电感耦合等离子体原子发射光谱(ICP-AES)法测定工业电解质中钙、镁、锂

Determination of Ca,Mg and Li in Industrial Electrolyte by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

工业电解质中微量元素钙、镁、锂对电解槽的正常运行非常重要。采用高氯酸加热挥发除氟,以盐酸(1+1)溶解残渣,选用Ca 317.9nm、Mg 297.5nm、Li 670.7nm作为分析谱线,考察了样品处理方法、共存元素对测定结果的影响。建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定工业电解质中钙、镁、锂的方法。结果表明:不同的电解质因其所含氧化铝的不同会有部分不溶杂质,但对微量元素的测定影响很小,可以忽略不计。共存元素铝和钠不干扰微量元素的测定。按照实验方法对2个电解质标准样品进行了测定,其测定值与标准值吻合。同时对不同电解槽的工业电解质样品进行了分析,其结果的相对标准偏差(RSD,n=11)在0.69%~5.7%,满足生产分析的需要。

The content of calcium,magnesium and lithium in industrial electrolytes are very important for the normal operation of electrolytic cells.In this paper,fluoride was removing by adding the perchlorate acid which has the function of removing fluoride under heating,then the residue was dissolved using hydrochloric acid（1＋1）.Lines of Ca 317.9 nm,Mg 297.5 nm,and Li 670.7 nm were selected as the analytical spectral lines.The influence of the sample processing method and the interference of the coexistence element on the measurement results were investigated.The determination method of Ca,Mg,and Li in industrial electrolyte by ICP-AES was established.Results showed that different electrolytes hadsome insoluble impurities because of their different alumina,but the determination of trace elements was small and negligible.Coexistence element Al and Na did not interfere with trace elements determination.According to the test method,the determination of two electrolyte standard samples was consistent with the given value.At the same time,the content of Ca,Mg,and Li in the different industrial electrolyte samples were determined.Relative standard deviation of（RSD,n=11）0.69% and 5.7% was obtained,which met the needs for production analysis.