微波消解-电感耦合等离子体质谱法测定锰电解固体溶质中铜、锌、钼和锑

Determination of Copper,Zinc,Molybdenum and Antimony in Manganese Electrolysis Solid Solute by ICP-MS with Microwave Digestion

采用体积比为1∶1的30%过氧化氢溶液-硝酸微波消解锰电解固体溶质,采用电感耦合等离子体质谱法(ICP-MS)测定其中标准电极电位高于锰的4种金属元素(铜、锌、钼和锑)的含量,待测元素同位素选择63Cu、66Zn、98 Mo和121Sb,加入45Sc和115In分别消除铜和锌及钼和锑的信号漂移。结果显示,4种元素的质量浓度均在0.1~500μg·L^-1内与其对应的响应值呈线性关系,相关系数均为0.9999,检出限(3s)分别为0.0030,0.0220,0.0010,0.0130μg·L^-1。按标准加入法进行回收试验,回收率为95.0%~103%,测定值的相对标准偏差(n=10)不大于2.0%。

The sample of manganese electrolysis solid solute was degested with a mixture composed of 30%hydrogen peroxide solution and nitric acid at a volume ratio of 1∶1by microwave,and the contents of 4metal elements,copper,zinc,molybdenum and antimony with their standard electrode potential more positive than that of manganese,in the degestion solution were determined by ICP-MS.63 Cu,66Zn,98 Mo and 121Sb were selected as isotopes of the 4elements;45Sc was added to eliminate the signal drift of copper and zinc,and 115In was added to eliminate the signal drift of molybdenum and antimony,respectively.The results showed that a linear relationship between mass concentration of 4elements and their corresponding response values was kept in the range of 0.1-500μg·L^-1,with correlation coefficients all over 0.9999.Detection limits(3s)found were 0.0030,0.0220,0.0010,0.0130μg·L^-1 respectively.Recovery test was made by standard addition method,giving values of recovery in the range of 95.0%-103%,with RSDs(n=10)of the measured values all lower than 2.0%.