Irradiation of the equilibrated gas mixture CF3O2NO2 reversible arrow CF3O2 + NO2 at room temperature using the output from UV fluorescent "blacklamps" provides a rapid and simple method for the production of pure samples of CF3ONO2 in high yield (ca. 80%). This synthetic procedure is superior to that described in the literature in two aspects: (i) the yield of CF3ONO2 is approximately a factor of 5 greater, and (ii) the present method avoids the need for a high pressure (70 bar) reactor.