The
formation of hydroxylated intermediates is the first step in
the persulfate-based advanced oxidation processes (AOPs) and depends
directly on the oxidation degree of recalcitrant pollutants. Therefore,
the monitoring of hydroxylated intermediates plays a vital role in
persulfate-based AOPs for evaluating the oxidation degree and understanding
the degradation mechanism. In this work, based on the attractive amplification
of luminol chemiluminescence (CL) signals by hydroxylated intermediates,
we developed a rapid, sensitive, and simple CL-based method to monitor
hydroxylated intermediate (i.e., 3,5-diethyl-1,4-benzenediol) generated
in persulfate-based AOPs of 1,2-divinylbenzene (DVB). The possible
mechanism of the proposed CL system was that hydroxylated intermediates
could be oxidized by persulfate in alkaline solution to form superoxide
anion radicals and thus lead to an increase in the luminol CL. Finally,
the proposed CL system was successfully applied in monitoring hydroxylated
intermediates generated during persulfate-based AOPs under different
degradation conditions, whose validity and reliability were verified
by liquid chromatography–mass spectrometry (LC-MS) and Fourier-transform
infrared spectroscopy (FT-IR). The generality of the proposed CL system
was verified by monitoring hydroxylated intermediates generated in
persulfate-based AOPs of methylbenzene and benzoic acid. These results
suggested that this present CL system provided a promising indicator
for monitoring hydroxylated intermediates in persulfate-based AOPs.