Very small maghemite nanoparticles (similar to 3 nm) are obtained through a one-step synthesis at room temperature. The fast neutralization reaction of a ferric solution in a basic medium produces an intermediate phase, presumably two-line ferrihydrite, which in oxidizing conditions is transformed to maghemite nanoparticles. The synthesis of maghemite, as final product of the reaction, was characterized by High-Resolution Transmission Electron Microscopy (HR-TEM), X-ray Absorption Fine Structure (XAFS), Mossbauer spectroscopy, and magnetometry. The XAFS technique allowed the analysis of the crystallographic variations into maghemite nanoparticles as a result of modification in its surface/volume ratio. Mossbauer spectroscopy at low temperature (4.2 K) confirms the presence of Fe(III) in tetrahedral and octahedral interstices, in the stoichiometry corresponding to maghemite. The specific magnetization, M vs H (3 K and 300 K, up to 7 T) and temperature dependence of the magnetization (50 Oe by ZFC mode, 2 K <= T <= 300 K) indicate that maghemite nanoparticles of 3 nm are in superparamagnetic state with a blocking temperature close to 36 K (C) 2013 Elsevier Ltd. All rights reserved.