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Preferred orientation of mineral grains in sample mounts for quantitative XRD measurements: How random are powder samples?

Published online by Cambridge University Press:  01 January 2024

Reinhard Kleeberg ,
Thomas Monecke  and
Stephen Hillier
Reinhard Kleeberg*
Affiliation:
TU Bergakademie Freiberg, Institute of Mineralogy, Brennhausgasse 14, D-09596 Freiberg, Germany
Thomas Monecke
Affiliation:
Department of Earth Sciences, University of Ottawa, Marion Hall, 140 Louis Pasteur, Ottawa, Ontario, K1N 6N5, Canada
Stephen Hillier
Affiliation:
Macaulay Institute, Craigiebuckler, Aberdeen AB15 8QH, UK
*
* E-mail address of corresponding author: kleeberg@mineral.tu-freiberg.de
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Abstract

The degree of preferred orientation of mineral grains in powder X-ray diffraction (XRD) samples prepared by standard techniques has been evaluated by means of a correction model implemented in the Rietveld program, BGMN. It is demonstrated that neither front- nor side-loading of mineral powders obtained by wet grinding in a McCrone micronizing mill yield powder mounts with randomly oriented particles. Despite fine grinding, the primary sizes and shapes of mineral grains contained in multi-phase samples influence the degree of preferred orientation in XRD powder mounts. Two minerals, both of platy habit, were found to show different degrees of preferred orientation in front- and side-loaded samples. In contrast to these methods of sample preparation, the spray-drying technique yielded perfect randomness of the particles. The experiments on artificial mineral mixtures demonstrate that the model applied can effectively correct for preferred orientation allowing reliable Rietveld quantitative phase analysis of moderately textured samples prepared by standard techniques.

Keywords

Correction of Preferred OrientationQuantitative Phase AnalysisRandom PowderRietveld MethodSample PreparationX-ray Diffraction
Type
Article
Information
Clays and Clay Minerals , Volume 56 , Issue 4 , August 2008 , pp. 404 - 415
Copyright
Copyright © 2008, The Clay Minerals Society

