[논문]HS-SPME-GC/MS에 의한 지표수에서 ng/L 농도 수준의 37개 휘발성유기화합물의 동시 분석

김태승; 홍석영; 김종은; 임현희; 신호상

doi:10.5806/ast.2012.25.1.039

HS-SPME-GC/MS에 의한 지표수에서 ng/L 농도 수준의 37개 휘발성유기화합물의 동시 분석
Simultaneous determination of 37 volatile organic compounds at ng/L concentration level in surface water by HS-SPME-GC/MS 원문보기

분석과학 = Analytical science & technology, v.25 no.1, 2012년, pp.39 - 49

김태승 (국립환경과학원 금강물환경연구소) , 홍석영 (국립환경과학원 금강물환경연구소) , 김종은 (충청남도 홍성군청) , 임현희 (공주대학교 환경과학과) , 신호상 (공주대학교 환경교육과)

초록
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HS-SPME GC-MS에 의한 지표수 중에 37개 휘발성유기물질을 동시에 분석하는 방법을 개발하였다. 이 방법은 물 중 휘발성유기물질을 헤드스페이스 vial에서 $40 ^{\circ}C$에서 30분간 가열 85 ${\mu}m$ carboxen-polydimethylsiloxane에 흡착시키는 방법이다. 4.0 mL의 물 시료를 사용하여 확립한 조건하에서 정량한계는 4.1-96 ng/L의 범위를 나타냈고 이러한 검출한계는 US EPA 또는 독일에서 확립한 준거치의 1/10 이하 값을 만족시켰으며 0.05 ${\mu}g/L$와 0.50 ${\mu}g/L$의 농도에서 정밀도는 15% 이내를 보였다. 이 정량한계는 준거치를 결정하기 위한 조사연구에서 요구하는 최소 감도이다. 확립한 방법을 사용하여 금강물 16개 시료를 분석한 결과 16개 휘발성유기화합물이 검출되었으며 측정값은 US EPA 또는 독일에서 확립한 준거치 이하의 값을 보였다.

Abstract ▼ AI-Helper

A method to detect 37 volatile organic compounds (VOCs) in surface water was described based on headspace solid-phase micro extraction and gas chromatography-mass spectrometry. VOCs in water were vaporized for 30 min at 40 $^{\circ}C$ in a headspace vial and adsorbed on 85 ${\mu}m$ carboxen-polydimethylsiloxane. Under the established condition, the lowest quantification limit was 4.1-96 ng/L by using 4.0 mL water sample, and the relative standard deviation was less than 15% at concentrations of 0.05 and 0.50 ${\mu}g/L$. The detection limits meet lower concentration than 1/10 of the water quality criteria for VOCs established by the US EPA or Germany. The LOQ is a sensitivity which the monitoring for the establishing water quality criteria requires. When the proposed method was used to analyze the target compounds in sixteen surface water samples and total 16 VOCs were detected in surface water samples collected from Gum-River. Maximum concentrations of VOCs detected were not exceeded the EPA or Germany guidelines in any of the samples.

주제어

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문제 정의

The present study aimed to develop a HS-SPME GC-MS method to detect of 37 VOCs in surface water and to apply the method to real sample analysis. This paper focuses on the validation of sample preparation and detection methodology.

제안 방법

Four SPME fibers (PDMS, PDMS-DVB, PA and CAR-PDMS) were evaluated to select a suitable fiber for detecting the VOCs. The adsorption efficiencies on the SPME fibers were evaluated by comparing the areas of the VOC peaks.
In this paper, we present a simple and automatic method to detect VOCs in surface water samples. The LOQs of VOCs were significantly lower than the EPA or Germany guidelines, and the accuracy and precision of this method were very good.
Four SPME fibers (PDMS, PDMS-DVB, PA and CAR-PDMS) were evaluated to select a suitable fiber for detecting the VOCs. The adsorption efficiencies on the SPME fibers were evaluated by comparing the areas of the VOC peaks. The highest efficiency was obtained using 85 µm carboxen-polydimethylsiloxane (CAR-PDMS) among the four fibers, and CAR-PDMS was selected as a fiber suitable for detecting VOCs.
The present study aimed to develop a HS-SPME GC-MS method to detect of 37 VOCs in surface water and to apply the method to real sample analysis. This paper focuses on the validation of sample preparation and detection methodology.

대상 데이터

The analytical instruments used were an Agilent 6890 A gas chromatograph with a split/splitless injector (Agilent Technologies, Santa Clara, CA, USA) and Agilent 5973 N mass spectrometer (Agilent Technologies, Santa Clara, CA, USA). Combipal Autosampler (Agilent Technologies, Santa Clara, CA, USA), which allows automated HS-SPME injections, were used. The ion source was operated in the electron ionization mode (EI; 70 eV).
Surface water samples were collected from 16 basins in the Gum River without headspace in 40 mL VOC bottles containing 1 drop of 2 M HCl. The sampling sites were selected to uniformly represent all streams of the River.
The analytical instruments used were an Agilent 6890 A gas chromatograph with a split/splitless injector (Agilent Technologies, Santa Clara, CA, USA) and Agilent 5973 N mass spectrometer (Agilent Technologies, Santa Clara, CA, USA). Combipal Autosampler (Agilent Technologies, Santa Clara, CA, USA), which allows automated HS-SPME injections, were used.

성능/효과

For five independent determinations at the concentration range of 0.05-0.5µg/L, the relative standard deviation was less than 15%.
The highest efficiency was obtained using 85 µm carboxen-polydimethylsiloxane (CAR-PDMS) among the four fibers, and CAR-PDMS was selected as a fiber suitable for detecting VOCs. The adsorption efficiencies on the PDMS-DVB, the PDMS and the PA were 90, 85 and 37% compared to that of CAR-PDMS. The heating temperature and time of VOCs were 30 min at 40, which were somewhat modified values of the conditions established by Park or Ezquerro.
The highest efficiency was obtained using 85 µm carboxen-polydimethylsiloxane (CAR-PDMS) among the four fibers, and CAR-PDMS was selected as a fiber suitable for detecting VOCs.
Total 16 VOCs were detected in surface water samples collected from Gum River in the concentration range and frequency as following:1,1,1-Trichloroethane (0.01-0.02 µg/L, 19%), benzene (0.06-0.13 µg/L, 100%), TCE (0.02-0.17 µg/L, 25%), PCE (0.02-0.03 µg/L, 13%), chloroform (0.03-1.04µg/L, 75%), toluene (0.10-0.18 µg/L, 100%), 1,2- dichloropropane (0.06 µg/L, 6%), 1,2-dichloroethane (0.09 µg/L, 6%), ethylbenzene (0.12-1.07 µg/L, 100%), m-xylene (0.12-0.26 µg/L, 100%), p-xylene (0.22-0.34 µg/L, 100%), o-xylene (0.19-0.37 µg/L, 100%), dichlorobromometane (0.02-0.28 µg/L, 50%), styrene (0.01-0.02 µg/L, 19%), chlorodibromomethane (0.02-0.14 µg/L, 63%) and naphthalene (0.01 µg/L, 6%).

후속연구

Maximum concentrations of VOCs detected were not exceeded the EPA guidelines in any of the samples. We will further use this method to detect VOCs in surface water and perform the risk assessment of the detected compounds.

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