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Assessment of quantitative accuracy of Rietveld/XRD analysis of the crystalline and amorphous phases in fly ash

Abstract

The internal standard method based on Rietveld/XRD whole-patten fitting analysis of fly ash is used to assess the quantitative accuracy to determine the crystalline and amorphous phases under various conditions such as internal standards (types, SiO2 or Al2O3 and dosages, 10-50%), incident X-rays (laboratory or synchrotron) and refinement software (GSAS or TOPAS). The results reveal that the quantitative stability is quite sensible to minor phases, identical to internal standard, in fly ash. Errors are positively correlated with the weight fraction of that minor phase and negatively correlated with the dosage of an internal standard and amorphous phase content in fly ash. The original equation for the amorphous phase calculation is not applicable for a case with a higher inherent quartz content (>2.5%) in fly ash while the dosages of internal standard is lower than 20%. The original equation is modified as proposed. Based on it, the quantitative results of five different patterns report a good reproducibility with the arithmetic mean errors and the standard errors of identified main phases of around 1%.

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Publication details

The article was received on 08 Feb 2017, accepted on 09 Mar 2017, published on 09 Mar 2017 and first published online on 09 Mar 2017


Article type: Paper
DOI: 10.1039/C7AY00337D
Citation: Anal. Methods, 2017, Accepted Manuscript
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    Assessment of quantitative accuracy of Rietveld/XRD analysis of the crystalline and amorphous phases in fly ash

    P. Zhao, X. Liu, A. G. De la Torre, L. Lu and K. Sobolev, Anal. Methods, 2017, Accepted Manuscript , DOI: 10.1039/C7AY00337D

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