• Title/Summary/Keyword: 가스크로마토그래피-질량 분석

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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.

나노 입자를 이용한 기상 전구체의 흡착거동 분석

  • Kim, Jong-Ho;Gang, Byeong-Su;Lee, Chang-Hui;Sin, Jae-Su;Gang, Sang-U
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.100.2-100.2
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    • 2015
  • 반도체 산업이 성장하고 기술이 향상됨에 따라 소자의 소형화가 이루어지고 있다. 공정법으로는 atomic layer deposition (ALD), chemical vapor deposition (CVD) 등이 있다. 이러한 공정을 이용하여 수십 nm까지 미세화가 진행되고 있으며, 복잡한 구조의 박막을 실현하기 위해 전구체의 개발이 활발히 진행되고 있다. 전구체의 특성을 비실시간으로 분석하는 방법으로는 질량 분석법, 가스크로마토그래피, 적외선 분광법 등이 있다. 전구체의 특성을 실시간으로 분석하기 위해 Fourier transform infrared spectroscopy (FTIR)내에 attenuated total reflectance (ATR)를 거치시켰다. 본 연구는 구조를 개선한 ATR-FTIR을 이용하여 Tris-(dimethylamino) Zirconium (CpZr) 전구체의 흡착 거동을 분석하였다. ATR용 crystal은 Ge crystal을 사용했으며, 온도를 각각 30, 40, $50^{\circ}C$에서 CpZr 전구체의 흡착특성을 연구했다. 흡착성을 증가시키기 위해 Ge crystal 표면에 $ZrO_2$나노입자를 분포시켜 흡착특성을 비교 분석하였다. 또한 CpZr 전구체가 흡착된 Ge crystal 표면에 오존가스를 주입시킨 후 변화를 관찰하였다. Ge crystal표면에 나노입자를 분포시켜 CpZr 전구체를 흡착한 결과 나노입자를 분포시키지 않았을 때 보다 흡착강도가 높게 나타났다. 또한 CpZr 전구체가 흡착된 Ge crystal 표면에 오존가스를 주입한 결과 C-H 결합이 분해됨을 확인했다.

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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 $0.675\sim1.970{\mu}g/kg$.

A Comparative Study on the Compositions of Hwangryeonhaedok-tang's Essential Oils Obtained by Supercritical Carbon Dioxide Extraction and Hydrodistillation Methods

  • Chang, Myeong-Jun;Lee, Sang-Ryong
    • Korean Journal of Acupuncture
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    • v.26 no.4
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    • pp.211-223
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    • 2009
  • 초임계추출법과 수증기증류법을 이용하여 황련해독탕의 정유성분을 추출하여 성분 패턴을 비교하였다. 이때 초임 계추출조건은 압력 200 atm, $45^{\circ}C$ 그리고 추출시간 25분 이었다. 이때의 추출된 성분의 93.9%인 37개의 성분을 가스크로마토그래피/질량분석기로 확인하였다. 주요성분으로는 tetradecenoic acid (11.7%), Vanillin (5.9%), dl-Limonene (5.5%) 및 Eicosane (4.6%)으로 나타났다. 수증기증류법으로 추출한 정유에서는 34개 성분을 확인할수 있었다. 주요성분으로는 tetradecenoic acid (8.9%), Vanillin (5.8%)및 Eicosane (4.7%)를 확인 할 수 있었다. 또한 구강내의 12균주를 이용하여 항균효과를 측정하여 최소엑제농도(MIC)와 사멸농도(MBC) 0.025 - 12.8 mg/ml와 0.05 - 12.8 mg/ml 각각 나타났다.

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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.

