【引用本文】 吴磊, 刘义博, 王家松, 等. 高压密闭消解-电感耦合等离子体质谱法测定锰矿石中的稀土元素前处理方法研究[J]. 岩矿测试, 2018, 37(6): 637-643. doi: 10.15898/j.cnki.11-2131/td.201712060189
WU Lei , LIU Yi-bo , WANG Jia-song , et al. Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2018, 37(6): 637-643. doi: 10.15898/j.cnki.11-2131/td.201712060189

高压密闭消解-电感耦合等离子体质谱法测定锰矿石中的稀土元素前处理方法研究

1. 中国地质调查局天津地质调查中心, 天津 300170;

2. 中国地质调查局泥质海岸带地质环境重点实验室, 天津 300170

收稿日期: 2017-12-06  修回日期: 2018-06-11 

基金项目: 中国地质调查局地质调查项目"地质调查标准制修订与升级推广"(DD20160094)

作者简介: 吴磊,高级工程师,从事岩矿分析测试工作。E-mail:a_lei82@163.com。。

Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry

1. Tianjin Geological Survey Center, China Geological Survey, Tianjin 300170, China;

2. Key Laboratory of Muddy Coast Geo-Environment, China Geological Survey, Tianjin 300170, China

Received Date: 2017-12-06
Revised Date: 2018-06-11

摘要:高压密闭消解因称样量小、用酸量少、空白低等优点成为测定稀土元素前处理的主要方法。但锰矿石组分复杂,锰含量差别较大且具有多种不同价态,常含有伴(共)生金属和其他杂质,该方法采用常规酸溶体系很难将其消解完全,造成ICP-MS测试结果不准确。本文从样品前处理消解效果出发,选择锰矿石标准物质GBW07261、GBW07263、GBW07266和一个锰矿石样品,试验了三种酸溶前处理方法对锰矿石稀土元素测试的影响。结果表明:方法一(氢氟酸-硝酸密闭消解,硝酸提取)不能将锰矿石样品完全消解,测定值偏低0.28%~61.31%;方法二(氢氟酸-硝酸-双氧水密闭消解,硝酸-双氧水复溶,硝酸提取)和方法三(氢氟酸-硝酸密闭消解,盐酸复溶,硝酸提取)均可将锰矿石样品消解完全,用ICP-MS测定稀土元素的数据较为接近,与传统的过氧化钠熔融ICP-MS法测定值吻合。但实验过程中发现对于锰含量较高的样品,方法三需多次重复加入盐酸复溶后方可将样品消解完全,而方法二复溶一次即可。因此,方法二对锰矿石样品的消解效率更高,精密度好(0.96%~2.68%),加标回收率在95.4%~107%之间,更适用于锰矿石中稀土元素的分析。

关键词: 锰矿石, 稀土元素, 高压密闭消解, 双氧水, 电感耦合等离子体质谱法

Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry

KEY WORDS: manganese ore, rare earth elements, high-pressure closed digestion, hydrogen peroxide, Inductively Coupled Plasma-Mass Spectrometry

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高压密闭消解-电感耦合等离子体质谱法测定锰矿石中的稀土元素前处理方法研究

吴磊, 刘义博, 王家松, 吴良英, 张楠, 王娜