Ni species on the spent NiMo catalyst from ultra-deep hydrodesulfurization of gas oil in a commercial plant were studied by Ni K-edge EXAFS and TEM measurement without contact of the catalysts with air. The Ni-Mo coordination shell related to the Ni-Mo-S phase was observed in the spent catalyst by quasi in situ Ni K-edge EXAFS measurement with a newly constructed high-pressure chamber. The coordination number of this shell was almost identical to that obtained by in situ Ni K-edge EXAFS measurement of the fresh catalyst sulfided at 1.
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