Extraction of polychlorinated biphenyls from soils by automated focused microwave-assisted Soxhlet extraction.
The application of a new focused microwave-assisted Soxhlet extractor for the extraction of polychlorinated biphenyls from differently aged soils is here presented. The new extractor overcomes the disadvantages of previous devices based on the same principle and enables a fully automated extraction of two samples simultaneously. The variables affecting the extraction step (namely, power of irradiation, irradiation time, extractant volume, extractant composition and number of extraction cycles) have been optimized using experimental design methodology. The optimized method has also been applied to a certified reference material (CRM910-050 "real" contaminated soil) for quality assurance validation. Quantification of the target compounds has been performed by GC with ion-trap MS. The mass spectrometer was operated in the electron-ionization mode, with selected-ion monitoring at m/z 152, 186, 292, 326 and 498. The results obtained have demonstrated that this approach is as efficient as conventional Soxhlet but with a drastic reduction of both extraction time (70 min vs. 24 h for the "real" contaminated soil) and organic solvent disposal, as 75-80% of the extractant is recycled.
Luque-García
J L
JL
Department of Analytical Chemistry, Annex C-3, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain. q52lugaj@uco.es
de Castro
Luque
L
D001331:Automation; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D008872:Microwaves; D011078:Polychlorinated Biphenyls / Q000302:isolation & purification*; D015203:Reproducibility of Results; D012987:Soil / Q000032:analysis*
D012987:Soil; D011078:Polychlorinated Biphenyls