A high-pressure high-temperature setup for in situ Raman spectroscopy of supercritical fluids

A high-pressure/high-temperature cell dedicated to Raman spectroscopy is presented. The P and T ranges are optimized for the study of supercritical fluids (T≤975K, P≤200MPa); the P and T parameters are controlled independently. The autoclave was adapted from a previous cell (designed for X-ray absorption and scattering spectroscopies) to answer the specific requirement of Raman spectroscopy. Original high pressure windows and sample cell have been developed to ensure both pressure resistance and transparency for the optical laser and Raman scattering beams. An optical integration of the autoclave in the Raman spectrometer setup was designed to perform in situ Raman experiments on fluids. The spectroscopic measurements can be combined with visual observation, which is particularly useful for the study of multi-phasic systems. As examples of the efficiency of the set-up and its scientific opportunities, we present Raman measurements on water, carbon dioxide and mixed H2O–CO2 system obtained from ambient to supercritical conditions.