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Rietveld full-profile quantification of Portland cement clinker: The importance of including a full crystallography of the major phase polymorphs

Published online by Cambridge University Press:  10 January 2013

J. C. Taylor ,
I. Hinczak  and
C. E. Matulis
J. C. Taylor
Affiliation:
CSIRO Division of Energy Technology, Lucas Heights Research Laboratories, PMB 7, Bangor, NSW, 2234, Australia
I. Hinczak
Affiliation:
Cementech Pty Limited, PO Box 362, Liverpool, NSW, 2170
C. E. Matulis
Affiliation:
CSIRO Division of Energy Technology, Lucas Heights Research Laboratories, PMB 7, Bangor, NSW, 2234, Australia
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Abstract

Crystalline phases present in the three NIST SRM Standard Portland cement clinkers 8486, 8487, and 8488 have been quantified from XRD powder patterns, (CoKα radiation), using the full-profile Rietveld method. Included in the Rietveld refinement are rhombohedral (R), monoclinic (M), and triclinic (T) crystal polymorphic forms of C3S, as well as crystal polymorphs of C2S and C3A. It is necessary to specify the phase crystallography including polymorphs, because of the extreme superposition of alite and belite XRD lines in the clinker patterns. Unsatisfactory results occur when only one or two of the C3S polymorphs are used in the Rietveld quantification; best results occur when all three polymorphs for C3S are included. The latter are called RMT-type refinements. The Rietveld full-profile XRD method is as precise as the microscope point-counting (MPC) method, but much less labor-intensive. The Rietveld method can quantify the C3S phase polymorphs, as well as total C3S. Rietveld and MPC methods give the same phase weight percentages for the three NIST standard clinkers. Calculated oxide weight percentages obtained from Rietveld phase weight percentages agree well with oxide percentages determined by XRF analysis. Bogue mineral weight percentages do not agree with Rietveld or MPC data, while transformation of the Bogue mineral percentages to oxides does not compare well with XRF analysis.

Type
Technical Articles
Information
Powder Diffraction , Volume 15 , Issue 1 , March 2000 , pp. 7 - 18
Copyright
Copyright © Cambridge University Press 2000

