高级搜索

吹扫捕集/气相色谱-原子荧光光度法测定土壤和沉积物中烷基汞

,  ,  ,  ,  ,  , 

downloadPDF

上一篇

下一篇

龙雯琪, 朱日龙, 林海兰, 魏凤, 童若辉, 刘丽, 张霖琳. 吹扫捕集/气相色谱-原子荧光光度法测定土壤和沉积物中烷基汞[J]. 环境化学, 2020, (7): 1934-1940. doi: 10.7524/j.issn.0254-6108.2019050301
引用本文: 龙雯琪, 朱日龙, 林海兰, 魏凤, 童若辉, 刘丽, 张霖琳. 吹扫捕集/气相色谱-原子荧光光度法测定土壤和沉积物中烷基汞[J]. 环境化学, 2020, (7): 1934-1940. doi: 10.7524/j.issn.0254-6108.2019050301
shu
LONG Wenqi, ZHU Rilong, LIN Hailan, WEI Feng, TONG Ruohui, LIU Li, ZHANG Linlin. Determination of alkyl mercury in soils and sediments by purge and trap/gas chromatography-atomic fluorescence spectrometry[J]. Environmental Chemistry, 2020, (7): 1934-1940. doi: 10.7524/j.issn.0254-6108.2019050301
Citation: LONG Wenqi, ZHU Rilong, LIN Hailan, WEI Feng, TONG Ruohui, LIU Li, ZHANG Linlin. Determination of alkyl mercury in soils and sediments by purge and trap/gas chromatography-atomic fluorescence spectrometry[J]. Environmental Chemistry, 2020, (7): 1934-1940. doi: 10.7524/j.issn.0254-6108.2019050301
shu

吹扫捕集/气相色谱-原子荧光光度法测定土壤和沉积物中烷基汞

  • 1. 湖南省生态环境监测中心, 国家环境保护重金属污染监测重点实验室, 长沙, 410019;

  • 2. 中国环境监测总站, 国家环境保护环境监测质量控制重点实验室, 北京, 100012;

  • 3. 湖南大学化学化工学院, 长沙, 410082

    • 通讯作者: 张霖琳, E-mail: zhangll@cnemc.cn
  • 基金项目:

    国家环保公益性行业科研专项（201309050）和首都科技条件平台科研项目（Z181100009518003）资助.

Determination of alkyl mercury in soils and sediments by purge and trap/gas chromatography-atomic fluorescence spectrometry

  • 1. Hunan Ecological and Environmental Monitoring Center, State Environmental Protection Key Laboratory of Monitoring for Heavy Metal Pollutants, Changsha, 410019, China;

  • 2. China National Environmental Monitoring Centre, State Environmental Protection Key Laboratory of Quality Control in Environmental Monitoring, Beijing, 100012, China;

  • 3. College of Chemistry and Chemical Engineering, Hunan University, Changsha, 410082, China

    • Corresponding author: ZHANG Linlin, zhangll@cnemc.cn
  • Fund Project: Supported by the National Scientific Research Project of Public Welfare Environmental Protection Industry(201309050)and Scientific Research Project of Capital Science and Technology Condition Platform(Z181100009518003).

