首页|基于破乳诱导萃取和ICP-MS/MS分析渣油中的微量金属元素

基于破乳诱导萃取和ICP-MS/MS分析渣油中的微量金属元素

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基于破乳诱导萃取提出利用电感耦合等离子体串联质谱(ICP-MS/MS)测定渣油中多种金属元素的新策略.渣油样品经二甲苯稀释降低黏度后采用质量分数6%的Triton X-114乳化,超声水浴破乳25 min,利用体积分数40%的盐酸萃取渣油中金属元素至水相,采用ICP-MS/MS测定其中10种金属元素Na、Mg、Al、Ca、V、Cr、Fe、Ni、Cu、Zn的含量.详细评估了破乳诱导萃取条件对渣油中金属元素萃取效率的影响,在串联质谱(MS/MS)模式下,利用氦碰撞气或不同反应气消除了金属元素的质谱干扰,采用标准参考物质NIST SRM 1634c(燃油中的微量元素)验证了方法的准确性,以微波消解技术处理渣油样品并采用扇形磁场电感耦合等离子体质谱(SF-ICP-MS)进行对比分析验证了方法的可靠性.结果显示,金属元素在各自的含量范围内呈现良好的线性关系(线性相关系数≥0.9997),检出限(LOD)为2.05~31.4 ng/L,NIST SRM 1634c的测定结果与标准参考物质提供的认证值及文献报道的参考值基本一致,置信度水平达到95%,ICP-MS/MS方法与SF-ICP-MS的对比分析结果无显著性差异.所建立的ICP-MS/MS方法操作简单,分析速率快,准确可靠性好,已用于渣油中多种金属元素的质量评价.
Analysis of Trace Metal Elements in Residual Oils Through Extraction Induced by Emulsion Breaking and ICP-MS/MS
A new strategy for determination of multiple metal elements in residual oils using inductively coupled plasma tandem mass spectrometry(ICP-MS/MS)was proposed based on extraction induced by emulsion breaking(EIEB).The residual oil sample was diluted with xylene to reduce the viscosity,emulsified by Triton X-114 with the mass fraction of 6%,demulsified in ultrasonic water bath for 25 mins;metal elements were extracted from the residual oil into aqueous phase using hydrochloric acid with the volume fraction of 40%.;the contents of 10 metal elements including Na,Mg,Al,Ca,V,Cr,Fe,Ni,Cu,and Zn were determined by ICP-MS/MS.The effect of EIEB conditions on the extraction efficiency of metal elements in residual oils was evaluated in details.In the MS/MS mode,He collision gas or different reaction gases were used to eliminate the spectral interference of metal elements.Moreover,the standard reference materials NIST SRM 1634c(trace elements in fuel oil)was used to evaluate the accuracy of the method.The residual oil samples were processed by microwave digestion and the comparative analysis of results were performed by sector field inductively coupled plasma mass spectrometry(SF-ICP-MS),so as to verify the reliability of the method.The results reveal that the metal elements show a good linear relationship in their respective concentration ranges(with the linearly dependent coefficient no less than 0.9997),the limit of detection(LOD)is 2.05-31.4 ng/L,the determination results of NIST SRM 1634c are basically consistent with the certified values provided by standard reference materials and the reference values reported in literature,the confidence level is 95%,and there is no significant difference in the comparative analysis results of ICP-MS/MS and SF-ICP-MS.ICP-MS/MS has the advantages of simple operation,fast analysis speed,good accuracy and reliability,and has been used for quality evaluation of metal elements in residual oil.

residual oilinductively coupled plasma tandem mass spectrometry(ICP-MS/MS)metal elementextraction induced by emulsion breakingspectral interference

朱乾华、刘宏伟、聂西度

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长江师范学院化学化工学院,重庆涪陵 408100

湖南工学院材料科学与工程学院,湖南衡阳 421002

渣油 电感耦合等离子体串联质谱(ICP-MS/MS) 金属元素 破乳诱导萃取 质谱干扰

国家自然科学基金面上项目湖南省应用特色学科材料科学与工程学科湖南省应用特色学科开放基金项目

21975289湘教通[2018]469号KFB20007

2024

石油学报(石油加工)
中国石油学会

石油学报(石油加工)

CSTPCD北大核心
影响因子:0.764
ISSN:1001-8719
年,卷(期):2024.40(1)
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