Solubilization of 1,2,3-propanetriol, PT, and its aqueous solution, PT-W, (W ) water), by reverse aggregates of sodium bis(2-ethylhexyl) sulfosuccinate, Aerosol-OT or AOT, in isooctane has been studied by FTIR and 1 H NMR spectroscopy, and the results were compared with those of solubilization of 1,2ethanediol, ED, and W by the same surfactant. Curve fitting of the IR νOD band of aggregate-solubilized PT or PT-W showed the presence of a main peak and a smaller one. Dependence on [solubilizate]/[AOT] of 1 H NMR chemical shifts, δproton, of solubilized PT, PT-W, as well as the surfactant protons showed monotonic increase or decrease. Both spectroscopic techniques indicated the following order of interaction with AOT: PT > ED > W. Over the entire range of [solubilizate]/[AOT], the main νOD peak areas correspond to 88 ( 2%, and 90 ( 2% of the total peak areas for PT, and PT-W, respectively. This result shows that aggregate-solubilized PT or PT-W do not seem to coexist in "layers" of different structures, as suggested by the multistate solubilization model.