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目的:建立大口径毛细管柱气相色谱法测定工作场所空气中肼的含量。方法:于2019年10月，用酸性硅胶管吸附工作场所空气中肼，硫酸溶液解吸，衍生剂糠醛衍生萃取后用DM-FFAP毛细管柱气相色谱氢火焰离子化检测器测定及气质联用定性。结果:肼浓度在0.1~2.0 μg/ml呈现良好的线性关系，线性方程为n y=353.8n x+21.2（n r=0.999 8）。检出限为0.030 μg/ml，定量下限为0.100 μg/ml，若采集15 L空气样品，则最低检出浓度为0.004 mg/mn 3，最低定量浓度为0.013 mg/mn 3。平均解吸效率为86.5%~89.4%，加标回收率为94.4%~97.1%，相对标准偏差为1.6%~4.9%。肼与糠醛衍生物为2-呋喃甲醛连氮。n 结论:该方法肼衍生物色谱峰峰形对称，分析时间短，易于操作，适用于工作场所空气中肼浓度的测定。“,”Objective:To determine hydrazine quantitatively in workplace air by gas chromatography with large bore capillary column.Methods:In October 2019, hydrazine in the air was adsorbed by acid silica gel tube sampling and desorped using sulfuric acid solution. After derivatization with furfural and extraction, the content of hydrazine was determined by DM-FFAP capillary column gas chromatography with flame ionization detector.Results:The linear regression equation was n y=353.8n x+21.2 (n r=0.9998) between 0.1-2.0 μg/ml of target concentration. The detection limit was 0.030 μg/ml. The lower limit of quantification was 0.100 μg/ml. If 15 L air sample was collected, the minimum detection concentration was 0.004 mg/m n 3 and the minimum quantitative concentration was 0.013 mg/mn 3 respectively. The average desorption efficiency was 86.5%-89.4%. The recovery was 94.4%-97.1%. The relative standard deviation was 1.6%-4.9%. Hydrazine and furfural derivative was 2-furaldehyde hydrazine.n Conclusion:The method has symmetrical peak shape of hydrazine derivatives chromatographic peaks, short analysis time, easy operation, and is suitable for the determination of the concentration of hydrazine in the air in the workplace.