600 MHz NMR spectrometer

CeMSA@HHU（分子和结构分析中心@ Heinrich-Heine-Universität）是一个中央分析中心，由两个部门组成。核磁共振光谱学部门拥有两台光谱仪（300 MHz和600 MHz），并为生物，化学和药学的25个团体提供测量服务。约200名科学家（博士生、博士后等）每年使用NMR部门。目前，NMR部门只能在有限的范围内处理样品量。到目前为止，没有不可接受的等待时间，但由于容量有限，我们不得不拒绝用户要求进行耗时的特殊测量。这主要涉及（i）15 N（15 N-{1H}、15 N-HSQC、15 N-HMBC）的1D和2D测量和（ii）多个氟化体系的13 C-{1H}-NMR。(i)含氮杂环在HHU的各个研究小组中发挥着重要作用。通常，特别是2D方法（15 N-HSQC，15 NHMBC）对于证明预期的结构和阐明意外反应产物或从自然界分离的物质的结构是必不可少的。由于除了常规操作外，15 N光谱的测量时间较长，因此仅在例外情况下才可能进行此类测量。因此，采购具有高信噪比的现代光谱仪对于提供良好的服务至关重要。因此，我们的选择落在一个现代化的600 MHz的光谱仪与氮（77 K）冷却线圈和前置放大器。氮气冷却的使用显著降低了电子噪声，并将15 N-{1H}的测量时间缩短到现代传统探头的1/4，15 N-HSQC，15 NHMBC缩短到1/2。因此，它应该是可能的，在未来测量迫切需要的15 N NMR光谱，在我们的许多用户的利益。(ii)我们的许多用户经常使用全氟烷基侧链。这导致13 C-{1H}-NMR谱中的复杂分裂，使得信号常常消失在噪声中。与现代探头相比，现代光谱仪与氮冷却探头的组合将13 C的测量时间减少到约1/9。此外，我们正计划采购一种探头，可以同时解耦1H和19 F。这将为特别复杂的系统提供特殊的解决方案。近年来，我们收到了几个关于杜塞尔多夫光谱仪测量范围之外的奇异核的请求。因此，我们计划采购具有大测量范围（31 P至103 Rh）的探头。作为进一步的选择，我们计划采购一个HRMS探头，用于粘性系统的研究。这对于GRK 2482 ModISC尤其重要，其中聚集诱导荧光起主要作用。

CeMSA@HHU (Center for Molecular and Structural Analytics @ Heinrich-Heine-Universität) is a central analytics center and consists of two departments. The department for NMR spectroscopy owns two spectrometers (300 MHz and 600 MHz) and provides measurement services for 25 groups in biology, chemistry and pharmacy. About 200 scientists (PhD students, postdocs, ...) use the NMR department per year. Currently, the NMR department can only handle the sample volume to a limited extent. So far there are no unacceptable waiting times, but due to the limited capacity we have to reject requests from users for time-consuming special measurements. This concerns mainly (i) 1D and 2D measurements of 15N (15N-{1H}, 15N-HSQC, 15N-HMBC) and (ii) 13C-{1H}-NMR of multiple fluorinated systems. (i) Nitrogen-containing heterocycles play a major role in various research groups at HHU. Often, especially the 2D methods (15N-HSQC, 15NHMBC) are essential to prove the expected structures and to elucidate the structure of unexpected reaction products or substances isolated from nature. Such measurements are only possible in exceptional cases due to long measurement times for 15N spectra in addition to routine operations. Therefore, the procurement of a modern spectrometer with a high signal-to-noise ratio is essential to provide a good service. Our choice therefore fell on a modern 600 MHz spectrometer with nitrogen (77 K) cooled coils and preamplifiers. The use of nitrogen cooling significantly reduces electronic noise and shortens the measurement time for 15N-{1H} compared to modern conventional probe heads to 1/4 of the time, for 15N-HSQC, 15NHMBC to 1/2 of the time. Thus, it should be possible in the future to measure the urgently needed 15N NMR spectra in the interest of many of our users. (ii) A number of our users regularly work with perfluorinated alkyl side chains. This leads to complex splitting in 13C-{1H}-NMR spectra, so that signals often disappear in the noise. A modern spectrometer in combination with a nitrogen cooled probe head reduces the measurement time for 13C to about 1/9 compared to modern probe heads. In addition, we are planning to procure a probe head that can decouple 1H and 19F simultaneously. This will then provide a special solution for particularly complex systems. In recent years, we have had several requests for exotic nuclei that are outside the measuring range of the spectrometers available in Düsseldorf. Therefore, we are planning to procure a probe head with a large measuring range (31P to 103Rh). As a further option, we are planning to procure an HRMS probe head for the investigation of viscous systems. This is particularly important with regard to the GRK 2482 ModISC, in which, among other things, aggregation-induced fluorescence plays a major role.