The potential of TD SEC for in situ analyses of thermoreversibly bonded polymers is discussed. TD SEC allows the evolution of the polymer’s molar mass distribution to be monitored during temperature-sensitive bonding and debonding reactions. Through quantitative evaluation of the chromatograms, the reaction-influencing parameters can be studied, which is crucial for the effective development of novel functional materials. By using TD SEC, the effect of polymer size and flexibility on the debonding temperatures of DA polymers was confirmed, their debonding and bonding ability studied, and the de-crosslinking of thermoreversibly cross-linked DA polymers assessed. TD SEC offers a versatile platform for a broad variety of different polymer materials and to assess a variety of different analytical questions.