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The hydrolysis of 0.06 mol dm−3 Fe(NO3)3 solutions was followed at 65°C by means of pH and dynamic light scattering measurements. The hydrolysis products were characterized by transmission electron microscopy and nitrogen adsorption. Depending on the heating procedure different phases were observed, i.e. α-FeOOH (goethite) was formed on heating a 0.06 mol dm−3 solution to 65°C, and α-Fe2O3 (hematite) if an appropriate amount of a concentrated stock solution was added to the preheated water at 65°C. An explanation of this behaviour is offered by taking into account the possible formation of quite different structural units of both solid phases in the course of the hydrolysis process.