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  被引量:3

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

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作  者:张歌[1] 张榕 曾秋予 降林华[1] ZHANG Ge;ZHANG Rong;ZENG Qiuyu;JIANG Linhua(State Environmental Protection Key Laboratory of Eco-Industry,Chinese Research Academy of Environmental Sciences,Beijing100012,China;School of Materials Science and Engineering,Anhui University of Science and Technology,Huainan 232001,China)

机构地区:[1]中国环境科学研究院国家环境保护生态工业重点实验室,北京100012 [2]安徽理工大学材料科学与工程学院,淮南232001

出  处:《理化检验(化学分册)》2020年第11期1173-1177,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基  金:水体污染控制与治理科技重大专项(2017ZX07402004、2018ZX07701001-7);环境基准与风险评估国家重点实验室经费(SKLECRA201754)。

摘  要: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%.

关 键 词:微波消解 电感耦合等离子体质谱法     锰电解固体溶质 

分 类 号:O657.63[理学—分析化学]

 

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