顶空气相色谱法测定溶剂型胶黏剂中苯、甲苯和二甲苯  

Determination of benzene,toluene and xylene in solvent-based adhesives by HS-GC

作　　者：金艳妮[1] 孙银生[1] 杜娟[1] JIN Yan-ni;SUN Yin-sheng;DU Juan(Henan Nuclear Industry Radionuclide,Zhengzhou 450044,China)

机构地区：[1]河南省核工业放射性核素检测中心,河南郑州450044

出　　处：《化学工程师》2023年第6期38-41,共4页Chemical Engineer

摘　　要：选用DMF(N-N二甲基甲酰胺)提取溶剂型胶黏剂中苯系物,以静态顶空气相色谱法进样,以正十一烷为内标物,采用内标标准曲线法测定苯、甲苯和二甲苯的含量。实验表明,在称样量为0.20g、DMF提取剂用量为0.80mL时,样品回收率达到峰值。通过优化顶空、气相色谱分离条件,确定顶空与色谱压力差为0.02MPa、柱流速为1.20mL·min^(-1)、分流比为4∶1时的色谱分离条件最佳,方法的检出限为0.005~0.006mg·kg^(-1);样品加标回收实验中苯回收率为95.2%,甲苯回收率为92.8%,二甲苯回收率为91.2%~93.6%;在精密度实验中,苯的RSD为1.9%,甲苯的RSD为2.4%,二甲苯的RSD为1.6%~3.6%。该方法简单,快速,灵敏度高,结果准确、可靠,适用于溶剂型胶黏剂中苯、甲苯和二甲苯的测定。Benzene was extracted from solvent-based adhesives by DMF(Top N-N dimethylformamide),and the contents of benzene,toluene and xylene were determined by internal standard curve method with n-undecane as internal standard.The results showed that the recovery rate reached the peak when the sample weight was 0.20g and DMF extraction agent dosage was 0.80mL.By optimizing the separation conditions of headspace and gas chromatography,the pressure difference between headspace and chromatography was determined to be 0.02MPa,the column flow rate was 1.20mL·min^(-1),the best separation condition was the shunt ratio of 4∶1.Experimental results:the detection limit of the method was 0.005~0.006 mg·kg^(-1);The recoveries of benzene,toluene and xylene were 95.2%,92.8%and 91.2%~93.6%respectively.The RSD for benzene,toluene and xylene were 1.9%,2.4%and 1.6%~3.6%respectively.The method is simple,rapid,sensitive,accurate and reliable,and suitable for the determination of benzene,toluene and xylene in solvent-based adhesives.

关 键 词：静态顶空-气相色谱 DMF提取 内标标准曲线法 胶黏剂 

分 类 号：O657.6[理学—分析化学]