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  • 한국과학기술정보연구원(KISTI) 서울분원 대회의실(별관 3층)
  • 2024년 07월 03일(수) 13:30
 

  • P-ISSN1225-0163
  • E-ISSN2288-8985
  • SCOPUS, ESCI, KCI

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  • P-ISSN 1225-0163
  • E-ISSN 2288-8985

반복적인 막 추출과 GC-MS를 이용한 물 중 BTEX의 분석

Solvent-free determination of BTEX in water using repetitive membrane extraction followed by GC-MS

분석과학 / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2011, v.24 no.5, pp.352-359
https://doi.org/10.5806/AST.2011.24.5.352
김희갑 (강원대학교)
김세영 (강원대학교)
이수형 (강원대학교)
  • 다운로드 수
  • 조회수

초록

용매를 사용하지 않고 반복적으로 막 추출한 후 저온농축과 GC-MS로 물 중 BTEX를 분석하는 방법을 시도하였다. 물로부터 비공성막의 silicone 막을 투과한 BTEX를 He 기체를 통해 <TEX>$-100^{\circ}C$</TEX>의 저온 농축장치로 보낸 후 열 탈착과 GC-MS로 분석하였다. 물 시료(30 mL)는 10 mL/min로 흘려주었고, 한 번 추출된 시료는 다시 되돌려서 두 번 더 추출하였다. Benzene에 대한 회수율은 가장 높아 약 80%인 반면에, ethylbenzene과 xylenes에 대한 회수율은 3.5-10%로 낮은 편이었다. 그렇지만, RSD는 모두 10% 미만이었고 검량선의 직선성(<TEX>$r^2$</TEX>)도 0.9976-0.9997로 높은 편이었으며, 방법검출한계도 1.8 <TEX>${\mu}g$</TEX>/L 이었다. 이 방법은 짧은 추출 시간, 용매의 미사용 및 분석의 편의성의 장점을 갖고 있다.

keywords
BTEX, cryofocusing, GC-MS, repetitive membrane extractions, nonporous silicone membrane Solvent-free determination of BTEX in water using repetitive membrane extraction followed by GC-MS

Abstract

An analytical method for solvent-free determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using repetitive membrane extractions coupled to cryofocusing and GC-MS was derived. BTEX compounds that permeated through a nonporous silicone membrane from the aqueous phase and evaporated into the acceptor phase were purged into a cryofocusing trap (-100 ℃) with helium gas. The BTEX compounds,thus enriched in the trap, were thermally desorbed into a capillary column GC and detected using an MS. The flow rate of the donor phase (30 mL water) was set at 10 mL/min, and membrane extractions, accomplished by returning the water drained from the extraction module to the sample container, were repeated three times at 20 ± 2 ℃. Although recoveries (%) were variable, from the highest for benzene (approximately 80%) to the lowest for ethylbenzene and xylenes (3.5-10%), the method showed satisfactory precision (RSD 2.2-10%)with good-linearity calibration curves (r^2 0.9976-0.9997 in 1-100 μg/L range) for all of the compounds. The method detection limits (MDLs) ranged from 0.16 to 1.8 μg/L. The results showed the method’s advantages such as short analysis time and overall simplicity without solvent compared to the conventional techniques.

keywords
BTEX, cryofocusing, GC-MS, repetitive membrane extractions, nonporous silicone membrane


참고문헌

1

1. Hylton, K. and Mitra, S., J. Chromatogr. A, 1152, 199-214 (2007).

2

2. Biziuk, M. and Przyjazny, A, J. Chromatogr. A, 733, 417-448 (1996).

3

3. Kolb, B., J. Chromatogr. A, 842, 163-205 (1999).

4

4. Louter, A. J. H., Vreuls, J. J. and Brinkman, U. A. Th., J. Chromatogr. A, 842, 391-426 (1999).

5

5. Ouyanga, G. and Pawliszyn, J., Trends Anal. Chem., 25, 692-703 (2006).

6

6. David, F. and Sandra, P., J. Chromatogr. A, 1152, 54-69(2007).

7

7. Cordero, B. M., Pavón, J. L. P., Pinto, C. G. Laespada, M. E. F., Martínez, R. C. and Gonzalo, E. R., J. Chromatogr. A, 902, 195-204 (2000).

8

8. Blanchard, R. D. and Hardy, J. K., Anal. Chem., 56, 1621-1624 (1984).

9

9. Zhang, G.-Z. and Hardy, J. K., J. Environ. Sci. Health, A24, 279-295 (1989).

10

10. Blanchard, R. D. and Hardy, J. K., Anal. Chem., 57, 2349-2351 (1985).

11

11. Zhang, G.-Z. and Hardy, J. K., J. Environ. Sci. Health, A24, 1011-1024 (1989).

12

12. Frantz, D. D. and Hardy, J. K., J. Environ. Sci. Health, A34, 695-704 (1999).

13

13. Köller, G., Popp, P., Weingart, K., Hauser, B. and Herrmann, W., Chromatographia, 57, S-229-S-233 (2003).

14

14. Pratt, K. F. and Pawliszyn, J., Anal. Chem., 64, 2107-2110 (1992).

15

15. Xu, Y. H. and Mitra, S., J. Chromatogr. A, 688, 171-180(1994).

16

16. Hauser, B. and Popp, P., J. Chromatogr. A, 909, 3-21(2001).

17

17. Sae-Khow, O. and Mitra, S., J. Chromatogr. A, 1217, 2736-2746 (2010).

18

18. Maden, A. J. and Hayward, M. J., Anal. Chem., 68, 1805-1811 (1996).

19

19. Hauser, B. and Popp, P., J. High Resol. Chromatogr., 22, 205-212 (1999).

20

20. Yang, M. J., Harms, S., Luo, Y. Z. and Pawliszyn, J., Anal. Chem., 66, 1339-1346 (1994).

21

21. 40 Code of Federal Register Appendix B to Part 136: Definition and Procedure for the Determination of the Method Detection Limit - Revision 1.11 (1994).

22

22. United States Environmental Protection Agency Method 524.3: Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry – Version 1.0 (2009).

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