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A new method to determine a ternary phase diagram of benzene–acetic acid–water system is provided to upper-division undergraduate students. The partially miscible liquid phase region can be accurately constructed using isothermal titration microcalorimetry (ITC). Compared with the traditional visual method, ITC can provide precise data and more information about the dissolution process despite the expensive instrument and the long titration time. This experiment can be conditionally incorporated into a physical chemistry laboratory curriculum as a modern acquisition of a classic ternary phase diagram.