Disclosed herein are a process for the refinement of nitrogen trifluoride gas and an adsorbent therefor. A nitrogen trifluoride (NF3) gas including carbon tetrafluoride (CF4) as an impurity is permeated into a bed of zeolite 3 A, 4A or 5 A which undergoes ion exchange and impregnation with alkali earth metal and is thermally treated at 150 to 600° C. for 0.5 to 100 hours so as to be able to selectively adsorb nitrogen trifluoride onto the bed, followed by the desorption of the nitrogen trifluoride therefrom.