Despite flash smelting's widespread use little is known about the actual processes taking place in flash furnace shafts and comparatively few reports of sampling campaigns have appeared in the published literature. his paper reviews the previous reports of the use of horizontal trough samplers and analyses their expected collection efficiency. In the light of the deficiencies revealed by this analysis an isokinetic sampler was produced and a vertical sampling technique was also developed to obtain samples from directly below the burners in the shaft of the flash furnace at the Kalgoorlie nickel smelter. Comparison of the sizing of the samples obtained with the horizontal trough and isokinetic samplers confirmed the theoretical analyses and showed that the trough samplers were not collecting the fine particles. Besides providing data to validate mathematical models of the burners and shaft, chemical analyses of the shaft samples showed that the coal in the charge was reacting preferentially and that the plume of at least one of the burners was being deflected from its axial position. In the region directly below the burner there was evidence that the disperser on the burner was imparting more momentum to the coarser particles and that these were concentrating in the outer regions of the particle plumes issuing from the burners.