有机溶剂辅助微波消解-电感耦合等离子体质谱法测定多种原油中微量金属元素  

Determination of Trace Metal Elements in Crude Oils by Microwave Digestion-Inductively Coupled Plasma-Mass Spectrometry Assisted with Organic Solvent

作　　者：李景喜[1] 陈发荣[1] 杨春茹[1] 崔维刚[1] 郑立[1] 王小如[1,2] 

机构地区：[1]国家海洋局第一海洋研究所海洋生态研究中心,山东青岛266061 [2]厦门大学化学化工学院化学系,现代分析科学教育部重点实验室,福建厦门361005

出　　处：《岩矿测试》2011年第1期12-16,共5页Rock and Mineral Analysis

基　　金：国家海洋局第一海洋研究所基本科研业务费专项资助(2010G23);海洋公益性行业科研专项资助(200705011);海洋溢油鉴别与损害评估技术重点实验室开放基金资助(200920)

摘　　要：建立了二氯甲烷溶剂辅助微波消解-电感耦合等离子体质谱法测定原油中V、Cr、Fe、Ni、Cu、Zn、Mo、Co、Pb等16种微量金属元素。研究表明,用CH2Cl2分散原油样品,以浓HNO3-H2O2为消解体系,采用CEM微波消解系统消解样品,各元素线性关系良好,相关系数≥0.9995;检出限可达ng/L;方法精密度较高,相对标准偏差(RSD,n=3)<5.0%;回收率为92%～110%。以w(Ni)/w(V)与w(Fe)/w(V)比值为变量参数对不同原油样品进行聚类分析,表明国内与国外不同地区原油样品中各金属元素含量差异较大。A method for determination of V,Cr,Fe,Ni,Cu,Zn,Mo Co,Pb,etc in different crude oils was established by inductively coupled plasma-mass spectrometry assisted with organic solvent microwave digestion.The oil sample was digested by microwave using HNO3-H2O2 as oxidant after dispersing in organic solvent（CH2Cl2）.The results showed that the detection limits of the method reached ng/L level for sixteen elements.The linear correlation of the method was preferable with the correlation coefficient of better than 0.9995.The recoveries of the method were in the range of 92%~110% with the precision of less than 5.0%RSD（n=3）.The ratios of w（Ni）/w（V） and w（Fe）/w（V） were distinct in different crude oil samples from oversea and domestic,and the index can be used to the cluster analysis for differencing the crude oil samples.

关 键 词：微量金属元素 原油 电感耦合等离子体质谱法 微波消解 有机溶剂 

分 类 号：O652.4[理学—分析化学] O657.63[理学—化学]