The synthesis of iron oxyhydroxides and hydroxides is reported in this work, by the use of a novel, simple and lowcost method. The preparation involves the hydrolysis of aqueous solutions of ferric salts followed by membrane purification and freeze drying of the products. Three different iron precursors have been tested and combined to three different volatile precipitating agents. The obtained products were akaganeite, goethite and iron(III) hydroxide. Irrespective of the starting materials used, all three products, although different in chemical nature, presented some very interesting and unique features; they consisted of nanoparticles with mean sizes ranging from 1 to 10 nm and they had very high surface areas and pore sizes in the meso- and micropore regions. The produced materials were examined by powder X-ray diffraction for crystalline phase identification, TEM and XRD for particle size estimation and nitrogen sorption for surface area, pore volume and pore size distribution measurement