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DIVISION S-2-SOIL CHEMISTRY

A digestion method for trace metals recovery from oil and grease contaminated soils

^a CSIRO Land and Water, Adelaide Lab., Glen Osmond, SA 5064, Australia, current)
^b Dep. of Natural Resource Sci., McGill Univ. - Macdonald Campus, 21,111 Lakeshore Rd., Ste. Anne de Bellevue, QC, Canada H9X 3V9

williamh{at}nrs.mcgill.ca

ikkin3{at}hotmail.com

Oil and grease contaminated soils are difficult to digest using the common HNO₃–H₂O₂ digestion method. Even after an overnight pre-digestion with HNO₃ and subsequent heating, the addition of H₂O₂ caused violent reactions in soils with oil and grease, resulting in the loss of the samples. At low metal concentrations at least a gram of soil needs to be digested to obtain concentrations measureable by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma–atomic emission spectrometry (ICP-AES). We developed a modified procedure using HNO₃–HClO₄ for the analysis of total trace metals that can be used on all types of soils including those with oil and grease. Recovery rates of 99, 94, 114, 92, and 83% for Cd, Cu, Ni, Pb and Zn, respectively, were obtained for standard reference material (SRM) NIST 2710 (Montana Soil). Soils with 1000 mg kg^-1 oil and grease were successfully digested and gave extract concentrations suitable for analysis on FAAS or ICP-AES. Compared to the common HNO₃–H₂O₂ soil digestion method, the proposed method was as effective (no significant difference) in extracting Cu, Pb, and Zn and was significantly better in liberating Ni from the soil. With the HNO₃–H₂O₂ soil digestion method the Cd concentrations were often below the limit of detection by FAAS but were measureable in the HNO₃–HClO₄ digests. Variability of results using the proposed method was reduced in some cases.

Abbreviations: ETAAS, electrothermal atomic absorption spectrometry • FAAS, flame absorption spectrometry • FAES, flame atomic emission spectrometry • HF, hydrofluoric acid • ICP-AES, inductively coupled plasma-atomic emission spectrometry • ID, isotope dilution • INAA, instrumental neutron activation analysis • POLAR, plarography • RNAA, radiochemical neutron activation analysis • SRM, standard reference material • TIMS, thermal ionization mass spectrometry