Electron probe microanalysis (EPMA) and quantitative X-ray diffraction (QXRD) techniques are capable of providing high-quality quantitative information regarding the phase mineralogy and distribution of alumina within iron ore samples. The techniques, however, use different methodologies in determining the mineralogical information (ie structural versus chemical), which introduces some limitations. In this study, EPMA was used to identify and quantify the deportment of alumina within mineral phases in iron ore samples (-1 mm crushed) sourced from different suppliers. Results were directly compared with quantitative mineralogical data derived from QXRD to provide an evaluation of the relative merits of both techniques. The four ores studied contained alumina either in the form of gibbsite, aluminosilicates (eg kaolinite), or associated with goethite.For minor phases, gibbsite and kaolinite, the abundance trends measured via QXRD were generally reflected in the EPMA data. Agreement was less satisfactory for the more abundant goethite phase (both low- and high-Al forms). The discrepancy may be the result of sampling issues arising from textural features such as grain size, and also a systematic overestimate in the amount of Al-rich goethite when hematite and Al-bearing phases are finely intermixed and the EPMA step size is coarse. A second difference in the EPMA results compared to the QXRD data was in regard to quantification of low-Al and high-Al goethite phases. The sensitivity of the chemical-based EPMA was better for distinguishing between high- and low-Al goethite although the results remain overprinted by potential errors introduced via sampling.Care should be taken when directly comparing results from each method, although in general the data should be considered complementary, as each approach provides slightly different results and interpretations regarding the overall mineralogy.CITATION:Pownceby, M I, MacRae, C M and Torpy, A, 2017. A comparison of X-ray and electron-based analysis techniques for characterising the mineralogy and alumina distribution in iron ores, in Proceedings Iron Ore 2017, pp 593-598 (The Australasian Institute of Mining and Metallurgy: Melbourne).