Abstract: A simple, effective and rapid chemical procedure for separating ⁷²Ga from a mixed sample of soil has been developed, by using NaOH precipitation and isopropyl ether extraction. The chemical recovery is greater than 90%. The decontamination factors of fission products are greater than 10³, and the decontamination factor of soil matrix is 4.1×10³. The total time of the whole procedure is less than 50min, then the method can meet the requirement of the detection of ⁷²Ga.