3,3′-二甲基-4,4-′(2-重氮氨基噻唑)联苯的合成及其与汞的显色反应  

Synthesis of a new reagent 3,3′-dimethyl-4,4′-(2-diazoaminothiazolyl)biphenyl and its color reaction with mercury(Ⅱ)

作　　者：王裔耿[1] 李崇宁[2] 王加林[2] 丁中涛[1] 曹秋娥[1] 高竹林[1] 

机构地区：[1]云南大学化学系,云南昆明650091 [2]云南大学成人教育学院,云南昆明650091

出　　处：《化学试剂》2005年第11期673-675,共3页Chemical Reagents

基　　金：云南省人才培引项目(2004PY01-4)资助

摘　　要：合成了一个三氮烯类试剂3,3′-二甲基-4,4′-(2-重氮氨基噻唑)联苯(DDATBP),研究了该试剂与Hg2+的显色反应,并建立了一个测定汞的光度分析新方法.在Tween-80存在下,试剂与汞在pH 11.0的Na2B4O7-NaOH缓冲溶液中迅速生成2∶1的桔红色配合物,其最大吸收波长为545nm.在最佳实验条件下,体系在545nm处的表观摩尔吸光系数为7.08×104L·mol-1·cm-1,Hg2+的浓度在0.10～2.5μg/mL范围内符合比尔定律.对30μg/25mL的Hg2+平行测定7次,算得方法的相对标准偏差(RSD)为1.8%,以3σ/k法算得方法的检出限为0.078μg/mL.该方法用于环境水样中微量汞的测定,结果满意.A new triazene reagent, 3,3＇-dimethyl-4,4＇- （ 2-diazoaminothiazolyl） bipbenyl （ DDATBP）, DDATBP was firstly synthesized, and the conditions of the color reaction between DDATBP and Hg （ Ⅱ ） were studied. Based on this color reaction, a new spectrophotometric method for the determination of Hg （ Ⅱ ） was developed. The results showed that the nacarat complex with a molar ratio of DDATBP to Hg（ Ⅱ ） of 2 ： 1 and maximum absorption wavelength of 545nm was formed in the presence of Tween-80 and Na2B4O7-NaOH buffer solution of pH 11.0. Under the optimum conditions ,Beer＇s law was obeyed in the concentration range of Hg（ Ⅱ ） over 0.10 - 2.5μg/mL with the molar absorptivity of 7.08 × 10^4L· mol^- 1· cm^-1. The relative standard deviation（RSD） for the determination of 30μg/25mL Hg（ Ⅱ ） was 1.8 % （n = 7）, and the limit of determination calculated as 3σ/k was 0.078μg/mL. The method was not sensitive, but was simple, rapid, and of wide linear range, and has been used for the determination of mercury in water with satisfactory results.

关 键 词：3 3'-二甲基-4 4’-(2-重氮氨基噻唑)联苯 汞 分光光度法 水 

分 类 号：O626[理学—有机化学]