高等学校化学学报

高等学校化学学报 ›› 2004, Vol. 25 ›› Issue (7): 1248.

• 研究简报 • 上一篇    下一篇

微波消解-微波等离子体炬原子发射光谱法测定无铅汽油中痕量铅的研究

张金生1,2, 李丽华2, 张金平2, 金钦汉1   

  1. 1. 吉林大学化学学院, 长春 130023;
    2. 辽宁石油化工大学石油化工学院, 抚顺 113001
  • 收稿日期:2003-08-26 出版日期:2004-07-24 发布日期:2004-07-24
  • 通讯作者: 金钦汉(1937年出生),男,教授,博士生导师,从事分析科学及微波化学研究.E-mail:qhjin@jlu.edu.cn E-mail:qhjin@jlu.edu.cn

Determination of Trace Lead in Unleaded Gasoline by Microwave Digestion-Microwave Plasma Torch Atomic Emission Spectrometry

ZHANG Jin-Sheng1,2, LI Li-Hua2, ZHANG Jin-Ping2, JIN Qin-Han1   

  1. 1. College of Chemistry, Jilin University, Changchun 130023, China;
    2. School of Petroleum & Chemical Technology, Liaoning University of Petroleum & Chemical Technology, Fushun 113001, China
  • Received:2003-08-26 Online:2004-07-24 Published:2004-07-24

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被引次数

26

摘要： 四乙基铅作为一种良好的抗爆添加剂,曾广泛用于汽油生产中,但由于四乙基铅有很强的毒性,目前国际上已停止生产和使用车用含铅汽油,因此在生产车用无铅汽油时严格控制和准确测定铅的含量十分必要.迄今,测定汽油中铅含量的常用方法是铬酸盐容量法[1]、一氯化碘法[2]、X射线光谱法[3]、分光光度法[4,5]、原子吸收光谱法[6]和等离子体光谱法[7].这些方法或操作烦琐,测定时间较长[4],或灵敏度低[1～3],或测定误差较大,且在测试中需使用毒性较大的四乙基铅[5],或所需的氯化甲基三辛基铵不易购买[6],或处理过程繁琐,且仪器设备昂贵[7].因此,建立一种简便、快速、灵敏、准确和无毒副作用的测定无铅汽油中痕量铅的方法已显得十分迫切.近年来发展的微波等离子体炬原子发射光谱法[8]已有商品化仪器问世[9].本文利用微波等离子体炬原子发射光谱仪研究了无铅汽油中痕量铅的测定方法,并提出用微波消解法预处理无铅汽油样品,将微波消解技术与微波等离子体炬原子发射光谱法相结合,建立了简便、快速、灵敏、准确和无污染的测定无铅汽油中痕量铅的新方法.

关键词: 微波消解, 微波等离子体炬原子发射光谱法, 无铅汽油, 痕量铅

Abstract: Two microwave digestion procedures were developed for unleaded gasoline. Microwave plasma torch atomic emission spectrometry(MPT-AES) was used to determine trace lead in unleaded gasoline after being digested. Optimal conditions (analytical wavelength, microwave power, flow rate of carrier gas for the trace lead determination, flow rate of supporting gas, flow rate of oxygen shielding gas and acid concentrations) were chosen. The effects of concommitant elements on determination of lead were studied. The detection limit for lead was 25 ng/mL, the linear range was 0.05-100 μg/mL. The relative standard deviation for determination of unleaded gasoline samples was less than 4 9%, relative error was less than 3.7%. Standard addition recoveries were all between 93.3%-104.0%. The determination results with microwave digestion were in agreement with those obtained with conventional method. The proposed method is simple, rapid, accurate, and with less possibility to be contaminated by the environment, and of great applied value.

Key words: Microwave digestion, Microwave plasma torch atomic emission spectrometry(MPT-AES), Unleaded gasoline, Trace lead

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