La 0.67 Sr 0.33 Fe x Mn 1-x O 3 , with x = 0.0, 0.1, 0.2 and 1 have been elaborated by mechanical system. X-ray diffraction, Scanning electron microscopy, Magnetic measurements and Mössbauer spectroscopy for the systems have been investigated. Rietveld analysis of the X-ray powder diffraction show that the samples crystallise in the orthorhombic perovskite system with Pnma space group. The average particle size of about 60 nanometre was obtained from scanning electron microscopy and X-ray diffraction. The investigated samples exhibit a ferromagnetic to paramagnetic transition with increasing temperature. The presence of manganese in the structure leads to an increase of the Curie temperature as well as to spontaneous magnetization. The magnetization versus applied magnetic field shows a small coercive field and an unsaturated magnetization which indicates that the nanoparticles of all samples are superparamagnetic at around room temperature. Room temperature A.-F. Lehlooh is on Sabbatical leave 154 W. Chérif et al.Mössbauer spectra show that the samples with x = 0.1 and x = 1.0 contain minority α-Fe 2 O 3 and other spinel ferrite species. Also, they indicate that Fe 3+ ions are present in slightly distorted octahedral sites in the samples with x = 0.1 and 0.2, while mixed Fe valency was observed for the sample with x = 1.0.