A custom-made, air-coupled ultrasonic device was applied to cure monitoring of thick samples (7-10 mm) of unsaturated polyester resin at room temperature. A key point was the optimization of the experimental setup in order to propagate compression waves during the overall curing reaction by suitable placement of the noncontact transducers, placed on the same side of the test material, in the so-called pitch-catch configuration. The progress of polymerization was monitored through the variation of the time of flight of the propagating longitudinal waves. The exothermic character of the polymerization was taken into account by correcting the measured value of time of flight with that one in air, obtained by sampling the air velocity during the experiment. The air-coupled ultrasonic results were compared with those obtained from conventional contact ultrasonic measurements. The good agreement between the air-coupled ultrasonic results and those obtained by the rheological analysis demonstrated the reliability of air-coupled ultrasound in monitoring the changes of viscoelastic properties at gelation and vitrification. The position of the transducers on the same side of the sample makes this technique suitable for on-line cure monitoring during several composite manufacturing technologies.