Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR

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Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR

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08-13-2015, 02:00 PM

nmrlearner

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Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR

Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR

Publication date: Available online 12 August 2015
Source:Journal of Magnetic Resonance

Author(s): Yoh Matsuki, Shinji Nakamura, Shigeo Fukui, Hiroto Suematsu, Toshimichi Fujiwara

Magic-angle spinning (MAS) NMR is a powerful tool for studying molecular structure and dynamics, but suffers from its low sensitivity. Here, we developed a novel helium-cooling MAS NMR probe system adopting a closed-loop gas recirculation mechanism. In addition to the sensitivity gain due to low temperature, the present system has enabled highly stable MAS (v R = 4 – 12 kHz) at cryogenic temperatures (T = 35 – 120 K) for over a week without consuming helium at a cost for electricity of 16 kW/hr. High-resolution 1D and 2D data were recorded for a crystalline tri-peptide sample at T = 40 K and B 0 = 16.4 T, where an order of magnitude of sensitivity gain was demonstrated versus room temperature measurement. The low-cost and long-term stable MAS strongly promotes broader application of the brute-force sensitivity-enhanced multi-dimensional MAS NMR, as well as dynamic nuclear polarization (DNP)-enhanced NMR in a temperature range lower than 100 K.
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Source: Journal of Magnetic Resonance

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