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Determination of Copolymer Block-Length Distributions Using Fragmentation Data Obtained from Tandem Mass

Tijmen S Bos1,2, Rick S van den Hurk1,2, Ynze Mengerink3,4

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Mass spectrometry/mass spectrometry (MS/MS) can now determine copolymer block-length distributions (BLDs), offering detailed insights into polymer chemistry. This new method complements traditional nuclear magnetic resonance (NMR) techniques for advanced material characterization.

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Area of Science:

  • Polymer Chemistry
  • Analytical Chemistry
  • Materials Science

Background:

  • Traditional methods like nuclear magnetic resonance (NMR) primarily determine number-average block length in copolymers.
  • Characterizing the full block-length distribution (BLD) provides deeper insights into polymer structure and properties.

Purpose of the Study:

  • To develop and validate a mass spectrometry/mass spectrometry (MS/MS) based method for determining copolymer BLDs.
  • To demonstrate the viability of MS/MS as an alternative to NMR for BLD characterization.
  • To enable detailed analysis of copolymer chemistry and its relation to synthesis methods.

Main Methods:

  • Development and implementation of a novel algorithm to analyze MS/MS fragmentation data.
  • The algorithm incorporates bond fragmentation preferences for accurate BLD determination.
  • Evaluation using polyamide and polyurethane model systems.

Main Results:

  • The developed algorithm successfully determined BLDs from MS/MS data for both polyamide and polyurethane copolymers.
  • Derived BLDs showed strong correlation with average block lengths obtained via 13C NMR.
  • The method revealed typical BLD trends linked to specific synthesis routes.

Conclusions:

  • MS/MS is a viable and powerful technique for characterizing copolymer BLDs.
  • The new algorithm provides detailed insights into copolymer microstructure, aiding in understanding property variations.
  • This approach enhances the ability to correlate synthesis methods with resulting polymer architectures and properties.