The purpose of this study was to determine whether temperature scanning ultrasonic velocity measurements could be used to monitor the complex thermal transitions that occur during the crystallization and melting of triglyceride solid lipid nanoparticles (SLNs). Ultrasonic velocity (u) measurements were compared with differential scanning calorimetry (DSC) measurements on tripalmitin emulsions that were cooled (from 75 to 5 °C) and then heated (from 5 to 75 °C) at 0.3 °C min−1. There was an excellent correspondence between the thermal transitions observed in δΔu/δT versus temperature curves determined by ultrasound and heat flow versus temperature curves determined by DSC. In particular, both techniques were sensitive to the complex melting behavior of the solidified tripalmitin, which was attributed to the dependence of the melting point of the SLNs on particle size. These studies suggest that temperature scanning ultrasonic velocity measurements may prove to be a useful alternative to conventional DSC techniques for monitoring phase transitions in colloidal systems.