Field dependence curve on 2 M 13C urea in glycerol-d8–D2O–H2O (60 : 30 : 10 volume ratio) with 15 mM TOTAPOL biradical. The NMR field was swept while the gyrotron remained at fixed frequency, 263.343 GHz. Each field position was measured with 13C CPMAS experiment with microwaves on and off for calculating the DNP signal enhancement. 4 scans, 10 s recycle delay, and 2 dummy scans per experiment, ωr/2π = 5.1 kHz, 105 K sample temperature. The transmitter frequency of the 1H and 13C channel was adjusted for each field point. Error bars on the DNP signal enhancement measurements are ±2%.