Solid–liquid
equilibrium data for the NaCl + Na2S2O3 + H2O system at 283.15 and 303.15 K were measured using
the method of isothermal solution saturation combined with a moist
residue method of Schreinemaker, the equilibrium solid phase was identified
by powder X-ray diffraction, and finally the solid–liquid phase
diagrams of the ternary system were constructed. The ternary NaCl
+ Na2S2O3 + H2O phase
diagrams at 283.15 and 303.15 K turned out to be of the simple eutectic
type. One invariant point, two univariant curves, and two crystallization
regions exist in each of the phase diagrams. The crystallization region
of NaCl is larger than that of Na2S2O3·5H2O at 283.15 K, and the crystallization region
of NaCl expands while that of Na2S2O3·5H2O decreases when the temperature rises to 303.15
K. Consequently, the invariant point at 303.15 K is located in the
Na2S2O3·5H2O single-salt
crystallization region of the phase diagram at 283.15 K. On the basis
of this thermodynamic characteristic, a method for separation of the
NaCl + Na2S2O3 mixture was proposed,
from which both of the pure salts could be obtained.
As the solvent system ethanol + cyclohexane is selected for the purification of clopidogrel hydrogen sulfate (Form II) [CHS(II)], the solubilities of CHS(II) in the binary solvent mixtures were measured at the temperatures ranging from (283.35 to 333.75) K. The solubility increased with both the rising temperature and mole fraction of ethanol in the binary solvent. The experimental data were well-fitted by the Jouyban−Acree model, and the thermodynamic parameters were calculated correspondingly. The result demonstrated that the dissolution process of CHS(II) in the ethanol + cyclohexane mixture was endothermic and entropy-driven.
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