Procedures for the sequential determination of low level (210)Po and uranium radioisotopes in drinking water by alpha-particle spectrometry are presented. After addition of (208)Po and (232)U tracers, the radionuclides were preconcentrated from water samples by co-precipitation on Fe(OH)(3) or MnO(2) at pH 9 using ammonia solution. The (210)Po source was prepared by spontaneous deposition onto a copper disc either before or after uranium separation. The uranium source for alpha-particle counting was prepared by micro co-precipitation with CeF(3). The procedures were tested on mineral water and the results obtained are compared.