Abstract:The accurate determination of impurity elements in rhodium octanoate dimer catalyst was one of important indicators to judge whether the product was qualified or not. The common method in the past was direct current arc emission spectrometry (spectrographic method). However, the detection period was long and the repeatability was poor. The determination of trace impurity elements in rhodium octanoate dimer catalyst by inductively coupled plasma atomic emission spectrometry (ICP-AES) was seriously interfered due to the presence of many organic components and rhodium matrix in catalyst sample.The organic components in sample were digested by dropwise adding nitric acid repeatedly. The salts were then dissolved with aqua regia. The interference of rhodium matrix was eliminated by selecting appropriate deduction of background points. Thus, a determination method of seven micro impurities in rhodium octanoate catalyst (including Pt, Pd, Pb, Fe, Cu, Al and Ni with mass fraction of 0.001%-0.1%) by ICP-AES was established. The mass concentration of elements in range of 0.10-10.00μg/mL was linear to the corresponding emission intensity with correlation coefficients higher than 0.9999. The detection limit (μg/mL) of the method was 0.075(Pt), 0.0033(Pd), 0.015(Pb), 0.0036(Fe), 0.010(Cu), 0.001(Al) and 0.012(Ni). The experimental method was applied for determination of Pt, Pd, Pb, Fe, Cu, Al and Ni in rhodium octanoate dimer catalyst samples. The relative standard deviations (RSD, n=7) of the determination results were between 1.4% and 9.6%. The content of Pt, Pd, Pb, Fe, Cu, Al and Ni in rhodium octanoate dimer catalyst was determined according to the experimental method and the found results were consistent with those obtained by direct current arc emission spectrometry.
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