A comprehensive understanding of mineralogical associations and gold deportment is important for identification of the causes of gold losses to tailings and in development of re-treatment procedures to recover this value. Recent advances in the QEMSCAN (R) system to enhance false positive identification have increased the speed and accuracy of gold particle determination. This increased capability has been combined with a suite of complementary diagnostic chemical techniques to provide a complete methodology for accurate and economic analysis of tailings material. Through this methodology the advantages of combining automated mineralogical techniques with more traditional diagnostic chemical assay have been demonstrated through a case study examining the flotation tailings stream of a Cu-Au operation in North Queensland, Australia. Outcomes of the case study indicated that a significant portion of gold losses were attributable to coarse free gold present in the flotation tailings. (c) 2008 Elsevier Ltd. All rights reserved.