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

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Nitrogen-doped carbon nanosheets from polyurethane foams and removal of Cr(VI)

  • Duan, Jiaqi;Zhang, Baohua;Fan, Huailin;Shen, Wenzhong;Qu, Shijie
    • Carbon letters
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    • v.22
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    • pp.60-69
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    • 2017
  • Nitrogen-doped carbon nanosheets with a developed porous structure were prepared from polyurethane foams by hydrothermal carbonization following $ZnCl_2$ chemical activation. Scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, solid state $^{13}C$ nuclear magnetic resonance (NMR) spectra and X-ray photoelectron spectroscopy were used to characterize the nitrogen-doped carbon nanosheet structure and composition. The removal of Cr(VI) by the N-doped carbon nanosheets was investigated. The results showed that the maximum removal capacity for chromium of 188 mg/g was found at pH=2.0 with PHC-Z-3. pH had an important effect on Cr(VI) removal and the optimal pH was 2.0. Moreover, amino groups and carboxyl groups in the nitrogen-doped carbon nanosheet played important roles in Cr(VI) removal, and promoted the reduction of Cr(VI) to Cr(III).

Preparation and Characterization of Surfactant-Exfoliated Graphene

  • Song, Yeari;Lee, Hoik;Ko, Jaehyoung;Ryu, Jungju;Kim, Minkyoung;Sohn, Daewon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.7
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    • pp.2009-2012
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    • 2014
  • An anionic surfactant, sodium dodecylbenzene sulfonate (SDBS), was introduced during the ultrasonication process for exfoliation of graphene. The surfactant plays the roles of exfoliator and stabilizer by binding to the graphene surface. The obtained modified graphene was characterized by Fourier-transform infrared spectroscopy (FT-IR) and solid state $^{13}C$ CP/MAS NMR to analyze the binding between molecules, and by X-ray diffraction (XRD) to characterize the bulk structure. The resulting graphene exhibited good dispersion stability in both water and organic solvents.

The Organization of Nanoporous Structure Using Controlled Micelle Size from MPEG-b-PDLLA Block Copolymers

  • Chang, Jeong-Ho;Kim, Kyung-Ja;Shin, Young-Kook
    • Bulletin of the Korean Chemical Society
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    • v.25 no.3
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    • pp.351-356
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    • 2004
  • Selected MPEG-b-PDLLA block copolymers have been synthesized by ring-opening polymerization with systematic variation of the chain lengths of the resident hydrophilic and hydrophobic blocks. The size and shape of the micelles that spontaneously form in solution are then controlled by the characteristics of the block copolymer template. All the materials prepared in this study showed the tunable pore size of 20-80 ${\AA}$ with the increase of hydrophobic chain lengths and up to 660 $m^2$/g of specific surface area. The formation mechanism of these nanoporous structures obtained by controlling the micelle size has been confirmed using both liquid and solid state $^{13}C\;and\;^{29}Si$ NMR techniques. This work verifies the formation mechanism of nanoporous structures in which the pore size and wall thickness are closely dependent on the size of hydrophobic cores and hydrophilic shells of the block copolymer templates.

Production and Amyloid fibril formation of tandem repeats of recombinant Yeast Prion like protein fragment

  • Kim, Yong-Ae;Park, Jae-Joon;Hwang, Jung-Hyun;Park, Tae-Joon
    • Journal of the Korean Magnetic Resonance Society
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    • v.15 no.2
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    • pp.175-186
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    • 2011
  • Amyloid fibrils have long been known to be the well known ${\alpha}$-helix to ${\beta}$-sheet transition characterizing the conversion of cellular to scrapie forms of the prion protein. A very short sequence of Yeast prion-like protein, GNNQQNY (SupN), is responsible for aggregation that induces diseases. KSI-fused tandem repeats of SupN vector are constructed and used to express SupN peptide in Escherichia coli (E.Coli). A method for a production, purification, and cleavage of tandem repeats of recombinant isotopically enriched SupN in E. coli is described. This method yields as much as 20 mg/L of isotope-enriched fusion proteins in minimal media. Synthetic SupN peptides and $^{13}C$ Gly labeled SupN peptides are studied by Congo Red staining, Birefringence and transmission electron microscopy to characterize amyloid fibril formation. To get a better understanding of aggregation-structure relationship of 7 residues of Yeast prion-like protein, the change of a conformational structure will be studied by $^{13}C$ solid-state nmr spectroscopy as powder of both amorphous and fibrillar forms.

