Scanning electron microscope-Mineral Liberation Analyser SEM-MLA can be used to discriminate between hematite/magnetite in iron ores, but achieving backscattered electron (BSE) segmentation between the two minerals is difficult for particles 75 m using typical preparation and analysis methods for the MLA based on a tungsten filament SEM (Quanta 400) with 25 kV high voltage. Preparing iron ore sample mounts using a slow-speed polishing method, and conducting the experiment on a field emission gun SEM-MLA (Quanta 650) with the high voltage (HV) setting lowered to 15 kV reduces instrument noise and results in very clean BSE images and segmentation. This method requires new X-ray standards to be acquired for each mineral identity at 15 kV because of major changes in the spectra at lower kV. However, once these X-rays are added to the mineral reference list, effective segmentation can be achieved and a proper analysis obtained.CITATION:Grant, D C, Goudie, D J, Voisey, C, Shaffer, M and Sylvester, P, 2017. Discriminating hematite/magnetite via scanning electron microscope-mineral liberation analyser in the - mesh size fraction of iron ores, in Proceedings Iron Ore 2017, pp 541-548 (The Australasian Institute of Mining and Metallurgy: Melbourne).