Zhu Qian-Hua
College of Chemistry and Chemical Engineering, Yangtze Normal University, Chongqing 408100, China.
Guang Pu Xue Yu Guang Pu Fen Xi. 2013 May;33(5):1350-3.
Samples of LiMn2O4 were digested by microwave digestion, and impurity elements amounts of Na, Mg, Al, K, Ca, Ti, Cr, Fe, Cu, Zn, As, Ag, Cd and Pb in sample solutions were determined by inductively coupled plasma mass spectrometry (ICP-MS). Sample preparation was achieved by digestion with HNO3 + HCl in a closed-vessel microwave system. The effects of mass spectrum interference were studied. Sc, Rh and Tl as internal standard elements were used to compensate matrix effect and signal drift. Under the optimal conditions, the detection limits of the 14 elements are in the range of 0.007-0.209 microg x L(-1). The recovery was 92.66%-108.34% by adding standard recovery experiment, and the relative standard deviation (RSD) was less than 4.80% for all the elements. This method was simple, sensitive and precise, which could satisfy the sample examination request and provide scientific rationale for determining impurity elements of LiMn2O4.
采用微波消解的方法对LiMn₂O₄样品进行消解,利用电感耦合等离子体质谱仪(ICP-MS)测定样品溶液中Na、Mg、Al、K、Ca、Ti、Cr、Fe、Cu、Zn、As、Ag、Cd和Pb等杂质元素的含量。通过在密闭容器微波系统中用HNO₃ + HCl进行消解来制备样品。研究了质谱干扰的影响。使用Sc、Rh和Tl作为内标元素来补偿基体效应和信号漂移。在最佳条件下,14种元素的检出限在0.007 - 0.209 μg·L⁻¹范围内。通过加标回收实验,回收率为92.66% - 108.34%,所有元素的相对标准偏差(RSD)均小于4.80%。该方法简便、灵敏、准确,能够满足样品检测要求,为测定LiMn₂O₄中的杂质元素提供科学依据。