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机构地区:[1]湖南工学院化学化工系,湖南衡阳421002 [2]南华大学化学化工学院,湖南衡阳421001 [3]中南大学化学化工学院,湖南长沙410083
出 处:《冶金分析》2009年第7期14-18,共5页Metallurgical Analysis
基 金:湖南省自然科技基金资助项目(05JJ40017)
摘 要:建立了电感耦合等离子体质谱(ICP—MS)测定渣油中Na,Mg,Al,Ca,V,Mn,Fe,Co,Ni,Cu,Zn,Pb等微量元素的分析方法。设计了渣油样品的优化微波消解程序;考察了渣油中12种微量元素的质谱干扰情况及可能的消除方法,选择适当的待测元素同位素克服了质谱干扰;以Sc、Y、Bi作为内标物质,校正信号漂移并补偿基体效应。结果表明,在优化的实验条件下,12种微量金属元素的检出限在0.001~2.035μg/L之间;线性关系良好,线性相关系数r≥0.9986;精密度良好,RSD〈2.3%;回收率在91%~106%之间。A method is established for the determination of Na, Mg, Al, Ca, V, Mn, Fe, Co, Ni, Cu, Zn and Ph in residual oil by inductively coupled plasma mass spectrometry (ICP-MS). An optimum micro-wave systerm is designed for sample digestion. The mass spectrum interference of twelve micro elements in residual oil and possible method for eliminating the interference have also been investigated in detail. The interferences of mass spectrum are minimized or eliminated by selecting different isotope. Internal standard elements such as Sc, Y and Bi are selected for correcting the drift of analytical signals. Under optimum conditions, the detection limits of the twelve elements are found as from 0. 001 μg/L to 2. 035 μg/L. The linear correlation coefficient r≥0. 998 6, demonstrating a good linear relationship. The precision is high (RSD〈2.3%) and the recoveries are 91%--106%.
关 键 词:渣油 微波消解 电感耦合等离子体质谱 微量金属元素 内标元素
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