High-energy ball milling treatment leads to full dissolution of natural ilmenite sands containing both FeTiO 3 and Fe 2 Ti 3 O 9 phases in a sulphuric acid solution at 100°C. The ilmenite material has been milled for various times in two environments (vacuum and air), and characterised by X-ray diffraction, Mössbauer spectroscopy and surface area analysis. It is found that after milling for only 10h, 50% of the sample can be dissolved as a result of the increased surface area, nanocrystalline structure and high level of lattice distortion present in the milled sample. Complete dissolution of the ilmenite is obtained on extended milling (200 h) in an oxygen free atmosphere. This occurs as a result of a gradual reduction of the Fe 3+ phase (Fe 2 Ti 3 O 9 ) to the relatively more soluble Fe 2+ phase (FeTiO 3 ) on milling in vacuum. The results overall show that the chemical reactivity of milled materials can be affected significantly by the milling conditions and environment.