Investigation of reactions that determine safety properties of LIB cells is key for understanding degradation (aging) effects of the cell system e.g. via deciphering thermally induced reactions of active materials. In this study, an approach is conducted to determine thermal profiles of anodes and cathodes at different states of charge (SOCs) after electrochemical aging. Thermal profiling is performed using three different methods to determine temperature-related loss of mass, detection of m/z, and heat flow. After determination of thermal profiles, detailed analysis using pyrolysis-GC-MS is accomplished. Main points that were concluded from this study are that electrophilic lithiated anodes show intense decomposition behavior and reactions with electron-rich binder molecules. Moreover, it is possible to prove thermally induced de-lithiation as it was suggested before. De-lithiated cathodes (layered material) are prone to phase changes which can be obtained via detection of distinct oxygen release. Different decomposition properties of the solid electrolyte interphase is obtained depending on the SOC. The cathode electrolyte interphase exposes a SOC-dependent detection behavior; oligocarbonates are obtained for SOC 100%, solely CO2 at high temperatures (>515 °C) for SOC 0%. Eventually, we provide a set of methods for thermal profiling to unravel reactions that determine safety properties of LIBs.