Summary: Infra-red absorption spectroscopy has been used to study the retention of hydroxyl groups by kaolinite and halloysite after heat treatment in the range 600° C. to 850° C. Structurally disordered specimens initially lose water more rapidly than do ordered specimens, but retain hydroxyl groups at higher temperatures. Work on the phases obtained above 1100° C. is incomplete, but results for the lower temperatures indicate that the ordered structures tend to retain their atomic arrangement and form metakaolin, whereas disordered structures readily rearrange to yield γ-alumina, to the formation of which water is probably essential.