HfO 2 is expected to be a gate dielectric used in ULSI alternatives to SiO 2. Although the materials used in ULSI are required to be significantly pure, commercial Hf contains > 2 mass% Zr. It is important to establish a process for removing Zr from Hf. In the present study, anion-exchange separation using a multi-column method was employed. The separation tests were carried out at variety of temperatures and flow rates. The decrease in the flow rate of the mobile phase made the elution curves of both Hf(IV) and Zr(IV) broaden contrary to the case of Co(II), Cu(II), or Fe(III). This is caused by the difference in adsorption rate on the anion-exchange resin. In addition, more than one column was connected in series in order to enhance the separation. As a result, the content of Zr(IV) was successfully reduced to 1/100 of that relative to the raw material.