• 제목/요약/키워드: $^{13}C-NMR$ 분석

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Phase Equilibria of Gas Hydrates Containing 1-propanol or 2-propanol (1-propanol 또는 2-propanol을 포함하는 가스 하이드레이트의 상평형)

  • Lee, Youngjun;Lee, Seungmin;Park, Sungmin;Seo, Yongwon
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.05a
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    • pp.145.1-145.1
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    • 2011
  • 본 연구에서는 알콜계 물질인 1-propanol과 2-propanol이 가스 하이드레이트 형성과정에서 격자내로 포집됨과 열역학적 촉진제로서 작용함을 알아보기 위해 $CH_4$ (또는 $CO_2$) + 1-propanol (또는 2-propanol) + 물계의 가스 하이드레이트 3상 평형 (하이드레이트(H) - 물(Lw) - 기상(V))을 측정하였으며, $^{13}C$ NMR 분석을 하였다. 1.0, 5.6, 10 mol%의 농도 1-propanol (또는 2-propanol) 용액을 가스 하이드레이트 계에 첨가하여 3상 평형을 측정한 결과, $CH_4$ 하이드레이트의 경우 전반적으로 촉진현상을 보였으며 5.6 mol%에서 가장 큰 촉진효과가 나타났다. 하지만 $CO_2$ 하이드레이트의 경우 순수 $CO_2$ 하이드레이트에 비해 저해효과가 나타났으며 농도가 높아질수록 저해현상은 커짐을 확인할 수 있었다. $^{13}C$ NMR을 통한 동공점유 특성과 하이드레이트 구조 분석 결과 $CH_4$ + 1-propanol (또는 2-propanol)은 구조-II를 형성하며 1-propanol (또는 2-propanol)이 동공에 포집되어 있음을 확인할 수 있었다. 이상의 결과로부터 알콜계 물질이 단순히 저해제로만 작용하지 않고 가스 하이드레이트 형성에 참여하는 촉진제로 작용할 수 있다는 사실을 알 수 있었다.

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Metal-Dinitrosyl Complexes(Ⅳ) : Synthesis and Characterization of Symmetric and Asymmetric Dinuclear Molybdenum and Tungsten Complexes (금속-디니트로실 착물 (제 4 보) : 몰리브덴과 텅스텐의 대칭 및 비대칭 이핵 착물의 합성과 특성)

  • O, Sang O;Mo, Seong Jong
    • Journal of the Korean Chemical Society
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    • v.38 no.7
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    • pp.485-495
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    • 1994
  • Several new symmetric and asymmetric homo and hetero dinuclear complexes of the type $[Cl(dppp)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$ and $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$(M,M'= Mo or W; phen = 1,10-phenanthroline; dppp = 1,3-bis(diphenylphosphino)propane; pyz = 1,4-pyrazine) were synthesized in three-steps starting from $[M(NO)_2Cl_2]_n(M = Mo, W)$. The final products were purified by eluting it through silica gel column ($2{\times}20$ cm) with acetone as the eluent. Characterization of these complexes and some related complexes was accomplished through UV-vis., $^1H$-NMR, $^{13}C$-NMR and IR spectroscopies as well as elemental analysis. The infrared spectra indicate that the NO groups occupy cis-positions of the octahedral. The $^1H$ and $^{13}C-NMR$ data for the new compounds revealed a dimeric structures with bridged pyz.

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Purification and Characterization of an Antifungal Antibiotic from Bacillus subtilis LAM 97-44 (Bacillus subtilis LAM 97-44가 생산하는 항진균성 항생물질의 정제 및 특성)

