A commercial metal oxide sorbent for the desulphurization of coal-derived gas requires high desulphurization reactivity, mechanical strength, ability to regenerate, and stability to endure many sulfidationregeneration cycles. In this paper, the sulfur capacity and multiple cycles of a nickel-modified ZnFe 2 O 4 sorbent prepared by the sol-gel auto-combustion method were measured in a fixed-bed reactor at middle temperature of 300°C (sulfidation temperature) and 500°C (regeneration temperature). Also, the BET surface area, pore volume, average pore diameter and X-ray diffraction (XRD) patterns of the sorbent through multicycles were studied. Multicycle runs indicate that the sulfidation reactivity decreases slightly during the second cycle and keeps steady in the following cycles. The results indicate that the nickel-modified ZnFe 2 O 4 keeps high reactivity and structural stability in the multicycle testing of sulfidation/ regeneration.