Previous studies have shown that calciothermic reduction can be applied to reduce the oxygen content of commercially pure titanium and titanium dioxide. In this investigation, the calciothermic reduction route was examined to assess whether the process could be applied to the commercial alloy Ti-6A1-4V. Ti-6A1-4V rods were sealed in a metal container and reacted with calcium in a molten flux. The resultant material was characterised using X-Ray Diffraction (XRD),Focused Ion Beam-Secondary Ion Mass Spectrometry (FIB-SI MS) and Inert Gas Fusion to determine the hulk oxygen concentration as well as the oxygen concentration profiles. The removal of oxygen from the samples was achieved in both an inert atmosphere and also when air was present within the vessel