This study was undertaken to investigate the feasibility of applying the Fered-Fenton process to the degradation of m-phenylenediamine, by examining the effect of varying the initial H2O2 and Fe(2+) concentrations, the initial pH and electric current on the process efficiency. The degradation behavior of m-phenylenediamine was also compared to that of aniline. The Fered-Fenton reactor consists of anodes and cathodes with mesh-type titanium metal coated with IrO2/RuO2 and stainless steel, respectively. The experiments showed that m-phenylenediamine was rapidly degraded by the Fered-Fenton process. Initial pH of 3.2 is optimal for the removal of m-phenylenediamine and chemical oxygen demand (COD). m-Phenylenediamine and COD removal efficiencies increased with the increasing electrical current from 0 A to 4 A, and decreased with a further increase in electrical current. Optimum efficiency resulting in 100% degradation of m-phenylenediamine and elimination of 30% of COD was achieved at pH 3.2 at 60 min in the presence of 10 mM of m-phenylenediamine, 0.268 mM of Fe(2+), 43.6 mM of H2O2, and under a current of 4 A.