The aqueous peroxyoxalate chemiluminescence (CL) reaction of bis[N-[2-(N'-methyl-2'-pyridiniumyl)ethyl]-N-[(trifluoromethyl)sulfonyl]]oxamide (METQ) with hydrogen peroxide in the presence of a fluorophor was characterized in different micellar and homogeneous media, and the effects of the various types of surfactants on chemiluminescence intensity and quantum efficiencies were assessed. The surfactants examined include cationic, anionic, neutral, and zwitterionic types. In the presence of hexadecyltrimethylammonium chloride (CTAC), polyoxyethylene (23) dodecanol (Brij 35), and 3-(N-dodecyl-N,N-dimethylammonio)-1-propanesulfonic acid (SB-12) micelles, enhancement of the CL intensity by factors of 1.6-130 was observed relative to that in buffer. It was found that in micellar medium not only were fluorescence efficiencies improved but also the reaction excitation efficiency. The various experimental variables that influence the magnitude of the CL enhancements were studied. Lastly, the micellar CL reaction systems were evaluated for the analysis of fluorophors and hydrogen peroxide, and analytical figures of merit were generally improved in micellar medium.