Optimization Condition of Trace Analysis of Fuel Oxygenated Compounds Using The Design of Experiment (DOE) in Solid-Phase Microextraction with GC/FID

고체상미량분석법(SPME-GC/FID)에서 실험계획법을 이용한 연료첨가제 미량분석의 최적조건

  • An, Sang-Woo (Department of Civil & Environmental Engineering, Hanyang University) ;
  • Lee, Si-Jin (Department of Environmental Energy & System Engineering, Kyonggi University) ;
  • Chang, Soon-Woong (Department of Environmental Energy & System Engineering, Kyonggi University)
  • 안상우 (한양대학교 토목공학과) ;
  • 이시진 (경기대학교 환경에너지시스템공학과) ;
  • 장순웅 (경기대학교 환경에너지시스템공학과)
  • Received : 2009.07.31
  • Accepted : 2009.10.23
  • Published : 2010.02.28

Abstract

In this study, Solid-phase micro-extraction (SPME) with Gas Chromatograph using Flame Ionization Detector (GC/FID) was studied as a possible alternative to liquid-liquid extraction for the analysis of Methyl tert-butyl ether (MTBE) and Tertiary-butyl ether (TBA) in water and an optimization condition of trace analysis of MTBE and TBA using the design of experiment (DOE) was described. The aim of our research was to apply experimental design methodology in the optimization condition of trace analysis of fuel oxygenated compounds in soil-phase microextraction with GC/FID. The reactions of SPME were mathematically described as a function of parameters of Temp ($X_1$), Volume ($X_2$), Time ($X_3$) and Salt ($X_4$) being modeled by the use of the partial factorial designs, which was used for fitting 2nd order response surface models and was alternative to central composite designs. The model predicted agreed with the experimentally observed result ($Y_1$(MTBE, $R^2$ = 0.96, $Y_2$ (TBA, $R^2$ = 0.98)). The estimated ridge of the expected maximum responses and optimal conditions for MTBE and TBA were 278.13 and (Temp ($X_1$) = $48.40^{\circ}C$, Volume ($X_2$) = 73.04 mL, Time ($X_3$) = 11.51 min and Salt ($X_4$) = 12,50 mg/L), and 127.89 and (Temp ($X_1$) = $52.12^{\circ}C$, Volume ($X_2$) = 88.88mL, Time ($X_3$) = 65.40 min and Salt ($X_4$) = 12,50 mg/L), respectively.

Keywords

References

  1. 박교범, 이석곤, 2000, SPME를 이용한 수용액 중의 휘발성 유기 화합물 분석, 분석과학회지, 13(3), 277-281.
  2. 안상우, 장순웅, 2004, SPME-GC/FID를 이용한 MTBE 및 TBA 분석에 관한 연구, 한국환경분석학회지, 7(2), 83-89.
  3. 안상우,이시진, 장순웅, 2004, 고체상 미량분석법을 이용한 GC/FID에서 PCE 및 TCE 최적 분석법, 한국환경과학회지, 13(10), 903-903.
  4. 조일형, 이내현, 장순웅, 안상우, 윤영환, 조경덕, 2006, 실험계획 법 중 Box-Behnken(박스-벤켄)법을 이용한 반응성 염료의 광촉매 산화조건특정해석 및 최적화, 대한환경공학회지, 28(9), 917- 927.
  5. 조일형, 이내현, 장순웅, 안상우, 윤영한, 조경덕, 2007, 화학적 응집 공정에서 중심합성설계법을 이용한축산폐수의 COD 제거특성평가및최적화연구, 한국물환경학회지, 23(1), 111-121.
  6. Achten, C., and Puttmann, W., 2000, Determination of methyl tert-butyl ether in surface water by use of solid-phase microextraction, Environ. Sci. Technol., 34, 1359-1364. https://doi.org/10.1021/es9906857
  7. Achten, C., Kolb, A., and Puttmann, W., 2001, Sensitive method for determination of methyl tert-butyl ether (MTBE) in water by use of headspace-SPME/GC-MS, Fresenius J. of Anal. Chem., 371, 519-525. https://doi.org/10.1007/s002160100984
  8. Cassada, D.A., Zhang, Y., Snow,D.D., and Spalding, R.E., 2000, Trace analysis of ethanol, MTBE, and related oxygenate compounds in water using solid-phase microextraction and gas chromatography/mass spectrometry, Anal. Chem., 72, 4654-4658. https://doi.org/10.1021/ac000462v
  9. Cho, D.H., Kong, S.H., and Oh, S.J., 2003, Analysis of trihalomethanes in drinking water using headspace-SPME technique with gas chromatography, Water Research, 37, 402-408. https://doi.org/10.1016/S0043-1354(02)00285-3
  10. Dron, J., Garcia, R., and Millan, E., 2002, Optimization of headspace solid-phase microextraction by means of an experimental design for the determination of methyl tert-butyl ether in water by gas chromatography-flame ionization detection, J. Chromatography. A, 963, 259-264. https://doi.org/10.1016/S0021-9673(02)00359-X
  11. Grecki, T., Khaled, A., and Pawliszyn, J., 1998, The effect of sample volume on quantitative analysis by solid phase microextraction Part 2. Experimental verification, The Analyst, 123(12), 2819-2824. https://doi.org/10.1039/a806788k
  12. Piazza, F., Barbieri, A., Saverio Violante, F., and Roda, A., 2001, A rapid and sensitive method for methyl tert-butyl ether analysis in water samples by use of solid phase microextraction and gas chromatography-mass spectrometry, Chemosphere, 44, 539-544. https://doi.org/10.1016/S0045-6535(00)00501-4