500-fold enhancement of in situ 13C liquid state NMR using gyrotron-driven temperature-jump DNP

A 550-fold increase in the liquid state C-13 NMR signal of a 50 mu L sample was obtained by first hyperpolarizing the sample at 20 K using a gyrotron (260 GHz), then, switching its frequency in order to apply 100 W for 1.5 s so as to melt the sample, finally, turning off the gyrotron to acquire the C-13 NMR signal. The sample stays in its NMR resonator, so the sequence can be repeated with rapid cooling as the entire cryostat stays cold. DNP and thawing of the sample are performed only by the switchable and tunable gyrotron without external devices. Rapid transition from DNP to thawing in one second time scale was necessary especially in order to enhance liquid H-1 NMR signal. (C) 2016 Elsevier Inc. All rights reserved.