Thesis

Determination and fractionation of potentially toxic elements in urban particulates

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Awarding institution
  • University of Strathclyde
Date of award
  • 2013
Thesis identifier
  • T13645
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Abstract
  • Urban environmental pollution is of increasing concern. There is a need for improved analytical methods to assess risk from potentially toxic elements in urban soils and related material. This thesis focuses on development and application of such methods, notably the modified BCR sequential extraction procedure. The analytes studied were Cr, Cu, Fe, Mn, Ni, Pb and Zn, and quantification was by ICP-AES and ICP-MS. Results obtained by BCR extraction of urban allotment soils were compared with those from aqua regia digestion, 0.05 M EDTA extraction, and the SBET. Correlation analysis and principal component analysis (PCA) grouped analytes into a set mainly of lithogenic origin (Cr, Fe, Mn,Ni) and another of mainly anthropogenic origin (Cu, Pb, Zn). The PCA indicated relationship between amounts of analytes released in step 1 of the sequential extraction and EDTA-extractable analytes, and between results of the SBET method and those obtained with EDTA. The BCR extraction was then miniaturised for application to urban airborne particles. The fractionation pattern was not affected by reducing the sample mass from 1 g to 0.0625 g for particles < 45 μm and 500 - 1000 μm in diameter, but changing the size of vessel used did have an effect. When the miniaturised extraction was applied to test samples presented on filter dynamics measurement system (FDMS) filters a significant Zn blank was found. Despite this, recoveries within 30 % of certified values were obtained when 0.1 g test portion of BCR CRM 701, loaded onto FDMS filters, were extracted. Finally, the chemometric identification of substrates and element distribution (CISED) method was miniaturised and adapted for application to particulate samples on FDMS filters. Four distinct physicochemical components were extracted from BCR 701 using the traditional CISED method, but 11 components when the CRM was loaded onto a filter. The mobilities of the PTE as predicted by the CISED were in good agreements with fractionation patterns obtained using the BCR sequential extraction protocol.
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DOI
Date Created
  • 2013
Former identifier
  • 1004645

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