气相色谱-质谱测定磷酸三甲酚酯邻位异构体

Determination of Tri-o-cresyl Phosphate by GC-MS

磷酸三甲酚酯是一种优良的抗磨剂,在润滑油中被广泛应用。磷酸三甲酚酯有邻位,间位和对位3种异构体,邻位异构体的生理毒性大,要求在磷酸三甲酚酯中的含量不能大于0.2%质量分数,因此准确测定磷酸三甲酚酯中邻位异构体的含量尤为重要。通过优化气相色谱-质谱(GC-MS)的测定参数,以三苯基膦为内标物,建立了测定磷酸三甲酚酯邻位异构体的方法。磷酸三甲酚酯邻位异构体定性分析和定量分析的下限分别为25.2μg/g和84.0μg/g。当磷酸三甲酚酯邻位异构体和三苯基膦的质量比在0.1933~3.8590时,质量比与其峰面积比呈线性关系,相关系数为0.999,平均回收率为99.4%,相对标准偏差为1.60%,满足小于5.0%的分析要求。GC-MS是一种测定磷酸三甲酚酯邻位异构体含量的可靠方法。(图4表4参考文献5)

Tricresyl phosphate was an excellent anti-wear additive,which was widely used in lubricants.Tricresyl phosphate had three isomers of ortho,meta and para.The ortho isomer had highly physiologically toxic and the content in tricresyl phosphate was required to be less than 0.2%.So it was particularly important to accurately determine the content of ortho isomer in tricresyl phosphate.By optimizing the determination parameters of GC-MS and taking triphenylphosphine as internal standard,a method for the determination of tri-o-cresyl phosphate was established.The lowest detection limits of qualitative and quantitative analysis of the tri-o-cresyl phosphate was 25.2μg/g and 84.0μg/g respectively.When the mass ratio of tri-o-cresyl phosphate to triphenylphosphine was 0.1933~3.8590,the mass ratio had a linear relationship with its peak area ratio,the correlation coefficient was 0.999,the average recovery rate was 99.4%,and the relative standard deviation was 1.60%,which met the analysis requirements of less than 5.0%.GC-MS was a reliable method for the determining of tri-o-cresyl phosphate(.Charts4 Tables4 References5)