• Title/Summary/Keyword: thermal desorption gas chromatography/mass spectrometry

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Analysis of Organic Compounds in Ambient PM2.5 over Seoul using Thermal Desorption-comprehensive Two Dimensional Gas Chromatography-time of Flight Mass Spectrometry (TD-GCxGC-TOFMS) (Thermal Desorption-comprehensive Two Dimensional Gas Chromatography-time of Flight Mass Spectrometry (TD-GCxGC-TOFMS)을 이용한 서울 대기 중 PM2.5 유기성분 분석)

  • Lee, Ji-Yi;Lane, Douglas A.;Huh, Jong-Bae;Yi, Sung-Muk;Kim, Yong-Pyo
    • Journal of Korean Society for Atmospheric Environment
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    • v.25 no.5
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    • pp.420-431
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    • 2009
  • Characteristics and advantages of the thermal desorption-comprehensive two dimensional gas chromatography-time of flight mass spectrometry (TD-GCxGC-TOFMS) were discussed and the organic compound's analysis result was shown for the ambient $PM_{2.5}$ sample collected in Seoul, Korea. Over 10,000 individual organic compounds were separated from about $70{\mu}g$ of aerosols in a single procedure with no sample pre-treatment. Among them, around 300 compounds were identified and classified based on the mass fragmentation patterns and GCxGC retention times. Several aliphatic compounds groups such as alkanes, alkenes, cycloalkanes, alkanoic acids, and alkan-2-ones were identified as well as 72 PAH compounds including alkyl substituted compounds and 8 hopanes. In Seoul aerosol, numerous oxidized aromatic compounds including major components of secondary organic aerosols were observed. The inventory of organic compounds in $PM_{2.5}$ of Seoul, Korea suggested that organic aerosol were constituted by the compounds of primary source emission as well as the formation of secondary organic aerosols.

A Low-Cost Open-Source Air Sampler for the Sorbent Tube Sampling for TD-GC/MS Analysis

  • Jang, Hwa-yong;Oh, Han Bin
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.95-102
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    • 2020
  • In this study, we provide full descriptions of how to make a low-cost and completely open-source laboratory-made air sampler that will be used for sample adsorption for thermal desorption-gas chromatography mass spectrometry (TD-GC/MS) analysis. It is well known that harmful gases cause bad effects on human bodies, so it is necessary to identify the types and amounts of gases in industrial sites. One of the most commonly used methods for gas sampling is to utilize a sorbent tube using an air sampler. Commercially available air samplers are expensive, typically priced between $1,000 and $2,000, and their design often cannot be modified to fit the experiment. To address these shortcomings, we have developed a do-it-yourself (DIY) air sampler that is not only cheap enough, but also completely open-source. Furthermore, the performance of the fabricated air sampler was validated in conjunction with TD-GC/MS for the analysis of volatile compounds.

Headspace gas chromatographic analysis as an objective method for measuring rancidity in soybean oil (Headspace 가스크로마토그라피를 이용한 대두유 산화진행도의 객관적 평가방법)

  • Chun, Ho-Nam;Kim, Ze-Uook
    • Applied Biological Chemistry
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    • v.34 no.2
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    • pp.154-161
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    • 1991
  • An objective method for measuring rancidity in soybean oil was developed based on the volatile contents obtained by headspace gas chromatographic analysis. Apparatus for headspace volatile cold trapping-thermal desorption was described, designed to collect and analyze volatiles of soybean oil. Samples of commercially processed soybean oil were stored under controlled condition and then evaluated for flavor by a eight member trained panel and for volatile contents by headspace gas chromatographic analysis. Twenty-three GC peaks were identified on the basis of relative retention time of reference compounds and gas chromatography-mass spectrometry. The volatile compounds identified were autoxidation products of principal unsaturated fatty acids of soybean oil. The simple linear regressions of flavor score with the pentanal or hexanal contents in aged soybean oil gave correlation coefficient of 0.990 and 0.994. respectively. Pentanal and hexanal contents could be used as a potentially useful index for predicting flavor scores of soybean oil.

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Evaluation of vegetable oil rancidity by headspace gas chromatographic analysis (Headspace 가스크로마토그라피를 이용한 식용유의 산패도 측정)

  • Chun, Ho-Nam;Kim, Ze-Uook
    • Applied Biological Chemistry
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    • v.35 no.1
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    • pp.36-41
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    • 1992
  • Several commercial cottonseed, corn and rapeseed oils were stored at $60^{\circ}C\;and\;70^{\circ}C$ with daily exposure of fluorescent light for 12 hours and evaluated their rancidity by headspace gas chromatographic analysis of pentanal and hexanal. The data of gas chromatographic analysis was compared with organoleptic flavor evaluation. For headspace gas chromatographic analysis, the volatile compounds were recovered by porous polymer trap and flushed into a fused silica capillary column at $250^{\circ}C$. Twenty-three GC peaks were identified on the basis of relative retention time of reference compounds and gas chromatography-mass spectrometry. The results showed that the contents of pentanal and hexanal were linearly increased during storage. A very simple linear relationship was found between organoleptic flavor scores and amounts of two volatile compounds with very high correlation coefficient. This results suggested the possible implication of pentanal and hexanal as an quality index for rancidity evaluation of cottonseed, corn and rapeseed oils.

