Determination of arsenic,selenium,tin,antimony,lead and bismuth in nickel-chromium alloy by inductively coupled plasma mass spectrometry
BAO Xiangchun1,2, LI Jianting1,2, LIU Chun1,2, WANG Sumei*1,2
1. State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization of Baotou Research Institute of Rare Earths, Baotou 014030, China; 2. Ruike National Engineering Research Center of Rare Earth Metallurgy and Function Materials,Baotou 014030, China
Abstract：The accurate determination of arsenic, selenium, tin, antimony, lead and bismuth in nickel-chromium alloy is of great significance for the production and application of nickel-chromium alloy. Due to the volatility of arsenic and selenium, a mixture of 10 mL of hydrochloric acid and 1mL of nitric acid was used to dissolve the nickel-chromium alloy. 75As, 77Se, 120Sn, 121Sb, 208Pb and 209Bi were selected as the measuring isotopes. The determination method of arsenic, selenium, tin, antimony, lead and bismuth in nickel-chromium alloy by inductively coupled plasma mass spectrometry method (ICP-MS) was established using rhodium as internal standard to calibrate the determination of arsenic, selenium, tin, and antimony, and using rhenium as internal standard to calibrate the determination lead and bismuth, respectively. The experiments showed that the heating at 200 ℃ to evaporate chloride ions in the sample solution and converting the hydrochloric acid medium into nitric acid medium could eliminate the interference effect of polyatomic ions 40Ar35Cl+ and 40Ar37Cl+ ions on the determination of 75As and 77Se. The determination medium was further optimized: 2% (V/V) hydrochloric acid was used as the medium to determine the contents of tin, antimony, lead, and bismuth, and 2% (V/V) nitric acid-ethanol was used for the determination of arsenic and selenium contents. Under the optimized experimental conditions, the ratio of signal intensity between the analyzed element to the internal standard element showed a good linear relationship with the concentration of the analyzed element in range of 2.00-25.00 ng/mL. The correlation coefficients were greater than 0.999 5. The limits of detection were between 0.012 ng/mL and 0.21 ng/mL, and the limits of quantification were between 0.04 ng/mL and 0.70 ng/mL. The contents of arsenic, selenium, tin, antimony, lead, and bismuth in nickel-chromium alloy were determined according to the experimental method, and the found results were basically consistent with those obtained by atomic fluorescence spectrometry (AFS). The relative standard deviations (RSDs, n=11) were between 5.4% and 12%. The spiked recoveries were between 96% and 120%.
包香春, 李建亭, 刘春, 王素梅. 电感耦合等离子体质谱法测定镍铬合金中砷硒锡锑铅铋[J]. 冶金分析, 2021, 41(11): 37-42.
BAO Xiangchun, LI Jianting, LIU Chun, WANG Sumei. Determination of arsenic,selenium,tin,antimony,lead and bismuth in nickel-chromium alloy by inductively coupled plasma mass spectrometry. , 2021, 41(11): 37-42.
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