The present research evaluates the efficiency of mixed resins between anion exchange resin and active carbon. We expected synergic effect from advantages of both adsorbents. Especially, this research focused on the removal of high cencentrated perchlorate ion from demilitarization solution. The total amount of the adsorbed perchlorate ion is increased considerably with mixed resins between mono functional anion exchange resin and granular active carbon from a single adsorbent. Results demonstated that this process not only improve the efficiency of adsorbing perchlorate, but save the time, space and cost for treating perchlotrate waste solution, because of reducing organic contaminant removing process. The interference effects from coexisting anions are not significant and can successfully applied to real demilitarization sample.