摘要
二甲基甲酰胺(DMF)萃取精馏生产的聚合级异戊二烯中含有环戊二烯、2-丁炔、异戊烯炔、1-戊炔、顺-1,3-戊二烯、反-1,3-戊二烯、DMF和对-叔丁基邻苯二酚(TBC)等微量杂质。采用中心切割技术,以毛细柱HP-1为主分析柱,毛细柱CP-Al_(2)O_(3)/Na_(2)SO_(4)为辅助分析柱,建立了上述8种微量杂质的气相色谱分析方法。结果表明:该方法将8种微量杂质含量集中在一套色谱上进行分析,单次进样可实现所有待测杂质的有效分离,回收率在95.6%~104.9%之间,相对标准偏差均小于2.2%;与通用方法相比,将填充柱色谱系统改为毛细柱系统,间戊二烯分析灵敏度明显提升,可满足对异戊二烯和丁基橡胶原料的分析要求;采用外标法定量,可提高分析结果的准确性。该方法已应用于日常异戊二烯的质量监控中,方法简单实用,具有可推广性。
The polymeric grade isoprene produced by the extraction and distillation method with dimethylformamide(DMF)contains trace impurities such as cyclopentadiene,2-butyne,iso-pentenylene,1-pentyne,cis-1,3-pentadiene,trans-1,3-pentadiene,DMF,and p-tert-butylcatechol(TBC).A gas chromatography method was developed for the determination of these eight trace impurities by central cutting technique with HP-1 as the main analytical column and CP-Al_(2)O_(3)/Na_(2)SO_(4)as the auxiliary analytical column.The results showed that 8 kinds of trace impurities could be separated and analyzed on a set of chromatograms by this method;the recovery rates were 95.6%-104.9%,the relative standard deviation was less than 2.2%,indicating high accuracy and reliability.Compared with the general method,the sensitivity of isoprene analysis was significantly improved by changing the packed column chromatography system to the capillary column system,it could meet the analysis requirements of isoprene and butyl rubber raw materials,and the accuracy of analysis results could be improved by using external standard method.It could simultaneously measure the content of DMF and TBC,saving analytical instrument resources and reducing workload.This method has been used for daily quality monitoring of isoprene,and its stability and reliability have been fully verified.
作者
赵亮
郝亚冉
陈雷
Zhao Liang;Hao Yaran;Chen Lei(SINOPEC Beijing Yanshan Company,Beijing 102500)
出处
《石油炼制与化工》
CAS
CSCD
北大核心
2024年第7期129-134,共6页
Petroleum Processing and Petrochemicals
关键词
中心切割法
聚合级异戊二烯
微量杂质
外标法
气相色谱
central cut gas chromatography
polymer-grade isoprene
trace impurities
external standard method
gas chromatography
