顶空固相微萃取-电热解塞曼原子吸收光谱法测定水中总汞

引用本文: 赵健, 张林楠, 雷永乾, 潘佳钏, 郭鹏然. 顶空固相微萃取-电热解塞曼原子吸收光谱法测定水中总汞[J]. 分析化学, 2021, 49(8): 1393-1401. doi: 10.19756/j.issn.0253-3820.211133 shu

Citation: ZHAO Jian, ZHANG Lin-Nan, LEI Yong-Qian, PAN Jia-Chuan, GUO Peng-Ran. Determination of Trace Total Mercury in Water by Headspace Solid Phase Microextraction and Electropyrolytic Zeeman Atomic Absorption Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2021, 49(8): 1393-1401. doi: 10.19756/j.issn.0253-3820.211133 shu

顶空固相微萃取-电热解塞曼原子吸收光谱法测定水中总汞

1.
沈阳工业大学环境与化学工程学院, 沈阳 110870;
2.
广东省科学院测试分析研究所(中国广州分析测试中心), 广东省化学危害应急检测技术重点实验室, 广州 510070;
3.
广东省科学院测试分析研究所(中国广州分析测试中心), 广东省水环境污染在线监测工程技术研究中心, 广州 510070

通讯作者: 郭鹏然,E-mail:prguo@fenxi.com.cn

基金项目:
国家自然科学基金项目（No.21777150）、广东省重点领域研究计划项目（No.2020B1111350002）和广州市科技计划项目（No.201803030042）资助。

摘要: 采用负载金的木牙签制备顶空固相微萃取探针，建立了一种便携式，可萃取、富集和检测水体中痕量总汞的方法。采用扫描电子显微镜及能谱分析（SEM-EDS）对负载金萃取探针表面的形貌及元素组成进行了表征。考察了溶液的pH值、盐度、溶解性有机物（DOM）浓度及共存金属离子对SnCl₂还原不同形态汞（无机汞、甲基汞和乙基汞）的影响。结果表明，pH值、盐度和溶解性有机物浓度对SnCl₂还原不同形态汞的影响很小。除Cu²⁺外，低浓度金属离子（≤1 mg/L）对SnCl₂还原不同形态汞的影响较小；高浓度（100 mg/L）的Fe³⁺、Zn²⁺、Ni²⁺、As³⁺、Cr³⁺、Cu²⁺、V⁵⁺和Pb²⁺等金属离子对SnCl₂还原有机汞存在不同程度的抑制，V⁵⁺和Pb²⁺的抑制尤其显著。SnCl₂对溶液中无机汞、甲基汞和乙基汞均具有良好的还原能力，多次还原相对标准偏差（RSD，n=10）分别为3.0%、3.7%和3.5%，表明SnCl₂还原溶液中各形态汞的稳定性较好。本方法对水中总汞的检出限（LOD）为0.03 μg/L，RSD<6.1%（n=6），加标回收率在82.0%~90.0%之间。本方法操作简单、耗时短、稳定性好，适用于地表水和自来水中痕量总汞的检测。

关键词:

English

Determination of Trace Total Mercury in Water by Headspace Solid Phase Microextraction and Electropyrolytic Zeeman Atomic Absorption Spectrometry

1.
School of Environmental and Chemical Engineering, Shenyang University of Technology, Shenyang 110870, China;
2.
Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals, Institute of Analysis, Guangdong Academy of Sciences, China National Analytical Center, Guangzhou 510070, China;
3.
Guangdong Provincial Engineering Research Center for Online Monitoring of Water Pollution, Institute of Analysis, Guangdong Academy of Sciences, China National Analytical Center, Guangzhou 510070, China

Corresponding author: GUO Peng-Ran, prguo@fenxi.com.cn

Received Date: 20 February 2021
Revised Date: 27 May 2021
Fund Project:
Supported by the National Natural Science Foundation of China (No.21777150), the Guangdong Provincial Key Research Development Programme (No.2020B1111350002) and the Scientific and Technological Project of Guangzhou (No.201803030042).

Abstract: A new and portable method for extraction, enrichment and detection of trace total mercury in water by a headspace solid phase microextraction probe loaded with gold and wood stickswas developed. The surface morphology and elemental composition of the gold-loaded probe were characterized by scanning electron microscopy and energy dispersive analysis (SEM-EDS). The effects of solution pH, salinity, dissolved organic matter (DOM) concentration and co-existing metal ions on SnCl₂ reduction of different forms of mercury (inorganic mercury, methyl mercury and ethyl mercury) were investigated. The results showed that the pH, salinity and DOM concentration of the solution had only weak effect on the reduction of different forms of mercury by SnCl₂. Except for Cu²⁺, low concentration of metal ions (≤1 mg/L) had little effect on reduction of different forms of mercuryby SnCl₂. High concentrations (100 mg/L) of Fe³⁺, Zn²⁺, Ni²⁺, As³⁺, Cr³⁺, Cu²⁺, V⁵⁺ and Pb²⁺ inhibited the reduction of organic mercury to different degrees by SnCl₂, especially V⁵⁺and Pb²⁺. The relative standard deviations (RSD, n=10) for reduction of inorganic mercury, MeHg and EtHg in solution by SnCl₂ were 3.0 %, 3.7 % and 3.5 %, respectively, indicating that the stability of three forms of mercury in SnCl₂ solution was good. The detection limit (LOD) of the method for total mercury in water was 0.03 μg/L, the RSD was less than 6.1% (n=6) and the standard recoveries was between 82.0% and 90.0%. This method was simple, less time-consuming and stable and could be applied to the detection of trace total mercury in surface water and tap water.

Key words:

Headspace solid phase microextraction
/ Electropyrolytic Zeeman atomic absorption spectrometry
/ Water
/ Trace total mercury

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

顶空固相微萃取-电热解塞曼原子吸收光谱法测定水中总汞

通讯作者: 郭鹏然,E-mail:prguo@fenxi.com.cn

English

Determination of Trace Total Mercury in Water by Headspace Solid Phase Microextraction and Electropyrolytic Zeeman Atomic Absorption Spectrometry

Corresponding author: GUO Peng-Ran, prguo@fenxi.com.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

顶空固相微萃取-电热解塞曼原子吸收光谱法测定水中总汞

通讯作者: 郭鹏然,E-mail:prguo@fenxi.com.cn

English

Determination of Trace Total Mercury in Water by Headspace Solid Phase Microextraction and Electropyrolytic Zeeman Atomic Absorption Spectrometry

Corresponding author: GUO Peng-Ran, prguo@fenxi.com.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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