自动顶空气相色谱法同时测定服装中残留丙烯腈和氯乙烯单体  

Determination of acrylonitrile monomer and vinyl chloride in clothing by capillary gas chromatography with AutoHS headspace sampler

作　　者：刘俊[1] 朱然[2] 田延河[1] 刘宏祥 全小盾[1] 张旭龙[1] 

机构地区：[1]新疆出入境检验检疫局技术中心,乌鲁木齐830063 [2]新疆大学化学与化工学院,乌鲁木齐830046

出　　处：《中国卫生检验杂志》2010年第9期2164-2166,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的：建立了自动顶空毛细管气相色谱法测定服装中残留丙烯腈和氯乙烯单体含量的分析方法。方法：准确称取样品于顶空瓶中,加入DMA,加盖密封,放入自动顶空进样器,供气相色谱分析,外标法定量。对不同极性色谱柱进行选择性实验,最终采用DB-624毛细管柱和氢火焰检测器测定,同时对平衡温度和平衡时间等顶空条件以及色谱条件进行优化。结果：丙烯腈和氯乙烯单体在各自的浓度范围内呈良好的线性关系（r分别为0.99987和0.99990,n=5）。对丙烯腈和氯乙烯分别做3组（n=5）浓度水平的加标回收实验,平均回收率在90%－110%之间,相对标准偏差（RSD）均小于4.25%,丙烯腈和氯乙烯检出限（LOD）分别为0.50μg/g和0.25μg/g。结论：实验结果表明,该方法简便、快速,适合出口服装中残留丙烯腈和氯乙烯单体的测定。Objective：An analytical method has been described for the quantitative determination of acrylonitrile monomer and vinyl chloride in clothing by.Methods： Headspace capillary gas chromatography has been developed.The acrylonitrile and chloroethlene monomer were isolated from a standard solution or samples using a headspace system,then quantified by GC-FID.The experimental conditions of headspace and GC were optimized.External standards were used for quantitative determination.DB-624 capillary column and flame ionization detector（FID） were employed.Results： Under the optimal condition,linear responses were obtained for acrylonitrile and chloroethlene monomer in their respective concentration ranges（R1=0.99987,n1=5;R2=0.99990,n2=5）.The average recoveries were 96.6%～99.2% for acrylonitrile monomer and 90.0%～110.0% for chloroethlene monomer,and relative standard deviations were 〈4.25% in three levels respectively.The limits of detection of acrylonitrile and chloroethlene monomer were 0.50 μg/g and 0.25 μg/g,respectively.Conclusion： The method was simple and quick.It was suitable for the determination of acrylonitrile monomer and vinyl chloride in exported clothing.

关 键 词：服装 毛细管色谱柱 顶空 气相色谱 丙烯腈单体 氯乙烯单体 

分 类 号：O657.71[理学—分析化学]