微波消解-ICP-MS法测定电解二氧化锰中的微量元素

Determination of Trace Elements in Electro1ytic Manganese Dioxide with Microwave Digestion by ICP-MS

建立电感耦合等离子体质谱法(ICP-MS)测定电解二氧化锰中Pb、Cd、Cr、Ni等微量元素的方法。样品用HNO3+HCl经微波消解后,试液直接用ICP-MS法同时测定上述4种微量元素,以Sc、In、Bi作为内标物质,补偿了基体效应,选择适当的待测元素同位素克服了质谱干扰,确定了实验的最佳测定条件。结果表明,4种微量元素的检出限为0.011～0.078μg/L;回收率为89.33%～112.00%;RSD<2.34%。该法准确、快速、简便,已应用于电解二氧化锰中微量微量元素的测定。

To establish the method for determination of Pb,Cd,Cr and Ni elements in electro1ytic manganese dioxide by inductively coupled plasma mass spectrometry（ICP-MS）.The sample was dissolved by microwave digestion in HNO3＋HCl,the solution was analyzed by ICP-MS.Seclect internal standard elements Sc,In and Bi for the method by which the analyse signal drift is corrected by the signal of another element added to both the standard solution and sample.The influence of mass spectrometry interference has been corrected by selecting different isotope.The optimum conditions for the determination is tested and discussed.The detection limits range from 0.011 μg/L to 0.078 μg/L depending on the elements.Recoveries of samples were of the range 89.33%~112.00% and precision was fine RSD2.34%.This method is accurate,quick-acquired and convenient.It is used in the determination of trace elements in electro1ytic manganese dioxide.