A procedure for preparing magnesium carbide, Mg 2 C 3 ; in 300 gm. lots is described. Propyne-d 4 was prepared in good yields by the action of deuterium oxide on this carbide. The acetylenic deuterium in propyne-d 4 was replaced by hydrogen via the mercury derivative giving propyne-3-d 3 The vapor pressures of propyne-3-d 3 ,and propyne-d 4 were determined between −25 °C. and −60 °C.