A method is described for the determination of the Po nuclides in a water sample. After the Po nuclides were purified from interfering elements in a water sample using a manganese dioxide precipitation followed by a solvent extraction method, the Po nuclides were deposited onto the silver plate. A large volume of the water sample was effectively pretreated with manganese dioxide precipitation method. To determine the optimum conditions for plating Po, the effects of the pH, volume, temperature and time on the Po deposition were investigated in hydrochloric acid solution. The investigated determination method of Po nuclides with solvent extraction was applied to a tap water sample.