The kinetics of the oxidative degradation of an azo dye Metanil Yellow (MY) was investigated in aqueous solution using dirhodium(II) caprolactamate, Rh2(cap)4, as a catalyst in the presence of H2O2 as oxidizing agent. The reaction process was followed by UV/Vis spectrophotometer. The decolorization and degradation kinetics were investigated and both followed a pseudo-first-order kinetic with respect to the [MY]. The effects of various parameters such as H2O2 and dye concentrations, the amount of catalyst and temperature have been studied. The studies show that Rh2(cap)4 is a very effective catalyst for the formation of hydroxyl radicals HO• which oxidized and degraded about 92% of MY into CO2 and H2O after 24 h as measured by total carbon analyzer.