In this study, ozone-oxidation was used to treat synthetic chemical plating solution containing Cu(II)/Ni(II)-EDTA solution to realize the purpose of decomplexation. The effects of solution pH, initial concentration of Cu(II)/Ni(II)-EDTA, the molar ratio of EDTA to Cu(II)/Ni(II), and the coexistence of Cu(II)/Ni(II) on their removal efficiencies were investigated. The degradation of EDTA-Cu(II) and EDTA-Ni(II) were mainly attributed to OH oxidation, and the removal rates of Cu(II)/Ni(II) depend on the complete decomplexation. The removal rates of Cu(II) and Ni(II) was affected by the pH of solution, and the optimal pH was found to be 7–9; nevertheless, their removal rates can still be up to 90% even in acidic pHs of 3~5. When the molar ratio of EDTA to Cu(II)/Ni(II) increased from 1:1 to 3:1, the kinetics of metal ion removal rate declined from 0.0788 and 0.1139 min-1 to 0.0250 and 0.0271 min-1. The synergistic effect was found in the Cu(II)/Ni(II) blended system due to the higher catalytic capability and the lower complexation affinity toward EDTA for Ni(II). In summary, ozone oxidation can be considered as an effective technology to realize the complete decomplexation of Cu(II)/Ni(II)-EDTA that contained in chemical plating industry wastewater.