The Fe/AIPO4-5 catalysts are prepared by impregnation with aqueous and organic solution (acetic acid, alcohol and acetone) of iron(III) nitrite respectively. The characterization of catalyst by means of XPS, Mossbauer spectroscopy, TPR and CO hydrogenation is reported. The catalyst prepared with the aqueous solution has no activity for CO hydrogenation because the Fe(III) in the catalyst cannot be reduced to alpha-Fe. However, the catalysts prepared with organic solution possess obvious hydrogenation activity, in which alpha-Fe is present in the initial reduced catalyst besides Fe3+ and Fe2+. The results may be explained by the interaction degrees between the metal and the support induced by the different impregnation solvents.