电感耦合等离子体原子发射光谱法测定钒铁中18种元素  

Determination of eighteen elements in ferro-vanadium by inductively coupled plasma atomic emission spectrometry

作　　者：成勇[1] 

机构地区：[1]攀钢集团研究院有限公司,四川成都611731

出　　处：《冶金分析》2011年第11期48-53,共6页Metallurgical Analysis

摘　　要：用盐酸、硝酸消解样品,以电感耦合等离子体原子发射光谱法(ICP-AES)同时测定50钒铁和80钒铁中微量杂质元素Ti、W、Si、Mo、Co、Cr、Ni、Cu、Pb、Cd、As、Sn、P、Mn、Ca、Mg、Zn以及80钒铁中的基体元素Fe。考察了样品基体V、Fe以及共存元素之间的干扰影响,优选了元素分析谱线、背景校正位置和仪器工作参数。采用基体匹配和同步背景校正相结合的方式消除钒铁基体对试液雾化传输、ICP平衡与激发和元素测定的各种干扰影响因素。用本法测定80钒铁中上述元素的结果表明:方法检出限为5～55μg/L,背景等效浓度为5～95μg/L,回收率在94.0%～106.0%之间,元素含量大于1.0%时RSD<0.86%,元素含量大于0.001%而小于0.10%时RSD<7.2%,元素含量大于0.10%而小于1.0%时RSD<1.4%。方法用于测定标准样品,其测定值与认定值一致。After the sample was digested with hydrochloric acid and nitric acid,micro amounts of impurities including Ti,W,Si,Mo,Co,Cr,Ni,Cu,Pb,Cd,As,Sn,P,Mn,Ca,Mg and Zn in 50 ferro-vanadium and 80 ferro-vanadium,and matrix Fe in 80 ferro-vanadium were simultaneously determined by inductively coupled plasma atomic emission spectrometry（ICP-AES）.The interferences of matrixes（Fe and V） and coexisting elements in sample were investigated.The analytical lines,background correction position and instrumental working parameters were optimized.The influence of matrixes（Fe and V） on sample solution atomization transmission,ICP equilibrium and excitation as well as determination was eliminated by combining matrix matching and synchronous background correction.The proposed method was used in the simultaneous determination of elements above in 80 ferro-vanadium.The results showed that the detection limit of the method was 5-55 μg/L,the background equivalent concentration was 5-95 μg/L,and the recoveries were 94%-106%.When the content of element was higher than 1.0 %,the RSD was less than 0.86 %.When content of element was between 0.001 % and 0.10 %,the RSD was less than 7.2 %.When the content of element was in range of 0.10 %-1.0 %,the RSD was less than 1.4 %.This method was applied to the determination of certified reference materials,and the found results were consistent with the certified values.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 钒铁 铁 微量元素 基体匹配 同步背景校正 

分 类 号：O657.31[理学—分析化学]