1-偶氮苯-3-(3-硝基-5-氯-2-吡啶)-三氮烯的合成及其与汞的显色反应
Synthesis of 1-Azobenzene-3-(3-Nitro-5-Chloro-2-Pyridyl)-Triazene and Study on Its Color Reaction with Mercury(Ⅱ)
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摘要: 合成了显色剂1-偶氮苯-3-(3-硝基-5-氯-2-吡啶)-三氮烯(ABNCPyT),并用元素分析法和红外光谱法对其分子结构作了鉴定.研究了ABNCPyT与汞的显色反应,在pH 10.5的Na2B4O7-NaOH缓冲溶液中和聚氧乙烯烷基酚(Triton X-100)表面活性剂存在下,试剂与汞(Ⅱ)生成4∶1型红色配合物.配合物的最大吸收峰位于525 nm,表观摩尔吸光率为1.92×105L·mol-1·cm-1.汞(Ⅱ)质量浓度在600 μg·L-1以内符合比耳定律.用拟定方法测定废水中微量汞,所得结果与原子吸收光谱法的结果一致,测得其相对标准偏差(n=5)≤2.5%,方法的回收率在97.5%~103.0%.Abstract: A new chromogenic reagent,1-azobenzene-3-(3-nitro-5-chloro-2-pyridyl)-triazene (abbreviated as ABNCPyT) was synthesized and its molecular structure was identified by elementary analysis and IR spectrometry.It was found that in a borate buffer medium of pH 10.5 and in the presence of surfactant Triton X-100,a red colored coordination complex was formed between ABNCPyT and Hg(Ⅱ) with mole ratio (R to Hg) of 4 to 1.Apparent molar absorptivity of the complex was found to be 1.92×105L·mol-1·cm-1,at the wavelength of its absorption maximum 525 nm.Beer′s law was kept in the range within 600 μg·L-1.The proposed method has been applied the determination of mercury in samples of waste water,giving results in consistency with the results obtained by AAS method.Values of RSD (n=5) of the method was found to be ≤2.5%.Recovery was also tested and values obtained were in the range of 97.5% to 103.0%.