The Bureau of Mines is developing nickel catalysts for converting synthesis gas derived from coal to synthetic natural gas. The present report describes the relationship between the composition of aluminum-nickel alloys in the composition range nial3 to ni2al3 equilibrated at 840 deg c and the properties of catalysts obtained from them. Methanation activity was determined in the temperature range of 300 deg to 360 deg c in a flowing gas stream containing 1 pct CO, 8 pct h2, and the remainder he. One part per million of h2s was added to the gas stream at 400 deg c to evaluate the susceptibility of catalysts to sulfur poisoning. The total surface area was measured by the adsorption of nitrogen at liquid nitrogen temperature, and the active surface area was measured by the adsorption of hydrogen at room temperature. Total surface area and active surface area were found to increase with increasing proportion of aluminum-saturated ni2al3 in the precursor alloy but methanation activity and resistance to poisoning by h2s were nearly constant. However, the methanation activity of the catalyst prepared from stoichmetric ni2al3 was less than half that of the other catalysts.