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References

Bergmann, J. and Kleeberg, R., 1998 Rietveld analysis of disordered layer silicates Materials Science Forum> 278–281 300–305 10.4028/www.scientific.net/MSF.278-281.300.CrossRefGoogle Scholar
Bergmann, J. Friedel, P. and Kleeberg, R., 1998 BGMN — a new fundamental parameters 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 5–8.Google Scholar
Bergmann, J. Monecke, T. and Kleeberg, R., 2001 Alternative algorithm for the correction of preferred orientation in Rietveld analysis Journal of Applied Crystallography> 34 16–19 10.1107/S002188980001623X.CrossRefGoogle Scholar
Bish, D.L. Reynolds, R.C. Jr., Bish, D.L. and Post, J.E., 1989 Sample preparation for X-ray diffraction Modern Powder Diffraction Washington, D.C Mineralogical Society of America 73–99 10.1515/9781501509018-007.CrossRefGoogle Scholar
Blount, A.M. and Vassiliou, A.H., 1979 A new method of reducing preferred orientation in diffractometer samples American Mineralogist> 64 922–924.Google Scholar
Brindley, G.W. and Kurtossy, S.S., 1961 Quantitative determination of kaolinite by X-ray diffraction American Mineralogist> 46 1205–1215.Google Scholar
Cheetham, A.K. Fender, B.E.F. and Cooper, M.J., 1971 Defect structure of calcium fluoride containing excess anions: I. Bragg scattering Journal of Physics C> 4 3107–3121 10.1088/0022-3719/4/18/016.CrossRefGoogle Scholar
Dermatas, D. Chrysochoou, M. Pardali, S. and Grubb, D.G., 2007 Influence of X-ray diffraction sample preparation on quantitative mineralogy: Implications for Chromate waste treatment Journal of Environmental Quality> 36 487–497 10.2134/jeq2006.0215.CrossRefGoogle ScholarPubMed
v. Engelhardt, W., 1955 Über die Möglichkeit der quantitativen Phasenanalyse von Tonen mit Röntgenstrahlen Zeitschrift für Kristallographie> 106 430–459.Google Scholar
Ferrari, M. and Lutterotti, L., 1994 Method for the simultaneous determination of anisotropic residual stresses and texture by X-ray diffraction Journal of Applied Physics> 76 7246–7255 10.1063/1.358006.CrossRefGoogle Scholar
Flörke, O.W. and Saalfeld, H., 1955 Ein Verfahren zur Herstellung texturfreier Röntgen-Pulverpräparate Zeitschrift für Kristallographie> 106 460–466.Google Scholar
Güven, N., 1971 The crystal structures of 2M 1 phengite and 2M 1 muscovite Zeitschrift für Kristallographie> 134 196–212.Google Scholar
Hillier, S., 1999 Use of an air brush to spray dry samples for X-ray powder diffraction Clay Minerals> 34 127–135 10.1180/000985599545984.CrossRefGoogle Scholar
Hillier, S., 2003 Quantitative analysis of clay and other minerals in sandstones by X-ray powder diffraction (XRPD) 213–251.CrossRefGoogle Scholar
Hughes, R. and Bohor, B., 1970 Random clay powders prepared by spray-drying American Mineralogist> 55 1780–1786.Google Scholar
Järvinen, M., 1993 Application of symmetrized harmonics expansion to correction of the preferred orientation effect Journal of Applied Crystallography> 26 525–531 10.1107/S0021889893001219.CrossRefGoogle Scholar
Klug, H.P. and Alexander, L.E., 1954 X-ray diffraction procedures for polycrystalline and amorphous materials New York John Wiley & Sons 716 pp.Google Scholar
Monecke, T. Köhler, S. Kleeberg, R. Herzig, P.M. 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 1617–1633 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.Google Scholar
Newnham, R.E., 1961 A refinement of the dickite structure and some remarks on polymorphism in kaolin minerals Mineralogical Magazine> 32 683–704 10.1180/minmag.1961.032.252.03.CrossRefGoogle Scholar
O’Connor, B.H. and Chang, W.J., 1986 The amorphous character and particle size distributions of powders produced with the micronizing mill for quantitative X-ray powder diffractometry X-ray Spectrometry> 15 267–270 10.1002/xrs.1300150409.CrossRefGoogle Scholar
Popa, N.C., 1992 Texture in Rietveld refinement Journal of Applied Crystallography> 25 611–616 10.1107/S0021889892004795.CrossRefGoogle Scholar
Reynolds, R.C. Jr., 1986 The Lorentz-Polarization factor and preferred orientation in oriented clay aggregates Clays and Clay Minerals> 34 359–367 10.1346/CCMN.1986.0340402.CrossRefGoogle Scholar
Reynolds, R.C. Jr., Pevear, D.R. and Mumpton, F.A., 1989 Principles and techniques of quantitative analysis of clay minerals by X-ray powder diffraction Quantitative Mineral Analysis of Clays Bloomington, Indiana The Clay Minerals Society 4–36.Google Scholar
Środoń, J., 2002 Quantitative mineralogy of sedimentary rocks with emphasis on clays and with applications to K-Ar dating Mineralogical Magazine> 66 677–687 10.1180/0026461026650055.CrossRefGoogle Scholar
Środoń, J., Bergaya, F. Theng, B.K.G. and Lagaly, G., 2006 Identification and quantitative analysis of clay minerals Handbook of Clay Science Amsterdam Elsevier 765–787 10.1016/S1572-4352(05)01028-7.CrossRefGoogle Scholar
Środoń, 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> 49 514–528 10.1346/CCMN.2001.0490604.CrossRefGoogle Scholar
Taylor, R.M. and Norrish, K., 1966 The measurement of orientation distribution and its application to quantitative X-ray diffraction analysis Clay Minerals> 6 127–142 10.1180/claymin.1966.006.3.01.CrossRefGoogle Scholar
Von Dreele, R.B., 1997 Quantitative texture analysis by Rietveld refinement Journal of Applied Crystallography> 30 517–525 10.1107/S0021889897005918.CrossRefGoogle Scholar
Williams, P.P. and Megaw, H.D., 1964 The crystal structures of low and high albites at — 180°C Acta Crystallographica> 17 882–890 10.1107/S0365110X64002341.CrossRefGoogle Scholar
Young, R.A. and Post, B., 1962 Electron density and thermal effects in alpha quartz Acta Crystallographica> 15 337–346 10.1107/S0365110X62000845.CrossRefGoogle Scholar
Zevin, L. and Viaene, W., 1990 Impact of clay particle orientation on quantitative clay diffractometry Clay Minerals> 25 401–418 10.1180/claymin.1990.025.4.01.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> 51 218–225 10.1346/CCMN.2003.0510212.CrossRefGoogle Scholar