Ultra-Low Temperature Nuclear Magnetic Resonance

Because NMR spectroscopy requests more sensitivity and more resolution, high-frequency and high-power microwave irradiation of electron spins in a magnetic field, Dynamic Nuclear Polarization (DNP) is becoming a common partner for fast sample spinning NMR experiments. Currently, this technics is performed at minimum sample temperatures ∼100 K, using cold nitrogen gas to pneumatically spin and cool the sample. The desire is to improve NMR by providing ultra-low temperatures, using cryogenic helium gas. It is shown that stable and fast spinning can be attained for sample temperatures down to 30 K using a cryostat developed in our laboratory. Using this cryostat to cool a closed-loop of helium gas results in spinning frequencies that can greatly surpass those achievable with nitrogen gas. It results in substantial sensitivity enhancements (∼ 600) and according experimental time-savings by 2 to 4 orders of magnitude. Therefore, access to this temperature range is demonstrated to be both viable and highly pertinent. (paper)