Stack emissions from five sources (one pulverized coal combustion operation, three sewage sludge incineration operations and one gray tin refractory operation) were sampled by use of U.S. EPA Modified Method 5 isokinetic sampling unit for vapor and particulate effluent. The sampling unit provided XAD-2 resin samples, polytetrafluoroethylene and glass fiber filters and impinger washings of dichloromethane. The resins were soxhlet extracted using dichloromethane (DCM) and the filters were soxhlet extracted using DCM followed by acetone. Fractionation of extracts was accomplished by thin layer chromatography. The resulting fractions were analyzed for polycyclic aromatic hydrocarbons (PAH), nitro-PAH and quinone-PAH by high-performance liquid chromatography (HPLC). Extractable organic matter (EOM) was also determined with a [sic] electrobalance. XAD samples from a gray tin refractory, and three sewage sludge incinerators higher molecular weight PAH. The volatility of the low MW PAH was responsible for the high concentration found in the resins. The lower boiling point of the higher MW PAH and the stronger association of high MW PAH with fly ash are reasons for their presence in the filter samples. No nitro-PAH or quinone-PAH compounds were detected in the emission samples. Of the four XAD resins analyzed for B(a)P by fluorescence scanning three samples showed very similar results. Concentrations from the three sources resulted from two different operations. Comparison of the HPLC results for B(a)P and fluorescence scanning of selected XAD resins have not resulted in good agreement. Phthalates tend to interfere with the HPLC chromatogram in the area where B(a)P elutes. This most likely is the reason for the disagreement. Tetrachloro-p-dibenzodioxin was observed in the resin and washings of the Parsippany Troy Hills source (sewer sludge incinerator). Heptachloro-p-dibenzodioxin was observed in the filter samples of the PSE&G source (coal combustion). The higher chlorinated species seem to form a stronger association with the particulate and a weaker association with the lower chlorinated species.