Accuracy of calibration procedure for energy‐dispersive x‐ray fluorescence spectrometry

Abstract

The quality of a calibration procedure was studied in terms of the accuracy of the calibration factors. In particular, the influence of the uncertainties of the incident and emerging angles and of the mass absorption coefficients on the calibration factors was described theoretically for a calibration procedure based on standard samples of any thickness. The calculations were carried out for an x-ray tube and a radioisotope excitation set-up. Practical consequences of the inaccuracies of the calibration factors were also demonstrated for a few test samples of intermediate thickness analysed by the emissiowtransmission method.

Quantitative X-ray fluorescence analysis of samples of less than ‘infinite thickness’: Difficulties and possibilities

“…The accuracy of the analysis of intermediate-thickness samples based on E-T method is discussed in Refs. [105][106][107]. Sitko and Jurczyk [108] proposed a 'two masses' (2M) method as an alternative to the E-T method.…”

Activities in the IAEA X‐ray fluorescence laboratory at Seibersdorf

“…The quality of the calibration (or accuracy of the calibration factors) depends on the uncertainties due to counting statistics and uncertainties in the concentrations of the elements in standard samples. A general approach was proposed 19 to evaluate an overall accuracy of a calibration procedure due to uncertainties of the incident and emerging angles and the mass attenuation coefficients for thin, intermediate thickness and thick standard samples. The approach was used for both an x-ray tube and radioisotope excitation EDXRF set-ups.…”

“…As the method allows identification of the major sources of the uncertainties, it can be used for the selection of the optimum calibration strategy for any EDXRF spectrometer. 19 In order to use a fundamental parameter method for quantification in a radioisotope excitation XRF setup, the effective incident and take-off angles should be evaluated carefully. However, because of a broad geometry, evaluation of the angles is not a trivial task and can be done either theoretically or experimentally.…”

“…Training programmes at the XRF Laboratory provide an opportunity not only for developing practical skills on XRF methodology and instrumentation but also to take part in research and development towards MSc and PhD degrees. Often the research projects included in the training programmes help to develop analytical procedures for special applications or to contribute to methodological advancement 1,6,8,12,19,26,29,36,37.…”

Theoretical influence coefficients for correction of matrix effects in x‐ray fluorescence analysis of intermediate‐thickness samples

“…mass-absorption coefficients and fluorescent yields, have an influence on the accuracy of analysis results to a lesser extent and better results can be expected when using FP methods in comparison with thick samples. 13 The databases of atomic parameters are still being compared and developed to obtain high-quality analytical results. 14,15 The mentioned FP methods are very flexible and versatile, and can be applied in the analysis of samples in which all the elements or compounds are quantified, e.g.…”