The behaviour of stable and inert metal chelates of 4-(2-pyridylazo)resorcinol and 4-(2-thiazolylazo)resorcinol in RP HPLC and in its ion-pair modification (IP RP HPLC) on Separon SGX RPS silica gel was studied. Good results were obtained by the ion-pair variant in water methanol solutions at pH 7 in the presence of cetyltrimethylammonium bromide. The technique proved to be convenient for the preconcentration, separation and quantitation of low concentrations of Fe, Co, and Ni in waters.