Hostname: page-component-8448b6f56d-c47g7 Total loading time: 0 Render date: 2024-04-25T05:15:04.461Z Has data issue: false hasContentIssue false
  • English
  • Français

Full-profile Rietveld quantitative XRD analysis of Portland cement: Standard XRD profiles for the major phase tricalcium silicate (C3S: 3CaO.SiO2)

Published online by Cambridge University Press:  10 January 2013

J. C. Taylor  and
L. P. Aldridge
J. C. Taylor
Affiliation:
CSIRO Division of Coal and Energy Technology, Lucas Heights Research Laboratories, Private Mail Bag 7, Menai, N.S.W., 2234, Australia
L. P. Aldridge
Affiliation:
Australia Nuclear Science and Technology Organisation, Lucas Heights Research Laboratories, Private Mail Bag 1, Menai, N.S.W., 2234, Australia
Get access Rights & Permissions [Opens in a new window]

Abstract

The calculated XRD profiles of alite (impure Ca3SiO5, the major phase in Portland cement) derived from seven postulated crystal structures for alite were compared with a measured alite profile, extracted from the XRD pattern of a standard Portland cement. Only two of these profiles were found suitable for multiphase Rietveld phase quantification, namely those given by the monoclinic superlattice and triclinic models. These, however, gave very slow computing times because the large low-symmetry structures generated many X-ray reflections over the pattern. Also tested was an “observed” standard profile for alite, derived from experimental alite profiles, and generated using the (hkl) file feature of the SIROQUANT P.C. quantitative analysis system. This file was based on rhombohedral pseudosymmetry and contained very few (hkl) reflections, compared to the low-symmetry models (64 reflections instead of 951 for the monoclinic and 1691 for the triclinic models, respectively). The latter standard profile gave the best fit to the known phase concentrations and gave computing times which were shorter by factors of 2.5 and 4.9 than those for the monoclinic and triclinic standard profiles, respectively.

Type
Research Article
Information
Powder Diffraction , Volume 8 , Issue 3 , September 1993 , pp. 138 - 144
Copyright
Copyright © Cambridge University Press 1993

