摘要
建立了一种测定工业丙烯腈和丙烯酸甲酯中微量阻聚剂对羟基苯甲醚(MEHQ)的气质联用法,利用SH-RXI-5MS(30 m×0.25 mm×0.25μm)型毛细管柱分离、质谱检测器(EI)检测、外标标准曲线法定量。MEHQ的加标回收率为99.4%~101.9%,相对误差为0.1%~6.7%,检出限低至0.024 mg/L,具有较高的灵敏度;目标化合物MEHQ在0.400~80.000 mg/L范围内有较好的线性关系,线性相关系数R2≥0.999。不同日测量结果的相对标准偏差均低于3.0%,具有较好的准确度和精密度。该方法已成功应用于工业用丙烯腈和丙烯酸甲酯中微量MEHQ的检测,同时保证测试人员的安全。
A gas chromatography-mass spectrometry method is established for the determination of trace phydroxyanisole polymerization inhibitor in industrial acrylonitrile and methyl acrylate.In which,a SH-RXI-5 MS(30 m×0.25 mm×0.25μm)type capillary column is used for separation,mass detection(EI)is used for detection,and external standard curve method is used for quantification.Standard recoveries of p-hydroxyanisole(MEHQ)are in the range of 99.4%-101.9%,the relative error is in the range of 0.1%-6.7%,the detection limit is as low as 0.024 mg·L-1,and the sensitivity is high.Target compound MEHQ shows a good linear relationship in the range of 0.400-80.000 mg·L-1,with a linear correlation coefficient of R2≥0.999.The relative standard deviations of the measurement results on different days are all lower than 3.0%,which has good accuracy and precision.This method has been successfully applied to the detection of trace MEHQ in industrial acrylonitrile and methyl acrylate,while ensuring the safety of testers.
作者
楚艳杰
袁航
张善营
刘文涛
刘浩
朱诚身
CHU Yan-jie;YUAN Hang;ZHANG Shan-ying;LIU Wen-tao;LIU Hao;ZHU Cheng-shen(School of Materials Science and Engineering,Zhengzhou University,Zhengzhou 450001,China;Modern Analysis and Gene Sequencing Center,Zhengzhou University,Zhengzhou 450001,China;Zhengzhou Siwei Special Materials Co.,Ltd.,Zhengzhou 450199,China;Henan Provincial Key Laboratory of Advanced Nylon Materials and Applications(Zhengzhou University),Zhengzhou 450001,China)
出处
《现代化工》
CAS
CSCD
北大核心
2020年第11期230-233,共4页
Modern Chemical Industry
基金
国家重点研发计划(2018YFD0400702)。
