Authors:M. Charyulu, C. Karekar, V. Rao, and P. Natarajan
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.
Authors:C. Karekar, Keshav Chander, G. Nair, and P. Natarajan
A potentiometric titration method was developed for the determination of plutonium and uranium in the same aliquot in nitric acid medium. Plutonium was first determined by oxidation to Pu/VI/ by fuming with conc. HClO4. Pu/VI/ formed was reduced to Pu/IV/ with known excess of Fe/II/ and the excess Fe/II/ was titrated with standard K2Cr2O7 to a potentiometric end point. Uranium in the same solution was determined by reduction to U/IV/ with Fe/II/ in conc. H3PO4 medium and titrating U/IV/ formed with standard K2Cr2O7 using the potentiometric end point detection technique. For the quantity of plutonium and uranium each in the range of 3–5 mg per aliquot a precision of ±0.2% and ±0.4%, respectively, was obtained.