Real-Time Determination of Molecular Weight: Use of MaDDOSY (Mass Determination Diffusion Ordered Spectroscopy) to Monitor the Progress of Polymerization Reactions

Tooley, Owen; Pointer, William; Radmall, Rowan; Hall, Mia; Swift, Thomas; Town, James; Aydogan, Cansu; Junkers, Tanja; Wilson, Paul; Lester, Daniel; Haddleton, David

doi:10.1021/acspolymersau.4c00020

ACS Polym. Au

2024

DOI: 10.1021/acspolymersau.4c00020

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Real-Time Determination of Molecular Weight: Use of MaDDOSY (Mass Determination Diffusion Ordered Spectroscopy) to Monitor the Progress of Polymerization Reactions

Owen Tooley,

William Pointer,

Rowan Radmall

et al.

Abstract: Knowledge of molecular weight is an integral factor in polymer synthesis, and while many synthetic strategies have been developed to help control this, determination of the final molecular weight is often only measured at the end of the reaction. Herein, we provide a technique for the online determination of polymer molecular weight using a universal, solvent-independent diffusion ordered spectroscopy (DOSY) calibration and evidence its use in a variety of polymerization reactions.

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Cited by 2 publications

References 37 publications

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Pure Shift NMR in Continuous Flow

Bazzoni,

Régheasse,

Caytan

et al. 2024

Chemistry A European J

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Flow NMR is an expanding analytical approach with applications that include in‐line analysis for process control and optimisation, and real‐time reaction monitoring. The samples monitored by flow NMR are typically mixtures that yield complex 1D 1H spectra. “Pure shift” NMR is a powerful approach to simplifying 1H NMR spectra, but its standard implementation is not compatible with continuous flow because of interference between sample motion and the position‐dependent spin manipulations that are required in pure shift NMR. Here we show that pure shift NMR spectra can be successfully collected for continuously flowing samples, thanks to an adapted acquisition scheme, robust solvent suppression, and a velocity‐compensation strategy. The resulting method is used to collect ultrahigh resolution reaction monitoring data. Pure shift NMR spectra are expected to benefit many applications of flow NMR.

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Pure Shift NMR in Continuous Flow

Bazzoni,

Régheasse,

Caytan

et al. 2024

Chemistry A European J

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Atomic-Scale Imaging of Polymers and Precision Molecular Weight Analysis

Marathianos,

Magiakos,

Han

et al. 2024

J. Am. Chem. Soc.

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Polymer design requires fine control over syntheses and a thorough understanding of their macromolecular structure. Herein, near-atomic level imaging of polymers is achieved, enabling the precise determination of one of the most important macromolecular characteristics: molecular weight. By judiciously designing and synthesizing different linear metal(loid)-rich homopolymers, subnanoscale polymer imaging is achieved through annular dark field-scanning transmission electron microscopy (ADF-STEM), owing to the incorporation of high Z atoms in the side chain of the monomeric units. The molecular weight of these polymers can be precisely determined by detecting and counting their metal(loid) atoms upon ADF-STEM imaging, at sample concentrations as low as 10 μg•mL −1 . Notably, a commonly used C, H, and O-containing polymer (i.e., poly(methyl acrylate)) that was thus far inaccessible at the atomic scale is derivatized to allow for subnano-level imaging, thus expanding the scope of our approach toward the atomic-level visualization of commodity polymers.

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Real-Time Determination of Molecular Weight: Use of MaDDOSY (Mass Determination Diffusion Ordered Spectroscopy) to Monitor the Progress of Polymerization Reactions

Cited by 2 publications

References 37 publications

Pure Shift NMR in Continuous Flow

Pure Shift NMR in Continuous Flow

Atomic-Scale Imaging of Polymers and Precision Molecular Weight Analysis

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