First GC-IRMS in Korea and Its Application Fields (국내 최초로 도입된 GC-IRMS와 응용분야 소개)

  • Shin, Woo-Jin;Lee, Kwang-Sik;Ko, Kyung-Seok
    • Economic and Environmental Geology
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    • v.40 no.5
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    • pp.699-703
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    • 2007
  • Compound-specific isotope analysis (CSIA) by isotope ratio mass spectrometer (IRMS) interfaced with gas chromatography (GC) is a state of the art analytical technique for stable isotopes in earth sciences, environmental sciences and forensics. Since early 1990s, GC-IRMS has been widely used to investigate the authenticity of food in forensic science and to trace the sources of organic contaminants in environmental science. In Korea, a GC-IRMS was firstly installed at the Korea Basic Science Institute (KBSI) in early 2005. In this study, we introduce the GC-IRMS of the KBSI shortly to stimulate various isotope-related researches of Korea, and report preliminary CSIA results for BTEX of different manufacturers.

The Study on the Thermal Isomerization of Pinane (PINANE의 열 이성화 반응에 관한 연구)

  • Lee, Jung-Bock;Kim, Chang-Bae
    • Analytical Science and Technology
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    • v.5 no.4
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    • pp.373-379
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    • 1992
  • The pyrolysis conditions for the thermal isomerization products of pinane were carried out by the furnace type pyrolyzer and the curie-point pyrolyzer equipped with gas chromatograph and mass spectrometer. It was confirmed that curie-point type is much better furnace type, and high yield (70%) of citronellene was obtained from pinane as the main isomerization product under the best conditions by curie-point type. The optimum conditions of pyrolysis are $590^{\circ}C$ for 4 sec. and the major products were indentified as citronellene, m-Menth-6-ene, m-Menth-1-ene and 1-Methyl-4-(1-methylethylidiene) cyclohexane.

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Analysis of adhesive material for joining pottery fragments excavated from Duurlig Nars, Mongolia (몽골 도르릭나르스 유적 토기의 접합에 사용한 물질 분석)

  • Yun, Eunyoung;Kang, Hyungtae
    • Journal of Conservation Science
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    • v.30 no.1
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    • pp.33-38
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    • 2014
  • The adhesive material was found for joining pottery fragments from Duurlig Nars, Mongolia estimated in AD 1C. In this study, analysis of natural substance for joining fragments of pottery was performed using gas chromatograph and mass spectrometer. As a result, it was identified triterpenoid substances, such as lupeol and betulin which were known to constituents of birch bark tar. It was suggested that Mongolian used adhesives made by birch bark tar for joining pottery fragments. Therefore if organic materials of ancient objects are systematically researched, it can provide significant evidence related to the way of life of ancient people.

Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography (어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Kim, Jong Won;Lee, Seok Ki
    • Analytical Science and Technology
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    • v.31 no.1
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    • pp.23-30
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    • 2018
  • Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

Simultaneous Determination of Amphetamine-Type Stimulants (ATS) in Human Hair by GC-MS (가스크로마토그래피-질량분석기를 이용한 모발에서 암페타민형 각성제 약물의 동시 분석)

  • 김진영;서승일;고범준;이재일;정재철;서용준;인문교
    • YAKHAK HOEJI
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    • v.47 no.3
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    • pp.142-147
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    • 2003
  • Gas chromatography-mass spectrometric (GC-MS) procedure is presented for the simultaneous qualification and quantitation of methamphetamine (MA), amphetamine (AMP), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), and 3,4-methylenedioxyethylamphetamine (MDEA) in human hair. The method procedure involves decontamination of hair with distilled water and acetone, acidic hydrolysis, extraction in the presence of deuterated internal standards, and GC-MS analysis after derivatization with trifluoroacetic anhydride (TFAA) in ethylacetate. The limit of detection for 5 drugs were about 0.1∼0.15 ng/mg using 30 mg hair sample. Coefficient variations of correlation ranged from 0.9941 to 0.9993. The recoveries of these drugs were found to be 93.4∼104.4%. The concentrations of AMP, MA, MDA, and MDMA in abusers' hair samples were measured 0.17∼2.88, 2.09∼18.34, 0.24∼3.83, and 3.10∼22.81 ng/mg, respectively. The ratios of MA/AMP and MDMA/MDA ranged 5.67∼49.57 and 4.78∼54.31, respectively. This assay has been successfully utilized in the evaluation of the deposition of amphetamine-type stimulants (ATS) in human hair.