The superconducting properties and the phase and chemical composition of BixPb0.3Sb0.1SryCa2Cu3Oz (x=1.5, 1.6, and 1.7;y=1.9, 2.0, and 2.1) materials synthesized by one-step and multistep thermal treatments have been investigated. The multistep annealing between 825-875°C promotes the 2223 phase. The change of Bi concentration has little effect on the 2223 phase formation, regardless of the kind of thermal treatment used, but increasing the Sr concentration (y> 2) strongly inhibits this phase. It has also been established that the loss of Pb after synthesis depends on the initial Bi concentration. The loss of Pb decreases when the initial Bi content is lower. © 1993 Plenum Publishing Corporation.