• Title/Summary/Keyword: Carbon 13 NMR

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Two different reaction mechanisms of cinnamate side groups attached to the various polymer backbones

  • Hah, Hyun-Dae;Sung, Shi-Joon;Cho, Ki-Yun;Jeong, Yong-Cheol;Park, Jung-Ki
    • 한국정보디스플레이학회:학술대회논문집
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    • 2006.08a
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    • pp.772-775
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    • 2006
  • Cinnamate polymers are well known photoreactive polymers due to [2+2] cycloaddition reaction of cinnamate side group. In this work, we have found that the cinnamate side groups could be also reacted by thermal energy, and this reaction is presumed to attribute to the radical reaction of carbon double bond in the cinnamate groups. Contrary to the photocycloaddition reaction of the cinnamate side groups, the thermal reaction of cinnamate side group was closely related to the flexibility of polymer backbone. The difference of the mechanism between the photocycloaddition reaction and thermal crosslinking reaction was confirmed by $^1H-NMR$$ and $^{13}C-NMR$ analysis of the model compound.

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Purification and Properties of Non-Cariogenicity Sugar Produced by Alkalophilic Bacillus sp. S-1013

  • Ryu, Il-Hwan;Kim, Sun-Sook;Lee, Kap-Sang
    • Journal of Microbiology and Biotechnology
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    • v.14 no.4
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    • pp.751-758
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    • 2004
  • The NCS(Non-Cariogenicity Sugar) from Bacillus sp. S-1013 was purified by cold acetone and methanol precipitation, and DEAE-cellulose ion-exchange and Sephadex G-100 column chromatographies, to yield an amorphous yellow syrup. The melting point and $[\alpha]_D^{20}$ were 155-$157^{\circ}C$ and +53, respectively. Instrumental analyses such as FT-IR, $^1H-NMR, and ^{13}C-NMR$ showed that the NCS contained an O-H group, C-H, C=O, $NH_2$, anomeric carbon, anomeric proton, N-acetylgalactose, fucose, and neuramic acid, thus, the NCS was determined to be a trisaccharide of Fuc($1\longrightarrow4$)GalNAc($2\longrightarrow6$) NeuAc.

An isolation of the active component of Carthamus tinctorius L. Semen and the evaluation of its hepato-protective effect

  • Jeong, Jeong-Suk;Jeong, Choon-Sik;Jung, Ki-Hwa
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1998.11a
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    • pp.179-179
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    • 1998
  • We previously reported the hepato-protective effect of butanol soluble fraction of methanolic extract of Carthamus tinctorius L. Semen on carbon tetrachloride induced hepatotoxicity. In this study, the active component from the butanol soluble fraction was isolated by column chromatographic separation using Silica gel and Sephadex LH -20 and identified by spectroscopic methods such as Mass, $^1$H - NMR and $\^$13/C-NMR. The hepato-protective effect of the isolated active component on the CCl$_4$-induced liver damaged rats has been evaluated by performing blood chemical analysis and biotransformational enzyme analysis.

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Production of Useful Chemicals from Sunflower Oil by Microorganisms

  • El-Sharkawy, Saleh Hassan
    • Natural Product Sciences
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    • v.1 no.1
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    • pp.10-16
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    • 1995
  • A number of microorganisms have been screened for growth on sunflower oil as a sale carbon source for production of useful chemicals. Rhizopus stolonifer NRRL 1478 was found to transform the lipid contents of sunflower oil into dodecyl ${\beta}$-D-glucopyranoside and dodecanedioic acid in 15 and 25% yield respectively. The produced compounds were isolated and purified by column chromatography and its chemical identity were established using MS, IR, $^1H\;and\;^{13}C\;NMR$ spectroscopy.

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Synthesis and Characterization of A Carbosilane Dendrimer Containing Allylic End Groups

  • 김정균;박은미;강은주
    • Bulletin of the Korean Chemical Society
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    • v.17 no.7
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    • pp.592-595
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    • 1996
  • A silane dendrimer with 48 allylic end groups has been synthesized in excellent yield, via repetitive alkenylation-hydrosilation cycles. Starting with hexaallylethylenedisilane ((CH2=CHCH2)3SiCH2)2 as the core molecule (G0), a succession of alternate platinum catalyzed hydrosilation (Pt/C, 10% platinum content on active carbon) of all allyl groups with methyldichlorosilane and the allylation of all SiCl2 groups with allylmagnesium bromide in THF provided 3rd generation (G3) as carbosilane dendrimer. All the generations of dendrimer have been characterized by 1H and 13C NMR spectroscopy as well as elemental analysis.

