In this paper, we report a new method to investigate the oxygen release process during heat treatment of (Bi,Pb)(2)Sr2Ca2Cu3Ox (BSCCO) powder, based on oxygen partial pressure measurement (OPPM) using an oxygen analyzer. The influence on oxygen release process of various processing parameters has been studied. Experimental results show that OPPM is a suitable method for investigation of the oxygen release process during heat treatment of BSCCO powder. It is suggested that oxygen release is related to decomposition of the Ca2PbO4 phase. (C) 2004 Kluwer Academic Publishers.