This paper presents a spectroscopic study of emulsions generated with a laser-assisted device. Fourier transform infrared (FTIR), Raman and UV–Vis–NIR reflectance spectra of emulsions, recorded before and after exposure to laser radiation were used to characterize the effect of laser irradiation. The paper also presents a comparison between the calculated IR spectra and the experimental FTIR spectra of an emulsion’s components. FTIR measurements allowed the identification of absorption bands specific to each of the emulsions’ components. Moreover, it enabled the observation of destabilization of the emulsion in real-time. Raman spectroscopy allowed the observation of the modifications at a molecular level, by identifying the vibrations of the representative functional groups and the polymerization of sodium tetradecyl sulfate (STS) molecules by analyzing the evolution of the carbonyl band. UV–Vis–NIR reflectance spectra of emulsions before and after exposure to laser radiation showed that the physical characteristics of the emulsions changed during irradiation—the dimensions of the droplets decreased, leading to an emulsion with a better time stability. These results proved that the employed spectroscopy techniques were powerful tools in emulsion analysis.