesite is related to that of angarfite, NaFe(5)(3+)(PO(4))(4)(OH)(4).4H(2)O and bakhchisaraitsevite, Na(2)Mg(5)(PO(4))(4)center dot 7H(2)O.
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We report a systematic study on the influence of the synthesis routes on the structural and magnetic properties of polycrystalline PrxY1-xBa2Cu3O7-delta. We have prepared high-quality samples of this material by following a sol-gel method based on heat treatment in both inert argon and oxygen atmospheres in order to compare their effect on the formation of the superconducting phase using X-ray powder diffraction. Magnetic measurements (DC and AC susceptibility) clearly demonstrate that, for the same concentration of Pr, the superconducting transition temperature markedly increases in all samples prepared in argon atmosphere, including pure Pr-123. (C) 2012 Elsevier B.V. All rights reserved.