An Apparatus for Production of Isotopically and Spin-Enriched Hydrogen for Induced Polarization Studies

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.