The EPS l‐AP‐74–1 method (equivalent of U.S. EPA method 5) modified by the addition of a fifth impinger containing the polymer adsorbent was used in stack sampling of an aluminum reduction plant. The cyclohexane soluble organics extracted from the fraction of nozzle and probe wash, particulates on filter, water in impingers and polymer adsorbent were analyzed using a gas chromatograph equipped with the SE‐54 fused silica capillary column and the flame ionization detector. The concentrations of vapor phase polycyclic aromatic hydrocarbons from fraction of water in impingers, XAD‐2 and Tenax GC were compared for evaluation of the relative efficiency of these three adsorption matrices.