• Title/Summary/Keyword: Proton-NMR

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Functionalized Emulsion Styrene-Butadiene Rubber Containing Diethylaminoethyl Methacrylate for Silica Filled Compounds

  • Park, Jinwoo;Kim, Kihyun;Lim, Seok-Hwan;Hong, Youngkun;Paik, Hyun-jong;Kim, Wonho
    • Elastomers and Composites
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    • v.50 no.2
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    • pp.110-118
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    • 2015
  • In this study, diethylaminoethyl methacrylate-styrene-butadiene terpolymer (DEAEMA-SBR), in which diethylaminoethyl methacrylate (DEAEMA) was introduced to the SBR molecule as a third monomer, was synthesized by cold emulsion polymerization. It is expected that amine group introduced to a rubber molecule would improve dispersion of silica by the formation of hydrogen bond (or ionic coupling) between the amine group and silanol groups of silica surface. The chemical structure of DEAEMA-SBR was analyzed using proton nuclear magnetic resonance spectroscopy (H-NMR), Fourier transform infrared spectroscopy (FTIR), gel permeation chromatography (GPC) and differential scanning calorimetry (DSC). Then, various properties of DEAEMA-SBR/silica composite such as crosslink density, bound rubber content, abrasion resistance, and mechanical properties were evaluated. As a result, bound rubber content and crosslink density of DEAEMA-SBR/silica compound were higher than those of the SBR 1721 composite. Abrasion resistance and moduli at 300% elongation of the DEAEMA-SBR/silica composite were better than those of SBR 1721 composite due to the high bound rubber content and crosslink density. These results are attributed to high affinity between DEAEMA-SBR and silica. The proposed study suggests that DEAEMA-SBR can help to improve mechanical properties and abrasion resistance of the tire tread part.

Potentiometric Study of Transition Metal Ions Complexes of Hexadentate($N_4$, $O_2$) Ligands (질소-산소계 여섯 자리 리간드들의 전이금속이온 착물에 대한 전위차법 연구)

  • Kim, Sun-Deuk;Kim, Jun-Kwang;Lee, Woo-Sik
    • Journal of the Korean Chemical Society
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    • v.44 no.6
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    • pp.518-525
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    • 2000
  • The open-chain hexadentate N$_4$, O$_2$ ligands 1,13-bis(2-hydroxybenzyl)-2,5,9,12-tetraazatridecane-tetrahydrochloride (BSATD${\cdot}$4HCl) and 1,14-bis (2-hydroxybenzyl)-2,6,9,12-tetraazatetradecane-tetrahydrochloride (BSATED${\cdot}$ 4HCl) have been synthesized as their tetrahydrochloride salt and characterized by EA, IR, NMR and Mass. Their proton dissociation constants(log$K^{n}_{H}$) and stability constants(log$K_{ML}$) for Cu(II), Ni(II), Co(II), and Zn(II) ions were determined in aqueous solution by potentiometry and compared with those of analogous N$_4$, O$_2$ ligands contain ethylenic spacers or propylenic spacers, which make six-membered chelate rings between the aliphatic nitrogen atoms. Synthesis and characterization of [Cu(BSATD)]ClO$_4$ and [Cu(BSATED)](ClO$_4$)$_2$ complexes are described.

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Preparation and Properties of Sulfonated Poly(ether Sulfone)s Containing BFBN for PEMFC (PEMFC용 고분자 전해질 막을 위한 BFBN을 포함한 sulfonated poly(ether sulfone)s의 합성 및 특성)

  • Lim, Young-Don;Seo, Dong-Wan;Lee, Hyun-Chul;Jin, Hyun-Mi;Hossain, MD. Awlad;Jeong, In-Seok;Kim, Whan-Gi
    • Journal of Hydrogen and New Energy
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    • v.22 no.5
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    • pp.579-584
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    • 2011
  • Sulfonated poly (ether sulfone)s containing BFBN were prepared from 2,3-bis(4-fluorophenyl)-2-butenedinitrile , 4,4-sulfonyldiphenol and sulfonated 4,4'-difluorodiphenylsulfone sodium salt using potassium carbonate, and followed acidification reaction with 1M $H_2SO_4$. BFBN was prepared from 4-fluorobenzylcyanide, $CCl_4$, NaOH using trimethylbenzylammoniumchloride . Sulfonated poly(ether sulfone)s containing BFBN were studied by FT-IR, $^1H$-NMR spectroscopy, and thermo gravimetric analysis (TGA). The water uptake of synthesized S-PBFBN membranes exhibit 31~62% compared with 28% of Nafion 211. The S-PBFBN membranes exhibit proton conductivities ($80^{\circ}C$, RH 100) of 53.8~117.4 mS/cm compared with 137.4 mS/cm of Nafion 211.

