Analysis Of Sediments And Soils By X-ray Fluorescence Spectrometry Using Matrix Corrections Based On Fundamental Parameters

Wavelength dispersive X-ray fluorescence spectrometry (WD-XRF) is widely used for the analysis of soils and sediments using well characterised procedures. However, difficulties can occur with samples such as unknowns containing small amounts of ore materials and samples collected from contaminated sites where trace elemental concentrations can exceed the concentration range for routine analysis. We studied the performance of a commercially available method, based on fundamental parameters (FP) to correct matrix effects. The spectrometer was originally calibrated with elemental or simple compound calibrants. Samples were analysed as pressed powder pellets. Eighteen sediment and soil reference materials, three of them with certified values for some of their constituents, were used to evaluate accuracy, by comparing results with recommended values and their standard deviations (RV ± 2s) or certified values and their confidence intervals (CV ± Cl). When results fell systematically outside these intervals, calibrations were refined with geochemical reference materials. The best agreement of results with recommended and certified values was obtained when the contents of H 2O and C in each sample were included as matrix constituents during calculations. The detection limits of trace elements tended to be relatively high, because the measuring conditions employed were not maximised for sensitivity. The main advantage of the method tested was that it enabled the analysis of samples with high concentrations of trace elements and the determination of elements such as F, Bi, Sb and W, which are not commonly included in quantitative XRF analysis of geological samples.281103112Borkhodoev, V.Y., Accuracy of the fundamental parameter method for X-ray fluorescence analysis of rocks (2002) X-ray Spectrometry, 31, pp. 209-218Criss, J.W., Birks, L.S., Methods for fluorescence X-ray spectrometry. Empirical coefficients versus fundamental parameters (1968) Analytical Chemistry, 40, pp. 1080-1086Gladney, E.S., Roelandts, I., 1988 compilation of elemental concentration data for USGS geochemical exploration reference materials GXR-1 to GXR-6 (1990) Geostandards Newsletter, 14, pp. 21-118Kane, J.S., Quality control and reference sample databases (1991) Geostandards Newsletter, 15, pp. 33-42Kane, J.S., Siems, D.F., Arbogast, B.F., Geochemical exploration reference samples GXR-1 to GXR-4 and GXR-6: Evaluation of homogeneity based on high precision analyses (1992) Geostandards Newsletter, 16, pp. 45-54Lachance, G.R., Claisse, F., (1995) Quantitative X-ray Fluorescence Analysis, Theory and Application, 402p. , John Wiley & Sons (Chichester)Longerich, H.P., Analysis of pressed pellets of geological samples using wavelength dispersive X-ray fluorescence spectrometry (1995) X-Ray Spectrometry, 24, pp. 123-136. , 1995Ma, G., Li, G., Application of X-ray fluorescence spectrometry to the analysis of geochemical prospecting samples in China (1989) X-Ray Spectrometry, 8, pp. 199-205Potts, P.J., A perspective on the evolution of geoanalytical techniques for silicate rocks (1998) Geostandards Newsletter. The Journal of Geostandards and Geoanalysis, 22, pp. 57-68Revenko, A.G., X-ray fluorescence analysis of rocks, soils and sediments (2002) X-ray Spectrometry, 31, pp. 264-273Xuejing, X., Analytical requirements in international geochemical mapping (1995) The Analyst, 120, pp. 1497-1504Zambello, F.R., Enzweiler, J., Multi-element analysis of soils and sediments by wavelength-dispersive X-ray fluorescence (2002) Journal of Soils and Sediments, 2, pp. 29-3