The adaptation and construction of an environmental chamber suitable for FT-Raman spectroscopy is described for the recording of Raman spectra of specimens at temperatures from 25 to 125 °C while exposed to different controlled synthetic atmospheric conditions. Test spectra were obtained from sulfur to illustrate the stability and applications of the system. The α rhombic/β monoclinic phase change in sulfur was monitored as a function of time, and bands sensitive to this phase change have been identified.