• Title/Summary/Keyword: Thermal Desorption (TD)

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A Study on Evaluation of Accuracy and Precision on B, T, X Analysis Using Thermal Desorption/Gas Chromatograph/Flams Ionization Detector (열탈착/GC/FID를 이용한 B, T, X 분석의 정확도 및 정밀도 평가)

  • 박정근;유기호
    • Journal of Korean Society for Atmospheric Environment
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    • v.16 no.3
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    • pp.265-275
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    • 2000
  • By using thermal desorption/gas chromatograph/flame ionization detector(TD/GC/FID), this study was carried out to evalute an accuracy and a precision on Benzene(B), Toluene(T), o-Xylene(X) analysis in an industrial hygiene laboratory. Limits of detection of TD/GC/FID on B, T, X were showed 13.75ng/sample or less. For the accuracy of the method by concentration levels, overall bias was showed 7.7% as an absolute value, and the pooled coefficient of variation showed 3.51%. For the precision on repeatability of peak area and retention time between within-run and between-run of analytical system, it is showed the results of within-run gave better than those of between-run. Also the accuracy by sorbents(Tenax TA and Chromosorb 106)was evaluated, and the precision on reproducibility between MDHS72 and this study was compared. It is showed it is possible for TD/GC/FID to evaluate accurately B, T, X concentration levels of less than 1ppm at indoor or outdoor of workplaces in Korea.

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A Study of Analytical Method for Ethylene and Low Weight Hydrocarbons (LWHC) using Thermal Desorption and Gas Chromatography-Flame Ionization Detector with (TD-GC-FID) (저온열탈착기술을 이용한 에틸렌 및 저분자 탄화수소 분석방법 연구)

  • Kim, Bo-Won;Kim, Ki-Hyun;Kim, Yong-Hyun;Ahn, Jeong-Hyeon
    • Journal of Korean Society for Atmospheric Environment
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    • v.30 no.1
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    • pp.77-87
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    • 2014
  • In this study, an experimental approach to measure a suite of low weight hydrocarbons was investigated with an emphasis on ethylene (EL) along with many others (ethane (EA), propane (PA), propylene (PL), n-butane (BA), acetylene (AL), methyl acetylene (ML)). Their concentrations were quantified using GC-FID system equipped with thermal desorption (TD) system. The TD-based analysis was conducted using both Link Tube/Thermal Desorber (LT/TD) method and Modified Injection through a Thermal Desorption (MITD) method. The results of these analyses were evaluated in a number of respects. The system allowed the detection of all compounds except methane with the mean response factor (RF) of 10.28 (EA) to 11.94 (PL). The method detection limits of target compounds were seen in the range of 0.027 (ML) to 0.146 ng (BA). The emission flux of some environmental samples (fruits), when measured using a small flux chamber system, fell in the range of 0.14 (AL: Kiwi) to $181ng{\cdot}g^{-1}{\cdot}hr^{-1}$ (EL: Apple Peel). The results of this study confirm that the experimental approach developed in this study allows to accurately measure emissions of low weight hydrocarbons (LWHC) like ethylene from various natural and man-made source processes.

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.

Composition and Evaluation of the Thermal Desorption-Gas Chromatographic System for the Measurement of Volatile Organic Compounds in Air (공기 중 휘발성 유기화합물의 측정을 위한 열탈착-분석시스템의 구성 및 평가)

  • 이수형;송희남;김희갑
    • Environmental Analysis Health and Toxicology
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    • v.17 no.1
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    • pp.63-71
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    • 2002
  • The thermal desorption-gas chromatographic (TD-GC) system has been constructed for the measurement of volatile organic compounds. The thermal desortion unit is composed of four major parts: 1) the control part; 2) the thermal desorption part; 3) the focusing part; and 4) the injection part. The peltier element was introduced to the focusing part for the temperature of the focusing tube to reach-35$^{\circ}C$. The system was tested for the linearity of the calibration curves and reproducibility of instrumental analyses using some disinfection by-products (DBPs) and BTXs (benzene, toluene and p-xylene). The coefficients of determination (r$^2$) for all the calibration curves made were higher than 0.998, and the coefficients of variation (CV) for triplicate measurements were all within 10%. The system also has been tested for field applicability. The analysis of field samples showed that there was no breakthrough problem in the sampling system and that the system could be applied to field measurements.

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.

A study of analytical method for volatile fatty acids (VFA) by cryogenic trapping-thermal desorption (CT-TD) technique (저온농축열탈착 시스템을 연계한 유기지방산의 분석법 평가 및 검토)

  • Ahn, Ji-Won;Kim, Ki-Hyun;Im, Moon-Soon;Ju, Do-Weon
    • Analytical Science and Technology
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    • v.24 no.3
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    • pp.200-211
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    • 2011
  • In this study, 13 compounds including four volatile fatty acids (VFA) and nine volatile organic compounds (VOC) were analyzed by cryogenic trapping-thermal desorption technique. In order to evaluate the analytical method for VFA, calibration experiments were performed using five different sorbent materials. When the calibration results are compared between different sorbents, sampling tube filled with Carbopack X showed the highest response factor (RF) for both VFA and VOC. To validate this new analytical method for VFA using cryogenic trapping-thermal desorption technique, this method was compared with alkali absorption method recommended by the odor prevention law of the Korea Ministry of Environment (KMOE). For this purpose, unknown samples were analyzed by two different methods, i.e., cryogenic trapping-thermal desorption (TD) and alkali absorption with solid phase microextraction (SPME). When the results of two different methods were compared, ratios of concentrations determined by the two analytical methods (TD/SPME) was found as 0.46 (valeric acid) ~ 0.71 (isovaleric acid). Therefore, additional study is required to properly establish and find stable analytical conditions for VFA analysis. Furthermore, comparison between two different methods should be made with more reliable calibration approaches.

