Online tracing of molecular weight evolution during radical polymerization via high-resolution FlowNMR spectroscopy

Jeroen Vrijsen; Isabel Thomlinson; Martin Levere; Catherine Lyall; Matthew Davidson; Ulrich Hintermair; Tanja Junkers

doi:10.1039/d0py00475h

Online tracing of molecular weight evolution during radical polymerization via high-resolution FlowNMR spectroscopy

Jeroen Vrijsen, Isabel Thomlinson, Martin Levere, Catherine Lyall, Matthew Davidson, Ulrich Hintermair, Tanja Junkers

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Abstract

High-resolution FlowNMR was coupled to a continuous flow reactor to monitor polymer molecular weight evolution online by diffusion ordered NMR spectroscopy. Polymers were synthesized by reversible addition fragmentation chain transfer polymerization in continuous flow. The setup allows to target various polymer chain lengths in a dynamic manner without requiring additional purification or sample preparation. Obtaining molecular weight information in this manner is shown to be more accurate than classical SEC analysis at comparable measurement times, with relative errors around 5%.

Original language	English
Pages (from-to)	3546-3550
Journal	Polymer Chemistry
Volume	11
Issue number	21
Early online date	6 May 2020
DOIs	https://doi.org/10.1039/d0py00475h
Publication status	Published - 7 Jun 2020

Funding

The authors are grateful to the Fonds Wetenschappelijk Onderzoek (FWO) for providing a SB scholarship for JHV, the Royal Society for a University Research Fellowship to UH (UF160458), and EPSRC for funding the Dynamic Reaction Monitoring Facility at the University of Bath (EP/P001475/1) and for the EPSRC Centre for Doctoral Training in Sustainable Chemical Technologies (EP/L016354/1, PhD studentship for IAT). We thank Joris Haven (Monash University), Maciek Kopec and John Lowe (University of Bath) for stimulating discussions.

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10.1039/d0py00475hLicence: CC BY

Online Tracing of Molecular Weight Evolution during Radical.PDFAccepted author manuscript, 295 KB

An Integrated, Multi-Dimensional In-Operando Reaction Monitoring Facility for Homogenous Catalysis Research
Davidson, M. (PI), Hintermair, U. (CoI), Knight, J. (CoI), Lowe, J. (CoI) & Lubben, A. T. (CoI)
Engineering and Physical Sciences Research Council
10/07/16 → 9/07/19
Project: Research council

Cite this

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abstract = "High-resolution FlowNMR was coupled to a continuous flow reactor to monitor polymer molecular weight evolution online by diffusion ordered NMR spectroscopy. Polymers were synthesized by reversible addition fragmentation chain transfer polymerization in continuous flow. The setup allows to target various polymer chain lengths in a dynamic manner without requiring additional purification or sample preparation. Obtaining molecular weight information in this manner is shown to be more accurate than classical SEC analysis at comparable measurement times, with relative errors around 5%.",

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AU - Lyall, Catherine

AU - Davidson, Matthew

AU - Hintermair, Ulrich

AU - Junkers, Tanja

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Online tracing of molecular weight evolution during radical polymerization via high-resolution FlowNMR spectroscopy

Abstract

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An Integrated, Multi-Dimensional In-Operando Reaction Monitoring Facility for Homogenous Catalysis Research

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