Disclosed is a distillation process for reducing the concentration of impurities dinitrogen difluoride and dinitrogen tetrafluoride in nitrogen trifluoride. The process comprises: (a) distilling a mixture comprising nitrogen trifluoride and dinitrogen difluoride and/or dinitrogen tetrafluoride in a distillation column in the presence of a compound having a higher normal boiling point than nitrogen trifluoride; (b) removing a mixture comprising dinitrogen difluoride and/or dinitrogen tetrafluoride as a sidedraw from the distillation column; (c) removing a mixture comprising the compound having a higher normal boiling point than nitrogen trifluoride from the bottom of the distillation column; and (d) removing a nitrogen trifluoride product having reduced concentration of dinitrogen difluoride and/or dinitrogen tetrafluoride from the top of the distillation column.