工业水处理2025,Vol.45Issue(1) :174-178.DOI:10.19965/j.cnki.iwt.2023-1226

HS-SPME-GC-MS测定水中六氯环戊二烯

Determination of hexachlorocyclopentadiene in water by HS-SPME-GC-MS

由希华 石敬华 王伟莉 曹方方 张凤菊 秦承华
工业水处理2025,Vol.45Issue(1) :174-178.DOI:10.19965/j.cnki.iwt.2023-1226

HS-SPME-GC-MS测定水中六氯环戊二烯

Determination of hexachlorocyclopentadiene in water by HS-SPME-GC-MS

由希华 1石敬华 1王伟莉 2曹方方 1张凤菊 1秦承华3
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作者信息

  • 1. 山东省生态环境监测中心,山东 济南 250101
  • 2. 南京卡佛科学仪器有限公司,江苏 南京 210042
  • 3. 中国环境监测总站,北京 100012
  • 折叠

摘要

建立了顶空固相微萃取-气相色谱-质谱法(HS-SPME-GC-MS)测定水中六氯环戊二烯的分析方法,采用顶空固相微萃取进样,DB-1色谱柱分离,气相色谱/质谱检测器检测,系统考察了不同涂层固相萃取针、进样口温度、固相萃取条件、盐效应等对测定结果的影响,并在最优实验条件下对方法进行了验证.结果表明,六氯环戊二烯在质量浓度为0.1~10 µg/L范围内与色谱峰面积线性良好,相关性系数为0.997,方法检出限为0.03 µg/L.对实际地表水和废水样品进行测定,废水样品监测结果为0.5 µg/L,地表水样品监测结果为未检出,对实际样品分别加标0.5 µg/L和1.0 µg/L测定,加标回收率为70%~87%,相对标准偏差为4.14%~13.9%(n=6).该方法操作简单,不使用有机溶剂萃取,精密度好,准确度高,可用于快速测定工业废水和地表水中六氯环戊二烯.

Abstract

A headspace solid-phase microextraction gas chromatography-mass spectrometry(HS-SPME-GC-MS)method was established for the determination of hexachlorocyclopentadiene in water,with using headspace solid-phase microextraction injection,DB-1 chromatographic column separation,and gas chromatography/mass spectrom-etry detector detection.The effects of coating solid-phase extraction needles,inlet temperatures,solid-phase extrac-tion conditions,salt effects on the determination were systematically investigated,and the method was validated un-der the optimal experimental conditions.The results showed that hexachlorocyclopentadiene exhibited good linearity with chromatographic peak area within the mass concentration range of 0.1-10 µg/L,with a correlation coefficient of 0.997 and a detection limit of 0.03 µg/L.The actual surface water and wastewater samples were measured,and the monitoring result of wastewater sample was 0.5 µg/L,while the monitoring result of surface water sample was not de-tected.The actual samples were spiked with 0.5 µg/L and 1.0 µg/L,respectively.The recovery rate was 70%-87%,and the relative standard deviation was 4.14%-13.9%(n=6).This method was simple to operate,did not use organic solvents for extraction,had good precision and high accuracy,which could be used for rapid determination of hexa-chlorocyclopentadiene in industrial wastewater and surface water.

关键词

顶空固相微萃取/气相色谱-质谱法//六氯环戊二烯

Key words

headspace solid-phase microextraction/gas chromatography-mass spectrometry/water sample/hexa-chlorocyclopentadiene

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出版年

2025
工业水处理
中海油天津化工研究设计院

工业水处理

CSTPCDCSCD北大核心
影响因子:0.737
ISSN:1005-829X
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