电感耦合等离子体原子发射光谱法测定铝质耐火材料中钙、镁、铁、钛及钾的含量

ICP-AES Determination of Calcium,Magnesium,Iron,Titanium and Potassium in Alumina Refractories

样品用碳酸锂-硼酸(2+1)混合熔剂熔融,盐酸(1+1)溶液浸取,电感耦合等离子体原子发射光谱法直接测定铝质耐火材料中钙、镁、铁、钛、钾五元素。优化了仪器参数和分析谱线,采用基体匹配法并应用仪器软件中的谱线干扰校正程序有效消除铝基体的干扰。对不同含量的2个试样进行精密度试验,测定结果的相对标准偏差(n=10)小于4.0%,该方法的检出限(3S/N)为0.004～0.06 mg·L^(-1)。对铝质耐火材料标准样品进行测定,结果与标准值相符。

Sample of alumina refractory was fused with a mixture of Li2CO3 and boric acid （2＋1）, and the melt was dissolved in HCI （1＋1）. An aliquot of the sample solution was taken and used for ICP-AES determination of contents of Ca, Mg, Fe, Ti and K after dilution to a definite volume. Working conditions of the instrument and choice of the analytical spectral lines were studied and optimized. The matrix interference was eliminated by the matrix-matching method and by using the program of spectral interference correction given in the software of the instrument. Precision of the method was tested on 2 samples with different contents of the 5 elements for 10 determinations, values of RSD＇s found were all less than 4%. Values of detection limit （3S/N） found for the 5 elements were in the range from 0. 004--0. 06 mg·L^-1. The proposed method was used in the analysis of standard samples giving results in consistency with the standard values.