Cryogenic-compatible spherical rotors and stators for magic angle spinning dynamic nuclear polarization.
Cryogenic-compatible spherical rotors and stators for magic angle spinning dynamic nuclear polarization.
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DOI：
10.5194/mr-4-231-2023
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发表时间：
2023
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影响因子：
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通讯作者：
Barnes AB
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文献类型：
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作者：
Price LE;Alaniva N;Millen M;Epprecht T;Urban M;Däpp A;Barnes AB
低温魔角旋转（MAS）是固体核磁共振（NMR）中用于动态核极化（DNP）的标准技术。在这里，我们描述了一个具有9.5 mm直径的球形转子的低温MAS定子的优化和实现，允许在大样本量上进行DNP实验。低温MAS定子和转子的设计基于MAS球体的最新进展，并进一步纳入样品插入和弹射以及 Hz的温度无关旋转稳定性。在7 T、2.0 kHz、样品温度为105-107 K的条件下，对124 L和223 L样品体积，分别由4 M C、n标记尿素和20 mM AMUPol组成的甘油-水玻璃基质，观察到DNP增强256和200。
Cryogenic magic angle spinning (MAS) is a standard technique utilized for dynamic nuclear polarization (DNP) in solid-state nuclear magnetic resonance (NMR). Here we describe the optimization and implementation of a stator for cryogenic MAS with 9.5 mm diameter spherical rotors, allowing for DNP experiments on large sample volumes. Designs of the stator and rotor for cryogenic MAS build on recent advancements of MAS spheres and take a step further to incorporate sample insert and eject and a temperature-independent spinning stability of Hz. At a field of 7 T and spinning at 2.0 kHz with a sample temperature of 105–107 K, DNP enhancements of 256 and 200 were observed for 124 and 223 L sample volumes, respectively, each consisting of 4 M C, N-labeled urea and 20 mM AMUPol in a glycerol–water glassy matrix.