Investigations have been carried out on the oxidative hydrolysis of iron(II) chloride using Na 2 CO 3 or NaOH. The products were subjected to hydrothermal agitation before being filtered and dried at 110°C. The samples were characterised by chemical analysis, surface area by nitrogen adsorption, thermal analysis and XRD. The studies indicate that samples prepared by different procedures and at different temperatures result in the formation of mixtures of goethite (α-FeOOH), maghemite (γ-Fe 2 O 3 ), e-Fe 2 O 3 and Fe 3 O 4 in varying compositions. All the samples, when heated to 400°C or above, are converted to α-Fe 2 O 3 .