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本法研究了在聚乙烯醇(PVA)存在下,钯与钼酸铵和乙基罗丹B(ERB)反应形成的有色离子缔合物用于微量钯的光度法测定。缔合物的最大吸收位于580nm,表观摩尔吸收系数ε为2.13×105L·mol-1·cm-1,钯量在0-5.5μg/25mL范围内服从比耳定律。体系至少稳定140h,检出限(3σ)8.64μg/L(n=11),对0.20mg/LPd(Ⅱ)测定的相对标准偏差为2.66%(n=12)。缔合物的摩尔比为Pd∶ERB=1∶4。考查了50多种共存离子的影响。本法用于炭基和铝基催化剂中微量钯的测定,结果满意。
This method was developed for the spectrophotometric determination of trace palladium with the presence of polyvinyl alcohol (PVA) in the presence of palladium and ammonium molybdate and ethylrhodamine B (ERB). The maximum absorption of the association at 580nm, the apparent molar absorption coefficient ε was 2.13 × 105L · mol-1 · cm-1, palladium content in the range of 0-5.5μg / 25mL obey Beer’s law. The system was stable at least for 140 h with a detection limit (3σ) of 8.64 μg / L (n = 11) and a relative standard deviation of 2.66% (n = 12) for the 0.20 mg / L PD (Ⅱ) assay. The molar ratio of association was Pd: ERB = 1: 4. Examined the impact of more than 50 kinds of coexisting ions. The method is applied to the determination of trace palladium in carbon-based and aluminum-based catalysts with satisfactory results.