The fluorination step in a fluidized-bed fluoride volatility process has been studied in a 2-in.-diam reactor using BrF5 and fluorine as fluorinating agents and sintered alumina as the fluidized bed. Fuel pellets containing UO2, PUO2, and nonradioactive fission product oxides were pulverized by oxidation before uranium was selectively fluorinated with dilute BrF5; plutonium was then fluorinated with concentrated recycled fluorine. Fission product elements added to the system simulated burnups of 10 000 and 30 000 MWd/ton. Several aspects of the fluoride volatility process are discussed: effect of variations in process parameters on residual plutonium in the bed, distribution of selected fission products and 106Ru tracer, demonstration of reduced plutonium losses by reuse of a single alumina bed to process three batches of pellets at each of the simulated burnups of 10 000 and 30 000 MWd/ton, plutonium inventory in the reactor, and sampling the fuel charge for material balance and accountability. A processing step for a hybrid process incorporating leaching of the fluidized bed with nitric acid after uranium fluorination with BrF5 was also demonstrated.