A temperature-controlled sample shuttle for field-cycling NMR

Abstract

We present a design for a temperature-controlled sample shuttle for use in NMR measurements at variable magnetic field strength. Accurate temperature control was achieved using a mixture of water-ethylene glycol as a heat transfer fluid, reducing temperature gradients across the sample to < 0.05 °C and minimising convection. Using the sample shuttle, we show how the longitudinal (T₁) and singlet order (T_S) relaxation time constants were measured for two molecules capable of supporting long-lived states, with new record lifetimes observed at low field and above ambient temperatures.