Abstract: Ten columns of various stationary phases were screened for the gas chromatographic separation of the impurities and muscone synthesized by three different routes. It was found that non-polar phases such as DC-200 were suitable for the separation of muscone and cyclopentadecanone; phases with low polarity, e. g. OV-17, were good for separating muscone and 3-methylcyclopentadecenone, while OV-17 columns of 4～5 m long was necessary for the separation of muscone and 4-methylcyclopentadecanone. The overall resolution efficiency K₁ of these columns have been calculated and its relationship with McReynolds constants discussed.n-Nonadecane was chosen as the internal standard for the quantitative determination of muscone, the calibration factor was calculated. Analytical results of samples of five different batches are reported.The impurities in samples synthesized by route A were studied in detail by GC, GC-MS, UV and IR, they were identified as α,β-3-methylpentadecenone and a nonconjugated 3-methylpentadecenone, and the constants of these compounds were determined. The cause of producing these impurities was discussed, which should be of help to the synthetic work.