Determination of rare earth elements in antimony ore by open acid dissolution-inductively coupled plasma mass spectrometry
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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。
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关键词:
- 锑矿石 /
- 稀土元素 /
- 除锑 /
- 电感耦合等离子体质谱法
Abstract: s:At present, the determination of rare earth elements mainly adopts inductively coupled plasma massspectrometry, and the sample pretreatment mainly adopts alkaline fusion and closed acid dissolution, but both ofthese pretreatment methods take a long time and are not suitable for batch sample processing. Open acid dissolu tion is a simple method to dissolve samples in a polytetrafluoroethylene beaker. It takes a short time and is themost sample processing method. It is widely used in the pretreatment of rocks, soils and various minerals. Anti mony ore usually contains high antimony content, which will cause pollution to the instrument after direct mea surement. 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, finallymeasured by inductively coupled plasma mass spectrometry.The internal standard rhodium was used for mass in terference correction to compensate for the matrix suppression effect and the correction sensitivity drift. The de tection limit was 0.006~0.037 μg/g, and the RSD (n=12) was between 0.57% and 7.89%. The results show thatthis method is suitable for the determination of rare earth elements in antimony ore. -
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