A method for analysis of a single tooth or small samples of bone for Po210, Ra226 and Ra224 is described. Polonium is separated by deposition on silver; radium is isolated by a two-stage coprecipitation with lead and barium sulfate. Radium 224 is distinguished from Ra 226 by nonrandom decay of its daughters, or by analysis of the time course of growth or decay of alpha-activity. There was nearly complete chemical recovery of Po210, and chemical recovery of radium was 74%. The coefficient of variation for chemical recovery was 7% for poloniun and 9% for radium. Combined separation and counting efficiency for Po was 51% and for Ra 33%. The chief advantages of the method are its simplicity and the relatively short time necessary for chemical analysis. Simultaneous analyses of Po 210, Ra226 and Ra224 can be done on the same small sample of calcified tissue and an ash content of 2gm or less is suitable. The method requires long counting periods for alpha-activity in low background proportional counters. It gave results in good agreement with those obtained by other laboratories using different methods.