The accurate determination of trace level gold in ores, metallurgical samples and process solutions is required because of the value of gold, the efficiency of the cyanide leach process and because of the high gold recovery from these cyanide solutions. It is thus necessary to routinely analyse geological and metallurgical samples with gold concentrations of 3 g tonne (ug g- 1ppm) and process solutions with a gold concentration of 0.01 mgL 1 (ppm) preferably with sufficient accuracy to quote at least two significant figures. Several techniques have been reviewed for their suitability for the routine gold analysis of these samples which also contain signif- icant concentrations of other ions. The classic fire assay technique has achieved the respect and confidence of mining personnel because of the results achieved by very experienced assayers. Other extraction and concentration techniques have now been shown to be equally effective. The use of instrumental analytical techniques particularly atomic absorption spectrometry have shown that cheaper procedures, which are as reliable, are now available to gold producers for the routine analysis required to maintain an efficient gold recovery process.