• Title/Summary/Keyword: NMR measurements

검색결과 157건 처리시간 0.02초

안트라센이 포함된 새로운 호스트 화합물의 합성과 물성 (Synthesis and Fluorescent Properties of New Host Compound Containing Anthracene Moiety)

  • 장승현
    • 한국환경과학회지
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    • 제17권12호
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    • pp.1373-1380
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    • 2008
  • Anthracene appended new host compounds have been synthesized by imine reaction. Fluorescent open chain host compounds Trisanthryl-tris(2-aminoethyl)imine 1 was synthesized from the reaction of tris(2-aminoethyl)amine and anthracene-9-carboxaldehyde in EtOH. Tris-10-chloroanthryl-tris(2-aminoethyl)imine 2 was synthesized from tris(2-aminoethyl)amine and 10-chloro-9-anthraldehyde in EtOH. The structures of all reaction product were identified by $^1H$ NMR, $^{13}C$ NMR, GC/MS, FAB Mass, IR spectrum and DSC. Cation complexation behavior was investigated by fluorescence spectroscopy measurements. The capability of transition metals cation recognition between fluorescent open chain host compound 1, 2 were investigated with $Co^{2+},\;Ni^{2+}\;and\;Cu^{2+}$. The fluorescence intensity was increased by host compounds corresponding guest cations. The relative order of fluorescence intensity changes were $Co^{2+}>Cu^{2+}>Ni^{2+}$. Compound 2 is very sensitive fluorescent sensor of $Co^{2+}$ ion.

환형 폴리옥시에틸렌 존재하의 피롤의 화학적 중합에 관한 연구 (Study on the Chemical Polymerization of Pyrrole in the Presence of Cyclic Poly(oxyethylene)s)

  • 차국찬;김진환;배진영
    • 폴리머
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    • 제26권5호
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    • pp.568-574
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    • 2002
  • 호스트 분자로서 환형 폴리옥시에틸렌을 사용한 inclusion 화합물을 이용하여 수용액상에서 피롤의 화학적 중합을 수행하였다. 이와 같은 합성 전략은 수용액상에서 화학적 산화방법에 의해 견고한 방향족 고분자의 사슬을 성장시킬 수 있는 가능성을 나타내며, 수용성 올리고 또는 폴리피롤을 손쉽게 얻을 수 있는 방법을 제시하고 있다. 본 연구에서는 부분적으로 고분자 주사슬에 환형 폴리옥시에틸렌을 함유한 수용성 폴리피롤을 얻었으며, NMR, IR, UV 및 MALDI-TOF MS 분석 등을 통하여 그 구조를 확인하였다.

195Pt NMR Study of the Influence of Nation Ionomer on the Enhanced Local Density of States at the Surface of Carbon-Supported pt Catalysts

  • Han, Kee-Sung;Lee, Moo-Hee
    • 한국자기공명학회논문지
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    • 제13권2호
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    • pp.135-142
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    • 2009
  • $^{195}Pt$ NMR measurements were performed to deduce the variation of local density of states at the Fermi energy ($E_F$-LDOS) at the surface of carbonsupported Pt catalysts due to the addition of $Nafion^{(R)}$ ionomer in the metalelectrode-assembly for fuel cells. The results showed that the EF-LDOS at the surface of Pt particles was enhanced by the addition of $Nafion^{(R)}$ ionomers whereas it was uninfluenced in the inner (bulk) part of the Pt particles. This suggests that the effects of ionomers on the electronic states of the Pt particle surface are related to the electrochemical activity of the catalysts.

Synthesis and Characterization of Bis(5,6-dihydro-1,4-dithiin-2,3-dithiolato)nickel(II), nickel(III) and of Related Dialkyl Nickel(III) Dithiolene Complexes

