Extensive research has been carried out to figure out safe means of disposing various industrial effluents. Industrial wastewaters from the aeration industry such as heavy metals and oily substances contain a high degree of contamination. The advanced oxidation process is one of the most effective and rapid methods of removing contaminations, which can lead to a high chemical oxygen demand (COD). The aim of the present study is to reduce the COD of an aeration effluent with the initial COD of 13,004 mg/L. About 20 sets of experimental tests were conducted to identify the contribution of H2O2, O3, and UV to the treatment process. The influence of the quantities of additives and the dose of the UV irradiance were, too, among the subjects of the study. These factors were altered throughout the experiments and their mutual effects were measured. To design the experiments, Minitab software 16 was utilized. The experimental conditions were set at the standard values of 25 °C and 1 bar to minimize any uncertainty. Based on the results, a correlation was derived, which was capable of expressing the effects of the input parameters (AOPs parameters) on the response (the COD level). Finally, the optimization process was conducted to find the quantities of H2O2, O3, and UV irradiance required to decrease the CODs of the effluent to their lowest possible. Based on the findings, when the doses of H2O2, O3, and UV to the treatment process were 40 mg/L, 8 mg/L and 86 mWs/cm2, respectively, the COD percent change was 51.5%.