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Title: A high pressure cell for supercritical CO{sub 2} on-line chemical reactions studied with x-ray techniques

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 CO{sub 2} 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.
Authors:
; ;  [1] ; ; ; ; ; ;  [2] ;  [3] ;  [4]
  1. DUBBLE@ESRF, Netherlands Organisation for Scientific Research (N.W.O.), CS40220, 38043, Grenoble, Cedex 9 (France)
  2. School of Chemistry, University of Nottingham, University Park, Nottingham NG7 2RD (United Kingdom)
  3. Department of Chemical Engineering, University of Liège B6A, allée du 6 Août 3, B-4000 Liège (Belgium)
  4. Element Six BV, P.O. Box 119, 5430 AC Cuijk (Netherlands)
Publication Date:
OSTI Identifier:
22314278
Resource Type:
Journal Article
Resource Relation:
Journal Name: Review of Scientific Instruments; Journal Volume: 85; Journal Issue: 9; Other Information: (c) 2014 AIP Publishing LLC; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; 36 MATERIALS SCIENCE; ABSORPTION; CARBON DIOXIDE; COPOLYMERS; DENSITY; DIAMONDS; DISPERSIONS; FLUCTUATIONS; FLUIDS; METHACRYLATES; METHACRYLIC ACID ESTERS; PHOTONS; POLYMERIZATION; PRESSURE RANGE MEGA PA 10-100; SMALL ANGLE SCATTERING; SUPERCRITICAL STATE; TEMPERATURE DEPENDENCE; TIME RESOLUTION; X RADIATION; X-RAY DIFFRACTION; X-RAY SPECTROSCOPY