This study investigates the effect of operation parameters on the separation of nitric acid-water mixture using air gap membrane distillation (AGMD). Porous hydrophobic PTFE membrane was used. The performance was evaluated based on the permeate flux and the nitric acid selectivity. Operating parameters such as feed solution temperature, feed concentration, flow rate, and air gap width were varied. Nitric acid selectivity was found to increase with the increase in feed solution temperature, feed concentration, flow rate, and air gap width. Permeate flux increased, when the feed temperature and the flow rate were increased. The effect of recirculation of the feed solution was also studied. With the recirculation mode, at different initial solution volumes, it was observed that the nitric acid concentration in the feed and the permeate, increased. The rate of flux decline was greater, when the initial feed solution volume was lower.