• 제목/요약/키워드: Thermal desorption unit(TDU)

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TDU-GC/MS를 이용한 한국품종 참당귀 국산 판별 기법 (Geographical origin discrimination of Korean variety, Angelica gigas Nakai by using TDU (Thermal Desorption Unit)-GC/MS)

  • 이미나;김윤석;김원일;김정규;권오경
    • Journal of Applied Biological Chemistry
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    • 제63권1호
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    • pp.29-33
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    • 2020
  • 한약재의 불법 유통을 방지하기 위해 신속 정확한 원산지 판별방법 개발이 필요함에 따라 TDU-GC/MS를 이용하여 한국품종 당귀와 외국품종 당귀를 판별함과 동시에 한국품종 당귀의 재배지가 한국인지를 판별할 수 있는 기법을 연구하였다. 당귀추출물을 열탈착 시킨 후 냉각응축시스템에서 응축시켜 일시에 GC/MS로 분석한 결과 국산 품종 당귀(참당귀)는 TIC의 RT 26.9-27.2에서 coumarin 유도체인 decursin과 decursinol peak가 확인되었다. 중국 품종 당귀(중당귀)의 경우 RT 17.2 부근에서 ligustilide의 peak가 검출되었다. 국산 품종 참당귀 원산지에 따른 휘발성분의 차이를 알아보기 위하여 twister로 흡착하여 TDU-GC/MS로 m/z 40-400 amu 범위에서 mass spectrum을 측정하였다. 참당귀의 국내 및 중국 재배 시료 TIC는 전반적으로 같은 경향을 냈으나 TIC를 부분 scan한 결과 RT 15.4-16.1에서 국내 및 중국 재배의 peak pattern 차이를 확인할 수 있었다. Peak A (RT 15.54)과 B (RT 16.05)의 비율은 국내 재배는 0.0-0.2, 중국 재배의 경우 0.5-2.8으로서 TDU-GC/MS의 TIC peak pattern 비교를 통한 원산지 판별 가능성을 확인하였다.

환경 대기 중 ppt 수준의 황화수소 분석을 위한 GC 방식의 검량 기법에 대한 연구 (Calibration Methods for the Gas Chromatographic Analysis of ppt-level Hydrogen Sulfide (H2) in Air)

  • 김기현;오상인;최여진;최규훈;주도원
    • 한국대기환경학회지
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    • 제19권6호
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    • pp.679-687
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    • 2003
  • In this study, we investigated the analytical techniques to quantify the ambient concentration of hydrogen sulfide (H$_2$S) in air at ppt concentration level. For this purpose, an on-line GC analytical system equipped with both pulsed-flame photometric detector (PFPD) and thermal desorption unit (TDU) was investigated by collecting ambient air samples. The results of our study generally indicated that calibration conditions of GC system is highly sensitive to affect the accuracy of the analytical technique. Most importantly. we found that the use of different matrices in the the preparation stage of working standards was sensitive to control the overall performance of this technique. The calibration of our analytical system was tested by the two types of working standard (prepared by mixing either with high purity $N_2$ or with the ambient air). According to this test, the latter represented more efficiently the detecting conditions of actual air samples. The peak occurrence patterns of both air samples and standards (prepared by mixing with ambient air) were altered in a similar manner as the function of the loaded volume; however, it was not the case for the $N_2$-mixed standards. Results of our study suggest that detection of H$_2$S is highly different from other sulfides and that its quantification requires minimiaing interfering effects of non -pure substance (like water vapor) and (either sorptive or destructive) loss effects.

연속측정방법을 이용한 도심권 대기질 내 저농도 황화합물의 관측에 대한 연구 (Continuous Measurements of Reduced Sulfur Gases in Urban Air)

  • 최여진;김기현;오상인;손장호
    • 한국대기환경학회지
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    • 제20권2호
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    • pp.195-204
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    • 2004
  • In this study, the concentrations of major reduced sulfur compounds (H$_2$S, $CH_3$SH, DMS, and DMDS) were determined from ambient air in a monitoring station located in the mid-eastern area of Seoul. Measurements of sulfur species were conducted by the combination of on -line air sampling, thermal desorption, and capillary GC/PFPD analysis. A total number of 143 hourly samples were collected in the two time periods set between June and July 2003. The mean concentrations of four sulfur species measured in the whole study period were found on the order: DMS (535$\pm$183) > H$_2$S (47$\pm$10) > DMDS (35$\pm$22) > $CH_3$SH (6.19$\pm$29.4 pptv). The results of this study show that the concentrations of DMS at the study area are generally higher than those reported previously in the oceanic environments, while those of other sulfur species are not easy to compare with due to the lack of data. The H$_2$S concentrations were generally higher during the daytime than the nighttime, whereas those of others generally exhibited a reversed diurnal pattern. The overall results of our study suggest that the distribution of major reduced S compounds should be controlled by diverse processes in the urban area.

