A new binary cobalt iron pyrophosphate, CoFeP2O7 was synthesized through solid phase reaction using cobalt carbonate, iron metal and phosphoric acid in the presence of water-methanol system with further calcinations at the temperature of 500 degrees C. The particle size obtained from X-ray line broadening is 36 +/- 7 nm for the CoFeP2O7. MR spectrum of CoFeP2O7 is assigned based on the P2O74- ion in the structure. The XRD, UV-Vis near IR and FTIR results of the synthesized CoFeP2O7 appear to be very similar to that Of M2P2O7 (M = Fe and Co), which indicates the monoclinic phase with space group C2/m. (C) 2009 Elsevier B.V. All rights reserved.