电感耦合等离子质谱(ICP-MS)法测定稀土矿石中稀土元素  

Determination of Rare Earth Elements in Rare Earth Ores by Inductively Coupled Plasma Mass Spectrometry(ICP-MS)

作　　者：徐进力[1,2,3] 陈润莎 陈卫明 张鹏鹏[1,2,3] 杜雪苗 白金峰 XU Jinli;CHEN Runsha;CHEN Weiming;ZHANG Pengpeng;DU Xuemiao;BAI Jinfeng(Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang,Hebei 065000,China;UNESCO International Centre on Global-Scale Geochemistry,Langfang,Hebei 065000,China;Key Laboratory of Ceochemical Cycling of Carbon and Mercury in the Earth's Critical Zone,Chinese Academy of Gcological Sciences,Langfang,Hebei 065000,China)

机构地区：[1]中国地质科学院地球物理地球化学勘查研究所,河北廊坊065000 [2]联合国教科文组织全球尺度地球化学国际研究中心,河北廊坊065000 [3]地球表层碳-汞地球化学循环重点实验室,河北廊坊065000

出　　处：《中国无机分析化学》2025年第5期644-651,共8页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点研发计划项目(2021YFC2903001);中国地质科学院基本科研业务费专项资金资助项目(AS2020J04)。

摘　　要：稀土元素(REE)是现代高科技领域不可或缺的功能材料,稀土矿石中稀土成分的准确分析对于资源开发和应用具有重要意义。通过考察两种稀土矿石样品的前处理方法:氢氧化钠-过氧化钠体系碱熔法和盐酸-硝酸-氢氟酸-高氯酸-硫酸(五酸)敞开酸溶法,并利用电感耦合等离子体质谱仪(ICP-MS)对稀土元素进行测定。实验表明,碱熔法在消解复杂基体的稀土矿石样品时具有更高的消解效率和更好的精密度(RSD≤4%),尽管其样品空白本底值略高于五酸消解法,基本不影响分析结果的准确度。通过优化仪器工作参数,建立了准确度、精密度高的分析方法。方法的检出限低(如Y为0.02μg/g,Lu为0.001μg/g),精密度良好(RSD小于3%),相对误差(RE)小于11%,适用于稀土矿石中稀土元素的准确测定。研究表明,碱熔法是稀土矿石样品前处理的优选方法,而五酸消解法可作为对比验证手段,可确保分析数据的可靠性。ICP-MS的高效性和准确性使其成为稀土元素分析的理想工具,为稀土资源的开发和研究提供了有力的技术支持。Rare earth elements(REEs) are essential functional materials in modern high-tech fields.The precise analysis of REE composition in rare earth ores is crucial for resource development and application.This research explored two pretreatment methods for rare earth ore samples:alkaline fusion using a sodium hydroxide-sodium peroxide system and open acid digestion with a hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid-sulfuric acid(five-acid) mixture.Inductively coupled plasma mass spectrometry(ICP-MS) was utilized for REE determination.Experimental findings indicated that the alkaline fusion method demonstrated higher digestion efficiency and better precision(RSD ≤ 4%) for rare earth ore samples with complex matrices.Although its sample blank background values were slightly higher than those of the five-acid digestion method,this difference had little effect on analytical accuracy.By optimizing instrumental parameters,a highly accurate and precise analytical method was developed.It had low detection limits(e.g.,0.02 μg/g for Y and 0.001 μg/g for Lu),excellent precision(RSD<3%),and relative errors(RE) below 11%.The study determined that alkaline fusion is the preferred pretreatment method for rare earth ore analysis,while the five-acid digestion method can be used as a reliable comparative validation tool to ensure data reliability.The high efficiency and accuracy of ICP-MS solidify its position as an ideal analytical technique for REE determination,offering crucial technical support for rare earth resource exploration and research.This methodology effectively overcomes the challenges of accurately quantifying trace REEs in geologically complex matrices.

关 键 词：稀土元素 稀土矿石 碱熔 酸溶 电感耦合等离子体质谱 

分 类 号：O657.63[理学—分析化学]