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Rietveld quantitative phase analysis with molybdenum radiation

  • Ana Cuesta (a1), Gema Álvarez-Pinazo (a1), Marta García-Maté (a1), Isabel Santacruz (a1), Miguel A. G. Aranda (a1) (a2), Ángeles G. De la Torre (a1) and Laura León-Reina (a3)...


Building materials are very complex samples of worldwide importance; hence quantitative knowledge of their mineralogical composition is necessary to predict performances. Rietveld quantitative phase analysis (RQPA) allows a direct measurement of the crystalline phase contents of cements. We highlight in this paper the use of laboratory X-ray powder diffraction (LXRPD) employing high-energy radiation, molybdenum (Mo), for attaining the RQPA of cements. Firstly, we evaluate the accuracy of RQPA employing a commercial calcium sulfoaluminate clinker with gypsum. In addition to Mo 1 and Mo 1,2 radiations, Cu and synchrotron patterns are also analyzed for the sake of comparison. Secondly, the assessment of the accuracy of RQPA results obtained using different radiations (synchrotron, Mo, and Cu) and geometries (reflection and transmission) is performed by analyzing two well-known commercial samples. As expected, for LXRPD data, accuracy in the RQPA results improves as the irradiated volume increases. Finally, three very complex aged hydrated cements have been analyzed using MoKα1-LXRPD and Synchrotron-XRPD. The main overall outcome of this work is the benefit for RQPA of using strictly monochromatic Mo 1 radiation. Best laboratory results arise from Mo 1 data as the effective tested volume is much increased but peak overlapping is not swelled.


