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

Anderson, Peter and Davidson, Christine M. and Littlejohn, David and Ure, Allan M. and Garden, Louise M. and Marshall, John (1998) Comparison of techniques for the analysis of industrial soils by atomic spectrometry. International Journal of Environmental Analytical Chemistry, 71 (1). pp. 19-40. ISSN 0306-7319

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Methods based on AAS, ICP-AES and XRFS have been developed for determination 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) for 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 for Cd when determined by ETAAS (30-40 % suppression). Despite lack of reference materials of industrial origin, analysis of two soil reference materials by these techniques produced concentrations that were within +/- 10 % of the certified or recommended values for elements extractable with aqua regia. Direct standard-less analysis of a soil reference material with a portable x-ray fluorescence (P-XRF) analyser gave concentrations for a range of elements that were within a factor of 2 of the certified values. When the XRFS and ICP-AES methods were used to analyse the industrial soils, the concentrations obtained were similar (to within 30%) for Cu, Pb and Zn in most of the samples and for Cr, Mn and Ni in some of the samples. The concentrations of V estimated with the P-XRF analyser were 4 to 7-fold higher than those obtained by ICP-AES. The discrepancies were thought to be caused by spectral enhancement interferences in XRFS. Cadmium was not determined accurately by either ICP-AES or P-XRFS owing to spectral interferences. The work has highlighted the importance of analysing samples from across a site and at different depths, when assessing the extent of metal contamination on industrial land.