A Study on the Chemical Composition and Structure of Sludge, Compost and Charcoal (폐수처리 슬럿지와 퇴비 및 목탄의 화학적 특성과 구조에 관한 연구)

  • 임기표;위승곤
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.35 no.1
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    • pp.27-32
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    • 2003
  • To understand the chemical structure of sewer sludge in comparison with commercial compost and charcoal used as a soil improver, it was carried out to analyse their ash contents and metal ions, and to elucidate the chemical structure of their residuals after a sequential treatment of alcohol-benzene(1:2) extraction in Soxhlet, 3% HCl reflux and 79% H₂SO₄ hydrolysis, using CHNS analyzer and solid C-13 NMR spectrometer. The results obtained were as follows: 1. Ash content of sludge was about 46% that is higher than those of compost (17%) and charcoal (4%). 2. The residual of sludge after a sequential treatment of HCl and H₂SO₄ hydrolyses had high ash content about 23%, too. 3. The sludge seems to be suitable to the soil improver because the content of heavy metal ions in sludge was near the compost and below the organic fertilizer standard. 4. Elemental composition of sludge residual after HCl-H₂SO₄ hydrolyes was C/sub 56/H/sub 91/O/sub 12/N₂S = (C/sub 6/H/sub 10/O/sub 5/)/sub 7/(C/sub 6/H₄)/sub 7/C₂H/sub 43/O₂N₂S, similar to C/sub 103/H/sub 122/O/sub 33/N/sub 6/S = (C/sub 6/H/sub 10/O/sub 5/)/sub 6/(C/sub 6/H₄)/sub 10/C/sub 7/H/sub 22/O₃N/sub 6/S of compost. 5. The sludge residual had proved to have both considerable aliphatic and aromatic groups, but the compost residual to have mainly aliphatic groups and the charcoal to have mainly aromatic groups, through the peak analysis of solid C-13 NMR charts. 6. So, the sewer sludge is proved to have a considerable amount of aromaticity like in woody biomass containing lignin.

Studies on the Fatty Acid Distribution in the Position of Triacylglycerols from the Seed of Pinus Koraiensis by Stereo-specific Analysis and $^{13}C-NMR$ Techniques (입본특이적(立本特異的) 방법(方法)과 $^{13}C-NMR$ 기법(技法)에 의한 잣기름의 트리아실 글리세롤의 구성지방산(構成脂肪酸)의 분포(分布)에 관한 연구(硏究))

  • Woo, Hyo-Kyeng;Kim, Seung-Jin;Joh, Yong-Goe
    • Journal of the Korean Applied Science and Technology
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    • v.15 no.4
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    • pp.35-44
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    • 1998
  • All the triacylglycerols including the molecular species having ${\Delta}^5$-unsaturated fatty acids from the seeds of Pinus Koraiensis, were split into a mixture of diacylglycerols by a Grignard reagent prepared with allyl bromide without arousing acyl chains of a glycerol moiety to migration, and were also easily partially hydrolyzed to diacylglycerols by pancreatic lipase. (S)-(+)-(1-naphthyl)ethyl urethane(NEU) derivatives of the diacylglycerol mixture derived from the triacylglycerols were fractionated into sn-1, 3-, sn-1, 2- and sn-2, 3-DG-NEU by silica-HPLC and the fatty acid composition of these fractions was analysed. $C_{18:1{\omega}9}$ is distributed evenly in the three positions of TG with $C_{18:2{\omega}6}$ mainly located in sn-2 position, while ${\Delta}^5$-unsaturated fatty acids such as ${\Delta}^{5.9}-C_{18:2}$, ${\Delta}^{5.9.12}-C_{18:3}$ and ${\Delta}^{5.11.14}-C_{20:3}$ are exclusively present in the sn-3 position. These results could be confirmed by $^{13}C$-NMR spectroscopy : the signals at $^{\delta}$173.231 ppm and $^{\delta}$172.811 ppm of the carbonyl carbon of acyl moieties indicate the presence of saturated acids and/or $C_{18:1{\omega}9}$ (oleic acid) in the ${\alpha}({\alpha}')$- or ${\beta}$- positions, and $C_{18:2{\omega}6}$ including $C_{18:1{\omega}9}$ in the ${\beta}$-position, respectively. In addition, the resonance at $^{\delta}$173.044 ppm suggested a location of ${\Delta}^5$-unsaturated fatty acid moiety in the ${\alpha}({\alpha}')$-position.

