• Title/Summary/Keyword: 가스크로마토그래피 /질량분석기

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Catalytic Pyrolysis of Waste Paper Cup Containing Coffee Residuals (커피 잔류물을 함유한 폐종이컵의 촉매 열분해)

  • Shin, Dongik;Jeong, Seokmin;Kim, Young-Min;Lee, Hyung Won;Park, Young-Kwon
    • Applied Chemistry for Engineering
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    • v.29 no.2
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    • pp.248-251
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    • 2018
  • Catalytic pyrolysis of the waste paper cup containing coffee residual (WPCCCR) was performed using a fixed bed reactor and pyrolyzer-gas chromatography/mass spectrometry (Py-GC/MS). Non-catalytic pyrolysis of WPCCCR produced a large amount of oil together with gas and char. The use of both HZSM-5 and HY decreased the yields of oil and increased the yield of gas due to the additional catalytic cracking. Owing to the acidic catalytic properties of HZSM-5 and HY, catalytic Py-GC/MS analysis of WPCCCR increased the selectivity to aromatic hydrocarbons in product oil. Owing to properties of HZSM-5 having a stronger acidity and medium pore size, the catalytic pyrolysis of WPCCR over HZSM-5 produced much larger amounts of aromatic hydrocarbons than that of using HY.

ATR 분광계를 이용한 화학증착소재 흡착에 따른 표면거동에 대한 연구

  • Park, Myeong-Su;Kim, Yeong-Gyu;Sin, Jae-Su;Lee, Chang-Hui;Yun, Ju-Yeong;Gang, Sang-U
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.120.2-120.2
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    • 2013
  • 반도체 소자의 소형화로 신개념 화학증착공정 구현을 위한 장비와 화학증착소재의 개발이 활발이 연구되고 있다. 특히 증착소재의 물리적 화학적 특성을 파악하고 가장 적합한 소재를 선택하기 위한 연구도 변행되고 있다. 많은 연구자들이 소재 평가를 위해 가스크로마토그래피, 질량분석기, 적외선 분광기 등을 이용한 화학증착소재의 특성을 파악하기 위해 노력하고 있다. 하지만 실제 화학기상증착(Chemical Vapor Deposition)법과 원자층증착(Atomic Layer Deposition)법 공정에서 웨이퍼 표면에서의 화학증착소재의 흡착거동에 대한 연구는 거의 전무한 실정이다. 따라서 본 연구에서는 개선된 Attenuated Total Reflectance(ATR)분광계를 이용하여 표면에 흡착된 소재의 흡착거동에 대해 분석을 수행하였다. 평가에 사용된 화학증착소재는 C-Zr (Tris (dimethylamino) cyclopentadienyl zirconium)이며, Fourier Transform Infrared Spectroscopy (FT- IR)시스템 내에 설치된 ATR 분광계 표면에 흡착된 C-Zr 증착소재를 다양한 공정조건(온도 및 반응가스, 플라즈마 파워 등)에서의 거동 변화를 연구하였다.

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Algorithm to Improve Mass Spectral Resolution of Gas Chromatography Mass Spectrometer (가스크로마토그래피 질량분석기의 질량 스펙트럼 해상도 개선 알고리즘)

  • Choi, Hun
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.67 no.9
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    • pp.1232-1238
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    • 2018
  • This paper proposes methods for improving mass spectral resolution for a gas chromatograph mass spectrometer. The slope signs of the 1st and 2nd fitting functions for the ion signal block of each mass index are obtained, and the unnecessary element signals in the ion signal block are removed. The spectrum can be obtained by obtaining the second-order fitting function of the reconstructed ion signal block using only the effective ion signals. In addition, the resolution of the mass spectrum can be improved by correcting the error caused by the shift of the spectral peak position. To verify the performance of the proposed methods, computer simulations were performed using the actual ion signals obtained from the GC-MS system under development. Simulation results show that the proposed method is valid.

A Study on the Development of Quantitative Analysis Methods to Characterize the Transport of Microplastics in Saturated Porous Media (포화 다공성 매체에서 미세플라스틱 이동 특성 규명을 위한 정량분석 방법 개발 연구)

