柴油中微量元素的质谱分析.pdf

石油学报(石油加工)
2015年8月
ACTA PETROLEI SINICA(PETROLEUM PROCESSING SECTION)
第31卷第4期
文章编号:1001-8719(2015)04-0972-06
柴油中微量元素的质谱分析
?宏伟,谢华林?,黄建华3,李坦平
(1.湖南工学院材料与化学工程系,湖南衡阳421002;2.长江师范学院化学化工学院,重庆涪陵408100
3.湖南中医药大学药学院,湖南长沙410208)
摘要:建立了煤油稀释·电感耦合等离子体质谱(ICP-MS)法测定柴油中Na、Mg、Al、Si、P、Ca、Ti、V、Cr
Mn、Fe、Ni、Cu、Zn、Mo、Ag、Cd、Sn、Ba、Pb等20种徴量元素的分析方法。通过优化等离子体功率和载气
流速等质谱参数,维持了等离子体工作的稳定性;在等离子体中混入O2,使高浓度有机基体充分燃烧,消除了积
炭现象;应用碰撞/反应池(CRC)技术校正了质谱干扰,优化了碰撞/反应气流速;采用Be、Y、In、Bi内标混合溶
液补偿黏度差别,校正了基体效应。结果表明,20种微量元素的检出限在2.7~69.6ng/L之间,RSD在1.5%~
4.3%范圃,加标回收率在92.2%~109.0%之间。方法简便、准确,可用于柴油的质量控制和安全评价
关键词:电感耦合等离子体质谱法;柴油;煤油;微量元素;碰撞/反应池
中图分类号:O657.63文献标识码:Adoi:10.3969/j,issn.1001-8719.2015.04.020
The Determination of Trace Metal Elements in Diesel by Inductively Coupled Plasma
Mass Spectrometr
LIU Hongwei], XIE Hualin, HUANG Jianhua, II Tanping
2. College of Chemistry and Chemical Engineering, Yanglse Normal University, Fuling 408100, Chin? a,
(1. Department of Material and Chemical Engineering, Hunan Institute of Technology, Hengyang 421002, China g
3. School of Pharmacy, Hunan University of Chinese Medicine, Changsha 410208, China)
Abstract: A method was proposed for the direct determination of Na, Mg, Al, Si, P, Ca, Ti, V
Cr, Mn, Fe, Ni, Cu, Zn, Mo, Ag, Cd, Sn, Ba and Pb in diesel by inductively coupled plasma
spectrometry (ICP-MS) with kerosene as diluent of sample. The condensation and deposition of
carbon can be avoided effectively by introducing O, to plasma, and the effects arising from flow rate
of carrier gas, radio frequency power on plasma stability with the existence of O2 were investigated
in detail. The mass spectral interferences of polyatomic ions to analysis were corrected by collision
reaction cell (CRC). The collision reaction gases flow rates were optimized. Be, Y, In and Bi as the
internal standard elements were used to corrected matrix effect. The results showed that the detection limits
for the investigated elements were in the range of 2.. 6 ng/L, with the relative standard deviation of
each element within 1.5%-4.3% and the recovery of each element in the range of 92.2%-109.0%. The
method was applied for the quality control and safety evaluation of diese
Key words inductively coupled plasma mass spectrometry; diesel; kerosene; trace elements
collision reaction cell
收稿日期:2014-0412
基金项目:国家自然科学基金(21075138)、湖南省高校产业化培育项目(10CYO02,13CY019)、溯南省自然科学基金(14J5032)和湖南省重
点学科建设项目资助
第一作者:刘宏伟,男,高级实验师,硕士,主要从事质谱分析方法的研究与应用
通讯联系人:谢华林,男,教授,博士,主要从事材料化学的研究与应用; E-mail: hualinxiet@vp.163,comn