Development of a combined solid-phase extraction-supercritical fluid extraction procedure for the determination of polychlorinated biphenyls in wastewater.

A combined solid-phase extraction (SPE)-supercritical fluid extraction (SFE) procedure was developed for the analysis of polychlorinated biphenyls (PCBs) in wastewater. The importance of cleaning and drying the filters and SPE-disks prior to eluting PCBs with SFE was studied, leading to improved recoveries for all congeners investigated. The average PCB recovery of the final procedure, at a concentration of 18 ng/L in reagent water, was 101% with relative standard deviations ranging from 1 to 5% for the different congeners. Spiked leachate to a final concentration of 4 ng/L was extracted directly after spiking, or after 24 h of spiking. An average recovery of 112% was obtained in the direct extraction of spiked leachate.