【引用本文】 门倩妮, 沈平, 甘黎明, 等. 敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪[J]. 岩矿测试, 2020, 39(1): 59-67. doi: 10.15898/j.cnki.11-2131/td.201905100060
MEN Qian-ni , SHEN Ping , GAN Li-ming , et al. Determination of Rare Earth Elements and Nb, Ta, Zr, Hf in Polymetallic Mineral Survey Samples by Inductively Coupled Plasma-Mass Spectrometry Coupled with Open Acid Dissolution and Lithium Metaborate Alkali Fusion[J]. Rock and Mineral Analysis, 2020, 39(1): 59-67. doi: 10.15898/j.cnki.11-2131/td.201905100060

敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪

1. 中国人民武装警察部队黄金部队第五支队, 陕西 西安 710100;

2. 甘肃智广地质工程勘察设计有限公司, 甘肃 兰州 730010

收稿日期: 2019-05-10  修回日期: 2019-07-05 

作者简介: 门倩妮,硕士,从事地质样品的分析测试工作。E-mail:menqianni-6019@163.com。。

Determination of Rare Earth Elements and Nb, Ta, Zr, Hf in Polymetallic Mineral Survey Samples by Inductively Coupled Plasma-Mass Spectrometry Coupled with Open Acid Dissolution and Lithium Metaborate Alkali Fusion

1. No.5 Gold Geological Party, Chinese People's Armed Police Force, Xi'an 710100, China;

2. Gansu Zhiguang Geological Engineering Survry and Design Co. Ltd., Lanzhou 730010, China

Received Date: 2019-05-10
Revised Date: 2019-07-05

摘要:用ICP-MS测定地质样品中的稀土及难熔元素,混合酸敞开酸溶法和碱熔融法是两种主要的溶样方法。但地质样品组分复杂,元素之间存在相互共生的现象,对于特殊元素、特殊样品用传统酸溶法会造成部分元素消解不完全,使测定结果不准确;而碱熔法的操作过程繁琐,且溶液盐度高,易产生基体干扰和堵塞仪器进样系统。本文改进了传统四酸和五酸体系,采用氢氟酸-硝酸-硫酸敞开酸溶体系,用国家一级标准物质制作标准曲线测定15种稀土元素,方法准确度(ΔlgC)为0.001~0.027。同时改进了偏硼酸锂碱熔法,样品用偏硼酸锂碱熔提取,加入氢氧化钠调节溶液至碱性条件,所测元素与偏硼酸锂共沉淀后过滤分离熔剂,再用硝酸复溶测定稀土及铌钽锆铪等19种元素。两种溶样方法的测定值与认定值的相对误差为1.09%~9.30%。将混合酸敞开酸溶法测定稀土元素、偏硼酸锂碱熔法测定铌钽锆铪的结果与其他实验室密闭酸溶法相比,两组数据的相对偏差为0.13%~15.32%。本实验表明,混合酸敞开酸溶法适用于测定地质样品中的稀土元素,偏硼酸锂碱熔法不仅适用于测定地质样品中的稀土元素及铌钽锆铪,也适用于测定如古老高压变质岩石及铝含量高的样品中的铌钽锆铪。

关键词: 多金属矿, 稀土元素, , , , , 氢氟酸-硝酸-硫酸敞开酸溶, 偏硼酸锂碱熔, 氢氧化钠, 电感耦合等离子体质谱法

Determination of Rare Earth Elements and Nb, Ta, Zr, Hf in Polymetallic Mineral Survey Samples by Inductively Coupled Plasma-Mass Spectrometry Coupled with Open Acid Dissolution and Lithium Metaborate Alkali Fusion

KEY WORDS: polymetallic minerals, rare earth elements, Nb, Ta, Zr, Hf, HF-HNO3-H2SO4 open dissolution, lithium metaborate alkali fusion, sodium hydroxide, inductively coupled plasma-mass spectrometry

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敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪

门倩妮, 沈平, 甘黎明, 冯博鑫