5-安替比林偶氮水杨基荧光酮的合成及其与钨显色反应的研究

来源期刊：冶金分析2010年第5期

论文作者：刘英红 马卫兴 李艳辉 沙鸥 繆缙

文章页码：24 - 27

关键词：5-安替比林偶氮水杨基荧光酮； 合成； 钨； 分光光度法； 十六烷基三甲基溴化铵

Key words：5-antipyriylazosalicylfluorone； synthesis； tungsten； spectrophotometry； cetyltrimethylammonium bromide

摘    要：报道了新试剂5-安替比林偶氮水杨基荧光酮(APASF)的合成方法,研究了在表面活性剂十六烷基三甲基溴化铵(CTMAB)存在下试剂与钨的显色反应。将4-氨基安替比林重氮化制得重氮盐溶液,然后水杨醛与重氮盐反应合成安替比林偶氮水杨醛,将事先合成的偏三酚三乙酸酯与安替比林偶氮水杨醛反应合成APASF,并用红外光谱分析法对其进行表征。产率为40%。在酸性介质中,表面活性剂十六烷基三甲基溴化铵(CTMAB)存在下,试剂与钨生成络合物的最大吸收波长为520 nm,表观摩尔吸光系数为7.4×10⁴ L·mol^-1·cm^-1,钨的质量浓度在0.1～1.0μg/mL范围内符合比尔定律。方法用于标准钢样中钨的测定,测得值与认定值相符。

Abstract: The synthesis method of a new reagent 5-antipyrine azo salicylfluorone (APASF) was reported.The coloring reaction of this reagent with tungsten was studied in the presence of surfactant cetyl trimethyl ammonium bromide (CTMAB).The diazosalt solution was firstly prepared by the diazotization of 4-amino-antipyrine.The salicylaldehyde reacted with diazosalt to synthesize antipyrine azo salicylaldehyde.The prepared hydroxyquinol triacetate reacted with obtained antipyrine azo salicylaldehyde to synthesize APASF which was then characterized with infrared spectrometric method.The yield was 40%.The coloring reaction of the reagent with tungsten took place in acid medium and in the presence of surfactant cetyl trimethyl ammonium bromide (CTMAB).The maximum Absorption wavelength of formed complex was 520 nm with apparent molar Absorptivity of 7.4×10⁴ L·mol^-1·cm^-1.Beer’s law was obeyed for tungsten in the range of 0.1-1.0 μg/mL.The proposed method has been applied to the determination of tungsten in standard steel sample.The results were consistent with the certified values.