ICP-AES法测定锰铁中硅和磷方法研究

Studies on the Determination of Silicon and Phosphorus in Ferromanganese by ICP-AES

对ICP AES法测定锰铁中硅和磷的方法进行了研究。对微波消解试样及分析方法的各种参数进行了优化 ,包括溶样酸的选择 ,溶样温度和压力的控制 ,分析谱线的选择 ,试样基体、分析酸度和干扰元素对测定结果的影响。通过各种分析参数的优化选择实现了锰铁中硅和磷的同时测定 ,取得了满意的效果。线性相关系数 :Si=0 9998,P =0 9996 ,检测限为 :Si 0 0 0 6 0 % ,P 0 0 30 % ,硅的加标回收率在 97 0 %～10 1%。分析方法准确快速 ,试剂用量少 ,线性范围宽 ,适用于低碳、中碳及高碳锰铁中硅、磷的测定。

An ICP-AES method for the determination of silicon and phosphorus in ferromanganese was studied. Digesting samples by microwave and all kinds of parameters of the analytical method were optimized, which included selecting the acid and controlling the temperature and pressure of dissolving the sample, confirming analytical spectrum, considering the effect of sample matrix, analytical pH and disturbing elements on the determination results. By optimizing and choosing all kinds of condition parameters, the simultaneous determination of silicon and phosphorus was realized and satisfactory results were obtained. The linear correlation coefficients of Si and P were 0.999 8 and 0.999 6, respectively. The detection limit for silicon was 0.006 0% with recovery of 97.0%-101%. The detection limit for phosphorus was 0.030%. This method is accurate and quick with less reagent dosage and broad linear range. The way of this determination is fit for the determination of silicon and phosphorus with low, middle and high carbon contents.