Polychlorinated biphenyls (PCBs) are one group of persistent organic pollutants (POPs) that are of international concern because of global distribution, persistence, and toxicity. Removal of these compounds from the environment remains a very diffi cult challenge because the compounds are highly hydrophobic and have very low solubility in water. A 900 W domestic microwave oven, pyrex vessel reactor, pyrex tube connector and condensing system were used in this experiment. Radiation was discontinuous and ray powers were 540, 720 and 900 W. The PCB S were analyzed by GC-ECD. The application of microwave radiation and H 2 O 2 /TiO 2 agents for the degradation of polychlorinated biphenyl contaminated oil was explored in this study. PCB -contaminated oil was treated in a pyrex reactor by microwave irradiation at 2450 MHz with the addition of H 2 O 2 /TiO 2 . A novel grain TiO 2 (GT01) was used. The determination of PCB residues in oil by gas chromatography (GC) revealed that rates of PCB decomposition were highly dependent on microwave power, exposure time, ratio to solvent with transformer oil in 3:1, the optimal amount of GT01 (0.2 g) and 0.116 mol of H 2 O 2 were used in the study. It was suggested that microwave irradiation with the assistance of H 2 O 2 /TiO 2 might be a potential technology for the degradation of PCB -contaminated oil. The experiments show that MW irradiation, H 2 O 2 oxidant and TiO 2 catalyst lead to a degradation effi ciency of PCBs only in the presence of ethanol. The results showed that the addition of ethanol signifi cantly enhanced degradation effi ciency of PCBs.