Modular pressurized liquid extraction for simultaneous extraction, clean-up and fractionation of PCDD/Fs in soil, sediment and sludge samples

Abstract

Modular pressurized liquid extraction (M-PLE) procedures were developed for simultaneous extraction, clean-up and fractionation of polychlorinated dioxins and furans (PCDD/Fs) in soil, sediment and sludge samples. The procedures utilize two coupled extraction cells: an upstream cell filled with the sample and layers of silica and acid- and base-modified silica, and a downstream cell filled with activated carbon. The silica layers were added to remove polar or hydrolysable matrix components, and the carbon to perform planarity-based fractionation. Two solvent systems (dichloromethane–heptane, DCM–Hp and diethyl ether–heptane, DEE–Hp) and two activated carbon loads (1% and 3% carbon on Celite) were evaluated using certified reference materials (CRM-529 and WMS-01) and materials from previous inter-calibration studies. Using any of the four procedures, data statistically equivalent to the certified or reference values were obtained. The M-PLE procedure using DCM–Hp and 1% carbon sometimes extracted the reference materials more efficiently than the reference methods, while the DEE–Hp procedure extracted them equally efficient, offering an alternative with less environmental impact. The methods with 1% carbon on Celite produced sufficiently pure extracts for sample loads up to one gram, but for greater sample loads the higher carbon load (3% carbon on Celite) was required to avoid breakthrough of target analytes. The new streamlined procedures are fast, cost-efficient, involve relatively low environmental impact (in the case of DEE–Hp) and are well suited for high-throughput analysis of solid samples, e.g. in connection with environmental monitoring campaigns and major soil remediation efforts.