固体吸附管捕集冷原子吸收光谱法测定工作场所空气中汞的研究

doi:10.3964/j.issn.1000-0593(2014)05-1412-04

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摘要：建立了工作场所空气中汞及其化合物的高锰酸钾-二氧化锰混合固体吸附管捕集、冷原子吸收测定方法。用高锰酸钾与二氧化锰按质量比1∶1混合后填装玻璃管制成固体吸附管捕集工作场所空气中汞，并以0.90 mol·L^-1的硫酸溶液解吸后冷原子吸收光谱法测定，与高锰酸钾-硫酸吸收液法的采样效率、样品稳定性、穿透容量进行了比对。在0.000 2~0.015 0 mg·L^-1的浓度范围内线性关系良好，相关系数为0.999 1，空气中汞在0.001~2.820 mg·m^-3范围内，平均采样效率为99.9%~100.0%，300 mg吸附剂对汞的穿透容量大于505.4 μg，吸附管对汞的平均加标回收率为96.4%~103.8%，日内、日间精密度分别为3.0%~3.3%，3.5%~5.2%，最低检出浓度为0.001 3 mg·m^-3(以采集7.5 L空气样品计)、0.000 6(以96 L空气样品计)。采集后的吸附管在室温下保存30 d，下降率小于0.1%。固体吸附管采样方法简单，适用于工作场所空气中汞及其化合物的短时间、时间加权平均浓度及个体暴露浓度的采样检测。

关键词：固体吸附剂;汞;冷原子吸收光谱

Abstract：A new KMnO₄-MnO₂ solid multisorbent tube for capturing mercury in workplace air was developed. Experimental conditions for solid multisorbent tube, efficiency of sampling, desorption efficiency and stability were studied. Mercury and its compounds in air were captured by solid KMnO₄-MnO₂ sorbent filled tube and desorbed with 0.90 mol·L^-1 sulfuric acid solution. Mercury and its compounds were quantitatively analyzed according to the method of GBZ/T 160.14—2004 cold vapor atomic absorption spectrometry. The linear range of the proposed method was 0.000 2~0.015 0 mg·L^-1 with r=0.999 1, the average efficiency of sampling was 99.9%～100.0% in the concentration range of 0.001~2.820 mg·m^-3, and the breakthrough capacity was more than 505.4 μg for 300 mg KMnO₄-MnO₂ solid multisorbent, the average recovery rate was 96.4%~103.8%, the intra-day and inter-day precision was 3.0%~3.3% and 3.5%~5.2% respectively, the limit of detection was 0.0013 mg·m^-3 (7.5 L of air ) and 0.000 6 mg·m^-3(96 L of air), after sampling, and the solid multisorbent tube could be kept at least 30 d at room temperature without significant loss. The present method was simple and suitable for capturing mercury and its compounds in the workplace air and ambient air. The solid multisorbent tube was useful for personal sampling and time weighted average sampling.

Key words：Solid sorbent;Mercury;Cold vapor atomic absorption spectrometry

收稿日期: 2013-07-09 修订日期: 2013-10-26

中图分类号:

O657.3

通讯作者: 黄汉林 E-mail: Huanghl@gdoh.org

引用本文:

黄振侬¹，孙毅¹，阮小林¹，吴邦华¹，张爱华¹，黄钧宜¹，黄燕玲²，黄汉林^1* . 固体吸附管捕集冷原子吸收光谱法测定工作场所空气中汞的研究 [J]. 光谱学与光谱分析, 2014, 34(05): 1412-1415.
HUANG Zhen-nong¹, SUN Yi¹, RUAN Xiao-lin¹, WU Bang-hua¹, ZHANG Ai-hua¹, HUANG Jun-yi¹, HUANG Yan-ling², HUANG Han-lin^1* . Study on the Solid Sorbent Tube for Capturing Mercury in the Workplace Air and Determination by Cold Vapor Atomic Absorption Spectrometry . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2014, 34(05): 1412-1415.

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