• Title/Summary/Keyword: 1H-NMR spectroscopy

Search Result 576, Processing Time 0.025 seconds

High Out-of-Plane Alignment of Liquid Crystalline Methacrylate Copolymer Bearing Photoreactive 4-Styrylpyridine Moiety

  • Kwak, Gi-Seop;Kong, Jong-Yun;Kim, Min-Woo;Hyun, Seok-Hee;Kim, Woo-Sik
    • Macromolecular Research
    • /
    • v.17 no.4
    • /
    • pp.271-275
    • /
    • 2009
  • This paper describes the out-of-plane order of a liquid crystalline(LC) methacrylate copolymer(3) comprised of a methacrylate(1) with a 4-styrylpyridine moiety as the photo-cyclodimerizable group and a benzoate moiety as the mesogenic group in the side chain, and another methacrylate(2) with a 4-(4-methoxyphenyl)benzoate moiety as the mesogenic group. The composition of 1 and 2 units in 3 was estimated to have a molar ratio of 54.2:45.8 by $^{1}H$ NMR spectroscopy. The X-ray diffraction study revealed that the copolymer forms a partial bilayer smectic structure. The copolymer gave rise to a high out-of-plane order parameter of about 0.74 in a wide LC temperature range of $110{\sim}160^{\circ}C$ after linearly polarized, UV light irradiation and subsequent annealing. Moreover, the external reflection IR analysis indicated that excess UV-light irradiation makes the out-of-plane LC structure of the copolymer appear in a higher and wider temperature range.

Production of Citrate by Anaerobic Fungi in the Presence of Co-culture Methanogens as Revealed by 1H NMR Spectrometry

  • Cheng, Yan Fen;Jin, Wei;Mao, Sheng Yong;Zhu, Wei-Yun
    • Asian-Australasian Journal of Animal Sciences
    • /
    • v.26 no.10
    • /
    • pp.1416-1423
    • /
    • 2013
  • The metabolomic profile of the anaerobic fungus Piromyces sp. F1, isolated from the rumen of goats, and how this is affected by the presence of naturally associated methanogens, was analyzed by nuclear magnetic resonance spectroscopy. The major metabolites in the fungal monoculture were formate, lactate, ethanol, acetate, succinate, sugars/amino acids and ${\alpha}$-ketoglutarate, whereas the co-cultures of anaerobic fungi and associated methanogens produced citrate. This is the first report of citrate as a major metabolite of anaerobic fungi. Univariate analysis showed that the mean values of formate, lactate, ethanol, citrate, succinate and acetate in co-cultures were significantly higher than those in the fungal monoculture, while the mean values of glucose and ${\alpha}$-ketoglutarate were significantly reduced in co-cultures. Unsupervised principal components analysis revealed separation of metabolite profiles of the fungal mono-culture and co-cultures. In conclusion, the novel finding of citrate as one of the major metabolites of anaerobic fungi associated with methanogens may suggest a new yet to be identified pathway exists in co-culture. Anaerobic fungal metabolism was shifted by associated methanogens, indicating that anaerobic fungi are important providers of substrates for methanogens in the rumen and thus play a key role in ruminal methanogenesis.

Reaction and Theoretical Study of the Coordination of an N2O-Donor Amino Alcoholic Ligand Toward Group 12 Metals Mixtures

  • Mardani, Zahra;Moeini, Keyvan;Kazemshoar-Duzduzani, Reza
    • Journal of the Korean Chemical Society
    • /
    • v.63 no.3
    • /
    • pp.160-165
    • /
    • 2019
  • A series of reactions between an amino alcoholic ligand, cis-2-((2-((2-hydroxyethyl)amino)ethyl)amino)cyclohexan-1-ol (HEAC), with the mixtures of group 12 metals including, $HgCl_2/CdCl_2$, $HgCl_2/CdI_2$, $ZnCl_2/CdCl_2$ and $ZnCl_2/CdCl_2/HgCl_2$ was experimentally and theoretically studied to determine the most stable product of these reactions. Furthermore, the Cambridge Structural Database (CSD) studies were done to evaluate the theoretical results. The products were characterized by elemental analysis, FT-IR, Raman, $^1H$ NMR spectroscopy and single-crystal X-ray diffraction. Based on these investigations a binuclear structure of cadmium, [$Cd_2(HEAC)_2({\mu}-Cl)_2Cl_2$] (1), is the most stable product that was formed in all studied reactions between HEAC and metals mixtures. In this structure, the cadmium atom has a $CdN_2O({\mu}-Cl)_2Cl$ environment and distorted octahedral geometry.

