摘要
采用反相高效液相色谱法测定聚对苯二甲酰对苯二胺(PPTA)回收溶剂N-甲基吡咯烷酮(NMP)中对苯二甲酰氯与对苯二胺(PPD)的残留量,探讨了高效液相色谱仪的色谱条件,并研究了分析方法的精密度、准确度、检出限。结果表明:采用反相高效液相色谱法测定回收溶剂NMP中PPD的含量,适宜的色谱条件为色谱柱采用十八烷基硅烷键合硅胶柱,流动相中水/改性剂(体积比为991)与乙腈体积比为955,紫外波长为280 nm,进样量为10μL;该分析方法精密度优、重复性好、线性方程的相关性好,相对标准偏差为0.85%,加标回收率为98.1%~101.1%,检出限为0.35μg/g,能满足PPTA回收溶剂NMP中微量PPD含量的测定需求。
The residual amounts of terephthaloyl chloride and p-phenylenediamine(PPD)in N-methylpyrrolidone(NMP)solvent recovered from poly-p-phenylene terephthamide(PPTA)synthesis were determined by reverse-phase high-performance liquid chromatography.The high-performance liquid chromatographic conditions were explored,and the precision,accuracy and detection limit of the analytical method were studied.The results showed that the rational chromatographic conditions were as followed:octadecyl stlane bonded silica gel(ODS)chromatographic column,the volume ratio of water/modifier(volume ratio 991)to acetonitrile of 955 in the mobile phase,the ultraviolet wavelength 280 nm and the injection amount 10μL when the reverse-phase high-performance liquid chromatography was adopted to determine the PPD content of recovered NMP solvent;and this analytical method had high precision,good repeatability,excellent linear equations correlation,relative standard deviation of 0.85%,standard addition recovery rate of 98.1%-101.1%and detection limit of 0.35μg/g,which can meet the determination requirements of trace PPD in recovered NMP solvent for PPTA production.
作者
陈建梅
苏凤仙
CHEN Jianmei;SU Fengxian(Research Institute of SINOPEC Yizheng Chemical Fiber Co.,Ltd.,Yizheng 211900;Jiangsu Key Laboratory of High Performance Fiber,Yizheng 211900)
出处
《合成纤维工业》
CAS
2023年第6期91-95,共5页
China Synthetic Fiber Industry
关键词
聚对苯二甲酰对苯二胺
N-甲基吡咯烷酮
对苯二甲酰氯
对苯二胺
反相高效液相色谱法
测定
poly-p-phenylene terephthamide
N-methylpyrrolidone
terephthaloyl chloride
p-phenylenediamine
reversed-phase high-performance liquid chromatography
determination
