• 제목/요약/키워드: 1H-NMR spectroscopy

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Positive-Type Photosensitive Polyimide Based on a Photobase Generator Containing Oxime-Urethane Groups as a Photosensitive Compound

  • Jang Young-Min;Seo Ji-Young;Chae Kyu-Ho;Yi Mi-Hye
    • Macromolecular Research
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    • 제14권3호
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    • pp.300-305
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    • 2006
  • The chemical structure of a semi-aromatic polyimide-I, which was prepared by the chemical imidization of cyclopentanetetracarboxylic dianhydride and 2,2-bis(4-aminophenyl)hexafluoropropane, was characterized by $^{13}C-NMR$ spectroscopy. The chemically imidized polyimide-I was used for the preparation of a photosensitive polyimide (PSPI) through the addition of benzophenone and benzophenone oxime hexamethylene diurethane (BOHD), a photobase generator containing oxime-urethane groups. The polyimide-I film containing benzophenone and BOHD was not soluble in 2.38 wt% tetrabutylammonium hydroxide solution in $H_2O$. However, it became soluble following irradiation with 310 nm UV light. A positive tone image with a resolution of $5{\mu}m$ was obtained with this PSPI, having sensitivity($D_c$) of $1.2J/cm^2$ and contrast(${\gamma}_p$) of 1.08. Thus, a polyimide, which is not intrinsically photosensitive, can become photosensitive through the addition of a photobase generator containing oxime-urethane groups as a photosensitive compound.

디아미노피리딘아조계 Red 분산염료들의 합성과 염색성 (Synthesis and Dyeing Properties of Red Disperse Dyes Derived from Diaminopyridines)

  • 박종호;고준석;배진석;김성동
    • 한국염색가공학회지
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    • 제17권6호
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    • pp.1-10
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    • 2005
  • Disperse dyes derived from heterocyclic compounds such as phenylindole, pyridone, diaminopyridine, and carbazole have been known to exhibit high light fastness and bathochromic shift compared to the coursponding aminoazobenzene. The synthetic method to obtain diaminopyridine derivatives, which can be used as coupling components, was chlorination of pyridone with phosphorous oxychloride, followed by substitution with various primary amines. Four azo disperse dyes were synthesized by coupling four diaminopyridines with 2-cyano-4-nitroaniline as a diazo component. Structures of these dyes were confirmed by $^1H$ NMR spectroscopy. The wavelengths of maximum absorption of the synthesized disperse dyes were in the range of $517\~528nm$, and molar extinction coefficients were $45,700\~50,100$. The dyeability of four disperse dyes toward PET fiber was generally good. Wash and rubbing fastnesses were excellent, while light and dry heat fastness were good.

공통의 1차 구조를 가진 우유 지방구막 구성단백질의 당쇄 구조에 관한 생화학적 연구 (Biochemical Studies on the Sugar Chain Structure of Glycoproteins with the Same Protein Core of Bovine Milk Fat Globule Membrane)

  • 석진석
    • Journal of Dairy Science and Biotechnology
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    • 제21권2호
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    • pp.138-147
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    • 2003
  • We here analyzed and proposed the structures of the N-linked sugar chains of PAS-7 from bovine milk fat globule membrane. The N-linked sugar chains were liberated from PAS-7 by hydrazinolysis and, after modifying the reducing ends with 2-aminopyridine (PA), were separated into one neutral (7N,55%) and two acidic (7M mono-, 43%; 7D, di-, 2%) sugar chain roups. The latter were converted into neutral groups (7MN and 7DN) by sialidase digestion. The structure of each of these PA-neutral sugar chains was determined by sugar analysis, sequential exoglycosidase digestion, partial acetolysis, and 1H-NMR spectroscopy. The results show that the 10 sugar chains were of the biantennary complex type with and without fucose. The structure of 7N2A one of the major sugar chains, was proposed as; [structure: see text] A structural comparison between PAS-6 and -7 indicated that although they shared the same protein core, their sugar moiety was markedly different, involving the existence of a different pathway during the post-transcriptional modification.

