An analytical procedure was developed for the alpha-spectrometric determination of uranium (238U, 235U, 234U) and transuranium isotopes (239+240Pu, 244Cm) in liquid radioactive wastes (sludges, evaporation residues) of low and medium activity from the VVER-440 reactor of the nuclear power plant in Paks, and in waste waters to be released into the environment. Radioactive sludge samples were separated to a liquid phase and a wet suspension (solid) phase by centrifuging, and the two phases were treated and analyzed separately, in different ways. A sample preparation procedure based on chemical separation was worked out for the isolation of the alpha-emitting components of radioactive evaporation residues which were saturated with boric acid. To the separate determination of the low activity alpha-emitting isotopes appearing in waste waters to be released into the environment, a microvawe concentration technique was applied. The accuracy of the results obtained using the above chemical separation and alpha-spectrometry was tested in the framework of the international U. S. DOE EML Quality Assessment Program.