化学学报 ›› 1981, Vol. 39 ›› Issue (5): 461-465. 上一篇    下一篇

研究简报

分光光度法测定微量铌的研究——用2-(5’-溴吡啶-2’-偶氮)-5-二乙胺基苯酚作显色剂

朱玉瑞, 魏复盛, 曲培华, 沈乃葵   

  1. 中国科学技术大学化学系 合肥
  • 投稿日期:1979-06-12 发布日期:2013-06-03

A STUDY OF SPECTROPHOTOMETRIC DETERMINATION OF MICROGRAM AMOUNTS OF NIOBIUM BY 2-(5’-BROMOPYRIDYL-2’-AZO) -5-DIETHYLAMINOPHENOL

ZHU YU-RUI, WEI FU-SHENG, QU PEI-HUA, SHEN NAI-KUI   

  1. Department of Chemistry, The China University of Science and Technology, Hefei
  • Received:1979-06-12 Published:2013-06-03

2-(5'-溴吡啶-2'-偶氮)-5-二乙胺基苯酚(简称5-Br-PADAP)的结构式为,在吡啶偶氮对位的苯环上存在一个强的助色团—N(C2H5)2,它与过渡金属离子如UO22+,CO2+,Fe3+,Ni2+,Zn2+,Mn2+,Bi3+等的显色反应灵敏度一般都比PAR要提高一倍至几倍,其摩尔吸收系数多在105数量级。但用该试剂测定铌尚未见报道,根据铌(V)与PAR的显色反应,我们估计5-Br-PADAP可能与Nb5+显色且灵敏度会更高,本文研究证实了这种预想。在含酒石酸的0.02~0.14N盐酸介质中,Nb5+与5-Br-PADAP和酒石酸生成1:1:1的紫蓝色三元络合物,其吸收峰位于626nm,摩尔吸收系数为6.6×104。此法用于部分合金钢中铌的测定,比用硫氰酸盐、溴邻苯三酚红,PAR,氯代磺酚S,N-肉桂酰-N-邻甲苯羟胺,及噻唑偶氮-5-二甲胺基酚等显色剂的灵敏度都高,色泽稳定,选择性良好,样品不经分离可直接测定。

This communication reports a spectrophotometric method for the determination of microgram amounts of niobium. 2-(5'-Bromopyridyl-2'-azo)-5-diethylamino-phenol is used as a complexing colorimetrio reagent. It reacts with niobium in H2O-EtOH medium and in the presence of tartaric acid at 0.02-0.14 N HCl to form a purple-blue ternary complex having an absorption maximum at 626 nm and molar absorptivity of 6.6×104·mole-1·cm-1, Boer's law is obeyed in the concentration range of 0~25μg Nb/25 ml. The effects of 40 ions have beon studied and found that only large amounts of Fe3+ and Cu2+ interfere. However, their interferences can be eliminated by addition of ascorbic acid and thiourea respectively. The composition of the ternary complex of niobium with 2-(5'-brompyridyl-2'-azo)-6-diethyl-aminopenol and tartaric acid has been determined by Job's continuous variation and slope ratio method ag well as the displacement of equilibrium method indicating that niobium may react with 2-(5'-bromopyridyl-2'-azo)-5-diethylaminophenol and tartaric acid in a molar ratio of 1:1:1.The proposed method is simple and rapid with high sensitivity and good selectivity. It.has been applied to the direct determination of niobium in alloy steels without preliminary separation and the results of the determination were reasonably accurate.