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Development of Fast Screening Method for Crop Protection Agents in Tobacco by Stir Bar Sorptive Extraction and Thermal Desorption coupled to GC/MS

  • Min, Hye-Jeong;Lee, Jeong-Min;Shin, Han-Jae;Lee, Moon-Yong;Jang, Gi-Chul
    • Journal of the Korean Society of Tobacco Science
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    • v.36 no.1
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    • pp.26-33
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    • 2014
  • Simultaneous determination of crop protection agents(CPAs) in food are done with multi-residue methods, which are composed of sample clean-up, concentration, chromatographic separation and detection. Stir Bar Sorptive Extraction(SBSE) technique is used for sample preparation of various analytes in several fields. The aim of this study was to develop a sensitive and fast method based on SBSE followed by thermal desorption - gas chromatography - mass spectrometry(TD - GC/MS) to determine CPAs in tobacco sample. For the analysis of tobacco sample prior to the SBSE method, solvent extraction or ultrasound-assisted solvent extraction was performed. methanol was used as the extraction solvent. The extract was then diluted with water. Finally, the sample was subjected to SBSE. A method for fast screening of crop protection agents in tobacco using SBSE-TD - GC/MS has been developed. About 17 CPAs including organochlorine, organophosphorous and others were identified and quantified. This method showed good linearity and high sensitivity for most of the target CPAs. The method was applied to the determination of CPAs at ng/mL levels in tobacco sample. This method is simple, rapid and may be applied in detection of other components.

Evaluation of the Measurement of Trace Phenols by Adsorption/Thermal Desorption/Gas Chromatography/Mass Spectrometry (ATD/GC/MS) in Artificial Air (흡착관/열탈착 GC/MS 방법에 의한 모사시료 중의 미량 페놀 분석에 관한 평가)

  • 허귀석;이재환;황승만;정필갑;유연미;김정우;이대우
    • Journal of Korean Society for Atmospheric Environment
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    • v.18 no.2
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    • pp.127-137
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    • 2002
  • Phenolic compounds in air are toxic even at their low concentrations. We had evaluated a total of five phenolic compounds (Phenol, o-Cresol, m-Cresol, 2-Nitrophenol and 4-Chloro-3-methylphenol) in artificial air using a combination of ATD/GC/MS. To compare the adsorption efficiency of these phenolic compounds, three adsorbents (Tenax TA, Carbotrap and Carbopack B) were tested. Tenax TA adsorbent was most effective of all the adsorbents used for the efficiency test. Five phenolic compounds were found to be very stable on adsorbent tubes for 4 days at room temperature. Detection limit of five phenolic compounds ranged from 0.05 to 0.08 ppb (when assumed to collect 10 L air). The calibration curve was linear over the range of 22∼ 164 ng. The reproducibility was less than 4%. Sampling of duplicate pairs (DPs) was made to demonstrate duplicate precision and sampling efficiency.

Analysis of Environmental Odor Factors for Dorim Stream in Gwanak-gu, Seoul (서울시 관악구 도림천 복개 정도에 따른 환경 악취 요인 분석)

  • Soyoung Park;Gokce Nur Ayaz;Heewon Kim;Hyungkee Yoon;Taehong Kwon;Sungkyoon Kim
    • Journal of Environmental Health Sciences
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    • v.50 no.2
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    • pp.83-92
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    • 2024
  • Background: In this study, we investigate the rapid increase in environmental odors and notable rise in civil complaints near Dorim Stream in the Gwanak-gu area of Seoul. Objectives: This study aims to identify the causal compounds responsible for environmental odors in the Dorim Stream and investigate the structural characteristics of the stream that influence odor generation. Methods: The research methodology involved setting up 41 sampling points, selecting panels for direct sensory evaluation to assess odor intensity, measuring dissolved oxygen and hydrogen sulfide concentrations, and using all-in-one low-temperature desorption gas chromatography (ATD-GC) and thermal desorption-gas chromatography-mass spectrometry (TD-GC/MS) analysis to identify odor-causing compounds. Results: The evaluation of Dorim Stream revealed that in areas with complete meandering, there were lower dissolved oxygen levels (4.5±2.67 mg/L) and higher odor intensity (4.0±0.92), while in partially meandering sections, higher dissolved oxygen levels (7.8±1.15 mg/L) and lower odor intensity (2.8±1.06) were observed. Hydrogen sulfide levels measured with sensors increased with higher temperatures, especially in the afternoon hours (12:00~14:00). Acetaldehyde was the dominant odor compound detected in both the Bonglim Bridge (0.4 ppm) area and Guro Bridge area (0.867 ppm), with concentrations more than twice as high near Guro Bridge. Odor-causing compounds identified by TD-GC/MS indicated a pungent, sulfurous odor in the Guro Bridge area and a musty odor in the Bonglim Bridge area. Conclusions: This study categorizes and analyzes the sources of odor in Dorim Stream in Seoul based on meandering patterns and the distribution of sewage facilities, highlighting the potential odor issues associated with combined sewage systems and sewer junctions and suggesting policy improvements.

