采用硫酸铵和硫酸溶解,在硫酸介质中选择5-Br-PADAP乙醇溶液作为显色剂,沸水浴10 min后,流水冷却至室温,在波长610 nm处进行测定,建立了5-Br-PADAP分光光度法测定锆合金中铌含量的分析方法.在最佳的分析条件下,铌质量浓度在0~0.8 μg/mL范围内与其吸光度呈线性关系,相关系数r=0.999 0,摩尔吸光系数ε=5.9×104 L/(mol·cm).按照实验方法测定锆合金中铌,结果的相对标准偏差(RSD,n=11)分别为2.9%和1.9%,并与电感耦合等离子体原子发射光谱法(ICP-AES)测定结果基本一致.
The zirconium alloy sample was dissolved with ammonium sulfate and sulfuric acid.The ethanol solution of 5-Br-PADAP was selected as coloring agent in sulfuric acid medium.After reaction in boiling water bath for 10 min, the solution was cooled to room temperature with flow water.The determination was conducted at wavelength of 610 nm.Thus the analysis method of niobium in zirconium alloys by 5-Br-PADAP spectrophotometry was established.Under the optimal analysis conditions, the mass concentration of niobium in range of 0-0.8 μg/mL was linear to the corresponding absorbance.The correlation coefficient was r=0.999 0, and the molar absorptivity was ε=5.9×104 L/(mol·cm).The content of niobium in zirconium alloy was determined according to the experimental method.The relative standard deviation (RSD, n=11) was 2.9% and 1.9%, respectively.The found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES).
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