A comparison of the performance of a fundamental parameter method for analysis of total reflection X-ray fluorescence spectra and determination of trace elements, versus an empirical quantification procedure

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The performance has been compared of two different quantification methods — namely, the commonly used empirical quantification procedure and a fundamental parameter approach — for determination of the mass fractions of elements in particulate-like sample residues on a quartz reflector measured in the total reflection geometry. In the empirical quantification procedure, the spectrometer system needs to be calibrated with the use of samples containing known concentrations of the elements. On the basis of intensities of the X-ray peaks and the known concentration or mass fraction of an internal standard element, by using relative sensitivities of the spectrometer system the concentrations or mass fractions of the elements are calculated. The fundamental parameter approach does not require any calibration of the spectrometer system to be carried out. However, in order to account for an unknown mass per unit area of a sample and sample nonuniformity, an internal standard element is added. The concentrations/mass fractions of the elements to be determined are calculated during fitting a modelled X-ray spectrum to the measured one. The two quantification methods were applied to determine the mass fractions of elements in the cross-sections of a peat core, biological standard reference materials and to determine the concentrations of elements in samples prepared from an aqueous multi-element standard solution.