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Separation of Effects due to Superimposition Using the Rietveld Method in Spectra Obtained by WDXRF

Journal Materials Science Forum (Volumes 530 - 531)
Volume Advanced Powder Technology V
Edited by Lucio Salgado and Francisco Ambrozio Filho
Pages 59-64
DOI 10.4028/www.scientific.net/MSF.530-531.59
Citation V.L.R. Salvador et al., 2006, Materials Science Forum, 530-531, 59
Online since November, 2006
Authors V.L.R. Salvador, Nelson Batista de Lima
Keywords GSAS, Rietveld, WDXRF
Abstract

This paper presents a new method to separate interfering spectra obtained in wavelength dispersive x-ray fluorescence spectrometry (WDXRF). This method permits improved results to be obtained, compared to conventional analytical results and enables the determination of chemical species of the same element without chemical separation. This is done by separation of the spectra due to electronic transitions of the valence electrons. The Rietveld method [11] overcomes the problem of superimposed peaks of the species present in the specimen and simultaneously enables determination of the species and does not require standard specimens and calibration curves. This signifies a marked improvement in comparison to other techniques. Specimen surface preparation to obtain spectra is a critical stage and its effects can be minimized by using Rietveld refinement, which permits the determination of intensity relationships of superimposed peaks with the aid of mathematical models. This establishes the basic conditions to obtain more accurate results in quantitative analysis. In the determination of chemical species, it is possible to separate, for example, Cr (III) and Cr (IV), with almost 100% superimposition.

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