• Title/Summary/Keyword: $^{13}C-NMR$ 분석

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Hydrolysis Stability of Sulfonated Phthalic and Naphthalenic Polyimide with Ester Bond (에스테르기를 도입한 술폰화 프탈계 폴리이미드와 나프탈렌계 폴리이미드의 수화안정성에 관한 연구)

  • 이영무;이창현;손준용;박호범
    • Membrane Journal
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    • v.13 no.2
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    • pp.110-117
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    • 2003
  • Sulfonated polyimides had been utilized and studied widely as available materials in chloro-alkali electrolysis, cationic exchange resins, and so on. However, a slow decrease in performance during experiments had been reported, which could be attributed to a loss of ionic conductivity related to either a continuous dehydration or polymer degradation. One of main reasons to account for the degradation of sulfonated polymers is the hydrolysis leading to polymer chain scission and decrement of molecular weight. Therefore, the objective of our study was to investigate possible imide cycle and additional ester bond cleavage connected with $SO_3$H presence under hydrated condition. In order to confirm and obtain as clear information as possible about breakages of bonds via $^1H\; and \;^{13}C$ NMR and IR spectroscopic analyses, our study was performed by model compound. Consequently, model compounds with both phthalic and naphthalenic imide ring and ester bonds were synthesized to evaluate the hydrolysis stability of sulfonated polyimide. The experiments were performed for prepared model compounds before and after aging in deionized water at $80^{\circ}C$ and were terminated by lyophilization technique. The aging products were finally analyzed by NMR and IR spectroscopy.

Separation and Identification of Antimicrobial Substances from Prunus mume extract (매실추출물로부터 항균물질의 분리 및 구조동정)

  • Park, Woo-Po;Lee, Seung-Cheol;Kim, Sung-Yong;Choi, Sung-Gil;Heo, Ho-Jin;Cho, Sung-Hwan
    • Food Science and Preservation
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    • v.15 no.6
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    • pp.878-883
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    • 2008
  • Prunus mume was extracted using various solvents including ethyl ether, ethyl acetate and n-butanol. The extracts were fractionated by column chromatography. Antimicrobial compounds (A, B and C) in fractions showing antimicrobial activity were purified by Sephadex LH 20 column chromatography, and identified by $^{1}H$- and $^{13}C$-NMR analysis as isoeugenol, nomilin and $\beta$-sitosterol, respectively.

Preparation and Characterization of BaTiO3 Powders and Thin films (티탄산바륨 분말과 박막의 제조 및 특성 연구)

  • Jung, Miewon;Son, Hyunjin;Lee, Jiyun;Kim, Hyunjung
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.173-179
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    • 2004
  • The $BaTiO_3$ powders and thin films were prepared by an alkoxide modified sol-gel process (polymerization-complex route) using ethylene glycol. The stable starting (Ba-Ti)-mixed metal organic sol was made by addition of acetylacetone. The $BaTiO_3$ powders, which had a particle size of 40~77 nm, were crystallized from an amorphous to a tetragonal phase on annealing at 700 and $1100^{\circ}C$ for 1 h. From FT-IR, solid-state $^{13}C$ CP/MAS NMR spectroscopy and X-ray diffractometry, the trace of the Ba-Ti-oxycarbonate phase first appeared at $400^{\circ}C$. Hydrolyzed sol was spin coated on a quartz wafer at 3500 rpm for 60 s and pyrolyzed at $1100^{\circ}C$ for 1 h. After heat treatment, the coated layer became dense and smooth.

Isolation and Purification of Berberine in Cortex Phellodendri by Centrifugal Partition Chromatography (Centrifugal Partition Chromatography에 의한 황백으로부터 Berberine의 분리 및 정제)

  • Kim, Jung-Bae;Bang, Byung-Ho
    • The Korean Journal of Food And Nutrition
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    • v.27 no.3
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    • pp.532-537
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    • 2014
  • Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections, and infections of the body surface. Many analytical methods have been used to study oriental herbal medicines, such as thin-layer chromatography, column liquid chromatography, and high performance liquid chromatography (HPLC). In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out in order to separate pure compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 mL/min in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. The $^1H$ NMR spectrum revealed that the resonances at ${\delta}$ 4.10 and 4.20 ppm corresponded to three protons ($-OCH_3$), whereas those at ${\delta}$ 6.10 ppm corresponded to two protons ($-OCH_2O-$). Further, two aromatic protons (H-11 and H-12) conveys a doublet-doublet pattern. The H-11 doublet and H-12 doublet appear at ${\delta}$ 7.98 and 8.11, respectively. The $^{13}C$ NMR. spectrum showed a tetrasubstituted with a methylenedioxy group at C2 and C3, and two methoxy groups at C9 and C10. The chemical structure of the berberine was identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

Synthesis of Some 2-Amino-5-Substituted-1,3,4-Oxadiazoles Through the Electrooxidation of Semicarbazone (세미카바존의 전기적 산화에 의한 2-Amino-5-Substituted-1,3,4-Oxadiazoles 합성)

  • Kumar, Sanjeev
    • Journal of the Korean Chemical Society
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    • v.53 no.2
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    • pp.159-165
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    • 2009
  • The synthesis of 2-amino-5-substituted-1,3,4-oxadiazoles 4 were carried out from the electrooxidation of semicarbazone 3 at the platinum electrode under controlled potential electrolysis in an undivided cell. This is an environmentally benign method in the field of synthetic organic chemistry. The non-aqueous solvents acetic acid and acetonitrile and a supporting electrolyte lithium perchlorate were used for the electrolysis in the electrooxidation. The products were structurally charecterised by IR, $^1H$-NMR, $^{13}C$-NMR and elemental analysis.

