Optimization of a microwave-assisted extraction method for the analysis of polychlorinated biphenyls in ash samples

An alternative method for the extraction of polychlorinated biphenyls (PCBs) in ash samples, which is less time and solvent consuming than Soxhlet extraction, is presented. A study was carried out to evaluate the possibilities of microwave-assisted extraction (MAE) to determine exactly which parameters affect the efficiency of the process, since direct extrapolation of extraction conditions for PCBs in other solid matrices, failed when applied to coplanar congeners in ash samples. Influence of the organic solvent on the yield of the extraction was first evaluated using two ash samples with different percentages of carbon. Once the extraction solvent was fixed, the effects of solvent volume, extraction temperature and extraction time were investigated using an experimental design. It was found that the volume of organic solvent played a more important role in the extraction efficiency than the other factors. In the optimal conditions microwave extractions were performed at 110degreesC, for 10 min and using 30 ml of toluene. Recoveries higher than 80% were obtained for all the highly chlorinated congeners, including coplanar species, in a spiked ash sample containing a relatively high concentration of carbon. The proposed method was also applied to the determination of PCBs in a reference material of urban dust. Recoveries were similar to those obtained for spiked ash samples. (C) 2002 Elsevier Science B.V. All rights reserved.