An electrocatalyzed process has been described for the dissolution of plutonium from the contaminated neoprene gauntlets used during the fabrication of plutonium-bearing fuels. Agents Ag(II) and Ce(IV) were used as catalysts. The results indicated that it was possible to leach out plutonium satisfactorily from such contaminated neoprene gauntlets. The problems involved in processing with Ag(II) and the limitations of the process are also discussed. Further, plutonium was separated from the leached solution by solvent extraction using di-2-ethylhexyl phosphoric acid as the extractant.