Effect of Extract from Paeoniae radix on Rabbit Platelets (작약 추출물의 혈소판 작용에 관한 연구)

  • 박영현;손동주
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.31 no.3
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    • pp.511-515
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    • 2002
  • Paeoniae radix has been considered as one of the most important crude drugs used in traditional oriental medicine and has been employed as a circulatory tonic in care of weakness, night sweats, and lumbar pain, etc. Platelet activation plays an important role in thrombosis and haemostasis. Active compounds for the inhibition of platelet activation from Paeoniae radix were extracted and fractionated into five fractions. Its fraction two and three of ethyl acetate extract inhibited the aggregation of washed rabbit platelets induced by collagen. Two active compounds, bezoyloxypaeoniflorin and paeoniflorin, were isolated from fraction two and three by silica gel column and high performance liquid chromatography. The chemical structures were determined by comparison of their proton and carbon nuclear magnetic resonance spectra. Benzoyloxypaeoniflorin showed strong inhibition at the concentration of 100 ug/mL against collagen-induced washed rabbit platelets aggregation. It is suggested that Paeoniae radix has become food material to prevent a cardiovascular disease.

Synthesis and Antitumor Evaluation of N-Alkyl-N-Nitrosocarbamoyl-$\alpha$-Amino- and 3$\beta$-Amino-$\alpha$-Cholestane Derivatives (N-Alkyl-N-Nitrosocarbamoyl-3$\alpha$-Amino-와 3$\beta$-Amino-5$\alpha$-Cholestane 유도체들의 합성 및 항암작용 평가)

  • 김정균;최순규;조인섭;유동식;유성호;문경호
    • YAKHAK HOEJI
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    • v.29 no.2
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    • pp.62-69
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    • 1985
  • The isomeric intermediates, $3{\alpha}$and $3{\beta}-amino-5{\alpha}-cholestane required for the synthesis of N-nitrosoureas, N-(2-chloroethyl)-N-nitrosocarbamoyl-$3{\alpha}-amino-5{\alpha}$-cholestane (9), N-methyl-N-nitrosocarbamoyl-3${\alpha}-amino-5{\alpha}-cholestane$ (10), N-(2-chloroethyl)-N-nitrosocarbamoyl-$3{\beta}-amino-5{\alpha}-cholestane$: (7), and N-methyl-N-nitrosocarbamoyl-$3{\beta}-amino-5{\alpha}-cholestane$ (8) were obtained through the $LiAlH_{4}$ reduction of $5{\alpha}$-cholestan-3-one oxime, followed by the chromatographic separation: the assignment of the stereochemistry of both isomers were based on the shape and chemical shift of $C_{3}$-proton resonances on their NMR spectra and on the elution mobility on the TLC. The urea intermediates, N-(2-chloroethyl) carbamoyl-3.alpha.-amino-5.alpha.-cholestane (13), N-methylcarbamoyl-$3{\alpha}-amino-5{\alpha}-cholestane$ (14), N-(2-chloroethyl) carbamoyl-$3{\beta}-amino-5{\alpha}-cholestane (11) and N-methyl-$3{\beta}-amino-5{\alpha}$-cholestane (12) were prepared by the treatment of each isomers ($3{\alpha}$-amino-and $3{\beta}-amino-5{\alpha}$-cholestane) with alkyl isocyanates in anhydrous $CHCl_{3}$, and the corresponding nitrosoureas, 7-10 were obtained by the nitrosation of the ureas, 11-14, with AcOH (or HCOOH)/$NaNO_{2}$ in ice-cold condition. The inhibitory activity of the nitrosoureas, 7-10, and their intermediates, 12-14 towards the growth of L1210 murine leukemia cells, were examined. Among them, the compounds 9 and 10 exhibited high activity having $ED_{50}$ to be 5.5g/ml and 6.1g/ml, respectively.

