Particles of Fe oxide were prepared by chemical coprecipitation and their sizes were shown by TEM and confirmed by XRD to be in the range of 5 nm. The Mössbauer spectra at 120 K clearly indicated the absence of magnetite and presence of the maghemite (γ-Fe2O3) phase. We studied the transition of the system to superparamagnetic behaviour, which strongly depends on the relevant time window amounting to ∼ 10 −7 s for Mössbauer spectroscopy of 57 Fe and units of seconds for d.c. magnetic measurements. From the temperature dependences of magnetic moments of zero-field-cooled (ZFC)) and field-cooled (FC) samples, the distributions of blocking temperatures were determined. The comparison of the transition temperatures derived from these two types of measurements gave an independent estimate for the pre-exponential factor and the energy barrier and thus magnetocrystalline anisotropy in an order-of-magnitude agreement with the published data for bulk γ-Fe2O3.PACS : 61.46.Df, 75.30.Gw