  • Suhyeon Park;Minjune Yang
    • Proceedings of the Korea Water Resources Association Conference
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    • 2023.05a
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    • pp.376-376
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    • 2023
  • 전 세계적으로 중요한 담수 자원인 지하수의 미세플라스틱 오염에 대한 우려가 커지고 있다. 지하수 환경에서 미세플라스틱의 오염을 예측하고 평가하기 위해 대수층 내 현장 실태조사가 수행 중에 있으며, 실험실 규모의 컬럼 실험을 통해 지하수에서 미세플라스틱 이동 메커니즘을 조사하는 연구들이 수행되고 있다. 이러한 연구들은 많은 개수의 분석 시료를 동반하며, 환경 중 미세플라스틱 정량분석을 위해서 고가의 분석기기(라만분광기, 푸리에 변환 적외선(FTIR) 분광기, 열분해 가스크로마토그래피 질량분석기)를 사용하여 플라스틱의 종류를 판별하고 개수를 측정하고 있다. 또한, 컬럼 실험을 수행한 대부분의 선행 연구에서는 미세플라스틱 정량분석을 위해 탁도 분석, 분광광도계를 이용한 흡광도 분석, 현미경을 이용한 계수 방법 등을 이용하여 고가의 분석기기를 사용하지 않고 연구를 수행하였다. 하지만, 이러한 방법들은 유체 속 다른 물질이 포함되어있을 경우에 민감하고 농도를 비율 혹은 개수로 표현하기 때문에 질량 측면에서 미세플라스틱의 농도를 과소·과대 평가할 수 있다. 특히, 현미경을 이용한 계수 방법의 경우에는 분석에 많은 시간이 소요된다는 단점이 있다. 위에 언급한 다양한 분석법들의 단점들을 보완하기 위하여, 본 연구에서는 대수층 내 미세플라스틱 이동 특성을 규명하기 위한 실내 실험에 사용될 수 있는 형광이미지 기반의 미세플라스틱 정량분석법을 개발하였다. Nile Red 형광염료를 이용하여 미세플라스틱을 염색하고 사진을 촬영하여 미세플라스틱 시료의 질량과 미세플라스틱 형광이미지의 형광강도 간 상관관계를 분석하였다. 또한, Nile Red로 염색된 미세플라스틱 입자의 수중 노출 테스트를 진행하여, 실내 대수층 모의실험 시 미세플라스틱 질량을 정량화할 수 있는 적용 가능성을 평가하였다. 상관 분석 결과, 미세플라스틱 질량과 이미지의 형광강도는 높은 상관관계를 보였으며, 수중 노출 실험 전과 후의 미세플라스틱 입자의 형광강도 차이는 미미한 것으로 나타났다. 이러한 연구결과를 통해 본 연구에서 개발된 미세플라스틱 정량분석 방법이 포화 다공성 매체로 구성된 컬럼실험 시 유출수의 미세플라스틱 질량 추정에 유용하게 사용될 것으로 생각되며, 대수층 내 미세플라스틱의 이동 특성 규명 연구에 많은 도움이 될 것으로 기대된다.

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Application of Freezing Filtration Method to the Analysis of Alkylphenols, Chlorophenols and Bisphenol a in Korean Aquatic Biological Samples Using GC/MS-SIM (GC/MS-SIM을 이용한 우리나라 수중 생물시료 중 알킬페놀, 클로로페놀과 비스페놀 A의 분석을 위한 냉동필터법의 응용)

  • Kim, Hyub;Jang, Cheol-Hyeon
    • Journal of Korean Society of Environmental Engineers
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    • v.29 no.6
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    • pp.689-698
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    • 2007
  • A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples. The alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at $-60^{\circ}C$ for 2 hours(freezing filtration method). Also, solid-phase extraction(SPE) was used to XAD-4 and subsequent conversion to isobutoxycarbonyl(isoBOC) or tert-butyldimethylsilyl(TBDMS) derivatives for sensitive analysis with gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM) mode. For isoBOC derivatization and TBDMS derivatization the recoveries were $70.1\sim150.6%$ and $93.8\sim108.3%$, the method detection limit(MDLs) of bisphenol A for SIM were $0.062{\mu}g/kg$ and $0.010{\mu}g/kg$, and the SIM respectively. When these methods were applied to korean aquatic biological samples, the concentrations of the 11 phenolic EDCs were $0.675\sim1.970{\mu}g/kg$.

Simple Method in Trace Analysis of Phthalates in Cosmetics : Analytical Conditions and Skills for Better Results (화장품에서 프탈레이트 미량분석을 위한 간편한 분석법 : 향상된 결과를 위한 분석조건과 기술)

  • Kim, Min-Kee;Jung, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.34 no.1
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    • pp.51-55
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    • 2008
  • Although phthalates aren't used as an cosmetic ingredient, some cosmetics especially nail lacquer, hair spray, and perfume still have phthalates. This is mainly caused by contamination and carryover during manufacturing process, so analysis of phthalates in those cosmetics has became a very important thing for quality-assurance(Q.A). The main phthalates under debate are diethyl phthalate(DEP), dibutyl phthalate(DBP), and bis(2-ethylhexyl) phthalate (DEHP) in domestic market. Gas chromatography-mass spectrometry(GC-MS) coupled with solvent extraction and concentration has been used for ppm level and sub ppm level analysis of phthalates. It requires much time and cost to use mass spectrometric detector and to prepare the test solution. Moreover analysis of phthalates at low concentrations is difficult because of contamination which results in wrong analytical results. In the present study, we showed a simple method using gas chromatography-flame ionization detector(GC-FID) which has fast analysis time, minimum use of solvent, reduced sample preparation steps for minimizing contamination and quantitative range of $2{\sim}50{\mu}g/g(ppm)$ in products. Consequently, this method will be proper for Q.A analysis in related companies.

