A B S T R A C TA statistical optimization of Reactive Red 141 (RR141) removal by heterogeneous photoFenton reaction using ZnFe 2 O 4 particles was performed. ZnFe 2 O 4 oxide was synthesized by microwave-assisted solvothermal route and characterized by X-ray diffraction, Fourier transform infrared spectroscopy, and N 2 adsorption-desorption isotherms. This material was used as a catalyst for the removal of RR141 dye from aqueous solution. Statistical optimization for the RR141 removal was performed using a 2 4−1 fractional experimental design, followed by the response surface methodology. Effects of pH, reaction time, dye concentration, and H 2 O 2 concentration were evaluated. ZnFe 2 O 4 particles presented a mesoporous structure with surface area of 65 m 2 g −1 . It was found that the more adequate conditions for the RR141 dye removal were pH 2.0, reaction time of 60 min, dye concentration of 60 mg L −1 , and H 2 O 2 concentration of 10 mM. In these conditions, 90% of color removal was achieved. The results demonstrate that the ZnFe 2 O 4 oxide is an efficient catalyst for the removal of RR141dye from aqueous solution through the heterogeneous photo-Fenton reaction.