Advanced oxidation technologies (AOTs) are processes affected by a large number of parameters such as iron (Fe2+) and H2O2 concentrations, pH, temperature, light intensity and chemical composition (organics and inorganics). In addition, for different industrial chemical processes, there are different effluents, which greatly vary in chemical composition from each other, not allowing a unique approach for all of them. Thus, it is necessary to adjust AOT parameters to the specific effluent to be treated. In such context, statistical design of experiments (DoE) and response surface methodology (RSM) emerge as important and widely used tools to determine the effects of multiple variables on wastewater treatment processes such as photo-Fenton. A revision of academic studies based on degradation of antibiotics-containing effluents is presented. The chapter also presents commercial cases of AOT and electrical efficiency considerations.