The nuclear industry has considerably contributed to the development of methods and procedures to cope with and solve the problems of safety and management of hazards. One of the problems of spent nuclear fuel reprocessing management is the treatment of organic radioactive wastes. This paper is intended to present a new process for radioactive waste treatment, based on two combined steps, i.e. preliminary distillation and wet oxidation. The results of distillation tests, carried out in a laboratory scale apparatus, on both simulated and radioactive liquid solutions, are reported. The tests carried out with simulated solution prove to be of significant value for a more thorough and fundamental understanding of distillation equipment. High decontamination factors were obtained by distillation of radioactive waste, showing no need for further particular treatment of the distillate, A noteworthy result from the point of view of safety and management of hazards connected to radioactive wastes in nuclear plants is the remarkable reduction in the volume of contaminated liquid wastes, which should encourage further investigations with a view to utilizing industrial distillation plant.