We have studied on the hydrogen storage materials based on Mg-Ni alloy and fabricated the sample constructed with the Pd thin layer (TL) on Mg6Ni alloy substrate. The adsorption behavior of the dimethyl disulfide (DMS) molecules on the sample has been measured to reveal the sulfur poisoning of the Pd TL/Mg6Ni by means of XPS and Sulfur K-edge NEXAFS techniques. The chemisorbed DMS, methanethiolate (MT) and atomic S have been observed on the surface. Especially, it is clear that some atomic S has been oxidized by air and detected the adsorbate of the SO32- and SO42- species. During exposure to the atmosphere, most of the adsorbed DMS and MT adsorbates desorb from the Pd TL surface. We thus conclude the Pd TL might be able to prevent the hydrogen storage materials from the sulfur poisoning. (C) 2012 Elsevier B. V. All rights reserved.