The chromatographic separation of magnesium isotopes was investigated by chemical ion exchange with 1, 16-dithia-4,7,10,13-tetraazacyclooctadecane-4,7,10,13-tetramerrifield peptide resin[N4S2'4M ] synthesized recently. The capacity of novel NaS 2 azacrown ion exchanger was 0.34 meq/g dry resin. The heavier isotopes of magnesium concentrated in the resin phase, while the lighter isotopes are enriched in the solution phase. The glass ion exchange column used was 30 cm long with inner diameter of 0.2 cm, and the 1.0M NH4CI solution was used as an eluent. The separation factors of 24Mg-25Mg, 25Mg-26Mg, and 24Mg-26Mg were 1.047, 1007, and 1.008, respectively.