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合成了苯异硫脲基乙酸(简称PTHA),首次研究了PTHA用于Pd(Ⅱ)的萃取分光光度性能,实验表明在较高盐酸酸度(3~5mol/L)下,PTHA与钯形成黄色络合物,能被乙酸丁酯、二氯乙烷萃取,络合物在有机相的最大吸收波长为368nm,摩尔吸光系数ε=1.3×104L·mol-1·cm-1,钯含量在0~30μg范围符合比尔定律,可应用于萃取光度法测定钯。研究了萃取光度法的最佳条件,包括酸度、试剂用量、反应速度、萃取时间与有色络合物的稳定性、以及其它离子对测定钯的干扰。同时用电子吸收光谱、平衡移动法测定了钯与PTHA形成的络合物的组成,用紫外光谱、红外光谱探讨PTHA与Pd(Ⅱ)的配位机理。提出高选择性、简单快速测定钯的新方法。
Synthesis of phenyl isothioureaacetic acid (referred to as PTHA), the first study of PTHA for Pd (Ⅱ) extraction spectrophotometric performance experiments show that the higher acidity of hydrochloric acid (3 ~ 5mol / L), PTHA and palladium yellow The complex can be extracted with butyl acetate and dichloroethane. The maximum absorption wavelength of the complex in the organic phase is 368nm, the molar absorptivity ε = 1.3 × 104L · mol-1 · cm-1, the content of palladium Beer’s law is obeyed in the range of 0 ~ 30μg and can be applied to the determination of palladium by extraction spectrophotometry. The optimum conditions of extraction spectrophotometry were studied, including acidity, reagent amount, reaction rate, extraction time and the stability of the colored complex, as well as the interference of other ions on the determination of palladium. At the same time, the composition of complexes of palladium and PTHA was determined by electron absorption spectroscopy and equilibrium shift method. The coordination mechanism between PTHA and Pd (Ⅱ) was investigated by UV and FTIR spectroscopy. A new method of high selectivity, simple and rapid determination of palladium was proposed.