600 MHz NMR spectrometer

CeMSA@HHU(分子和结构分析中心@Heinrich-Heine-University)是一个中央分析中心，由两个部门组成。核磁共振波谱部拥有两台光谱仪(300 MHz和600 MHz)，为生物、化学和制药领域的25个小组提供测量服务。大约200名科学家(博士生、博士后等)每年使用核磁共振部门。目前，核磁共振部门只能有限地处理样本量。到目前为止，没有不可接受的等待时间，但由于能力有限，我们不得不拒绝用户提出的耗时的特殊测量请求。这主要涉及(I)多个含氟体系的15N(15N-{1H}，15N-HSQC，15N-HMBC)和(Ii)13C-{1H}-核磁共振的一维和二维测量。(I)含氮杂环在卫生与公众服务部的不同研究小组中发挥主要作用。通常，特别是2D方法(15N-HSQC，15NHMBC)对于证明预期的结构和阐明意外反应产物或从自然中分离出来的物质的结构是必不可少的。这种测量只有在特殊情况下才有可能，因为除了常规操作外，15N光谱的测量时间很长。因此，采购一台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，我们选择了带有氮气(77K)冷却线圈和前置放大器的现代600 MHz分光计。氮气冷却的使用大大降低了电子噪声，与现代传统探头相比，15N-{1H}的测量时间缩短了1/4，15N-HSQC、15NHMBC的测量时间缩短了1/2。因此，为了我们的许多用户的利益，在未来应该可以测量迫切需要的15N核磁共振谱。(2)我们的一些用户经常使用全氟烷基侧链。这导致了~(13)C-{1H}-核磁共振谱的复杂分裂，因此信号常常消失在噪声中。与现代探头相比，现代光谱仪与氮气冷却探头相结合，将13C的测量时间减少到约1/9。此外，我们正计划采购一种可以同时解耦1H和19F的探头。这将为特别复杂的系统提供一种特殊的解决方案。近年来，我们收到了几个关于奇异核的请求，这些请求超出了杜塞尔多夫现有分光计的测量范围。因此，我们计划采购一个大测量范围(31P到103Rh)的探头。作为另一种选择，我们正计划采购一台HRMS探头，用于研究粘性系统。这一点对于GRK 2482 ModISC尤其重要，在其中，聚集诱导的荧光发挥了主要作用。

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.