A procedure for separating rAaPu from a Np sample irradiated with neutrons is described. Rapid separation of Pu by HDEHP solvent extraction was attempted, and without adjusting its valency states in the dissolver solution of the sample. Both Pu(N) and Pu(VI) were extracted along with Np from the HNO. solutions of various concentrations. The Pu and Np extracted in the organic solution were backextracted with oxalic acid solutions. The decontamination factors of the crude products were of the order of lo2 for gross r-activity. The Pu in the products was separated from Np by means of ion exchange resin columns. Approximately 0.5 mg of 2 a s P~ was obtained with an efficiency exceeding 95%.