气相色谱法测定磷酸三甲苯酯异构体含量  

Seperation and Analyzation of Tricresyl Phosphate Isomers

作　　者：刘多强[1] 冀德坤[2,3] 易玉峰 孙超[2] 丁福臣 王家钰 

机构地区：[1]中国人民解放军空军油料研究所,北京100076 [2]北京石油化工学院化学工程学院,北京102617 [3]燃料清洁化及高效催化减排技术北京市重点实验室,北京102617

出　　处：《化学分析计量》2017年第6期19-22,共4页Chemical Analysis And Meterage

基　　金：国家科技支撑计划课题(20152015BAK16B03);北京石油化工学院研究生创新活动计划(15033981002/072);URT项目(2017J00082)

摘　　要：建立测定磷酸三甲苯酯临、间、对位异构体含量的气相色谱方法。通过优化色谱分析条件,如降低初始柱箱温度和程序升温速度,可较好分离开TCP的10种同分异构体。选用弱极性的AB–5MS色谱柱,设置柱箱初始温度为120℃,升温速度为3℃/min,终温为300℃。使用相应的纯物质,对其中的临-临-临,间-间-间,对-对-对进行了定量分析。三种异构体在各自的线性范围内均呈良好的线性,线性相关系数大于0.999,检出限为0.162 7~0.168 8 mg/L,测定结果的相对标准偏差小于5%(n=6)。该方法检出限低,重现性好,适合于磷酸三甲苯酯异构体含量的检测。A method for the determination of ortho-, meta- and para- isomers of TCP were established. The GC conditons was optimezed, such as decreasing the initial temperature of column oven and rising rate of temperature, and ten isomers of TCP could be absolutely seperated. AB-5MS weak polarity column was selected. The optimized GC conditions were as following initial temperature of column oven 120℃, temperature rising rate of 3℃/min, final temperature at 300℃. The ortho- ortho- ortho, meta- meta- meta and para- para- para isomers were quantitatively conformed by using its pure substance. The linear correlation index was above 0.999, the detecting linear range was between 0.162 7～0.168 8 mg/L, and the relative standard deviation was less than 5%（n=6）. The method has lower detecting linear and higer repeatability and is suitable for the monitoring standards.

关 键 词：磷酸三甲苯酯临、间、对位异构体 异构体分离 定量分析 

分 类 号：O657.7[理学—分析化学]