微波消解样品-原子荧光光谱法测定原油中铅、砷和汞含量  

AFS Determination of Pb,As and Hg in Crude Oil with Microwave Assisted Sample Digestion

作　　者：王豪[1] 邬蓓蕾[1] 陈平[1] 林振兴[1] 孙妮妮[1] 潘意隆[1] 

机构地区：[1]宁波出入境检验检疫局,宁波315000

出　　处：《理化检验（化学分册）》2012年第9期1027-1029,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局科技计划项目(2006IK057)

摘　　要：采用微波消解法,用硝酸-过氧化氢(10+2)溶液作消解剂,以硫脲溶液作为预还原剂,以溶于氢氧化钾溶液中的硼氢化钾溶液作为还原剂,利用原子荧光光谱法测定原油中铅、砷和汞的含量。分析中采用载气及屏蔽气的流量依次为300mL.min-1及800mL.min-1。铅、砷和汞的荧光强度与它们的质量浓度依次在2.0～80.0,2.0～100.0,1.0～20.0μg.L-1之间呈线性关系,方法的检出限(3S/N)依次为0.05,0.05,0.01mg.kg-1。应用此法对原油样品进行分析,铅、砷和汞的回收率分别在103%～115%,87.5%～92.1%,87.5%～102%之间。AFS was applied to the determination of Pb, As and Hg in crude oil. The sample was digested with mixed solution of HNO3-H2O2 （10 ＋ 2）, and thiourea solution was added to the sample solution as pre- reductant and KBH4 solution （dissolved in KOH solution） as reductant, Flow-rates of 300 mL·min-1 for carrier gas and 800 mL. min-1 for shielding gas were taken in the analysis. Linear relationships between values of fluorescence intensity and mass concentration of Pb, As and Hg found were in the ranges of 2.0--80. 0, 2.0--100. 0 and 1.0--20. 0 μg·L-1 , with detection limit （3S/N） of 0. 05, 0. 05 and 0. 01 mg·kg-1 respectively. The proposed method was applied to the analysis of samples of crude oil, giving values of recovery in the ranges of 103%--115% for Pb, 87.5%--92.1% for As and 87.5%--102% for Hg.

关 键 词：微波消解样品 原子荧光光谱法 原油 铅 砷 汞 

分 类 号：O657.31[理学—分析化学]