Previous research has shown that trifluoronitromethane (CF3NO2), when subjected to UV light, will break down with the products being CF2O and FNO. Outside sources have determined the heat of reaction for the dissociation of CF3NO2 to be -28 kcal/mol. Exposure of CF3NO2 to light in the ultraviolet region would induce a photolytic breakdown of the molecule. This dissociation is controlled via matrix isolation, in which small quantities of trifluoronitromethane gas are trapped in a nitrogen matrix at dilutions of 1:18.4, 1:60.4, 1:561, and 1:3350 (CF3NO2:N2). Subsequent photolysis of the matrix was performed via a hydrogen lamp, the output of which is directed through both sodium chloride and calcium fluoride windows. Photolysis of the trapped matrix was conducted in the range of 20 to 27 K. Molecular reactions were then observed by use of Fourier Transform infrared spectroscopy (FTIR). Analysis of the results indicate the presence of CF2O and FNO, as well as traces of CF3NO. CF3NO2 was monitored at frequencies of 1620 cm-1, 865 cm-1, and 751 cm-1. The products CF2O and FNO were monitored at the frequencies 1938 cm-1, 1907 cm-1, 965 cm-1, 1844 cm-1, and 765 cm-1 respectively. The change in absorbance of CF3NO2 was plotted against both CF2O and FNO. Trifluoronitromethane gas can be prepared via oxidation of CF3NO by H2O2, as described by previous research.