Mineralogical characterization of a highly-weathered soil by the Rietveld Method

The mineralogical characterization through mineral quantification of Brazilian soils by X-ray diffraction data using the Rietveld Method is not common. A mineralogical quantification of an Acric Ferralsol from the Ponta Grossa region, state of Paraná, Brazil, was carried out using this Method with X-Ray Diffraction data to verify if this method was suitable for mineral quantification of a highly-weathered soil. The A, AB and B3 horizons were fractioned to separate the different particle sizes: clay, silt, fine sand (by Stokes Law) and coarse sand fractions (by sieving), with the procedure free of chemical treatments. X-ray Fluorescence, Inductively Coupled Plasma Atomic Emission Spectrometry, Infrared Spectroscopy and Mössbauer Spectroscopy were used in order to assist the mineral identification and quantification. The Rietveld Method enabled the quantification of the present minerals. In a general way, the quantitative mineralogical characterization by the Rietveld Method revealed that quartz, gibbsite, rutile, hematite, goethite, kaolinite and halloysite were present in the clay and silt fractions of all horizons. The silt fractions of the deeper horizons were different from the more superficial ones due to the presence of large amounts of quartz. The fine and the coarse sand fractions are constituted mainly by quartz. Therefore, a mineralogical quantification of the finer fraction (clay and silt) by the Rietveld Method was successful.

Applications of the Rietveld method to quantify the crystalline phases of Portland cement clinker doped with nickel and chromium

The effects of chromium or nickel oxide additions on the composition of Portland clinker were investigated by X-ray powder diffraction associated with pattern analysis by the Rietveld method. The co-processing of industrial waste in Portland cement plants is an alternative solution to the problem of final disposal of hazardous waste. Industrial waste containing chromium or nickel is hazardous and is difficult to dispose of. It was observed that in concentrations up to 1% in mass, the chromium or nickel oxide additions do not cause significant alterations in Portland clinker composition. (C) 2008 International Centre for Diffraction Data.

Quantitative analysis of aluminum dross by the Rietveld method

Aluminum white dross is a valuable material principally due to its high metallic aluminum content. The aim of this work is to develop a method for quantitative analysis of aluminum white dross with high accuracy. Initially, the material was separated into four granulometric fractions by means of screening. Two samples of each fraction were obtained, which were analyzed by means of X-ray fluorescence and energy dispersive spectroscopy in order to determine the elements present in the samples. The crystalline phases aluminum, corundum, spinel, defect spinel, diaoyudaoite, aluminum nitride, silicon and quartz low were identified by X-ray diffraction. The quantitative phase analysis was performed by fitting the X-ray diffraction profile with the Rietveld method using the GSAS software. The following quantitative results were found: 77.8% aluminum, 7.3% corundum, 2.6% spinel, 7.6% defect spinel, 1.8% diaoyudaoite, 2.9% aluminum nitride, and values not significant of quartz and silicon.

Structural characterization of Ti-15Mo alloy used as biomaterial by Rietveld method

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Quantitative structural analysis of the transition from LT-LixCoO2 to HT-LixCoO2 using the rietveld method: correlation between structure and electrochemical performance

A quantitative phase analysis was made of LiXCoO2 powders obtained by two distinct chemical methodologies at different temperatures (from 400 to 700degreesC). A phase analysis was made using Rietveld refinements based on X-ray diffraction data, considering the LiXCoO2 powders as a multiphase system that simultaneously contained two main phases with distinct, layered and spinel-type structures. The sults showed the coexistence of both structures in LiXCoO2 obtained at low temperature (400 and 500degreesC), although only the layered structure was detected at higher temperatures (600 and 700degreesC, regardless of the chemical powder process employed. The electrochemical performance, evaluated mainly by the cycling reversibility of LiXCoO2 in the form of cathode insertion electrodes, revealed that there is a close correlation between structural features and the electrochemical response, with one of the redox processes (3.3 v/3.9 v) associated only with the presence of the spinel-type structure. (C) 2003 Elsevier B.V. All rights reserved.

