Five polycyclic aromatic hydrocarbons, i.e. acenaphthene, fluoranthene, pyrene, benz[a]anthracene and benzo[a]pyrene were simultaneously determined by variable-angle synchronous scanning (VASS) microemulsion phosphorimetry at room temperature. The phosphorescence emissions of the five compounds have been obtained using sodium sulphite as O-2 scavenger and thallium(I) nitrate as heavy atom salt perturbation in sodium dodecyl sulphate (SDS) microemulsion aqueous solutions. In order to obtain the optimum phosphorescence responses, a statistical model of central composite design type, was applied. Despite the closely overlapping profiles of the five phosphorescent compounds, the increased selectivity afforded by the VASS technique has permitted their simultaneous determination after addition to road dust samples giving mean recoveries of 87.6% with a relative standard deviation of 3.0%, (n=5). (C) 1997 Elsevier Science B.V.