Accuracy of XRPD QPA using the combined Rietveld–RIR method

Abstract

QPA (quantitative phase analysis) of polycrystalline materials using XRPD (X-ray powder diffraction) can be performed using the combined Rietveld and reference intensity ratio (RIR) methods, providing an estimate of both the crystalline and the amorphous phase in a mixture. Although the accuracy of estimates of the phase composition of simple ternary or quaternary mixtures is generally very good, uncertainties remain and bias the accuracy of phase determinations in complex systems such as pyroclastic rocks, which may contain two or more zeolite species, a number of other phases (generally up to four or five), and glass. The contribution of the incoherent scattering, biasing accuracy, in the glass determination has been discussed in an earlier work on the modal analysis of pyroclastic rocks [Gualtieri (1996).Powder Diffr.11, 97–106]. In this work, the assumption of the crystal structure, the influence of the spike addition, background and atomic (thermal) displacement parameters are discussed. It is shown that the structure-model assumption no longer holds for systems containing complex phases such as zeolites, as the accuracy is degraded and, as far as the influence of the added spike is concerned, there is an underestimation of the glass content with increasing amounts of added spike.