400 MHz NMR console with solid-state probes

我们正在申请的一揽子计划包括一个新的600兆赫核磁共振仪器，带有一个低温氮气冷却探头以及一个备用探头，一个新的400兆赫控制台，带有两个固态探头，以及一个备用探头和一个新的400兆赫控制台，带有宽带探头。这种全面的现代化是必要的，因为乌尔姆大学化学系的核磁共振控制台和磁体都有15-27年的历史，而且最近几位教员的招聘和合作研究计划需要改变核磁共振基础设施。我们设想，带有低温探头的600 MHz仪器将用于大多数13C核磁共振测量、二维核磁共振测量以及稀薄样品和复杂混合物的1H核磁共振测量。在对低温探头进行维护、清洁或维修时，一个高价值的室温探头应作为磁体上的备份。两个400 MHz控制台中的一个将能够执行固态核磁共振波谱，并因此配备三个探头：第一，新的魔角旋转(MAS)探头，该探头针对高分辨率1H和13C核磁共振“半固体”(主要用户：有机和高分子研究小组)进行了优化。第二，宽带交叉极化(CP)-MAS探测器，该探测器针对金属氧化物纳米颗粒(主要用户：无机和电化学研究小组)等“真实固体”的固态核磁共振表征进行了优化。第三，常规的宽带探头还应允许在溶液中进行核磁共振测量，以便优化核磁共振设施的总容量。具有宽带探头的第二个400 MHz控制台将允许以高灵敏度进行全自动1H和X核(例如11B、19F、31P)核磁共振测量。在可行的温度范围内，所有三台仪器都应适合进行变温(VT)核磁共振测量。所有仪器应配备自动取样器和自动调谐装置，以便在夜间和周末进行多次测量。

We are applying for a package consisting of one new 600 MHz NMR instrument with a cryogenic, nitrogen-cooled probe as well as a backup probe, a new 400 MHz console with two solid state probes as well as a backup probe and a new 400 MHz console with a broadband probe. This comprehensive modernisation is necessary, because the NMR consoles and magnets at the Chemistry Department at the University of Ulm are all 15-27 years old and because several recent faculty hires and collaborative research initiatives require changes in the NMR infrastructure.We envisage that the 600 MHz instrument with the cryogenic probe will be used for most 13C NMR measurements, for two-dimensional NMR measurements and for 1H NMR measurements of dilute samples and complex mixtures. A high-value room-temperature probe shall serve as a backup on this magnet, while the cryogenic probe is being maintained, cleaned or repaired. One of the two 400 MHz consoles shall be capable of performing solid state NMR spectroscopy and hence be equipped with three probes: first, a new magic angle spinning (MAS) probe that is optimized for high-resolution 1H and 13C NMR spectroscopy of “semi-solids“ (main users: organic and macromolecular research groups). Second, a broadband cross-polarization (CP)-MAS probe that is optimized for the solid-state NMR characterization of “real solids” such as metal oxide nanoparticles (main users: inorganic and electrochemical research groups). Third, a conventional, broadband probe shall also allow NMR measurements in solution, so that the total capacity of the NMR facility can be optimized. The second 400 MHz console with a broadband probe will allow fully automated 1H and X nuclei (e.g. 11B, 19F, 31P) NMR measurements at high sensitivity.Within the feasible temperature ranges, all three instruments shall be suitable for carrying out variable temperature (VT) NMR measurements. All instruments shall be equipped with autosamplers and autotuning units so that several measurements can be carried out during nights and weekends.