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用于固态核磁共振样品和转子处理的完整3D打印工具套件。

A complete 3D-printed tool kit for Solid-State NMR sample and rotor handling.

作者信息

Olson Martin A, Han Ruixian, Ravula Thirupathi, Borcik Collin G, Wang Songlin, Viera Perla A, Rienstra Chad M

机构信息

Department of Biochemistry, University of Wisconsin-Madison, Madison, WI, 53706 USA.

Department of Chemistry, University of Wisconsin-Madison, Madison, WI, 53706 USA.

出版信息

J Magn Reson. 2024 Sep;366:107748. doi: 10.1016/j.jmr.2024.107748. Epub 2024 Aug 6.

Abstract

Solid state NMR (SSNMR) is a highly versatile and broadly applicable method for studying the structure and dynamics of biomolecules and materials. For scientists entering the field of SSNMR, the many quotidian activities required in the workflow to prepare samples for data collection can present a significant barrier to adoption. These steps include transfer of samples into rotors, marking the reflective surfaces for high sensitivity tachometer signal detection, inserting rotors into the magic-angle spinning (MAS) stator, achieving stable spinning, and removing and storing rotors to ensure reproducibility of data collection conditions. Even experienced spectroscopists experience occasional problems with these operations, and the cumulative probability of a delay to successful data collection is high enough to cause frequent disruptions to instrument schedules, particularly in the context of large facilities serving a diverse community of users. These problems are all amplified when utilizing rotors smaller than about 4 mm in diameter. Therefore, to improve the reliability and robustness of SSNMR sample preparation workflows, here we describe a set of tools for rotor packing, unpacking, tachometer marking, extraction and storage. Stereolithography 3D printing was employed as a cost-effective and convenient method for prototyping and manufacturing a full range of designs suitable for several types of probes and rotor geometries.

摘要

固态核磁共振(SSNMR)是一种用于研究生物分子和材料结构与动力学的极具通用性且广泛适用的方法。对于刚进入SSNMR领域的科学家而言,在工作流程中为数据采集准备样品所需的诸多日常活动可能会成为采用该技术的重大障碍。这些步骤包括将样品转移至转子中、标记反射面以进行高灵敏度转速计信号检测、将转子插入魔角旋转(MAS)定子中、实现稳定旋转,以及取出和存放转子以确保数据采集条件的可重复性。即使是经验丰富的光谱学家在这些操作中也偶尔会遇到问题,并且成功采集数据出现延迟的累积概率高到足以频繁打乱仪器使用计划,尤其是在为不同用户群体服务的大型设施环境中。当使用直径小于约4毫米的转子时,这些问题会被放大。因此,为提高SSNMR样品制备工作流程的可靠性和稳健性,我们在此描述了一套用于转子装填、卸载、转速计标记、取出和存储的工具。立体光刻3D打印被用作一种经济高效且便捷的方法,用于制作和制造适用于多种类型探头和转子几何形状的全系列设计。

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