High-Pressure-Low-Temperature Cryostat Designed for Use with Fourier Transform Infrared Spectrometers and Time-Resolved Infrared Spectroscopy

摘要

The design for a new high-pressure-low-temperature infrared (IR) cell for performing experiments using conventional Fourier transform infrared or fast laser-based time-resolved infrared spectroscopy, in a range of solvents, is described. The design builds upon a commercially available compressor and cold end (Polycold PCC and CryoTiger), which enables almost vibration-free operation, ideal for use with sensitive instrumentation. The design of our cell and cryostat allows for the study of systems at temperatures from 77 to 310 K and at pressures up to 250 bar. The CaF_2 windows pass light from the mid-IR to the ultraviolet (UV), enabling a number of experiments to be performed, such as Raman, UV-visible absorption spectroscopy, and time-resolved techniques where sample excitation/probing using continuous wave or pulsed lasers is required. We demonstrate the capabilities of this cell by detailing two different applications: (i) the reactivity of a range of Group V-VII organometallic alkane complexes using time-resolved spectroscopy on the millisecond timescale and (ii) the gas-to-liquid phase transition of CO_2 at low temperature, which is applicable to measurements associated with transportation issues related to carbon capture and storage.