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A nonthermal, pulsed spark discharge is applied to three polymer powders in Ar and Ar–H2 ${{\rm{H}}}_{2}$ gas mixtures. Hydrogen is introduced to assess plasma‐driven decomposition. Gaseous decomposition products, including methane, acetylene, and ethylene, are observed with Fourier‐transform infrared (FTIR). Surface modifications are observed on the residual polymer via attenuated total internal reflection‐FTIR. Time‐averaged rotational, vibrational, and excitation temperatures are characterized in the discharge. The plasma density is found to be around 3×1022 m−3 $3\times 1{0}^{22}\unicode{x0200A}{{\rm{m}}}^{-3}$, with rotational and vibrational temperatures ranging from 1500 to 2200 K and an excitation temperature of 1–2 eV. While spark properties did not change with either gas composition or polymer composition, it was determined that the addition of hydrogen promoted higher concentrations of gaseous phase products (promoting hydrogenolysis). [ABSTRACT FROM AUTHOR]