摘要
建立了微波消解一电感耦合等离子体质谱法（ICP—MS）同时测定高纯镍板中Si，P，Fe，Cu，Zn，As，Cd，Sn，Sb，Pb，A1，Mn，Mg等13种痕量元素的方法。试验考察了微波消解条件、基体效应、质谱干扰，并对ICP离子源以及质谱仪的检测条件和微波消解参数进行了优化。结果表明，以硝酸为消解试剂，采用斜坡升温方式能完全消解试样；以基体匹配法或以Sc，Rh作为内标元素可以消除基体效应的影响，通过选择适宜待测元素的同位素或选用干扰元素校正方程可以克服质谱干扰。方法用于测定高纯镍板中13种痕量元素，检出限范围为0．01～O．05μg／L，加标回收率为92．0％～112．0％，相对标准偏差均小于8．5％；方法测定值与其他方法对照，结果相吻合。
A method for simultaneous direct determination of thirteen trace elements in high-purity nickel including Si, P, Fe, Cu, Zn, As, Cd, Sn, Sb, Pb, A1, Mn, Mg by inductively coupled plasma mass spectrometry （ICP-MS） with microwave digestion has been established. The conditions of microwave digestion, the matrix effect and spectral interferences were investigated, and the operating parameters of the ICP ionization source, mass spectrometry and microwave digestion were optimized. It was found that the matrix effect could be eliminated by matching matrix or selecting Se,Rh as internal standard element and the spectral interference could be calibrated by selecting different isotope or correction equation of interference elements. The detection limits range of the method is from 0.01 to 0.05μg/L for thirteen trace elements. The precision and recovery tests were made and the results obtained were as follows： the recoveries in the range 92.0%--112.0% and RSD 〈8.5 %. The determination results of actual samples are consistent with those obtained by other methods.
出处
《冶金分析》
CAS
CSCD
北大核心
2008年第3期9-13,共5页
Metallurgical Analysis
