敞开酸溶—电感耦合等离子体质谱法测定锑矿石中的稀土元素  

Determination of rare earth elements in antimony ore by open acid dissolution-inductively coupled plasma mass spectrometry

作　　者：曾江萍 王家松 王娜[1,2] 郑智慷 王力强 张楠 ZENG Jiang-ping;WANG Jia-song;WANG Na;ZHENG Zhi-kang;WANG Li-qiang;ZHANG Nan(Tianjin Institute of Geology and Mineral Resources,China Geological Survey,Tianjin 300170,China;North China Geological Science and Technology Innovation Center,Tianjin 300170,China;Key Laboratory of Coast Geo-Environment,China Geological Survey,Tianjin 300170,China)

机构地区：[1]中国地质调查局天津地质调查中心,天津300170 [2]华北地质科技创新中心,天津300170 [3]中国地质调查局海岸带地质环境重点实验室,天津300170

出　　处：《华北地质》2021年第4期80-84,共5页North China Geology

基　　金：中国地质调查局项目“地质调查标准化与标准值修订(中国地质调查局天津地质调查中心)(DD20190472)”。

摘　　要：目前测定稀土元素主要采用电感耦合等离子体质谱法,样品前处理主要采用碱熔和封闭酸溶,但这两种前处理方式均耗时较长,不适合批量样品处理,敞开酸溶是一种操作较简便的方法,在聚四氟乙烯烧杯中溶解样品,用时较短,是处理样品最多的方法,广泛应用于岩石、土壤及各种矿物的样品前处理。锑矿石通常含锑量较高,直接测定后会对仪器造成污染,本文通过加入盐酸和氢溴酸除锑后,经硝酸-氢氟酸-硫酸混酸消解,制成王水介质溶液,建立了电感耦合等离子体质谱法测定锑矿石中稀土元素的方法。用内标铑进行质谱干扰校正,弥补了基体抑制效应和校正灵敏度漂移,检出限为0.006~0.037μg/g,RSD(n=12)在0.57%~7.89%之间。结果表明,本法适用于锑矿石中稀土元素的测定。At present, the determination of rare earth elements mainly adopts inductively coupled plasma mass spectrometry, and the sample pretreatment mainly adopts alkaline fusion and closed acid dissolution, but both of these pretreatment methods take a long time and are not suitable for batch sample processing. Open acid dissolution is a simple method to dissolve samples in a polytetrafluoroethylene beaker. It takes a short time and is the most sample processing method. It is widely used in the pretreatment of rocks, soils and various minerals. Antimony ore usually contains high antimony content, which will cause pollution to the instrument after direct measurement. In this paper, after adding hydrochloric acid and hydrobromic acid to remove antimony, samples were digested by nitric acid-hydrofluoric acid-sulfuric acid mixed acid to prepare aqua regia medium solution,finally measured by inductively coupled plasma mass spectrometry.The internal standard rhodium was used for mass interference correction to compensate for the matrix suppression effect and the correction sensitivity drift. The detection limit was 0.006~0.037 μg/g, and the RSD(n=12) was between 0.57% and 7.89%. The results show that this method is suitable for the determination of rare earth elements in antimony ore.

关 键 词：锑矿石 稀土元素 除锑 电感耦合等离子体质谱法 

分 类 号：P575[天文地球—矿物学] O657.31[天文地球—地质学]