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Dimesogenic Compounds with Chiral Tails: Synthesis and Liquid Crystalline Properties of a Homologous Series of a, w-Bis[4-(4'-(S)-( -)-2-methylbutoxycarbonylbiphenyl- 4-oxycarbonyl)phenoxy]alkanes

  • 최이준;최봉구;김재훈;진정일
    • Bulletin of the Korean Chemical Society
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    • 제21권1호
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    • pp.110-117
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    • 2000
  • A series of new liquid crystalline dimesogenic compounds with chiral tails was synthesized, and their thermal and liquid crystalline properties were studied. The chain length of the central polymethylene spacers (x) was varied from dimethylene (2) to decamethylene (12). These compounds were characterized by elemental analysis, IR and NMR spectroscopy, differential scanning calorimetry (DSC), and cross-polarizing microscopy. All compounds were found to be enantiotropically liquid crystalline, and the values of melting ($T_m$) and isotropization temperature ($T_i$) as well as enthalpy change (Δ$H_i$) and entropy change for isotropization (Δ$S_i$) decreased in a zig-zag fashion revealing the so-called odd-even effect as x increases. Their mesomorphic properties fall into three categories depending upon x; (a) compounds with x=2 and 4 formed two different mesophases, smectic and cholesteric phases in that order on heating, and vice versa on cooling, (b) compounds with x=3, 7, 8, 10 and 11 reversibly formed only the cholesteric phase, and (c) compounds with x=5, 6, 9 and 12 exhibited only a cholesteric phase on heating, whereas on cooling they formed two different mesophases, cholesteric and smectic phases, sequentially.

Liquid Crystalline Properties of Dimers Having o-, m- and p- Positional Molecular Structures

  • Park, Joo-Hoon;Choi, Ok-Byung;Lee, Hwan-Myung;Lee, Jin-Young;Kim, Sung-Jo;Cha, Eun-Hee;Kim, Dong-Hyun;Ramaraj, B.;So, Bong-Keun;Kim, Kyung-Hwan;Lee, Soo-Min;Yoon, Kuk-Ro
    • Bulletin of the Korean Chemical Society
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    • 제33권5호
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    • pp.1647-1652
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    • 2012
  • With the objective to design and synthesis of Schiff's base symmetrical liquid crystal dimmers and to study the effect of molecular structure variation ($o-ortho$, $m-meta$, $p-para$) and change in alkoxy terminal chain length on mesomorphic properties of liquid crystals, We have synthesized Schiff base dimers from dialdehyde derivative containing 2-hydroxy-1,3-dioxypropylene as short spacer with aniline derivatives having different lengths of terminal alkoxy chains ($n$ = 5, 7, 9). The chemical structure of the final products was characterized by proton nuclear magnetic resonance ($^1H$ NMR) spectroscopy and fourier transform infrared (FT-IR) spectroscopy. The mesomorphic properties and optical textures of the resultant dimers were characterized by differential scanning calorimetry (DSC) and polarized optical microscopy (POM). The existence of smectic A phase transition was confirmed by the observation of batonnets and fan shaped textures in optical microscopy when compound were heated from crystalline phase. All of the dimers of this series, with the exception of $\mathbf{2S_5}$ -ortho, -meta, -para, were thermotropic liquid crystal. The compound $\mathbf{2S_9}$ -meta was monotropic, while the rest were enantiotropic. It was found that the change in terminal alkoxy chain length has pronounced effect on the mesomorphic properties. The temperature range of smectic A phase window widens with increasing alkoxy chain length.

Synthesis of Biosurfactant-Based Silver Nanoparticles with Purified Rhamnolipids Isolated from Pseudomonas aeruginosa BS-161R

