In order to prepare the new monoclinic Pb2FeV3O11 at low temperature; an acidic solution of vanadium oxide, pH 2, was mixed with a corresponding amount of both lead and iron nitrate at boiling temperature. The yellow precipitate obtained is a mixture of lead pyrovanadate Pb2V2O7 and an amorphous phase. At 500°C, the new monoclinic Pb2FeV3O11 phase appears but mixed with Pb2V2O7. At higher temperature, 570°C, the monoclinic phase disappears and a new phase appears. This phase is similar to triclinic Pb2Fe2V4O15, recently reported, although the EDAX analysis shows the as-prepared sample with higher amount of vanadium and iron. To understand the mechanism involved, lead and iron nitrate solution were reacted separately with vanadium oxide solution. The phases formed were found to be sensitive to initial concentration and to stirring time