Abstract

This research evaluates the analytical capabilities of a field portable X-ray fluorescence spectrometer (pXRF) for the measurement of contaminated soil samples using a matrix-matched calibration. The calibrated pXRF generated exceptional data quality from the measurement of ten soil reference materials. Elemental recoveries improved for all 11 elements post-calibration with reduced measurement variation and detection limits in most cases. Measurement repeatability of reference values ranged between 0.2 and 10% relative standard deviation, while the majority (82%) of reference recoveries were between 90 and 110%. Definitive data quality, the highest of the US EPA's three level quality ranking, was achieved for 15 of 19 elemental datasets. Measurement comparability against inductively coupled plasma atomic emission spectrometry (ICP-AES) values was excellent for most elements (e.g, r2 0.999 for Mn and Pb, r2 > 0.995 for Cu, Zn and Cd). Parallel measurement of reference materials revealed ICP-AES and ICP-MS measured Ti and Cr poorly when compared to pXRF. Individual recoveries of soil reference materials by both ICP-AES and pXRF showed that pXRF was equivalent to or better than ICP-AES values for all but two elements (Ni, As). This study demonstrates pXRF as a suitable alternative to ICP-AES analysis in the measurement of Ti, Cr, Mn, Fe, Cu, Zn, Sr, Cd, and Pb in metal-contaminated soils. Where funds are limited, pXRF provides a low-cost, high quality solution to increasing sample density for a more complete geochemical investigation.

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