Using a new highly stable automated electron microprobe analyser, detection limits for gold in arsenopyrite have been improved. Using the AuLA emission tine at 40kV and 500nA, a limit of approximately 10gpt is attained in 10- lSmins. Some unusual features of the background need to be taken into account. Several ores containing different levels of gold in arsenopyrite have been examined, and it has been shown that gold is not evenly distributed between grains (some may contain more than 1%, invisible optically), and that the grains containing gold are often zoned. Gold may be released from the arsenopy rite by weathering or by heating in an inert or slightly oxidising atmosphere.