This study introduced Taylor Dispersion Analysis of Micellization (TDAM), a microcapillary technique combining intrinsic and extrinsic fluorescence detection, to characterize the assembly and dissociation of α-, β- and κ-casein micelles in milk. Taylor Dispersion Analysis (TDA), the method behind Flow Induced Dispersion Analysis (FIDA), was used to measure the calcium-dependent colloidal stability, viscosity and association/dissociation kinetics of the three casein types. α-casein micelles were the least stable and rapidly dissociated without Ca²⁺, β-casein formed concentration-dependent micellar species with complex dissociation, and κ-casein micelles stayed highly stable. Complemented by dynamic light scattering and modeling, TDAM showed how Ca²⁺ governs micelle association, viscosity and dissociation.