Analytical and Bioanalytical Chemistry

, Volume 405, Issue 28, pp 8981–8993

Temperature-dependent size exclusion chromatography for the in situ investigation of dynamic bonding/debonding reactions

  • Josef Brandt
  • Nathalie K. Guimard
  • Christopher Barner-Kowollik
  • Friedrich G. Schmidt
  • Albena Lederer
Research Paper

DOI: 10.1007/s00216-013-7203-8

Cite this article as:
Brandt, J., Guimard, N.K., Barner-Kowollik, C. et al. Anal Bioanal Chem (2013) 405: 8981. doi:10.1007/s00216-013-7203-8
Part of the following topical collections:
  1. Separation and Characterization of Natural and Synthetic Macromolecules

Abstract

Polymers capable of dynamic bonding/debonding reactions are of great interest in modern day research. Potential applications can be found in the fields of self-healing materials or printable networks. Since temperature is often used as a stimulus for triggering reversible bonding reactions, an analysis operating at elevated temperatures is very useful for the in situ investigation of the reaction mechanism, as unwanted side effects can be minimized when performing the analyses at the same temperature at which the reactions occur. A temperature-dependent size exclusion chromatographic system (TD SEC) has been optimized for investigating the kinetics of retro Diels−Alder-based depolymerization of Diels−Alder polymers. The changing molecular weight distribution of the analyzed polymers during depolymerization gives valuable quantitative information on the kinetics of the reactions. Adequate data interpretation methods were developed for the correct evaluation of the chromatograms. The results are confirmed by high-temperature dynamic light scattering, thermogravimetric analysis, and time-resolved nuclear magnetic resonance spectroscopy at high temperatures. In addition, the SEC system and column material stability under application conditions were assessed using thermoanalysis methods, infrared spectroscopy, nitrogen physisorption, and scanning electron microscopy. The findings demonstrate that the system is stable and, thus, we can reliably characterize such dynamically bonding/debonding systems with TD SEC.

Figure

3D illustration of chromatograms of a polymer after different times of a depolymerization reaction

Keywords

Self-healing Retro Diels−Alder High-temperature SEC Temperature-dependent SEC 

Copyright information

© Springer-Verlag Berlin Heidelberg 2013

Authors and Affiliations

  • Josef Brandt
    • 1
    • 2
  • Nathalie K. Guimard
    • 3
    • 4
    • 5
  • Christopher Barner-Kowollik
    • 3
    • 4
  • Friedrich G. Schmidt
    • 6
  • Albena Lederer
    • 1
    • 2
  1. 1.Leibniz-Institute of PolymerResearch DresdenDresdenGermany
  2. 2.Technische Universität DresdenDresdenGermany
  3. 3.Preparative Macromolecular Chemistry, Institut für Technische Chemie und PolymerchemieKarlsruhe Institute of Technology (KIT)KarlsruheGermany
  4. 4.Institut für Biologische GrenzflächenKarlsruhe Institute of Technology (KIT)Eggenstein-LeopoldshafenGermany
  5. 5.Functional Surfaces GroupINM - Leibniz-Institute for New Materials GmbHSaarbrückenGermany
  6. 6.Evonik Industries AGMarlGermany

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