X-ray fluorescence spectroscopy used for the analysis of mill samples results in improved control of flotation concentrators.Techniques and equipment for sampling pulp streams, filtration and drying, grinding, briquetting and X-ray fluorescence analysis of samples have been developed.The current methods in use permit the analysis for lead and zinc in six pulp samples within 30 min total elapsed from the start of sampling. The X-ray method gives a precision at least equal to the former routine wet-way assay methods.The equipment is used also for pilot plant control, as a means of solving complicated analytical problems and in the rapid qualitative analysis of exploration samples.INTRODUCTIONIn milling and concentrating operations, classical methods for the assay of lead and zinc have been mainly of use for accounting purposes and for the post-mortem examination of plant operations, but have been of little value for rapid mill control. Where attempts have been made to apply these methods to control assaying, it has been necessary to modify the procedures and introduce short cuts which have tended to reduce their reliability.Even with these shortened procedures, the time taken to obtain a limited amount of information rendered them of little value for the control of milling operations where sudden, large fluctuations can occur. In recent years, a number of new and rapid analytical techniques, based on physical rather than chemical principles, have been introduced.These include direct reading emission spectroscopy, x-ray fluorescence spectroscopy and atomic absorptionspectroscopy.