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In this work, a dodecylsulfate-doped nano porous polypyrrole gas sensor (PPy-DS) has been prepared by vapor deposition polymerization of pyrrole on surfaces of commercial polymer fiber in the presence of dodecyl sulfate (DS) as an anion dopant. The sensing behavior of PPy-DS in the presence of several aromatic hydrocarbons: benzene (B), ethyl benzene (E), toluene (T), 1,3,5-trimethylbenzene (TMB), and some other volatile organic compounds were studied experimentally. The PPy-DS had demonstrated fast response time ( <; s), sensitive for BTE and TMB with good reproducibility when reused. The sensitivity of the PPy-DS for various organic hydrocarbons was in the following order: BTE, TMB ≫ alcohol, acetone, acetonitrile, chloroform, and carbon disulfide. The PPy-DS coupled to a gas chromatograph and used for speciation determination of BTE and TMB in water samples by using a dispersive liquid-liquid microextraction (DLLME) method.