The recovery of 252Cf from palladium-252Cf cermet wires was investigated to determine the feasibility of implementation into the cermet wire production operation at the Radiochemical Engineering Development Center at Oak Ridge National Laboratory. The dissolution of Pd wire in 8 M HNO3 and trace amounts of HCl was studied at both ambient and elevated temperatures. These studies showed that it took days to dissolve the wire at ambient temperature and only 2 hours at 60°C. Adjusting the ratio of the volume of solvent to the mass of the wire segment from 0.176 mL/mg down to 0.019 mL/mg resulted in little change in the kinetics of dissolution. A successful separation of 153Gd, a surrogate for 252Cf, from Pd was demonstrated using ion exchange chromatography.