Component Analysis of Liguefied Lignins (액화리그닌의 성분분석)

  • 황병호;조국란;공영토;도금현
    • Journal of Korea Foresty Energy
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    • v.18 no.1
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    • pp.17-24
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    • 1999
  • This study was conducted to examine the change in the structure of the lignin during liquefaction of kraft pulp lignin in Pinus korainsis and lignin sulfonic acid. The lignin liquefied compounds were extracted with chloroform from aqueous, liquefied lignins. Through the examination by IR, H($^{13}$C) - NMR and GC-MS spectrometers, phenolic compounds such as diguaiacol, acetic acid phenyl ester, phenol, 1-phenyl ethanone were identified with many of unknown phenolic compounds.

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Structural Elucidation and Magnetical Properties of La0.5Ca0.5MnO3 Powders and Pellets (La0.5Ca0.5MnO3 분말과 Pellet의 구조분석 및 자기적 성질)

  • Jung, Miewon;Lee, Jiyun;Kim, Hyunjung
    • Korean Chemical Engineering Research
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    • v.43 no.1
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    • pp.71-75
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    • 2005
  • $La_{0.5}Ca_{0.5}MnO_3$ colossal magnetoresistance (CMR) powders and pellets were synthesized by sol-gel process. The structural changes were investigated by FT-IR, CP/MAS $^{13}C$ solid state NMR spectroscopy and XRD. The particle characterization, microstructure of sintered samples, and cation composition of gel powders were studied by FE-SEM/EDS, TEM and ICP-AES. The structure refinement reveals that $La_{0.5}Ca_{0.5}MnO_3$ has orthorhombic, perovskite type unit cell. The magnetic characterizations were identified through measurement of magnetic moment by VSM.

Studies on coexistence phenomena of structure I and H hydrates (구조-I 및 구조-H 하이드레이트의 공존 현상 규명 연구)

  • Seo, Yu-Taek;Lee, Jong-Won;Seo, Young-Won;Lee, Huen
    • 한국신재생에너지학회:학술대회논문집
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    • 2007.11a
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    • pp.573-576
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    • 2007
  • 가스 하이드레이트의 구조-I 및 구조-H의 공존 현상을 13C NMR과 Raman spectroscopy를 이용하여 분석하였다. 하이드레이트 생성 조건이 구조-H 영역에만 있을 때는 CH4+neohexane 혼합 하이드레이트가 구조-H만을 나타냈지만, 구조-I의 영역에서는 구조-H의 혼합 하이드레이트와 구조-I의 순수 메탄 하이드레이트가 공존하는 것을 $^{13}C$ NMR spectra를 통해 확인하였다. 이러한 현상은 구조-H 생성자로 알려진 isopentane, MCP, MCH 에서도 관찰되었으며, Raman spectroscopy를 이용해서도 확인할 수 있었다.

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Isolation and Characterization of Cinnamic Acid with Antimicrobial Activity from Needle of Pinus densiflora (솔잎에서 항미생물 활성을 갖는 Cinnamic Acid 의 분리 및 동정)

  • Kuk, Ju-Hee;Ma, Seung-Jin;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
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    • v.29 no.4
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    • pp.823-826
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    • 1997
  • The EtOAc extracts from needles of Pinus densiflora showed antimicrobial activities against bacteria, yeast and fungi. The antimicrobial principle was successively purified by solvent fractionation, silica gel adsorption column chromatography and Sephadex LH-20 column chromatography. The active substance was further purified by HPLC using $C_{18}$ column. The active substance was identified as trans-cinnamic acid by MS, $^{1}H-NMR\;and\;^{13}C-NMR$. The amount of cinnamic acid was $9.27\;{\mu}g$ Per gram of fresh needle of Pinus densiflora.

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Isolation and Identification of Antimicrobial Compound from Dansam (Saliuia miltiorrhiza Bunge) (단삼으로부터 식품부패미생물에 대한 항균성 물질의 분리 및 동정)

  • 최해연;한영실
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.1
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    • pp.22-28
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    • 2003
  • Antimicrobial effect of Dansham (Saliuia miltiorrhiza Bunge) was investigated. Methanol extract of dried Dansham was fractionated to hexane, chloroform, ethylacetate, butanol and aqueous fraction. Chloroform fraction showed the highest inhibitory effect on the microorganisms such as B. subtilis, S. aureus, E. coli, L. monocytogenes and V. parahaemolyticus at 250 $\mu\textrm{g}$/disc. Chloroform fraction was further fractionated by silica gel column and thin layer chromatography (TLC). The antimicrobial compound was isolated from their fractions and its chemical structure was identified as a cryptotanshinone by GC-MS and $^1$H-NMR, $^{13}$ C-NMR.