Liquid–liquid equilibria (LLE) data for the water + acetic acid + nopol + nopyl acetate quaternary system was measured at (298.15, 323.15, and 348.15) K and at atmospheric pressure of 85.8 kPa. Thermodynamic consistencies of the experimental data were verified by Othmer-Tobias, Bachman, and Hand correlations. LLE experimental results were correlated with NRTL thermodynamic model. Binary interaction parameters for NRTL model are reported.