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Abstract Control of surface functionalization of MXenes holds great potential, and in particular, may lead to tuning of magnetic and electronic order in the recently reported magnetic Cr₂TiC₂T_x. Here, vacuum annealing experiments of Cr₂TiC₂T_xare reported with in situ electron energy loss spectroscopy and novel in situ Cr K‐edge extended energy loss fine structure analysis, which directly tracks the evolution of the MXene surface coordination environment. These in situ probes are accompanied by benchmarking synchrotron X‐ray absorption fine structure measurements and density functional theory calculations. With the etching method used here, the MXene has an initial termination chemistry of Cr₂TiC₂O_1.3F_0.8. Annealing to 600 °C results in the complete loss of F, but O termination is thermally stable up to (at least) 700 °C. These findings demonstrate thermal control of F termination in Cr₂TiC₂T_xand offer a first step toward termination engineering this MXene for magnetic applications. Moreover, this work demonstrates high energy electron spectroscopy as a powerful approach for surface characterization in 2D materials.