The grouping and segregation error is one of Gy's seven errors that cannot be measured in any qualitative manner because of its transient and changing characteristics each time the sample is handled mechanically. Attempts to calculate the mean and variance of the segregation error is considered by some as an exercise in futility' that would not help us achieve representative sampling. This research is aimed at understanding the process of segregation of dense, finely divided and dilute particulate materials supported in a clean quartz substrate during intense agitation. Several mixtures of fine-grained materials including steel, tungsten carbide and gold grains were used in these experiments. Four hundred grains of each of the minerals and metals at a top size of 2 mm were mixed with approximately 600 g of finely ground quartz material (95 per cent passing 2000 microns) in a 500 ml plastic jar with a sealable lid. The mineral-metal mixtures were analysed in three steps using microfocus X-ray computed tomography. Step one consisted of rolling the containers on a flat surface in an attempt to concentrate the mineral and metal grains in the core of the supporting substrate; this is a base case that can be reconstructed after each session of analysis. The second step involved gentle and vigorous shaking of the mixtures in order to segregate the denser minerals and metals from the supporting quartz substrate. In some cases, a third step involved splitting the sample through a riffle splitter. Three-dimensional images of the surface of each grain, its volume and its X-, Y- and Z-coordinates, before and after intense agitation of the container, were interpreted from the reconstruction of the tomographic X-ray data. The spatial analysis of grains using cell declustering and 3D variography provided a useful means of characterising the distribution of the grains in space and the extent to which they had become segregated during the process of agitation. Spatial analysis indicates that in general, grouping and continuity of grains is weakly developed. The modelled nugget effect remains high for most tests, indicating that grains of similar size did not group together strongly. Agitation through rolling provided the best continuity, although not consistently in the long axis of the plastic jar. The nugget effect was consistently highest, and the range of continuity shortest in samples that had been split, indicating that the grouping and continuity were reduced through splitting the sample. Initial results indicate that very little segregation of the minerals and metals occurs in the quartz substrate. This is somewhat counter-intuitive, but suggests that the effects of agitation on mixtures of dense minerals and metals in substrates of lower density do not lead to excessive segregation. Differences in behaviour between dense materials in response to agitation are evident. Grains of different composition and shape did not group and segregate in a predictable manner in response to the agitation methods. Initial results indicate that the degree to which a material groups and segregates relates more to the characteristics of the denser material itself, rather than the agitation method employed.CITATION:Minnitt, R C A, Jashashvili, T, Gilchrist, G and Dominy, S C, 2017. Quantifying segregation of minerals and metals in particulate materials using computed X-ray tomography and variography, in Proceedings Eighth World Conference on Sampling and Blending , pp 173-182 (The Australasian Institute of Mining and Metallurgy: Melbourne).