In this work, the response surface methodology was applied as a tool for the optimization of the operational conditions of phenol photo-degradation over Ti O2 and 2% wt Mo/TiO2 catalysts. A multifactorial experimental design was proposed, including the following variables: phenol initial concentration (Ci), catalyst loading (Cat) and pH. The apparent reaction rate constant and the percentage of phenol degradation were chosen as the response variables. When TiO2 was used as catalyst, the following optimal operational conditions were found: Ci=10ppm, Cat=0.7g/L and pH=8 for both UV and visible light. For 2% wt Mo/TiO2 catalyst, the optimal operating conditions strongly depended on the applied radiation source. Thus, under UV radiation: Ci=10 ppm, Cat=0.7 g/L and pH=8 were found as the optimum conditions. Using visible light, and the following optimized conditions, Ci=10 ppm, Cat=0.1 g/L, pH =3.6, the Mo containing catalyst showed to be the most efficient. Under these conditions, the amount of 2% wt. Mo/TiO2 was 7 times lower than that of unsupported TiO2. [ABSTRACT FROM AUTHOR]