高分辨电感耦合等离子体质谱法测定电池锌粉中杂质元素  

Determination of impurity elements in zinc powder of battery by high resolution inductively coupled plasma mass spectrometry

作　　者：周学忠[1] 聂西度[2] 谢华林[1,2] 

机构地区：[1]湖南工学院化学化工系,湖南衡阳421008 [2]中南大学化学化工学院,湖南长沙410083

出　　处：《冶金分析》2010年第8期12-16,共5页Metallurgical Analysis

基　　金：湖南省教育厅科研资助重点项目(09A021)

摘　　要：应用高分辨电感耦合等离子体质谱法（HR-ICP-MS）测定电池锌粉中Mg、Mn、Fe、Co、Ni、Cu、As、Mo、Cd、Sb、Pb、Bi 12种痕量元素。考察了试样消解时引入的氯离子、试样中基体锌和共存元素对被测元素的影响及其消除方法。结果表明,高浓度氯离子对Bi、Cd、Mn、Mg、Fe的信号产生抑制作用,但其浓度小于5%时影响较小,因此可以通过控制试液中氯离子浓度来减少氯离子的影响;基体锌和其他共存元素的质谱干扰可以根据被测元素选择不同的质谱分辨率来克服;基体锌的质量浓度达到100 mg/L时,所有被测元素均受基体效应影响,但可以通过选择合适的内标元素进行校正。Bi的检出限为0.003μg/L,Fe的检出限为0.25μg/L,其它10种痕量元素的检出限在0.012~0.074μg/L之间。方法用于电池锌粉12个微量元素的测定,测定结果与其他方法（ICP-AES、GF-AAS、HG-AAS）相符,加标回收率在94.0%~108.6%之间,相对标准偏差（RSD）小于4.2%。Twelve trace elements in zinc powder of battery including Mg,Mn,Fe,Co,Ni,Cu,As,Mo,Cd,Sb,Pb and Bi were determined by high resolution inductively coupled plasma mass spectrometry（HR-ICP-MS）.The effect of chlorine ion introduced in the digestion of sample,matrix zinc and coexisting elements in the sample on the determination and the elimination method were studied.The results showed that the high-concentration chlorine ion had inhibitory effect to the signal generation of Bi,Cd,Mn,Mg and Fe.However,when its concentration was smaller than 5 %,the effect was trivial.Therefore,the effect of chlorine ion could be reduced by controlling its concentration in sample solution.The mass spectrometric interference of matrix zinc and coexisting elements could be overcome by selecting the resolution of testing elements.When the mass concentration of matrix zinc was above 100 mg/L,all testing elements were interfered by the matrix effect.However,the matrix effect could be corrected by selecting proper internal standard element.The detection limits of Bi and Fe were 0.003 μg/L and 0.25 μg/L,respectively.The detection limits of other ten trace elements were 0.012-0.074 μg/L.The proposed method has been applied to the determination of twelve trace elements in zinc powder of battery.The results were consistent with those obtained by other methods（ICP-AES,GF-AAS and HG-AAS）.The recovery rate was 94.0 %-108.6 %,and the relative standard deviation（RSD） was smaller than 4.2 %.

关 键 词：电池锌粉 高分辨电感耦合等离子体质谱法 痕量元素 质谱干扰 基体效应 

分 类 号：TG115.337[金属学及工艺—物理冶金]