• Title/Summary/Keyword: GC-SPME

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Integration of Headspace Solid Phase Micro-Extraction with Gas Chromatography for Quantitative Analysis of Formaldehyde

  • Lo, Kong Mun;Yung, Yen Li
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.139-142
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    • 2013
  • A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

고체상 미량분석법(SPME)을 이용한 GC/FID에서의 BTEX 및 TCE 동시 분석

  • 이재선;장순웅;이시진
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.04a
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    • pp.405-408
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    • 2003
  • The soild phase microextraction(SPME)fiber which contains 100${\mu}{\textrm}{m}$ polydimethyl siloxane of a stationary phase was used for the analysis of volatile organic compounds contained in aqueous solution. volatile organic compounds, which were spiked in blank water and extracted by the headspace SPME techique, were analyzed by gas chromatography/flame ionization detector(GC/FID). The optimu condition of SPME fiber is determined that the analytes were extracted for 40min from extracts by using PDAfS100${\mu}{\textrm}{m}$ fiber. This new method could have wide application for the analysis of VOCs in aqueous solution.

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Analysis of 111 VOCs using SPME-GC/MS (SPME-GC/MS에 의한 111종 VOCs 분석법 확립)

  • 김대원;허귀석;유혜경;홍진희
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2001.11a
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    • pp.344-345
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    • 2001
  • 대기 중에는 ppb 수준의 매우 미량으로 많은 VOC 성분이 존재하고 있어 이를 효과적으로 신속하고 적은 비용으로 분석할 수 있는 분석할 필요성이 커지고 있다. 그러므로, 본 연구에서는 대기중의 VOC성분을 SPME-GC/MS법을 이용하여 효율적으로 분석하기 위한 분석법을 개발하고자 하였다. 유해성이 큰 halocarbon, aromatic, haloaromatic V()Cs 42 종(USEPA TO-14)과, 오존을 유발시키는 오존전구물질 VOCs 53 종, 국내 규제 VOCs 33종, 그리고 악취물질(국내 8종 포함 일본 악취물질 22종)을 전부 포함하는 111종의 VOC를 SPME-GC/MS를 이용하여 신속하게 정성, 정량분석할 수 있는 방법을 확립하고저 하였다. (중략)

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SPME-GC/MS와 전자코(Electronic Nose)를 이용한 재래흑돼지와 개량종 돼지 가열육의 휘발성 향기 성분 및 향기 패턴 비교

  • Gang, Seon-Mun;Lee, Seong-Gi
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2006.05a
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    • pp.209-213
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    • 2006
  • 본 연구는 재래흑돼지와 개량종 돼지 가열육의 SPME-GC/MS와 전자코를 이용한 휘발성 향기 성분 및 향기 패턴 비교를 구명하고자 실시하였으며, 평균 생시 체중이 70 kg인 재래흑돼지(거세돈) 5두와 103 kg인 개량종 돼지($Landrace{\times}Yorkshire$,거세돈) 5두를 도축후 뒷다리 부위를 시료로 이용하였다. SPME-GC/MS를 이용한 휘발성 향기 성분에서 6-mehtyl-1-heptanol이 재래흑돼지육에서만 검출되었고, 1-octen-3-ol과 benzaldehyde가 재래흑돼지육이 개량종 돼지육보다 유의적으로 높았다(p<0.05). 전자코의 PCA에 의한 향기 패턴은 두 품종간에 큰 차이를 보이지 않았다. 따라서 재래흑돼지 가열육이 개량종 돼지 가열육보다 높은 6-mehtyl-1-heptanol, 1-octen-3-ol, benzaldehyde를 가졌으며, SPME-GC/MS와 전자코에 의해 품종이 다른 가열 돈육의 휘발성 향기 성분과 패턴을 성공적으로 분별하였다.

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Determination of Petroleum Aromatic Hydrocarbons in Seawater Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography/Mass Spectrometry (HS-SPME-GC/MS를 이용한 해수 내 유류계 방향족탄화수소 분석법)

  • An, Joon Geon;Shim, Won Joon;Ha, Sung Yong;Yim, Un Hyuk
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.17 no.1
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    • pp.27-35
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    • 2014
  • The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

Comparative analysis of sensory profiles of commercial cider vinegars from Korea, China, Japan, and US by SPME/GC-MS, E-nose, and E-tongue (한국, 중국, 일본, 미국산 시판 사과식초의 관능적 품질 비교를 위한 SPME-GC/MS, 전자코 및 전자혀 분석)

  • Jo, Yunhee;Gu, Song-Yi;Chung, Namhyeok;Gao, Yaping;Kim, Ho-Jin;Jeong, Min-Hee;Jeong, Yong-Jin;Kwon, Joong-Ho
    • Korean Journal of Food Science and Technology
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    • v.48 no.5
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    • pp.430-436
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    • 2016
  • Solid phase microextraction and gas chromatography-mass spectrometry (SPME/GC-MS), electronic nose, and electronic tongue were used to characterize the sensory profiles of cider vinegars from Korea (K1-2), China (C1-2), Japan (J1-2), and US (U1-2). SPME-GC/MS detected acetic acid as the common volatile compound in all vinegars, in addition to isovaleric acid, octanoic acid, and phenethyl acetate. Acids and acetic esters were the major components of Korean and US vinegar samples, respectively. Chinese vinegars had high ethyl acetate content, while Japanese samples were characterized by a low content of acetic acid. Principal component analysis (PCA) pattern provided a clear categorical discrimination of Chinese vinegars by E-nose and E-tongue analyses. The instrumental sensory scores and the taste attributes for flavor ($r^2=0.9431$), sourness ($r^2=0.9515$), and sweetness ($r^2=0.8325$) were highly correlated. Therefore, SPME/GC-MS, E-nose, and E-tongue analyses may be useful tools to discriminate the sensory profiles of cider vinegars of different origins.

