甲醇-二硫化碳解吸-气相色谱法测定工作场所空气中1,2-二氯乙烯

Determination of 1,2-dichloroethylene in workplace air by methanol-carbon disulfide desorption coupled with gas chromatography

目的建立甲醇-二硫化碳解吸-气相色谱法测定工作场所空气中1,2-二氯乙烯的方法。方法空气中1,2-二氯乙烯用活性炭管采集,经甲醇-二硫化碳溶剂解吸,DB-FFAP毛细管色谱柱(30 m×0.25 mm,0.25μm)分离,火焰离子化检测器检测,保留时间定性,峰高或峰面积定量。结果顺-1,2-二氯乙烯、反-1,2-二氯乙烯的检出限分别为0.35μg/ml、0.81μg/ml;定量下限分别为1.16μg/ml、2.67μg/ml(相应的最低检出浓度分别为0.23 mg/m^(3)、0.54 mg/m^(3))。批内相对标准偏差分别为0.32%~0.60%、0.50%~0.79%,批间相对标准偏差分别为0.60%~0.95%、0.78%~0.90%;平均解吸效率分别为97.6%~101%、96.0%~98.0%;在2.5μg/ml~500μg/ml内线性关系良好,相关系数分别为0.999 8、0.999 6。结论本方法灵敏度高、准确度和精密度好,解吸效率高,可用于工作场所空气中1,2-二氯乙烯的检测。

Objective To establish a method for the determination of 1,2-dichloroethylene in workplace air by methanol-carbon disulfide desorption-gas chromatography. Methods 1,2-dichloroethylene in the air was collected with activated carbon tube,and desorbed with methanol-carbon disulfide solvent,separated by DB-FFAP capillary column( 30 m ×0. 25 mm,0. 25 μm),and detected by flame ionization detector( FID). The qualitative analysis was based on retention time and the quantitative analysis was based on peak height or peak area. Results The detection limits were 0. 35 μg/ml for cis-1,2-dichloroethylene and 0. 81 μg/ml for trans-1,2-dichloroethylene;the limits of quantification were 1. 16 μg/ml and2. 67 μg/ml,respectively( the corresponding detectable concentrations were 0. 23 mg/m^(3) and 0. 54 mg/m^(3)). The intra-batch relative standard deviations were respectively within 0. 32%-0. 60%,and 0. 50%-0. 79%. The average desorption efficiencies were respectively within 97. 6%-101% and 96. 0%-98. 0%;the method had a linear range of 2. 5 μg/ml-500 μg/ml,with correlation coefficients( r) of 0. 999 8-0. 999 6. Conclusion The method has high sensitivity,good accuracy and precision,and high desorption efficiency,and it can be used for the detection of 1,2-dichloroethylene in the air of workplaces.