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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 | |
| 引用本文： | 张磊,周伟,朱云,屈文俊,樊兴涛,李迎春.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. |
| 作者姓名： | 张磊 周伟 朱云 屈文俊 樊兴涛 李迎春 |
| 作者单位： | 国家地质实验测试中心 |
| 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） |
| 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(Mg~(2+)、NH_4~+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 |
| 收稿时间： | 2017/12/11 0:00:00 |
| 修稿时间： | 2018/5/2 0:00:00 |
An Optimized Method for Determination of Ionic-phase Rare Earth Elements by ICP-MS Using Ammonium Sulfate Leaching |
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| ZHANG Lei,ZHOU Wei,ZHU Yun,QU Wen-jun,FAN Xing-tao and LI Ying-chun.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. | |
| Authors: | ZHANG Lei ZHOU Wei ZHU Yun QU Wen-jun FAN Xing-tao and LI Ying-chun |
| Institution: | National Research Center for Geoanalysis, Beijing 100037, China,National Research Center for Geoanalysis, Beijing 100037, China,National Research Center for Geoanalysis, Beijing 100037, China,National Research Center for Geoanalysis, Beijing 100037, China,National Research Center for Geoanalysis, Beijing 100037, China and National Research Center for Geoanalysis, Beijing 100037, China |
| 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 content 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 limit was 0.05-5.11 ng/g, and the relative standard deviation (RSD) was 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 verified 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. |
| Keywords: | ion-adsorption type rare earth ionic-phase rare earth elements ammonium sulfate leaching rate Inductively Coupled Plasma-Mass Spectrometry |
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