Fig. shows the TGA/MS analysis of BM1, BM2, and BM3 samples carried out under pyrolytic conditions (i.e., Argon gas) to study the mass change happening due to different reactions and analyze the gases evolved during the process. Pyrolysis pretreatment not only results in phase transformations of Li[NixMnyCoz]O₂ and graphite (as discussed in Fig. ) but also removes organic impurities from particle surfaces (such as electrolytes, PVDF, and other organic species). TGA/MS under pyrolytic conditions can be used to efficiently plan pretreatment and recycling strategies by analyzing gases evolved from the decomposition of residual electrolytes, PVDF, and other organic species. Fig. , Fig. , and Fig. show that the mass loss occurred in samples BM1, BM2, and BM3, respectively, within the temperature range of 50 °C -200 °C is ~4 -5 wt. %. MS spectra for BM1, BM2, and BM3 in Fig. , Fig. , and Fig. , respectively, show that this mass loss is attributable to evaporation of EMC (ethyl methyl carbonate) and decomposition of other electrolyte solvents such as EC (ethylene carbonate). Fig. shows that the BM2 sample also gives rise to various MS signals other than just the EMC MS signal within the 50 °C -200 °C temperature range, such as PO (propylene carbonate), HF, CH 4, and CO. These species likely originate from the decomposition of carbonate-based electrolyte solvents, while the detection of HF suggests the decomposition of the LiPF6 in BM2. The results indicate that despite undergoing low-temperature treatment (<200 °C), these BM samples retain residual electrolytes. TGA/MS analysis of pure 1.0 M LiPF6 in EC/EMC under inert conditions (Fig. ) further supports these findings. Moreover, the ATR-FTIR spectrum of evaporated species captured from BM3 at 200 °C (Fig. ) matches that of the same 1.0 M LiPF6 in EC/EMC, confirming that the evaporated species within 50 °C -200 °C range are residual electrolytes. Fig. shows a mass loss of ~4 wt. % within the 200 °C -500 °C temperature range for the three BM samples and can be attributed to mainly the decomposition of the PVDF binder. The decomposition temperature of PVDF binder is reported to be ~475 °C, however, it can start to decompose at ~380 °C and the majority of PVDF decomposes by ~500 °C, as shown by TGA/MS analysis of pure PVDF in Fig. . However, the complete decomposition of PVDF can require heating the BM at significantly higher temperatures, as it is reported that PVDF can form a liquid film on the surface of CAM at ~500 °C. TGA/MS analysis of pure PVDF under inert conditions (Fig. ) shows that the total mass loss till 1000 °C is ~75 %, leaving behind ~25 % carbonaceous char. As the temperature reaches 500 °C, Li[NixMnyCoz]O2 CAM particles react with graphite under an inert atmosphere and reduce into separate metal oxides, as shown in equations (S1) and (S2). Further increase in temperature (Fig. ) results in a significant mass loss of ~20 wt. % within the 500 °C -800 °C region for BM1, BM2, and BM3. This is caused by the further reduction of metal oxides (such as NiO, CoO) into metallic phases (such as Ni, Co). These findings are in agreement with the XRD analysis of pyrolyzed BM (Fig. ). MS spectra for each BM1, BM2, and BM3 in Fig. , Fig. , and Fig. , respectively, show that mass loss within this region produces a large amount of CO2 gas, whereas BM2 also produces MS spectra for CO as well as CH4 gases within this region.