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Conductance Study on the Characteristics of Solution Containing Crown Ethers and Univalent Cation Perchlorates

  • Lee, Shim-Sung;Park, Sung-Oh;Jung, Jong-Hwa;Lee, Bu-Yong;Kim, Si-Joong
    • Bulletin of the Korean Chemical Society
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    • v.11 no.4
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    • pp.276-281
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    • 1990
  • The equivalent conductance of univalent cation (potassium, silver, thallium and ammonium) perchlorates in methanol containing 18-membered crown ethers, 18-crown-6 (18C6) and 1,10-dithia-18-crown-6 (DT18C6) were measured at different temperatures. The equivalent conductances of ammonium perchlorate were increased by increasing content of DT18C6 exceptionally, due to more favorable solvations than complexations. From the equivalent conductance changes, the formation constants for 1:1 compmlexes have been determined, and the values of enthalpy and entropy changes have been calculated. The complexations of 18C6 and DT18C6 with the univalent cations under investigation are all exothermic and the ${\Delta}$S values are all negative and no considerable differences around 50 J/ (k mol). The selectivity order of 18C6 is $K^+ > Tl^+ > Ag^+ > NH_4^+$, while that of DT18C6 is $Ag^+ > Tl^+ > NH_4^+ > K^+$. By sulfur substitutions in 18C6 result in significant decrease in stability, but the stability of $Ag^+$-DT18C6 complex are $10^4$ times larger than those of $K^+$. This increase of stabilities for $Ag^+$-DT18C6 complex are primary due to the result of favorable exothermic heat of reaction between the polarizable soft cation and soft sulfur centers. In NMR experiment, the stepwise additions of cation perchlorates into crown ether solutions induced two major spectral changes. First, the resonance all shift down field and the cation induced shifts were linear up to 1:1 cation/crown ratio, above which no further changes were observed. On the basis of these results, it could be concluded that 1:1 complex is formed. Second, the magnitudes of cation induced shifts were different each other in same ligand. By addition of silver ion to the solution of DT18C6, the largest shift of proton peak near the sulfur atom was observed. These effects are also arisen from the results of covalent bonding between "soft-soft" interactions.

Synthesis of Hydrophobic Imidazolium Ionic Liquids and Studies of Their Physiochemical Properties (소수성의 이미다졸리움 이온성 액체 합성과 이들의 물리화학적 특성 조사)

  • Salman, Muhammad;Lee, Sooyoung;Lee, Hye Jin
    • Applied Chemistry for Engineering
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    • v.32 no.3
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    • pp.277-282
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    • 2021
  • Two hydrophobic imidazolium based ionic liquids including 1-benzyl-3-butylimidazolium hexafluorophosphate [BzBIM]PF6 and 1-pentyl-3-butylimidazolium hexafluorophosphate [PBIM]PF6 having the same anion and different cation parts were synthesized. The structural composition of these ionic liquids were confirmed with Fourier-transform infrared spectroscopy (FT-IR) and proton nuclear magnetic resonance (1H-NMR). Their physiochemical properties such as viscosity, ionic conductivity and thermal stability alongside electrochemical potential window range for both ionic liquid electrolytes were characterized and compared to each other. The overall results revealed that [BzBIM]PF6 has higher thermal and electrochemical stabilities and viscosity than that of [PBIM]PF6 probably due to the presence of benzyl ring in the imidazolium cation providing strong intermolecular π-π interactions.

Effect of Temperature Abuse on Quality and Metabolites of Frozen/Thawed Beef Loins

  • Kwon, Jeong A;Yim, Dong-Gyun;Kim, Hyun-Jun;Ismail, Azfar;Kim, Sung-Su;Lee, Hag Ju;Jo, Cheorun
    • Food Science of Animal Resources
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    • v.42 no.2
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    • pp.341-349
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    • 2022
  • The objective of this study was to examine the effect of temperature abuse prior to cold storage on changes in quality and metabolites of frozen/thawed beef loin. The aerobic packaged samples were assigned to three groups: refrigeration (4℃) (CR); freezing (-18℃ for 6 d) and thawing (20±1℃ for 1 d), followed by refrigeration (4℃) (FT); temperature abuse (20℃ for 6 h) prior to freezing (-18℃ for 6 d) and thawing (20±1℃ for 1 d), followed by refrigeration (4℃) (AFT). FT and AFT resulted in higher volatile basic nitrogen (VBN) values than CR (p<0.05), and these values rapidly increased in the final 15 d. Cooking loss decreased significantly with an increase in the storage period (p<0.05). In addition, cooking loss was lower in the FT and AFT groups than in the CR owing to water loss after storage (p<0.05). A scanning electron microscope (SEM) revealed that frozen/thawed beef samples were influenced by temperature abuse in the structure of the fiber at 15 d. Metabolomic analysis showed differences among CR, FT, and AFT from partial least square discriminant analysis (PLS-DA) based on proton nuclear magnetic resonance (1H NMR) profiling. The treatments differed slightly, with higher FT than AFT values in several metabolites (phenylalanine, isoleucine, valine, betaine, and tyrosine). Overall, temperature abuse prior to freezing and during thawing of beef loin resulted in accelerated quality changes.

