The paper deals with the degradation of nitrobenzene (NB) by advanced catalytic oxidation based on an anodic Fenton’s reagent. . The degradation or the conversion of nitrobenzene in to CO2, H2O and other minerals was performed by electrochemical method in the electrolysis system with direct current, with the iron anode section volume of 53ml, with potential 2.5 V, consisting of EDTA (1mM), O2 (10mg/l), Na2SO4 (0.1M), the graphite cathode section volume of 53ml consisting electrolyte of Na2SO4 (0.1M). Concentrations of NB during electrochemical degradation were monitored using high-performance liquid chromatography, (HPLC, Aligent USA). The electrochemical degradation of NB can be explained by the free radicalOH· generated during electrolysis using direct current with iron anode in presence of EDTA, oxygen in weak acid pH – solution.