A rapid, accurate method for the determination of zirconium by activation analysis with radiochemical separation is described. After neutron irradiation of the sample, it is dissolved and allowed to stand over 4 h; then the 97Nb daughter of 97Zr is extracted from the sample solution. A high degree of recovery and separation, esecially from hafnium and other elements usually associated with zirconium, is obtained. These features, coupled with high sensitivity, combine to give the method advantages relative to previous procedures for the determination of zirconium.