Phase Guard: A False Positive Filter for Automatic Rietveld Quantitative Phase Analysis Based on Counting Statistics in HighScore Plus

Abstract

Accurate quantification of minor mineral phases is important in Powder X-Ray Diffraction (PXRD) and Rietveld phase quantification. The precise limit of quantification for the various phases is rarely considered but rather approximated to 0.2–2 wt% by applying a global minimum weight percentage threshold. This approximation often leads to false positive or false negative phase quantity, jeopardizing the trustworthiness of the analytic method in general. In this work (1) we propose a dynamic and adaptable false positive filtering method for Rietveld Quantitative X-ray diffraction (QXRD) based on a phase-specific signal-to-noise ratio referred to as “Phase-SNR”; (2) we introduce the method baptized “Phase Guard” which is implemented in the software HighScore Plus. Phase Guard is based on peaks counting statistics and it automatically adapts to different mineral scattering powers, different mineral crystallinity, instrumental configuration and measurement time. Its applicability and benefits are demonstrated with several examples in cement and mining applications. The adoption of Phase Guard is especially beneficial for industrial black-box solutions, where all “probable” phases are included in the model, even when they are absent from the sample. Phase Guard eliminates false positives, it reduces the likelihood of false negatives, and it is an essential tool to answer the question “what is the limit of quantification for Rietveld analysis?”