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Rietveld quantitative phase analysis with molybdenum radiation

Published online by Cambridge University Press:  15 October 2014

Ana Cuesta ,
Gema Álvarez-Pinazo ,
Marta García-Maté ,
Isabel Santacruz ,
Miguel A. G. Aranda ,
Ángeles G. De la Torre  and
Laura León-Reina
Ana Cuesta
Affiliation:
Departamento de Química Inorgánica, Universidad de Málaga, Campus Teatinos S/N, 29071 Málaga, Spain
Gema Álvarez-Pinazo
Affiliation:
Departamento de Química Inorgánica, Universidad de Málaga, Campus Teatinos S/N, 29071 Málaga, Spain
Marta García-Maté
Affiliation:
Departamento de Química Inorgánica, Universidad de Málaga, Campus Teatinos S/N, 29071 Málaga, Spain
Isabel Santacruz
Affiliation:
Departamento de Química Inorgánica, Universidad de Málaga, Campus Teatinos S/N, 29071 Málaga, Spain
Miguel A. G. Aranda
Affiliation:
Departamento de Química Inorgánica, Universidad de Málaga, Campus Teatinos S/N, 29071 Málaga, Spain ALBA-CELLS Synchrotron, Carretera BP 1413, Km. 3.3, E-08290 Cerdanyola, Barcelona, Spain
Ángeles G. De la Torre
Affiliation:
Departamento de Química Inorgánica, Universidad de Málaga, Campus Teatinos S/N, 29071 Málaga, Spain
Laura León-Reina*
Affiliation:
Servicios Centrales de Investigación SCAI, Universidad de Málaga, 29071 Málaga, Spain
*
a) Author to whom correspondence should be addressed. Electronic mail: lauralr@uma.es
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Abstract

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 MoKα 1 and MoKα 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 MoKα 1 radiation. Best laboratory results arise from MoKα 1 data as the effective tested volume is much increased but peak overlapping is not swelled.

Keywords

Mo and Cu radiationssynchrotron radiationirradiated volumecementaccuracy
Type
Technical Articles
Information
Powder Diffraction , Volume 30 , Issue 1 , March 2015 , pp. 25 - 35
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Copyright
Copyright © International Centre for Diffraction Data 2014 

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