Summary A moisture desorption method has been developed for estimating the water of crystallization of alpha -lactose and indirectly the crystalline alpha hydrate itself in certain types of dry whey solids. It is based upon the difference in the rates of dehydration of crystalline alpha -lactose hydrate and other moisture adsorbing constituents and also upon the uni-molecular dehydration of the hydrate itself. Good recovery was obtained using mixtures of known composition of crystalline alpha -lactose hydrate and casein. Results obtained by this method were in close agreement with those by an indirect method in which the difference between total moisture as determined by the Karl Fischer method and “free” moisture as determined by an oven procedure was considered to be water of crystallization of alpha -lactose. Aside from an effect on the rate of dehydration, particle size, within the range of 54 to 210 μ , was found to have no influence on the results obtained by the moisture desorption method.