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

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0.500 g用20 mL甲苯超声萃取40 min，在离心后的上层清液10 mL中加入10.0 mg·L^-1 3，3'-二氯联苯胺溶液10 μL和N-甲基双三氟乙酰胺（衍生化试剂）20 μL。用DB-5色谱柱（30 m×0.25 mm，0.25 μm）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0.10~5.00 mg·L^-1，检出限（3S/N）为1.50 mg·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%。

Abstract: 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 20 μL of MBTFA (derivatization reagent) were added in the supernatant (10 mL). The analyte was separated on DB-5 column (30 m×0.25 mm, 0.25 μm) 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%.