Abstract: A process is provided for separating ammonia from an ammonia synthesis purge gas stream containing ammonia, hydrogen, and contaminant gases. The process involves introducing the gas stream into a permeator equipped with a polysulphone amide gas separation membrane, to selectively permeate ammonia therethrough. The gas stream is at a temperature less than about 0.degree. C. upon introduction to the permeation step. The polysulphone amide membrane surprisingly exhibits high permeability to ammonia permeation (relative to hydrogen) at low temperature. The ammonia is thus first separated by low temperature permeation and the hydrogen may then be recovered from the residue gas using a conventional membrane that exhibits high permeability to hydrogen. The two-step permeation process recovers ammonia and hydrogen in two separate streams and permits the use of a second stage membrane that would be deleteriously affected by ammonia in the hydrogen recovery step.