Publication date: 15th December 2025
Coupled benchtop EPR-NMR provides a powerful platform for studying reactions that contain both radical and organic species. NMR monitoring approaches typically rely on the 1D 1H spectra, but interpreting these signals on benchtop NMR systems can be complicated due to substantial spectral overlap, arising from the instrument’s low magnetic field and limited sensitivity. To address this limitation, we employed Multivariate Curve Resolution-Alternating Least Squares (MCR-ALS) analysis, a rigorous chemometric deconvolution approach that can extract pure component spectra from overlapping signals and track their concentration profiles over time.
Here for the first time, we established a robust analytical framework for mechanistic investigations into the electrochemical TEMPO mediated lignin conversion by integrating MCR-ALS with our operando benchtop EPR–NMR platform. The complex lignin model compound and product signal can be deconvoluted and identified in benchtop NMR spectra. Therefore, it provides detailed mechanistic insight like the kinetics, TEMPO regeneration pathway.
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