A design of a high-temperature cell (used with a Spex-1403 Ramalog spectrophotometer) for Raman studies with 90" geometry isgiven. Raman spectra of normal (do) and deuteriated (dlz) tetramethylammonium chlorides in phases 111 and I1 are reported, together with their assignments. On the basis of the temperature dependence of the thermosensitive bands, the 1II + I1 phase transition was found at 367 f 2 K for normal (do) tetramethylammonium chloride and at 4 0 7 f 5 K for deuteriated (dI2) tetramethylammonium chloride. It is observed that the III+ I1 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 111.
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