This study focused on the action of Fe~(2+)/UV/H_(2)O_(2) in degradation of aniline and nitrobenzene. Wastewater containing aniline and nitrobenzene flowed through a resin (H-103) column for primary treatment by adsorption. The experimental investigation showed a remarkable decomposition of aniline and nitrobenzene with removals of 99.7% and 95.3% respectively.