Abstract:A novel palladium chelating agent can enrich trace palladium in solution. There is residual palladium in chelating agent after the extraction of palladium with very complex existing form, which cannot be completely dissolved in acid.The palladium-rich chelating agent residue was pretreated by fire assaying method. The residual palladium was enriched in silver granules. Then, the silver granules were dissolved with nitric acid and hydrochloric acid. Pd 340.458nm was selected as the analytical line. The content of palladium was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Thus the determination method of residual palladium in palladium chelating agent was established. The effect of silver amount added in the melting process, the acid medium and acidity during the determination of palladium and the precipitation time after acid dissolution of silver granules on the determination results of palladium content was investigated. The results showed that the determination of palladium content was accurate under the following conditions: the amount of silver added in melting was more than 3 times of palladium amount, the determination medium was 10% aqua regia, and the precipitation time was 4h or overnight. The calibration curve of palladium was linear when the content of palladium was in the range of 1-15μg/mL, and the correlation coefficient was 0.999998. The detection limit was 0.019μg/mL. The residual palladium in 4 palladium chelating agents was determined according to the experimental method. The relative standard deviations (RSD, n=12) of determination results ranged from 0.46% to 0.62%. The recoveries were between 99% and 102%.
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