In situ microscopic measurement is a novel approach to clarify the intrinsic mechanism of complexation reactions occurring at liquid/liquid interfaces. The present review was mainly focused on recent three topics of methodology of in situ fluorescence microscopic observation and measurement of interfacial complexation reactions: (1) two kinds of self-assemblies of Pd2+ and 5,10,15,20-tetra(4-pyridy1)-21H, 23H-porphine complexes formed at the toluene/water interface, (2) microextraction of Eu3+

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... ith 2thenoyltrifluoroacetone at the dodecane/water interface, (3) rapid complexation of Zn2+ with 5-octyloxymethy1-8-quinolinol in the 1-butanol/water interfacial region. The inhomogeneities of adsorption and reaction of complexes or the fast complexation rate at the liquid/liquid interface was measurable only by the microscopic methods.