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References

Bish, D. L., and Howard, S. A. (1988). “Quantitative phase analysis using the Rietveld method,” J. Appl. Crystallogr. 21, 86–91.CrossRefGoogle Scholar
Catti, M., Gazzoni, G., and Ivaldi, G. (1984). “Order–disorder in the α|-(Ca, Sr)2SiO 4 solid solution: A structural and statistical-thermodynamic analysis.”Acta Crystallogr., Sect. B: Struct. Sci. 40, 537–544.CrossRefGoogle Scholar
Colville, A. A., and Geller, S. (1972). “Crystal structures of Ca 2Fe 1.43Al 0.57O 5 and Ca 2Fe 1.28Al 0.72O 5,”Acta Crystallogr., Sect. B: Struct. Crystallogr. Cryst. Chem. 28, 3196–3200.CrossRefGoogle Scholar
Czaya, R. (1971). “Refinement of the structure of γ-Ca 2SiO 4,”Acta Crystallogr., Sect. B: Struct. Crystallogr. Cryst. Chem. 27, 848–849.CrossRefGoogle Scholar
Golovastikov, R., Matveeva, R. G., and Belov, N. V. (1975). “Crystal structure of the tricalcium silicate 3CaO.SiO 2=C 3S,”Sov. Phys. Crystallogr. 20, 441–445.Google Scholar
Hill, R. J., and Howard, C. J. (1987). “Quantitative phase analysis from neutron powder diffraction data using the Rietveld method,” J. Appl. Crystallogr. 20, 467–474.CrossRefGoogle Scholar
Ilinets, A. M., Malinovskii, Y., and Nevskii, N. N. (1985).Dokl. Akad. Nauk SSSR 281, 332–336.Google Scholar
Ilinets, A. M., Bikbau, M. Ya., and Simanov, N. A. (1987). “Crystal structure of the new rhombohedral modification of tricalcium silicate,” Communication of the NII Cement, 91, 3–42.Google Scholar
Ilinets, A. M., and Bikbau, M. Ya. (1989a). “Fifth All-Union Conference on Crystal Chemistry of Inorganic and Coordination Compounds,” Abstract, Vladivostok.Google Scholar
Ilinets, A. M., and Bikbau, M. Ya. (1989b). XII European Crystallographic Meeting, Collected Abstracts, Moscow, Vol. 2, pp. 77–78.Google Scholar
Ilinets, A. M., and Bikbau, M. Ya. (1990). “Structural mechanism of polymorphic transitions of dicalcium silicate, Ca 2SiO 4. Part II. Refinement of crystal structure of high-temperature α1| modification of dicalcium silicate, Ca 2SiO 4,”Sov. Phys. Crystallogr. 35, 54–56.Google Scholar
Ilinets, A. M., and Bikbau, M. Ya. (1992). “Phase transitions in dicalcium and tricalcium silicates,” in Diffraction Methods in Materials Science, edited by J. Hasek (Nova Science, New York).Google Scholar
Jost, K. H., Ziemer, B., and Seydel, R. (1977). “Redetermination of the structure of β-dicalcium silicate,” Acta Crystallogr., Sect. B: Struct. Crystallogr. Cryst. Chem. 33, 1696–1700.CrossRefGoogle Scholar
Lea, F. M. (1970). The Chemistry of Cement and Concrete, 3rd ed. (Edward Arnold, London), p. 48.Google Scholar
Maki, I., and Kato, K. (1982). “Phase identification of alite in portland cement clinker,” Cem. Concr. Res. 12, 93–100.CrossRefGoogle Scholar
Moller, H. (1995). “Standardless quantitative phase analysis of Portland cement clinkers,” World Cem.September issue, 75–84.Google Scholar
Mumme, W. G. (1995). “Crystal structure of tricalcium silicate from a Portland Cement clinker and its application to quantitative XRD analysis,” Neues Jahrb. Mineral., Monatsh. 1995, 145–160.Google Scholar
Mumme, W. G., Hill, R. J., Bushnell-Wye, G., and Segnit, E. R. (1995). “Rietveld crystal structure refinements, crystal chemistry and calculated powder diffraction data for the polymorphs of dicalcium silicate and related phases,” Neues Jahrb. Mineral., Abh. 169, 35–68.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. 170, 171–188.Google Scholar
Nishi, F., and Takeuchi, Y. (1984). “The rhombohedral structure of tricalcium silicate at 1200 °C,” Z. Kristallogr. 168, 197–212.CrossRefGoogle Scholar
Nishi, F., Takeuchi, Y., and Maki, I. (1985). “Tricalcium silicate, Ca 3O(SiO 4): The monoclinic superstructure,” Z. Kristallogr. 172, 297–314.CrossRefGoogle Scholar
NIST (1989). National Institute of Standards and Technology, Report of Investigation, Reference Materials 8486, 8487, 8488, Portland Cement Clinker, S. D. Rasberry, Chief, Office of Standard Reference Materials, May 22nd, Gaithersburg, MD.Google Scholar
O’Connor, B. H., and Raven, M. D. (1988). “Application of the Rietveld refinement procedure in assaying powdered mixtures,” Powder Diffr. 3, 2–6.CrossRefGoogle Scholar
Rietveld, H. M. (1969). “A profile refinement method for nuclear and magnetic structures,” J. Appl. Crystallogr. 2, 65–71.CrossRefGoogle Scholar
Takeuchi, Y., Nishi, F., and Maki, I. (1980). “Crystal-chemical characterisation of the 3CaO.Al 2O 3–Na 2O solid-solution series,” Z. Kristallogr. 152, 259–307.CrossRefGoogle Scholar
Taylor, H. F. W. (1990). Cement Chemistry (Academic, London).Google Scholar
Taylor, J. C. (1991). “Computer programs for the standardless quantitative analysis of minerals using the full powder diffraction profile,” Powder Diffr. 6, 2–9.CrossRefGoogle Scholar
Taylor, J. C., and Aldridge, L. P. (1993a). “Full-profile quantitative analysis of Portland cement: Testing of possible standard XRD profiles for the major phase, tricalcium silicate,” Powder Diffr. 8, 138–144.Google Scholar
Taylor, J. C., and Aldridge, L. P. (1993b). “Phase analysis of Portland cement by full profile standardless quantitative X-ray diffraction—Accuracy and precision,” Adv. X-Ray Anal. 36, 309–314.Google Scholar
Udagawa, S., Urabe, K., Takada, K., and Natsume, M. (1979). “Studies on the dusting of Ca 2SiO 4—The crystal structure of ∝1i−Ca 2SiO 4,”Cem. Assoc. Jpn. Rev. Gen. Meet. Tech. Sess. 33, 35–38.Google Scholar