The extraction of zirconium and hafnium from aqueous HCl solutions by means of Aliquat 336 in organic diluents was systematically studied. The following three aspects were discussed: the extraction dependence on HCl, the Aliquat 336 concentrations, and the nature of diluents. Both of the metals were stripped with deionized water and the influence of phase ratio on the efficiency of the stripping has been investigated. The stoichiometry of the extracted Zr and Hf species from single metal ion were studied and a possible extraction mechanism for the Zr-Hf mixture is discussed in the light of the results obtained.