电感耦合等离子体原子发射光谱法测定钴产品生产过程净化液中12种微量元素

钴产品生产过程CoCl₂净化液和Co(NO₃)₂净化液中含有大量钴离子,一般采用基体匹配原子吸收光谱法或萃取分离-分光光度法测定其中Cu、Fe、Ni、Cd、Zn、Mn、Ca、Mg、Na、Si、As、S等12种杂质元素。但是此类方法分析时间长、操作繁琐、费用高,而且只能进行单一元素测定。实验提出了采用电感耦合等离子体原子发射光谱法(ICP-AES)测定钴产品生产过程净化液中以上目标元素,在优化的仪器工作条件下,使用内标法有效地克服了基体效应及仪器波动所产生的影响。各元素校准曲线的线性相关系数均大于0.9999;方法检出限为0.00003~0.00026g/L。按照实验方法测定钴产品生产过程CoCl₂净化液和Co(NO₃)₂净化液两个体系中Cu、Fe、Ni、Cd、Zn、Mn、Ca、Mg、Na、Si、As、S,结果的相对标准偏差(RSD,n=11)为2.8%~8.9%,加标回收率为93%~107%。实验方法用于Co光谱分析标准样品中Cu、Fe、Ni、Cd、Zn、Mn、Mg、Si、As的测定,测定值与认定值相一致。

Determination of twelve microelements in purified solution duringproduction process of cobalt products by inductively coupledplasma atomic emission spectrometry

The cobalt chloride purified solution and cobalt nitrate purified solution during production process of cobalt products contained a lot of cobalt ions. Usually,12 impurity elements in it, including Cu, Fe, Ni, Cd, Zn, Mn, Ca, Mg, Na, Si, As and S, were determined by matrix matching-atomic absorption spectrometry or extraction separation-spectrophotometry. However, these methods had some disadvantages such as long analytical time, complicated operation and high cost. Moreover, only single element could be determined at one time. Thus, inductively coupled plasma atomic emission spectrometry (ICP-AES) was proposed for determination of these elements in purified solution during production process of cobalt products. Under the optimized working conditions of instrument, the influence of matrix effect and instrumental fluctuation could be effectively overcome with internal standard method. The linear correlation coefficients of calibration curves of elements were all higher than 0.999 9. The detection limits of method were between 0.00003g/L and 0.00026g/L. The contents of Cu, Fe, Ni, Cd, Zn, Mn, Ca, Mg, Na, Si, As and S in two systems during production process of cobalt products, i.e., cobalt chloride purified solution and cobalt nitrate purified solution, were determined according to the experimental method. The relative standard deviations (RSD, n=11) of determination results were between 2.8% and 8.9%. The recoveries were between 93% and 107%. The proposed method was applied for determination of Cu, Fe, Ni, Cd, Zn, Mn, Ca, Mg, Na, Si, As and S in cobalt certified reference material for spectral analysis. The results were consistent with the certified values.