电感耦合等离子体原子发射光谱法测定粗硒物料中17种杂质元素

建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定粗硒物料中铝、铋、镉、钴、铬、铜、铁、镓、铟、镁、锰、镍、铅、碲、钛、钒、锌17种杂质元素的定量分析方法。样品用硝酸-盐酸(V(硝酸)∶V(盐酸)= 5∶10)溶解,在少量硫酸存在下,以盐酸-氢溴酸混合酸挥发除硒,加热冒尽硫酸烟后在15%(V/V)盐酸-硝酸混合酸V(硝酸)∶V(盐酸)= 3∶1]介质中测定。因为不需要在挥发炉中挥硒,所以操作简单,硒挥发率高,测定元素无挥发损失,且样品中残存硒及共存元素不干扰测定。方法的检出限为0.000 2～0.179 4 μg/mL,测定下限为0.1～15.0 μg/g,各元素质量浓度为0～10 μg/mL时,校准曲线的相关系数r≥0.999 9。方法用于粗硒样品中上述17种杂质元素的测定,测定值与有色金属行业标准分析方法的测定值一致,平均回收率在92%～112%之间,相对标准偏差(RSD,n=7)除含量较低的Cd,Co,Cr,Ga,In,V痕量元素外,其他元素均小于10%。

Determination of seventeen impurity elements in crude selenium materials by inductively coupled plasma atomic emission spectrometry

A quantitative analysis method for the determination of seventeen impurity elements(including aluminum, bismuth, cadmium, cobalt, chromium, copper, iron, gallium, indium, manganese, magnesium, nickel, lead, tellurium, vanadium, titanium and zinc) in crude selenium materials by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The sample was dissolved with mixed acid of nitric acid and hydrochloric acid (V (HNO₃)∶V (HCl)=5∶10). Selenium was volatilized and removed using mixed hydrochloric acid-hydrobromic acid in presence of little sulfuric acid. After removing sulfuric acid fume by heating, the solution was determined in 15 %(V/V) hydrochloric acid-nitric acid mixed medium(V (HNO₃)∶V (HCl)=3∶1). Since the volatilization of selenium was not conducted in volatilizing furnace, the operation was simple and the volatilization efficiency was high. The testing elements had no volatilization loss. Moreover, the residual selenium and coexisting elements had no interference in the determination. The detection limit of method was 0.000 2-0.179 4 μg/mL, and the limit of quantitation was 0.1-15.0 μg/g. The correlation coefficient of calibration curve was higher than or equal to 0.999 9 when the mass concentration of elements was in range of 0-10 μg/mL. The proposed method was applied to the determination of seventeen impurity elements in crude selenium samples. The determination results were consistent with those obtained by nonferrous industrial standard analysis methods. The average recoveries were between 92% and 112%. The relative standard deviations (RSD, n=7) were less than 10% except for trace elements (Cd, Co, Cr, Ga, In and V) with low content.