A new method of synchronous solid-substrate roomtemperature phosphorimetry for the simultaneous determinations of m-terphenyl and p-terphenyl is described. Tl2SO4 is used as heavy atom perturber. The measurement is carried out on filter paper, with △λ 180nm for synchronous scanning, which gives peaks at 450nm and 490nm for m-terphenyl and p- terphenyl, respectively. m -Terphenyl can be directly determined from the corresponding synchronous signals, while synchronous signal of p -terphenyl at 490nm is slightly interfered by that of m -terphenyl, and should be corrected. The linear ranges of the determination are 0. 46to 92 nanogram for m -terphenyl, 0. 46 to 46 nanngram for p -terphenyl.