A rapid method for the separation of 210 Po from 210 Pb was developed utilizing extraction of triisooctylamine (TIOA)/xylenein HCl+H2O2 medium. Polonium in the form of PoCl 62– was extracted into TIOA phase and 210Pb remains in the aqueous phase. Lead-210 was determined by -countingof its granddaughter, 210 Po ingrown from 210 Pb forsome period of time. Distribution of 210 Po and 210Pb in TIOA and aqueous phases was investigated in various concentrations ofHCl media. Hydrogen peroxide was used to further decompose organic matterand to remove sulfur to prevent its deposition on the silver disc. The improvedprocedure resulted in a good chemical yield (80–95%) and a good á-resolution.