Small angle X-ray scattering techniques have been used to investigate the shape and size distribution of Zr(IV) species in aqueous solution. This study has shown that when zirconyl chloride solutions, containing the zirconyl tetramer, are subjected to various treatments polymerisation occurs. While ageing and addition of base produces an increase in particle size the shape remains globular. Refluxing the solutions produces “rod” like particles of varying length but constant cross sectional radius.