Determination of non-extractable residues in soils: Towards a standardised approach

After exposure of soils to anthropogenic organic chemicals non-extractable residues (NER) can be formed. The quantitative proportion of a compound which remains non-extractable is operationally defined by the extraction procedure employed and can be quantified only when using isotope labelled compounds (e.g. ¹⁴C or ¹³C). In Germany and the EU, there is no standardised procedure, how to determine NER, especially when different legal regulations apply. Consequently, the comparability of NER data is low. Hence, a major task of this study was the development of a general approach for the quantification of non-extractable residues (NER) in soils using radiotracer analysis. For that, extraction efficiencies were determined for 42 non-labelled organic chemicals spiked onto 3 soils applying a number of extraction techniques and conditions, developing an extraction procedure which provides high extraction efficiencies and a low variability for a broad spectrum of analytes. Additionally, NER generated within soil transformation studies according to OECD 307 using ¹⁴C-triclosan, ¹⁴C-fenoxycarb and ¹⁴C-acetaminophen were analysed using sequential batch extraction and pressurised liquid extraction (PLE). Depending on the extraction procedure used, the NER fraction related to ¹⁴C-triclosan in a soil varied greatly between 96% and 28%. In this study a widely universal extraction procedure was developed to improve the comparability of the NER data and limit overestimation of NER, which can be of enormous consequence for the assessment of persistence and environmental risk of organic chemicals. Furthermore, silylation, EDTA-extraction and HCl-treatment were compared regarding a further analysis of NER using radiotracer analysis.