A Fiber-Optic Probe is Developed for the Fast, In-Situ Measurement of Volumetric Expansion of Multiphase and Multicomponent Systems. an Experiment with the Binary Mixtures of CO2-Toluene and CO2-Ethanol Was Conducted to Demonstrate the Usefulness of the Fiber-Optic Probe in Accurately Tracking the Isothermal Volumetric Expansion as a Function of Pressure. in the 1-L Autoclave that Has Been Used, the Probe Was Shown to Detect the Liquid Level Height within a Precision of 0.35% of the Total Height of the Vessel. the Results for the Volumetric Expansion of Toluene and Ethanol with CO2 Correlate Well with Those Found in the Literature. the Probe itself Can Be Used Up to Pressures of 140 Barg and Temperatures of 120°C. © 2007 American Chemical Society.