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On reproducibility of Rietveld analysis of reference Portland cement clinkers

Published online by Cambridge University Press:  05 March 2012

O. Pritula ,
Lˇ. Smrcˇok  and
B. Baumgartner
O. Pritula
Affiliation:
Institute of Inorganic Chemistry, Slovak Academy of Sciences, Du´bravska´ cesta, 845 36 Bratislava, Slovak Republic
Lˇ. Smrcˇok
Affiliation:
Institute of Inorganic Chemistry, Slovak Academy of Sciences, Du´bravska´ cesta, 845 36 Bratislava, Slovak Republic
B. Baumgartner
Affiliation:
STOE & CIE GmbH., P.O. Box 101302, D-64213 Darmstadt, Germany
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Abstract

Weight fractions of four dominant phases (C3S, C2S, C4AF and C3A) present in the NIST Reference Portland clinkers 8486, 8487 and 8488 were estimated by a series of Rietveld refinements. Calculated powder patterns were derived from the structural data for monoclinic C3S and C2S, orthorhombic C4AF and cubic C3A. X-ray diffraction data were collected in two laboratories with two diffractometers, a reflection and a transmission one. There were no significant differences between the results of the refinements based on the data sets collected on the machines with different experimental arrangements. Estimated phase compositions were compared to the reference values found by optical microscopy (MPC). Median agreement between refined and reference values within ±5% (absolute) was found only for 8488 clinker; for 8486 and C3A-rich 8487 it was within ±10% (absolute). In the majority of the refinements numerical instabilities were detected, leading to large correlations between FWHM and temperature parameters of some phases. The results obtained for C4AF were probably influenced by the presence of possible solid solutions with the structures close to that of C4AF. Weight fractions of low abundant C3A were estimated with the largest relative errors reaching in several cases ∼100%.

Type
Technical Articles
Information
Powder Diffraction , Volume 18 , Issue 1 , March 2003 , pp. 16 - 22
Copyright
Copyright © Cambridge University Press 2003

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