【引用本文】 张楠, 徐铁民, 吴良英, 等. 微波消解-电感耦合等离子体质谱法测定海泡石中的稀土元素[J]. 岩矿测试, 2018, 37(6): 644-649. doi: 10.15898/j.cnki.11-2131/td.201803160023
ZHANG Nan, XU Tie-min, WU Liang-ying, et al. Determination of Rare Earth Elements in Sepiolite by ICP-MS Using Microwave Digestion[J]. Rock and Mineral Analysis, 2018, 37(6): 644-649. doi: 10.15898/j.cnki.11-2131/td.201803160023

微波消解-电感耦合等离子体质谱法测定海泡石中的稀土元素

中国地质调查局天津地质调查中心, 天津 300170

收稿日期: 2018-03-16  修回日期: 2018-05-03  接受日期: 2018-06-11

基金项目: 国家重点研发计划项目“国家质量基础的共性技术研究与应用”(2016YFF0201103);中国地质调查局地质调查工作项目(DD20160094)

作者简介: 张楠, 高级工程师, 从事岩石矿物分析研究。E-mail:nan5460@126.com

Determination of Rare Earth Elements in Sepiolite by ICP-MS Using Microwave Digestion

Tianjin Center of Geological Survey, China Geological Survey, Tianjin 300170, China

Received Date: 2018-03-16
Revised Date: 2018-05-03
Accepted Date: 2018-06-11

摘要:海泡石是一种纤维状含水的富镁硅酸盐黏土矿,其中的稀土元素含量在1×10-7~1×10-5之间,目前还没有建立海泡石中稀土元素的国家标准分析方法。测定岩石中的稀土元素主要是采用电感耦合等离子体质谱法(ICP-MS),样品前处理一般采用封闭溶矿和碱熔,但这两种处理方法耗时较长,效率不高。本文通过比较硝酸-氢氟酸-过氧化氢、硝酸-氢氟酸、硝酸-过氧化氢三种样品前处理方法,确定使用硝酸-氢氟酸溶矿,然后进行微波消解同时赶去氢氟酸,避免氢氟酸与稀土元素生成难溶的氟化物,再采用ICP-MS法测定15种稀土元素的含量。由于海泡石中的镁含量较高,为降低基体效应,以103Rh和185Re作内标补偿基体效应和校正灵敏度漂移,各元素测定值的准确性显著提高,回收率为91.2%~110.9%,检出限为0.002~0.011 μg/L,精密度≤ 2.79%。本方法与封闭酸溶ICP-MS法的分析结果吻合较好,且用酸量少(7 mL),溶矿效率高(1 h),检出限更低。

关键词: 海泡石, 稀土元素, 微波消解, 硝酸-氢氟酸, 电感耦合等离子体质谱法

要点

(1) 采用微波消解高效溶样方式,ICP-MS法测定了海泡石中15种稀土元素的含量。

(2) 比较了硝酸-氢氟酸-过氧化氢、硝酸-氢氟酸、硝酸-过氧化氢三种溶样体系对微波消解海泡石的影响。

(3) 本方法用酸量少,溶矿效率高,分析结果与封闭酸溶ICP-MS法吻合较好。

Determination of Rare Earth Elements in Sepiolite by ICP-MS Using Microwave Digestion

ABSTRACT

BACKGROUND:

Sepiolite is a fibrous hydrous magnesium rich silicate clay mineral with the content of rare earth elements between 1×10-7 and 1×10-5. There is no national standard method for the determination of rare earth elements in sepiolite. Determination of rare earth elements in rocks commonly uses ICP-MS. Sample pretreatments generally use closed digestion and alkaline fusion, but these two treatments are time consuming and inefficient.

OBJECTIVES:

To find an efficient dissolution method for the determination of 15 rare earth elements in sepiolite.

METHODS:

By comparing three sample pretreatment methods of nitrate hydrofluoric acid hydrogen peroxide, nitric acid-hydrofluoric acid and nitric-acid hydrogen peroxide, the nitric acid-hydrofluoric acid solution system was selected. Microwave digestion was carried out and the hydrofluoric acid was driven off to avoid the formation of insoluble fluorides from the hydrofluoric acid. The content of 15 rare earth elements was determined by ICP-MS.

RESULTS:

Due to the high content of magnesium in sepiolite, two internal standards of 103Rh and 185Re are selected to compensate for the drift of analytical signals and to correct matrix effects. The recoveries of the method range from 91.2% to 110.9%. The detection limits are 0.002-0.011 μg/L, and the precisions are 0.81%-2.79%.

CONCLUSIONS:

The result of this method is in good agreement with that of the closed acid-digestion ICP-MS method, and with a small amount of acid (7 mL), high digestion efficiency (1 h), and a lower detection limit.

KEY WORDS: sepiolite, rare earth elements, microwave digestion, nitric acid-hydrofluoric acid, Inductively Coupled Plasma-Mass Spectrometry

HIGHLIGHTS

(1) The contents of 15 rare earth elements in sepiolite were determined by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) using microwave digestion.

(2) Three dissolving systems were compared to evaluate the dissolution effect of nitric acid-hydrofluoric acid-hydrogen peroxide, nitric acid-hydrofluoric acid and nitric acid-hydrogen peroxide.

(3) The method used less acid and had higher dissolution efficiency and the analytical results were in good agreement with those of the closed acid dissolution ICP-MS method.

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微波消解-电感耦合等离子体质谱法测定海泡石中的稀土元素

张楠, 徐铁民, 吴良英, 魏双, 方蓬达, 王家松