The dissolution of carbide fuels was tried with the aid of various oxidants like H2O2, NaBiO3, (NH4)2Ce(NO3)6, (NH4)2S2O8, and AgO in nitric acid medium. During the dissolution, the carbon dioxide liberated has been measured. Among the oxidants studied, H2O2 and NaBiO3 appeared to be more effective for dissolution of carbides. 200–300 mg of sintered uranium carbide sample dissolved within 15 minutes in the presence of oxidants H2O2 or NaBiO3. Mixed carbide sample (70%) was dissolved within 30 min, whereas plutonium carbide required more than one hour. From the resulting solutions uranium and plutonium could be determined by conventional redox methods. More than 97% of plutonium could be recovered and purified from the resulting carbide solutions by conventionally used anion exchange method.