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研究了在自制的十六烷基三甲基溴化铵、正丁醇、正庚烷和水微乳溶液存在下,氯酚偶氮罗丹宁与Pd(的显色反应,建立了分光光度法测定微量PdⅡ的新方法。结果表明,在pH5.3的HAc-NaAc缓冲溶液中,Pd(与试剂形成1∶2的暗红色络合物,络合物的最大吸收峰在500nm波长处,表观摩尔吸光系数ε为1.79×105L.mol-1.cm-1。在10mL显色液中,Pd(量在0.01～12μg范围内符合比尔定律,检出限为0.0003μg/mL。本法可用于碳钯催化剂和含钯分子筛中微量钯的测定,回收率在98.1%～98.6%之间,RSD在1.17%～2.34%(n=6)范围内。
The color reaction of chlorophenazopyrodin with Pd (CN) was studied in the presence of self-made cetyltrimethylammonium bromide, n-butanol, n-heptane and water microemulsion. Spectrophotometry A new method was established for the determination of trace amounts of PdⅡ.The results showed that in the HAc-NaAc buffer solution at pH5.3, Pd (the dark red complex formed with 1: 2 with the reagent, the maximum absorption peak of the complex was at 500nm, The molar extinction coefficient ε was 1.79 × 10 5 L · mol -1 · cm -1. In 10 mL of color developing solution, the content of Pd in the range of 0.01 ~ 12 μg was Beer’s law with the detection limit of 0.0003 μg / mL. The results showed that the recovery of trace palladium was between 98.1% and 98.6% and the RSD was between 1.17% and 2.34% (n = 6) for the determination of trace palladium in carbon-palladium catalyst and palladium-containing molecular sieve.