基于ICP-MS的球团矿中痕量元素检测方法及其优化
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贾雷(1990—),男,工程师,从事电感耦合等离子体质谱分析方面的研究工作。

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TF046.6;O657.31

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辽宁省教育厅高校基本科研项目(JYTQN2023016);辽宁省菱镁矿高值利用工程研究中心基金资助项目(LMNY2024020202)


Detection method and optimization of trace elements in iron ore pellets by ICP-MS
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    摘要:

    球团矿中P、S、As、Sn、Cu、Sb、Pb、Zn、Cr、Cd等10种痕量元素对钢材的热脆性、耐腐蚀性及机械强度具有显著负面影响,因此对其在球团原料中的含量进行严格监控十分重要。本文建立一种高效、准确的电感耦合等离子体质谱分析(inductively coupled plasma mass spectrometry,ICP-MS)方法,用于测定上述元素。试验采用微波消解对球团矿样品进行前处理,确保难溶矿物相完全溶解;针对硫在常规ICP-MS中灵敏度低的问题,优化碰撞反应池技术条件以消除多原子离子干扰并提高信噪比;在其余元素检测中,通过动能歧视模式有效克服基体干扰,并采用Sc-In-Tb混合内标校正基体效应与信号漂移保证测定结果的准确性。结果表明:各元素的相关系数均大于0.999 0,检出限为0.02~1.56μg/g,定量限为0.06~4.68μg/g,精密度为1.95%~4.12%,加标回收率为95.2%~103.5%。本文研究方法能为球团矿的质量控制及炼钢残余元素的风险评估提供可靠的技术支撑。

    Abstract:

    Ten trace elements including P,S,As,Sn,Cu,Sb,Pb,Zn,Cr and Cd in iron ore pellets has significant negative effects on the hot brittleness,corrosion resistance,and mechanical strength of steel,therefore,it is very important to strictly monitor their content in pellet raw materials. In this paper,an efficient and accurate inductively coupled plasma mass spectrometry( ICP-MS) method is established for the determination of the aforementioned elements. In the test,the microwave digestion was used for pretreatment of iron ore pellet samples to ensure complete dissolution of refractory mineral phases. As for the low sensitivity of sulfur in conventional ICP-MS,the collision/reaction cell technology conditions were optimized to eliminate polyatomic ion interferences and enhance the signal-to-noise ratio. In the detection of the remaining elements,the matrix interferences were effectively overcome through kinetic energy discrimination mode. Additionally,a mixed internal standard of Sc-In-Tb was used to correct the matrix effects and signal drift,ensuring the accuracy of the determination results. The results show that the correlation coefficients for all elements exceed 0. 999 0,with detection limits ranging from 0.02 to 1.56 μg/g,quantification limits from 0. 06 to 4.68 μg/g,precision between 1.95% and 4.12%,and spiked recoveries between 95.2% and 103.5%. The method studied in this paper can provide reliable technical support for quality control of iron ore pellets and risk assessment of residual elements in steelmaking.

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贾雷,左修源,朱明芳,李雨蒙.基于ICP-MS的球团矿中痕量元素检测方法及其优化[J].工程建设,2025,50(6):76-83

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  • 收稿日期:2025-06-13
  • 最后修改日期:2025-08-18
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  • 在线发布日期: 2025-11-16
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