Hostname: page-component-586b7cd67f-dlnhk Total loading time: 0 Render date: 2024-11-23T06:15:19.724Z Has data issue: false hasContentIssue false
  • English
  • Français

Effect of microabsorption on the determination of amorphous content via powder X-ray diffraction

Published online by Cambridge University Press:  22 March 2018

Nicola V. Y. Scarlett  and
Ian C. Madsen
Nicola V. Y. Scarlett*
Affiliation:
CSIRO Mineral Resources, Box 312 Clayton South, Victoria 3169, Australia
Ian C. Madsen
Affiliation:
CSIRO Mineral Resources, Box 312 Clayton South, Victoria 3169, Australia
*
a)Author to whom correspondence should be addressed. Electronic mail: [email protected]
Get access Rights & Permissions [Opens in a new window]

Abstract

Powder X-ray diffraction has become a routine procedure for the quantification of phases in mixtures. The most common method for this measurement is the Rietveld method, which generally returns the relative weight percentages of the crystalline components within the mixture. However, in many instances, it is also desirable to obtain an estimate of the amorphous content of a sample. There are several methods that may be used for this measurement and their accuracy has been assessed previously with a number of ideal, synthetic mixtures. Many samples, especially in the mineralogy sphere, are far from ideal and contain multiple phases of varying absorption contrast. This creates a microabsorption problem which affects the accuracy of the determination of both the crystalline and amorphous components. This paper assesses commonly used methods of amorphous determination with a series of synthetic samples designed to create a considerable microabsorption problem.

Keywords

powder X-ray diffractionX-ray diffractionquantitative phase analysisquantitative phase analysisamorphous
Type
Technical Articles
Information
Powder Diffraction , Volume 33 , Issue 1 , March 2018 , pp. 26 - 37
Copyright
Copyright © International Centre for Diffraction Data 2018 

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

Antao, S. M., Hassan, I., Jun, W., Lee, L. P., and Toby, B. H. (2008). “State-of-the-art high-resolution powder X-ray diffraction (HRPXRD) illustrated with Rietveld structure refinement of quartz, sodalite, tremolite and meionite,” Can. Mineral. 46, 1501–1509.CrossRefGoogle Scholar
Bates, S., Zografi, G., Engers, D., Morris, K., Crowley, K., and Newman, A. (2006). “Analysis of amorphous and nanocrystalline solids from their X-ray diffraction patterns,” Pharm. Res. 23, 2333–2349.Google Scholar
Bish, D. L. and Howard, S. A. (1988). “Quantitative phase analysis using the Rietveld method,” J. Appl. Cryst. 21, 86–91.Google Scholar
Brindley, G. W. (1945). “The effect of grain or particle size on X-ray reflections from mixed powders and alloys, considered in relation to the quantitative determination of crystalline substances by X-ray methods,” Philos. Mag. 36, 347–369.Google Scholar
Chipera, S. J. and Bish, D. L. (2002). “FULLPAT: a full-pattern quantitative analysis program for X-ray powder diffraction using measured and calculated patterns,” J. Appl. Cryst. 35, 744–749.Google Scholar
Ferreira, F. F., Granado, E., Carvalho, W. J., Kycia, S. W., Bruno, D., and Droppa, R. J. (2006). “X-ray powder diffraction beamline at D10B of LNLS: application to the Ba2FeReO6 double perovskite,” J. Synchrotron Radiat. 13, 46–53.CrossRefGoogle Scholar
Finger, L. W. and Hazen, R. M. (1978). “Crystal structure and compression of ruby to 46 kbar,” J. Appl. Phys. 49, 5823–5826.Google Scholar
Hancock, B. C. and Zografi, G. (1997). “Characteristics and significance of the amorphous state in pharmaceutical systems,” J. Pharm. Sci. 86, 1–12.Google Scholar
Heller, R. B., McGannon, J., and Weber, A. H. (1950). “Precision determination of the lattice constants of zinc oxide,” J. Appl. Phys. 21, 1283–1284.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
Hudson-Edwards, K. A. (2003). “Sources, mineralogy, chemistry and fate of heavy metal-bearing particles in mining-affected river systems,” Min. Mag. 67, 205–217.Google Scholar
Jamieson, H. E. (2011). “Geochemistry and mineralogy of solid mine waste: essential knowledge for predicting environmental impact,” Elements 7(6), 381–386.Google Scholar
Kaduk, J. A. (2000). “Petroleum and petrochemicals,” in Industrial Applications of X-ray Diffraction, edited by Chung, F. H. and Smith, D. K. (New York: Marcel Dekker), pp. 207–253.Google Scholar
Klug, H. P. and Alexander, L. E. (1974). X-ray Diffraction Procedures: For Polycrystalline and Amorphous Materials (New York: Wiley).Google 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 1 h,” J. Appl. Crystallogr. 34, 409–426.CrossRefGoogle Scholar
Madsen, I. C., Scarlett, N. V. Y., and Kern, A. (2011). “Description and survey of methodologies for the determination of amorphous content via x-ray powder diffraction,” Z. Kristallogr. 226, 944–955.Google Scholar
Mursic, Z., Vogt, T., Boysen, H., and Frey, F. (1992). “Single-crystal neutron diffraction study of metamict zircon up to 2000 K,” J. Appl. Crystallogr., 25, 519–523.CrossRefGoogle 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.Google Scholar
Okudera, H. (1997). “Single crystal X-ray studies of cation-deficient magnetite,” Z. Kristallogr. 212, 458–461.Google Scholar
Riello, P. (2004). “Quantitative analysis of amorphous fraction in the study of the microstructure of semi-crystalline materials,” in Diffraction Analysis of the Microstructure of Materials, edited by Mittemeijer, E. J. and Scardi, P. (Berlin: Springer Verlag), pp. 167–184.Google Scholar
Rietveld, H. M. (1969). “A profile refinement method for nuclear and magnetic structures,” J. Appl. Cryst. 2, 65–71.Google Scholar
Sawada, H. (1994). “Residual electron density study of chromium sesquioxide by crystal structure and scattering factor refinement,” Mater. Res. Bull. 29, 239–245.Google Scholar
Scarlett, N. V. Y. and Madsen, I. C. (2006). “Quantification of phases with partial or no known crystal structures,” Powder Diffr. 21, 278–284.Google Scholar
Scarlett, N. V. Y., Madsen, I. C., Cranswick, L. M. D., Lwin, T., Groleau, E., Stephenson, G., Aylmore, M., and Agron-Olshina, N. (2002). “Outcomes of the International Union of Crystallography Commission on powder diffraction round robin on quantitative phase analysis: samples 2, 3, 4, synthetic bauxite, natural granodiorite and pharmaceuticals,” J. Appl. Crystallogr. 35, 383–400.Google Scholar
Walenta, G. and Füllmann, T. (2004). “Advances in quantitative XRD analysis for clinker, cements, and cementitious additions,” Adv. X-ray Anal. 47, 287–296.Google Scholar
Whitfield, P. S. and Mitchell, L. D. (2003). “Quantitative Rietveld analysis of the amorphous content in cements and clinkers,” J. Mater. Sci. 38, 4415–4421.Google Scholar
Supplementary material: File

Scarlett and Madsen supplementary material

Scarlett and Madsen supplementary material 1

Download Scarlett and Madsen supplementary material(File)
File 634.5 KB