N,N-dimethylhydroxylamine (DMHA) is a novel salt-free reductant used for the separation of U from Pu and Np in the reprocessing of spent fuel. We investigated the effect of HNO3 on the radiolysis of DMHA and its radiolytic liquid product. Results show that 0.1 and 0.5 mol•L -1 DMHA containing 0.3-1.0 mol• L -1 HNO3 have good radiation stability at a reasonable dose level during the U/Pu separation cycle and the Pu purification cycle. For 5-25 kGy the main radiolytic liquid products are N-methyl hydroxylamine, HCHO, HCOOH, and HNO2. The concentration of these organic compounds is much higher than that of HNO2 and increases with both HNO3 concentration and absorbed dose. At the same HNO3 concentration and dose, the concentration of N-methyl hydroxylamine in irradiated 0.