Abstract

Robust analytical procedures for the measurement of decamethylcyclopentasiloxane (D 5) in river and estuarine sediments and their application in determining environmental concentrations in the UK are presented for the first time in this work. Novel approaches to minimise commonly reported artefacts are utilised, improving the confidence in the concentrations of D 5 reported. Accelerated solvent extraction (ASE) and liquid–solid extraction methods are compared. Both methods use on-column injection gas chromatography/mass spectrometry (GC/MS). Measurements of D 5 concentrations in sediments sampled from the river Great Ouse and from the Humber estuary (UK) are also reported. ASE was suitable to measure concentrations of D 5 in sediments obtained from the river Great Ouse, UK (186–1450 ng g −1, dry weight) and octamethyltetracyclosiloxane (D 4, 12–24 ng g −1, dry weight). C 12 linear alkybenzene (C 12 LAB), which can be used as a chemical marker for sewage effluent related emissions, was also measured in this analysis. Liquid–solid extraction was optimised to provide more confidence in the lower D 5 concentrations measured in the Humber estuary, UK (49–256 ng g −1, dry weight). A Limit of quantitation (LOQ) for D 5 of 57–110 and 4 ng g −1 dry weight was determined for ASE and liquid–solid extraction, respectively.

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