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observe 31P-15N/1H) will remain in use, we intend to replace of the 14-year-old spectrometer console (technically outdated; with serious spare parts problems; “end of service” announced already for the end of 2017) including the automatic sample changer and the defective cryo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.

“化学研究所中央核磁共振实验室”是布伦瑞克工业大学无机与分析化学研究所和有机化学研究所的联合设施。它在整个大学提供核磁共振波谱服务和专业知识。对大学化学、生物、制药和材料科学研究所获得或制造的天然物质以及有机、无机、有机金属和高分子合成产品进行检查。到目前为止，这里可用的五台 NMR 波谱仪中最灵敏的是带有 He 冷却反三重共振低温探针（1H/13C/15N；仅间接 15N）的 600 MHz 设备。由于大约 1 年后探头及其外围设备完全损坏。 110,000 个运行小时（2006-2019 年）后，光谱仪不再满足其主要用途，即以最大检测灵敏度检查样品。因此，光谱采集需要之前测量时间的倍数，或者对于极少量的物质来说是无用的。这会导致严重的容量问题，也会间接影响其他光谱仪，尤其是 500 MHz 设备。为了恢复 600 MHz 光谱仪的性能并使其现代化，需要部分更换该设备。虽然磁铁和一个探头（不是冷冻头：宽带观察 31P-15N/1H）将继续使用，但我们打算更换使用了 14 年的光谱仪控制台（技术上已经过时；存在严重的备件问题；已宣布于 2017 年底“停止服务”），包括自动进样器和有缺陷的冷冻设备。后者包括低温冷却装置、氦压缩机、氦冷却逆三共振低温探头以及合适的温度控制选项。需要新组件来至少恢复原始设备的全部性能。因此，与以前一样，重点是最大 1H 灵敏度，同时尽可能最高的 13C 和 15N 灵敏度，以补充其他光谱仪。鉴于工作组的多样性，应消除先前设备的弱点（例如19F不可观测；15N不可直接观测；低温探头温度范围太小，0-80°C）。因此我们申请以下组件：具有三通道的600 MHz光谱仪控制台，带有He冷却反三重共振低温探头的低温设备 （1H&19F/13C/15N；15N 也可直接观察）以获得最大可能的温度范围，自动换样器以实现设备的最佳使用。由此产生的改进将是：恢复最大灵敏度（极其重要）、最先进的 NMR 实验的可行性（例如“NOAH”）；直接观测19F和15N；可达温度范围-40至+150°C。