The effect of compositions, sintering temperatures and furnace atmospheres on the superconducting transition temperatures of several members of the series Pb2Sr2R1−xCaxCu3Oz(0.0⩽x⩽0.7, R=Y, Gd) has been studied. The effect of partial replacement of Pb, Ca and Y by In has also been studied. The shapes of the resistivity-temperature curves and the zero resistance temperatures are found to be extremely sensitive to the synthesis parameters employed. Superconductivity is not observed in samples treated in oxidizing atmosphere or heated at very high temperatures. Samples sintered in flowing nitrogen showed incomplete transition in resistivity starting at about 75 K and extending down to 15 K. A new and comparatively simple synthesis procedure involving treatment of the samples in vacuum has been employed to obtain nearly single-phase materials showing metallic behaviour. Using this procedure, samples of the above composition, but containing no Ca(i.e. Pb2Sr2RCu3Oz, R=Y and Dy), are also found to be superconducting with zero resistance up to 48 K.