Journal
ANALYTICAL METHODS
Volume 5, Issue 5, Pages 1231-1237Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/c2ay26411k
Keywords
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Funding
- EU research network Northern Sweden Soil Remediation Centre
- Kempe foundation
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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 intercalibration 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.
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