Supercritical fluid extraction of polychlorinated dibenzo‐<i>p</i>‐dioxins from municipal incinerator fly ash

Abstract

Abstract The supercritical fluid extraction of polychlorinated dibenzo‐ p ‐dioxins from an incinerator fly ash sample has been investigated; supercritical nitrous oxide and its mixtures with methanol and toluene were employed as mobile phases. Recoveries of individual polychlorinated dibenzo‐ p ‐dioxins congeners were calculated from results of analysis of 13 C‐labeled dioxins by high resolution GC‐MS employing selected ion monitoring. The extraction procedure was compared with extraction in a Soxhlet apparatus, which is currently used as a standard method for removing chlorinated dibenzo‐ p ‐dioxins from fly ash samples: the results indicated that the time required for the extraction and clean‐up can be reduced from 24 to 2.5 hours/sample. Quantitative recovery of the chlorinated dibenzo‐ p ‐dioxins was achieved at μg/kg levels, the relative standard deviation was between 1.8 and 5.8%. The use of a virtually inert fluid such as pure nitrous oxide provides significant improvement over conventional extraction procedures because no solvent residue is left in the processed extract.