固体核磁共振样品制备系统的自主研制
Independent Development of Sample Preparation Tools for Solid-state NMR
Received date: 2023-07-18
Online published: 2023-09-06
近年来，国内多个科研单位引进了固体核磁共振波谱仪．由于目前固体核磁共振波谱仪还没有国产化，完全依赖进口，因此仪器及配套的样品制备系统价格昂贵．转子是魔角旋转核磁共振实验的关键耗材，其尺寸精密度要求极高，加工难度大．通过分析进口成品3.2 mm固体核磁共振转子及其配套样品制备工具的特性和实际应用需求，改进转子各零部件之间的连接方式，优化转子的密封性，成功实现了固体核磁共振转子和配套样品制备工具箱的自主研制．测试结果表明，自主研制的转子能在12 kHz转速下正常运行，满足常规固体核磁共振实验需求，且配套的样品制备工具箱操作简单，安全可靠．
陈阳 , 周萌 , 李勇 , 杨海军 . 固体核磁共振样品制备系统的自主研制[J]. 波谱学杂志, 2024 , 41(1) : 77 -86 . DOI: 10.11938/cjmr20233074
In recent years, several research units have introduced solid-state nuclear magnetic resonance (NMR) spectrometers. So far, solid-state NMR spectrometers have not been domestically manufactured and the equipment is completely dependent on imports. Therefore, both the instruments and sample preparation systems are expensive. The sample loading rotor is the crucial consumable in the magic angle spinning (MAS) NMR experiment. However, the extremely tough requirement on dimensional precision poses a great challenge in the machining of rotors. By analyzing the characteristics and practical applications of the imported 3.2 mm rotor and its sample preparation tools, we optimized the connection between the rotor parts, improved the sealing of rotor, and developed the MAS rotor and its sample preparation tools independently. The test results show that the self-made MAS rotor can run normally at 12 kHz, which meets the requirements of conventional solid-state NMR experiments. The sample preparation toolbox has advantages of simplicity and safety.
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