Hygroscopicity of 1:2 Choline Chloride:Ethylene Glycol Deep Eutectic Solvent: A Hindrance to its Electroplating Industry Adoption

  • Brusas, John Raymund;Dela Pena, Eden May B.
    • Journal of Electrochemical Science and Technology
    • /
    • v.12 no.4
    • /
    • pp.387-397
    • /
    • 2021
  • Deep eutectic solvents have been established as feasible metal electroplating solvent alternatives over traditional toxic aqueous plating baths. However, water, either added intentionally or unintentionally, can significantly influence the solvent's physical properties and performance, thereby hindering its industry application. In this study, the hygroscopicity, or the ability to absorb moisture from the environment, of synthesized ethaline (1:2 choline chloride:ethylene glycol) was investigated. The kinematic viscosity, electrical conductivity, electrochemical window, and water content of ethaline were monitored over a 2-week period. Karl Fischer titration tests showed that ethaline exposed to the atmosphere displayed significant hygroscopicity compared to its unexposed counterpart. 1H NMR spectroscopy revealed that water vapor was readily absorbed at the surface due to the hydrophilic groups present in the ethaline molecule. Water uptake resulted in the decrease in viscosity, increase in electrical conductivity and narrowing of the electrochemical window of ethaline. Solution heating at 100℃ removed the absorbed moisture and allowed the recovery of the solvent's initial properties.

Synthesis And Ionic Conductivity of Siloxane Based Polymer Electrolytes with Propyl Butyrate Pendant Groups

  • Jalagonia, Natia;Tatrishvili, Tamara;Markarashvili, Eliza;Aneli, Jimsher;Grazulevicius, Jouzas Vidas;Mukbaniani, Omar
    • Korean Chemical Engineering Research
    • /
    • v.54 no.1
    • /
    • pp.36-43
    • /
    • 2016
  • Hydrosilylation reactions of 2.4.6.8-tetrahydro-2.4.6.8-tetramethylcyclotetrasiloxane with allyl butyrate catalyzed by Karstedt's, $H_2PtCl_6$ and Pt/C catalyst were studied and 2.4.6.8-tetra (propyl butyrate)-2.4.6.8-tetramethylcyclotetrasiloxane was obtained. The reaction order, activation energies and rate constants were determined. Ringopening polymerization of 2.4.6.8-tetra (propyl butyrate)-2.4.6.8-tetramethylcyclotetrasiloxane in the presence of $CaF_2$, LiF, KF and anhydrous potassium hydroxide in $60-70^{\circ}C$ temperature range was carried out and methylsiloxane oligomers with regular arrangement of propyl butyrate pendant groups were obtained. The synthesized products were studied by FTIR and NMR spectroscopy. The polysiloxanes were characterized by wide-angle X-ray, gel-permeation chromatography and DSC analyses. Via sol-gel processes of oligomers doped with lithium trifluoromethylsulfonate or lithium bis (trifluoromethylsulfonyl)imide, solid polymer electrolyte membranes were obtained. The dependences of ionic conductivity of obtained polyelectrolytes on temperature and salt concentration were investigated, and it was shown that electric conductivity of the polymer electrolyte membranes at room temperature changed in the range $3.5{\times}10^{-4}{\sim}6.4{\times}10^{-7}S/cm$.

Influence of Lithium Ions on the Ion-coordinating Ruthenium Sensitizers for Nanocrystalline Dye-sensitized Solar Cells

  • Cho, Na-Ra;Lee, Chi-Woo;Cho, Dae-Won;Kang, Sang-Ook;Ko, Jae-Jung;Nazeeruddin, Mohammad K.
    • Bulletin of the Korean Chemical Society
    • /
    • v.32 no.spc8
    • /
    • pp.3031-3038
    • /
    • 2011
  • Ion-coordinating ruthenium complexes [cis-Ru(dcbpy)(L)(NCS)$_2$, where dcbpy is 4,4'-dicarboxylic acid-2,2'-bipyridine and L is 1,4,7,10-tetraoxa-13-azacyclopentadecane, JK-121, or bis(2-(2-methoxy-ethoxy)ethyl) amine, JK-122] have been synthesized and characterized using $^1H$ NMR, Fourier transform IR, UV/vis spectroscopy, and cyclic voltammetry. The effect of $Li^+$ in the electrolyte on the photovoltaic performance was investigated. With the stepwise addition of $Li^+$ to a liquid electrolyte, the device shows significant increase in the photo-current density, but a small decrease in the open circuit voltage. The solar cell with a hole conductor, the addition of $Li^+$ resulted in a 30% improvement in efficiency. The JK-121 sensitized cells in the liquid and solid-state electrolyte give power conversion efficiencies of 6.95% and 2.59%, respectively, under the simulated sunlight.

Isolation and Identification of Pratensein with Antimicrobial Activity from the Peanut Shells (땅콩껍질에서 항미생물 활성을 지닌 pratensein의 분리 및 동정)

  • Wee, Ji-Hyang;Moon, Jae-Hak;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
    • /
    • v.36 no.4
    • /
    • pp.643-647
    • /
    • 2004
  • Natural antimicrobial substance from peanut (Arachis hypogaea) shells was isolated and structurally elucidated. Peanut shells were extracted with methanol (MeOH) and concentrated in vacuo, MeOH extract was solvent-fractionated with ethyl acetate (EtOAc) and various buffer to obtain EtOAc acidic, neutral, and phenolic fractions. EtOAc neutral fraction, which showed antimicrobial activity, was purified through silica gel adsorption column, Sephadex LH-20 column, ODS column, and high performance liquid chromatographies, and its active substance was isolated and identified as pratensein (3',5,7-trihydroxy-4'-methoxyisoflavone) by spectroscopic methods of proton-nuclear magnetic resonance, mass spectrometry, and nuclear overhauser enhancement spectroscopy.

