High-pressure phase equilibria for the systems containing carbon dioxide, an organic (methanol, toluene, or acetone), and perfluoro-n-hexane were measured using a variable-volume view cell, by a method capable of rapid and facile measurement of compositions and density in both phases with no sampling or calibration. This phase behavior gives insight into the use of gaseous carbon dioxide (CO2) as a miscibility switch for organic and fluorous phases in homogenous catalyst recovery.