The invention relates to the separation of metals in Fe-bearing zinc leaching residues, in particular neutral and weak acid leach residues. The process comprises the steps of: preparing agglomerates containing, besides the Zn leaching residue, at least 5 wt % of carbon and 2 to 10 wt. % of S; fuming said agglomerates in a static bed at a temperature above 1250.degree. C., thereby producing a reduced Fe-bearing phase and Zn-bearing fumes; and extracting said Zn-bearing fumes. The high S content of the feed allows for a relatively high operating temperature without production of molten phases. This guarantees fast reduction and fuming kinetics, and permits the use of a compact technology such as a static bed furnace.