Abstract：Germanium,which is an element with low melting point,in nickel-based superalloy will cause harmful effects on the mechanical properties and microstructure of alloy.Therefore,the content of germanium should be tested and strictly limited.The sample was decomposed by microwave digestion in closed system with HF-HNO3 mixture (volume ratio of 1∶1).The mass spectrum interference was eliminated by selecting 72Ge as the analytical isotope and using kinetic energy discrimination(KED) mode.The calibration curve prepared by matrix matching method and the correction by Rh internal standard were used to overcome the influence of matrix effect and instrument drift.The determination method of germanium in nickel-based superalloy by inductively coupled plasma mass spectrometry was established.The results showed that the linear range of method was 2-100 μg/L with linear correlation coefficient (r) of 1.000.The limit of detection (LOD) and limit of quantification (LOQ) was 0.036 μg/g and 0.12 μg/g,respectively.The content of germanium in certified reference materials of nickel-based superalloy was determined according to the experimental method.The found results were in good agreement with the certified values.The relative standard deviations (RSD,n=5) were less than 5%.The proposed method was applied for the determination of germanium in nickel-based superalloy sample and the recoveries were between 100% and 104%.
范小芬, 刘晓波, 刘庆斌, 杨国武. 电感耦合等离子体质谱法测定镍基高温合金中锗[J]. 冶金分析, 2021, 41(1): 63-68.
FAN Xiaofen, LIU Xiaobo, LIU Qingbin, YANG Guowu. Determination of germanium in nickel-based superalloy by inductively coupled plasma mass spectrometry. , 2021, 41(1): 63-68.
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