Upgrade 600-MHz-NMR Spectrometer

"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和分析化学研究所与有机化学研究所的联合设施。它在整个大学提供NMR光谱服务和专业知识。天然物质以及有机，无机，有机金属和大分子合成产品进行检查，这些产品是在大学的化学，生物，制药和材料科学研究所获得或制造的。到目前为止，这里可用的五种NMR光谱仪中最灵敏的是一种600 MHz的设备，带有He冷却的反向三重共振冷冻探针（1H/13 C/15 N; 15 N仅间接）。由于探头及其外围设备在大约10分钟后完全损坏。110，000工作小时（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。因此，光谱采集需要先前测量时间的倍数，或者对于非常少量的物质是无用的。这也间接地在其他光谱仪上，特别是在500 MHz设备上，引起严重的容量问题。为了恢复600 MHz频谱仪的性能并使其现代化，需要部分更换该设备。虽然磁体和一个探头（不是低温探头：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; 2017年底已经宣布“服务终止”），包括自动换样器和有缺陷的低温设备。后者包括低温冷却单元、He压缩机、He冷却反向三重共振低温探头以及适当的温度控制选项。需要新的组件，以恢复至少原始设备的全部性能。因此，与以前一样，重点是最大的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，（例如：19F不可观测; 15N不可直接观测;低温探头的温度范围太小，0 - 80 ° C）。因此，我们适用于以下组件：600 MHz光谱仪控制台，带三个频率通道，低温设备，带氦冷反向三重共振低温探头（1H&19F/13C/15N; 15N也可直接观察到），用于最大可能的温度范围，自动换样器用于最佳使用设备。（非常重要），最先进的NMR实验的可行性（例如"NOAH"）;直接观察19F和15N;可达温度范围-40至+150 °C。

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observe 31P-15N/1H) will remain in use, we intend to replace of the 14-year-old spectrometer console (technically outdated; with serious spare parts problems; “end of service” announced already for the end of 2017) including the automatic sample changer and the defective cryo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