  • 김영진;최성낙;오영희
    • Bulletin of the Korean Chemical Society
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    • 제18권9호
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    • pp.1022-1028
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    • 1997
  • The reaction between Ni(Ⅱ) and sodium salt of 5,6-dihydro-1,4-dithiin-2,3-dithiolate (DDDT2-) in the presence of oxygen results in the formation of Ni(Ⅲ) species, Ni(DDDT)2-, which is isolated as tetraalkylammonium salt. The same reaction performed in the absence of oxygen yields dianionic Ni(Ⅱ) species, Ni(DDDT)22-, which is also isolated as the tetraethylammonium salt. The bis(5,6-dihydro-1,4-dithiin-2,3-dithiolato) nickelate (Ⅱ) dianion, Ni(DDDT)22-, reacts with methyl iodide to yield unusually stable bis(methylthio)dithiolene complex, Ni(CH3)2C8H8S8. All the isolated dithiolato-nickel(Ⅱ) and nickel(Ⅲ) complexes are characterized by 1H NMR, UV/Vis, IR and mass spectroscopic methods. The internal redox reaction of the nickel(Ⅱ)-dithiolate has been studied by spectro-electrochemical method and the results were compared with those of other metal-dithiolenes. The alkylated nickel(dithiolene) complex presumably undergoes cis-trans isomerization reaction in solution, judging from the experimental results of variable-temperature 1H NMR measurements.

코코넛 오일로부터 유래된 아미노산계 음이온 계면활성제의 합성 및 계면 특성 연구 (Synthesis of Amino Acid-based Anionic Surfactants from Coconut Oil and Characterization of Interfacial Properties)

  • 예다난;조선희;임종주
    • 공업화학
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    • 제29권5호
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    • pp.524-532
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    • 2018
  • 본 연구에서는 천연 유래의 코코넛 오일을 원료로 사용하여 2종류의 아미노산계 음이온 생체계면활성제 포타슘 코코일 글루타메이트(potassium cocoyl glutamate, CTK)와 소듐 코코일 글루타메이트(sodium cocoyl glutamate, CTN)를 합성하였으며, 합성한 계면활성제의 구조를 FT-IR, $^1H-NMR$$^{13}C-NMR$ 분석을 통하여 규명하였다. 합성한 계면활성제에 대하여 정적 및 동적 표면장력과 유화력 등의 계면 물성을 측정한 결과, CTK와 CTN 모두 계면 활성이 우수하고 계면 에너지를 낮추는데 효과적임을 알 수 있었다. 특히, CTK 계면활성제가 CTN 계면활성제와 비교하여 계면 에너지를 낮추는데 보다 효과적이었는데 이는 CTK가 소수성이 더 크고 계면활성제 단분자가 벌크 용액으로부터 공기와 수용액의 계면으로 이동하는 속도가 빨라서 공기와 수용액의 계면이 계면활성제 단분자에 의하여 더 짧은 시간에 포화되기 때문임을 알 수 있었으며, 생활용품이나 화장품 제조에 적용될 수 있을 것으로 기대된다.

[4.3.0] 환상 유사 우레아의 이성화 개환중합과 특성평가 (Characteristics of Ring-Opening Isomerization Polymerization of [4.3.0] Cyclic Pseudoureas)

  • 이찬우;정진도
    • 폴리머
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    • 제35권4호
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    • pp.308-313
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    • 2011
  • 5원환의 2,3,5,6-tetrahydroimidazo[2,1-b] [1,3] oxazole(TIO)와 비교하여 6원환인 2,5,6,7-tetrahydro-3H-imidazo[2,1-b] [1,3] oxazine(TII)가 중합반응성이 낮은 결점을 개선하고자 각종의 조건하에서 중합을 실시한 결과, 최적의 중합조건으로 methyl trifluoromethanesulfonate(MeOTf)을 개시제로 사용한, 극성이 높은 니트로벤젠 용매의 $60^{\circ}C$에서 24시간 반응시킴에 의해 고수율의 중합체를 얻었다. 생성된 중합체를 $^1H$ NMR과$^{13}C$ NMR, IR 스펙트럼으로 분석하였으며, GPC로부터 구한 분자량과 이론분자량이 거의 일치함도 확인하였으며, 융점($T_m$)은 알킬 그룹의 길이에 따라 큰 차이를 나타내었다.

Improved Purification of Thermophilic FoF1-ATP Synthase c-Subunit Rings and Solid-State NMR Characterization of Them in Different Lipid Membranes

