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Precipitating polymer in a completely aqueous environment is conceptualized as a process of aqueous phase separation (APS) and lends itself to the environmentally friendly fabrication of membranes. In an effort to effectively regulate the morphological formation in APS, it is of fundamental concern to elucidate how asymmetry can be developed in the absence of an unbalanced exchange of the 'nonsolvent' and solvent. Therefore, technical modifications were made by this study to essentially improve the in-situ characterization based on optical coherence tomography (OCT). In particular, a process of APS was modeled by passively contacting an acidic aqueous dope of chitosan with another aqueous solution of sodium hydroxide in a mini-coagulation bath, where the OCT scan was implemented in a high speed mode to capture the onset and evolution of gelation at the coagulant-dope interface with a temporal resolution of 6.25 ms. The quantitative analysis indicated that the gelation could be initiated at the interface in a period shorter than ∼10 ms and evolved in an oscillating way; a skin layer with a smaller critical size would be formed by damping the interfacial oscillations. This study not only sheds light on the APS-based fabrication of membranes, but also establishes a novel paradigm for in-situ characterizing the film formation via an OCT-based approach. [Display omitted] • Formation of asymmetry in APS was modeled by the gelation of chitosan. • OCT was used to in-situ characterize the initial gelation occurring at the interface. • Passive contact was employed to eliminate the delay resulting from immersion. • High speed scan mode enabled achieving a temporal resolution of 6.25 ms. • Interfacial oscillations in the gelation were correlated with the skin rejection. [ABSTRACT FROM AUTHOR]