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X-ray and neutron Rietveld quantitative phase analysis of industrial Portland cement clinkers

Published online by Cambridge University Press:  06 March 2012

O. Pritula*
Affiliation:
Institute of Inorganic Chemistry, Slovak Academy of Sciences, Dúbravská cesta, 845 36 Bratislava, Slovak Republic
Ľ. Smrčok
Affiliation:
Institute of Inorganic Chemistry, Slovak Academy of Sciences, Dúbravská cesta, 845 36 Bratislava, Slovak Republic
D. M. Többens
Affiliation:
BENSC, Hahn-Meitner Institute, Glienickerstrasse 100, D-14109 Berlin, Germany
V. Langer
Affiliation:
Department of Environmental Inorganic Chemistry, Chalmers University of Technology, S-412 96 Gothenburg, Sweden
*
a)Author to whom correspondence should be addressed. Electronic mail: uachprit@savba.sk

Abstract

Weight fractions of four dominant phases (C3S, C2S, C4AF, and C3A) present in five industrial clinkers were estimated by a series of neutron and X-ray Rietveld refinements. Calculated powder patterns were derived from the structural data for monoclinic and triclinic C3S, monoclinic C2S, orthorhombic C4AF, cubic C3A and MgO. Neutron diffraction data were collected with the high resolution E9 diffractometer (BENSC) using two different wavelengths, X-ray diffraction data with a high resolution transmission diffractometer. Elemental composition of the samples obtained by ESEM/EDX technique were in a good agreement with the data delivered by the producers. Convergence of the refinements was remarkably different for X-ray and for neutron data. Several refinements were not completed due to numerical instabilities. Neutron refinements were found to be more stable than X-ray, but there was not any notable difference in the final estimated phases’ compositions. Calculated absolute deviates of phases’ weight fractions were mostly within ±10%, which for the less abundant phases corresponded to relative deviations within ±50%. © 2004 International Centre for Diffraction Data.

