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Iron immobilized on supports such as silica, alumina, titanium oxide, and zeolite can activate hydrogen peroxide (H 2 O 2 ) into strong oxidants. However, the role of the support and the nature of the oxidants produced in this process remain elusive. This study investigated the activation of H 2 O 2 by a TiO 2 -supported catalyst (FeTi-ox). Characterizing the catalyst surface in situ using X-ray absorption spectroscopy (XAS), together with X-ray photoelectron spectroscopy (XPS) and electron paramagnetic resonance (EPR), revealed that the interaction between H 2 O 2 and the TiO 2 phase played a key role in the H 2 O 2 activation. This interaction generated a stable peroxo−titania Fe(III)−Ti−OOH complex, which reacted further with H 2 O to produce a surface oxidant, likely Fe[IV]  O 2+ . The oxidant effectively degraded acetaminophen, even in the presence of chloride, bicarbonate, and organic matter. Unexpectedly, contaminant oxidation continued after the H 2 O 2 in the solution was depleted, owing to the decomposition of Fe(III)−Ti−OOH by water. In addition, the FeTi-ox catalyst effectively degraded acetaminophen over five testing cycles. Overall, new insights gained in this study may provide a basis for designing more effective catalysts for H 2 O 2 activation.

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