Extraction with a tertiary amine in hydrocarbon solution is recommended for recovery of the technetium and neptunium that can accumulate in uranium fluorination plant residues, together with recovery of the uranium for recycle. A single-cycle process provides coextraction of these three elements and separation by consecutive stripping, giving good recoveries and relatively high mutual separation. The chemical flowsheet has been tested through the stage of continuous countercurrent demonstration in laboratory scale equipment using a commercial tertiary amine to process actual plant feed solution.