  • Lee, No-Woon;Kwon, Tae-Jong;Yi, Dong-Heui
    • Applied Biological Chemistry
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    • v.46 no.2
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    • pp.69-73
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    • 2003
  • A novel antifungal antibiotic for azole-resistant Candida albicans was purified from the culture broth of Bacillus subtilis LAM 97-44 by butanol extraction, Diaion HP-20 and Dowex-50 adsorption chromatography, silica gel flash chromatography followed by HPLC and designated LAM-44A. LAM-44A was stable for 60 min at $100^{\circ}C$, and pH range from 2 to 10. MIC values were observed at $0.5-3.5\;{\mu}g/ml$ against various Candida albicans strains. The antibiotic showed no cytotoxicity for S180, MKN-45, P388, HeLa and 373 at the concentration of 1 mg/ml. LAM-f4A was colorless powder soluble in water, methanol, ethanol, butanol and negative to ninhydrin reaction. The antibiotic had maximum absorption at 273 nm in methanol, and melting point was $202^{\circ}C$. The molecular weight and formula were determined to be 282 and $C_{14}H_{34}O_5$ by $^1H-NMR,\;^{13}C-NMR$, IR spectrum and elemental analysis.

Anionic Synthesis of Dipyridine Chain End-Functionalized Polystyrene and Polybutadiene (리빙 음이온 중합에 의한 Dipyridine 말단 관능화 폴리스티렌 및 폴리부타디엔의 합성)

  • Ji, Sang-Chul;Lee, Jong-Seop;Kim, Doo-Hwan;Kang, Cheol-Han;Park, Jong-Hyuk;Lee, Bum-Jae
    • Polymer(Korea)
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    • v.34 no.2
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    • pp.159-165
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    • 2010
  • Dipyridine-terminated polystyrenes and polybutadienes were synthesized by the chain endfunctionalization reaction of polystyryllithium (PSLi) and polybutadienyllithium (PBDLi) with di(2-pyridyl) ketone(DPK) using a living anionic polymerization method in the Ar-glove box. Living polymeric lithiums with low molecular weights (Mw=1000~2000 g/mol) were used to investigate the chain end-functionalization yield with DPK and the degree of coupling reaction by the attack of organolithium to the pyridine ring in the presence of TMEDA using GPC, $^1H$-NMR, $^{13}C$ analysis. DPK-terminated PBD exhibited much higher functionalization yield and less amount of coupling reaction compared with DPK-terminated PS. 86% functionalization yield with 9% degree of coupling was obtained when the PBDLi was added dropwise to DPK solution at room temperature. The functionalization yield was increased as the reaction temperature decreased, however, no LiCl effect was observed in this chain end-functionalization reaction with DPK.

A New Compound Isolation and Structure Analysis from Phellodendron Amurense Fruit Extract (황벽나무 열매 추출물로부터 신규 화합물의 분리 및 구조분석)

  • Kim, Young-Hee;Choi, Jung Eun;Hong, Jin-Young;Jo, Chang Wook;Lee, Jeung-Min;Kim, Soo Ji
    • Journal of the Korean Wood Science and Technology
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    • v.41 no.4
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    • pp.269-275
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    • 2013
  • Antifungal and insecticidal activity of Korean traditional medicinal plants was carried out to develop natural material for the development of organic cultural heritage conservation. As a result, Phellodendron amurense fruit was finally selected as a candidate of antifungal and insecticidal natural material. An novel active compound was purified from the ethylacetate fraction of Phellodendron amurense fruits using silica gel and Sephadex LH-20 column chromatography and PTLC. The compound was obtained as yellow oil form; UV ${\lambda}_{max}$(MeOH): 260 nm. The chemical structure of novel compound was determined as (4'-ethyl-2'-methylfuranyl)-6-methoxy-7-methylnona-2E,4E,6Z,8E-tetraenoic acid on the basis of various NMR experiments including $^1H$- and $^{13}C$-NMR, HMQC, HMBC and ESI-mass spectrum.

