The formation property of Mo precipitate was investigated and improved the existing process was using H2O2 that acts as an interfering compound in a subsequent alumina adsorption process. The property of the Mo precipitate was investigated by using SEM, FTIR, TG-DTA, and XRD. The simulated solution consisted of 1M nitric acid containing seven elements (Mo, I, Ru, Zr, Ce, Nd, Sr) and their radioactive tracers. As a result, the precipitate was composed of the Mo precipitate and re-precipitated a-benzoinoxime which was added excessively for increasing the precipitation efficiency. It was confirmed that the Mo precipitate was formed by the reaction of two a-benzoinoxime molecules and one MoO22+. Molybdenum precipitate was dissolved in 0.4M NaOH solution within 5 minutes without H2O2. Hydrogen peroxide induced only the rapid dissolution of the a-benzoinoxime re-precipitate. Also, the dissolution method without H2O2 was favorable in the purification aspect because Zr and Ru were contained as a small fraction of 1.3% and 7.7%, respectively, in the dissolving solution.