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Alvarez-Pinazo, G., Santacruz, I., León-Reina, L., Aranda, M. A. G., and De la Torre, A. G. (2013). “Hydration reactions and mechanical strength developments of iron-rich sulfobelite eco-cements,” Ind. Eng. Chem. Res. 52, 1660616614.
Alvarez-Pinazo, G., Cuesta, A., García-Maté, M., Santacruz, I., Losilla, E. R., Sanfélix, S. G., Fauth, F., Aranda, M. A. G., and De la Torre, A. G. (2014). “In-situ early-age hydration study of sulfobelite cements by synchrotron powder diffraction,” Cem. Concr. Res. 56, 1219.
Aranda, M. A. G. and De la Torre, A. G. (2013) “Sulfoaluminate cement,” in Eco-efficient Concrete, edited by Pacheco-Torgal, F., Jalali, S., Labrincha, J. and John, V. M. (Woodhead Publishing Limited, Cambridge), pp. 488522.
Aranda, M. A. G., De la Torre, A. G., and León-Reina, L. (2012). “Rietveld quantitative phase analysis of OPC clinkers, cements and hydration products,” Rev. Mineral. Geochem. 74, 169209.
Bellmann, F., Damidot, D., Moser, B., and Skibsted, J. (2010). “Improved evidence for the existence of intermediate phase during hydration of tricalcium silicate,” Cem. Concr. Res. 40, 875884.
Buhrke, V. E., Jenkins, R., and Smith, D. K. (Eds.) (1998). A practical Guide for the Preparation of Specimens for X-ray Fluorescence and X-ray Diffraction Analysis (Wiley, New York).
Cromer, D. T. and Liberman, D. A. (1981). “Anomalous dispersion calculations near to an on the long-wavelength side of an absorption edge,” Acta Crystallogr. A37, 267268.
Delhez, R. and Mittemeijer, E. J. (1975). “An improved α2 elimination,” J. Appl. Crystallogr. 8, 609611.
De la Torre, A. G. and Aranda, M. A. G. (2003). “Accuracy in Rietveld quantitative phase analysis of portland cements,” J. Appl. Crystallogr. 36, 11691176.
De la Torre, 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. 32, 13471356.
De la Torre, A. G., Lopez-Olmo, M. G., Alvarez-Rua, C., Garcia-Granda, S., and Aranda, M. A. G. (2004). “Structure and microstructure of gypsum and its relevance to Rietveld quantitative phase analyses,” Powder Diffr. 19, 240246.
De la Torre, A. G., De Vera, R. N., Cuberos, A. J. M., and Aranda, M. A. G. (2008). “Crystal structure of low magnesium-content alite: application to Rietveld quantitative phase analysis,” Cem. Concr. Res. 38, 12611269.
Dinnebier, R. E. and Billinge, S. J. L. (Eds.) (2008). Powder Diffraction: Theory and Practice (Royal Society of Chemistry, Cambridge).
Dollase, W. A. (1986). “Correction of intensities for preferred orientation in powder diffractometry: application of the March model,” J. Appl. Crystallogr. 19, 267272.
Dunstetter, F., De Noirfontaine, M.-N., and Courtial, M. (2006). “Polymorphism of tricalcium silicate, the major compound of Portland cement clinker: 1. Structural data: review and unified análisis,” Cem. Concr. Res. 36, 3953.
Elton, N. J. and Salt, P. D. (1996). “Particle statistics in quantitative X-ray diffractometry,” Powder Diffr. 11, 218229.
Finger, L. W., Cox, D. E., and Jephcoat, A. P. (1994). “A correction for powder diffraction peak asymmetry due to axial divergente,” J. Appl. Crystallogr. 27, 892900.
García-Maté, M., Santacruz, I., De la Torre, A. G., León-Reina, L., and Aranda, M. A. G. (2012). “Rheological and hydration characterization of calcium sulfoaluminate cement pastes,” Cem. Concr. Compos. 34, 684691.
Hill, R. J. and Madsen, I. C. (2002). “Sample preparation, instrument selection and data collection,” in Structure Determination from Powder Diffraction Data, edited by David, W., Shankland, K., McCusker, L. and Baerlocher, C. (Oxford University Press, New York).
Klug, H. P. and Alexander, L. E. (1974). X-ray Diffraction Procedures for Polycrystalline and Amorphous Materials (Wiley, New York), 2nd ed., p. 618.
Knapp, M., Peral, I., Nikitina, L., Quispe, M., and Ferrer, S. (2011). “Technical concept of the materials science beamline at ALBA,” Z. Kristallogr. Proc. 1, 137142.
Larson, A. C. and Von Dreele, R. B. (2004). General Structure Analysis System (GSAS) (Report LAUR 86–748). Los Alamos, New Mexico: Los Alamos National Laboratory.
León-Reina, L., De la Torre, A. G., Porras-Vázquez, J. M., Cruz, M., Ordonez, L. M., Alcobé, X., Gispert-Guirado, F., Larrañaga-Varga, A., Paul, M., Fuellmann, T., Schmidt, R., and Aranda, M. A. G. (2009). “Round Robin on Rietveld quantitative phase analysis of Portland cements,” J. Appl. Crystallogr. 42, 906916.
León-Reina, L., Compana, J. M., De la Torre, A. G., Moreno, R., Ochando, L. E., and Aranda, M. A. G. (2011). “Powder diffraction analysis of gemstone inclusions,” Powder Diffr. 26, 4852.
Le Saout, G., Kocaba, V. and Scrivener, K. (2011). “Application to the Rietveld method to the analysis of anhydrous cement,” Cem. Concr. Res. 41, 133148.
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. 34, 409426.
Mitchell, L. D., Margeson, J. C., and Whitfield, P. S. (2006). “Quantitative Rietveld analysis of hydrated cementatious systems,” Powder Diffr. 21, 111113.
Rachinger, W. A. (1948). “A correction for the α1: α2 doublet in the measurement of widths of X-ray diffraction lines,” J. Sci. Instrum. 25, 254259.
Rajczyk, K. and Nocun-Wczelik, W. (1992). “Thermal methods and microcalorimetry application in the studies of low energy cements,” J. Therm. Anal. Calorim. 38, 771775.
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, 383400.
Scrivener, K. L. and Nonat, A. (2011). “Hydration of cementitious materials, present and future,” Cem. Concr. Res. 41, 651665.
Scrivener, K. L., Fullmann, T., Gallucci, E., Walenta, G., and Bermejo, E. (2004). “Quantitative study of Portland cement hydration by X-ray diffraction/Rietveld analysis and independent methods,” Cem. Concr. Res. 34, 15411547.
Smith, D. K. (2001). “Particle statistics and whole-pattern methods in quantitative X-ray powder diffraction analysis,” Powder Diffr. 16, 186191.
Stutzman, P. (2005). “Powder diffraction analysis of hydraulic cements: ASTM Rietveld round-robin results on precision,” Powder Diffr. 20, 97100.
Thompson, P., Cox, D. E., and Hasting, J. B. (1987). “Rietveld refinement of Debye–Scherrer synchrotron X-ray data from Al2O3,” J. Appl. Crystallogr. 20, 7983.



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