This paper reports on the difficulties of finding an accurate and consistent test method for quantifying the segregation of two fine powders. The background is from an industrial project investigating the feasibility of blending pulverised coal and crushed nickel ore in a bulk materials handling application, to ultimately produce nickel. The feasibility of combining the two products early in the process was investigated due to the blend requiring various different handling methods throughout the industrial process, making the constituent products susceptible to segregation. In the experimental investigation, representative samples of each bulk material were used to create a range of blends of the two products in the hopes of being able to develop a calibration curve to compare against collected samples. A number of tests were investigated; colour intensity, laser particle sizing, particle density, loose-poured bulk density, relative density and tapped bulk density. Each test method produced varied and at times inconsistent results and these will be discussed, however, ultimately one tapped bulk density method proved to show consistency.