Nuclear magnetic resonance spectrometer for measurements at elevated pressures

用于高压测量的核磁共振波谱仪

• 批准号: 516655476
• 金额: --
• 依托单位: Ludwig-Maximilians-Universität München (LMU)
• 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/516655476?language=en
• 关键词: Nuclear; magnetic; resonance; spectrometer; measurements

Pressure is a basic physical parameter that can generally be used i) to modulate kinetics and thermodynamics of chemical processes and ii) to elucidate reaction mechanisms down to the molecular level of bond-making and bond-braking. Our group has a long-term research interest and expertise in applying high pressures (up to 2 kbar) for both purposes, in particularly in combination with NMR technique for investigations of reactions in solutions that are of biological, catalytic, environmental or energy-conversion relevance. The herewith applied-for NMR spectrometer for measurements at elevated pressures should enable our versatile mechanistic research under diverse conditions that in addition to high pressures include: i) operation at variable and low temperatures (153 K to 373 K), ii) measurements in aqueous and organic solvents, iii) oxygen and/or light sensitive samples, iv) biological/medical samples, v) one- (liquid) or two-phase (liquid-gas) systems, etc. The application of such a rather rare set-up is beyond standard use of NMR technique and will predominantly involve mechanistic pressure-dependent studies to determine activation and/or reaction volumes, for “visualization” of transition states, characterization of reaction intermediates, dynamic processes and equilibria in solutions (e.g. water exchange at metal centers, coordination-, spin-, host-guest-equilibria). For realisation of these quite challenging research tasks the requested NMR spectrometer should provide high resolution and sensitivity for measurement under high pressures, for which a 500 MHz magnet would be the best choice. Since we investigate a broad range of (in)organic molecules and (bio)macromolecules, a 5 mm multinuclear broad band double-resonance probe with Z-gradient, which in addition to 1H and 19F displays high sensitivity for the nuclei 13C, 17O, 31P and 57Fe would be optimal. The most essential feature of the applied-for instrumentation, however, is its compatibility with two different high-pressure setups i) one commercially available (for aqueous samples or two-phase (gas-liquid) experiments) and (ii) another that will be a home-made high-pressure NMR probe (based on the system already used by us for more sophisticated measurements with light/oxygen sensitive samples, various organic solvents and at low temperatures). Such a high-pressure NMR instrument, with unique performances that enable mechanistic studies of multidisciplinary relevance under very diverse conditions, does not exist at LMU, in the area of Munich and in this combination, to best of our knowledge, not even in Germany. Such a device is indispensable for our ongoing and planned projects, and also has the potential to contribute to the international research collaborations in the fields of bioinorganic chemistry, biological chemistry, catalysis and chemical energy conversion.

压力是一种通常可以使用的基本物理参数i）调节化学过程的动力学和热力学，ii）阐明了反应机制，直至建立结合和键制的分子水平。我们的小组具有长期的研究兴趣和专业知识，可用于将高压（最多2 kbar）用于这两个目的，特别是与NMR技术结合使用，以研究具有生物学，催化，环境或能源转化相关性的溶液中的反应。在升高压力下进行测量的NMR光谱仪的本文应使我们在潜水条件下的多功能机械研究，除了高压外，还包括：i）在可变和低温下（153 K至373 k）（153 K至373 K），II）在水溶液和有机溶液中的测量值，III和/或光剂，或光剂量 - 或光敏感性，或/或光敏感的样品，IIV），IIV），IIV），IIV，IIV），IIV），IIV），IIV），IIV），IIV（IIV）IIV（IIV），IIV）。 two-phase (liquid-gas) systems, etc. The application of such a rather rare set-up is beyond standard use of NMR technique and will predominantly involve mechanical pressure-dependent studies to determine activation and/or reaction volumes, for “visualization” of transition states, characterization of reaction intermediates, dynamic processes and equilibria in solutions (e.g. water exchange at metal centers, coordination-, spin-,寄主 - 阵线平衡）。为了实现这些非常具有挑战性的研究任务，请求的NMR光谱仪应在高压下为测量值提供高分辨率和敏感性，为此，500 MHz磁铁将是最佳选择。由于我们研究了一系列有机分子和（BIO）大分子，因此具有5 mm的多核宽带双带双共声探针，具有Z级别，除1H和19F外，还显示出对核13C，17o，17o，31p和57fe的高灵敏度，这是最佳的。但是，应用仪器的最重要特征是它与两种不同的高压设置i）i）一个商业上可用（用于水性样品或两相或两相（气体）实验）和（ii）另一个将是本自制的高压NMR探针（基于US的较高的型号，都可以使用更为复杂的型号，该系统是由usife symentive symentions systame使用的。温度）。这种高压NMR仪器具有独特的性能，可以在非常多样化的条件下对多学科相关性进行机械研究，在LMU，慕尼黑和这种组合中，不存在于我们所知，甚至在德国，甚至不存在。这种设备对于我们正在进行的和计划的项目来说是必不可少的，并且也有可能为生物无机化学，生物化学，催化和化学能量转化领域的国际研究合作做出贡献。