Characterization and performance of post treated PVDF hollow fiber membrane

  • Eman S. Sayed;Hayam F. Shaalan;Magda I. Marzouk;Heba A. Hani
    • Membrane and Water Treatment
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    • v.15 no.2
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    • pp.79-88
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    • 2024
  • Modification of Polyvinylidene fluoride (PVDF) hollow fiber membranes (HFMs) characteristics and performance were investigated via post treatment using different oxidants. sodium hypochlorite (NaOCl), hydrogen peroxide (H2O2) and potassium persulfate (KPS). Fourier transform infrared (FTIR) and Proton nuclear magnetic resonance (1H-NMR) results revealed no structural differences after post treatment. Cross-sectional micrographs show finger-like structures at the outer and inner walls of the HFMs and sponge-like structures in middle, where NaOCl and KPS post treated fibers exhibited a decrease in finger-like structures in addition to aggregates appearing on the surface, consequently leading to an increase in the surface roughness (Ra) from 48 nm to 52.8nm and 56 nm, respectively. Hydrogen peroxide post treatment only was observed to decrease the water contact angle from 98° to 81.4°. It was also observed that the elongation at break and the modulus deceased after NaOCl post treatment from 34.5 to 28.5% and from 19.3 Mpa to 16.6 Mpa, respectively. Moreover, pure water flux after H2O2 post treatment increased from 87.8 LMH/bar to 113 LMH/bar at 0.45 bar, while no changes were detected for the methylene blue dye rejection (74%) between raw and hydrogen peroxide post treated fibers at the same pressure. According to the findings hydrogen peroxide post treated PVDF HFMs have the most uniform surfaces, with almost no alterations in structural and mechanical properties or porosities with enhanced hydrophilicity and pure water flux maintaining appropriate rejection. Therefore, it is considered an efficient surface modifying agent for UF/NF membranes or low-pressure separators.

Structural Analysis of the Unusual Sugar-Containing Oligosaccharides Formed by the Selective Cleavage of Weakly Acidic Polysaccharide (약산성 다당의 선택적 분해 과정에서 얻어진 특이당 함유 Oligo당의 구조적 분석)

  • Shin, Kwang-Soon;Lee, Ho
    • Korean Journal of Food Science and Technology
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    • v.29 no.6
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    • pp.1105-1112
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    • 1997
  • By sequential degradation using partial acid hydrolysis of a weakly acidic polysaccharide (GL-4IIb2'), two acidic oligosaccharide fragments, PA-2' and PA-1-III were isolated and their structures were characterized. PA-2' consisted of almost equal proportion of a rhamnose (Rha) and an unusual sugar, 3-deoxy-D-manno-2-octurosonic acid (Kdo). When permethylated oligosaccharide-alditol derived from PA-2' was analyzed by GC-MS, the peak gave the fragment ions at m/z 189 $(bA_1,\;6-deoxyhexose)$ and at m/z 308 $(aJ_2,\;alditol\;from\;Kdo)$. The peak also gave the characteristic ion at m/z 162 but it did not give the fragment ion at m/z 177, suggesting that Kdo is substituted at C5 but not at C4. Methylation analysis also indicated that PA-2' was composed mainly of terminal Rhap and 5-substituted Kdo. When the reduced product from PA-2' was analyzed by $^1H-NMR$, it gave a signal at 5.09 ppm due to an anomeric proton of ${\alpha}-L-Rha$. These results indicated that PA-2' mainly contained ${\alpha}-L-Rhap-(1{\rightarrow}5)-Kdo$. On the other hand, PA-1-III mainly comprised Rha and Kdo in addition to small proportions of arabinose (Ara) and 3-deoxy-D-lyxo-2-heptulosaric acid (Dha). MS analysis of permethylated oligosaccharide-alditols from PA-1-III suggested that the major peak 1P was $Rhap-(1{\rightarrow}5)-Kdo$ whereas the minor peaks 2P and 3P possessed $Araf-(1{\rightarrow}5)-Dha$ unit and these peaks were produced as epimers during reduction of carbonyl groups in Dha.

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