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Polymers are one of the major constituents in electrical components. A study investigating pre-combustion off-gassing and particle release by polymeric materials over a range of temperatures can provide an understanding of thermal degradation prior to failure which may result in a fire hazard. In this work, we report simultaneous measurements of pre-combustion vapor and particle release by heated polymeric materials. The polymer materials considered for the current study are silicone and Kapton. The polymer samples were heated over the range 20 to 400°C. Response to vapor releases were recorded using the JPL Electronic Nose (ENose) and Industrial Scientific's ITX gas monitor configured to detect hydrogen chloride (HCl), carbon monoxide (CO) and hydrogen cyanide (HCN). Particle release was monitored using a TSI P-TRAK particle counter.