Solubility of Liquid Crystalline Hydroxypropyl Chitin in Organic Solvent (액정성 히드록시프로필키틴의 유기용매에 대한 용해성)

  • Lee, Young Moo;Kim, Seong Soo;Kim, Seon Jeong;Sung, Yong Kiel;Kang, In Kyu;Son, Tae II
    • Applied Chemistry for Engineering
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    • v.4 no.2
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    • pp.403-408
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    • 1993
  • Hydroxypropyl chitin(HPCH) was prepared from chitin by reacting it with propylene oxide. The formation of liquid crystalline character of HPCH was investigated using halogenated organic solvents. Solid state $^{13}C$ NMR spectra for chitin and HPCH confirmed the incorporation of hydroxypropyl moiety. The degree of substitution of HPCH was around 0.8 as detected by elemental analysis. WAXD patterns of chitin and HPCH showed that an incorporation of hydroxypropyl unit in chitin contributed to reducing the crystallinity and enhancing the solubility in organic solvents. Polarized light microscopic pictures of concentrated HPCH solution showed that HPCH formed cholesteric liquid crystalline character at about 25w/v% solution in dichloroacetic acid and 1, 2-dichloroethane. Inherent viscosity of HPCH solution in a mixed solvent showed a transient decrease.

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Spectroscopic Studies on the Reaction between Amino Groups on Silica Nanoparticle Surface and Glycidyl Methacrylate (실리카 나노입자 표면에 결합된 아미노기와 Glycidyl Methacrylate의 반응에 관한 분광학적 연구)

  • Lee, Sangmi;Ha, KiRyong
    • Polymer(Korea)
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    • v.37 no.6
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    • pp.777-783
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    • 2013
  • We used dipodal type bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify silica nanoparticles to introduce secondary amino groups on the silica surface. These grafted N-H groups were reacted with glycidyl methacrylate (GMA) to introduce polymerizable methacrylate groups on the silica surface. After modification reaction, we used several analytical techniques such as Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state $^{13}C$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to analyze the effects of reaction time, reaction temperature and used GMA concentration on the modification degree between N-H groups on the silica surface and epoxide groups of GMA. We found increased introduction of methacrylate groups on the silica surface by ring opening reaction of epoxide groups of GMA with N-H groups on BTMA treated silica with increased reaction time, reaction temperature and used GMA concentration within our experimental conditions.

Synthesis and Characterization of (THF)3 Li(NC)CU(C6H3-2,6-Mes2)and Br(THF)2 Mg(C6H3-2,6-Trip2) (Mes = C6H2-2,4,6-Me3; Trip = C6H2-2,4,6-i-Pr3): The Structures of a Monomeric Lower-Order Lithi

  • Hwang, Cheong-Soo;Power, Philip P.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.5
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    • pp.605-609
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    • 2003
  • The lower-order lithium organocyanocuprate compound, (THF)₃Li(NC)Cu($C_6$H₃-2,6-Mes₂) (1), and the bulky terphenyl Grignard reagent, Br(THF)₂Mg($C_6$H₃-2,6-Trip₂) (2), have been synthesized and structurally characterized both in the solid state by single crystal x-ray crystallography and in solution by multi-nuclear NMR and IR spectroscopy. The compound (1) was isolated as a monomeric contact ion-pair in which the C (organic ipso)-Cu-CN-Li atoms are coordinated linearly. The lithium has a tetrahedral geometry as a result of solvation by three THF molecules. The compound (1) is the first example of fully characterized monomeric lower order lithium organocyanocuprate. The bulky Grignard reagent (2) was also isolated as a monomer in which the magnesium, solvated by two THF molecules, has a distorted tetrahedral geometry. The crystals of (1) possess triclinic symmetry with the space group $P{\={1}}$, Z = 2, with a = 12.456(3) Å, b = 12.508(3) Å, c = 13.904(3) Å, α = 99.81°, β = 103.72(3)°, and γ = 119.44(3)°. The crystals (2) have a monoclinic symmetry of space group $P2_{1/C}$, Z = 4, with a = 13.071(3) Å, b = 14.967(3) Å, c = 22.070(4) Å, and β = 98.95(3)°.

