Polychlorinated Biphenyls (PCBs) exist in all compartments of the ecosystem due to wide industrial applications and production during burning processes. The PCBs congeners were quantified in the industrial, municipal and agricultural wastes of the most industrialized area of the country, Raipur city, India. The concentration of ΣPCBs in the sludge, sewage and agriculture wastes (n = 4) was ranged from 497 -800 µg/kg with mean value of 634 ± 146 µg/kg. The PCBs congeners detected in the waste materials were ranged from 56 -85 with mean value of 75 ± 13. The highest number of congeners was quantified in the sludge materials due to the existence of the heavy PCBs. The PCBs congeners were found to decrease vertically due to the adsorption by the geo-media. The distribution, sources and toxicities of PCBs congeners in the waste materials are discussed.