Hostname: page-component-78c5997874-dh8gc Total loading time: 0 Render date: 2024-11-15T23:46:26.977Z Has data issue: false hasContentIssue false

Quantitative phase analysis of bentonites by the rietveld method

Published online by Cambridge University Press:  01 January 2024

K. Ufer*
Affiliation:
TU Bergakademie Freiberg, Institute of Mineralogy, 09596 Freiberg, Germany
H. Stanjek
Affiliation:
Clay and Interface Mineralogy, RWTH Aachen University, 52056 Aachen, Germany
G. Roth
Affiliation:
Institute of Crystallography, RWTH Aachen University, 52056 Aachen, Germany
R. Dohrmann
Affiliation:
BGR/LBEG, 30655 Hannover, Germany
S. Kaufhold
Affiliation:
BGR/LBEG, 30655 Hannover, Germany
*
* E-mail address of corresponding author: kristian.ufer@bgr.de
Rights & Permissions [Opens in a new window]

Abstract

Core share and HTML view are not available for this content. However, as you have access to this content, a full PDF is available via the ‘Save PDF’ action button.

Thirty six bentonite samples from 16 different locations were examined in order to demonstrate the applicability of a new Rietveld description approach for quantitative phase analysis. X-ray diffraction patterns of the bulk material were obtained and analyzed by the Rietveld method. The samples contain up to ten different minerals, with dioctahedral smectite as the major component. A model for turbostratic disorder of smectites was formulated inside a structure-description file of the Rietveld program BGMN. The quality of the refinements was checked using an internal standard mineral (10.0 or 20.0 wt.% corundum) and by cross-checking results with X-ray fluorescence (XRF) data. The corundum content was reproduced with only small deviations from the nominal values. A comparison of the chemical composition obtained by XRF and the composition as re-calculated from quantitative Rietveld results shows a satisfactory agreement, although X-ray amorphous components such as volcanic glasses were not considered. As a result of this study, the Rietveld method combined with the new structure model for turbostratic disorder has proven to be a suitable method for routine quantitative analysis of bentonites with smectites as the dominant clay minerals.