Development of Near-Critical Water Reaction System for Utilization of Lignin as Chemical Resources

  • Eom, Hee-Jun;Hong, Yoon-Ki;Park, Young-Moo;Chung, Sang-Ho;Lee, Kwan-Young
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.251.2-251.2
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    • 2010
  • Plant biomass has been proposed to be an alternative source for petroleum-based chemical compounds. Especially, phenolic chemical compounds can be obtained from lignin by chemical depolymerization processes because lignin consists of complex aromatic polymer such as trans-p-coumaryl, coniferyl and sinapyl alcohols, etc. Phenolic chemical compounds from lignin were usually produced in super critical water. However, we applied Near-critical water (NCW) system because NCW is known as a good solvent for lignin depolymerization. Organic matter like lignin can be solved in NCW system and the system has a unique acid-base property without conventional non-eco-friendly chemicals such as sulfuric acid and sodium hydroxide. In this work, we tried to optimize the NCW depolymerization system by adjusting the processing variables such as reaction time, temperature and pressure. Moreover, the amount of additional phenol was optimized by changing the molar ratio between water and phenol. Phenol was used as capping agent to prevent re-polymerization of active fragment such as formaldehyde. Alkali-lignin was used as a starting material and characterized by a Solid State 13C-NMR, FT-IR and EA (Elemental Analysis). GC-MS analysis confirmed that o-cresol, p-cresol, anisole and 4-hydroxyphathalic acid were the main product and they were quantitatively analyzed by HPLC.

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Study on Separation Characteristics of Flue Gas Using Hydroquinone Clathrate Compounds (하이드로퀴논 크러스레이트를 이용한 배가스 분리 특성 연구)

  • Lee, Jong-Won;Choi, Ki-Jong
    • Korean Chemical Engineering Research
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    • v.49 no.6
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    • pp.865-868
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    • 2011
  • An organic substance, hydroquinone is used to form clathrate compounds in order to identify separation characteristics of carbon dioxide in flue gas. Formed samples were analyzed by means of the solid-state $^{13}C$ nuclear magnetic resonance (NMR) and Raman spectroscopic methods to examine enclthration behaviors of guest species. In addition, elemnetal analysis was also performed in order to evaluate separation efficiency of $CO_2$ in a quantitative way. Based on the experimental results obtained, $CO_2$ molecules are found to be captured into the clathrate compound more readily than $N_2$ molecules. Moreover, because such preferential enclathration is even more significant at low pressure conditions, $CO_2$ separation/recovery from flue gas can be achieved with minimizing additional energy cost for the technique. Experimental results obtained in this study can provide useful information on separation techniques of flue gas or selective separation of gas mixtures in the future.

Transition Metal Complexes Derived From 2-hydroxy-4-(p-tolyldiazenyl)benzylidene)-2-(p-tolylamino)acetohydrazide Synthesis, Structural Characterization, and Biological Activities

  • Alhakimi, Ahmed N.;Shakdofa, Mohamad M.E.;Saeed, S. El-Sayed;Shakdofa, Adel M.E.;Al-Fakeh, Maged S.;Abdu, Ashwaq M.;Alhagri, Ibrahim A.
    • Journal of the Korean Chemical Society
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    • v.65 no.2
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    • pp.93-105
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    • 2021
  • Mononuclear Cu(II), Ni(II), Co(II), Mn(II), Zn(II), Fe(III), Ru(III), and UO2(II) complexes of 2-hydroxy-4-(p-tolyldiazenyl)benzylidene)-2-(p-tolylamino)acetohydrazide (H2L) were prepared by direct method. The ligand and its complexes were isolated in solid state and characterized by analytical techniques such as elemental and thermal analyses, molar conductance, magnetic susceptibility measurements and spectroscopic techniques such as UV-Visible, IR, 1H-NMR and 13C-NMR. The spectral data indicated that the ligand acted as neutral/monobasic bidentate or monobasic/dibasic tridentate ligand bonded to the metal ions through the oxygen atom of ketonic or enolic carbonyl group, azomethine nitrogen atom and deprotonated/protonated phenolic oxygen atom forming either tetragonally distorted octahedral or octahedral. Antimicrobial activities of the ligand and its complexes were evaluated against Escherichia coli, Bacillus subtilis and Aspergillus niger by well diffusion method. The results of antifungal activity showed that the Fe(III) complex (10) exhibited higher antifungal against Aspergillus niger than the other complexes. However, the results of antibacterial activity revealed that Cu(II) complex (4) is the most active against Escherichia coli while the Cu(II) complex (5) and Fe(III) complex (10) exhibited higher antibacterial effect on Bacillus subtilis than the other complexes.