This paper addresses the synthesis structural and electrochemical properties of LiFe0.5Mn0.5PO4 electrode materials for Li-ion batteries. The charge–discharge reaction of Li/LiPF6-EC–DEC/LiFe0.5Mn0.5PO4 cell carried out at the 1-C rate shows a capacity retention of 128 mAh/g. The local structure of the delithiated LixFe0.5Mn0.5PO4 phases have been studied by Fourier transform infrared spectroscopy and magnetometry. Spectral features indicate that the structure of the delithiated phase remains in the orthorhombic system. The compositional dependence of the magnetic moment is found to be in quantitative agreement with the theoretical value predicted for oxidation of M2+ ions in the high spin state