衍生化反应-气相色谱法测定聚氨酯胶黏剂中3,3′-二氯-4,4′-二氨基二苯基甲烷  

GC Determination of 3,3′-Dichloro-4,4′-diaminodiphenylmethane in Polyurethane Adhesives with Derivatization Reaction

作　　者：陈鹏 刘实华 袁庆丹 徐丹华 郭中宝 CHEN Peng;LIU Shihua;YUAN Qingdan;XU Danhua;GUO Zhongbao(China Building Material Test and Certification Group Co.,Ltd.,Beijing 100024,China)

机构地区：[1]中国建材检验认证集团股份有限公司,北京100024

出　　处：《理化检验（化学分册）》2018年第8期888-891,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家重点研发计划项目(2016YFC0700600)

摘　　要：采用衍生化反应-气相色谱法测定聚氨酯胶黏剂中3,3′-二氯-4,4′-二氨基二苯基甲烷(MOCA)的含量。聚氨酯胶黏剂样品0.500g用20mL甲苯超声萃取40min,在离心后的上层清液10mL中加入10.0mg·L^(-1 )3,3′-二氯联苯胺溶液10μL和N-甲基双三氟乙酰胺(衍生化试剂)20μL。用DB-5色谱柱(30m×0.25mm,0.25μm)分离,电子捕获检测器检测。以3,3′-二氯联苯胺为内标物。MOCA的线性范围为0.10~5.00mg·L^(-1),检出限(3S/N)为1.50mg·kg^(-1)。加标回收率为85.4%~96.7%,测定值的相对标准偏差(n=6)均小于2.0%。GC was applied to the determination of 3,3＇-dichloro-4, 4＇-diaminodiphenylmethane （MOCA） in polyurethane adhesives with derivatization reaction. The polyurethane adhesive sample （0. 500 g） was extracted ultrasonically with 20 mL of toluene for 40 min. After centrifugation, 10 μL of 10. 0 mg·L^-1 DCB solution and 20μL of MBTFA （derivatization reagent） were added in the supematant （10 mL）. The analyte was separated on DB-5 column （30 m×0. 25 ram, 0. 25μm） and detected by ECD. DCB was used as internal standard. Linearity range of MOCA was found in the range of 0. 10--5.00 mg· L-1 with detection limit （3S/N） of 1.50 mg~ kg-1. Values of recovery found by standard addition method were in the range of 85.4%-96. 7%, and values of RSDs （n=6） were less than 2. 0%.

关 键 词：气相色谱法 聚氨酯胶黏剂 3 3′-二氯-4 4′-二氨基二苯基甲烷 衍生化反应 

分 类 号：O657.7[理学—分析化学]