The recovery of ethylene glycol from its crude solutions in the production of polyethylene terephthalate (PET) has become important recently because of the rising cost of feedstocks for the manufacture of synthetic fibers and other polymeric materials. This work dealt with procedures for separation of ethylene glycol from its crude solutions and also with the identification of impurities, primarily phenols. The separation was carried out by fractional distillation techniques using three different additives: kerosene, hexachloronaphthalene, and naphthalene. The best additive was found by comparing the amounts of· recovered glycol. The identification of impurities was done by infrared spectroscopy and nuclear magnetic resonance spectroscopy.