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Three differently prepared cobalt/ZSM-5 catalysts were Investigated with respect to physical and chemical properties and to activity and selectivity for conversion of synthesis gas. The catalyst preparations consisted of the following:(1) direct decomposition of C5H5Co(CO)2 on ZSM-5, (2) Impregnation of ZSM-5 with an aqueous solution of cobalt nitrate, and (3) physical admixture of precipitated cobalt oxide with ZSM-5. At about 3 wt % cobalt loading, the first catalyst showed higher dispersion, higher (H2 + CO) conversion, and about 10 times higher yield of gasoline-range hydrocarbons (g/h) than the catalyst prepared by the other two methods. Some H2 and CO chemisorption studies and magnetization measurements were conducted to measure the average particle diameter. Infrared studies of chemisorbed pyridine on these samples indicate that ion exchange of Co2+ for acidic protons occurs in organometallic-impregnated and aqueous solution-impregnated catalysts.