Abstract: Technological conditions for treating a 50μg ~(252)Cf neutron source in hot cellare investigated. The process included following steps: disso1ution of stainless steelcladding and Pd-Cf_2O_3 cermet, removal of chloride ion by distillation, extraction of Cfand Cm with 50% TBP, absorption of Pd With EDTA chelating resin and separation ofCf from Cm by 1-methylheptyl phenylphosphonic acid(P5706) extraction chroma-tography. Process could be realized in a hot. cell, Yield of Cf in chemical processis more than 90%. Satisfactofy separation of Cf from Cm and other cations forFe, Pd and so on could be obtained. Purified Cf is used in research work onnuclear physics and radiochemistry.