The recovery of zinc and its separation from iron, hydrochloric acid, and minor elements in the galvanizing pickling baths were studied by anion exchange. The breakthrough curves demonstrated that the resins, Lewatit MonoPlus MP 500 and AMBERLYST A21, exhibit a greater capacity for zinc than for cadmium, copper, and lead. The results indicated the feasibility of operating the ion exchange process to treat a real effluent. During the loading, lead started eluting until its complete removal from the resin. Like this, a two-step removal solution is proposed, using two columns with Lewatit MonoPlus MP 500, for separating zinc and lead.