Research on the Method for Determining Compound Specific Carbon Isotopes of Trace Benzenes in Water by Solid Phase Microextraction/Gas Chromatography/Combustion-Isotope Ratio Mass Spectrometry

QI Yan; YIN Xi-jie; LI Yu-hong; LIN Xi-huang

doi:10.12452/j.fxcsxb.24041501

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Research on the Method for Determining Compound Specific Carbon Isotopes of Trace Benzenes in Water by Solid Phase Microextraction/Gas Chromatography/Combustion-Isotope Ratio Mass Spectrometry

Scientific Papers | 更新时间：2024-11-04

- Research on the Method for Determining Compound Specific Carbon Isotopes of Trace Benzenes in Water by Solid Phase Microextraction/Gas Chromatography/Combustion-Isotope Ratio Mass Spectrometry
- Journal of Instrumental Analysis Vol. 43, Issue 9, Pages: 1474-1480(2024)
- 作者机构：
  
  1.自然资源部第三海洋研究所分析测试中心，福建厦门 361005
  2.中国地质调查局舟山海洋地质灾害野外科学观测研究站，山东青岛 266237
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.24041501
  CLC： O657.63;X132
- Published：15 September 2024，
  
  Received：15 April 2024，
  
  Revised：31 May 2024，
- 稿件说明：
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漆艳,尹希杰,李玉红,林锡煌.固相微萃取/气相色谱/燃烧-同位素比值质谱技术测定水体中微量苯系物单体碳同位素方法研究[J].分析测试学报,2024,43(09):1474-1480.

QI Yan,YIN Xi-jie,LI Yu-hong,LIN Xi-huang.Research on the Method for Determining Compound Specific Carbon Isotopes of Trace Benzenes in Water by Solid Phase Microextraction/Gas Chromatography/Combustion-Isotope Ratio Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(09):1474-1480.
漆艳,尹希杰,李玉红,林锡煌.固相微萃取/气相色谱/燃烧-同位素比值质谱技术测定水体中微量苯系物单体碳同位素方法研究[J].分析测试学报,2024,43(09):1474-1480. DOI： 10.12452/j.fxcsxb.24041501.

QI Yan,YIN Xi-jie,LI Yu-hong,LIN Xi-huang.Research on the Method for Determining Compound Specific Carbon Isotopes of Trace Benzenes in Water by Solid Phase Microextraction/Gas Chromatography/Combustion-Isotope Ratio Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(09):1474-1480. DOI： 10.12452/j.fxcsxb.24041501.

摘要

该文建立了固相微萃取/气相色谱/燃烧-同位素比值质谱（SPME/GC/C-IRMS）技术测定水体中7种苯系物碳同位素（

C）的方法。实验结果表明，萃取温度30 ℃，萃取时间60 min条件下萃取效果最佳，萃取温度（30~60 ℃）和萃取时间（15~60 min）对顶空萃取（HS-SPME）过程中的碳同位素分馏无影响。最佳萃取条件下，利用HS-SPME和直接萃取（D-SPME）方法分别测试7种苯系物的

C值，标准偏差分别为 0.08‰~0.45‰和0.05‰~0.39‰，测试误差分别为-0.16‰~0.33‰和-0.41‰~0.46‰，两种SPME方式在萃取过程中均未发生明显碳同位素分馏，HS-SPME的灵敏度比D-SPME方法高1~2个数量级。通过移动平均值算法计算苯、间/对二甲苯、异丙苯的检出限为1 μg/L，甲苯、乙苯、邻二甲苯、苯乙烯的检出限为2 μg/L。测得江苏某废弃农药场地下水中7种苯系物

C值的标准偏差为0.01‰~0.43‰。该方法样品前处理简单、灵敏度高、准确性好，适用于水体中痕量苯系物单体碳同位素的检测。

Abstract

This study introduces a solid phase microextraction/gas chromatography/combustion-isotope ratio mass spectrometry（SPME/GC/C-IRMS） technology for analyzing the carbon isotopes of seven benzene series compounds in water. The pretreatment conditions for headspace solid phase microextraction（HS-SPME） were optimized. The results demonstrated that the extraction efficiency reached its maximum at an extraction temperature of 30 ℃ and an extraction time of 60 minutes. Variations in extraction temperature（30-60 ℃） and extraction time（15-60 m

in） did not cause carbon isotope fractionation during HS-SPME. Under the optimized extraction conditions，both HS-SPME and D-SPME methods were employed to measure the

C values of the seven benzene series compounds. The standard deviations ranged from 0.08‰-0.45‰ and 0.05‰-0.39‰，and the test error varied from -0.16‰-0.33‰ and -0.41‰-0.46‰，respectively. No obvious carbon isotope fractionation occurred during the extraction process in both SPME methods，and the sensitivity of the HS-SPME method is 1-2 orders of magnitude higher than the D-SPME method. Utilizing the moving average algorithm，the detection limits for benzene，

-xylene，and isopropylbenzene were determined to be 1 μg/L，while for toluene，ethylbenzene，

-xylene and styrene，the detection limits were 2 μg/L. This method was applied to analyze groundwater from an abandoned pesticide factory in Jiangsu，yielding

C values for the seven benzene series compounds with good repeatability （standard deviation：0.01%-0.43‰）. This method can be applied to detect the carbon isotope for trace benzene series compounds in water，because of the simple pretreatment procedure，high sensitivity and good accuracy.

关键词

苯系物固相微萃取气相色谱/燃烧-同位素质谱单体碳稳定同位素分析水体

Keywords

benzene series compoundssolid phase microextractiongas chromatography/combustion-isotope ratio mass spectrometrycompound specific carbon isotope analysiswater

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