【引用本文】 刘贵磊, 许春雪, 陈宗定, 等. 氟化氢铵快速分解-电感耦合等离子体质谱法测定含刚玉铝土矿中锂镓锆稀土等痕量元素[J]. 岩矿测试, 2020, 39(5): 667-678. doi: 10.15898/j.cnki.11-2131/td.202003120031
LIU Gui-lei , XU Chun-xue , CHEN Zong-ding , et al. Determination of Lithium, Gallium, Zirconium, Rare Earth Elements and Other Trace Elements in Corundum-bearing Bauxite by Inductively Coupled Plasma-Mass Spectrometry with Rapid Decomposition of Ammonium Bifluoride[J]. Rock and Mineral Analysis, 2020, 39(5): 667-678. doi: 10.15898/j.cnki.11-2131/td.202003120031

氟化氢铵快速分解-电感耦合等离子体质谱法测定含刚玉铝土矿中锂镓锆稀土等痕量元素

国家地质实验测试中心, 北京 100037

收稿日期: 2020-03-12  修回日期: 2020-04-08 

基金项目: 中国地质调查局地质调查项目(DD20190323,DD20190475);国家自然科学基金项目(21601041)

作者简介: 刘贵磊,博士,助理研究员,主要从事岩矿测试分析和标准化工作。E-mail:liuguilei2008@163.com。。

Determination of Lithium, Gallium, Zirconium, Rare Earth Elements and Other Trace Elements in Corundum-bearing Bauxite by Inductively Coupled Plasma-Mass Spectrometry with Rapid Decomposition of Ammonium Bifluoride

National Research Center for Geoanalysis, Beijing 100037, China

Received Date: 2020-03-12
Revised Date: 2020-04-08

摘要:铝土矿中常伴有锂、镓、锆、稀土等有用组分,完全提取并准确测定其含量对于铝土矿资源综合评价和综合利用具有重要意义。然而铝土矿中常常含有少量刚玉,常规的四酸、五酸和封闭压力酸溶法对其分解不完全,导致测定结果偏低。本文采用氟化氢铵作熔剂,高温下在旋盖PFA小瓶中分解样品,通过在熔样过程中使用少量硫酸,对不同熔矿温度、消解时间及试剂用量等因素详细考察,确定了最佳熔矿条件[200℃,3h,试样比4:1(称样量50mg)],建立了氟化氢铵分解-电感耦合等离子体质谱法测定含刚玉铝土矿中37种痕量元素的分析方法。本方法能快速、有效地分解含刚玉铝土矿,经三种铝土矿国家标准物质GBW07177、GBW07181和GBW07182验证,并与四酸、五酸和封闭压力酸溶法的测定结果对比,三种标准物质中Li、Ga、Sr、Zr、Pb等9种元素的回收率分别在95.0%~115.0%、90.0%~110.0%和90.0%~110.0%之间,结果与认定值相符。同时,本方法实现了铝土矿(Al2O3含量在42.97%~90.36%之间)中Al、Ti、P等主量元素的精确分析,进一步验证了其用来测定铝土矿中痕量元素的准确性。方法检出限为0.002~0.43μg/g,与传统硝酸-氢氟酸密闭消解法的检出限(0.000~0.48μg/g)基本相当,精密度在1.14%~8.84%之间,能够满足铝土矿中痕量元素的分析要求。

关键词: 氟化氢铵, 快速分解, 电感耦合等离子体质谱法, 含刚玉铝土矿, 痕量元素

Determination of Lithium, Gallium, Zirconium, Rare Earth Elements and Other Trace Elements in Corundum-bearing Bauxite by Inductively Coupled Plasma-Mass Spectrometry with Rapid Decomposition of Ammonium Bifluoride

KEY WORDS: ammonium bifluoride, rapid decomposition, inductively coupled plasma-mass spectrometry, corundum-bearing bauxite, trace elements

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氟化氢铵快速分解-电感耦合等离子体质谱法测定含刚玉铝土矿中锂镓锆稀土等痕量元素

刘贵磊, 许春雪, 陈宗定, 温宏利