An MAS probe is disclosed for obtaining a substantial improvement in
signal to
noise (S / N) in triple-
resonance high-resolution (HR) magic-angle-
spinning (MAS) NMR of samples near
room temperature (RT) in high-field magnets where the
magnet's RT shim bore is greater than 60 mm. All critical circuit components, including the sample coils, are located along with the spinner
assembly in a thermally insulated
cold zone pressurized with
helium gas. The spinner
assembly attaches to a sealed, curved, rotor-loading tube to permit automatic sample change, and it is surrounded by a partially insulated jacket cooled with a cryogenic fluid, generally
nitrogen gas. The MAS probe is also compatible with
magic angle gradients, variable temperature operation, field locking, and commonly available closed-cycle cold fingers. One major challenge in implementing CryoMAS is solving the problem of gas leakage from the spinner bearing, drive, and exhaust
nitrogen into the
cold zone, as some components will necessarily be
ceramic, some plastic, and some
metal. It is not desirable to use
helium for the spinner bearing and drive gases for cost reasons and to prevent risk of degradation of o-ring-sealed
magnet cryostats. A pressurized
helium atmosphere in the
cold zone may be utilized to prevent
nitrogen flow from the spinner exhaust streams or
atmosphere into the cold zone. The drawback to a pressurized cold zone is that the
heat transfer coefficient in dense helium at low temperatures is very high, making it challenging to cool the sample coils and all the large, critical, circuit components in a practical manner. Part of the solution here is to use a first-stage cooling-jacket around the major heat leaks near the spinner exhaust flows. The critical components may be insulated with fine
glass wool or teflon foam and conduction cooled without cooling much of the cold zone below the temperature of the first-stage cooling. The use of coaxial
sapphire capacitors allows the
noise contributions from the most critical capacitors to be reduced to a minor fraction of the total.