Fluorescence technology was examined as an analytical tool for identifying naphthenic acids in process-affected water. The fluorescence signal from process-affected water was narrowed down to the extractable organic acid fraction, known to contain naphthenic acids. A characteristic intensity peak was observed in a consistent location in the emission spectrum when scanned at 280nm excitation wavelength for water obtained from three oil sands operations. The signals obtained for each water source exhibited similar shapes but varied by intensity. The intensity observed was compared to naphthenic acid concentration determined by the industry standard analytical method. When examined individually there was a strong linear correlation between fluorescence intensity and concentration for the water sources. Models developed using the parallel factor analysis method found that process-affected water from each oil sand operation had five fluorescent species which contributed to the overall signal, and that the species were similar between process-affected water from each company.