This paper presents the results of an examination of four samples representative of the low-lead matte, high-lead matte, lead speiss and antimony speiss, respectively, produced during smelting operations at Port Pirie Smelters. The investigation was undertaken at the request of the Broken Hill Associated Smelters Pty. Ltd., as part of the research programme of the Mineragraphic Section of the Council for Scientific and Industrial Research.Analyses of the specimens are as follows:-