A study was made of the instrumentation and technique of atomic absorption spectroscopy developed by Walsh of the Commonwealth Scientific and Industrial Research Organisation (CSIRO), Australia.The method was evaluated for the determination of silver in lead sulphide concentrate. The precision of the procedure developed is equal to that of the uncorrected fire assay method and the accuracy is greater.Brief mention is made of the use of this technique for the determination of silver and other elements in ores and concentrator products.