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硫酸根

为了准确测定钴产品生产过程CoCl₂净化液和Co(NO₃)₂净化液中的SO^2-₄含量,研究了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CoCl₂净化液和Co(NO₃)₂净化液中SO^2-₄含量的方法及其影响因素。选择S 180.669nm作为分析谱线,考察了射频发生功率、雾化气流量、辅助气流量、溶液酸度和基体钴对测定的影响。基体效应通过基体匹配法绘制校准曲线的方法消除。试液中钴的质量浓度为20.0g/L时,SO^2-₄的检出限达0.0008g/L。用实验方法测定钴产品生产过程净化液中SO^2-₄,结果的相对标准偏差(RSD,n=11)为8.4%和6.7%;加标回收率为93%~107%。实验方法用于氧化亚镍、四氧化三钴中S(以SO^2-₄计)的测定,结果与标准方法YS/T 710.3—2009测定值基本一致。

Determination of sulfate in purification liquid for cobalt productionby inductively coupled plasma atomic emission spectrometry

In order to accurately determine the content of sulfate (SO^2-₄) in purification liquid for cobalt production CoCl₂ and Co(NO₃)₂], the determination method and influencing factors by inductively coupled plasma atomic emission spectrometry (ICP-AES) were studied. S 180.669nm was selected as the analytical line. The effect of radio frequency generation power, atomizing gas flow, auxiliary gas flow, solution acidity and cobalt matrix on determination was investigated. The matrix effect could be eliminated by matrix matching method to prepare the calibration curve. When the mass concentration of cobalt in sample solution was 20.0g/L, the detection limit of SO^2-₄ was 0.0008g/L. The proposed method was applied to the determination of SO^2-₄ in purification liquid for cobalt production. The relative standard deviation (RSD, n=11) was 8.4% and 6.7%, respectively. The spiked recoveries were between 93% and 107%. The experimental method was used for the determination of S (in SO^2-₄) in nickel protoxide and cobaltosic oxide. The found results were basically consistent with those obtained by standard method YS/T 710.3-2009.