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Parametric Rietveld refinement of coexisting disordered clay minerals

Published online by Cambridge University Press:  02 January 2018

K. Ufer  and
R. Kleeberg
K. Ufer*
Affiliation:
BGR, Bundesanstalt für Geowissenschaften und Rohstoffe, Stilleweg 2, D-30655 Hannover, Germany
R. Kleeberg
Affiliation:
TU Bergakademie Freiberg, Institute of Mineralogy, 09596 Freiberg, Germany
*
*Email: Kristian.ufer@bgr.de
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Abstract

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X-ray diffraction is one of the most effective tools for the characterization of the stacking defects which occur frequently in clay minerals. Modelling of the diffraction patterns of oriented mounts is often used for obtaining structural information about the nature of stacking order. Manual matching of calculated and observed patterns is time consuming and the results are user dependent and especially troublesome if a consistent model of the same mineral measured under different conditions needs to be obtained. It was shown recently that the Rietveld method could be applied successfully for the evaluation of the X-ray patterns of oriented mounts. Nevertheless, this automatic refinement procedure can also lead to inconsistent results if independent refinements are performed that describe the same sample measured under different conditions. One way to solve this problem is the application of parametric Rietveld refinement. For this approach a set of different measurements of the same sample was collected and fitted in one combined refinement by the connection of the structural models via external parameters. These conditions may involve different pre-treatments (e.g. different intercalations), different temperatures or relative humidities and/or different experimental setup (powder or oriented samples). All patterns were fitted in one overall refinement process by the BGMN software.

This approach was demonstrated on a mixture of two disordered reference materials and on a set of geological samples. Two different states for each sample were refined independently and parametrically and it was shown that this approach leads to consistent results, saves computation time and may even resolve small structural differences.

Keywords

Rietveld methodstacking disorderparametric refinementBGMN
Type
Research Article
Information
Clay Minerals , Volume 50 , Issue 3 , August 2015 , pp. 287 - 296
Creative Commons
Creative Common License - CCCreative Common License - BY
Copyright © The Mineralogical Society of Great Britain and Ireland 2015 This is an Open Access article, distributed under the terms of the Creative Commons Attribution license. (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted re-use, distribution, and reproduction in any medium, provided the original work is properly cited.
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2015

References

Bergmann, J., Friedel, P. & Kleeberg, R. (1998) BGMN -a new fundamental parameter based Rietveld program for laboratory X-ray sources, its use in quantitative analysis and structure investigations. CPD Newsletter, Commission of Powder Diffraction, International Union of Crystallography, 20, 5–8.Google Scholar
Bethke, C.M., Vergo, N. & Altaner, S.P. (1986) Pathways of smectite illitization. Clays and Clay Minerals, 34, 125–135.10.1346/CCMN.1986.0340203Google Scholar
Drits, V.A. & Tchoubar, C. (1990) X-ray Diffraction by Disordered Lamellar Structures. Springer, Berlin Heidelberg, 37 Pp.10.1007/978-3-642-74802-8CrossRefGoogle Scholar
Heuser, M., Andrieux, P., Petit, S. & Stanjek, H. (2013) Iron-bearing smectites: a revised relationship between structural Fe, b cell edge lengths and refractive indices. Clay Minerals, 48, 97–103.10.1180/claymin.2013.048.4.06Google Scholar
Rajiv, P., Dinnebier, R.E., Jansen, M. & Joswig, M. (2011) Automated parametric Rietveld refinement: Applications in reaction kinetics and in the extraction of micro structural information. Powder Diffraction Supplement, 26, (S1), S26'-37.Google Scholar
Reynolds, R.C. Jr. (1983) Calculation of absolute diffraction intensities for mixed-layered clays. Clays and Clay Minerals, 31, 233–234.10.1346/CCMN.1983.0310310Google Scholar
Reynolds, R.C. Jr. (1985) NEWMOD© a computer program for the calculation of one-dimensional diffraction patterns of mixed-layered clays. R.C. Reynolds, Jr., 8 Brook Rd., Hanover, NH, USA.Google Scholar
Sakharov, B.A., Lindgreen, H., Salyn, A., and Drits, V.A. (1999) Determination of illite-smectite structures using multispecimen X-ray diffraction profile fitting. Clays and Clay Minerals, 47, 555–566.10.1346/CCMN.1999.0470502Google Scholar
Stinton, G.W. & Evans, J.S.O. (2007) Parametric Rietveld refinement. Journal of Applied Crystallography, 40, 87–95.10.1107/S0021889806043275Google Scholar
Treacy, M.M.J., Newsam, J.M. & Deem, M.W. (1991) A general recursion method for calculating diffracted intensities from crystals containing planar faults. Proceedings of the Royal Society, London, A433, 499–520.10.1098/rspa.1991.0062Google Scholar
Ufer, K., Kleeberg, R., Bergmann, J., Curtius, H. & Dohrmann, R. (2008) Refining real structure parameters of disordered layer structures within the Rietveld method. Zeitschrift für Kristallographie, 27, 151–158.10.1524/zksu.2008.0020Google Scholar
Ufer, K., Kleeberg, R., Bergmann, J. & Dohrmann, R. (2012) Rietveld refinement of disordered illite-smectite mixed-layer structures by a recursive algorithm — I: One-dimensional patterns. Clays and Clay Minerals, 60, 507–534.10.1346/CCMN.2012.0600507Google Scholar