CPMAS HFX WB triple resonance probe 0.7 mm
CPMAS HFX WB triple resonance probe 0.7 mm
批准号:
465296153
负责人:
金额:
$0.0万
依托单位:
依托单位国家:
德国
项目类别:
Major Research Instrumentation
财政年份:
2021
资助国家:
德国
项目状态:
未结题
起止时间:
2020-12-31 至 --
中文摘要
拜罗伊特大学计划为北巴伐利亚核磁共振中心的600 MHz WB固态核磁共振仪(Avance III HD,Bruker)购买一个转子直径为0.7 mm的CPMAS HFX三重共振探头。采购和有效科学使用的责任由尤尔根·森克(无机化学III)工作组负责。此外,Seema Agarwal(高分子化学II)和Roland Marschall(物理化学III)的研究小组表示有兴趣将该探针用于他们的科学研究。通过购买0.7 mm的MAS探针,我们的目标是实现主要基于质子的高分辨率固态核磁共振光谱,用于表征无机、有机、杂化和聚合物材料。要做到这一点,需要一个能够足够快地旋转的探测器,以有效地平均非常强的同核1H-1H偶极耦合。最近的结果表明,这些条件在超过100千赫的旋转速度后才能满足。由于0.7 mm的MAS探头允许旋转频率高达110 kHz,因此满足了必要的要求。在这些条件下,1H MAS核磁共振谱具有极好的灵敏度,并允许探测同核空间接近到大约1 nm。1H MAS核磁共振实验接近于类液体条件下的核磁共振观察值的时间依赖关系,因此能够在固体中与间接检测方案一起工作。除了能够记录高分辨率的1H MAS核磁共振谱,不受同核偶极耦合的影响,以及更容易获得1H-1HZQ和DQ重新耦合实验外,间接检测为广泛的异核相关实验提供了一种有前途的替代方案。要成功地处理所提出的研究课题,需要高分辨率的质子HETCOR谱,X核包括6/7Li,13C,14N,17O,19F,23Na,27Al,29Si,69Ga,91Zr,113Cd和119Sn。其中一些异核,如14N和17O,很难直接激发。此外,对于计划中的1H和19F之间的关联实验,还需要一个三重共振装置,可以同时激发1H,19F和另一个X核。
英文摘要
The University of Bayreuth plans the purchase of a CPMAS HFX triple resonance probe with a rotor diameter of 0.7 mm for the 600 MHz WB solid-state NMR spectrometer (Avance III HD, Bruker) of the North Bavarian NMR centre. The responsibility for the procurement and an efficient scientific use is located in the work group of Juergen Senker (Inorganic Chemistry III). Additionally, the research groups of Seema Agarwal (Macromolecular Chemistry II) and Roland Marschall (Physical Chemistry III) expressed their interest in using the probe for their scientific research.With the purchase of the 0.7 mm MAS probe, we aim at implementing high-resolution solid-state NMR spectroscopy mainly based on protons for characterising of inorganic, organic, hybrid and polymer materials. Doing so, requires a probe able to spin fast enough to even average very strong homonuclear 1H-1H dipolar couplings effectively. Recent results suggest that these conditions become to be fulfilled beyond spinning speeds of 100 kHz. As the 0.7 mm MAS probe allows for rotation frequencies up to 110 kHz, it meets the necessary requirements. Under these conditions 1H MAS NMR spectroscopy features excellent sensitivities and allows for probing homonuclear spatial proximities up to roughly 1 nm. 1H MAS NMR experiments approach liquid-like conditions for the time dependence of NMR observables and thus enables to work with indirect detections schemes in the solid state. Besides of being able to record high-resolution 1H MAS NMR spectra, free of influences of the homonuclear dipolar coupling, and to acquire 1H-1H ZQ and DQ recoupling experiments more easily, indirect detection provides a promising alternative, for a broad range of heteronuclear correlation experiments. A successful handling of the proposed research topics, requires high-resolution proton HETCOR spectra with X nuclei like 6/7Li, 13C, 14N, 17O, 19F, 23Na, 27Al, 29Si, 69Ga, 91Zr, 113Cd and 119Sn. Some of these heteronuclei like 14N and 17O are difficult to excite directly. For the planned correlation experiments between 1H and 19F, additionally, a triple resonance setup with the possibility of simultaneously excite 1H, 19F and one further X nucleus is required.
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