Quantitative Phase Analyses Through The Rietveld Method with X-Ray Powder Diffraction Data of Heat-Treated Carbamazepine Form III

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

Quantitative structural analysis of the transition from LT-Li xCoO2 to HT-LixCoO2 using the rietveld method: Correlation between structure and electrochemical performance

A quantitative phase analysis was made of LixCoO2 powders obtained by two distinct chemical methodologies at different temperatures (from 400 to 700°C). A phase analysis was made using Rietveld refinements based on X-ray diffraction data, considering the Li xCoO2 powders as a multiphase system that simultaneously contained two main phases with distinct, layered and spinel-type structures. The results showed the coexistence of both structures in LixCoO 2 obtained at low temperature (400 and 500°C), although only the layered structure was detected at higher temperatures (600 and 700°C), regardless of the chemical powder process employed. The electrochemical performance, evaluated mainly by the cycling reversibility of Li xCoO2 in the form of cathode insertion electrodes, revealed that there is a close correlation between structural features and the electrochemical response, with one of the redox processes (3.3 v/3.9 v) associated only with the presence of the spinel-type structure. © 2003 Elsevier B.V. All rights reserved.

Evaluation via multivariate techniques of scale factor variability in the rietveld method applied to quantitative phase analysis with X ray powder diffraction

ABSTRACT: The present work uses multivariate statistical analysis as a form of establishing the main sources of error in the Quantitative Phase Analysis (QPA) using the Rietveld method. The quantitative determination of crystalline phases using x ray powder diffraction is a complex measurement process whose results are influenced by several factors. Ternary mixtures of Al2O3, MgO and NiO were prepared under controlled conditions and the diffractions were obtained using the Bragg-Brentano geometric arrangement. It was possible to establish four sources of critical variations: the experimental absorption and the scale factor of NiO, which is the phase with the greatest linear absorption coefficient of the ternary mixture; the instrumental characteristics represented by mechanical errors of the goniometer and sample displacement; the other two phases (Al2O3 and MgO); and the temperature and relative humidity of the air in the laboratory. The error sources excessively impair the QPA with the Rietveld method. Therefore it becomes necessary to control them during the measurement procedure.

Lanthanum-doped Bi4Ti3O12 prepared by the soft chemical method: Rietveld analysis and piezoelectric properties

Bi4-xLaxTi3O12 (BLT) thin films and powders with x ranging from 0 to 0.75 were prepared by the polymeric precursor solution. The effect of lanthanum on the structure of BIT powders was investigated by Rietveld Method. The increase of lanthanum content does not lead to any secondary phases. Orthorhombicity of the bismuth titanate (BIT) crystal lattice decreased with the increase of lanthanum content due the reduction of a/b ratio. The BLT films show piezoelectric coefficients of 45, 19, 16 and 10 pm/V for x = 0, 0.25, 0.50 and 0.75, respectively. The piezoelectric response is strongly reduced by the amount of lanthanum added to the system. (c) 2006 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Synthesis and crystal phase evaluation of hydroxylapatite using the rietveld-maximum entropy method

Bioceramic systems based on hydroxylapatite (HAP) are an important class of bioactive materials that may promote bone regeneration. The aim of this research was to evaluate how the stoichiometry of HAP influences its microstructural properties when diagnosed using the combined Rietveld method and Maximum entropy method (MEM). The Rietveld Method (RM) is recognizably a powerful tool used to obtain structural and microstructural information of polycrystalline samples analyzed by x-ray diffraction. Latterly have combined the RM with the maximum entropy method (MEM), with the goal of improve structural refinement results. The MEM provides high resolution maps of electron density and their analysis leave the accurate localization of atoms inside of unit cell. Like that, cycles Rietveld-MEM allow an excellent structural refinement In this work, a hydroxylapatite sample obtained by emulsion method had its structure refined using one cycle Rietveld-MEM with x-ray diffraction data. The indices obtained in initial refinement was Rwp = 7.50%, Re = 6.56%, S - 1.14% e RB = 1.03%. After MEM refinement and electron densities maps analysis to correction of atomics positions, the news indicators of Rietveld refinement quality was Rwp = 7.35%, Re = 6.56%, S = 1.12% and RB = 0.75%. The excellent result obtained to RB shows the efficiency of MEM as auxiliary in the refinement of structure of hydroxylapatite by RM.