Determination of Volatile Organic Compounds (VOCs) Using Tedlar Bag/Solid-phase Microextraction/Gas Chromatography/Mass Spectrometry (SPME/GC/MS) in Ambient and Workplace Air

  • Lee, Jae-Hwan;Hwang, Seung-Man;Lee, Dai-Woon;Heo, Gwi-Suk
    • Bulletin of the Korean Chemical Society
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    • v.23 no.3
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    • pp.488-496
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    • 2002
  • SPME techniques have proven to be very useful tools in the analysis of wide VOCs in the air. In this study, we estimated VOCs in ambient and workplace air using a Tedlar ba /SPME/GC/MS system. The calibration curve was set to be linear over the range of 1-30 ppbv. The detection limits ranged from 10 pptv to 0.93 ppbv for all VOCs. Reproducibility of TO-14 target gas mixtures by SPME/GC/MS averaged at 8.8 R.S.D (%). Air toxic VOCs (hazardous air pollutants, HAPs) containing a total of forty halohydrocarbons, aromatics, and haloaro-matic carbons could be analyzed with significant accuracy, detection limit and linearity at low ppbv level. Only reactive VOCs with low molecular weight, such as chloromethane, vinylchloride, ethylchloride and 1,2-dichloro-ethane, yielded relatively poor results using this technique. In ambient air samples, ten VOCs were identified and quantified after external calibration. VOC concentration in ambient and workplace air ranged from 0.04 to 1.85 ppbv. The overall process was successfully applied to identify and quantify VOCs in ambient/workplace air.

Evaluation of TVOC contribution from Raw materials of PVC wallpaper using the Headspace-SPME-GC/MS (HS-SPME-GC/MS 법을 이용한 PVC벽지 원자재의 TVOC 기여도 평가)

  • Jang, Mi-Ok;Jeong, Tak-Kyo;Jeong, Yung-Rim;Kim, Man-Goo
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.488-495
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    • 2007
  • A wallpaper having many surfaces in indoor is composed of various raw materials. In this study, TVOC contribution from raw materials of PVC wallpaper was evaluated by using headspace-solid phase microextraction (HS-SPME)-GC/MS. Samples were diluent, resin stabilizer, plasticizer, filler, blowing agent and PVC resin. 9 mL of each sample was put into 22 mL glass vial and they were equilibrated for 1 hour at $100^{\circ}C$. Headspace in vial was absorbed to $75{\mu}m$ Carboxen-PDMS fiber and analyzed by GC/MS. Aromatic compounds like a toluene, ethylbenzene and xylene, ketones compounds like a acetone, methoxyacetone and 2-butanone and alkane compounds like a nonane decane and undecane were identified from raw materials. And alcohol compounds like a ethanol and butanol and aldehydes were detected. TVOC emission of diluent, resin stabilizer, plasticizer, PVC resin, blowing agent and filler were $54.20{\mu}g/g$, $32.88{\mu}g/g$, $0.50{\mu}g/g$, $0.88{\mu}g/g$, $0.22{\mu}g/g$ and $0.11{\mu}g/g$, respectively. Contribution of TVOC emission of diluent, resin stabilizer and PVC resin that were concerned about add ratio were 0.708, 0.129, 0.115, respectively. In conclusion, it's necessary to reduce TVOC emission through improvement of diluent, resin stabilizer and PVC resin. Also, HS-SPME-GC/MS method which was developed in this study will be used for raw materials analysis effectively.

The Identification of Blended Sesame Oils by Electronic Nose (전자코를 이용한 혼합 참기름의 판별 연구)

  • Shin, Jung-Ah;Lee, Ki-Teak
    • Korean Journal of Food Science and Technology
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    • v.35 no.4
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    • pp.648-652
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    • 2003
  • Precise and rapid method out for distinguishing blended sesame oils through the electronic nose analysis was developed. Sesame oil was blended with corn oil at the ratio of 95 : 5, 90: 10, and 80 : 20 (w/w), respectively. Samples were then analyzed by gas chromatography, SPME-GC/MS, and the electronic nose composed of 12 different metal oxide sensors. Sensitivities $(delta\;R_{gas}/R_{air})$ of sensors from electronic nose were analyzed by principal component analysis (PCA). Proportion of the first principal component was 98.76%.

Analysis of Trace Levels of Halonitromethanes (HNM) in Water using Headspace-SPME and GC-ECD (Headspace-SPME와 GC-ECD를 이용한 수중의 미량 Halonitromethane (HNM)류 분석)

  • Kang, So-Won;Son, Hee-Jong;Seo, Chang-Dong;Kim, Kyung-A;Choi, Jin-Taek
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.5
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    • pp.293-302
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    • 2015
  • Halonitromethanes (HNMs) are one of the most toxic groups of disinfection by-products. Recently, various studies have been fulfilled. An automated headspace-solid phase microextraction (SPME) gas chromatography/electron capture detector (GC-ECD) technique was developed for routine analysis of 9 HNMs in water samples. The optimization of the method is discussed. The limits of detection (LOD) and limits of quantification (LOQ) range from 90 ng/L to 260 ng/L and from 270 ng/L to 840 ng/L for 9 HNMs, respectively. Matrix effects in tap water and sea water were investigated and it was shown that the method is suitable for the analysis of trace levels of HNMs, in a wide range of waters. The method developed in the present study has the advantage of being rapid, simple and sensitive.