1-(4-硝基苯基)-3-(3,5-二溴吡啶)三氮烯的合成及其与镍的显色反应

Synthesis of 1-(4-Nitrophenyl)-3-(3,5-Dualbromopyridyl)-Triazene and Its Chromatogenic Reaction with Nickel(Ⅱ)

合成了1-（4-硝基苯基）-3-（3，5-二溴吡啶）三氮烯（NPDBPDT），并研究了NPDBPDT与镍的显色反应。在pH10.0的Na2B4O7-NaOH缓冲溶液介质中，表面活性剂Triton X-100存在下，镍与试剂生成摩尔比为1：4的络合物在470nm处有最大正吸收峰，表观摩尔吸光系数为1.02×10^5L·mol^-1·cm^-1；在540nm处有最大负吸收峰，表观摩尔吸光系数为1．15×10^5L·mol^-1·cm^-1；以540nm为参比波长、470nm为测量波长进行双波长测定，表观摩尔吸光系数为2．17×10^5L·mol^-1·cm^-1。镍含量在0～480μg/L内符合比尔定律。方法用于合金样品中镍的测定，结果与原子吸收法相符，加标回收率为98．0％～102．0％；精密度小于5％（RSD，n=6）。

The synthesis of a new reagent 1-（4-nitrophenyl）-3-（3,5-dualbromopyridyl）-triazene （NPDBPDT） and its chromatogenic reaction with nickel（Ⅱ） were reported in this paper. In the buffer solution of Na2B4O7-NaOH （pH = 10.0） and in the presence of surface active agent of Triton X-100, nickel reacts with the chromogenic absorptivity of 1.15×10^5 L·mol^-1·cm^-1. The apparent molar absorptivity is 2.17×10^5 L·mol^-1·cm^-1 using dual-wavelengh spectrophotometric measurement with the reference wavelengh at 540 nm and measurement wave- lengh at 470 nm. Beer＇s law is obeyed in the range of 0～480 μg/L for Ni（Ⅱ）. The method has been applied to the determination of Ni（Ⅱ） in practical samples and the results are in agreement with those provieded by AAS. The recoveries of the method are 98.0%～102.0% with precision of less than 5% RSD （n = 6）.