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A centrifuge method to determine the solid-liquid phase behavior of eutectic mixtures.

Adriaan van den Bruinhorst1, Laura J B M Kollau1, Maaike C Kroon2

  • 1Laboratory of Physical Chemistry, Department of Chemical Engineering and Chemistry, Eindhoven University of Technology, Het Kranenveld, Building 14 (Helix), 5612 AZ Eindhoven, The Netherlands.

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A new centrifuge method accurately determines phase diagrams for binary eutectic mixtures, including challenging deep eutectic solvents (DESs). This equilibrium-based technique offers an alternative to dynamic methods, especially for supercooling mixtures.

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Area of Science:

  • Materials Science
  • Physical Chemistry
  • Chemical Engineering

Background:

  • Constructing solid-liquid phase diagrams is crucial for understanding binary eutectic mixtures.
  • Conventional methods like differential scanning calorimetry and hot-stage microscopy are dynamic and can struggle with mixtures prone to supercooling.
  • Deep eutectic solvents (DESs) often exhibit significant supercooling, complicating phase diagram determination.

Purpose of the Study:

  • To develop and verify a novel, equilibrium-based analytical procedure, the centrifuge method, for constructing solid-liquid phase diagrams of binary eutectic mixtures.
  • To demonstrate the centrifuge method's advantage over dynamic techniques for mixtures with strong supercooling behavior.
  • To validate the method using both a nearly ideal and a strongly non-ideal eutectic system.

Main Methods:

  • The centrifuge method involves equilibrating mixtures at a constant temperature.
  • This equilibrium-based approach avoids the need for recrystallization from the melt during analysis.
  • The method was tested on the biphenyl-bibenzyl system and the urea-choline chloride deep eutectic solvent.

Main Results:

  • The centrifuge method successfully reproduced the binary eutectic phase behavior of both tested systems.
  • The method proved advantageous for the urea-choline chloride system, which is prone to supercooling.
  • Equilibration at constant temperature allows for accurate phase diagram construction without melt recrystallization.

Conclusions:

  • The centrifuge method is a viable and effective alternative for quantifying the liquid range of binary eutectic mixtures.
  • It offers a significant advantage for analyzing mixtures, such as deep eutectic solvents, that exhibit strong supercooling.
  • This novel technique expands the analytical toolkit for phase diagram determination in materials science and chemistry.