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Conducting polymer (Polypyrrole) and tin oxide (SnO2) composite films have been fabricated with layer-by-layer technique. SnO2 film was screen-printed on Al2O3 substrate and then it was dip-coated with polypyrrole (PPy) solution. The microstructures of composite films were evaluated by a field emission scanning electron microscope (FE-SEM). It was observed the sensing properties of PPy/SnO2 sensor to various VOCs. Methanol, ethanol, benzene and toluene were analyzed. The target vapors were vaporized using their vapor presents and their concentrations were precisely controlled using mass flow controller (MFC) and temperature controller. The reproducibility of sensing properties was evaluated and the humidity effect of PPy/SnO2 was checked.