高压密闭消解-电感耦合等离子体质谱法测定和田玉中15种稀土元素

周安丽; 武志远; 宁海龙; 王东; 杨丽; 吕新明

doi:10.15898/j.cnki.11-2131/td.201907170106

高压密闭消解-电感耦合等离子体质谱法测定和田玉中15种稀土元素

Determination of 15 Rare Earth Elements in Hetian Jade by Inductively Coupled Plasma-Mass Spectrometry with High-pressure Closed Digestion

摘要

摘要: 和田玉的稀土元素丰富，准确测定稀土元素含量对于揭示和田玉成矿物质来源、成矿流体的性质和矿床成因具有重要的意义。本文通过比较硝酸-氢氟酸、四硼酸锂-偏硼酸锂碱熔两种前处理方法，确定了使用硝酸-氢氟酸溶样，再采用电感耦合等离子体质谱法(ICP-MS)测定和田玉中钇镧铈镨钕钐铕钆铽镝钬铒铥镱镥15种稀土元素的含量。为降低基体效应，以¹⁰³Rh和⁴⁹In作内标补偿基体效应和校正灵敏度漂移，样品检出限为0.0008~0.0091μg/L，回收率为101.0%~120.0%，精密度(RSD)为0.55%~1.83%(n=11)。本方法的用酸量少，空白值低，应用于不同地区和田玉的分析，其稀土元素的配分模式特征为右倾型轻稀土富集，初步探讨的稀土元素丰度特征可为研究主产区宝玉石的矿床成因提供依据。

Abstract:
BACKGROUNDThere are abundant rare earth elements in Hetian jade. The accurate determination of the content of rare earth elements is of great significance for revealing the source of ore-forming materials, the nature of ore-forming fluids and the genesis of the deposit.
OBJECTIVESTo compare the different acid systems in microware digestion and investigate the elimination test of polyatomic interferences, so as to develop a method for the determination of REE in Hetian jade by inductively coupled plasma-mass spectrometry (ICP-MS) with microwave digestion.
METHODSAfter comparing the efficiency of HNO₃-HF acid dissolution and Li₂B₄O₇-LiBO₂ fusion, the Hetian jade samples were digested by HNO₃-HF. Fifteen rare earth elements were determined by ICP-MS. ¹⁰³Rh and ⁴⁹In are used as internal isotopes to complement matrix effect and correct sensitivity drift, in order to reduce matrix effect.
RESULTSThe detection limits of the method were 0.0008-0.0091μg/L, whereas the recoveries were 101.0%-120.0%. The relative standard deviation was 0.55%-1.83%(n=11).
CONCLUSIONSThis method uses less acid and has a low blank value. It is applied to the analysis of Hetian jade in different regions. The distribution pattern of rare earth elements is characterized by right-inclined light rare earth enrichment, which provides constraints on the genesis of the jade deposit.

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