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observe 31P-15N/1H) will remain in use, we intend to replace of the 14-year-old spectrometer console (technically outdated; with serious spare parts problems; “end of service” announced already for the end of 2017) including the automatic sample changer and the defective cryo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，它为整个大学提供核磁共振光谱服务和专业知识。迄今为止，该大学的化学、生物、制药和材料科学研究所获得或生产的有机、无机、有机金属和高分子合成产品。这里提供的五种 NMR 波谱仪中最灵敏的是带有 He 冷却逆三重共振冷冻探头的 600 MHz 设备（1H/13C/15N；仅间接使用 15N）。 110,000 运行小时（2006-2019），光谱仪不再满足其主要目的，即以最大检测灵敏度检查样品。结果，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，这也会间接导致其他光谱仪的严重容量问题，特别是在 500 MHz 设备上。 600 MHz 光谱仪，需要部分更换设备，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，但我们打算更换该设备。使用了 14 年的光谱仪控制台（技术过时；备件存在严重问题；已于 2017 年底宣布“停止服务”），包括自动样品更换器和有缺陷的低温设备（后者包括低温冷却装置、氦压缩机）。 ，He 冷却逆三共振低温探头，具有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，以前设备的弱点（例如 19F 不可观测；15N 不可直接观测；低温的温度范围）。探头太小（0-80°C）应被淘汰。因此，我们申请以下组件：具有三个频道的 600 MHz 光谱仪控制台、具有He 冷却逆三重共振低温探头（1H&19F/13C/15N；15N 也可直接观察）可实现最大可能的温度范围，自动进样器可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”）；可直接观察 19F 和 15N 的温度范围； -40 至 +150°C。