Fe-3(PO4)(2)(.)8H(2)O has been precipitated under supersaturation conditions from deaerated Fe(NH4)(2)(SO4)(2)(.)6H(2)O and K-2-HPO4 aqueous, ethanol-water and iso-propanol-water solutions at pH = 6.5 and ambient temperature. The precipitates have been characterised by TG/DTG/DTA and DSC techniques, chemical analysis, BET, and X-ray powder diffraction. The presence of ethanol and iso-propanol in the spontaneous precipitation process of ferrous phosphate leads to highly crystalline powder. Thermal treatment at 500degreesC yields a poorly crystalline dehydrated iron phosphate.