Different alumina-supported metal sulfides catalysts were studied for the H 2 S oxidative decomposition reaction to simultaneously obtain sulfur and hydrogen in the presence of CH 4 . Mono and bimetallic catalysts were prepared, characterized, and tested at 1273 K by varying the contact time. X-ray diffraction and Raman evidenced a good dispersion of the Mo, Fe, and Co sulfide species on the Al 2 O 3 support. From the experimental results, it was argued that Mo sulfide species are the active phases able to inhibit the formation of SO 2 , while the Fe sulfide species promote the selective abatement of COS and CS 2 obtained because of the presence of CH 4 in the gaseous feed stream. The bimetallic sample containing both Mo and Fe sulfide species (5Fe-10Mo/Al 2 O 3 ) exhibited very interesting catalytic performances since it allowed us to achieve a H 2 yield, CH 4 , and H 2 S conversion very close to the equilibrium values and the complete removal of sulfur compounds at low contact times.