碰撞反应池-电感耦合等离子体质谱法测定镍基高温合金中痕量铜锌钡

doi:10.13228/j.boyuan.issn1000-7571.011643

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摘要在采用电感耦合等离子体质谱法对镍基高温合金中Cu、Zn、Ba进行测定时,Ti、Cr、Mo合金元素形成的多原子离子如⁴⁷Ti¹⁶O⁺、⁵⁰Cr¹⁶O⁺、⁹⁸Mo⁴⁰Ar⁺会干扰测定。实验采用王水-氢氟酸溶解样品,选择⁶³Cu、⁶⁶Zn、¹³⁸Ba作为分析同位素,选择He碰撞反应池模式,用基体匹配法绘制校准曲线,Sc、Rh混合内标校正基体效应及仪器信号漂移的影响,实现了电感耦合等离子体质谱法对镍基高温合金中Cu、Zn、Ba的测定。考察了在标准模式和He碰撞反应池两种模式下Ti对Cu、Cr对Zn、Mo对Ba测定的影响。结果表明,在标准模式下,⁴⁷Ti¹⁶O⁺、⁵⁰Cr¹⁶O⁺、⁹⁸Mo⁴⁰Ar⁺带来的干扰不可忽略,而采用He碰撞反应池模式可成功克服上述干扰。分别在标准模式和He碰撞反应池两种模式下采集1 000 μg/mL Ti溶液中Cu的信号强度、1 000 μg/mL Cr溶液中Zn的信号强度、1 000 μg/mL Mo溶液中Ba的信号强度。结果表明,在He碰撞反应池模式下,3种待测元素的背景等效浓度(BEC)比标准模式降低至少一个数量级。在优化的实验条件下,校准曲线的线性相关系数大于0.999 0,方法的检出限和定量限分别为0.074~0.131 μg/g和0.25~0.43 μg/g。采用所建立的方法测定镍基高温合金标准物质和实际样品中Cu、Zn、Ba,并进行加标回收试验。结果表明,Cu、Zn测定结果与认定值相符;3种元素测定结果的相对标准偏差(RSD,n=7)小于4.0%;加标回收率为93%~105%。

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关键词 ：电感耦合等离子体质谱法(ICP-MS), 镍基高温合金, 碰撞反应池, 铜, 锌, 钡, 氦气

Abstract：During the determination of Cu, Zn and Ba in nickel-based superalloy by inductively coupled plasma mass spectrometry (ICP-MS), the polyatomic ions formed by alloying elements (Ti, Cr and Mo) such as ⁴⁷Ti¹⁶O⁺, ⁵⁰Cr¹⁶O⁺, ⁹⁸Mo⁴⁰Ar⁺ will interfere with the determination. The samples were digested with aqua regia-hydrofluoric acid in experiments. ⁶³Cu, ⁶⁶Zn and ¹³⁸Ba were selected as the analytical isotopes. Helium (He) collision reaction cell mode was adopted. The calibration curve was prepared by matrix matching method, and the influence of matrix effect and instrument signal drift was corrected by Sc and Rh mixed internal standards. Consequently, the determination of Cu, Zn and Ba in nickel-based superalloy by ICP-MS was realized. The effects of Ti, Cr and Mo on the determination of Cu, Zn and Ba were investigated in both standard mode and He collision reaction cell mode. The results showed that the interference caused by ⁴⁷Ti¹⁶O⁺, ⁵⁰Cr¹⁶O⁺ and ⁹⁸Mo⁴⁰Ar⁺ could not be ignored in standard mode, while it could be successfully overcome in the He collision reaction cell mode. The signal intensity of Cu in 1 000 μg/mL Ti solution, Zn in 1 000 μg/mL Cr solution and Ba in 1 000 μg/mL Mo solution were collected in standard mode and He collision reaction cell mode, respectively. The results showed that the background equivalent concentration (BEC) of three testing elements in the He collision reaction cell mode was at least one order of magnitude lower than that in the standard mode. Under the optimized experimental conditions, the linear correlation coefficients of the calibration curves were greater than 0.999 0. The limits of detection and limits of quantification of the method were 0.074-0.131 μg/g and 0.25-0.43 μg/g, respectively. The established method was used to determine Cu, Zn and Ba in certified reference materials and actual samples of nickel-based superalloy. Moreover, the recovery tests were carried out. The results showed that the found results of Cu and Zn were consistent with the certified values. The relative standard deviations (RSD, n=7) of the determination results of three elements were less than 4.0%. The spiked recoveries were between 93% and 105%.

Key words： inductively coupled plasma mass spectrometry (ICP-MS) nickel-based superalloy collision reaction cell copper zinc barium helium

收稿日期: 2021-09-28

ZTFLH:	O657.63
	TF125.2+12

基金资助:国家科技重大专项(J2019-VI-0023-0139)

通讯作者: 胡净宇(1969—),女,教授,博士,从事钢铁材料痕量元素分析测试与研究工作;E-mail:hujingyu@ncschina.com

作者简介: 张馨元(1997—),女,硕士生,从事金属材料痕量元素分析研究;E-mail:18811329896@163.com

引用本文:

张馨元, 胡净宇, 侯艳霞, 齐荣, 刘晓波, 刘庆斌. 碰撞反应池-电感耦合等离子体质谱法测定镍基高温合金中痕量铜锌钡[J]. 冶金分析, 2022, 42(5): 15-20. ZHANG Xinyuan, HU Jingyu, HOU Yanxia, QI Rong, LIU Xiaobo, LIU Qingbin. Determination of trace copper, zinc and barium in nickel-based superalloy by inductively coupled plasma mass spectrometry with collision reaction cell. , 2022, 42(5): 15-20.

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http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.011643 或 http://yjfx.chinamet.cn/CN/Y2022/V42/I5/15

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