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The effect of calcium oxide additive in iron oxide sorbent for hot gas desulfurization was investigated by XRD and TPR techniques. XRD characterization showed that CaO was highly dispersed after the calcination of sorbents. Calcium sulfate formed in the desulfurization was decomposed and regenerated to CaO by reacting with CO before the next sulfidation process. Calcium participated in every sulfidation/regeneration cycle and contributed to the enhancement of sulfur capacity. The TPR results showed that the reduction temperature of the sorbent increased with the increase of the content of calcium. Calcium played a role of retarding reduction. Therefore, the addition of calcium oxide additive will benefit the utilization of iron oxide sorbent in strongly reducing atmospheres.