A novel method to recover zinc and iron from zinc leaching residue (ZLR) by the combination of reduction roasting, acid leaching and magnetic separation was proposed. Zinc ferrite in the ZLR was selectively transformed to ZnO and Fe3O4 under CO, CO2 and Ar atmosphere. Subsequently, acid leaching was carried out to dissolve zinc from reduced ZLR while iron was left in the residue and recovered by magnetic separation. The mineralogical changes of ZLR during the processes were characterized by XRF, TG, XRD, SEM-EDS and VSM. The effects of roasting and leaching conditions were investigated with the optimum conditions obtained as follows: roasted at 750 degrees C for 90 min with 8% CO and CO/CO + CO2 ratio at 30%; leached at 35 degrees C for 60 min with 90 g/l sulfuric acid and liquid to solid ratio at 10:1. The iron was recovered by magnetic separation with magnetic intensity at 1160 G for 20 min. Under the optimum operation, 61.38% of zinc was recovered and 80.9% of iron recovery was achieved. This novel method not only realized the simultaneous recovery of zinc and iron but also solved the environmental problem caused by the storage of massive ZLR. (C) 2013 Elsevier Ltd. All rights reserved.