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Updated: Apr 23, 2026

High-pressure Sapphire Cell for Phase Equilibria Measurements of CO2/Organic/Water Systems
Published on: January 24, 2014
A high pressure cell for supercritical CO₂ on-line chemical reactions studied with X-ray techniques
Daniel Hermida-Merino1, Giuseppe Portale1, Peter Fields2
1DUBBLE@ESRF, Netherlands Organisation for Scientific Research (N.W.O.), CS40220, 38043, Grenoble, Cedex 9, France.
Abstract:
A versatile high pressure X-ray sample cell has been developed for conducting in situ time-resolved X-ray scattering experiments in the pressure and temperature regime required (pressures up to 210 bars and temperatures up to 120 °C) for chemical reactions in supercritical fluids. The large exit opening angle of the cell allows simultaneous performance of SAXS-WAXS experiments. Diamond windows are used in order to benefit from the combination of maximum strength, minimal X-ray absorption and chemical inertia. The sample cell can also be utilised for X-ray spectroscopy experiments over a wide range of photon energies. Results of the online synthesis of a block copolymer, poly(methyl methacrylate-block-poly(benzyl methacrylate), by Reversible Addition-Fragmentation Chain Transfer (RAFT) in a supercritical CO2 dispersion polymerisation will be discussed. The contribution of the density fluctuations, as function of temperature, to the X-ray scattering signal has been quantified in order to allow appropriate background subtractions.
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