采用盐酸或硝酸溶解稀土产品样品或分取适量体积稀土生产流程中间控制样品后,加入草酸沉淀稀土元素,然后用高氯酸消除过量的草酸,采用电感耦合等离子体原子发射光谱法(ICP-AES)根据不同的基体,分别采用Al 396.153 nm、Al 237.373 nm为分析谱线测定溶液中的铝。铝的线性范围为0.10~5.0 mg·L-1,检出限在3.1~3.5 mg·kg-1之间,测定下限在15.5~17.5 mg·kg-1之间。加标回收率在85.0%~110%之间,测定值的相对标准偏差(n=11)小于9.0%。本方法用于测定稀土产品和中间控制样品中的铝,测定结果与ICP-MS和分光光度法的结果相吻合。

After the rare earth product samples were dissolved with hydrochloric acid or nitric acid, or the appropriate amount of the intermediate control samples in the production process was taken, oxalic acid was added into the solution to precipitate the rare earth elements. Then perchloric acid was added into the solution to eliminate the excessive oxalic acid and aluminium in the solution was determined by ICP-AES with Al 396.153 nm or Al 237.373 nm as the analytical spectral line dependent on the matrix. The linearity range of aluminium was 0.10-5.0 mg·L-1, with detection limits in the range of 3.1-3.5 mg·kg-1, and the lower limits of determination in the range of 15.5-17.5 mg·kg-1. Recovery rates obtained by standard addition method were in the range of 85.0%-110% and RSDs (n=11) were less than 9.0%. The proposed method was used to determine aluminium in rare earth products and the intermediate control samples, giving results in consistent with those obtained by ICP-MS and spectrophotometry.