Absorption contrast effects in the quantitative XRD analysis of powders by full multiphase profile refinement

Abstract

It is shown that quantitative X‐ray powder diffraction analyses using full profile multiphase refinement should include corrections for the Brindley particle absorption contrast effect. This is demonstrated with synthetic mixtures of the highly contrasting phases LiF and Pb(NO3)2 (μ/ρ = 20 and 231 cm−1 for Co Kα). With contrast corrections, the only parameter which needs to be input is an effective particle radius R for each phase. For mixtures of LiF and Pb(NO3)2 over the whole composition range, quantification is achieved, under the present specimen preparation method, with an effective particle radius of 51 μm for both phases, giving analyses correct to within 1 percentage point. Without Brindley corrections, the analysis is grossly in error.

Post-depositional origin of highly 13C-depleted carbonate in the Doushantuo cap dolostone in South China: Insights from petrography and stable carbon isotopes

“…The divergence, scattering and receiving slits were 1°, 1°a nd 0.3 mm, respectively. The XRD patterns were subsequently analyzed using the program SIROQUANT, which is based upon the Rietveld method to quantify mineralogical content (Taylor and Matulis, 1991).…”

Rietveld Quantitative Phase Analysis of OPC Clinkers, Cements and Hydration Products

“…This problem has been extensively discussed for cements (Le Saout et al 2011) so it is not further treated here. We want just to mention that this effect may be corrected (Brindely 1945;Taylor and Matulis 1991) but its implementation in practice is extremely difficult.…”

Insight Into the Formation of Lithium Alloys in All-Solid-State Thin Film Lithium Batteries

“…In this system the discrepancy between the calculated intensity and observed intensity can be attributed primarily to two contributions, micro-absorption and sample texturing. Micro-absorption which can arise in systems where there is a large difference in X-ray absorption coefficients between two phases (Taylor and Matulis, 1991), e.g., between Li and Bi in this system. Due to the nature of thin film samples, in which growth of films can occur along particular crystallographic planes, sample texturing can also lead to mismatch between the intensity of calculated models and the observed data for particular reflections (Zolotoyabko, 2009).…”