In five laboratory-scale experiments in which irradiated UO2 reactor fuel was processed in a fluidized bed, high removals of uranium and plutonium were achieved by oxidizing with O2, fluorinating with BrF5 to convert uranium to volatile UF6, then fluorinating with F2 to convert plutonium to volatile PuF6. The principal activities volatilized during the oxidation step were ∼ 27% of the krypton and ∼ 3.5% of the ruthenium. During the uranium separation step, >99.5% of the uranium and <0.5% of the plutonium volatilized with ∼ 60% of the ruthenium, ∼ 67% of the krypton, ∼76% of the molybdenum, and ∼2.7% of the antimony. During the F2 step, the principal activities that volatilized concurrently with the plutonium were ∼ 38% of the molybdenum, ∼8% of the ruthenium, ∼ 0.2% of the zirconium, ∼ 5.8% of the niobium, ∼ 1% of the antimony, and ∼ 5% of the krypton. Analyses for tellurium, technetium, and neptunium, which are other possible contaminants in the uranium and plutonium stream, were not completed.