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The uptake and reaction of methanol at the air-liquid interface of 0 to 96.5 wt% sulfuric acid (SA) solutions has been observed directly using vibrational sum frequency generation spectroscopy (VSFG) and Raman spectroscopy. Evidence for the formation of methyl hydrogen sulfate (MHS) was obtained by the presence of a new peak in the 800
cm-1 region, not present in either the neat methanol or concentrated sulfuric acid spectra. This peak is attributed to the singly bonded OSO symmetric stretch of MHS. The maximum yield of MHS with a large SA excess (7 SA : 1 methanol) is shown to be (95 ± 5) % at –(15 ± 2) ºC. No evidence was found to suggest formation of dimethyl sulfate.
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