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基于2-(5-溴-2-吡啶偶氮)-5-二甲氨基苯胺(5-Br-PADMA)与钯(II)的高选择性显色反应,建立了激光热透镜光谱法测定微量钯的新方法。在0.6 mol/L HClO4介质中,于室温下放置10 min,Pd(II)与5-Br-PADMA反应形成稳定的青蓝色配合物,其最大吸收波长位于611 nm处,与所用He-Ne激光器输出波长632.8 nm能较好匹配。钯质量浓度在5~150 ng/mL范围内与激光热透镜信号强度呈线性关系,检出限为1.6 ng/mL,以工作曲线的斜率计算,灵敏度较光度法提高115倍。常见金属离子及10倍量的铂、铑、铱、钌、锇和金等贵金属离子不干扰钯的测定,方法具有良好的选择性。本法应用于催化剂、矿石和合金中钯的测定。
Based on the highly selective color reaction of 2- (5-bromo-2-pyridylazo) -5-dimethylaminoaniline (5-Br-PADMA) with palladium (II), a laser thermal lens spectrometry was developed for the determination of trace New method of palladium. Pd (II) reacted with 5-Br-PADMA to form a stable blue-green complex in 0.6 mol / L HClO4 medium at room temperature for 10 min. The maximum absorption wavelength was at 611 nm, The laser output wavelength of 632.8 nm can better match. The concentration of palladium in the range of 5 ~ 150 ng / mL has a linear relationship with the signal intensity of laser thermal lens with the detection limit of 1.6 ng / mL. The sensitivity is 115 times higher than that of photometric method. Common metal ions and 10 times the amount of platinum, rhodium, iridium, ruthenium, osmium and gold and other precious metal ions do not interfere with the determination of palladium, the method has good selectivity. This method is applied to the determination of palladium in catalysts, ores and alloys.