铜业工程:2025(6):138-142
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碰撞反应池-三重四极杆ICP-MS测定纯铜中的痕量硫含量
刘宏, 桂诗浪
(江西铜业技术研究院有限公司, 江西 南昌 330096)
Determination of Trace Sulfur in Pure Copper by Collision/Reaction Cell Triple Quadrupole ICP-MS
LIU Hong,GUI Shilang
(Jiangxi Copper Technology Institute Co.,Ltd.,Nanchang 330096,China)
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投稿时间:2025-03-17    修订日期:2025-08-20
中文摘要: 硫(S)含量是纯铜的关键指标之一。由于严重的质谱干扰,常规四极杆ICP-MS难以准确测定纯铜中S元素的含量。本研究建立了碰撞反应池-电感耦合等离子体质谱法(ICP-MS/MS)测定纯铜样品中痕量硫含量的方法,并通过对比三重四极杆ICP-MS的四种不同检测模式,证明了在氧气反应-质量转移模式下检测S元素可以显著降低质谱干扰、提高信噪比。通过ICP-MS/MS测定硫元素的3种同位素(32S,33S和34S),建立的标准曲线R2系数皆优于0.999。由于33S同位素相比32S和34S同位素,丰度和信噪比较低,故选择32S和34S同位素进行定量分析。最终,ICP-MS/MS测定32S和34S得到的方法检出限分别为1.2 μg/g和1.1 μg/g,能够满足3N~5N纯铜S含量分析需求。所测定的两个纯铜标准样品的S含量均在误差范围内,与推荐值一致,表明了本方法的可靠性。
Abstract:Sulfur (S) content is a key index of pure copper. A dynamic reaction cell inductively coupled plasma mass spectrometry (ICP MS/MS) was developed for the determination of trace sulfur in pure copper samples. Due to serious mass spectrum interference, it is difficult to determine the content of S element in the sample by the common Q-ICP-MS. In this study, four different detection modes of NexION 5000G ICP-MS were compared, and the detection of S element in oxygen reaction mass-shift mode can significantly reduce the mass spectrum interference and improve the signal-to-noise ratio. Three isotopes of sulfur (32S, 33S and 34S) were determined by ICP MS/MS, and the correlation coefficients (R2) of the established standard curves were all better than 0.999. However, due to the low abundance and signal-to-noise ratio of 33S compared with 32S and 34S, 32S and 34S isotopes were chosen for quantitative analysis. Finally, the detection limits of the method obtained by ICP-MS/MS for 32S and 34S were 1.2 μg/g and 1.1 μg/g, respectively, which can meet the requirements of S content analysis of 3-5N pure copper. The S content values of two pure copper standard samples were consistent with the recommended value within the error range, which indicated the reliability of the method.
文章编号:20250317003     中图分类号:O655
基金项目:中央引导地方科技发展资金(20231ZDD02005); 稀贵稀散金属材料江西省重点实验室项目(2024SSY05051)
引用文本: 刘宏,桂诗浪.碰撞反应池-三重四极杆ICP-MS测定纯铜中的痕量硫含量[J].铜业工程,2025,(6):138-142