【引用本文】 张磊, 周伟, 朱云, 等. 硫酸铵溶液淋滤-电感耦合等离子体质谱测定离子相稀土分量的方法优化[J]. 岩矿测试, 2018, 37(5): 518-525. doi: 10.15898/j.cnki.11-2131/td.201712110192
ZHANG Lei, ZHOU Wei, ZHU Yun, et al. An Optimized Method for Determination of Ionic-phase Rare Earth Elements by ICP-MS Using Ammonium Sulfate Leaching[J]. Rock and Mineral Analysis, 2018, 37(5): 518-525. doi: 10.15898/j.cnki.11-2131/td.201712110192

硫酸铵溶液淋滤-电感耦合等离子体质谱测定离子相稀土分量的方法优化

国家地质实验测试中心, 北京 100037

收稿日期: 2017-12-11  修回日期: 2018-05-02  接受日期: 2018-06-11

基金项目: 中国地质科学院基本科研业务费项目(CSJ201602);中国地质调查局地质调查工作项目(DD20179152)

作者简介: 张磊, 硕士, 工程师, 从事岩矿测试技术应用与研究。E-mail:zhang.lei.198806@163.com

通讯作者: 周伟, 工程师, 从事岩矿测试技术应用与研究。E-mail:zhouwei@cags.ac.cn

An Optimized Method for Determination of Ionic-phase Rare Earth Elements by ICP-MS Using Ammonium Sulfate Leaching

National Research Center for Geoanalysis, Beijing 100037, China

Corresponding author: ZHOU Wei, zhouwei@cags.ac.cn

Received Date: 2017-12-11
Revised Date: 2018-05-02
Accepted Date: 2018-06-11

摘要:离子吸附型稀土中离子相稀土的准确测定对稀土矿体资源评价具有重要意义。离子相稀土以羟基或水合羟基的形式吸附在黏土矿物上,可与强电解质(Mg2+、NH4+等)交换解吸进入溶液。前人以硫酸铵为淋滤液,实现了离子相稀土的解吸、提取,但在溶液浓度、浸取过程等方面选择各异,淋滤浸取率(60%~90%)差异大,未形成高效、统一的浸取方法,不利于离子相稀土元素的精确测定。本文通过对比实验规范了硫酸铵淋滤离子相稀土的各项淋滤参数(固液比、硫酸铵浓度、样品最佳称样量、浸泡时间),减少了淋滤过程中离子相稀土的损失,浸取率达到88%~98%,进而利用ICP-MS测定离子相稀土分量。方法检出限为0.05~5.11 ng/g;三类岩性离子吸附型稀土样品的精密度为:火山岩1.80%~10.01%,变质岩1.06%~7.27%,沉积岩1.72%~7.58%。协作实验室的分析结果验证了本方法的可靠性和准确性。本方法操作简便,分析效率高,为建立相关的行业标准乃至国家标准奠定了基础。

关键词: 离子吸附型稀土, 离子相稀土, 硫酸铵, 淋滤浸取率, 电感耦合等离子体质谱法

要点

(1) 选取南岭地区离子吸附型稀土样品进行不同条件下的淋滤浸取实验。

(2) 明确了淋滤实验中固液比、硫酸铵溶液浓度、称样量、淋滤浸取时间等实验条件,实现高效浸取。

(3) 利用ICP-MS实现离子相稀土元素的精确测定。

An Optimized Method for Determination of Ionic-phase Rare Earth Elements by ICP-MS Using Ammonium Sulfate Leaching

ABSTRACT

BACKGROUND:

The accurate determination of ionic phase rare earths in ion-adsorption rare earths is of great significance for the evaluation of rare earth ore bodies. Ionic phase rare earths are adsorbed on clay minerals in the form of hydroxyl or hydrated hydroxyls and can be exchanged and desorbed with strong electrolytes (Mg2+, NH4+, etc.) into solution. The former used ammonium sulfate as the leachate to achieve the desorption and extraction of rare earth ions in the ion phase, but the solution concentration, leaching process and other aspects of choice, leaching rates (60% to 90%) are different. There is no efficient and uniform leaching method conducive to the accurate determination of ionic phase rare earth elements.

OBJECTIVES:

To establish a high-efficiency leaching process by ammonium sulfate solution and determine the accurate contents of ionic-phase rare earth elements.

METHODS:

The leaching parameters (solid-to-liquid ratio, ammonium sulfate concentration, best sample weight, and soaking time) of rare-earth ions by ammonium sulfate were standardized through comparative experiments, which reduced the loss of ionic phase rare earth during leaching. The leaching rates were from 88% to 98%, and ICP-MS was used to accurately determine the ion phase rare earth component.

RESULTS:

The detection limits are 0.05-5.11 ng/g, and the relative standard deviations (RSDs) are 1.80%-10.01% for volcanic rock, 1.06%-7.27% for metamorphic rock, and 1.72%-7.58% for sedimentary rock.

CONCLUSIONS:

The analytical results of the collaborative laboratory verify the reliability and accuracy of the method. This method is easy to operate and has high analysis efficiency. It provides the base for the establishment of relevant industry standards and national standards.

KEY WORDS: ion-adsorption type rare earth, ionic-phase rare earth elements, ammonium sulfate, leaching rate, Inductively Coupled Plasma-Mass Spectrometry

HIGHLIGHTS

(1) Ion-adsorption-type rare earth samples were selected from the Nanling region and leached with ammonium sulfate solution under different conditions.

(2) The leaching conditions such as solid-to-liquid ratio, concentration of ammonium sulfate and leaching time were determined.

(3) The accurate contents of ionic-phase rare earth elements by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) were determined.

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硫酸铵溶液淋滤-电感耦合等离子体质谱测定离子相稀土分量的方法优化

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