A single phase Pb2Sr0.8La1.2Cu2O6.1+δ superconductor was prepared by a polymeric citrate precursor method. Metal nitrates of the nominal compositions were used as the starting materials. After pyrolysis of the gel-like polymeric citrates, the precursor obtained was calcined at 800 °C for 4 h, sintered at 790 °C for 6 h in the flowing nitrogen atmosphere followed by furnace cooling. The processing period was greatly reduced by this method compared with the conventional solid state reaction method. The chemical titration found that all the Pb ions were in the +2 state and the average copper valence was 1.601 indicating the δ value of 0.101 equivalent to hole concentration of 0.202 in the Cu-O plane of this superconductor.