摘要
合成了5-(4-安替吡啉偶氮)水杨醛(AASA),探讨了试剂与铌(Ⅴ)的显色反应条件,建立了测定铌(Ⅴ)的光度分析新方法.实验表明,在pH 2.0的HCl-KCl缓冲体系中,铌(Ⅴ)与AASA形成摩尔比为1∶1的浅黄色络合物,最大吸收波长为460 nm.铌(Ⅴ)的质量浓度在0~1.6 μg/mL符合比尔定律,其回归方程为A=0.077 79+0.012 91ρNb(μg/25 mL),相关系数r=0.999 6,表观摩尔吸光系数为3.0×104 L·mol-1·cm-1.将AASA分光光度法应用于铁-铌合成溶液中铌的测定,结果与氯磺酚S法一致,相对标准偏差为1.6%~1.7%.
5-(4-antipyrinylazo) salicylaldehyde (AASA) were synthesized, and the conditions for its chromogenic reaction with niobium(v) were investigated. Thus, a novel method for the determination of niobium(V) was established by spectrophotometry. The experimental results showed that niobium(V) and AASA could form a pale yellow complex with molar ratio of 1 : 1 and maximum absorption wave- length of 460 nm in pH 2.0 HCl-KCl buffer solution. Beer's Law was complied within the concentra- tion range of 0-1.6 μg/mL for niobium(Ⅴ) with linear regression equation of A=0. 077 79+0. 012 91ρNb (μg/25 mL) and r of 0. 999 6,and the apparent molar absorptivity was 3.0×10^4 L· mol ^-1 . cm 1 AASA spectrophotometry was applied to the determination of niobium in iron-niobium synthetic solu- tion, and the results were consistent with those obtained by sulfochlorophenol S method with relative standard deviation of 1.6 %-1.7 Y00.
出处
《冶金分析》
CAS
CSCD
北大核心
2013年第12期67-69,共3页
Metallurgical Analysis
基金
辽宁省教育厅2012年度辽宁省普通高等教育本科教学改革研究资助项目(有机化学实验教学方法创新研究与应用
指南题号3-4)