The diazonium salts of aniline and 4,4Ј-diaminodiphenylmethane coupled with phenol and resorcinol were condensed with formaldehyde in alkaline media to yield polymeric resins. These polymers were found to readily react with metal ions like Cu 2ϩ and UO 2 2ϩ , forming polychelates. The azodyes, resins, and polychelates were characterized by several instrumental techniques such as elemental analysis, FTIR, 1 H-NMR, GPC, XRD, TG-DTG, and DSC studies. The chelating capacity of the resins toward Cu 2ϩ and UO 2 2ϩ ions was studied by spectrophotometry. The extent of metal loading of the resins was studied by varying the time of contact, metal-ion concentration, and pH of the reaction medium. The alkali and alkaline earth metal ions had little effect on the metal-ion uptake behavior of the resins. The resin derived from the azodye of 4,4Ј-diaminodiphenylmethane was found to be more efficient in removing the metal ions from solution than were the resins from aniline. The optimum conditions for effective separation of Cu 2ϩ from UO 2 2ϩ were determined.