Abstract
A simple model peroxyoxalate chemiluminescence system was monitored directly across a range of temperatures (from −80 to +20 °C) using 13 C nuclear magnetic resonance spectroscopy. These experiments were made possible by the utilisation of 13 C doubly labelled oxalyl chloride, which was reacted with anhydrous hydrogen peroxide in dry tetrahydrofuran. Ab initio quantum calculations were also performed to estimate the 13 C nuclear magnetic resonance (NMR) shift of the most commonly postulated key intermediate 1,2-dioxetanedione and this data, in concert with the spectroscopic evidence, confirmed its presence during the reaction.
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