Comparison of techniques for the analysis of industrial soils by atomic spectrometry

Methods based on AAS, ICP-AES and XRFS have been developed for determinatio n of Cd, Cr, Cu, Mn, Ni, Pb, V and Zn in soil layers from pits excavated on a redundant industrial site. Samples were dried and sieved, and the < 2 mm fraction was ground in a ball mill prior to analysis. For ICP-AES and AAS, Ig sub-samples were digested with aqua regia in a microwave oven. The dry weight detection Limits of the analytes were in the range 2-25 mu g g(-1) f or FAAS, 0.003-0.2 mu g g(-1) for ETAAS and 0.04-1.6 mu g g(-1) for ICP-AES . When digests of the industrial soils were analysed, calibration with acid -matched standards gave acceptable accuracy for all the analytes, except fo r Cd when determined by ETAAS (30-40 % suppression). Despite lack of refere nce materials of industrial origin, analysis of two soil reference material s by these techniques produced concentrations that were within +/- 10 % of the certified or recommended values for elements extractable with aqua regi a. Direct standard-less analysis of a soil reference material with a portab le x-ray fluorescence (P-XRF) analyser gave concentrations for a range of e lements that were within a factor of 2 of the certified values. When the XR FS and ICP-AES methods were used to analyse the industrial soils, the conce ntrations obtained were similar (to within 30%) for Cu, Pb and Zn in most o f the samples and for Cr, Mn and Ni in some of the samples. The concentrati ons of V estimated with the P-XRF analyser were 4 to 7-fold higher than tho se obtained by ICP-AES. The discrepancies were thought to be caused by spec tral enhancement interferences in XRFS. Cadmium was not determined accurate ly by either ICP-AES or P-XRFS owing to spectral interferences. The work ha s highlighted the importance of analysing samples from across a site and at different depths, when assessing the extent of metal contamination on indu strial land.