Objective:To establish a method for the simultaneous determination of Cyclohexane and Methyl Cyclohexane in the air of workplace by Gas chromatography.Methods:Cyclohexane and Methyl Cyclohexane in the air of workplace were collected with charcoal tube,then injected after being desorbed with carbon disulfide,through 5% SE-30 glass column(2 m×4 mm) with constant temperature,detected by FID.Results:Retention time of Cyclohexane and Methyl Cyclohexane were 2.514 min,3.609 min.The linearity ranges were 8 μg/ml~389 μg/ml,8 μg/ml~385 μg/ml.The limits of detection were both 8 μg/ml.The coefficient of correlation were 0.9999,0.9999.Conclusion:The method is suitable to determine Cyclohexane and Methyl Cyclohexane in the air of workplace simultaneously.