3,5-二甲基-4’-磺酸基苯基重氮氨基偶氮苯的合成及其在分光光度测定汞中的应用  

Synthesis of 3,5-dimethyl-4'-sulfobenzenediazoaminoazobenzene and its application to spectrophotometric determination of mercury

作　　者：李艳辉[1,2] 刘英红[1] 许兴友[1,2] 马卫兴[1] 孙吉佑[1] 郝昌静 

机构地区：[1]淮海工学院化学工程学院,江苏连云港222005 [2]南京理工大学材料化学实验室,江苏南京210094

出　　处：《冶金分析》2008年第11期32-35,共4页Metallurgical Analysis

基　　金：江苏省高校自然科学研究计划课题(08KJD150002);淮海工学院自然科学课题(Z2007044)

摘　　要：报道了3，5-二甲基-4’-磺酸基苯基重氮氨基偶氮苯（DMSDAA）的合成方法及其与汞的显色反应。3，5-二甲基苯胺重氮化得到重氮盐，重氮盐与4-磺酸基对氨基偶氮苯发生偶联反应生成了目标产物。用红外光谱、元素分析对其结构进行了表征。在Tween-80存在下，pH11．0的Na2B4O7-NaOH缓冲溶液中，Hg（Ⅱ）与DMSDAA形成1：2的红色络合物。络合物的最大吸收峰位于476nm波长处，表观摩尔吸光系数ε-1．59×10^5L·mol^-1·cm^-1。Hg（Ⅱ）含量在0．052-400μg／L范围内符合比尔定律。采用巯基葡聚糖凝胶（SDG）分离水中共存离子富集汞，提高了方法的选择性。本法用于水样分析，相对标准偏差为0．8％～2．9％，加标回收率为99．5％～103．2％。The synthesis of a new reagent 3,5-dimethyl-4＇-sulfobenzenediazoaminoazobenzene （DMSDAA） and its color reaction with mercury are studied. 3,5-dimethylaniline is diazotized to give a diazonium salt,which reacts with 4 - sulfo-p- amino-azobenzene to form the target product. The structure of DMSDAA was characterized by IR and element analysis . Results show that in the presence of Tween-80 ,the reagent reacts with mercury to form a stable red complex（1 ： 2） in Na2B4O7-NaOH buffer medium at pH 11.0. The maximum absorption wavelength and apparent molar absorptivity of the complex are 476 nm and 1.59 × 10^5L ·mol^-1 ·cm^-1 respectively. Beer＇s law is obeyed in the range of 0. 025-400μg/L. The coexisting ions can be separated from Hg（Ⅱ） in sample by sulphydryl dextrane gel to improve the selectivity. The method has been applied to the determination of water sample with the recovery of 99.5%-103.2% and the relative standard deviation of 0. 8%-2.9%.

关 键 词：3 5-二甲基-4’-磺酸基苯基重氮氨基偶氮苯 分光光度法 巯基葡聚糖凝胶(SDG) 汞 

分 类 号：O657.32[理学—分析化学]