Jump to main content
Jump to site search


On-line SEC-MR-NMR hyphenation: optimization of sensitivity and selectivity on a 62 MHz benchtop NMR spectrometer

Author affiliations

Abstract

The development of sophisticated synthetic routes for polymeric materials and more complex formulations used in current products require more advanced analytical techniques. As simple 1D experiments do not suffice to provide the necessary information. The development of coupled techniques, especially liquid chromatography (LC) in conjunction with molecular spectroscopy, is one promising approach to fit these requirements. The focus of this article is the optimization of a medium resolution (MR), benchtop 1H-NMR spectrometer coupled to a SEC instrument, where the NMR acts as an on-line chemical selective detector. The approach is to retain typical SEC selectivity while obtaining NMR on-line data with the highest possible sensitivity through full optimization of the entire set-up, pulse sequence and numerical data evaluation. A detailed description will be provided on how each part has been improved, including instrumental demands e.g. custom designed flow cells. Application examples of a PS/PMMA blend and PS-b-PMMA block copolymer are given to illustrate the potential of the hyphenated technique and the necessity of optimization. It is shown that the MR-NMR can be successfully hyphenated to SEC as an information rich chemical detector, providing the average chemical composition (CC) as a function of molar mass distribution (MMD), for polymers at isocratic mobile phase conditions.

Graphical abstract: On-line SEC-MR-NMR hyphenation: optimization of sensitivity and selectivity on a 62 MHz benchtop NMR spectrometer

Back to tab navigation

Publication details

The article was received on 27 Jan 2019, accepted on 03 Apr 2019 and first published on 09 Apr 2019


Article type: Paper
DOI: 10.1039/C9PY00140A
Citation: Polym. Chem., 2019, Advance Article
  • Open access: Creative Commons BY license
  •   Request permissions

    On-line SEC-MR-NMR hyphenation: optimization of sensitivity and selectivity on a 62 MHz benchtop NMR spectrometer

    C. Botha, J. Höpfner, B. Mayerhöfer and M. Wilhelm, Polym. Chem., 2019, Advance Article , DOI: 10.1039/C9PY00140A

    This article is licensed under a Creative Commons Attribution 3.0 Unported Licence. Material from this article can be used in other publications provided that the correct acknowledgement is given with the reproduced material.

    Reproduced material should be attributed as follows:

    • For reproduction of material from NJC:
      [Original citation] - Published by The Royal Society of Chemistry (RSC) on behalf of the Centre National de la Recherche Scientifique (CNRS) and the RSC.
    • For reproduction of material from PCCP:
      [Original citation] - Published by the PCCP Owner Societies.
    • For reproduction of material from PPS:
      [Original citation] - Published by The Royal Society of Chemistry (RSC) on behalf of the European Society for Photobiology, the European Photochemistry Association, and RSC.
    • For reproduction of material from all other RSC journals:
      [Original citation] - Published by The Royal Society of Chemistry.

    Information about reproducing material from RSC articles with different licences is available on our Permission Requests page.

Search articles by author

Spotlight

Advertisements