The physicochemical properties of the synthetic fibrillar boehmite, Baymal, were comprehensively studied using vacuum microbalance, differential thermal analysis, x-ray, infrared spectroscopy, and nitrogen adsorption techniques. The boehmite contained water in excess of stoichiometry which exerted a definite influence on the properties of the solid. Part of the excess water was incorporated between the layers of the boehmite lattice. A structural rearrangement of the lattice occurred on heating Baymal in vacuo above 360° C. An intermediate structure in the boehmite calcination was observed and identified as containing isolated AI-OH groups. The texture of the material did not change during the decomposition. © 1969, American Chemical Society. All rights reserved.