MaDDOSY: Mass determination diffusion ordered spectroscopy on the bench top Owen Tooley, William Pointer, Rowan Radmall, Mia Hall, Daniel Lester, Paul Wilson, David Haddleton University of Warwick, Department of Chemistry, UK Control over molecular weight is one of the most important parameters in polymer synthesis, and yet often only once a reaction has finished is the molecular weight of the polymer determined. Here we present a universal, solvent-independent [1] calibration curve for the rapid determination of polymer molecular weight using a benchtop NMR spectrometer, which provides a system in which no external calibration is required prior to measurement. We show results of calculated molecular weight for a wide range of polymer types and solvent systems. We also present an automated sampling method for the monitoring of monitoring molecular weight as a reaction proceeds using rapid diffusion-ordered spectroscopy (DOSY) measurements. We evidence the reaction monitoring capability of this system through the monitoring of 4 polymerizations in non-deuterated solvents using a range of mechanisms. We see the results are comparable to those obtained by offline GPC, while providing a much shorter measurement time, and requiring the use of no additional solvent, whilst being able to return the sample to the reaction mixture following measurement. References 1. P.-J. Voorter, A. McKay, J. Dai, O. Paravagna, N. R. Cameron and T. Junkers, Angew. Chem. Int. Ed., 2022, 61, e202114536.
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