A modified (one-cycle) Purex process has been developed for the separation and recovery of plutonium and uranium from mixed actinide residues. The process utilizes 30 vol % tributyl phosphate--dodecane to extract uranium from a 5M nitric acid-plutonium (III)-uranium(VI) feed. After uranium extraction, plutonium in the aqueous feed solution is purified by anion exchange technology. Uranium in the organic is scrubbed and stripped to effectively purify the uranium so that it contains <5,000 ppM plutonium. The process has been used successfully to separate residues consisting of plutonium and uranium oxide.