Abstract
An apparatus for the production of hydrogen for hydrogenation-induced polarization studies was developed. The apparatus provides hydrogen gas from a solid source, thereby simplifying the requirement for siting of the apparatus. The produced hydrogen can be either isotopically enriched (with deuterium) or spin-enriched (with parahydrogen). These specialty gases were produced at small predetermined quantities and ambient pressure. The properties of the hydrogen mixtures were characterized by gas-phase nuclear magnetic resonance. The T 1 of the hydrogen mixtures (3.7 ms) was not affected by para-enrichment. The line width of the hydrogen signal in the para-enriched mixture was 34% larger. The reaction of ethyl propiolate hydrogenation served to evaluate the performance in terms of the ability to create hyperpolarized states. In this reaction, a polarization of 11.2% was measured for protons. Consecutive alkene hydrogenations as well as hydrogenations of the catalyst ligand resulted in additional hyperpolarized signals which were systematically assigned.
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Acknowledgments
We thank Aaron K. Grant, Elena Vinogradova, and Robert E. Lenkinski for useful discussions during the course of this work. We thank Magnus Karlsson for helpful discussions on gas-phase NMR measurements. We thank Shimon Vega for discussions on orthodeuterium. This study has been supported in part by the DANA foundation, the Bi-National Science Foundation (BSF, grant number 2006118), the German Israel Foundation (GIF, grant number 2131-1586.5/2006), the Abisch-Frenkel Foundation, and the Center for Complexity Science (grant number GR2007-053). R.K.B thanks the generosity of the Tchorz fund, the Speijer inheritance fund, and the Goldin-Savad inheritance fund.
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Gamliel, A., Allouche-Arnon, H., Nalbandian, R. et al. An Apparatus for Production of Isotopically and Spin-Enriched Hydrogen for Induced Polarization Studies. Appl Magn Reson 39, 329–345 (2010). https://doi.org/10.1007/s00723-010-0161-9
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DOI: https://doi.org/10.1007/s00723-010-0161-9