The organic fluoronitrogen compounds bis(difluoroamino)difluoromethane (I) and tris(difluoroamino)fluoromethane (II) are energetic materials which are gases at room temperature and relatively difficult to prepare in high purity because of similarity of properties and thermodynamic instability. The compounds were quantitatively separable by selective and reversible adsorption of the smaller molecule (I) on crystalline zeolites of controlled pore size””molecular sieves. The separation process and the character of the zeolite inclusion compounds with I and II are described. The unsaturated pentafluoroguanidine (III) decomposes in the presence of the basic zeolites. © 1969, American Chemical Society. All rights reserved.