采用5.0 mL氢氟酸和10.0 mL硝酸混合酸消解样品,选择Ce 407.570 nm、Cu 217.895 nm、Fe 234.350 nm、Er 390.631 nm、Mg 383.829 nm、Mn 257.610 nm、Pb 283.305 nm、Zn 213.857 nm为分析线,使用电感耦合等离子体原子发射光谱法(ICP-AES)进行测定,从而建立了电感耦合等离子体原子发射光谱法测定钼铌合金中Ce、Cu、Fe、Er、Mg、Mn、Pb、Zn等8种元素的分析方法.考察了主要元素Mo、Nb和Al对待测元素的影响,结果表明,这些元素对待测元素基本无影响.各元素校准曲线的线性相关系数均大于0.999;方法中各元素检出限为5.4~63 μg/g.按照实验方法测定钼铌合金样品中Ce、Cu、Fe、Er、Mg、Mn、Pb、Zn,结果的相对标准偏差(RSD,n=6)为0.89%~4.4%;回收率为98%~102%.按照实验方法测定钼铌合金样品中Cu、Fe、Er、Mg、Mn、Pb、Zn、Ce,并与电感耦合等离子体质谱法(ICP-MS)的测定结果进行比对,二者基本一致.
The sample was digested with the mixed acid combined with 5.0 mL of hydrofluoric acid and 10.0 mL of nitric acid.Ce 407.570 nm, Cu 217.895 nm, Fe 234.350 nm, Er 390.631 nm, Mg 383.829 nm, Mn 257.610 nm, Pb 283.305 nm and Zn 213.857 nm were selected as analytical lines.Consequently, an analysis method of eight elements (including Ce, Cu, Fe, Er, Mg, Mn, Pb and Zn) in molybdenum-niobium alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established.The influence of major elements (Mo, Nb and Al) on test elements was investigated.The results indicated that these elements had no significant influence on determination.The linear correlation coefficients of calibration curves were all higher than 0.999.The detection limits of elements were between 5.4 μg/g and 63 μg/g.The proposed method was applied for the determination of Ce, Cu, Fe, Er, Mg, Mn, Pb and Zn in molybdenum-niobium alloy samples.The relative standard deviations (RSD, n=6) were between 0.89% and 4.4%.The recoveries were between 98% and 102%.The content of Ce, Cu, Fe, Er, Mg, Mn, Pb and Zn in molybdenum-niobium alloy samples was determined according to the experimental method.The results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).
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