Type
Research Article
Copyright
Copyright © 2008, The Clay Minerals Society

References

Bergmann, J. and Kleeberg, R., 1998 Rietveld analysis of disordered layer silicates Materials Science Forum 278–281 300305 10.4028/www.scientific.net/MSF.278-281.300.CrossRefGoogle Scholar
Bergmann, J. Friedel, P. and Kleeberg, R., 1998 BGMN — a new fundamental parameter based Rietveld program for laboratory X-ray sources, its use in quantitative analysis and structure investigations Commission of Powder Diffraction. International Union of Crystallography, CPD Newsletter 20 58.Google Scholar
Biscoe, J. and Warren, B.E., 1942 An X-ray study of carbon black Journal of Applied Physics 13 364371 10.1063/1.1714879.CrossRefGoogle Scholar
Bish, D.L. and Post, J.E., 1993 Quantitative mineralogical analysis using the Rietveld full-pattern fitting method American Mineralogist 78 932940.Google Scholar
Cheary, R.W. and Coelho, A.A., 1992 A fundamental parameters approach to X-ray line-profile fitting Journal of Applied Crystallography 25 109121 10.1107/S0021889891010804.CrossRefGoogle Scholar
Dohrmann, R., 2006 Cation exchange capacity methodology I: An efficient model for the detection of incorrect cation exchange capacity and exchangeable cation results Applied Clay Science 34 3137 10.1016/j.clay.2005.12.006.CrossRefGoogle Scholar
Drits, V.A. and Tchoubar, C., 1990 X-ray Diffraction by Disordered Lamellar Structures New York Springer Verlag 10.1007/978-3-642-74802-8 371 pp.CrossRefGoogle Scholar
Herrmann, W. and Berry, R.F., 2002 MINSQ — a least squares spreadsheet method for calculating mineral proportions from whole rock major element analyses Geochemistry: Exploration, Environment, Analysis 2 361368.Google Scholar
Hillier, S., 1999 Use of an air-brush to spray dry samples for X-ray powder diffraction Clay Minerals 34 127135 10.1180/000985599545984.CrossRefGoogle Scholar
Kahr, G., Henning, K.-H. and Kasbohm, J., 1998 Methoden zur Bestimmung des Smektitgehaltes von Bentoniten Berichte der DTTG Greifswald, Germany DTTG 163172.Google Scholar
Kahr, G. Meier, L.P., Wolf, D. Starke, R. and Kleeberg, R., 1996 Einfache Bestimmungsmethode des Kationenaustauschvermögens von Tonen mit Komplexverbindungen des Kupfer(II)-Ions mit Triethylentetramin und Tetraethylenpentamin Berichte der DTTG Freiberg, Germany DTTG 122126.Google Scholar
Kaufhold, S. Dohrmann, R. Ufer, K. and Meyer, F.M., 2002 Comparison of methods for the quantification of montmorillonite in bentonites Applied Clay Science 22 145151 10.1016/S0169-1317(02)00131-X.CrossRefGoogle Scholar
Kleeberg, R., 2004 Results of the second Reynolds Cup contest in quantitative mineral analysis Commission of Powder Diffraction, International Union of Crystallography CPD Newsletter 30 2224.Google Scholar
Monecke, T. Köhler, S. Kleeberg, R. Herzig, P. and Gemmell, J.B., 2001 Quantitative phase-analysis by the Rietveld method using X-ray powder-diffraction data: Application to the study of alteration halos associated with volcanic-rock-hosted massive sulfide deposits The Canadian Mineralogist 39 16171633 10.2113/gscanmin.39.6.1617.CrossRefGoogle Scholar
Moore, D.M. and Reynolds, R.C. Jr., 1997 X-ray Diffraction and the Identification and Analysis of Clay Minerals 2 New York Oxford University Press 332 pp.Google Scholar
Omotoso, O. McCarty, D.K. Hillier, S. and Kleeberg, R., 2006 Some successful approaches to quantitative mineral analysis as revealed by the 3rd Reynolds contest Clays and Clay Minerals 54 748760 10.1346/CCMN.2006.0540609.CrossRefGoogle Scholar
Reynolds, R.C., 1989 Principles and techniques of quantitative analysis of clay minerals by X-ray powder diffraction Quantitative Mineral Analysis of Clays 1 437.Google Scholar
Rietveld, H.M., 1967 Line profiles of neutron powder-diffraction peaks for structure refinement Acta Crystallographica 22 151152 10.1107/S0365110X67000234.CrossRefGoogle Scholar
Snyder, R.L. Bish, D.L., Bish, D.J. and Post, J.E., 1989 Quantitative analysis Modern Powder Diffraction Washington, D.C Mineralogical Society of America 101144 10.1515/9781501509018-008.CrossRefGoogle Scholar
Srodon, J. Drits, V.A. McCarty, D.K. Hsieh, J.C.C. and Eberl, D.D., 2001 Quantitative X-ray diffraction analysis of clay-bearing rocks from random preparations Clays and Clay Minerals 49 514528 10.1346/CCMN.2001.0490604.CrossRefGoogle Scholar
Taylor, J.C. and Matulis, C.E., 1994 A new method for Rietveld clay analysis. Part I. Use of a universal measured standard profile for Rietveld quantification of montmorillonites Powder Diffraction 9 119123 10.1017/S0885715600014093.CrossRefGoogle Scholar
Treacy, M.M.J. Newsam, J.M. and Deem, M.W., 1991 A general recursion method for calculating diffracted intensities from crystals containing planar faults Proceedings of the Royal Society, London A433 499520 10.1098/rspa.1991.0062.Google Scholar
Tsipursky, S.I. and Drits, V.A., 1984 The distribution of octahedral cations in the 2:1 layers of dioctahedral smectites studied by oblique texture electron diffraction Clay Minerals 19 177192 10.1180/claymin.1984.019.2.05.CrossRefGoogle Scholar
Ufer, K. Roth, G. Kleeberg, R. Stanjek, H. Dohrmann, R. and Bergmann, J., 2004 Description of X-ray powder pattern of turbostratically disordered layer structures with a Rietveld compatible approach Zeitschrift für Kristallographie 219 519527.CrossRefGoogle Scholar
Viani, A. Gualtieri, A.F. and Artioli, G., 2002 The nature of disorder in montmorillonite by simulation of X-ray powder patterns American Mineralogist 87 966975 10.2138/am-2002-0720.CrossRefGoogle Scholar
Ward, C.R. and Gómez-Fernández, F., 2003 Quantitative mineralogical analysis of Spanish roofing slates using the Rietveld method and X-ray powder diffraction data European Journal of Mineralogy 15 10511062 10.1127/0935-1221/2003/0015-1051.CrossRefGoogle Scholar
Warren, B.E., 1941 X-ray diffraction in random layer lattices Physical Reviews 59 693698 10.1103/PhysRev.59.693.CrossRefGoogle Scholar
Yang, D. and Frindt, R.F., 1996 Powder X-ray diffraction of turbostratically stacked layer systems Journal of Materials Research 11 17331738 10.1557/JMR.1996.0217.CrossRefGoogle Scholar
Zhang, G. Germaine, J.T. Martin, R.T. and Whittle, A.J., 2003 A simple sample-mounting method for random powder X-ray diffraction Clays and Clay Minerals 51 218225 10.1346/CCMN.2003.0510212.CrossRefGoogle Scholar