The photocatalytic activity and stability of 3% Fe-TiO2 materials synthesized by incipient wet impregnation (% Fe-TiO2-DP25) and sol-gel (3% Fe-TiO2-sol-gel) were studied using the phenol degradation as test reaction. The effects of various operation parameters including photocatalyst concentration, solution pH and initial H2O2 concentration on phenol degradation were also investigated. The higher phenol degradation was achieved using 26 mg of photocatalyst, H2O2 initial concentration of 600 mg/l and initial pH of 3.0 with both materials. It was found that 3% Fe-TiO2-DP25 enhanced activity, achieving a 99% phenol degradation, in comparison with 70% phenol degradation with the 3% Fe-TiO2-sol-gel. Notwithstanding, the material prepared by incipient wet impregnation method, evidenced leaching of iron ions from the material surface. Therefore, this catalyst is not suitable for the phenol degradation for environmental and economic reasons. The catalyst prepared by the sol-gel method did not show iron leaching during the reaction and maintain its catalytic activity after several reuses.