• Title/Summary/Keyword: Proton Nuclear Magnetic Resonance

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Structural and Chemical Characterization of Aquatic Humic Substances in Advanced Water Treatment Processes (고도정수처리 공정에서 수질계 휴믹물질의 구조 및 화학적 특성분석)

  • Kim, Hyun-Chul;Yu, Myong-Jin
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.3
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    • pp.240-246
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    • 2005
  • Humic substances HS) from process waters at advanced water treatment plant consisted of GAC and Ozone/GAC processes were isolated and extracted by physicochemical fractionation methods to investigate their characteristics. They are characterized for their functionality, chemical composition, spectroscopic characteristics using FT-IR and $^1H$-NMR spectroscopy. Humic fraction gradually decreased from 36.3% to 24.2% from 0.45 to 0.30 mgC/L) through ozonation and carbon adsorption. The humic fraction was isolated into the phenolic and carboxylic groups using A-21 resin, and the concentration of phenolic groups gradually decreased from 38.4% to 23.5% (from 4.9 to $3.2\;{\mu}M/L$ as phenolic-OH) through ozonation and carbon adsorption. In the case of carboxylic groups, the concentration decreased from 61.6% to 43.3% (from 7.8 to $5.8\;{\mu}M/L$ as COOH) through the water treatment processes. On the other hand, concentrations of those roups decreased from 38.4% to 24.0% and 61.6% to 44.9% through carbon adsorption without ozonation, respectively. The structural changes of HS identified from FT-IR and $^1H$-NMR were consistent with the results from the isolation of functional groups in HS.

Effect of Length of Alkyl Group on Thermal-Liquid Crystalline Properties of Cholesteryl 4-n-Alkoxybenzoate (알킬기의 길이가 콜레스테릴 4-n-알콕시벤조에이트의 열적-액정 특성에 미치는 영향)

  • Yoon, Doo-Soo;Bang, Moon-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.18 no.10
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    • pp.69-74
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    • 2017
  • In this study, cholesteryl 4-n-alkoxybenzoates (Chol-n), with alkyl groups used for controlling the temperature of transition to the liquid crystal phase, were synthesized, and the effects of the length of the alkyl groups on the physical properties of the liquid crystal compounds were investigated. The chemical structures and thermal and liquid crystalline properties of the synthesized compounds were investigated by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectroscopy ($^1H$-NMR), differential scanning calorimetry (DSC), and polarizing optical microscopy (POM). The synthesized compounds showed melting transition temperatures ($T_m$) in the range of $103^{\circ}C$ to $143^{\circ}C$ and all of the compounds except Chol-6 exhibited a wide liquid crystal phase temperature range of about $60^{\circ}C$ to $100^{\circ}C$. No correlation between the number of carbon atoms in the molecule and the thermal properties of the compounds was found. All of the synthesized compounds showed an enantiotropic cholesteric phase, which was accompanied by a chiral smectic phase in the compounds Chol-6, Chol-8, Chol-9, and Chol-10. All of the compounds exhibited thermochromism in the liquid crystal state, and their color changed from red to blue as the temperature was increased.

Contribution of a Low-Barrier Hydrogen Bond to Catalysis Is Not Significant in Ketosteroid Isomerase

  • Jang, Do Soo;Choi, Gildon;Cha, Hyung Jin;Shin, Sejeong;Hong, Bee Hak;Lee, Hyeong Ju;Lee, Hee Cheon;Choi, Kwan Yong
    • Molecules and Cells
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    • v.38 no.5
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    • pp.409-415
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    • 2015
  • Low-barrier hydrogen bonds (LBHBs) have been proposed to have important influences on the enormous reaction rate increases achieved by many enzymes. ${\Delta}^5$-3-ketosteroi isomerase (KSI) catalyzes the allylic isomerization of ${\Delta}^5$-3-ketosteroid to its conjugated ${\Delta}^4$-isomers at a rate that approache the diffusion limit. Tyr14, a catalytic residue of KSI, has been hypothesized to form an LBHB with the oxyanion of a dienolate steroid intermediate generated during the catalysis. The unusual chemical shift of a proton at 16.8 ppm in the nuclear magnetic resonance spectrum has been attributed to an LBHB between Tyr14 $O{\eta}$ and C3-O of equilenin an intermediate analogue, in the active site of D38N KSI. This shift in the spectrum was not observed in Y30F/Y55F/D38N and Y30F/Y55F/Y115F/D38N mutant KSIs when each mutant was complexed with equilenin, suggesting that Tyr14 could not form LBHB with the intermediate analogue in these mutant KSIs. The crystal structure of Y30F/Y55F/Y115F/D38N-equilenin complex revealed that the distance between Tyr14 $O{\eta}$ and C3-O of the bound steroi was within a direct hydrogen bond. The conversion of LBHB to an ordinary hydrogen bond in the mutant KSI reduced the binding affinity for the steroid inhibitors by a factor of 8.1-11. In addition, the absence of LBHB reduced the catalytic activity by only a factor of 1.7-2. These results suggest that the amount of stabilization energy of the reaction intermediate provided by LBHB is small compared with that provided by an ordinary hydrogen bond in KSI.

