Development of Novel 2D NMR Techniques for Mixture Analysis

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Abstract

The analysis of high dynamic range mixtures by 1H NMR is complicated by the presence of 13C satellite signals. While satellites caused by long-range couplings are usually buried beneath homonuclear multiplet structure, one-bond satellites of major mixture components often overlap with signals from minor components, complicating both quantification and identification. Broadband 13C decoupling can eliminate, or at least greatly reduce, interference in 1H NMR from 13C isotopomer signals, but only at the cost of significant sample heating. This limits spectral resolution, because longer acquisition times will increase this heating. A recent NMR experiment, DISPEL (Destruction of Interfering Satellite by Perfect Echo Low-pass filtration), suppresses one-bond 13C satellite signals in 1D 1H spectra without the need for decoupling. This new approach is generally applicable, and it is possible to concatenate it with a wide variety of multidimensional NMR methods such as COSY and TOCSY at very low cost in signal-to-noise ratio, making it significantly easier to analyze the spectra of high dynamic range mixtures by 1H NMR.

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All the experimental and simulation data and parameters for the work described are freely available at https://dx.doi.org/10.17632/2zvkcp3hjf.1.

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NMR

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