Functionalized surfactant as iron(II) bis(ethyl-2-hexyl)sulfosuccinate, Fe(AOT)a, is used to synthesize metallic nanoparticles of alpha-Fe and of a Fe-B alloy through chemical reduction with NaBH4. The particles are observed by transmission electron microscopy and characterized by X-ray diffraction, electron diffraction, Mossbauer spectroscopy, and electron energy loss spectrometry. The room-temperature magnetization curve is also presented.