Peroxicoagulation treatment of aqueous solution containing hazardous dye, Rhodamine B, with commercially available graphite as cathode and iron as anode has been studied. The effect of various operational parameters such as solution pH, applied voltage, electrode area, other ions, etc. on the dye removal was investigated. The experimental result showed that pH-regulated peroxicoagulation system is an efficient process for the dye removal. Ninety-five percent of the dye was removed after 180 min of electrolysis. Anions such as carbonate, bicarbonate, chloride and sulphate negatively affected the efficiency of peroxicoagulation system. From the present study, it can be concluded that peroxicoagulation process is an efficient tool for dye removal from aqueous solution.