600 MHz NMR spectrometer

600MHz核磁共振波谱仪

• 批准号: 520306642
• 金额: --
• 依托单位: Heinrich-Heine-Universität Düsseldorf
• 依托单位国家: 德国
• 项目类别: Major Research Instrumentation
• 财政年份: 2023
• 资助国家: 德国
• 起止时间: 2022-12-31 至 无数据
• 项目状态: 未结题
• 来源: https://gepris.dfg.de/gepris/projekt/520306642?language=en
• 关键词: 600; MHz; NMR; spectrometer; 600; MHz; NMR; spectrometer

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.

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。 NMR光谱部门拥有两个光谱仪（300 MHz和600 MHz），并为生物学，化学和药房的25个组提供测量服务。每年约有200名科学家（博士生，博士学位，博士学位，...）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，还没有不可接受的等待时间，但是由于能力有限，我们必须拒绝用户要求进行耗时的特殊测量的请求。这主要涉及（i）1D和2D测量值（15n- {1H}，15n-HSQC，15N-HMBC）和（ii）13C- {1H} -NMR多氟化系统的NMR。 （i）含氮的杂环在HHU的各个研究组中都起着重要作用。通常，尤其是2D方法（15N-HSQC，15NHMBC）对于证明预期结构并阐明与自然隔离的意外反应产物或物质的结构至关重要。此类测量只能在特殊情况下，由于经常操作外，由于15N光谱的长期测量时间。因此，具有高信噪比的现代光谱仪的采购对于提供良好的服务至关重要。因此，我们的选择落在现代的600 MHz光谱仪上，氮（77 K）冷却的线圈和前置放大器。与现代传统的探针头相比，使用氮气冷却可显着降低15n- {1H}的测量时间，并缩短15n- {1H}的测量时间，至15n-HSQC，15NHMBC至当时的1/2。这是为了使许多用户的利益，将来应该有可能测量急需的15N NMR光谱。 （ii）我们的许多用户定期使用全氟的酒精侧链。这会导致复杂的13C- {1H} -NMR光谱中的分裂，因此信号经常在噪声中消失。与现代探针头相比，现代光谱仪与氮气冷却探针头结合使用，将13C的测量时间降低到约1/9。此外，我们计划采购一个可以简单地将1H和19F解次的探针头。然后，这将为特别复杂的系统提供特殊的解决方案。近年来，我们已经提出了几种异国核的要求，这些要求超出了杜塞尔多夫可用的光谱仪的测量范围。因此，我们计划采购具有较大尺寸范围（31p至103RH）的探针头。作为另一个选择，我们计划采购HRMS探测头，以调查粘性系统。对于GRK 2482 MODISC，这一点尤其重要，其中，汇总诱导的荧光起着主要作用。