燃烧离子色谱法测定α-烯烃齐聚反应体系中催化剂BF_(3)的含量  

Determination of BF_(3)Content in theα-Olefin Oligomerization Reaction System by Combustion Ion Chromatography

作　　者：赵文慧 徐冰 苏朔 徐广通 史军歌 ZHAO Wenhui;XU Bing;SU Shuo;XU Guangtong;SHI Junge(SINOPEC Research Institute of Petroleum Processing Co.,Ltd.,Beijing 100083,China)

机构地区：[1]中石化石油化工科学研究院有限公司,北京100083

出　　处：《石油学报（石油加工）》2023年第2期458-464,共7页Acta Petrolei Sinica(Petroleum Processing Section)

基　　金：中国石油化工股份有限公司项目(ST19030)基金资助。

摘　　要：BF_(3)作为α-烯烃齐聚反应催化剂,其含量控制对催化反应的调控与产品质量的把控至关重要。通过建立样品前处理方法、优化仪器测试条件与标准溶液配制方法,建立利用燃烧离子色谱测定BF_(3)·醇催化的α-烯烃齐聚反应体系中F元素含量,进而计算出BF_(3)含量的方法,并考察了方法的重复性和准确性。结果表明:利用该方法可测定BF_(3)质量分数范围为2.68~53.50 g/kg的样品,前处理时适量的正丁醇和白油可有效稳定和稀释样品;测定稀释样品中F元素含量的标准曲线分为2段,线性范围分别为300~2000 mg/L和2000~3000 mg/L,线性相关系数R^(2)分别为0.9992和0.9940;测定5次BF_(3)质量分数结果相对标准偏差均小于5%,方法加标回收率在95.0%~105.0%之间,方法检出限取决于前处理时的取样量,当取样量为5 g时,检出限为1 mg/kg。The content control of BF_(3)as theα-olefin oligomerization catalyst is vital to the control of catalytic reaction and product quality.Through establishing the sample pretreatment method,optimizing instrument test conditions and the preparation method of standard solution,a method was built for determining F element content in theα-olefin oligomerization reaction system under BF_(3)·balcohol catalysis by combustion ion chromatography,so as to further calculate the content of BF_(3);the repeatability and accuracy of the method were also investigated.The results show that the method is suitable for determining samples with the BF_(3)mass fraction of 2.68—53.50 g/kg.During pretreatment,a proper amount of n-butanol and white oil can effectively stabilize and dilute the samples.The standard curve of determining F element content in the diluted sample can be divided into two sections,with the linear range of 300 to 2000 mg/L and 2000 to 3000 mg/L,and the linear correlation coefficients of 0.9992 and 0.9940,respectively.The relative standard deviation of BF_(3)mass fraction results after 5 times of determination is less than 5%,and the standard recovery rate is between 95.0%and 105.0%.The detection limit is determined by sampling amount during the pretreatment procedure.when the sampling amount is 5 g,the detection limit is 1 mg/kg.

关 键 词：燃烧离子色谱 BF3 聚Α-烯烃 F含量测定 烯烃齐聚反应 

分 类 号：O657.7[理学—分析化学]