Sorption of PAHs by Soil Humins and Effect of Soil Inorganic Matrixs (PAHs의 토양휴민과의 흡착특성 및 토양 무기물의 영향 해석)

  • Lim, Dong-Min;Lee, Seung-Sik;Shin, Hyun-Sang
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.12
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    • pp.1337-1346
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    • 2006
  • Soil humin is the insoluble fraction of humic materials and play an important roles in the irreversible sorption of hydrophobic organic contaminants onto soil particles. However, there have been limited knowledge about the sorption and chemical properties of humin due to the difficulties in its separation from the inorganic matrix(mainly clays and oxides). In this study, de-ashed soil humins($Hu_1-Hu_6$) were isolated from a soil residues(Crude Hu) after removing alkali-soluble organic fractions followed by consecutive dissolution of the mineral matrix with 2%-HF for 2 hr. The humin samples were characterized by elemental analysis and $^{13}C$ NMR spectroscopic method and their sorption-desorption behavior for 1-naphthol were investigated from aqueous solution. The results were compared one another and that with peat humin. $^{13}C$ NMR spectra features indicate that the soil humin molecules are mainly made up of aliphatic carbons(>80% in total carbon) including carbohydrate, methylene chain. Freundlich sorption parameter, n was increased from 0.538 to 0.697 and organic carbon-normalized sorption coefficient(log $K_{OC}$) values also increased from 2.43 to 2.74 as inorganic matrix of the soil humin removed by HF de-ashing. The results suggest that inorganic phase in humin plays an important, indirect role in 1-naphthol sorption and the effects on the sorption non-linearity and intensity are analyzed by comparison between the results of soil humin and peat humin. Sorption-desorption hysteresis were also observed in all the humin samples and hysteresis index(HI) at low solute concentration($C_e$=0.1 mg/L) are in order of Peat humin(2.67)>De-ashed humin(0.74)>Crude Hu(0.59).

해양 유래 Pseudomonas aeruginosa BYK-2(KCTC 18012P)가 생산하는 Biosurfactant의 구조분석

  • Lee, Gyeong-Mi;Kim, Hak-Ju;Ha, Sun-Deuk;Gang, Yang-Sun;Gong, Jae-Yeol
    • 한국생물공학회:학술대회논문집
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    • 2000.11a
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    • pp.626-629
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    • 2000
  • The Pseudomonas aeruginosa BYK-2(KCTC 18012p) produced three kinds of glycolipids on olive oil as a substrate and purified two types of major glycolipids(Rf=0.48, BS-1; Rf=0.65, BS-2) using silica gel chromatography, TLC, HPLC, etc. From the analysis of the chemical structure, the glycolipid of BS-1 was estimated as rhamnolipid($2-O-{\alpha}-L-rhamnopyranosyl- {\alpha}-L-rhamnopyranosyl-{\beta}-hydroxyldecanoyl-{\beta}-hydroxydecanoic$ acid; M.W. 650) and BS-2 was detected as rhamnolipid methyl ester($2-O-{\alpha}-L-rhamnopyranosyl-{\alpha}-L-rhamnopyranosyl-{\beta}-hydroxyldecanoyl-{\beta}-hydroxydecanoic$ acid methyl ester; M.W. 664) by FT-IR, FAB Mass spectrometry, $^1H-NMR$, $^{13}C$ FT-NMR, DEPT, 2D-NMR (TOCSY, RELAY, NOESY, HSQC, HMBC). In particular, It was found that a marine bacterium Pseudomonas aeruginosa BYK-2(KCTC 18012P) remarkably produced rhamnolipid and rhamnolipid methyl ester simultaneously.

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Microscopic Analysis on New Water-soluble Hydrate Systems (새로운 수용성 하이드레이트 시스템에 대한 미세 분광학적 분석연구)

