Tetraazamacrocyclic ion-exchangers, 1,4,8,11-tetraazacyclotetradecane bonded Merrifield peptide resin(TDM), 1,4,8,12-tetraazacyclopentadecane bonded Merrifield peptide resin(TPM) were prepared, and the ion-exchange capacity of these TDM and TPM were characterized. The distribution coefficients in various conc. of NH4Cl for magnesium with ion exchangers were determined by using the batch method. We found the isotope separation factors on new prepared tetraazamacrocyclic ion-exchangers bonded Merrifield peptide resin(TDM, TPM). The isotope separation of magnesium was determined by using of breakthrough method of column chromatography.