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Issue 6, 2020
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DNP NMR spectroscopy of cross-linked organic polymers: rational guidelines towards optimal sample preparation

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Abstract

Cross-linked polystyrenes (PS) are an important class of polymers, whose properties are strongly dependent on incorporated functionalities, for which detailed understanding of their structure remains a challenge. Here, we develop a rational guideline for dynamic nuclear polarization (DNP) sample formulation for cross-linked PS to interrogate their structure. We show that the DNP enhancement on a series of cross-linked PS bearing alkylammonium groups as prototypical organic polymers correlates with the polymer swelling properties in both apolar and polar formulations (TEKPol/1,1,2,2-tetrachloroethane and AMUPol/dimethyl sulfoxide). This work provides guidelines to easily optimize DNP formulation using a simple swelling test and enables natural abundance 15N NMR to be recorded on a series of PS-supported quaternary alkylammonium salts, allowing a detailed structural analysis.

Graphical abstract: DNP NMR spectroscopy of cross-linked organic polymers: rational guidelines towards optimal sample preparation

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Article information


Submitted
21 Sep 2019
Accepted
11 Dec 2019
First published
12 Dec 2019

Phys. Chem. Chem. Phys., 2020,22, 3184-3190
Article type
Paper

DNP NMR spectroscopy of cross-linked organic polymers: rational guidelines towards optimal sample preparation

S. Tanaka, W. Liao, A. Ogawa, K. Sato and C. Copéret, Phys. Chem. Chem. Phys., 2020, 22, 3184
DOI: 10.1039/C9CP05208A

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