The preparation conditions, phase composition, and superconducting properties of Bi-Pb-Sr-Ca-Cu oxide materials from different nominal compositions have been investigated. Nearly single-phase samples from Bi2Pb0.4Sr2Ca3Cu4Oy, as well as from the proposed compositions Bi1.8Pb0.4Sr2Ca3Cu4Oy and Bi1.8Pb0.4Sr2Ca2.5Cu3.5Oy were obtained by a solid-state reaction in air. Samples with the third nominal composition showed the best superconducting properties (Ton=111 K and zero resistance at T0=103 K). A possible mechanism for the 2223 phase formation in the three investigated compositions has been discussed. © 1993 Plenum Publishing Corporation.