电感耦合等离子体原子发射光谱法测定低碳低钛硅铁中痕量铌钒锆

采用硝酸、氢氟酸和高氯酸冒烟溶解样品,选取Nb 322.548nm、V 310.230nm和Zr 319.418nm为分析谱线,采用基体匹配法配制标准溶液系列并绘制校准曲线消除基体效应的影响;使用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定铌、钒和锆,从而建立低碳低钛硅铁中铌、钒和锆的测定方法。共存元素的干扰校正试验表明,样品中共存元素对待测元素无干扰影响。各待测元素校准曲线的线性相关系数均大于0.9995;各元素的检出限分别为0.0006%,0.0005%和0.0005%。实验方法应用于低碳低钛硅实际样品中铌、钒、锆的测定,结果的相对标准偏差(RSD,n=10)为1.2%~4.7%,回收率为98%~104%。按实验方法测定低碳低钛硅铁样品中铌、钒、锆,测定结果与YB/T 4395—2014、GB/T 223.14—2000和GB/T 223.30—1994测定值相符。

Determination of trace niobium,vanadium and zirconium in low carbon and low titanium ferrosilicon by inductively coupled plasma atomic emission spectrometry

The sample was dissolved with nitric acid, hydrofluoric acid and perchloric acid fuming. Nb 322.548nm, V 310.230nm and Zr 319.418nm were selected as the analytical lines. The standard solution series were prepared by matrix matching method to plot the calibration curve and eliminate the influence of matrix effect. The simultaneous determination method of niobium, vanadium and zirconium in low carbon and low titanium ferrosilicon by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The interference correction tests of coexisting elements showed that the coexisting elements in sample had no influence on the testing elements. The linear correlation coefficients of calibration curves were all higher than 0.9995. The detection limit of niobium, vanadium and zirconium was 0.0006%, 0.0005% and 0.0005%, respectively. The experimental method was applied for the determination of trace niobium, vanadium and zirconium in actual low carbon and low titanium ferrosilicon samples. The relative standard deviations (RSD, n=10) of measured results were between 1.2% and 4.7%. The recoveries were between 98% and 104%. The contents of niobium, vanadium and zirconium in low carbon and low titanium ferrosilicon sample were determined according to the experimental method, and the found results were consistent with those obtained by YB/T 4395-2014, GB/T 223.14-2000 and GB/T 223.30-1994.