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Separations research at the Rocky Flats Plant /RFP/ has found ways to significantly improve plutonium secondary recovery from nitric acid waste streams generated by plutonium purifications operations. Capacity and break-through studies show anion exchange with Dowex 1×4 /50–100 mesh/ to be superior for secondary recovery of plutonium. Extraction chromatography with TOPO /tri-n-octylphosphine oxide/ on XAD-4 removes the final traces of plutonium, including hydrolytic polymer.