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

Journal Article · Mon Sep 15 00:00:00 EDT 2014 · Review of Scientific Instruments

DOI:https://doi.org/10.1063/1.4895717· OSTI ID:22314278

Hermida-Merino, Daniel; Portale, Giuseppe; Bras, Wim ^[1]; Fields, Peter; Wilson, Richard; Bassett, Simon P.; Jennings, James; Dellar, Martin; Gommes, Cedric ^[2]; Vrolijk, Benno C. M. ^[3]

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1. DUBBLE@ESRF, Netherlands Organisation for Scientific Research (N.W.O.), CS40220, 38043, Grenoble, Cedex 9 (France)
2. Department of Chemical Engineering, University of Liège B6A, allée du 6 Août 3, B-4000 Liège (Belgium)
3. Element Six BV, P.O. Box 119, 5430 AC Cuijk (Netherlands)

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.

• OSTI ID: 22314278
• Journal Information: Review of Scientific Instruments, Vol. 85, Issue 9; Other Information: (c) 2014 AIP Publishing LLC; Country of input: International Atomic Energy Agency (IAEA); ISSN 0034-6748
• Country of Publication: United States
• Language: English

Related Subjects

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