摘要
0.500 0g柴油抗磨剂样品用10mL甲苯溶解,然后用甲苯定量至30g,采用电感耦合等离子体原子发射光谱法测定样品溶液中钠、钾、钙、镁、铁、钼、锌、磷、硼、硅、锡等11种微量元素。氧气流量为30mL·min^(-1),钠、钾、钙、镁、铁、钼、锌、磷、硼、硅、锡的分析谱线依次为588.957 0,766.444 0,393.386 0,279.512 1,259.913 0,202.016 7,213.815 8,214.915 7,249.713 5,251.613 4,189.917 7nm。在等离子体气体中加入氧气有效消除了积碳现象,以钇为内标元素。11种元素的线性范围均为0.05~10.0mg·L^(-1),检出限(3s)为0.001 2~0.086 1 mg·kg^(-1)。在1.000 mg·kg^(-1)浓度水平进行加标回收试验,回收率为95.7%~107%,测定值的相对标准偏差(n=6)为1.3%~4.7%。
The sample of diesel antiwear agent(0.500 0 g)was dissolved with 10 mL of toluene,and then diluted to 30 g with toluene.ICP-AES was applied to the determination of trace amounts of 11 elements,i.e.Na、K、Ca、Mg、Fe、Mo、Zn、P、B、Si and Sn in the sample solution.Oxygen flow was 30 mL·min-1.Analytical spectral lines of 588.957 0,766.444 0,393.386 0,279.512 1,259.913 0,202.016 7,213.815 8,214.915 7,249.713 5,251.613 4,189.917 7 nm were chosen for the determination of Na、K、Ca、Mg、Fe、Mo、Zn、P、B、Si and Sn respectively.The deposition of carbon could be avoided effectively by introducing oxygen to plasma.Y was used as internal standard.Linearity ranges of the 11 elements were found in the same range of 0.05-10.0 mg·L-1 with detection limits(3 s)in the range of 0.001 2-0.086 1 mg·kg-1.Tests for recovery were made by standard addition method at the concentration level of 1.000 mg·kg-1,giving values of recovery and RSD′s(n=6)in the ranges of95.7%-107% and 1.3%-4.7% respectively.
作者
李鹰
俞晓峰
夏晓峰
李剑
赵琎
LI Ying;YU Xiaofeng;XIA Xiaofeng;LI Jian;ZHAO Jin(Focused Photonics (Hangzhou) Inc. , Hangzhou 310000, China)
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2018年第5期516-519,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
"重大科学仪器设备开发"重点专项(2016YFF0100200)