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Understanding how electrolyte composition controls electrocatalytic reactions requires molecular-level insight into electrode/electrolyte interaction. Perhaps the most basic aspect of this interaction, the speciation of the interfacial ion, is often controversial for even relatively simple systems. For example, for Pt(111) in 0.5 M H 2 SO 4 it has long been debated whether the adsorbed anion is SO 4  2- , HSO 4  - or an H 3 O + SO 4  2- ion pair. Here we apply interface-specific vibrational sum frequency (VSF) spectroscopy and theory to this problem and perform an isotope exchange study: we collect VSF spectra of Pt(111) in H 2 SO 4 (H 2 O) and D 2 SO 4 (D 2 O) as a function of bias and show that at all potentials they are identical. This is the most direct spectroscopic evidence to date that SO 4  2- is the dominant adsorbate, despite the fact that at 0.5 M H 2 SO 4 bulk solution is dominated by HSO 4  - . This approach is based on the unique selection rule of the VSF spectroscopy and thus offers a new way of accessing general electrode/electrolyte interaction in electrocatalysis.

Resolving the chemical identity of H2SO4 derived anions on Pt(111) electrodes: they're sulfate

Resolving the chemical identity of H₂SO₄ derived anions on Pt(111) electrodes: they're sulfate