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新显色剂5-(5-氟-2-吡啶偶氮)-2,4-二氨基甲苯的合成及其与钯的显色反应

  • 摘要: 合成并用红外光谱和元素分析鉴定了氟代吡啶偶氮氨类新试剂5-(5-氟-2-吡啶偶氮)-2,4-二氨基甲苯(5-F-PADAT),并研究了该试剂与钯显色的反应。结果表明,在0.32~3.84 mol/L 高氯酸溶液中,试剂与钯形成1∶1的紫红色络合物,其最大吸收峰位于566 nm,表观摩尔吸光系数为4.84×104 L·mol-1·cm-1,钯的浓度在0~2000 μg/L符合比耳定律。方法选择性好,大量常见金属离子不干扰钯的测定,操作简单,应用于矿样和催化剂中微量钯的测定,结果与原子吸收光谱法相符。

     

    Abstract: A new chromogenic reagent 5-(5-fluoro-2-pyridylazo)-2,4-diaminotoluene(5-F-PADAT) has been synthesized and characterized by infred spectometry and elemental analyzer. The chromogenic reaction of 5-F-PADAT with palladium (Ⅱ) was also studied. The experimental results show that Pd(Ⅱ) reacts with 5-F-PADAT to form a stable violetred complex in a solution of 0.32~3.84 mol/L HClO4. The molar ratio of Pd (Ⅱ) to 5-F-PADAT is 1∶1 with apparent molar absorptivity of 4.84×104 L·mol-1·cm-1 at the maximum absorption of 566 nm. Beer′s law is obeyed in the range of 0~2000 μg/L for palladium. The method provides high selectivity and most common ions do not interfere with the determination of Pd (Ⅱ). The method has been successfully applied to the determination of micro-amount of palladium in ore and catalyst samples. The results are in agreement with those obtained by atomic absorption spectrometry.

     

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