Analysis of Mint Essential Oils from Jeju Island, Korea by Gas Chromatography-mass Spectrometry and Headspace-Gas Chromatography-mass Spectrometry (Gas Chromatography-mass Spectrometry와 Headspace-Gas Chromatography-mass Spectrometry를 이용한 제주산 민트 에센셜오일 성분 분석)

  • Hyun, Ho Bong;Boo, Kyung Hwan;Kang, Hye Rim;Kim Cho, Somi
    • Journal of Applied Biological Chemistry
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    • v.58 no.2
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    • pp.175-181
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    • 2015
  • Compositions of essential oils extracted from mint herb such as Mentha piperita, Mentha spicata, and Mentha ${\times}$ piperita var. citrate produced in Jeju were analyzed using gas chromatography-mass spectrometry (GC-MS) and headspace-GC-MS (HS-GC-MS). By the GC-MS analysis, 13 compounds were tentatively identified in Mentha piperita, Mentha spicata, and Mentha ${\times}$ piperita var. citrate, respectively. Peperitenone oxide, carvone, and linalool were detected as major compounds in Mentha piperita, in Mentha spicata, in Mentha ${\times}$ piperita var. citrate, respectively, based on the ratio of peak intensity in the total ion chromatogram. The greater number of compounds, including volatile alcohols and acetates were identified by HS-GC-MsS than by GC-MS in these all three essential oils. Similar patterns of composition were detected in both Mentha spicata and Mentha ${\times}$ piperita var. citrate by either one of GC-MS methods. However, in case of Mentha piperita, $\small{L}$-(-)-menthol, which was identified as the major compound by HS-GC-MS was detected in dramatically reduced quantity by GC-MS. Interestingly, we found that both linalyl acetate and linalool were identified as the dominant compounds in the essential oil of Mentha ${\times}$ piperita var. citrate.

Research on Pyrolysis Properties of Waste Plastic Films (폐플라스틱 필름의 열분해특성에 대한 연구)

  • Kim, Young-Min;Lee, Boram;Han, Tae Uk;Kim, Seungdo;Yu, Tae-U;Bang, Byoung Yeol;Kim, Joug-Su;Park, Young-Kwon
    • Applied Chemistry for Engineering
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    • v.28 no.1
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    • pp.23-28
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    • 2017
  • Pyrolysis characteristics of waste plastic films were investigated by using a thermogravimetric analysis and pyrolyzer-gas chromatography/mass spectrometry. Thermogravimetric analysis results revealed that the pyrolysis of waste plastic films can be divided into two distinct reactions; (1) the decomposition reaction of starch at between 200 and $370^{\circ}C$ and (2) that of other plastic polymers such as PS, PP, PE at between 370 and $510^{\circ}C$. The kinetic analysis results obtained by using the revised Ozawa method indicated that the apparent activation energy of the pyrolysis reaction of waste plastic films was also changed dramatically according to the different decomposition reactions of two major waste plastic film components. Py-GC/MS results also revealed that the typical pyrolyzates of each polymer in waste plastic films were levoglucosan (starch), terephthalic acid (PET), styrene monomer, dimer, and trimer (PS), methylated alkenes (PP), and triplet peaks (PE) composed of alkadiene/alkene/alkane. The phthalate, used as a polymer additive, was also detected on the pyrogram of waste plastic films mixture.

Accurate Analysis of Trace Phthalates and Method Validation in Cosmetics using Gas Chromatography with Mass Spectrometric Detection (화장품에 함유된 미량의 프탈레이트 함량을 정확히 분석하기 위한 가스크로마토그래피-질량분석 시험법 및 그 시험법의 유효성)

  • Kim, Min-Kee;Jeong, Hye-Jin;Cho, Jun-Cheol
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.38 no.1
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    • pp.33-41
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    • 2012
  • An effective, environmentally friendly analytic methods using gas chromatography with mass spectrometric detector (GC-MSD) have been developed for the quantitative analysis of trace phthalate levels in cosmetics such as nail lacquer and hair spray. Since such cosmetics are largely comprised of organic solvents, conventional clean-up methods that have been widely used for phthalate analyses are in adequate. In addition, analysis of trace phthalate levels is notorious for its sensitivity to contamination, which causes high analytical values. A direct sample dilution method using an organic solvent was adopted to the sample preparation process to determine the exact amounts of phthalates and simultaneously avoid the high risk of secondary contamination. The method has many advantages including high accuracy, sensitivity, and simplicity in sample preparation. Dibutyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) were selected for analysis because they have been frequently detected in cosmetics and consistently reported as endocrine disruptors in humans and animals. Internal standard method using two deuterium substitutes (DBP-$d_4$, DEHP-$d_4$) as the internal standard was also used. The results of 'Method validation' showed the capabilities of this method for the routine analysis of phthalates at the ppm level. The recovery ranges were between 95 % and 106.1 %, and relative standards deviations (RSD) were less than 3.9 % in fortified nail lacquer and hair spray samples at the concentration of $25{\mu}g/g$.

Simultaneous Determination of Pesticides in Water Using a GC/MS Coupled with Micro Extraction by Packed Sorbent (MEPS-GC/MS를 이용한 농약류 동시 수질분석)

  • Lee, Ki-chang;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.5
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    • pp.262-268
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    • 2015
  • This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using $30{\mu}L$ of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and $0.08{\sim}0.59{\mu}g/L$, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of $0.5{\sim}5.0{\mu}g/L$. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.