The Fentonprocess,whichemploys Fe2+/H2O2, has been used for the treatment of azo dye-containing wastewater. Disadvantages of the Fenton process include production of large amounts of sludge and formation of a high concentration of anions in the treated wastewater. Recently, a few researchers successfully applied the ZVI/H2O2 to the treatment of dyes [1,4,5] and MTBE [6].