This research was a preparation of Ni/Alumina by impregnation method. The impregnant solution was nickel in concentrated ammonia solution having pH 11.6. Alumina, diameter of 0.3 to 0.5 cm. and BET surface area 325.2 m2/g, was used 10 g as supporter. The variables for a impregnation process are impregnant concentration (1.0, 1.25, 1.5, 2.0, 3.0 and 5.0% nickel), volume of impregnant solution (50, 100, 150 and 200 cm3), impregnation time (0.5, 1.0, 2.0, 4.0 and 8.0 hr.) and impregnation temperature (30, 40, 50, 60 and 70 ํC). The results showed the percentage of dispersion of nickel on supporter by using hydregen chemisorption on the surface of catalyst with Pulse Chemisorb 2700. The results of preparation of Ni/Alumina Catalyst was found that the distribution of Nickel on alumina look like eggshell. The catalyst optimum condition of variables of the preparation were, impregnant concentration, 2.00% nickel, volume of impregnant solution, 100 cm3, impregnation time, 2 hr. and at temperature 30 ํC, giving percentage dispersion, 80.05.