Investigation of the influence of particle size on the quantitative analysis of glasses by energy‐dispersive micro x‐ray fluorescence spectrometry

Abstract

Abstract Micro x‐ray fluorescence analyses were undertaken on individual glass particles of different compositions for selected particle sizes between 50 µm and ≥1 mm. These experiments revealed a complex behaviour in the fluorescence spectra; this behaviour is influenced by the glass matrix, topology, particle volume, energy range and polycapillary properties and cannot be corrected by simple approaches. Net fluorescence intensities and reproducibility measured with two different polycapillaries (40 and 60 µm) were evaluated for six element lines between 1 and 10 keV and compared with the same standard glasses provided as ideal specimens (i.e. with flat, polished surface and of ‘infinite’ thickness). A standardless quantification using the fundamental parameter model gave a reasonable accuracy for particle sizes ≥1 mm ( ca 15% relative standard deviations for the main elements) without further sample preparation. The feasibility of principal components analysis for a fast identification of compositional types using the measurement data of individual particles was demonstrated. Copyright © 2002 John Wiley & Sons, Ltd.