This study investigates the ozonation of 2-naphthalenesulfonate (2-NS) combined with UV radiation in the electroplating solution. 2-NS is commonly used as a brightening and stabilization agent in the electroplating solution. Semibatch ozonation experiments were conducted under various reaction conditions to study the effects of ozone dosage and UV radiation on the oxidation of 2-NS. The concentrations of 2-NS were analyzed at specified time intervals to elucidate the decomposition of 2-NS. Total organic carbon (TOC) is chosen as a mineralization index of the ozonation of 2-NS. In addition, values of pH and oxidation reduction potential were continuously measured in the course of experiments. As a result, the nearly complete mineralization of 2-NS via the ozonation treatment can be achieved. The mineralization of 2-NS is found accelerated by the introduction of UV radiation and has a distinct relationship with the consumption of applied ozone. These results can provide useful information for the proper removal of 2-NS in the electroplating solution by the ozonation with UV radiation.