Semi-Quantitative XRD Analysis of Fly Ash Using Rutile as an Internal Standard

Abstract

AbstractXRD analysis of fly ash was quantitated using the Reference Intensity Ratio (RIR) method and rutile (TiO2) as an internal standard. Rutile RIR's for 15 of the crystalline phases commonly observed in North American fly ash were determined. Error analysis on the various steps in quantitation indicated that precision ranged from ±10% of the amount present for phases that diffract x-rays strongly to ±21% for weakly diffracting phases. Limit of detection in the mostly glassy fly ashes ranged from 0.2% for lime, the most strongly diffracting phase, to 3.5% for weakly diffracting mullite. Accuracy evaluated with a simulated fly ash was within the limits established by precision, but in actual fly ash samples, accuracy will be a function of the match between the crystallinity and composition of the analyte and the analyte standard. Overlaps among peaks of some of the important phases require intensity proportioning; for this reason, the method is best described as semi-quantitative.