In this paper, a new method of synchronous microemulsion stabilized room temperature phosphorimetry for thf simultaneous determination of fluoranthene and chrysene, fluoranthene and acenaphthene, fluoranthene and p-terphenyl is described, The experiments indicate that suitable Delta lambda are 188 nm, 185 nm and 191 nm in proper order, Synchronous peaks are situated at 360 nm and 323 nm (fluoranthene and chrysene), 360 nm and 306 nm (fluoranthene and acenaphthene), 360 nm and 317 nm (fluoranthene and p-terphenyl) respectively in the mixture. The limit quantity of interference between components in binary mixture was examined, The linear range of determination reached two amount order and relative standard deviation less than 5%. The results of determination for double components synthetic sample are satisfactory.