  • Lee, Jong-Won;Lu, Hailong;Moudrakovski, Igor L.;Ratcliffe, Christopher I.;Ripmeester, John A.
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.215.1-215.1
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    • 2010
  • 가스 하이드레이트는 작은 고체 부피 내에 막대한 양의 가스를 저장할 수 있다는 특성으로 인하여, 최근 천연가스 혹은 메탄의 저장 매체로 활용하기 위한 연구가 활발히 진행중에 있다. 하지만 실제 응용을 위해서는 미세구조 분석이 수행되어 하이드레이트 형태로 저장할 수 있는 정확한 저장 용량을 파악할 필요가 있다. 본 연구에서는 여러가지의 고리형 에테르, 고리형 에스테르 및 고리형 케톤 화합물들을 테스트하여 메탄 가스와 반응하는 6가지의 새로운 sII 혹은 sH 하이드레이트 형성제를 파악하였다. 또한 새로이 발견된 형성제 모두에 대하여 하이드레이트 상평형도 측정하였다. 얻어진 상평형 데이터는 하이드레이트 안정영역과 게스트 분자 크기 간에 뚜렷한 상관관계가 있음을 입증하였다. 아울러 형성된 하이드레이트 샘플은 고체 분말 X-선 회절과 고체상 13C NMR 분석을 수행하여 하이드레이트 구조와 게스트 포집률을 조사하였다. 마지막으로, 비슷한 화학 구조식을 갖고 있음에도 2-methyltetrahydrofuran과 3-methyltetrahydrofuran, 혹은 4-methyl-1,3-dioxane과 4-methyl-1,3-dioxolane은 서로 다른 하이드레이트 결정 구조를 보여 주었는데, 이러한 차이는 하이드레이트 결정 구조를 결정짓는 게스트 분자 크기, 즉 임계 게스트 분자 크기를 파악하는 데에도 매우 유용한 정보를 제공할 수 있을 것이라 판단된다.

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Synthesis, Characterization and Correlation Analysis in Styryl 6-Methoxy-2-Naphthyl Ketones (Styryl-6-Methoxy-2-Naphthyl Ketone 유도체의 합성 및 특성 분석)

  • Thirunarayanan, G.
    • Journal of the Korean Chemical Society
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    • v.51 no.2
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    • pp.115-124
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    • 2007
  • A series of α, β-unsaturated ketones are synthesized by Crossed - Aldol condensation reaction, from ecofriendly 6-methoxy-2-naphthyl ketones and substituted benzaldehydes under solvent free conditions using silica-sulfuric acid as a catalytic reagent. The yields of ketones are more than 90% and the catalyst was reusable for further run. There is no appreciable decrease in the yield of product and the activity of catalyst. These chalcones were characterized by their physical constants and spectral data (IR, 1H-, 13C-NMR and Mass). These spectral data are subjected to correlate various Hammett substituent constants with single and multiparameter correlation equations. From the results of statistical analysis the influence of electronic effects of substituents on the spectral data of the ketones were explained.

Synthesis and photoproperties of digold conjugated chain (공액계 사슬을 갖는 이 핵 금 착체의 합성과 광학적 특성에 관한 연구)

  • Kim, Dong-Hwan;Kim, Hwa-Sun;Ahn, Ho-Geun;Kwak, Ji-Hoon;Lee, Ji-Hoon;Jung, Min-Chung
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2006.06a
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    • pp.455-456
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    • 2006
  • 최근 많은 학자들에 의해서 차세대 디스플레이로 각광 받고 있는 유기EL에 대한 연구가 활발하게 진행되고 있다. 그 중에서 본 연구에서 수행하고자 하는 분야는 유기EL의 발광재료의 개발에 대한 연구이다. 그 분야중 하나가 세계적으로 많은 학자들에 의해서 연구되고 있는 전이금속을 이용한 발광재료의 개발이다. 그 중 본 연구에서는 양 말단 금속을 가교체로 연결한 이 핵 금 착체에 관한 연구를 수행하였다. 이러한 가교체들은 유기물의 결합 상태에서 나타나는 전자전이외에 금속과 유기물사이의 결합에 의해 나타날 수 있는 전자전이 또 한 가지고 있다. 이러한 전자전이로 인해 발광재료로서의 특징을 가질 수 있다. 이러한 착체를 합성하기위해 가교체 $H-C{\equiv}C-C{\equiv}C-C-H$$(Cis)H-C{\equiv}C-CH=CH-C{\equiv}C-H$를 이용하여 금과 N-Heterocyclic-Carbene가 배위결합된 양말단의 금속 그룹을 연결하여 합성하였다. 합성된 착체는 FT-IR, $^1H$-NMR, $^{13}C$-NMR, UV/VIS/NIRspectrophotometer, Emission spectrometer를 사용하여 분석하였다.

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