Type
Technical Articles
Copyright
Copyright © Cambridge University Press 2004

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References

Aldridge, L. P. (1982a). “Accuracy and precision of phase analysis in Portland cement by Bogue, microscopic and X-ray diffraction methods,” Cem. Concr. Res. CCNRAI 12, 381398. ccn, CCNRAI CrossRefGoogle Scholar
Aldridge, L. P. (1982b). “Accuracy and precision of an X-ray diffraction method for analysing Portland cements,” Cem. Concr. Res. CCNRAI 12, 381398. ccn, CCNRAI CrossRefGoogle Scholar
Anwander, A., Neyran, B., Haase, J., and Baskurt, A. (1998). “Automatic image analysis,” World Cement Research and Development77–83.Google Scholar
Berliner, R., Ball, C., and Presbury, B. W. (1997). “Neutron powder diffraction investigation of model cement compounds,” Cem. Concr. Res. CCNRAI 27, 551575. ccn, CCNRAI CrossRefGoogle Scholar
Colville, A. A., and Geller, S. (1972). “Crystal structures of Ca2Fe1.43Al0.57O5 and Ca2Fe1.28Al0.72O5,Acta Crystallogr., Sect. B: Struct. Crystallogr. Cryst. Chem. ACBCAR 28, 31963200. acb, ACBCAR CrossRefGoogle Scholar
Dollase, W. A. (1986). “Correction of intensities for preferred orientation in powder diffractometry: Application of the March model,” J. Appl. Crystallogr. JACGAR 19, 267272. acr, JACGAR CrossRefGoogle Scholar
Golovastikov, N. I., Matveeva, R. G., and Belov, N. V. (1975). “Crystal structure of the tricalcium silicate 3CaO⋅SiO2=C3S,Kristallografiya KRISAJ 20, 721729. krg, KRISAJ Google Scholar
Gutteridge, W. A. (1979). “On the dissolution of the intersticial phases in Portland cement,” Cem. Concr. Res. CCNRAI 9, 319324. ccn, CCNRAI CrossRefGoogle Scholar
Madsen, I. C., Scarlett, N. V. Y., Cranswick, L. M. D., and Lwin, T. (2001). “Outcomes of the International union of crystallography commission on powder diffraction round robin on quantitative phase analysis: samples 1a to 1h,” J. Appl. Crystallogr. JACGAR 34, 409426. acr, JACGAR CrossRefGoogle Scholar
McCusker, L. B., Von Dreele, R. B., Cox, D. E., Louër, D., and Scardi, P. (1999). “Rietveld refinement guidelines,” J. Appl. Crystallogr. JACGAR 32, 3650. acr, JACGAR CrossRefGoogle Scholar
Mumme, W. G. (1995a). “Crystal structure of tricalcium silicate from a Portland cement clinker and its application to quantitative XRD analysis,” Neues Jahrb. Mineral., Monatsh. NJMMAW 4, 145160. nja, NJMMAW Google Scholar
Mumme, W. G., Hill, R. J., Bushnell-Wye, G., and Segnit, E. R. (1995b). “Rietveld crystal structure refinements, crystal chemistry and calculated powder diffraction data for the polymorphs of dicalcium silicate and related phases,” Neues Jahrb. Mineral., Abh. NJMIAK 169, 3568. njm, NJMIAK Google Scholar
Mumme, W. G., Cranswick, L., and Chakoumakos, B. (1996). “Rietveld crystal structure refinements from high temperature neutron powder diffraction data for the polymorphs of dicalcium silicate,” Neues Jahrb. Mineral., Abh. NJMIAK 170, 171188. njm, NJMIAK Google Scholar
Nishi, F., and Takeuchi, Y. (1975). “The Al6O18 rings of tetrahedra in the structure of Ca8.5NaAl6O18,Acta Crystallogr., Sect. B: Struct. Crystallogr. Cryst. Chem. ACBCAR 31, 11691173. acb, ACBCAR CrossRefGoogle Scholar
Nurse, R. W. (1980). “Phase equilibria and formation of Portland cement minerals,” Proceedings on the 5th International Symposium on the Chemistry of Cement, Tokyo 1, 77–89.Google Scholar
Peterson, V., Hunter, B., Ray, A., and Aldridge, L. P. (2002). “Rietveld refinement of neutron, synchrotron and combined powder diffraction data of cement clinker,” Appl. Phys. A: Mater. Sci. Process. APAMFC 74, S1409S1411. mfc, APAMFC CrossRefGoogle Scholar
Pritula, O., Smrčok, Ľ., and Baumgartner, B. (2003). “On reproducibility of Rietveld analysis of reference Portland clinkers,” Powder Diffr. PODIE2 18, 1622. pdj, PODIE2 CrossRefGoogle Scholar
Pritula, O., Smrčok, Ľ., Ivan, J., and Iždinský, K. (2004). “X-ray quantitative phase analysis of residues of the reference Portland clinkers,” Ceramics ZZZZZZ 48 (1), 3439.Google Scholar
Pritula, O. (2004). “X-ray and neutron Rietveld quantitative phase analysis of Portland cement clinkers,” PhD Thesis (In Slovak.)CrossRefGoogle Scholar
Rodriguez-Carvajal, J. (2000). “FULLPROF2000,” http://www-llb.cea.fr/fullweb/fp2kGoogle Scholar
Schiebold, E. (1921). “Über die Kristallstruktur des Periclas,” Z. Kristallogr. ZEKRDZ 56, 430435. zek, ZEKRDZ Google Scholar
Stutzman, P. E. (1996). “Guide for X-ray powder diffraction analysis of Portland cement and clinker,” NISTIR 5755.Google Scholar
Takeuchi, Y., Nishi, F., and Maki, I. (1980). “Crystal-chemical characterization of the (CaO)3⋅(Al2O3)-(Na2O) solid-solution series,” Z. Kristallogr. ZEKRDZ 152, 259307. zek, ZEKRDZ CrossRefGoogle Scholar
Torre, de la A. G., Bruque, S., Campo, J., and Aranda, M. A. G. (2002). “The superstructure of C3S from synchrotron and neutron powder diffraction and its role in quantitative phase analyses,” Cem. Concr. Res. CCNRAI 32, 13471356. ccn, CCNRAI CrossRefGoogle Scholar
Többens, D. M., Stüsser, N., Knorr, K., Mayer, H. M., and Lampert, G. (2001). “E9: The new high-resolution neutron powder diffractometer at the Berlin neutron scattering center,” Mater. Sci. Forum MSFOEP 387–381, 288293. msf, MSFOEP CrossRefGoogle Scholar