Quantificação de Fases Cristalinas de Incrustações em Colunas de Produção de Petróleo pelo Método Rietveld

The scale is defined as chemical compounds from inorganic nature, initially soluble in salt solutions, which may precipitate accumulate in columns of production and surface equipment. This work aimd to quantify the crystalline phases of scale through the Rietveld method. The study was conducted in scale derived from columns production wells in development and recipients of pigs. After collecting samples of scale were performed the procedure for separations of inorganic and organic phase and preparation to be analyzed at the X-ray Laboratory. The XRD and XRF techniques were used to monitor whether identifying and quantifying crystalline phases present in the deposits. The SEM technique was used to visualize the morphology of the scales and assess their homogeneity after the milling process. XRD measurements were performed with and without milling and with or without the accessory spinner. For quantify crystalline phases the program DBWStools was used. The procedure for conducting the first refinement was instrumental in setting parameters, then the structural parameters of the phases in the sample and finally the parameters of the function profile used. In the diffraction patterns of samples of scale observed that the best measures were those that passed through the mill and used the accessory spinner. Through the results, it was noted that the quantitative analysis for samples of scale is feasible when need to monitor a particular crystalline phase in a well, pipeline or oil field. Routinely, the quantification of phases by the Rietveld method is hardwork because in many scale was very difficult to identify the crystalline phases present

Structural characterization of phase transition of Al2O3 nanopowders obtained by polymeric precursor method

Nanocrystalline Al(2)O(3)powders have been synthesized by the polymeric precursor method. A study of the evolution of crystalline phases of obtained powders was accomplished through X-ray diffraction, micro-Raman spectroscopy and refinement of the structures through the Rietveld method. The results obtained allow the identification of three steps on the gamma-Al2O3 to alpha-Al2O3 phase transition. The single-phase alpha-Al2O3 Powder was obtained after heat-treatment at 1050 degrees C for 2 h. A study of the morphology of the particles was accomplished through measures of crystallite size, specific surface area and transmission electronic microscopy. The particle size is closely related to gamma-Al2O3 to alpha-Al2O3 phase transition. (c) 2007 Elsevier B.V. All rights reserved.

Correlation between the spectroscopic and structural properties with the occupation of Eu3+ sites in powdered Eu3+-doped LiTaO3 prepared by the Pechini method

In this work we studied the structural and optical properties of lithium tantalate (LiTaO3) powders doped with Eu3+ ions. We have examined the different sites occupied by the rare earth ion through the correlation of the DRX data analyzed with the Rietveld method and some spectroscopic parameters derived from the Eu3+ luminescence. Adirect relation was established between the lattice parameters and the occupation fraction of Eu3+ in each LiTaO3 site. The occupation fraction was set as the relative population of Eu3+ ions for each site obtained by means of the intensity, baricenter, and the spontaneous emission coefficients of the D-5(0)-> F-7(0) transitions. We concluded that the unit cell parameter a presents the same behavior of the Eu3+ occupation fraction in Ta5+ sites as a function of the Eu3+ content in LiTaO3. The same was observed for the variation in Eu3+ occupation fraction in the Li+ site and the unit cell parameter c with the Eu3+ content. (C) 2009 American Institute of Physics. [doi: 10.1063/1.3204967]

Caracterização estrutural da cerâmica Ti x(Sm0,2Ce0,8)1-xO 2-delta pelo método de Rietveld

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