QPA (Quantitative Phase Analysis) of carbonate rocks bearing calcite
and dolomite using X-ray diffractometry (XRD) can be performed using the
combined Rietveld Structure Refinement (RSR) and semiquantitative Reference
Intensity Ratio (RIR) methods, providing an estimation of crystalline phase in
a mixture. Different ratios of five samples were prepared by mixing these
crystal minerals with high sensitively. The scan speeds, adequate to determine
mineral phases in rock samples, were used as 6 degrees per minute with 0.08
steps. The XRD analysis with commercial TOPAS 3.0 program, defined by a new
generation of profile and structure analysis software, based on RSR provides Bragg
reflection profiles and the dimension of the unit cell of a phase. The weight
fractions of each phase were found byLe Bail and Pawley methods in RSRusing a
pseudo-Voigt peak shape model. The samples were also characterized by using
X-ray fluorescence (XRF) and
atomic absorption spectrometer (AAS). These analyses were conducted to compare
these results with those obtained from the RSR. In addition to these, RSR of
phases is very important to improve the goodness of fit (GOF). Therefore, the
discussions of refinement of the carbonate mixing were made and a refinement
procedure was given for these mixing in detail. Taking advantage of the RSR
with the addition of an internal standard, the phase fraction of all the
crystalline phases as well as the amorphous component, has been accurately
determined. RSR technique offers a valid support for the characterization of
marble in the light of industrial products.
Cite this paper
M. Tamer, "Quantitative Phase Analysis Based on Rietveld Structure Refinement for Carbonate Rocks," Journal of Modern Physics, Vol. 4 No. 8, 2013, pp. 1149-1157. doi: 10.4236/jmp.2013.48154.
 B. D. Cullity, “Elements of X-ray Diffraction,” 2nd Edition, Addison-Wesley, Boston, 1978.
 J. W. Reid, A. Jason and J. Hendry, “Rapid, Accurate Phase Quantification of Multiphase Calcium Phosphate Materials Using Rietveld Refinement,” Journal of Applied Crystallography, Vol. 39, 2006, pp. 536-543.
 D. L. Bish and S. A. Howard, “Quantitative Phase Analysis Using the Rietveld Method,” Journal of Applied Crystallography, Vol. 21, 1998, pp. 86-91.
 R. J. Hill, G. Tsambourakis and I. C. Madsen, “Improved Petrological Modal Analyses from X-Ray Powder Diffraction Data by Use of the Rietveld Method,” Journal of Petrology, Vol. 34, No. 5, 1993, pp. 867-900.
 F. H. Chung, “Quantitative Interpretation of X-Ray Diffraction Patterns of Mixtures. II. Adiabatic Principle of X-Ray Diffraction Analysis of Mixtures,” Journal of Applied Crystallography, Vol. 7, 1974, pp. 519-525.
 C. R. Hubbard, E. H. Evans and D. K. Smith, “The Reference Intensity Ratio, I/Ic, for Computer Simulated Powder Patterns,” Journal of Applied Crystallography, Vol. 9, 1976, pp. 169-174. doi:10.1107/S0021889876010807
 I. C. Madsen, N. V. Y. Scarlett, L. M. D. Cranswick and T. Lwin, “Outcomes of the International Union of Crystallography Commission on Powder Diffraction Round Robin on Quantitative Phase Analysis: Samples 1a to 1h,” Journal of AppliedCrystallography, Vol. 34, 2001, pp. 409-426. doi:10.1107/S0021889801007476
 N. V. Y. Scarlett, I. C. Madsen, L. M. D. Cranswick and T. Lwin, “On-Line X-Ray Diffraction for Quantitative Phase Analysis: Application in the Portland Cement Industry,” Powder Diffraction, Vol. 16, No. 2, 2002, pp. 71-80. doi:10.1107/S0021889801007476
 N. V. Y. Scarlett and I. C. Madsen, “Quantification of Phases with Partial or No Known Crystal Structures,” Powder Diffraction, Vol. 21, No. 4, 2006, pp. 278-284.
 B. Beckhoff, B. Kanngieβer, N. Langhoff, R. Wedell and H. Wolff, “Handbook of Practical X-Ray Fluorescence Analysis,” Springer, Berlin, 2006.
 R. J. Hill, “Improved Petrological Modal Analyses from X-Ray Powder Diffraction Data by Use of the Rietveld Method I. Selected Igneous, Volcanic, and Metamorphic Rocks,” Powder Diffraction, Vol. 6, No. 2, 1991, pp. 74-77. doi:10.1017/S0885715600017036
 R. A. Young, “Introduction to the Rietveld Method,” International Union of Crystallography Monographs on Crystallography, Vol. 5, Oxford University Press, Oxford, 1993, pp. 1-39.
 D. L. Bish and J. E. Post, “Quantitative Mineralogical Analysis Using the Rietveld Full-Pattern Fitting Method,” American Mineralogist, Vol. 78, 1993, pp. 932-940.
 W. A. Deer, R. A. Howie and J. Zussman, “Introduction to the Rock Forming Minerals,” Longman, London, 1966, pp. 489-493.
 C. S. Hurlbut Jr., “Dana’s Manual of Mineralogy,” 17th Edition, John Wiley and Sons, Inc., New York, 1959, pp. 330-340, 609.
 R. W. Cheary and A. A. Coelho, “A Fundamental Parameters Approach to X-Ray Line-Profile Fitting,” Journal of Applied Crystallography, Vol. 25, 1992, pp. 109-121. doi:10.1107/S0021889891010804
 R. W. Cheary and A. A. Coelho, “Axial Divergence in a Conventional X-Ray Powder Diffractometer. II. Realization and Evaluation in a Fundamental-Parameter Profile Fitting Procedure,” Journal of Applied Crystallography, Vol. 31, 1998, pp. 862-868.
 “Diffrac plus TOPAS v. 3.0 (Manual),” BRUKER AXS GmbH, Karlsruhe, 2006.
 R. J. Hill and C. J. Howard, “Quantitative Phase Analysis from Neutron Powder Diffraction Data Using the Rietveld Method,” Journal of Applied Crystallography, Vol. 20, 1987, pp. 467-474.
 F. Guirade, S. Gali and S. Chinchon, “Quantitative Rietveld Analysis of Aluminous Cement Clinker Phases,” Cement and Concrete Research, Vol. 30, No. 7, 2000, pp. 1023-1029. doi:10.1016/S0008-8846(00)00289-1
 H. M. Rietveld, “A Profile Refinement Method for Nuclear and Magnetic Structures,” Journal of Applied Crystallography, Vol. 2, 1969, pp. 65-71.
 R. E. Dinnebier and S. J. L. Billinge, “Powder Diffraction: Theory and Practice,” Royal Society of Chemistry, 2008. doi:10.1039/9781847558237