Raman spectra of the III → II phase transition in normal (d0) and deuteriated (d12) tetramethylammonium chlorides

A design of a high‐temperature cell (used with a Spex‐1403 Ramalog spectrophotometer) for Raman studies with 90° geometry is given. Raman spectra of normal (d0) and denteriated (d12) tetramethylammonium chlorides in phases III and II are reported, together with their assignments. On the basis of the temperature dependence of the thermosensitive bands, the III → II phase transition was found at 367 ± 2 K for normal (d0) tetramethylam monium chloride and at 407±5 K for deuteriated (d12) tetramethylammonium chloride. It is observed that the III → II phase transition is irreversible if the samples are kept under vacuum during the investigation. Traces of moisture present in the samples are responsible for the stability of the room‐temperature phase III.