  • 摘要: 本文将原子荧光光谱检测技术与吹扫捕集/气相色谱检测技术联用，结合优化的碱性法消解前处理技术，建立了碱性法消解-吹扫捕集/气相色谱-原子荧光光谱（PT-GC-AFS）联用技术测定土壤和沉积物中烷基汞含量的方法，能够在一次分析中同时获得样品中甲基汞和乙基汞的含量.本文分别用酸性法和碱性法处理了沉积物标准样品ERM-CC580、沉积物实际样品和土壤实际样品，重点比较了本方法提出的碱性法消解和使用率较高的酸性法消解两种前处理方式.采用本方法处理实际样品进行了色谱分离研究，对低浓度的实际土壤样品进行了检出限实验，用3种不同浓度的沉积物和3种不同浓度的土壤样品验证了精密度，对沉积物标准参考物质ERM-CC580进行了测定，并用两种实际土壤样品和两种实际沉积物样品进行了加标回收率试验.实验表明，碱性法消解精密度和准确度优于酸性法消解，且步骤少、耗时短，使用的试剂种类少、毒性小，方法稳定性高、可操作性强，适用于分析测试实验室大量土壤/沉积物样品的烷基汞测定.采用碱性法消解土壤/沉积物样品，目标物实现完全分离，甲基汞、乙基汞的线性相关系数分别为0.9999、1.0000，最低检出限分别为0.02 μg·kg-1、0.10 μg·kg-1（取样量为0.50 g），样品分析甲基汞、乙基汞的RSD范围分别为1.0%-4.7%、2.5%-6.0%，加标回收率范围分别为85.1%-109%、90.3%-96.3%.
    Abstract: A method for the determination of alkyl mercury in soils and sediments by purge and trap/gas chromatography coupled with atomic fluorescence spectrometry (PT-GC-AFS) was established by using alkaline digestion. Atomic fluorescence spectrometry was combined with purge and trap/gas chromatography, and the optimized alkaline digestion pretreatment was used. The simultaneous determination of methyl mercury and ethyl mercury in soils and sediments was achieved. In this paper, the standard sediment sample ERM-CC580, the sediment samples and the soil samples were treated by acidic digestion and alkaline digestion respectively to compare the acidic digestion and the alkaline digestion. The actual samples were treated by alkaline digestion for chromatographic separation test. The method detection limit experiment was carried out with the soil samples of low concentration. The precision was tested with three different concentrations of sediments and soils. The standard sediment sample ERM-CC580 was determined. Two kinds of soil samples and sediment samples were used to test the recovery. The experimental results showed that the alkaline digestion demonstrated better precision and accuracy. Moreover, the alkaline digestion had the advantages of less steps, less time, less reagents, less toxicity, better stability and easier to operate. This method was suitable for the determination of alkyl mercury in laboratory with large sample size. Under the optimal experimental conditions, the alkyl mercury could be completely separated. The linear correlation coefficients of methyl mercury and ethyl mercury were 0.9999 and 1.0000, respectively. The method detection limit (MDL) were 0.02 μg·kg-1 and 0.10 μg·kg-1 (sample quantity 0.50 g), respectively. The relative standard deviation (RSD) were 1.0%-4.7% and 2.5%-6.0%, respectively. The recoveries of the method respectively were 85.1%-109% and 90.3%-96.3%.
  • 加载中
  • [1] 许秀艳,朱红霞,于建钊,等. 环境中汞化学形态分析研究进展[J]. 环境化学,2015,34(6):1086-1094.

    XU X Y, ZHU H X, YU J Z, et al. Research progress on chemical speciation analysis of mercury in the environment[J]. Environmental Chemistry, 2015, 34(6):1086-1094(in Chinese).

    [2] MERGLER D, ANDERSON H A, CHAN L H M. Methymercury exposure and health effects in humans:A worldwide concern[J]. A Journal of the human Environment, 2007, 36(1):3-11.
    [3] EPA 1630. Methyl mercury in water by distillation, aqueous ethylation, purge and trap, and CVAFS, EPA-821-R-01-020, January 2001[S].
    [4] CHEN H Y, WU C L, SHEN L H, et al. Online anion exchange column preconcentration and high performance liquid chromatographic separation with inductively coupled plasma mass spectrometry detection for mercury speciation analysis[J]. Analytica Chimica Acta, 2014, 828(9):9-16.
    [5] 顾昱晓,孟梅,邵俊娟,等. 在线吹扫捕集-气相色谱-原子荧光光谱法测定土壤中甲基汞[J]. 分析化学,2013,41(11):1754-1757.

    GU Y X, MENG M, SHAO J J, et al. Determination of methylmercury in soil samples with online purge and trap gas chromatography-atomic fluorescence spectrometry[J]. Chinese Journal of Analytical Chemistry, 2013, 41(11):1754-1757(in Chinese).

    [6] 高兰兰,徐浩,杨琼,等. PT-GC-CAFS联用技术测定污水处理厂外排水中烷基汞残留量[J]. 中国环境监测,2016,32(1):98-103.

    GAO L L, XU H, YAN Q, et al. Determination of the alkyl mercury residue in external drainage of partial of sewage treatment plants by purging capture-gas chromatography-cold atomic fluorescence spectrometry[J]. Environmental Monitoring in China, 2016, 32(1):98-103(in Chinese).

    [7] 潘怡,林长青,高鹏. 在线衍生化吹扫捕集-气相色谱质谱联用法检测地表水中的甲基汞和乙基汞[J]. 环境化学,2014,33(1):171-172.

    PAN Y, LIN C Q, GAO P. Determination of methylmercury and ethyl mercury in surface water with online derivatization purge and trap gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2014, 33(1):171-172(in Chinese).

    [8] 吴建刚,赵金平,赵志南. 四丙基硼化钠衍生吹扫捕集冷原子荧光光谱法同时测定水中的甲基汞和乙基汞[J]. 环境化学,2015,34(2):390-391.

    WU J G, ZHAO J P, ZHAO Z N. Simultaneous determination of methyl mercury and ethyl mercury in water by purge and trap cold atomic fluorescence spectrometry with derivatization of sodium tetrapropyl boride[J]. Environmental Chemistry, 2015, 34(2):390-391(in Chinese).

    [9] 何天容,冯新斌,戴前进,等. 萃取-乙基化结合GC-CV AFS法测定沉积物及土壤中的甲基汞[J]. 地球与环境,2004,32(2):83-86.

