A process scheme is suggested for the treatment of a metal-containing spent pickling liquor, with the purposes of possible acid recovery and metal separation. Use of anion exchange, followed by packed-bed cementation, was studied for the treatment of a model wastewater containing HNO₃, HF, Fe²⁺, and Ni²⁺. Acids and metal ions were separated through a Dowex 1-X8 anion exchanger of the Cl-form, and the sorbed acids were recovered by regenerating the exchanger with HCl. The obtained Fe-Ni mixture (Fe²⁺ : 3 g/L; Ni²⁺: 1.3 g/L; I L) went through a continuous cementation process using an iron-packed bed (40 g iron in a 14-mm-diameter column), where Ni²⁺ was reductively deposited onto iron and the Fe²⁺ concentration increased in an aqueous stream. In a recycled closed-loop cementation system, 99.8% of the nickel was removed from the mixture solution (from 1.3 g/L to 2 mg/L) and the aqueous Fe²⁺ concentration was increased more than 10-fold (from 3 g/L to 34 g/L) during a 13 BV passage.