방향족 휘발성 유기화합물의 겨울철 연속 관측 연구 (Continuous Measurements of Aromatic VOCs in a Mid-eastern Region of Seoul during Winter 2002/2003)

  • 최여진;오상인;김기현
    • 한국대기환경학회지
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    • 제19권5호
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    • pp.491-502
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    • 2003
  • In the present work, the distribution characteristics of ambient volatile organic compounds (VOCs) were investigated at high temporal resolution from a monitoring station located in a mid-eastern area of Seoul. A total number of 587 samples were collected during December 2002 to January 2003. The measurements of VOC were conducted by a combination of on-line air sampling and thermal desorption unit (TDU) coupled with capillary GC/FID analysis. A total of five aromatic compounds (BTEX: benzene, toluene, ethylbenzene, m, p-xylene, and o-xylene) were measured routinely at hourly intervals during the whole study period. The mean concentrations of BTEX measured in our study period were found in the order: toluene (8.99 $\pm$5.38 ppb) > benzene (0.92$\pm$0.52 ppb) > m, p-xylene (0.51$\pm$0.34 ppb) > 0- xylene (0.48$\pm$0.35 ppb) > ethyl benzene (0.43$\pm$ 0.32 ppb). The BTEX concentrations were generally higher during the daytime than the nighttime, exhibiting certain patterns on a weekly basis. Results of our analysis indicate that the unusually high concentrations of toluene, while showing good correlations with other VOCs, can be a good indicator of air pollution in the study area.

GC 분석 시스템의 설정과 그에 따른 감도의 차이: 열탈착 방식 대비 루프주입방식에 의한 황성분의 분석 (Changes in the gas chromatographic sensitivity with its analytical setting: Comparison of TDU and loop-injection system for the analysis of sulfur compounds)

  • 김기현;최여진;김성천
    • 분석과학
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    • 제18권1호
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    • pp.66-73
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    • 2005
  • 본 연구에서는 주요 환원황 화합물에 해당하는 4가지 황성분, $H_2S$, $CH_3SH$, DMS, DMDS을 이용하여, 이들의 주요 검출방법에 해당하는 GC/PFPD 방식의 검출특성을 대부분의 환경시료의 분석에 활용할 수 있는 두 가지 기준에서 비교 분석하였다. 우선 수 십 ppb 단위의 고농도 시료들에 대한 분석특성을 이해하기 위해, GC/PFPD에 루프주입장치를 결합한 고농도 모드 시스템을 구성하고, 이에 대한 평가를 시도하였다. 그리고 이에 대비하여, 열탈착 시스템을 연계한 저농도 모드 시스템을 이용하여, 환경대기와 같이 극단적으로 낮은 농도 (ppt 수준)로 존재하는 시료들의 분석기법을 평가하였다. 양 분석방식의 비교에 의하면, 개별 황성분들의 검출특성은 대단히 규칙적인 특성을 유지하는 것으로 나타났다. 고농도모드를 이용한 비교결과에 의하면, 황화수소의 경우 가장 약한 감도를 보인 반면, 황원소를 두개 함유한 DMDS는 가장 민감한 감도를 보였다. 고농도 모드에 대비하여 저농도 모드의 감도를 비교할 경우, 감도가 수십 배 수준으로 감소하는 것으로 나타났다. 양 방식의 뚜렷한 감도차이에도 불구하고, 선택한 모드에 상관없이 황성분들의 상대적인 검량특성은 비교적 규칙적인 경향성이 유지되는 것으로 나타났다. 이들 성분에 대한 정확한 검량을 위해서는 다양한 관점에서 검출특성을 정의하기 위한 노력이 수반되어야 할 것으로 사료된다.

The Analysis of Sulfur Compounds of Odorous Material in Kunsan Industrial Complex

  • Kim, Seong-Cheon;Kim, Ki-Hyun;Choi, Yeo-Jin
    • 한국환경보건학회:학술대회논문집
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    • 한국환경보건학회 2005년도 국제학술대회
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    • pp.399-405
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    • 2005
  • In this study, we investigated the gas chromatography (GC) and pulsed flame photometric detection (PFPD) system for the analysis of four major reduced S compounds including hydrogen sulfide ($H_2S)$; methyl mercaptan ($CH_3SH$); dimethyl sulfide (DMS); and dimethyl disulfide(DMDS) contained in environmental samples. To analyze these compounds in high concentration range (above ppb level), we developed a high mode analytical setting with the loop-injection system. By contrast, we also established a low mode setting for the analysis of low concentration samples (ppt-level samples from ambient air) by the combination with thermal desorption unit(TDU). Comparative analysis of both settings revealed that relative detection properties of four S compounds are systematic enough. The results of high mode analysis indicated that the patterns were systematic among compounds: H2S exhibited the lowest sensitivity, while DMBS showed the strongest one. The results were also compared in terms of sensitivity reductions for all compounds by dividing slope ratios between low and high mode system. Although low mode system exhibited significant reductions on the order of a few tens times, their detection characteristics were highly consistent as it was shown in the high mode setting. To learn more about absolute and relative relations between two different modes of S analysis, future studies may have to be directed to cover more complicated nature of GC/PFPD performance. Hydrogen sulfide($H_2S$) was over in summer about low level of olfactory sense 410 ppt, Methyl mercaptan(C$H_3SH$) was over in apring and summer about low level of olfactory sense 70, Dimethyl sulfide(DMS) was not over in four season about low level of olfactory sense 2,200 ppt. Carbon disulfide($CS_2$) was not over in four deason about Tow level of olfactory sense 210,000, Dimethyl disulfide(DMDS) was not over in summer about low level of olfactory sense2,000.

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