聚氯乙烯(PVC)管材中氯乙烯单体的溶解沉淀-顶空-气相色谱法测定  

Determination of Vinyl Chloride Monomer in Poly(vinyl chloride)(PVC)Pipes by Dissolution Precipitation-Headspace-Capillary Gas Chromatography

作　　者：余胜兵[1] 朱炳辉[1] 许瑛华[1] 戴光伟[1] 钟秀华[1] 

机构地区：[1]广东省疾病预防控制中心,广东广州510300

出　　处：《分析测试学报》2010年第10期1083-1086,共4页Journal of Instrumental Analysis

基　　金：广东省医学科研基金资助项目(B2010027)

摘　　要：建立了聚氯乙烯(PVC)管材中氯乙烯单体的溶解沉淀-顶空-气相色谱法。选择HP-Wax毛细管柱为分离色谱柱,4mL含水量为37.5%(体积分数)的N,N-二甲基乙酰胺(DMA)溶液溶解PVC管材,在75℃平衡35min的条件下顶空进样进行气相色谱分析。结果显示,氯乙烯在0.025～2.50mg/L范围内线性关系良好,相关系数r=0.9993。以3倍信噪比计算,该方法的检出限为4.75μg/L。对样品加标测定6次,加标回收率为90%～96%,相对标准偏差(RSD)小于6.0%。该方法比常规的顶空进样方法的灵敏度提高了近9倍,具有操作简单、快速、灵敏度高、准确度和精密度好等优点,适合于PVC管材中氯乙烯单体的检测。A new method was established for the determination of vinyl chloride monomer in poly（vinyl chloride）（PVC）pipes by dissolution precipitation-headspace-capillary gas chromatography with flame ionization detector（FID）.The principle of this method was based on that a proper percent of water added to N,N-dimethylacetamide（DMA）solution could decrease the solubility of vinyl chloride in DMA solution and thus increase the concentration of vinyl chloride in gas phase.Smashed pipes were dissolved by DMA and water was added to precipate the polymers.4 mL DMA solution with 37.5%（by volume）water was used for the dissolution and precipitation of the polymer.The samples were injected into the gas chromatograph with headspace sampler after equilibrated at 75 ℃ for 35 min.The vinyl chloride was separated by HP-Wax capillary column and quantified by the external standard method.The calibration curve of vinyl chloride was linear in the range of 0.025-2.50 mg/L（r=0.999 3）.The limit of detection（S/N=3）was 4.75 μg/L,which is 9 times higher than that of the conventional headspace gas chromatography.The spiked recoveries of vinyl chloride were in the range of 90%-96% with relative standard deviations（RSDs,n=6）less than 6.0%.The new method was simple,convenient,sensitive and accurate,and was suitable for the determination of vinyl chloride monomer in PVC pipes.

关 键 词：溶解沉淀 顶空 毛细管色谱柱 氯乙烯 

分 类 号：O657.71[理学—分析化学] TQ222.423[理学—化学]