We report on the measurement of molecular scale self-organization of aqueous adipic acid solutions near and above their saturation concentrations. We use the steady-state and time-resolved fluorescence responses of the probe molecule 1-pyrenecarboxylic acid to elucidate information on precrystalline adipic acid aggregates in solution. We have used this probe molecule to ensure the proximity of the fluorescent moiety to the solution phase aggregation events of interest. Steady-state fluorescence data demonstrate the pH dependence of the chromophore response, with an acid dissociation constant of K-a = 1.64 x 10(-5). The fluorescence lifetime of protonated I-pyrenecarboxylic acid (HPCA) exhibits a discontinuous change at the saturation concentration of adipic acid, although there is Little structural information contained in such data. The rotational diffusion behavior of HPCA reveals the presence of aggregates of adipic acid with the fluorophore. We discuss these data in the context of solute local organization and the limits these data place on the lifetime of the aggregates.