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5. Low‐field 1 H NMR spectroscopy: Factors impacting signal‐to‐noise ratio and experimental time in the context of mixed microstructure polyisoprenes

   https://doi.org/10.1002/mrc.5022  

   Minkler, Jr, Michael J. ; Kim, Jung Min ; Shinde, Vinita V. ; Beckingham, Bryan S. ( April 2020 , Magnetic Resonance in Chemistry)

   Low‐cost, high‐accuracy characterization of polymeric materials is critical for satisfying societal demand for high‐quality materials with ultra‐specific requirements. Low‐field nuclear magnetic resonance (NMR) spectroscopy presents an opportunity to replace costlier or destructive methods while utilizing nondeuterated solvents. Many factors play key roles in the ability of low‐field NMR spectroscopy to accurately analyze polymer systems. Sample characteristics such as polymer concentration, composition, and molecular weight all directly affect the capability of low‐field spectrometers to accurately determine polymer microstructure compositions. In addition to inherent sample properties affecting instrumental accuracy, many choices concerning instrumental parameters (including number of scans, relaxation delay, spectral width, and points per scan) must be made that impact the quality of the resulting NMR spectra. In this work, we benchmark the capability of a 60‐MHz low‐field NMR spectrometer for analyzing polymer materials using mixed microstructure polyisoprenes as a model polymer system of interest. The aforementioned critical sample and instrumental variables are varied, and we report on the ability to quantitatively characterize polyisoprene microstructure to within 1–2% of a higher field NMR spectrometer (400 MHz). We anticipate our findings to be generally applicable to other low‐field spectrometers of similar field strength and other polymer systems.

    

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