The photo-oxidation of Rhodamime B was carried out in the presence of H2O2/ Fe2+ ion using UV light. The effects of dye concentration, pH, H2O2 dose and Fe2+ dose. These parameters strongly influenced the degradation of the dye. As expected, the increase of initial dye concentration decreased the percentage decoloration. Likewise increasing H2O2, Fe2+ concentration also increased the dye decoloration up to a certain limit after which it starts decreasing. The optimum operating conditions of the method were found to be [Dye] = 10mg/l; [H2O2] = 300mg/l; [Fe2+] = 250 mg/l at pH 2. Under these conditions, a maximum of 92% decoloration of the dye was achieved. The actual breakdown of the dye was confirmed using HPLC analyses.