微波消解-高分辨电感耦合等离子体质谱(HR-ICP-MS)法测定原油中22种微量元素  

Determination of 22 Trace Elements in Crude Oil by High Resolution Inductively Coupled Plasma Mass Spectrometry with Microwave Digestion

作　　者：李银花 赵雨薇 刘曙 安雅睿 LI Yinhua;ZHAO Yuwei;LIU Shu;AN Yarui(Institute of Bismuth and Rhenium,University of Shanghai for Science and Technology,Shanghai 200093,China;Technical Center for Industrial Product and Raw Material Inspection and Testing of Shanghai Customs,Shanghai 200135,China)

机构地区：[1]上海理工大学铋铼科学研究中心,上海200093 [2]上海海关工业品与原材料检测技术中心,上海200135

出　　处：《中国无机分析化学》2022年第6期94-102,共9页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点研发计划项目(2018YFF0215400)。

摘　　要：准确测定原油中微量元素含量,对研究原油地球化学,揭示原油原产地信息,具有重要意义。通过采用微波消解原油样品,优化样品质量、消解试剂、消解程序等微波消解条件,考察原油中B、Mg、Al、P、Ti、Ca、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、As、Sr、Mo、Cd、Sn、Ba、Pb等22种微量元素在低、中、高分辨率下的质谱干扰及校正方法,采用高分辨测定Ca,中分辨测定P、V、Cr、Mn、Fe、Ni、Cu、Cd、Co、Sr,低分辨率模式测定其余元素,建立了微波消解-高分辨电感耦合等离子体质谱(HR-ICP-MS)法测定原油中22种元素的方法。在优化的实验条件下,22种元素的线性相关系数均大于0.999,方法检出限为0.0002~0.07μg/g。选择原油多元素均质标准品(Conostan S-21)进行方法验证,B、Mg、Al、P、Ti、Ca、V、Cr、Mn、Fe、Ni、Cu、Zn、Mo、Cd、Sn、Ba、Pb元素测定结果的相对标准偏差为0.20%~2.8%,测定值与标准值基本一致;选择巴西原油、安哥拉原油、喀麦隆原油、尼日利亚原油进行Co、Ga、As、Sr元素加标回收实验,加标回收率为95.3%~104%,测定结果的相对标准偏差为0.20%~2.3%。选取巴西原油、安哥拉原油、喀麦隆原油、尼日利亚原油进行22种元素测定,分析了不同产地原油的元素含量差异。方法能够应用于原油中多种微量元素的同时测定,灵敏度高,选择性好,检出限低,结果准确可靠,可为原油地球化学研究提供技术支持。Accurate determination of trace elements in crude oil is of great significance to study crude oil geochemistry and to reveal the information of crude oil orign.In this work,microwave digestion as crude oil sample pretreatment was used to optimize the sample quality,digestion reagent,digestion process and other microwave digestion conditions.The mass spectrum interference and correction methods of 22 trace elements in crude oil,including B,Mg,Al,P,Ti,Ca,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,As,Sr,Mo,Cd,Sn,Ba and Pb,at low,medium,and high resolution were investigated.Ca was determined with high resolution,P,V,Cr,Mn,Fe,Ni,Cu,Cd,Co and Sr were determined with medium resolution,and other elements were determined with low resolution mode.A method for the determination of 22 elements in crude oil by microwave digestion and high resolution inductively coupled plasma mass spectrometry was established.Under the optimized experimental conditions,the linear correlation coefficients of 22 elements were all greater than 0.999,and the detection limits of the method were 0.0002—0.07μg/g.Conostans-21 was selected to verify the method.The relative standard deviations of B,Mg,Al,P,Ti,Ca,V,Cr,Mn,Fe,Ni,Cu,Zn,Mo,Cd,Sn,Ba and Pb were 0.20%—2.8%.The measured value is basically consistent with the standard value.The spiked recoveries of Co,Ga,As and Sr from Brazil,Angola,Cameroon and Nigeria crude oil were 95.3%—104%,and the relative standard deviations(RSD)were 0.20%—2.3%.The crude oils from Brazil,Angola,Cameroon and Nigeria were selected for the determination of 22 elements,and the differences of element contents in crude oils from different producing areas were analyzed.This method can be applied to the simultaneous determination of trace elements in crude oil,with high sensitivity,good selectivity and low detection limit.The results are accurate and reliable,which can provide technical support for the study of crude oil geochemistry.

关 键 词：原油 微量元素 微波消解 高分辨电感耦合等离子体质谱 

分 类 号：O657.63[理学—分析化学] TH843[理学—化学]