The UV/TiO2/H2O2 degradation of Basic Yellow 28 dye (BY28) in aqueous solutions was investigated with immobilized P-25 TiO2 powder on a glass plate by a heat attachment method. A central composite design (CCD) was employed for the screening of the significant parameters (flow rate, initial dye concentration, solution pH, and initial H2O2 concentration) and to identify the most relevant interactions between the operating parameters. Results showed that solvent type and thickness of the coating are very effective on the photoactivity of immobilized TiO2. The model equation obtained led to a classification of the parameters based on their level of significance. In addition, a relevant interaction between the initial dye concentration and the initial H2O2 concentration was highlighted. After performing a screening of the various operating parameters, response surface analysis led to the optimal conditions for the yield of BY28 degradation, resulting in 96% decolorization yield.