Abstract:5-(4-antipyrinylazo) salicylaldehyde (AASA) were synthesized,and the conditions for its chromogenic reaction with niobium were investigated. Thus,a novel method for the determination of niobium was established by spectrophotometry. The experimental results showed that niobium and AASA could form a pale yellow complex with molar ratio of 1∶1 and maximum absorption wavelength of 460 nm in pH 2.0 HCl-KCl buffer solution. Beer’s Law was complied within the concentration range of 0-1.6 μg/mL for niobium 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 3.0×104 L· mol-1· cm-1. AASA spectrophotometry was applied to the determination of niobium in iron-niobium synthetic solution,and the results were consistent with those obtained by sulfochlorophenol S method with relative standard deviation of 1.6%-1.7%.
Nagiev Kh D. Spectrophotometric determination of simultaneously present niobium and tantalum[J].J. Anal.Chem., 2004, 59(10):930-934.
[2]
Gojmerac Iv ic A, N Galic N, Tomi ic V. Formation and extraction of niobium(V) complex with xylenol orange in the presence of a 4-pyridone derivative[J]. J. Solution Chem., 2009, 38(2): 149-158.
[3]
Ivanov V M. Ninety years of using azo compounds of the pyridine series as analytical reagents[J]. J. Anal.Chem., 2005, 60(5):486-490.
[4]
陶慧林, 朱仕毅, 郑省政. K比例H点标准加入吸光光度法同时测定矿样中铌和钽[J]. 岩矿测试(Rock and Mineral Analysis),2010,29(6):699-702.
[5]
Chhakkar A K, Kakkar L R. Extractive spectrophotometric determination of niobium(V) with 3-hydroxy-2-(2-thienyl)-4H-chromen-4-one[J]. Fresenius J. Anal. Chem., 1995, 351(8):720-723.
[6]
王影,李艳杰,沈亮亮,等. 铌-酒石酸-铬天青S-溴化十六烷基吡啶分光光度法测定微量铌[J].光谱实验室(Chinese Journal of Spectroscopy Laboratory),2013,30(1):220-223.
Dedkov Yu M, Korsakova N V, Radugina O G. Color reactions of niobium and tantalum with bromine-substituted reagents of the PAR-PAN group[J]. J. Anal. Chem., 2003, 58(9):836-840.
[10]
朱传征, 沈骎, 徐超, 等. 间羧基氯磺酚的合成及其光度法测定钢中铌[J]. 理化检验-化学分册(Physical Testing and Chemical Analysis Part B: Chemical Analysis), 2000, 36(3):108-109, 111.
[11]
Metwally M A, Metwally A, Abdel-Galil A, et al. Substituted 5-Antipyrinylazo-4-phenyl-2 -aminothiazoles as disperse dyes for dyeing polyester fabrics[J]. Monatshefte für Chemie, 2008,139(1):35-42.