• 한국대기환경학회지
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• 제16권3호
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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.

• 한국대기환경학회지
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• 제30권1호
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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.

• 한국대기환경학회지
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• 제25권5호
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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.

• Environmental Analysis Health and Toxicology
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• 제17권1호
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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.

• 한국연초학회지
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• 제36권1호
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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.

• 분석과학
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• 제24권3호
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• pp.200-211
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• 2011

본 연구에서는 저온농축열탈착법을 이용하여, 4가지 유기지방산 및 9가지 휘발성유기화합물을 포함하는 13가지 성분의 분석기법을 비교연구하였다. 저온농축열탈착법을 이용한 유기지방산의 분석기법을 평가하기 위해, 5가지 흡착소재 각각에 대해 5점 검량에 기초한 비교를 시도하였다. 그 결과, 유기지방산 및 휘발성 유기화합물에서 Carbopack X를 충진한 고체흡착관의 response factor (RF)가 가장 높은수준을 유지하면서, 유기지방산과 휘발성유기화합물의 동시분석에 가장 적합한 것으로 나타났다. 그러나 Tenax TA 단일소재를 제외하면, 조사에 이용한 대부분의 흡착제도 양호한 것으로 나타났다. 저온농축열 탈착법의 검정을 위한 임의의 방안으로 기체상 표준시료를 저온농축열탈착법과 알칼리흡수법으로 동시에 비교분석하였다. 그 결과, 유기지방산에서 저온농축열탈착법 대비 알칼리흡수법의 비율 (T/S비)이 0.46 (valeric acid)~0.71 (isovaleric acid)으로 나타나 저온농축열탈착법의 결과가 상대적으로 낮게 나타났다. 보다 안정적인 분석조건을 찾기 위한 연구를 추가적으로 지속한다면, 유기지방산의 분석법을 향상시키는 것이 가능할 것으로 사료된다.

• 분석과학
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• 제19권6호
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• pp.553-558
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• 2006

본 연구에서는 Tedlar bag을 사용하여 조제한 작업용 기체상 표준시료를 열탈착과 GC/FID를 조합한 시스템으로 분석할 때, 발생 가능한 오차를 평가하고자 하였다. 이를 위해, 여러 가지 VOC성분(Benzene, Toluene, p-Xylene, Styrene)을 함유하는 표준시료를 4 가지 초기농도대(4~40 ppb)에서 조제하였다. 그리고 이들 작업용 시료를 이용하여, 각각의 검량결과를 도출하고 비교분석을 실시 하였다. 본 실험에서 설정한 4~40 ppb 농도대의 검량결과를 비교하기 위해, 공기분배/저온농축/열탈착 전용기(Air server/thermal desorber (AS/TD))와 조합한 GC/FID 시스템을 사용하였다. 본 연구의 결과, 표준시료의 조제방식이나 그와 연관된 초기농도의 차이가 검량 특성에 영향을 미친다고 하기는 어렵다는 결론을 내릴 수 있었다. 그러나 테들러백을 사용하는 경우, 여타 성분들에 비해 Styrene성분에서 감도가 떨어지는 경향이 크게 나타나는 점을 확인할 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제32권4호
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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.

• 한국대기환경학회지
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• 제30권5호
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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.

• Mass Spectrometry Letters
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• 제11권4호
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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.