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

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 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
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 85; Journal Issue: 9; Other Information: (c) 2014 AIP Publishing LLC; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0034-6748
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

Citation Formats

Hermida-Merino, Daniel, Portale, Giuseppe, Bras, Wim, E-mail: Wim.Bras@esrf.eu, E-mail: Steve.Howdle@nottingham.ac.uk, Fields, Peter, Wilson, Richard, Bassett, Simon P., Jennings, James, Dellar, Martin, Howdle, Steven M., E-mail: Wim.Bras@esrf.eu, E-mail: Steve.Howdle@nottingham.ac.uk, Gommes, Cedric, and Vrolijk, Benno C. M. A high pressure cell for supercritical CO{sub 2} on-line chemical reactions studied with x-ray techniques. United States: N. p., 2014. Web. doi:10.1063/1.4895717.
Hermida-Merino, Daniel, Portale, Giuseppe, Bras, Wim, E-mail: Wim.Bras@esrf.eu, E-mail: Steve.Howdle@nottingham.ac.uk, Fields, Peter, Wilson, Richard, Bassett, Simon P., Jennings, James, Dellar, Martin, Howdle, Steven M., E-mail: Wim.Bras@esrf.eu, E-mail: Steve.Howdle@nottingham.ac.uk, Gommes, Cedric, & Vrolijk, Benno C. M. A high pressure cell for supercritical CO{sub 2} on-line chemical reactions studied with x-ray techniques. United States. doi:10.1063/1.4895717.
Hermida-Merino, Daniel, Portale, Giuseppe, Bras, Wim, E-mail: Wim.Bras@esrf.eu, E-mail: Steve.Howdle@nottingham.ac.uk, Fields, Peter, Wilson, Richard, Bassett, Simon P., Jennings, James, Dellar, Martin, Howdle, Steven M., E-mail: Wim.Bras@esrf.eu, E-mail: Steve.Howdle@nottingham.ac.uk, Gommes, Cedric, and Vrolijk, Benno C. M. Mon . "A high pressure cell for supercritical CO{sub 2} on-line chemical reactions studied with x-ray techniques". United States. doi:10.1063/1.4895717.
@article{osti_22314278,
title = {A high pressure cell for supercritical CO{sub 2} on-line chemical reactions studied with x-ray techniques},
author = {Hermida-Merino, Daniel and Portale, Giuseppe and Bras, Wim, E-mail: Wim.Bras@esrf.eu, E-mail: Steve.Howdle@nottingham.ac.uk and Fields, Peter and Wilson, Richard and Bassett, Simon P. and Jennings, James and Dellar, Martin and Howdle, Steven M., E-mail: Wim.Bras@esrf.eu, E-mail: Steve.Howdle@nottingham.ac.uk and Gommes, Cedric and Vrolijk, Benno C. M.},
abstractNote = {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.},
doi = {10.1063/1.4895717},
journal = {Review of Scientific Instruments},
issn = {0034-6748},
number = 9,
volume = 85,
place = {United States},
year = {2014},
month = {9}
}