Aluminum oxide exists in several forms which on addition of water give a complex range of oxide-hydroxide; boehmite, bayerite and gibbsite. High frequency dielectric measurements {300 kHz-3 GHz} are reported on the hydrated and dehydration of certain of these oxide-hydroxides. The amplitude of the observed dielectric relaxation correlates approximately with the water content, however anomalies can be observed during dehydration due to the retention of water in an immobilized form within the oxide matrix which highlights complexities in their structure and properties. These data indicate the potential of the dielectric method for quantification of the deg ree of hydration of an oxide in adhesive bonded structures. Two silane coupled alumina samples were studied to simulate the interface generated in the pre-treatment of real adhesive bonded structures.