An inexpensive apparatus for up to 97% continuous-flow parahydrogen enrichment using liquid helium

[Display omitted] •Low cost home-built cryostat for parahydrogen enrichment at 30 K.•Cryostat is immersed in a liquid helium storage dewar.•Parahydrogen enrichment to 97% at 300 mL/min and 4.5 bar.•Approximate 3-fold gain in all parahydrogen derived NMR signal relative to enrichment at 77 K. Nuclear...

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Veröffentlicht in:Journal of magnetic resonance (1997) 2020-12, Vol.321, p.106869-106869, Article 106869
Hauptverfasser: Du, Yong, Zhou, Ronghui, Ferrer, Maria-Jose, Chen, Minda, Graham, John, Malphurs, Bill, Labbe, Greg, Huang, Wenyu, Bowers, Clifford R.
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Sprache:eng
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Zusammenfassung:[Display omitted] •Low cost home-built cryostat for parahydrogen enrichment at 30 K.•Cryostat is immersed in a liquid helium storage dewar.•Parahydrogen enrichment to 97% at 300 mL/min and 4.5 bar.•Approximate 3-fold gain in all parahydrogen derived NMR signal relative to enrichment at 77 K. Nuclear spin hyperpolarization derived from parahydrogen can enable nuclear magnetic resonance spectroscopy and imaging with sensitivity enhancements exceeding four orders of magnitude. The NMR signal enhancement is proportional to 4xp-1, where xp is the parahydrogen mole fraction. For convenience, many labs elect to carry out the ortho–para conversion at 77 K where 50% enrichment is obtained. In theory, enrichment to 100% yields an automatic three-fold increase in the NMR signal enhancement. Herein, construction and testing of a simple and inexpensive continuous-flow converter for high para-enrichment is described. During operation, the converter is immersed in liquid helium contained in a transport dewar of the type commonly found in NMR labs for filling superconducting magnets. A maximum enrichment of 97.3±1.9% at 30 K was observed at 4.5 bar and 300 mL/min flow rate. The theoretically predicted 2.9-fold increase in the signal enhancement factor was confirmed in the heterogeneous hydrogenation of propene to propane over a PdIn/SBA-15 catalyst. The relatively low-cost to construct and operate this system could make high parahydrogen enrichment, and the associated increase in the parahydrogen-derived NMR signals, more widely accessible.
ISSN:1090-7807
1096-0856
DOI:10.1016/j.jmr.2020.106869