Abstract: Natural iron is plated on copper to be irradiated by 7.5 MeV deuteron to produce 57Co through the reaction 57Fe (d, n) 57Co. The irradiated target after cooling is dissolved in 9 N HC1 with the addition of H2O2 to bring the Fe into the trivalent state. The solution is evaporated to dryness and redissolved in enough 4 N HC1 to make the Fe3+ concentration smaller than 10 mg/ml, and TBP-C6H6 (1:1) is added to remove 99.82% of the Fe3+ in the aqueous phase. A procedure is described for the recovery and purification of 57Co from the aqueous phase by means of ion exchange, The percentage recovery of 57Co is 95%, which is qualified for use as a Mossbauer source with a line width of 0.104-0.114 mm/s.