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以1亚硝基2萘酚为萃取剂,以90℃熔融萘作稀释剂萃取痕量钯(Ⅱ),萘相中钯经氯仿溶解后用光度法测定其含量。实验条件下络合物能从pH=0.8~110范围内定量萃入萘中,络合物波长λmax=440nm,摩尔吸光系数ε440=241×104L·mol-1·cm-1,组成比Pd∶HR=1∶2,萃取反应平衡常数Kex=631×1011。钯量在048~34μg/10ml范围内符合朗伯比耳定律,检测限为0044μg/10ml。同时确定了光度法测定的最佳条件及常见阴阳离子的干扰允许量。利用该法进行合成样与实际样中钯含量的测定,结果满意。
Nitrobenzyl2naphthol was used as extractant to extract trace palladium (Ⅱ) with molten naphthalene as diluent at 90 ℃. The content of palladium in naphthalene phase was determined by spectrophotometry after it was dissolved in chloroform. Under the experimental conditions, the complex can be quantitatively extracted into naphthalene from pH = 0.8-11.0. The wavelength of the complex is λmax = 440nm, the molar absorptivity ε440 = 241 × 104L · mol-1 · cm- 1, composition ratio Pd: HR = 1: 2, extraction equilibrium constant Kex = 6 31 × 1011. In the range of 048 ~ 34μg / 10ml, the content of palladium conforms to Lambert-Beer’s law with the detection limit of 0044μg / 10ml. At the same time, the best conditions for photometric determination and the allowable amount of interference of common anion and cation were determined. The method was used to determine the content of palladium in the sample and the sample, the results were satisfactory.