ICP-AES法测定碳化铌中杂质元素

Determination of Impurity Elements in Niobium Carbide by ICP-AES Method

用硝酸-氢氟酸在电热消解仪上溶解试样,采用碳化铌作为配制标准工作曲线的基体,用以消除基体对杂质元素的光谱干扰。在ICP-AES仪器上制作标准工作曲线并测量碳化铌中铁、硅、铝、锰、钛、钴、锡、铬、钙、钼、钨11个杂质元素。该方法的检出限为0.4-4.8μg/g,加标回收率为96.8%-106%,精密度RSD〈10%。结果表明该方法简便快速,检出限低,准确度和重现性好,适用于生产分析。

Niobium carbide samples were dissolved in nitric acid and hydrofluoric acid on electric heating digestion apparatus, and niobium carbide was used as reference material for standard working curve so as to eliminate the spectral interference to impurity element from the matrix. The standard working curve was created by using ICP-AES instrument and the contents of 11 impurity elements in the niobium carbide sample including iron, silicon, aluminum, manganese, titanium,cobalt, tin, chromium, calcium, molybdenum and tungsten were determined. The detection limit of the method is 0.4~4.8 μg/g,the standard addition recovery reaches 96.8%~106%, and the relative standard deviation is less than 10%. The results show that the method is simple and rapid with low detection limit, high accuracy and good reproducibility, which is suitable for the analysis of production.