一种H酸衍生物新试剂的合成并用于铜(Ⅱ)离子的显色反应
Synthesis of a New Azo Reagent of H-acid Derivative and Its Use in the Color Reaction with Cupric Ion
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摘要: 以H酸钠盐和4-氨基苯磺酸为主要反应物,制备了偶氮类试剂7-(4-磺酸基苯偶氮)-8-羟基-1-氨基-3,6-萘二磺酸(简称SPAHANS).采用红外光谱法、紫外-可见分光光度法和元素分析法对SPAHANS的组成及结构作了检测.研究了该试剂与铜(Ⅱ)的显色反应.在pH 4.5的乙酸-乙酸钠缓冲体系中,在40~65 ℃加热5 min后,铜(Ⅱ)和SPAHANS反应生成配合比为1∶2的棕褐色配合物,在其最大吸收波长510 nm处的摩尔吸光率为1.6×105L·mol-1·cm-1.铜(Ⅱ)量在0.22~3.0 mg·L-1范围内服从比耳定律.方法的检出限(3s/k)为5.6×10-2mg·L-1,取质量浓度为1.0 mg·L-1铜(Ⅱ)标准溶液,同时测定9次,测得相对标准偏差为0.17%.Abstract: A new azo reagent,7-(4-sulfophenylazo)-8-hydroxy-1-amino-3,6-naphthalene disulfonic acid (SPAHANS),was synthesized by the reaction of diazonium compound of 4-aminobenzene sulfonic with H acid in 0.25 mol·L-1 Na2CO3 solution of pH 9.0.Molecular composition and structure of SPAHANS were determined by FT-IRS,UV-VIS spectrophotometry and elementary analysis.It was found that in an acetate buffer medium of pH 4.5 and heated at 40-65 ℃ for 5 min,a stable coordination complex (Cu2+∶R=1∶2) was formed by the reaction of SPAHANS with cupric ion,having the absorption maximum at 510 nm.Linear relationship between values of absorbance and concentration of Cu2+-ion was obtained in the range of 0.22-3.0 mg·L-1.Detection limit (3s/k) found was 5.6×10-2mg·L-1.The molar absorptivity of the color system was found to be 1.6×105L·mol-1·cm-1.Test for precision was made with standard Cu2+ solution of 1.0 mg·L-1 for 9 determinations,giving value of RSD 0.17%.