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出 处:《理化检验(化学分册)》2009年第11期1336-1338,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:甘肃省教育厅科研基金项目(No.0710B-03)
摘 要:合成了一种新的荧光试剂3-甲氧基-4-羟基苯甲醛-2-肼基苯甲酸(香草醛缩邻肼基苯甲酸),并用红外光谱法及元素分析法对其分子结构作了验证。试验发现:在pH 5.1的乙酸盐缓冲介质中,上述新试剂在激发波长为308.8 nm时,在476.8 nm波长处出现发射荧光峰,而当在此条件下加入银离子时,由于两者相互反应生成络合物而导致试剂发生荧光猝灭现象,其荧光强度的减弱程度(△F)与银离子的质量浓度在3.0~160μg·L^(-1)范围内呈线性关系。测得此反应对Ag^+离子的检出限(3S/N)为0.28μg·L^(-1)。据此,提出了测定痕量银的新方法。用标准加入法测得方法的回收率在98.3%~103.3%之间。A new fluorescence reagent, 3-mehoxy-4-hydroxybenzaldehyde-2-hydrazinobenzoic acid (MHBHBA) was synthesized and its molecular structure was identified by IR-spectrometry and elementary analysis. It was found that in an acetate buffer of pH 5. 1, the new reagent, MHBHBA reacted with Ag+ ion to form a stable complex, leading to quenching of fluorescence of the reagent, and that the magnitude of fluorescence quenching of MHBHBA kept linear relationship with mass concentration of Ag+ ion in the range of 3. 0--160μg·L^-1, when measured at the wavelengths of (λex) 308. 8 nm and (λen) 476. 8 nm. Detection limit (3S/N) found was 0. 28 μg ·L^-1. Based on these facts, method for determination of trace amount of silver was proposed. Recovery of the method was tested by standard addition method, giving values of recovery ranged from 98. 3% to 103. 3%.
关 键 词:合成 3-甲氧基-4-羟基苯甲醛-2-肼基苯甲酸 银离子 荧光猝灭反应
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