摘要
采用硝酸+盐酸混合酸消解体系对锰酸锂样品进行微波消解处理制样,用电感耦合等离子体质谱(ICP-MS)法同时测定锰酸锂中Na,Mg,Al,K,Ca,Ti,Cr,Fe,Cu,Zn,As,Ag,Cd,Pb共14种杂质元素的含量。详细研究了质谱干扰影响及校正,选用Sc,Rh,Tl作内标元素校正基体效应和信号漂移,对14种待测元素的检出限为0.007～0.209μg.L-1,通过添加标准进行加标回收,所有待测元素的回收率在92.66%～108.34%之间,相对标准偏差(RSD)均小于4.80%,结果准确可靠。该法可为锰酸锂中杂质元素的快速检测提供科学依据。
Samples of LiMn2O4 were digested by microwave digestion, and impurity elements amounts of Na, Mg, A1, 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 ＋ HC1 in a closed-vessel microwave system. The effects of mass spectrum interference were studied. Sc, Rh and T1 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 μg.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.
出处
《光谱学与光谱分析》
SCIE
EI
CAS
CSCD
北大核心
2013年第5期1350-1353,共4页
Spectroscopy and Spectral Analysis
基金
国家自然科学基金项目(20971129)
重庆市教委科学技术研究项目(KJ121311)资助
关键词
锰酸锂
电感耦合等离子体质谱
微波消解
杂质元素
LiMr2O4
Inductively coupled plasma mass spectrometry
Microwave digestion
Impurity elements
