Upgrade 600-MHz-NMR Spectrometer

升级 600 MHz 核磁共振波谱仪

• 批准号: 456890320
• 金额: --
• 依托单位: Technische Universität Braunschweig
• 依托单位国家: 德国
• 项目类别: Major Research Instrumentation
• 财政年份: 2020
• 资助国家: 德国
• 起止时间: 2019-12-31 至 无数据
• 项目状态: 未结题
• 来源: https://gepris.dfg.de/gepris/projekt/456890320?language=en
• 关键词: Upgrade; 600; MHz; NMR; Spectrometer

The "Central NMR Laboratory of the Chemical Institutes" is a joint facility of the Institute of Inorganic and Analytical Chemistry and the Institute of Organic Chemistry at the TU Braunschweig. It provides NMR-spectroscopic services and know-how throughout the university. Natural substances as well as organic, inorganic, organometallic and macromolecular synthesis products are examined, which are obtained or manufactured in the chemical, biological, pharmaceutical and materials science institutes of the university. So far, the most sensitive of the five NMR spectrometers available here has been a 600 MHz device with a He-cooled inverse triple resonance cryo probe (1H/13C/15N; 15N only indirectly). Due to total damage to the probehead and its peripheral devices after approx. 110,000 operating hours (2006-2019), the spectrometer no longer fulfills its main purpose, namely the examination of samples with maximum detection sensitivity. As the consequence, spectra acquisitions require a multiple of the previous measurement time or are useless for very small amounts of substance. This causes severe capacity problems, indirectly also on the other spectrometers, especially on the 500 MHz device. To restore the performance and modernize the 600 MHz spectrometer, a partial replacement of the device is necessary. While the magnet and one probehead (not a cryo head: broadband observe 31P-15N/1H) will remain in use, we intend to replace of the 14-year-old spectrometer console (technically outdated; with serious spare parts problems; “end of service” announced already for the end of 2017) including the automatic sample changer and the defective cryo equipment. The latter include cryo cooling unit, He compressor, He-cooled inverse triple resonance cryo probehead with a suitable temperature control option.New components are required that restore at least the full performance of the original device. Therefore, as before, the focus is on maximum 1H sensitivity and, at the same time, the highest possible 13C and 15N sensitivity in order to complement the other spectrometers. In view of the diversity of the working groups, weaknesses of the previous equipment (e.g. 19F not observable; 15N not directly observable; temperature range of the cryo probehead too small, 0-80 °C) should be eliminated.We therefore apply for the following components: 600 MHz spectrometer console with three frequency channels, cryo equipment with He-cooled inverse triple resonance cryo probe head (1H&19F/13C/15N; 15N also directly observable) for the largest possible temperature range, automatic sample changer for optimal use of the device .Resulting improvements will be: restoration of maximum sensitivity (extremely important), feasibility of state-of-the-art NMR experiments (e.g. "NOAH"); direct observation of 19F and 15N; accessible temperature range -40 to +150 ° C.

“化学研究所的中央NMR实验室”是无机和分析化学研究所的联合设施，以及Tu Braunschweig的有机化学研究所。它提供NMR-SpectRoscotic服务和整个大学的专业知识。研究了自然物质以及有机，无机，有机和大分子合成产品，这些产品是在大学的化学，生物，药物和材料科学研究院中获得或制造的。到目前为止，这里可用的五个NMR光谱仪中最敏感的是一种600 MHz设备，具有他冷却的逆三重共振冷冻探针（1H/13C/15N；仅间接使用15N）。由于对探针的总损坏及其外周装置后近似后。 110,000工作时间（2006-2019），光谱仪不再实现其主要目的，即检查具有最大检测灵敏度的样品。结果，光谱采集需要以前的测量时间的倍数，或者对于少量物质而言是无用的。这会导致严重的容量问题，这也间接地在其他光谱仪上，尤其是在500 MHz设备上。为了恢复性能并使600 MHz光谱仪现代化，需要部分更换设备。虽然将继续使用磁铁和一个探针（不是冷冻头：宽带观察31p-15n/1h），但我们打算替换14岁的光谱仪控制台（技术上过时；存在严重的备件问题；在2017年底已经宣布的“终结”服务），包括自动样品变形器和缺陷的冷冻冷冻机设备。后者包括冷冻冷却单元，HE压缩机，他冷却具有适当温度控制选项的逆三重共振探针。新的组件必须至少恢复原始设备的全部性能。因此，像以前一样，焦点是最大1H敏感性，同时，为了补充其他光谱仪，最高可能的13C和15N敏感性。 In view of the diversity of the working groups, weaknesses of the previous equipment (e.g. 19F not observable; 15N not directly observable; temperature range of the cryo probehead too small, 0-80 °C) should be eliminated.We therefore apply for the following components: 600 MHz spectrometer console with three frequency channels, cryo equipment with He-cooled inverse triple resonance cryo probe head （1H＆19F/13C/15N;也可以直接观察到）对于最大的温度范围，自动样品更换器以最佳使用设备。恢复改进将是：恢复最大灵敏度（极为重要），最先进的NMR实验的可行性（例如，“ Noah”）;直接观察19F和15N；可及温度范围-40至+150°C。