Evaluation of experimental reliability for trace-quantity of gaseous VOC working standards based on thermal desorption analysis (극미량 휘발성유기화합물질의 기체상 표준시료 조제와 열탈착분석방식에 기초한 분석안정도의 평가)

  • Park, Shin-Young;Kim, Ki-Hyun
    • Analytical Science and Technology
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    • v.19 no.6
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    • pp.553-558
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    • 2006
  • In this study, an attempt was made to measure uncertainties involved in the VOC analysis for the VOC working standards prepared by a dilution technique using Tedlar bags. For this purpose, VOC standard gases of benzene, toluene, xylene, and styrene were prepared at four different concentrations (4, 8, 20, and 40 ppb). These standard samples were then loaded on to the GC system equipped with air server/thermal desorption (AS/TD) system. Each of these four standard concentrations was analyzed individually to derive their respective calibration results. These calibration data sets were then compared across four different compounds. According to this comparison, differences in calibration patterns were moderately insignificant within the selected concentration range of 4~40 ppb. It was also observed that the loss of styrene standard was fairly high compared to other VOCs investigated simultaneously. The results of our study suggest that the analytical uncertainty associated with the preparation of VOC starndard gas using a dilution technique can be assessed in a fairly reasonable manner for samples with a narrow concentration range.

Surface Structures and Thermal Desorption Behaviors of Cyclopentanethiol Self-Assembled Monolayers on Au(111)

  • Kang, Hun-Gu;Kim, You-Young;Park, Tae-Sun;Park, Joon-B.;Ito, Eisuke;Hara, Masahiko;Noh, Jae-Geun
    • Bulletin of the Korean Chemical Society
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    • v.32 no.4
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    • pp.1253-1257
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    • 2011
  • The surface structures, adsorption conditions, and thermal desorption behaviors of cyclopentanethiol (CPT) self-assembled monolayers (SAMs) on Au(111) were investigated by scanning tunneling microscopy (STM), X-ray photoelectron spectroscopy (XPS), and thermal desorption spectroscopy (TDS). STM imaging revealed that although the adsorption of CPT on Au(111) at room temperature generates disordered SAMs, CPT molecules at $50^{\circ}C$ formed well-ordered SAMs with a $(2{\surd}3{\times}{\surd}5)R41^{\circ}$ packing structure. XPS measurements showed that CPT SAMs at room temperature were formed via chemical reactions between the sulfur atoms and gold surfaces. TDS measurements showed two dominant TD peaks for the decomposed fragments ($C_5H_9^+$, m/e = 69) generated via C-S bond cleavage and the parent molecular species ($C_5H_9SH^+$, m/e = 102) derived from a recombination of the chemisorbed thiolates and hydrogen atoms near 440 K. Interestingly, dimerization of sulfur atoms in n-alkanethiol SAMs usually occurs during thermal desorption and the same reaction did not happen for CPT SAMs, which may be due to the steric hindrance of cyclic rings of the CPT molecules. In this study, we demonstrated that the alicyclic ring of organic thiols strongly affected the surface structure and thermal desorption behavior of SAMs, thus providing a good method for controlling chemical and physical properties of organic thiol SAMs.

Characteristics of PM2.5 Carbonaceous Aerosol using PILS-TOC and GC/MS-TD in Seoul (PILS-TOC 및 GC/MS-TD를 이용한 서울시 대기 중 초미세먼지(PM2.5) 유기탄소의 특성 분석)

  • Park, Da-Jeong;Ahn, Joon-Young;Shin, Hye-Jung;Bae, Min-Suk
    • Journal of Korean Society for Atmospheric Environment
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    • v.30 no.5
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    • pp.461-476
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    • 2014
  • Continuous Water-Soluble Organic Carbons (WSOC) by the Particle Into Liquid Sampler - Total Organic Carbon (PILS-TOC) analyzer were measured at the Seoul intensive monitoring site from June 17 through July 5 in 2014. In addition, the 24 hour integrated PM2.5 collected by Teflon and Quartz filters were analyzed for water soluble ions by Ion chromatography (IC), WSOC by TOC from water extracts, organic carbon (OC), elemental carbon (EC) by carbon analyzer using the thermal optical transmittance (TOT) method, and mass fragment ions (m/z) related to alkanes and PAHs (Poly Aromatic Hydrocarbons) by Gas Chromatography-Mass Spectrometer-Thermal Desorption (GC/MS-TD). Based on the statistical analysis, four different Carbonaceous Thermal Distributions (CTDs) from OCEC thermal-gram were identified. This study discusses the primary and secondary sources of WSOC based on the Classified CTD, organic mass fragments, and diurnal patterns of WSOC. The results provide knowledge regarding the origins of WSOC and their behaviors.

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.