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Simultaneous dissociation of two weak acids is considered as a model for simultaneous equilibria. Three\u2010way data obtained from excitation\u2013emission spectrofluorimetric monitoring of a pH\u2010metric titration is analyzed using a proper combination of well\u2010known soft\u2010modeling methods. Multivariate curve resolution\u2010alternating least squares is used for calculating the excitation and emission spectral profiles of involved species and rank annihilation factor analysis for obtaining the contribution of each species in measured excitation\u2013emission matrices at different pHs. The results of simulated and real simultaneous acids dissociation equilibria showed that the proposed combined method performs well even in situation when the equilibrium constants are close to each other. The applicability of method for study of an acidic dissociation is also shown. 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