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57Fe Mossbauer spectroscopy was used to investigate the evolution of Fe-Zn binary metal oxide sorbent in the process of high-temperature fuel gas desulfurization. The results of phase analyses show that Fe-Zn binary metal oxide sorbent is rapidly reduced in hot fuel gas and decomposed to new phases of highly dispersed microcrystalline elemental iron and zinc oxide, both of which become the active desulfurization constituents. A complementary and synergistic effect between active iron acting as a high sulfur capacity constituent and active zinc oxide acting as a deep refining desulfurization constituent exists in this type of sorbent for hot fuel gas desulfurization.