  • Bak, Suyeon;Kang, Su-Jin;Suzuki, Toshiharu;Yoshida, Masasuke;Fujiwara, Toshimichi;Akutsu, Hideo
    • 한국자기공명학회논문지
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    • 제17권2호
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    • pp.67-75
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    • 2013
  • ATP synthase produces ATP, a major energy source for metabolic processes in organisms, from ADP and inorganic phosphate in cellular membranes. ATP synthase is known as a rotary motor, in which the c-subunit ring functions as a rotor. In this work, we have tried to develop a more general preparation procedure of thermophilic $F_oc$-ring ($TF_oc$-ring) for NMR measurements. The expression of $TF_oF_1$ is easily affected by various experimental conditions such as temperature, shape and size of a flask, a volume of medium, and shaking rate of an incubator. Accordingly, we have tried to optimize the expression conditions of $TF_oF_1$. $TF_oc$-rings were purified from $TF_oF_1$ according to a reported method. We modified purification procedures to improve purity and yield of $TF_oc$. On top of them, we found a new combination of detergents for the purification at anion-exchange column chromatography. To examine the effect of lipid environments on the structure, the $TF_oc$-rings were reconstituted into two kinds of lipid bilayers, namely, saturated and unsaturated lipid ones. Then, we have compared characteristics of the $TF_oc$-ring structures in these membranes with solid-state NMR.

코코넛 오일로부터 유래된 카르복실레이트계 음이온 계면활성제의 합성 및 계면 특성에 관한 연구 (Synthesis of Carboxylate-Based Anionic surfactant from Coconut Oil Source and Characterization of Interfacial Properties)

  • 이예진;박기호;신희동;임종주
    • 공업화학
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    • 제32권3호
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    • pp.260-267
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    • 2021
  • 본 연구에서는 코코넛 오일로부터 카르복실레이트계 음이온 계면활성제 SLEC-3을 합성하였으며, 합성된 계면활성제의 구조를 FT-IR, 1H-NMR 및 13C-NMR 분석을 통하여 확인하였다. 합성한 계면활성제 SLEC-3에 대하여 임계 마이셀 농도, 정적 및 동적 표면장력, 유화력, 거품 안정성 등의 계면 물성을 측정한 결과, 기존 세제 제품에서 널리 사용되는 음이온 계면활성제 SLES와 비교하여 계면 활성이 보다 우수하고 계면 에너지를 낮추는데 더 효과적이었다. 또한 SLCE-3에 대한 생분해성, 급성 경구 독성 및 급성 피부자극 시험을 실시한 결과, 저자극 및 저독성을 가지고 있기 때문에 세제 및 세정제 제품에 적용할 수 있을 것으로 판단되었다.

On-line Magnetic Resonance Quality Evaluation Sensor

  • Kim, Seong-Min;McCarthy, Michael J.;Chen, Pictiaw;Zion, Boaz
    • 한국농업기계학회:학술대회논문집
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    • 한국농업기계학회 1996년도 International Conference on Agricultural Machinery Engineering Proceedings
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    • pp.314-324
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    • 1996
  • A high speed NMR quality evaluation sensor was designed , constructed and tested . The device consists of an NMR spectrometer coupled to a conveyor system. The conveyor was run at speeds ranging from 0 to 250 mm/s. Spectral of avocado fruits and one-dimensional magnetic resonance images of pickled olives were acquired while the samples were moving on a conveyor belt mounted through a 20Tesla NMR magnet with a 20 mm diameter surface coil and a 150 mm diameter imaging coil respectively. Fro a magnetic resonance spectrum analysis, motion through variations in the magnetic field tends to narrow spectral line width just like using sample rotation in high resolution NMR to narrow spectral line width. Spectrum analysis was used to detect the dry weight of avocado fruits using the ratio oil and water resonance peaks. Good correlations maximum r=0.970@ 50 mm/s and minimum r=0.894@250mm/s ) between oil and water resonance peak ratio and dry weight of avocados were observed at speeds ra ging from0 to 250mm/s. For the application of magnetic resonance imaging (MRI) method, the projections were used to distinguish between pitted and non-pitted olives . Effect of fruit position in the coil was tested and coil degree effects were noticed when projects were generated under dynamic conditions. Various belt speeds (up to 250mm/s) were tested and detection results were compared to static measurements. Higher classification errors were occurred at dynamic conditions compared to errors while olives were at rest.

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Superconductivity in Fluorinated $YBa_2Cu_3O_{6+x}$

  • Lee, Cheol-Eui;D, White;P.K, Davies
    • Journal of Magnetics
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    • 제1권2호
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    • pp.57-59
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    • 1996
  • The YBa$_2$Cu$_3$O6+xstructures have been fluorinated by a gas phase exchange technique, and 19F NMR was used to identify the structural fluorine. Magnetic susceptibility measurements showed that the fluorination turned a marginally nonsuperconducting sample into a 40 K superconductor, as well as that it raised the onset of the superconducting transition of the 60 K superconductor YBa$_2$Cu$_3$O6.7 to about 100 K.

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