    HE T R, FENG X B, DAI Q J, et al. Detemination of methyl mercury in sediments and soils by GC-CV AFS after aqueous phase ethylation[J]. Earth and Environment, 2004, 32(2):83-86(in Chinese).

    [10] 颜雪,司友斌,邹嫣,等. 碱消解-HPLC同时测定土壤中的无机汞和甲基汞[J]. 环境科学与技术,2012,35(9):89-94.

    YAN X, SI Y B, ZOU Y, et al. Simultaneous determination of inorganic mercury (Ⅱ) and methyl mercury in soil by alkaline digestion-high performance liquid chromatography[J]. Environmental Science & Technology, 2012, 35(9):89-94(in Chinese).

    [11] ARIANE V Z, SERGIO C, CARMEN I, et al. Method development for the simultaneous determination of methylmercury and inorganic mercury in seafood[J]. Food Control, 2014, 46:351-359.
    [12] 史建波,廖春阳,王亚伟,等. 气相色谱和原子荧光联用测定生物和沉积物样品中甲基汞[J]. 光谱学与光谱分析,2006,26(2):336-339.

    SHI J B, LIAO C Y, WANG Y W, et al. Determination of methylmercury in biological and sediment samples by capillary gas chromatography on-line coupled with atomic fluorescence spectrometry[J]. Spectroscopy and Spectral Analysis, 2006, 26(2):336-339(in Chinese).

    [13] 史伟玲,杨静,李飞鹏,等. 环境样品中甲基汞测定方法的研究进展[J]. 环境科学与技术,2014,37(120):310-315.

    SHI W L, YANG J, LI F P, et al. Research progress of methylmercury determination methods in environmental samples[J]. Environmental Science & Technology, 2014, 37(120):310-315(in Chinese).

    [14] POPP M, HANN S, KOELLENSPERGER G. Environmental application of elemental speciation analysis based on liquid or gas chromatography hyphenated to inductively coupled plasma mass spectrometry:A review[J]. Analytica Chimica Acta, 2010, 668(2):114-129.
  • 加载中
WeChat 点击查看大图
计量
  • 文章访问数:  1979
  • HTML全文浏览数:  1979
  • PDF下载数:  45
  • 施引文献:  0
出版历程
  • 收稿日期:  2019-05-03

吹扫捕集/气相色谱-原子荧光光度法测定土壤和沉积物中烷基汞

    通讯作者: 张霖琳, E-mail: zhangll@cnemc.cn
  • 1. 湖南省生态环境监测中心, 国家环境保护重金属污染监测重点实验室, 长沙, 410019;
  • 2. 中国环境监测总站, 国家环境保护环境监测质量控制重点实验室, 北京, 100012;
  • 3. 湖南大学化学化工学院, 长沙, 410082
  • 收稿日期:  2019-05-03
基金项目:

国家环保公益性行业科研专项（201309050）和首都科技条件平台科研项目（Z181100009518003）资助.

摘要: 本文将原子荧光光谱检测技术与吹扫捕集/气相色谱检测技术联用，结合优化的碱性法消解前处理技术，建立了碱性法消解-吹扫捕集/气相色谱-原子荧光光谱（PT-GC-AFS）联用技术测定土壤和沉积物中烷基汞含量的方法，能够在一次分析中同时获得样品中甲基汞和乙基汞的含量.本文分别用酸性法和碱性法处理了沉积物标准样品ERM-CC580、沉积物实际样品和土壤实际样品，重点比较了本方法提出的碱性法消解和使用率较高的酸性法消解两种前处理方式.采用本方法处理实际样品进行了色谱分离研究，对低浓度的实际土壤样品进行了检出限实验，用3种不同浓度的沉积物和3种不同浓度的土壤样品验证了精密度，对沉积物标准参考物质ERM-CC580进行了测定，并用两种实际土壤样品和两种实际沉积物样品进行了加标回收率试验.实验表明，碱性法消解精密度和准确度优于酸性法消解，且步骤少、耗时短，使用的试剂种类少、毒性小，方法稳定性高、可操作性强，适用于分析测试实验室大量土壤/沉积物样品的烷基汞测定.采用碱性法消解土壤/沉积物样品，目标物实现完全分离，甲基汞、乙基汞的线性相关系数分别为0.9999、1.0000，最低检出限分别为0.02 μg·kg-1、0.10 μg·kg-1（取样量为0.50 g），样品分析甲基汞、乙基汞的RSD范围分别为1.0%-4.7%、2.5%-6.0%，加标回收率范围分别为85.1%-109%、90.3%-96.3%.

English Abstract

    全文HTML

参考文献 (14)

目录

/

返回文章
返回

Copyright © 2019 中国科学院生态环境研究中心