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建立了采用电感耦合等离子体原子发射光谱法(ICP-OES)同时测定钒电池级固体硫酸氧钒中8种关键杂质含量的分析方法,检测范围包括0.001%~0.100%铁铬镍和0.005%~0.100%钾钠钙硅铝。试验考察了样品中高钒基体和硫酸根离子共存体系下基体效应、光谱干扰以及连续背景叠加等影响因素对痕量杂质测定的干扰。研究得到:硫酸根离子对测定无影响,高浓度钒离子的基体效应或连续背景叠加对钾钠产生负干扰,对砷钴铁镍等其余杂质元素产生正干扰的试验结论,并且方法采用基体匹配法和同步背景校正法相结合方式消除高钒基体对杂质测定的影响。通过光谱干扰试验分类归纳总结了钒基体对杂质元素的光谱干扰情况,并且优选了元素分析谱线、背景校正区域以及光谱仪工作条件。分析方法的技术性能达到:背景等效浓度-0.000 3%~0.000 3%,元素检出限0.000 1%~0.000 3%,含量在0.001%~0.007%范围内RSD<10%,回收率91.0%~110.0%。
A method for the simultaneous determination of 8 key impurities in Vanadium Sulfate Vanadium Sulfate by inductively coupled plasma atomic emission spectrometry (ICP-OES) was established. The detection range includes 0.001% ~ 0.100% Fe-Cr-Ni and 0.005% 0.100% potassium soda lime silica alumina. The influence of substrate factors such as high vanadium matrix and sulfate ion coexistence system, spectral interference and continuous background superposition on the determination of trace impurities was investigated. The results show that the sulfate ion has no effect on the determination, the matrix effect of high-concentration vanadium ions or the continuous background superimposition negatively interferes with potassium-sodium, and produces the positive interference of other impurity elements such as arsenic, cobalt, iron-nickel and the like. Method and the synchronous background correction method to eliminate high vanadium matrix on the determination of impurities. The spectral interferences of vanadium matrix on the impurity elements were summarized and classified according to the spectral interference test, and the working conditions of the elemental analysis line, the background correction area and the spectrometer were optimized. The technical performance of the analytical method was as follows: background equivalent concentration -0.000 3% to 0.000 3%, elemental detection limit 0.000 1% to 0.000 3%, RSD <10% in the range of 0.001% to 0.007% and the recovery rate of 91.0% ~ 110.0%.