Abstract Activation of FeTi alloy could either give rise to surface segregation and subsequent oxidation of titanium and the formation of iron clusters or the formation of metastable TiFeO, suboxide. The validity of either of the postulates could be gauged by monitoring the nature and concentration of each of the oxidation states of iron and titanium by depth profile analysis by XPS. These studies showed that fresh samples contained multiple oxidation states of iron and titanium though the concentrations of lower valent oxides are usually small. Sputtering studies showed that this oxide layer is of considerable depth and during activation, iron oxides are easily reduced to the metallic state as compared to the oxides of titanium. The chemical reaction induced, segregation may be the contributing factor for the enhanced concentration of titanium on the surface of these alloys.