A preparation method of thermoreversible poly(vinyl chloride) (PVC) gels was presented. The PVC/bis(2-ethylhexyl) phthalate (DOP) gels were prepared by evaporation of tetrahydrofuran (THF) from PVC/DOP/THF solutions. The residual THF concentration in the gels was measured using headspace gas chromatography (HSGC). Results showed that the residual THF concentration was too low to affect the viscoelastic properties of PVC gels.