Abstract: The invention relates to improved methods for regenerating the exhausted anion and cation exchange resins in a mixed bed demineralizer system. The exhausted bed of resin is directed into a separation vessel which contains a buffer volume of anion and cation resins remaining therein from the previous regeneration cycle. The resin in the separation vessel is classified into an upper anion resin layer, a lower cation resin layer and an intermediate layer of intermingled anion and cation resin. The cation resin is transferred from the bottom of the separation vessel to a cation regeneration vessel through a cation transfer conduit having isolation valves associated with the respective ends thereof. The resin transfer is terminated upon the detection of anion resin in the transfer conduit, at which time the isolation valves are closed so as to isolate the bulk of the intermingled anion and cation resin layer in the cation transfer conduit.