Spectroscopic Characterization and Seasonal Distribution of Aquatic Humic Substances Isolated from Han River Water (한강원수로부터 분리된 수중휴믹물질의 계절적 분포와 분광학적 특성분석)

  • Kim, Hyun-Chul;Lee, Seock-Heon;Kim, Kyung-Ju;Yu, Myong-Jin
    • Journal of Korean Society of Environmental Engineers
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    • v.29 no.5
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    • pp.540-547
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    • 2007
  • Humic substances(HS) from Han River water was physic-chemically isolated by fractionational methods to investigate the seasonal distribution and to characterize the properties compared with intrinsic humic materials. Various HS samples were analyzed by element, Fourier transform infrared(FT-IR), proton nuclear magnetic resonance$(^1H-NMR)$ and fluorescence analyzers. The portion of HS from Han River water(HRHS) was 47.0% on the average, however it appeared that rainfall event brought about higher fraction of HS in Han River water by the periodic investigation. Aromaticity and humification degree of the HRHS were relatively lower than those of intrinsic humic materials originated from decomposing vegetation. FT-IR, $^1H-NMR$ and fluorescence spectroscopy showed the distinct differences between HRHS and intrinsic humic materials. Commercial humic materials could not represent structural and functional characteristics of local HS. The fluorescence spectroscopy, a relatively simple measurement, was found most useful tool to estimate humification degree for humic materials from particular sources.

Isolation and Identification of Low Molecular Phenolic Antioxidants from Ethylacetate Layer of Korean Black Raspberry (Rubus coreanus Miquel) Wine (복분자(Rubus coreanus Miquel) 와인의 에틸아세테이트층으로부터 저분자 페놀성 항산화 화합물의 단리·동정)

  • Kim, Seong-Ja;Lee, Hyoung-Jae;Park, Keun-Hyung;Rhee, Chong-Ouk;Lim, Ik-Jae;Chung, Hee-Jong;Moon, Jae-Hak
    • Korean Journal of Food Science and Technology
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    • v.40 no.2
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    • pp.129-134
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    • 2008
  • Five antioxidative active substances were isolated from the EtOAc layer (20 g/56.2 g) of Korean black raspberry (Rubus coreanus Miquel) wine (11 L, black raspberry 15.7 kg fresh wt. eq.) by various column chromatography and high performance liquid chromatography (HPLC). Proton nuclear magnetic resonance ($^1H$-NMR) spectroscopy and gas chromatography Electro Ionization-Mass Spectrometry (GC-EI-MS) identified these as 4-hydroxybenzoic acid (1, 0.1 mg), 3,4-dihydroxybenzoic acid (2, 0.3 mg), 4-(2-hydroxyethyl)-phenol (3, 0.6 mg; tyrosol), pyrocatechol (4, 0.3 mg), 3,4,5-trihydroxybenzoic acid ethyl ester (5, 0.6 mg; ethyl gallate). The presence of 1 and 2 in Korean black raspberry has previously been reported. However, the presence of 3-5 in Korean black raspberry, and the identification of 1-5 from the Korean black raspberry wine have never before been reported.

Synthesis and Characterization of Polymers with Azobenzene and Hexamethylene Groups in Main Chain (주사슬에 아조벤젠기와 헥사메틸렌기를 갖는 고분자의 합성 및 특성)

  • Gu, Su-Jin;Lee, Eung-Jae;Bang, Moon-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.86-92
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    • 2019
  • Polymers with various compositions of azobenzene and hexamethylene groups in the main chain were synthesized by a Schotten-Baumann reaction and their properties were investigated. The chemical structures and physical properties of the synthesized polymers were investigated by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, thermogravimetric analysis, polarized optical microscopy, and x-ray diffraction. The polymers showed an inherent viscosity of 1.28-1.36 dl/g and were relatively insoluble in most organic solvents. The melt transition temperature increased rapidly with increasing number of azobenzene groups in the polymer. When the azobenzene monomer content was more than 50 mol%, no melting transition occurred below the decomposition temperature. Among the polymers with a melt transition temperature, the MP-A3C7 and MP-A5C5 polymers were liquid crystalline materials and exhibited a nematic phase with weak liquid crystallinity over a wide liquid crystal temperature range. This difference in the properties of the synthesized polymers is likely due to the changes in intermolecular forces resulting from the linearity and polarity of the trans-form of azobenzene.

The synthesis of dextran from rice hydrolysates using Gluconobacter oxydans KACC 19357 bioconversion (Gluconobacter oxydans 생물전환을 통한 쌀 가수분해물 유래 dextran 합성)

  • Seung-Min Baek;Hyun Ji Lee;Legesse Shiferaw Chewaka;Chan Soon Park;Bo-Ram Park
    • Food Science and Preservation
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    • v.31 no.1
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    • pp.149-160
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    • 2024
  • Dextran is a glucose homo-polysaccharide with a predominantly α-1,6 glycosidic linkage of microbial source and is known to be produced primarily by lactic acid bacteria. However, it can also be obtained through the dextran dextrinase of acetic acid bacteria (Gluconobacter oxydans). The dextrin-based dextran was obtained from rice starch using G. oxydans fermentation of rice hydrolysate, and its properties were studied. Both dextrin- and rice hydrolysate-added media maintained the OD value of 6 after 20 h of incubation with acetic acid bacteria, and the gel permeation chromatography (GPC) analysis of the supernatant after 72 h of incubation confirmed that a polymeric material with DP of 480 and 405, which was different from the composition of the substrate in the medium, was produced. The glucose linkage pattern of the polysaccharide was confirmed using the proton nuclear magnetic resonance (1H-NMR) and the increased α-1,4:α-1,6 bond ratio from 0.23 and 0.13 to 1:2.37 and 1:4.4, respectively, indicating that the main bonds were converted to α-1,6 bonds. The treatment of dextrin with a rat-derived alpha-glucosidase digestive enzyme resulted in a slow release of glucose, suggesting that rice hydrolysate can be converted to dextran using acetic acid bacteria with glycosyltransferase activity to produce high-value bio-materials with slowly digestible properties.