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Detection of toxic and flammable gases and volatile organic compounds (VOCs) released from Li-ion batteries during thermal runaway can generate an early warning. A submicron (∼0.15 μm)-thick poly(3,4-ethylenedioxythiophene) polystyrene sulfonate (PEDOT:PSS) sensor film is coated on a platinum electrode through a facile aqueous dispersion. The resulting sensor reliably detected different volatile organic compounds (VOCs) released during the early stages of thermal runaway of lithium-ion batteries (LIBs) even at low concentrations. The single-electrode sensor utilizes impedance spectroscopy to measure ethyl methyl carbonate and methyl formate concentrations at 5, 15, and 30 ppm independently and in various combinations using ethanol as a reference. In contrast to DC resistance measurement, which provides a single parameter, impedance spectroscopy provides a wealth of information, including impedance and phase angle at multiple frequencies as well as fitted charge transfer resistance and constant-phase elements. Different analytes influence the measurement of different parameters to varying degrees, enabling distinction using a single sensing material. The response time for ethyl methyl carbonate was measured to be 6 s. Three principal components (PCs) preserve more than 95% of information and efficiently enable discrimination of different classes of analytes. Application of low-power PEDOT:PSS-based gas sensors will facilitate cost-effective early detection of VOCs and provide early warning to battery management systems (BMS), potentially mitigating catastrophic thermal runaway events.