Synthesis and Characterization of a New PPV Derivative Containing a Sterically Hindered 2,5-Dimethylphenyl Group

  • Kim, Yun-Hi;Lee, Hyun-Ouk;Lee, Ki-Suk;Kwon, Soon-Ki
    • Macromolecular Research
    • /
    • v.11 no.6
    • /
    • pp.471-475
    • /
    • 2003
  • A new poly[2-(2',5'-dimethylphenyl)-1,4-phenylenevinylene] (PDMPPV) that features a bulky 2',5'-dimethylphenyl substituent, which can induce steric hindrance between the PPV backbone and the methyl groups, was designed and synthesized. The polymer structure having no TBB defects was confirmed by $^1$H-NMR and $\^$13/CNMR spectroscopy. The polymer showed good thermal stability with high T$\_$g/. The polymer film showed a maximum absorption at 415 nm with an absorption onset at 480 nm. The maximum emission peak showed at ca. 515 nm, with a shoulder at 530 nm. The turn-on voltages of ITO/PEDOT/PDMPPV/Al and ITO/PDMPPV/Al devices were 8 and 10 V, respectively. The electroluminescence spectrum from the device showed a maximum peak at 510 nm with a shoulder at ca. 535 nm.

Cytotoxic Effects of Furanosesterterpenes, Cyclitol Derivatives, and Bromotyrosine Derivative Isolated from Marine Sponges

  • Sohn, Jae-Hak;Oh, Hyun-Cheol;Jung, Jee-H.;Bae, Song-Ja
    • Preventive Nutrition and Food Science
    • /
    • v.10 no.3
    • /
    • pp.257-261
    • /
    • 2005
  • Marine sponges are known to produce a number of cytotoxic secondary metabolites. In the course of searching for cytotoxic metabolites from marine organisms, we have evaluated cytotoxic activities of six marine secondary metabolites isolated from various sponges. The cytotoxic compounds 1-6 were isolated by the application of various chromatographic methods, including column chromatography and HPLC. The molecular structures were mostly determined using mass spectrometry (MS) and Nuclear Magnetic Resonance (NMR) Spectroscopy. Furanosestererpenes (compounds 1-3) from Psammocinia sp., cyclitol derivatives (compounds 4 and 5) from Sarcotragus sp., and bromotyrosine-type compound (6) from an association of two sponges Jaspis wondoensis and Poecillastra wondoensis were evaluated for their cytotoxic activity against three cancer cell lines; Hep G2, HeLa, and MCF-7. All tested compounds exhibited cyctoxicity at concentrations ranging from $5\;\mug/mL\;to\;25\;\mug/mL.$ Particularly, among the tested compounds, compound 6 showed the highest potency displaying at least $80\%$ of cytotoxicity at $5\;\mug/mL$ level against all three cancer cell lines.

Preparation and Characterization of Nanoparticles Using Poly(N-isopropylacrylamide)-$Poly({\varepsilon}-caprolactone)$ and Poly(ethylene glycol)-$Poly({\varepsilon}-caprolactone)$ Block Copolymers with Thermosensitive Function

  • Choi, Chang-Yong;Jang, Mi-Kyeong;Nah, Jae-Woon
    • Macromolecular Research
    • /
    • v.15 no.7
    • /
    • pp.623-632
    • /
    • 2007
  • Thermosensitive nanoparticles were prepared via the self-assembly of two different $poly({\varepsilon}-caprolactone)$-based block copolymers of poly(N-isopropylacrylamide)-b-$poly({\varepsilon}-caprolactone)$ (PNPCL) and poly(ethylene glycol)-b-$poly({\varepsilon}-caprolactone)$ (PEGCL). The self-aggregation and thermosensitive behaviors of the mixed nanoparticles were investigated using $^1H-NMR$, turbidimetry, differential scanning microcalorimetry (micro-DSC), dynamic light scattering (DLS), and fluorescence spectroscopy. The copolymer mixtures (mixed nanoparticles, M1-M5, with different PNPCL content) formed nano-sized self-aggregates in an aqueous environment via the intra- and/or intermolecular association of hydrophobic PCL chains. The microscopic investigation of the mixed nanoparticles showed that the critical aggregation concentration (cac), the partition equilibrium constants $(K_v)$ of pyrene, and the aggregation number of PCL chains per one hydrophobic microdomain varied in accordance with the compositions of the mixed nanoparticles. Furthermore, the PNPCL harboring mixed nanoparticles evidenced phase transition behavior, originated by coil to the globule transition of PNiPAAm block upon heating, thereby resulting in the turbidity change, endothermic heat exchange, and particle size reduction upon heating. The drug release tests showed that the formation of the thermosensitive hydrogel layer enhanced the sustained drug release patterns by functioning as an additional diffusion barrier.