Jeong Keunhong, Min Sein, Chae Heelim, Namgoong Sung Keon
Department of Chemistry, Korea Military Academy, Seoul, 01805, South Korea.
Department of Chemistry, Seoul Women's University, Seoul, 01797, South Korea.
Magn Reson Chem. 2018 Nov;56(11):1089-1093. doi: 10.1002/mrc.4756. Epub 2018 Jun 19.
Parahydrogen is a potentially significant source of hyperpolarization. However, a heat exchanger at an ultralow temperature, which is normally sustained wastefully using liquid nitrogen, is essential for the generation of hyperpolarized parahydrogen. In order to cut down on the use of liquid nitrogen, we employed a cryogenic storage dewar as the key component of our home-built parahydrogen generator, which lasted over 20 days with a single filling. Small concentrations of an unsaturated compound in a mixture were identified by hydrogenation in a principle-based experiment involving the use of hyperpolarization and phase difference. Less than 1 μl of styrene in 1 ml of chloroform was identified in a single scan with a 43 MHz benchtop nuclear magnetic resonance (NMR) spectrometer following hydrogenation with 50% parahydrogen. This method can potentially undergo a significant development through the use of high-field NMR techniques, higher parahydrogen concentrations, and increased scan times for data collection, among others. Because hydrogenation with parahydrogen induces a phase reversal during attachment to unsaturated CC bonds, it may be possible to detect many other unsaturated bonds in organic molecules. All in all, this study not only broadens the research on parahydrogen-based unsaturated-bond detection, but also facilitates the use of hyperpolarization by a broader range of researchers through the introduction of a long-lasting home-built parahydrogen generator.
仲氢是超极化的一个潜在重要来源。然而,通常需要大量浪费液氮来维持的超低温热交换器,对于产生超极化仲氢至关重要。为了减少液氮的使用,我们采用了低温储存杜瓦瓶作为自制仲氢发生器的关键部件,一次充装可持续使用20多天。在一个基于原理的实验中,通过使用超极化和相位差的氢化反应,鉴定了混合物中低浓度的不饱和化合物。在用50%仲氢进行氢化反应后,使用43兆赫的台式核磁共振(NMR)光谱仪在单次扫描中鉴定出1毫升氯仿中少于1微升的苯乙烯。通过使用高场NMR技术、更高的仲氢浓度以及增加数据收集的扫描时间等,该方法可能会有显著发展。由于用仲氢进行氢化反应在与不饱和CC键结合时会引起相位反转,因此有可能检测有机分子中的许多其他不饱和键。总而言之,本研究不仅拓宽了基于仲氢的不饱和键检测的研究,还通过引入一种持久的自制仲氢发生器,促进了更广泛的研究人员对超极化的使用。