An ultraviolet-visible laser absorption-scattering technique (UV-LAS) was developed for obtaining the evaporation characteristics of binary-component fuel spray. P-xylene and fluorobenzene were selected as the substitutes for low and high boiling points components, respectively, in a binary fuel spray. The molar absorption coefficients (MAC) of p-xylene and fluorobenzene at 266 nm wavelength were measured with relative uncertainty of 2.8% in a calibration system, which was designed to facilitate control of the mixture temperature and vapor concentration. UV-LAS was applied to a quantitative detection of vapor concentration distributions of each component in a binary-component fuel spray injected into a high-temperature and high-pressure constant volume chamber. A difference in spatial stratification of each component fuel in the spray due to their volatility difference was observed. An uncertainty estimation of UV-LAS for binary-component fuel spray was performed, and the results show that the maximum uncertainty is less than 9.8% in measurement of vapor mass.