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Using the Mossbauer spectroscopy and other physical methods it was demonstrated the presence of different iron compounds like β-FeOOH, α-Fe2O3, and jarosite mineral type compounds: (R4N,H3O)[Fe3(OH)6(SO4)2] or coordination modes: {RCOO-Fe(L4)-OOCR}1+, {R-CO2=Fe(X2)=O2C-R}n, {R-COO-Fe(X4)-OOC-R}n, and {(-NCH2CH2N-)= Fe(X2) =(-NCH2CH2N-)}, where X= H2O, OH-, SO42-., n= from 3- to 1+ in the ion-exchange resins (KU-2, AN-31, AV-17, Varian – AD, EDE-10P) after the contact with sulphate of iron(III) solutions at different conditions: type of solvent, temperature, air atmosphere. In special conditions the ultrafine superparamagnetic particles of Fe2O3 have been obtained