【引用本文】 阳国运, 唐裴颖, 张洁, 等. 电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗[J]. 岩矿测试, 2019, 38(2): 154-159. doi: 10.15898/j.cnki.11-2131/td.201805070055
YANG Guo-yun, TANG Pei-ying, ZHANG Jie, et al. Determination of Boron, Iodine, Tin and Germanium in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2019, 38(2): 154-159. doi: 10.15898/j.cnki.11-2131/td.201805070055

电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗

广西壮族自治区地质矿产测试研究中心, 广西 南宁 530023

收稿日期: 2018-05-07  修回日期: 2018-12-12  接受日期: 2019-01-01

作者简介: 阳国运, 高级工程师, 从事岩矿测试工作, 主要从事ICP-OES及ICP-MS检测。E-mail:731757094@qq.com

Determination of Boron, Iodine, Tin and Germanium in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry

Guangxi Geological and Mineral Testing Research Center, Nanning 530023, China

Received Date: 2018-05-07
Revised Date: 2018-12-12
Accepted Date: 2019-01-01

摘要:在多目标的配套方法中,硼、碘、锡、锗四个元素的分析涉及三个配套方法,发射光谱法测定硼、锡,原子荧光光谱法测定锗,分光光度法或电感耦合等离子体质谱法(ICP-MS)测定碘,分析成本高、检测效率低。本文建立了一种ICP-MS同时测定地球化学样品中硼、碘、锡、锗的方法。样品用过氧化钠熔矿,使难熔元素锡分解完全,熔盐经水提取后加入铼内标,再用阳离子交换树脂分离大量钠盐及大部分阳离子,保证了盐分满足质谱测定的要求。方法检出限分别为硼0.92μg/g、碘0.10μg/g、锡0.29μg/g、锗0.09μg/g,满足多目标测试要求。用国家一级标准物质验证,测定值与认定值一致,相对标准偏差(RSD,n=12)≤ 5%,适用于批量地球化学样品中硼、碘、锡、锗的测定,样品处理过程简便,检测效率高。

关键词: 碱熔, 阳离子树脂分离, 电感耦合等离子体质谱法, , , ,

要点

(1) 采用阳离子交换树脂吸附大量阳离子。

(2) 优化实验条件,提高测定效率及准确度。

(3) 整合配套方法,实现ICP-MS同时准确测定地球化学样品中的硼碘锡锗。

Determination of Boron, Iodine, Tin and Germanium in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry

ABSTRACT

BACKGROUND:

In the multi-objective method, the analysis of four elements of boron, iodine, tin and germanium involves three supporting methods. Boron and tin were determined by Emission Spectrometry, germanium was determined by Atomic Fluorescence Spectrometry, and iodine was determined by Spectrophotometry or Inductively Coupled Plasma-Mass Spectrometry. The analysis cost is high and the detection efficiency is low.

OBJECTIVES:

To establish an easy, highly efficient and precise, low-cost method for determination of boron, iodine, tin and germanium in geochemical samples by Inductively Coupled Plasma-Mass Spectrometry.

METHODS:

The sample is fused with sodium peroxide to completely decompose the refractory element tin. The molten salt is extracted by water and the internal standard is added, and then the cation exchange resin is used to separate a large amount of sodium salt and most of the cations, ensuring that the salt meets the requirements of mass spectrometry analysis.

RESULTS:

The element detection limits were 0.92μg/g, 0.10μg/g, 0.29μg/g, 0.09μg/g for boron, iodine, tin and germanium, respectively. The relative standard deviation (RSD, n=12) was smaller than 5%. The method was verified by certified reference materials, and the measured values were consistent with the certified values.

CONCLUSIONS:

The method is suitable for the determination of boron, iodine, tin and germanium in batch geochemical samples.

KEY WORDS: alkali fusion, cation resin separation, Inductively Coupled Plasma-Mass Spectrometry, boron, iodine, tin, germanium

HIGHLIGHTS

(1) Abundant cations were absorbed by cation exchange resin.

(2) The experimental conditions were optimized to improve the detection efficiency and accuracy.

(3) A simple, rapid and sensitive method for determination of boron, iodine, tin and germanium in geochemical samples by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) was investigated.

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电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗

阳国运, 唐裴颖, 张洁, 战大川, 覃盛, 何雨珊