Carbon-13 Nuclear Magnetic Resonance Spectroscopic Studies of $^{13}CO$ Adsorbed on Platinum Particles in L-Zeolites

  • 한옥희;Gustavo Larsen;Gary L. Haller;Kurt W. Zilm
    • Bulletin of the Korean Chemical Society
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    • v.19 no.9
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    • pp.934-942
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    • 1998
  • $^13CO$ chemisorbed on platinum particles in L-zeolite has been investigated by static and magic angle spinning NMR spectroscopy. The representative spectra are composed of a broad asymmetric peak with a center of gravity at 230±30 ppm and a sharp symmetric peak at 124±2 ppm which is tentatively assigned to physisorbed $CO_2$, on inner walls of L-zeolite. Overall, the broad resonance component is similar to our previous results of highly dispersed (80-96%) CO/Pt/silica or CO/Pt/alumina samples, still showing metallic characters. The principal difference is in the first moment value. The broad peak in the spectra is assigned to CO linearly bound to Pt particles in the L-zeolites, and indicates a distribution of isotropic shifts from bonding site to bonding site. The NMR results reported here manifest that the Pt particles inside of the L-zeolites channels are not collectively the same with the ones supported on silica or alumina with similar dispersion in terms of Pt particle shape and/or ordering of Pt atoms in a particle. As a result, Pt particles of CO/Pt/L-zeolite were agglomerated accompanying CO desorption upon annealing. There were no definite changes in the NMR spectra due to differences of exchanged cations. Comparison of our observation on CO/Pt/L-zeolite with Sharma et al.'s reveals that even when the first moment, the linewidtb, and the relaxation times of the static spectra and the dispersion measured by chemisorption are similar, the properties of Pt particles can be dramatically different. Therefore, it is essential to take advantage of the strengths of several techniques together in order to interpret data reliably, especially for the highly dispersed samples.

Microscopic analysis of gas hydrates using X-ray diffraction method (X-ray diffraction을 이용한 가스 하이드레이트 미세구조 분석)

  • Lee, Jong-Won;Seol, Ji-Woong;Koh, Dong-Yeun;Lee, Huen
    • 한국신재생에너지학회:학술대회논문집
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    • 2008.10a
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    • pp.178-181
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    • 2008
  • 다양한 조성을 갖는 $CH_4+CO_2$ 혼합 기체 하이드레이트 샘플의 미세 구조 분석을 위하여 X-ray 회절 방법을 이용하였다. X-ray 회절 분석을 이용할 경우, 하이드레이트로의 전환율과 같은 정성적인 분석뿐 아니라 각 객체별 cage occupancy와 같은 정량적인 분석까지도 가능한 것으로 나타났다. 또한 이렇게 얻어진 X-ray 회절 분석 결과 및 refinement 결과를 $^{13}C$ 고체 NMR 방법과 교차 비교함으로써 측정 결과의 신뢰도를 높이려 하였다. 얻어진 분석 결과는 이후 가스 하이드레이트를 이용한 다양한 연구 분야에서 저장용량 평가 및 객체 점유율과 같은 미세 구조 정보를 얻는 데에 유용하게 사용될 것으로 전망된다.

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Solid State NMR Study of PAZO-6 and Related Materials

  • Han, Oc Hee;Jin, Jung-Il;Kim, Jong-Sung;Yoon, Yong-Kook;Huh, Sung-Mu
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.493-498
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    • 1995
  • PAZO-6 is a new combined type liquid crystalline polymers (LCP) which has two types of mesogens combined non linearly. Ordering of branch mesogen azo group, in PAZO-6 is an important parameter to observe as well as the substitution effect on the backbone. The related small molecules sllch as monomers as well as the polymer itself are studied by solid state NMR techniques. Preliminary $^{13}C$ CP/MAS (cross polarization/ magic angle spinning) spectral results suggest that the azo groups in the monomers are not aligned with themselves. Azo groups in the monomers seem to be poorly ordered between well ordered p-phenylene terephthalate moeities. Similar disordering tendency of the azo group in PAZO-6 is deduced from the overall aromatic carbon peak positions which are not much different from those of the monomer.

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