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

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。

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

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.