Effluents from production of petroleum bitumens were submitted to treatment by three different AOPs at basic pH (i.e., O-3, H2O2 and the combination of O-3 and H2O2, a so-called peroxone). The paper presents studies on the identification and monitoring of the volatile organic compounds (VOCs) degradation present in the effluents and formation of byproducts, COD, BOD5, sulfide ions, biotoxicity, and biodegradability changes during treatment. Peroxone at 25 degrees C with a ratio of oxidant in relation to the COD of the effluents (r(ox)) of 0.49 achieved 43% and 34% of COD and BOD5 reduction resulting in the most effective AOP studied. S2- ions were effectively oxidized in all technologies studied. Ozonation at 25 degrees C and with a r(ox) of 0.34 was the most effective process to degrade VOCs. Decrease in the biotoxicity was reported in O-3 and peroxone processes. Byproduct formation in different AOPs was reported. These reductions revealed that these technologies are effective if used as pretreatment methods.