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目的:建立自动顶空-气相色谱质谱联用技术测定化工原料中1,2-二氯乙烷含量的方法。方法:采用自动顶空进样,组分经HP-5MS毛细管色谱柱分离后依次进入质谱检测器进行定性和定量检测,以保留时间和特征离子进行定性,峰面积外标法定量。结果:1,2-二氯乙烷绝对含量在1.07μg～1070μg内呈良好线性关系,相关系数为0.9999,最低检出浓度为0.2 mg/kg,加标回收率为85.8%～101.5%,相对标准偏差(RSD)为2.21%～6.58%(n=6)。结论:本法可用于化工原料中1,2-二氯乙烷含量的测定,并可同时测定各挥发性有机组分相对百分含量。
Objective: To establish a method for the determination of 1,2-dichloroethane in chemical raw materials by automatic headspace-gas chromatography-mass spectrometry. Methods: Automated headspace sampling was used. The components were separated by HP-5MS capillary column and then entered into mass spectrometry detector for qualitative and quantitative detection. The retention time and characteristic ions were used for qualitative and peak area external standard quantification. Results: The absolute content of 1,2-dichloroethane showed a good linearity in the range of 1.07μg ~ 1070μg, the correlation coefficient was 0.9999, the lowest detection limit was 0.2 mg / kg and the recoveries were 85.8% ~ 101.5% The standard deviation (RSD) was 2.21% ~ 6.58% (n = 6). Conclusion: This method can be used for the determination of 1, 2-dichloroethane in chemical raw materials, and can simultaneously determine the relative percentage of volatile organic components.