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Treatment of a dye solution containing C.I. Basic Red 46 (BR46) by homogeneous photoelectro-Fenton (PEF) combined with heterogeneous photocatalytic process was studied. The investigated photocatalyst was TiO₂ nanoparticles (Degussa P-25) immobilized on glass plates. Carbon nanotube-polytetrafluoroethylene (CNT-PTFE) electrode was used as cathode. Response surface methodology (RSM) was employed to assess individual and interactive effects of the four key factors (initial amount of Fe(III), initial concentration of the dye, reaction time and applied current) in PEF/UV/TiO₂ process. Analysis of variance (ANOVA) showed a high coefficient of determination value (R²=0.935) and satisfactory prediction second-order regression. Graphical response surface and contour plots were used to locate the optimum point. The optimum initial amount of Fe(III), initial dye concentration, reaction time and applied …