Determination of trace cadmium in superalloy by inductively coupled plasma mass spectrometry with precipitation separation
NA Duo1,2, GAO Huiying1,2, LI Hui1, ZHANG Zhongyuan1
1. Institute of Metal Research,Chinese Academy of Sciences, Shenyang 110016, China; 2. School of Materials Science and Engineering, University of Science and Technology of China, Shenyang 110016, China
Abstract：Cadmium has harmful effects on the mechanical properties and microstructure of superalloys,so the control and accurate determination of cadmium content in superalloys is important.During the determination of cadmium in superalloys by inductively coupled plasma mass spectrometry (ICP-MS), the high-content molybdenum in sample will cause interference.The sample was dissolved with hydrochloric acid-nitric acid-hydrofluoric acid. Lead acetate was added to react with molybdenum to form lead molybdate precipitate to realize the separation of molybdenum from testing elements.Rhodium was used as internal standard element to overcome the matrix effect and instrument signal drift.111Cd was selected as the testing isotope.Finally,the determination method of trace cadmium in superalloy by ICP-MS was established.The suspension before precipitate standing and the precipitate after ageing were analyzed by scanning electron microscopy and energy dispersive spectrum,respectively,to optimize the precipitation conditions.The linear correlation coefficient of calibration curve was 0.999 8.The limit of detection and the limit of quantification was 0.070 μg/g and 0.20 μg/g,respectively.The superalloy samples and superalloy reference materials made by Institute of Metal Research (IMR) of Chinese Academy of Sciences (CAS) were for investigation.The content of cadmium was determined according to the experimental method.The found results were basically consistent with the certified values or those obtained by graphite furnace atomic absorption spectrometry (GFAAS).The relative standard deviations (RSD, n=9) of the determination results of actual samples were between 0.46% and 7.4%.
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