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Rietveld quantification of amorphous portions with an internal standard—Mathematical consequences of the experimental approach

Published online by Cambridge University Press:  29 February 2012

Torsten Westphal ,
Thomas Füllmann  and
Herbert Pöllmann
Torsten Westphal*
Affiliation:
Technische Universität Bergakademie Freiberg, Freiberg, Germany
Thomas Füllmann
Affiliation:
PANalytical B. V., Almelo, The Netherlands
Herbert Pöllmann
Affiliation:
Martin-Luther-Universität Halle-Wittenberg, Halle, Germany
*
a)Author to whom correspondence should be addressed. Electronic mail: torsten.westphal@ikgb.tu-freiberg.de
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Abstract

The Rietveld method is increasingly used for amorphous portion determination. This article describes the quantification of amorphous portions using an internal standard in a formal mathematical way. From a set of basic assumptions and postulations, equations for the amorphous portion quantification, the optimum amount of internal standard, and the slope of the amorphous portion calculation formula were derived. With this tool set, the influence of the method principle on the analytical uncertainty is discussed. It is shown that the amount of internal standard has a strong influence on the precision of the amorphous portion determination. A poor choice can make the determination impossible, while a clever choice can enhance the precision compared to the precision of the Rietveld refinement.

Keywords

amorphousinternal standardRietvelduncertainty
Type
Technical Articles
Information
Powder Diffraction , Volume 24 , Issue 3 , September 2009 , pp. 239 - 243
Copyright
Copyright © Cambridge University Press 2009

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References

Jones, R. C., Babcock, C. J., and Knowlton, W. B. (2000). “Estimation of the total amorphous content of Hawai’i soils by the Rietveld method,” Soil Sci. Soc. Am. J. SSSJD4 64, 1100–1108.CrossRefGoogle Scholar
Westphal, T. (2007). “Quantitative Rietveld-Analyse von amorphen Materialien am Beispiel von Hochofenschlacken und Flugaschen,” Doctoral thesis (http://sundoc.bibliothek.uni-halle.de/diss-online/07/07H017/index.htm).Google Scholar