A multistage process combining photocatalytic degradation of organic complexes and complexants followed by separation of the radionuclides by ion exchange was developed and tested for the treatment of aqueous waste from chemical or electrochemical decontamination of NPP primary circuit internals. In these solutions, both the oxalic and citric acids could be quantitatively degraded within 10-12 hours of irradiation by 254 nm UV radiation in the presence of TiO2 photocatalyst. For the group radionuclides separation, a standard cation exchanger was found to be preferable to any of the set of the tested inorganic-organic composite absorbers.