Interaction of methanol with a layered α-Sn(IV) phosphate on its surface: A solid-state NMR study

A layered crystalline phosphate, alpha-Sn(HPO4)2 center dot H2O, treated with CD3OD was characterized by the 31P, 119Sn, 1H and 2H solid-state NMR techniques. The 2H solid-echo MAS NMR spectra of the product have unexpectedly revealed deuterated hydronium ions on the surface of this material instead of intercalated methanol. According to the 13C NMR and GC-MS studies, these ions are formed by water molecules following a dehydration of the methanol-d4 to yield deuterated dimethyl ether.

Automated summary

A layered crystalline phosphate, alpha-Sn(HPO4)2 center dot H2O, treated with CD3OD was characterized by solid-state NMR techniques. Surprisingly, deuterated hydronium ions were found on the surface of the material instead of intercalated methanol. This phenomenon was confirmed by 13C NMR and GC-MS studies, indicating the formation of deuterated dimethyl ether from the dehydration of methanol-d4.