Heavy ion activation of natural terbium foil with 75 MeV 12C6+ results in the formation of carrier-free lutetium isotopes, 165–167Lu, and their corresponding decay products, 165–167Yb and 165–167Tm, in the matrix. Carrier-free lutetium and ytterbium isotopes have been separated quantitatively from terbium bulk target matrix using HDEHP liquid cation exchanger. Radiochemically pure thulium radionuclides have been obtained after the decay of ytterbium radionuclides.