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

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. 12, 381–398.CrossRefGoogle Scholar
Aldridge, L.P. (1982b). “Accuracy and Precision of an X-Ray Diffraction Method for Analysing Portland Cements,” Cem. Conc. Res. 12, 437–446.CrossRefGoogle Scholar
Bigare, M., Guinier, A., Mazieres, C., Regourd, M., Yannaquis, N., Eysel, W., Hahn, T., and Woermann, E. (1967). “Polymorphism of Tricalcium Silicate and its Solid Solutions,” J. Am. Ceram. Soc. 50, 609–619.Google Scholar
Bish, D.L., and Howard, S.A. (1988). “Quantitative Phase Analysis Using the Rietveld Method,” J. Appl. Cryst. 21, 86–91.CrossRefGoogle Scholar
Dent Glasser, L.S. (1965). “Relationships Between Sr3SiO5, Cd3SiO5 and Ca3SiO5,” Acta Cryst. 18, 455–457.CrossRefGoogle Scholar
Eysel, W., and Breuer, K.-H. (1983). “Crystal Chemistry of Compounds M3O(TO4),” Zeit. Kristallogr. 163, 1–17.Google Scholar
Eysel, W., and Hahn, T. (1970). “Polymorphism and Solid Solution of Ca3GeO5 and Ca3SiO5,” Zeit. Kristallogr. 131, 40–59.Google Scholar
Fayos, J., Glasser, F.P., Howie, R.A., Lachowski, E., and Perez-Mendez, M. (1985). “The X-Ray Crystal Structure of Dodeca-Calcium-Potassium Dioxofluorure-di-sulphate-tetrasilicate KF · 2[Ca6(SO4)(SiO4)2O), a fluorine containing phase encountered in Cement Clinker Production Process,” Acta Cryst. C41, 814–816.Google Scholar
Fayos, J., and Perez-Mendez, M. (1986). “Crystallo-chemistry of Ca3O(SiO4)(C3S) Related Phases,” Am. Ceram. Soc. Bull. 65, 1191–1195.Google Scholar
Golovastikov, R., Matveeva, R.G., and Belov, N.V. (1975). “Crystal Structure of the Tricalcium Silicate 3CaO.SiO2 = C3S,” 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. Cryst. 20, 467–474.CrossRefGoogle Scholar
Il'inets, A.M., Malinovskii, Y., and Nevskii, N.N. (1985). “Crystal Structure of the Rhombohedral Modification of Tricalcium Silicate, Ca3SiO5,” Dokl. Akad. Nauk. SSSR 281, 332–336.Google Scholar
English Translation in Sov. Phys. Dokl. 30, 191–192 (1985).Google Scholar
Il'inets, A.M., and Simonov, V.I. (1987). “Unified Structural Basis of Polymorphic Modifications of Tricalcium Silicate, Ca3SiO5,” Sov. Phys. Crystallogr. 32, 692–695.Google Scholar
Jeffery, J.W. (1952). “The Crystal Structure of Tricalcium Silicate,” Acta Cryst. 5, 26–35.Google Scholar
Maki, I., and Chomy, S. (1978). “Microscopic Study on the Polymorphism of Ca3SiO5,” Cem. Concr. Res. 8, 407–414.CrossRefGoogle Scholar
Maki, I., and Kato, K. (1982). “Phase Identification of Alite in Portland Cement Clinker,” Cem. Concr. Res. 12, 93–100.CrossRefGoogle Scholar
Nishi, F., and Takeuchi, Y. (1984). “The Rhombohedral Structure of Tricalcium Silicate at 1200 °C,” Zeit. Kristallogr. 168, 197–212.Google Scholar
Nishi, F., and Takeuchi, Y. (1985). “Tricalcium Silicate, Ca3O(SiO4): The Monoclinic Superstructure,” Zeit. Kristallogr. 172, 297–314.CrossRefGoogle Scholar
O'Connor, B.H., and Raven, M.D. (1988). “Application of the Rietveld Refinement Procedure in Assaying Powdered Mixtures,” Powder Diff. 3, 2–6.CrossRefGoogle Scholar
Perez-Mendez, M., Fayos, J., Howie, R.A., Gard, J.A., and Glasser, F.P. (1985). “Calcium Fluorosilicates: the Ca6-0.5xSi2O10-x Fx Phase,” Cem. Conc. Res. 15, 600–604.CrossRefGoogle Scholar
Perez-Mendez, M., Groves, G.W., and Fayos, J. (1986). “Effect of Fluorine and Magnesium on the Polymorphism of Tricalcium Silicate: Anew fluorine-containing Tricalcium Silicate Superlattice,” J. Am. Ceram. Soc. 69, 670–673.CrossRefGoogle Scholar
Perez-Mendez, M., Howie, R.A., and Glasser, F.P. (1984). “Ca3SiO5 and its fluorine-stabilised Aristotype: Synthesis, Stability and Postulated Structure of Ca6-0.5xSi2O2O10-xFx,” Cem. Conc. Res. 14, 57–63.CrossRefGoogle Scholar
Regourd, M. (1964). “Lattice Determination of Microcrystals: Application to Polymorphs of Tricalcium Silicates,” Bull. Soc. Fr. Min. Cristallogr. 87, 241–272.Google Scholar
Regourd, M. (1983). “Crystal Chemistry of Portland Cement Phases,” in Structure and Performance of Cements, edited by Barnes, P. (Applied Science, England), Chap. 3.Google Scholar
Rietveld, H.M. (1969). “A Profile Refinement Method for Nuclear and Magnetic Structures,” J. Appl. Cryst. 2, 65–71.Google Scholar
Sinclair, W., and Groves, G.W. (1984). “Transmission Electron Microscopy and X-Ray Diffraction of Doped Tricalcium Silicate,” J. Am. Ceram. Soc. 67, 325–330.Google Scholar
Smith, D.K., Johnson, G.G., Schieble, A., Wims, A.M., Johnson, J.L., and Ullman, G. (1987). “Quantitative X-Ray Powder Diffraction Method Using the Full Diffraction Pattern,” Powder Diff. 2, 73–77.CrossRefGoogle Scholar
Takeuchi, Y., Nishi, F., and Maki, I. (1984). “Structural Aspects of the Phase Transitions in Tricalcium Silicate, Ca3SiO5(=C3S),” Acta Cryst. A40, C215.CrossRefGoogle Scholar
Taylor, J.C. (1991). “Computer Programs for Standardless Quantitative Analysis of Minerals Using the Full Powder Diffraction Profile,” Powder Diff. 6, 2–9.CrossRefGoogle Scholar
Taylor, J.C., and Clapp, R.A. (1992). “New Features and Advanced Applications of SIROQUANT: A Personal Computer XRD Full Profile Quantitative Analysis Software Package,” Adv. X-Ray Analy., 35, 49–55.Google Scholar
Taylor, J.C., and Rui, Zhu (1992). “Simultaneous Use of Observed and Calculated Standard Profiles in Quantitative XRD Analysis of Minerals by the Multiphase Rietveld Method: The Determination of Pseudorutile in Mineral Sands Products,” Powder Diff., 7, 152–161.CrossRefGoogle Scholar
Yamaguchi, G., and Miyabe, H. (1960). “Precise Determination of the 3CaO.SiO2 Cells and Interpretation of Their X-Ray Diffraction Patterns,” J. Am. Ceram. Soc. 43, 219–224.CrossRefGoogle Scholar