Abstract: The analytical method for determination of methanol and ethanol in 2BP solution of the reprocessing by capillary gas chromatography was investigated in this paper. The test results show that the linearity between the peak area and concentration is excellent in the range of 16.395 mg/L with a correlation coefficient of over 0.999; the relative standard deviation of methanol (RSD) is better than 7.0% (n=6), the relative standard deviation of ethanol (RSD) is better than 9.0% (n=6); the minimum detectable limit (MDL) are 2.7 mg/L and 1.6 mg/L; the recovery rate of measurement is 95%-111%. The possible impurities which such as formaldehyde, methanoic acid, acetic acid, nitric acid, hydrazine, monomethyl hydrazine, methylamine and N,N -dimethylhydroxylamine did not affect the quantitative determination of methanol and ethanol by the analytical system.