The isophthalic acid(IPA) is present in polyethylene glycol terephthalate(PET) at small level, but plays an important role for the properties of polyester fiber. Thus the PET sample was hydrolysated by 100 g/L of sodium hydrate in methanol at 70 degrees C during 10 h and finally assayed by HPLC. A reversed-phase high performance liquid chromatographic method for the separation of isophthalic acid from terephthalic acid(TPA) has been developed. The operating conditions were Novapak C18 column, methanol-water(15:85, V/V)(pH3) as mobile phase with the flow rate of 1.0 mL/min and UV detection wavelength at 254 nm.