电感耦合等离子体原子发射光谱法测定碳化钼催化剂中钼

研究了电感耦合等离子原子发射光谱法测定碳化钼催化剂中钼的测定条件包括溶样酸、仪器参数、分析线和干扰的消除等,在此基础上建立了碳化钼催化剂中钼的测定方法。样品用 HNO₃、HF、HClO₄的混酸溶解处理后,在体积分数为2.5%的硝酸和1%氢氟酸混酸介质中,以Mo 202.030{166} nm 作为分析谱线,采用电感耦合等离子原子发射光谱法测定。通过筛选分析谱线、合理设置背景扣除位置,避免了光谱干扰。方法应用于碳化钼催化剂样品中钼的测定,结果与重量法(GB 50591-85)一致,相对标准偏差(n=6)小于1.5%,回收率在99%～100%之间。

Determination of molybdenum in molybdenum carbide catalyst by inductively coupled plasma atomic emission spectrometry

The determination conditions of molybdenum in molybdenum carbide catalyst by inductively coupled plasma atomic emission spectrometry were studied, including the selection and dose of acid for sample dissolution, the selection of instrumental parameters and analysis lines, and the elimination of interference. On the basis of this, the determination method of molybdenum in molybdenum carbide catalyst was established. The sample was dissolved with mixed HNO₃, HF and HClO₄. Then, the content of molybdenum was determined in mixed acid medium (2.5 % (V/V) HCl + 1 % (V/V) HF) by inductively coupled plasma atomic emission spectrometry using Mo202.030{166} nm as analysis line. The spectral interference was eliminated by properly selecting analysis line and setting background deduction position. The detection limit of method was 0.05-3 mg/g. The proposed method was applied to the determination of molybdenum carbide catalyst samples. The found results were consistent with those obtained by gravimetric method (GB 50591-85). The relative standard deviation (RSD, n=6) was less than 1.5%. The recoveries were between 99% and 100%.