多谱线拟合-电感耦合等离子体原子发射光谱法测定高纯镍中痕量钴  

Multi-spectral Fitting-Determination of Trace Cobalt in High Purity Nickel by Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：严子心 曲景奎[1,2] 余志辉[1,2] 宋静[1,2] 魏广叶[1,2] YAN Zi-Xin;QU Jing-Kui;YU Zhi-Hui;SONG Jing;WEI Guang-Ye(National Engineering Laboratory for Hydrometallurgical Cleaner Production Technology,Beijing 100190,China;Key Laboratory of Green Process and Engineering,Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院过程工程研究所湿法冶金清洁技术国家工程实验室,北京100190 [2]中国科学院过程工程研究所绿色过程与工程重点实验室,北京100190 [3]中国科学院大学,北京100049

出　　处：《分析化学》2019年第3期423-428,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.51704270);中国科学院科技服务网络计划STS计划项目(No.KFJ-STS-ZDTP-040)资助~~

摘　　要：采用基体匹配、标准加入和多谱线拟合(MSF)等校正方法进行干扰消除,通过对3种校正方法的比较,建立了MSF-电感耦合等离子体原子发射光谱(ICP-AES)测定高纯镍中痕量钴的分析方法。确定了最优仪器参数为:射频功率1350 W,雾化器流速0.5 L/min,观测距离15 mm,蠕动泵泵速1.0 mL/min。应用基体匹配、标准加入和MSF3种校正方法分别测定了加标高纯镍溶液,当钴加标浓度为0.10和0.20 mg/L、镍浓度为5 g/L时,3种方法均得到较高的回收率(95.0%～102.0%),线性相关系数均大于0.9996,RSD在2.1%～4.6%之间,其中MSF法的线性范围最宽(0.02～0.5 mg/L),检出限最低(0.002 mg/L);当钴加标浓度分别为0.02和0.06 mg/L、镍浓度为15 g/L时,只有MSF法能够得到准确的结果,线性相关系数为0.9999,线性范围为0.02～0.10 mg/L,检出限为0.002 mg/L,回收率为95.0%～105.0%,RSD在3.9%～4.6%之间。采用MSF法测试实际样品的分析结果为0.000154%,与辉光放电质谱(GD-MS)法的结果(0.000149%)基本一致,进一步验证了方法的准确性和精密性。MSF法不仅抗干扰能力强、操作简便、经济实用,且精密度高、检出限低,测量下限(0.0001%)和范围均优于国标原子吸收光谱法(0.001%),为高纯样品中痕量杂质元素的测定提供了重要的方法学手段。By comparing the methods of matrix matching and standard addition and multi-spectral fitting(MSF)for elimination of interference,an analytical method for the determination of trace cobalt in high purity nickel by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The optimum parameters of the instrument were determined as follows:RF power of 1350 W,atomizer velocity of 0.5 L/min,observation distance of 15 mm,and peristaltic pump speed of 1.0 mL/min.Three calibration methods,matrix matching,standard addition and MSF,were used to determine the standard addition of pure nickel solution.When the standard addition concentrations were 0.10 and 0.20 mg/L,and nickel concentration was 5 g/L,the three methods all could get good recovery.The linear correlation coefficients were all greater than 0.9996,the recoveries were 95.0%-102.0%,and the RSDs were 2.1%-4.6%.The linear range of MSF method was the best(0.02-0.5 mg/L)and the detection limit was the lowest(0.002mg/L).When the standard addition concentrations of nickel were 0.02 and 0.06 mg/L and the nickel concentration was 15 g/L,the results showed that only the MSF method could get accurate results with linear correlation coefficient of 0.9999,linear range of 0.02-0.1mg/L,detection limit of 0.002mg/L,recoveries of 95.0%-105.0%,and RSDs of 3.9%-4.6%.The MSF method was used to test the actual samples.The analytical results were 0.000154%,which was consistent with the GD-MS method.The RSD was 2.3%.The accuracy and precision of the method were further verified.MSF method is not only strong in anti-interference,simple in operation,economical and practical,but also has high precision,low detection limit.The lower limit of detection(0.0001%)and detection range are superior to the national standard atomic absorption spectrometry(0.001%).It provides an important methodological method for the determination of trace impurities in high-purity samples.

关 键 词：电感耦合等离子体原子发射光谱法 高纯镍 钴 多谱线拟合 

分 类 号：O657.31[理学—分析化学]