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<p>We
demonstrate that heterogeneous/biphasic chemical reactions can be monitored with
high spectroscopic resolution using zero-field nuclear magnetic resonance. This
is possible because magnetic susceptibility broadening is insignificant at
ultralow magnetic fields. We show the two-step hydrogenation of dimethyl
acetylenedicarboxylate with <i>para</i>-enriched hydrogen gas in conventional
glass NMR tubes, as well as in a titanium tube. The low frequency zero-field
NMR signals ensure that there is no significant signal attenuation due to
shielding by the electrically conductive sample container. This method paves
the way for <i>in situ</i> monitoring of reactions in complex heterogeneous
multiphase systems and in reactors made from conductive materials without
magnetic susceptibility induced line broadening.</p></div>