Abstract: In order to effectively extract no-carrier-added radioactive hafnium, such as ¹⁷⁶Hf in archaeological dating or ¹⁸²Hf in nuclear astrophysics, three dissolution methods, the alkali melting, the acid dissolution, and a combination of both were studied by using ¹⁸¹Hf as a tracer whose γ-rays were measured with a HPGe gamma spectrometer. The radiochemical yield of ¹⁸¹Hf during its separation and purification from the leaching solution by anionic exchange chromatography, cationic exchange chromatography, and solvent extraction with N-benzoyl-N-phenylhydroxylamine were separately studied. A complete process for dissolution, concentration, separation and purification of hafnium from rack sample is suggested. The radiochemical yields for each step were measured. A recovery of 94% in the rock sample dissolution stage, and 52% in the separation and purification stage are achieved.