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Structure and microstructure of gypsum and its relevance to Rietveld quantitative phase analyses

Published online by Cambridge University Press:  06 March 2012

Ángeles G. De la Torre ,
María-Gema López-Olmo ,
Carmen Álvarez-Rua ,
Santiago García-Granda  and
Miguel. A. G. Aranda
Ángeles G. De la Torre
Affiliation:
Dept. Química Inorgánica, Cristalografía y Mineralogía, Universidad de Málaga, Campus de Teatinos, 29071-Málaga, Spain
María-Gema López-Olmo
Affiliation:
Dept. Química Inorgánica, Cristalografía y Mineralogía, Universidad de Málaga, Campus de Teatinos, 29071-Málaga, Spain
Carmen Álvarez-Rua
Affiliation:
Dept. Química Física y Analítica, Universidad de Oviedo, C Julian Claveria, 33006-Oviedo, Spain
Santiago García-Granda
Affiliation:
Dept. Química Física y Analítica, Universidad de Oviedo, C Julian Claveria, 33006-Oviedo, Spain
Miguel. A. G. Aranda*
Affiliation:
Dept. Química Inorgánica, Cristalografía y Mineralogía, Universidad de Málaga, Campus de Teatinos, 29071-Málaga, Spain
*
a)Author to whom correspondence should be addressed; electronic mail: [email protected]
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Abstract

Single crystals of gypsum were studied in a diffractometer equipped with a CCD two-dimensional detector. The microstructure of the crystal gave wide poorly shaped spots showing sometimes curved streaks around the spots, which made the integration process very difficult, yielding a low quality structure. The crystal structure and microstructure of gypsum has been studied by high-resolution synchrotron powder diffraction of a ground single crystal. The intensities in the synchrotron powder pattern can be reliably fitted although the peak shape displays anisotropic peak broadening. The Rietveld results for gypsum were a=6.522 91(3) Å, b=15.197 63(9) Å, c=6.522 91(3) Å, β=118.479(1)°, V=494.536(5) Å3 and Z=4 (s.g. I2/c) with RWP=5.39% and RF=1.64%. We have also studied the influence of the structural description used for gypsum in a synchrotron Rietveld quantitative phase analysis of a standard mixture containing 50 wt % of CaSO4⋅2H2O and Al2O3. Finally, the effects of the type of preferred orientation correction for laboratory X-ray powder data are also discussed. © 2004 International Centre for Diffraction Data.

Type
Technical Articles
Information
Powder Diffraction , Volume 19 , Issue 3 , September 2004 , pp. 240 - 246
Copyright
Copyright © Cambridge University Press 2004

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