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Hydrogen was found to accumulate on the surface of Ni - containing detonation linnodiamond. Nickel was deposited to the nanodiamond by wet impregnation with nickel formate mid thermal decomposition under dynamic vacuum. The hydrogen formed by dissoatiative mlsorption on nickel nanoparticles was likely to migrate ("spill over") to the carbon support. Amount of the hydrogen adsorbed was determined using catalytic method. Acetylene was liydrogenated by the pre-adsorbed hydrogen on the Ni-nanodiamond catalyst - the hydrogen storage capacity was determined as the total amount of the acetylene converted. The hydrogen adsorption and catalytic reactions were carried out in the microcatalytic npparatus. Nanodiamond specimen containing nanometer sized nickel particles was placed into a quartz reactor. Hydrogen pre-adsorption was performed in the hydrogen flow for 4 h. at ЗООоС. During the reaction, the hydrogen was changed to nitrogen and impulses of 1 ml of acetylene were introduced using syringe. Reaction products were analysed using a chromatograph equipped with a llame ionisation detector. The research performed demonstrated that the hydrogen adsorbed was folly consumed by the acetylene hydrogenation after 20 impulses, which allowed us to make a lower bound estimation of the catalyst hydrogen storage capacity as 1.3% mass. Catalysts obtained using the same methods from synthetic diamond "DALAN" and carbon specimen obtained by the sugar burning in air demonstrated no activity in the acetylene hydrogenation by the pre-adsorbed hydrogen. Meanwhile their catalytic activity in this reaction in the flow of hydrogen was high.