Clinical-Scale Production of Nearly Pure (>98.5%) Parahydrogen and Quantification by Benchtop NMR Spectroscopy.

Clinical-Scale Production of Nearly Pure (>98.5%) Parahydrogen and Quantification by Benchtop NMR Spectroscopy.
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DOI:
10.1021/acs.analchem.0c05129
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发表时间:
2021-02-23
影响因子:
7.4
通讯作者:
Chekmenev EY
Chekmenev EY
中科院分区:
化学1区
文献类型:
--
作者:
Nantogma S;Joalland B;Wilkens K;Chekmenev EY

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由于仲氢广泛的化学、物理和生物医学应用,需要以稳健和有效的方式开发高度富集的仲氢。在此,我们提出了一种仲氢富集设备,其大大改进了先前的发生器,具有将仲氢富集到>98.5%的能力和高达4标准升/分钟(SLM)的生产率,并具有实时定量的附加优势。我们的发生器采用脉冲喷射系统,该系统具有3/16英寸外径的铜螺旋管,其中填充有氧化铁催化剂。该管道与定制的铜附件配合,以提供与冷头的有效热耦合。该设备允许在高达34 atm的高压下稳定运行。通过将发生器的p-H2出口直接耦合到1.4 T NMR光谱仪,使用常规5 mm NMR管,该NMR管在约8 atm压力下连续再填充有退出的仲氢气体,可以通过台式NMR光谱进行实时定量。使用高氢气压力提供了两个关键的NMR信号检测好处:增加浓度和线变窄。我们的工作提出了一个全面的描述,方便和强大的仲氢的生产,分配和定量系统,特别是仲氢为基础的超极化NMR研究的装置。
Due to the extensive chemical, physical and biomedical applications of parahydrogen, the need exists for the development of highly enriched parahydrogen in a robust and efficient manner. Herein, we present a parahydrogen enrichment equipment which substantially improves upon previous generators with its ability to enrich parahydrogen to >98.5% and a production rate of up to 4 standard liters per minute (SLM) with the added advantage of real-time quantification. Our generator employs a pulsed injection system with a 3/16-inch outside diameter copper spiral tubing filled with iron-oxide catalyst. This tubing it mated to custom-made copper attachment to provide efficient thermal coupling to the cold head. This device allows for robust operation at high pressures up to 34 atm. Real-time quantification by benchtop NMR spectroscopy is made possible by the direct coupling of the p-H2 outlet from the generator to a 1.4 T NMR spectrometer using regular 5-mm NMR tube that is continuously refilled with exiting parahydrogen gas at ~8 atm pressure. The use of high hydrogen gas pressure offers two critical NMR signal detection benefits: increased concentration and line narrowing. Our work presents a comprehensive description of the apparatus for convenient and robust parahydrogen production, distribution and quantification system especially for parahydrogen-based hyperpolarization NMR research.
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