Rapid-melt DNP for multidimensional and heteronuclear high-field NMR experiments

Low sensitivity is the main limitation of NMR for efficient chemical analysis of mass-limited samples. Hyperpolarization techniques such as Dynamic Nuclear Polarization (DNP) have greatly improved the efficiency of NMR experiments. In this manuscript, we demonstrate a 400 MHz rapid-melt DNP setup. With this setup it is possible to perform liquid-state NMR experiments with solid-state DNP enhancement at high magnetic field. Sample volumes of 100 nL in fused-silica capillaries are detected using a stripline microcoil. Due to the small heat capacity of these samples it is possible to melt them with relatively low relaxation losses. With this 400 MHz setup, proton enhancements of up to -175 have been obtained in the liquid-state. The probe is double tuned, so it can be used for heteronuclear DNP-NMR and since the sample composition does not change during the experiment, it is possible to perform signal averaging and multidimensional experiments. This type of rapid-melt DNP setup thus allows for most types of liquid-state NMR experiments to be combined with efficient solid-state DNP. This makes rapid-melt DNP an interesting method for high-throughput chemical analysis of mass-limited samples. (C) 2019 The Author(s). Published by Elsevier Inc.