Study on Thermal Properties of CdS - Embedded Poly(2-Acetamidoacrylic acid) Hydrogel Composite (CdS 나노입자틀 삽입한 Poly(2-Acetamidoacrylic acid) 수화젤 복합체의 열적 특성에 관한 연구)

  • Park, Chun-Ho;Ha, Eun-Ju;Jung, Jong-Mo;Lee, Jang-Oo;Paik, Hyun-Jong
    • Polymer(Korea)
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    • v.33 no.1
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    • pp.1-6
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    • 2009
  • We report the template-based synthesis of well-dispersed CdS nanoparticles (NPs) in the interior of poly (2-acetamidoacrylic acid) (PAAA) hydrogel as a novel type of nanocomposite without particle aggregation via ion exchange in a aqueous system. As revealed by the TEM image analysis, the mean crystallite diameter of CdS NPs embedded in hydrogel composite was 4.5 nm, and the composite did not suffer any observable change after 6 months. Desorption/decomposition of CdS/PAAA hydrogel composite was studied by evolved gas analysis-gas chromatography-mass spectrometry (EGA-GC-MS), and thermogravimetric analysis (TGA) methods. From the TGA data, the thermal stability of the composite system increased by ca. 100 $^\circ$C and the content of CdS NPs in a dry composite gel was over 70 wt%. In addition, the chemical pathway was proposed for the entire decomposition process.

Biogenic Volatile Organic Compounds (BVOC) Emissions from Fruit Samples Based on Sorbent Tube Sampling and Thermal Desorption (ST-TD) Analysis (흡착튜브 - 열탈착 정량분석 기법에 기반한 과일시료로부터 자연적 휘발성유기화합물의 배출특성 연구)

  • Ahn, Jeong-Hyeon;Kim, Ki-Hyun
    • Journal of Korean Society for Atmospheric Environment
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    • v.29 no.6
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    • pp.757-772
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    • 2013
  • In this study, a combination of sorbent tube (ST)-thermal desorption (TD)-gas chromatography (GC)-mass spectrometry (MS) was used for quantitative analysis of liquid phase standards of 10 BVOC ((1) (+)-${\alpha}$-pinene, (2) (+)-${\beta}$-pinene, (3) ${\alpha}$-phellandrene, (4) (+)-3-carene, (5) ${\alpha}$-terpinene, (6) p-cymene, (7) (R)-(+)-limonene, (8) ${\gamma}$- terpinene, (9) myrcene, and (10) camphene). The results of BVOC calibration yielded comparatively stable pattern with response factor (RF) of 23,560~50,363 and coefficient of determination ($R^2$) of 0.9911~0.9973. The method detection limit (MDL) of BVOC was estimated at 0.03~0.06 ng with the reproducibility of 1.30~5.13% (in terms of relative standard error (RSE)). Emissions of BVOC were measured from four types of fruit samples ((1) tangerine (TO), (2) tangerine peel (TX), (3) strawberry (SO), and (4) sepals of strawberry (SX)). The sum of BVOC flux (${\sum}flux$ (BVOC) in ng/hr/g) for each sample was seen on the descending order of (1) TX=291,614, (2) TO=2,190, (3) SO=1,414, and (4) SX=2,093. If the results are compared between the individual components, the highest flux was seen from (R)-(+)-limonene (265,395 ng/hr/g) from TX sample.

Safety Profile Assessment and Identification of Volatile Compounds of Krill Eupausia superba Oil and Residues Using Different Extraction Methods

  • Haque, A.S.M. Tanbirul;Kim, Seon-Bong;Lee, Yang-Bong;Chun, Byung-Soo
    • Fisheries and Aquatic Sciences
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    • v.17 no.2
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    • pp.159-165
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    • 2014
  • In this study, Krill Eupausia superba oil was extracted using different solvents and supercritical carbon dioxide (SC-$CO_2$). During SC-$CO_2$ extraction, the pressure was set at 40 MPa and temperatures ranged from $40^{\circ}C$ to $55^{\circ}C$. We examined the differences in volatile compounds and safety profiles among extraction methods. Volatile compounds were determined using the thermal desorption system integrated with gas chromatography-mass spectrometry (GC-MS). Heavy metal content was analyzed by inductively coupled plasma mass spectrometry (ICP-MS). According to our results 10 volatile compounds were identified in krill sample. After SC-$CO_2$ extraction of oil, the concentrations of volatile compounds decreased, but increased after solvent extraction. In krill, heavy metal concentrations remained within the permissible limit. Moreover, Zn and Fe which have health benefits were detected at high concentrations. During a 90 days storage period at different temperatures, microbial activity was found to be lowest in SC-$CO_2$ extracted residues. Thus, the quality of krill oil and the residues obtained using SC-$CO_2$ extraction was higher and the oil was safer than those obtained using conventional solvent extraction. These results can be applied to the food industry to maintain high quality krill products.