Abstract：The temperature of graphite digester was increased to 120 ℃ in 7 min and then kept for 20 min. Thus, eighteen impurity elements in sponge palladium, which had an affect on the quality of sponge palladium, were determined by inductively coupled plasma mass spectrometry (ICP-MS) with 10% (V/V) aqua regia as medium. The results showed that the matrix effect could be effectively corrected with 20 μg/L 45Sc, 89Y and 159Tb as internal standard respectively and the mass concentration of matrix Pd in determination solution as 2.0 mg/mL. The elements including aluminum, nickel, copper, zinc, ruthenium, rhodium, platinum, silver, tin, iridium, gold, lead and bismuth were determined under standard mode, while magnesium, silicon, chromium, manganese and iron were determined under ammonia reaction mode to eliminate the mass spectrometry interference. Under the selected experimental conditions, the linear correlation coefficients of calibration curves of test elements were all not less than 0.999 6. The detection limit of method was 1.0-42 ng/L. The proposed method was applied to the determination of impurity elements in sponge palladium. The relative standard deviations (RSD, n=11) of the results were between 0.8% and 2.8%, and the recoveries were between 90% and 107%. The results for sponge palladium actual samples obtained by the proposed method were compared with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES), and the consistency was good.
杨加桂,李先和,张晓天,王 颖. 石墨消解-电感耦合等离子体质谱法测定海绵钯中18种杂质元素[J]. 冶金分析, 2016, 36(7): 46-50.
YANG Jia-gui,LI Xian-he,ZHANG Xiao-tian,WANG Ying. Determination of eighteen impurity elements in sponge palladium by inductively coupled plasma mass spectrometry with graphite digestion. , 2016, 36(7): 46-50.
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