顶空-GC法快速测定聚丙烯酸酯类胶黏剂中的残留单体  

Rapid determination of residual monomers in polyacrylate adhesives by headspace-gas chromatography

作　　者：黄飞[1] 卢科 HUANG Fei;LU Ke(Zhejiang Transfar Co.,Ltd.,Hangzhou 311215,China)

机构地区：[1]浙江传化股份有限公司,浙江杭州311215

出　　处：《印染》2020年第4期54-59,共6页China Dyeing and Finishing

摘　　要：建立了一种快速测定聚丙烯酸酯类印花胶黏剂中苯乙烯、醋酸乙烯酯、甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸乙酯和丙烯酸丁酯6种典型残留单体的顶空-气相色谱分析方法。配制体积比为65:35的N,N-二甲基甲酰胺-水混合溶液作为溶剂,样品稀释后经80℃、30min顶空加热,通过DB-WAX强极性色谱柱(30m×0.25 mm×0.25 μm)分离和FID检测器分析后采用外标法定量。结果表明,6种残留单体在该色谱条件下均能较好分离,检出限(3倍信噪比)为0.166-0.287mg/kg,定量限(10倍信噪比)为0.553~0.957mg/kg,平均回收率为101.5%~120.9%,相对标准偏差(RSD,n=5)小于5.1%。该方法仪器成本低、前处理简单、定性定量准确、灵敏度高,适用于快速检验、检测胶黏剂产品中苯乙烯、醋酸乙烯酯、甲基丙烯酸甲酯和丙烯酸酯类残余单体。A rapid headspace gas chromatography method for the determination of six typical residual monomers of styrene,vinyl acetate,methyl methacrylate,methyl acrylate,ethyl acrylate and butyl acrylate in polyacrylate printing adhesives is developed.The mixture of N,N-dimethylformamide and water with a volume ratio of 65:35 is prepared as solve nt.The sample is diluted and heated at 80°C for 30 min in headspace.After separation by DB-WAX column(30m×0.25 mm×0.25μm)and analysis by FID detector,the external standard method is used for quantitative analysis.The results show that the six kinds of residual monomers can be separated well under the chromatographic conditions.The detection limit(S/N=3)is 0.166-0.287 mg/kg,the quantitative limit(S/N=10)is 0.553-0.957 mg/kg,the average recovery is 101,5%~120.9%,and the relative standard deviation(RSD,n=5)is less than 5.1%.This method has the advantages of low cost,simple pretreatment,accurate qualitative and quantitative analysis,and high sensitivity.It is suitable for the rapid inspection and detection of styrene,vinyl acetate,methyl methacrylate and acrylate residual monomers in a large number of adhesive products.

关 键 词：测试 顶空-气相色谱法 印花胶黏剂 残留单体 聚丙烯酸酯 

分 类 号：TS197[轻工技术与工程—纺织化学与染整工程]