  • Kumar, C. Ganesh;Mamidyala, Suman Kumar;Das, Biswanath;Sridhar, B.;Devi, G. Sarala;Karuna, Mallampalli SriLakshmi
    • Journal of Microbiology and Biotechnology
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    • 제20권7호
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    • pp.1061-1068
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    • 2010
  • The biological synthesis of nanoparticles has gained considerable attention in view of their excellent biocompatibility and low toxicity. We isolated and purified rhamnolipids from Pseudomonas aeruginosa strain BS-161R, and these purified rhamnolipids were used to synthesize silver nanoparticles. The purified rhamnolipids were further characterized and the structure was elucidated based on one- and two-dimensional $^1H$ and $^{13}C$ NMR, FT-IR, and HR-MS spectral data. Purified rhamnolipids in a pseudoternary system of n-heptane and water system along with n-butanol as a cosurfactant were added to the aqueous solutions of silver nitrate and sodium borohydride to form reverse micelles. When these micelles were mixed, they resulted in the rapid formation of silver nanoparticles. The synthesized nanoparticles were characterized by UV-Visible spectroscopy, transmission electron microscopy, and energy dispersive X-ray spectroscopy (EDS). The nanoparticles formed had a sharp adsorption peak at 410 nm, which is characteristic of surface plasmon resonance of the silver nanoparticles. The nanoparticles were monodispersed, with an average particle size of 15.1 nm (${\sigma}={\pm}5.82$ nm), and spherical in shape. The EDS analysis revealed the presence of elemental silver signal in the synthesized nanoparticles. The formed silver nanoparticles exhibited good antibiotic activity against both Grampositive and Gram-negative pathogens and Candida albicans, suggesting their broad-spectrum antimicrobial activity.

Synthesis and Light-Emitting Properties of Phenyl-Thiophene-Based Alternating Copolymers Synthesized by Heck Coupling Reaction

  • Shim, Hong-Ku;Taek Ahn;Lee, Hye-Young;Lee, Jeong-Ik
    • Macromolecular Research
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    • 제9권2호
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    • pp.116-121
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    • 2001
  • A series of poly(1,4-phenylenevinylene-alt-3-alkyl-2,5-thienylenevinylene)s (alkyl = hexyl [PPV-alt-6-TV] and octyl (PPV-alt-8-TV] group) have been synthesized by the Heck coupling reaction. These polymers were characterized using $^1$H-NMR, FT-IR spectroscopy, and thermogravimetric analysis (TCA). They are solvent processible and have obviously copolymeric structure. The photophysical properties of the polymers were investigated using UV-visible and steady-state photoluminescence(PL) spectroscopy. We studied the change of light-emitting properties by incorporating the thiophene group into the PPV polymer backbone using alternating copolymer system. The properties of two synthesized polymers are very similar, but they exhibited apparent changes of light-emitting properties compared with other PPV backbone based polymers. The broad absorption bands from 350 to 570 nm are due to $\pi$-$\pi$* transitions of the polyconjugated systems. The absorption maxima of the two polymers were found at about 452 and 448 nm for PPV-alt-6-TV and PPV-alt-8-TV, respectively. The copolymers showed broad PL spectra between 550 and 700 nm without vibronic bands and PL emission maxima of PPV-alt-6-TV and PPV-alt-8-TV are about 620 and 605 nm, respectively. The copolymers exhibited the red emission (PPValt-6-TV), but more red shifted emissions are needed to obtain real red color.

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A detailed study of physicochemical properties and microstructure of EmimCl-EG deep eutectic solvents: Their influence on SO2 absorption behavior

  • Zhu, Jiahong;Xu, Yingjie;Feng, Xiao;Zhu, Xiao
    • Journal of Industrial and Engineering Chemistry
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    • 제67권
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    • pp.148-155
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    • 2018
  • To get a better understanding of the effect of physicochemical properties and microstructure on $SO_2$ absorption behavior of DESs with different molar ratios of EmimCl and EG (from 2:1 to 1:2), densities (${\rho}$), viscosities (${\eta}$), speeds of sound (u), refractive indices ($n_D$), and thermal decomposition temperatures ($T_d$) of EmimCl-EG DESs were measured and used to obtain the other derived properties, such as thermal expansion coefficient (${\alpha}_p$) and activation energy for viscous flow ($E_{\eta}$). Moreover, FT-IR spectra and in situ variable-temperature NMR spectroscopy were employed to study the microstructures of DESs. Based on physicochemical and spectroscopic properties, the influence of the concentrations of EmimCl on the interactions in DESs was explored to be associated with their $SO_2$ absorption behavior. The results show that the interactions between $Emim^+$ and $Cl^-$ of EmimCl is gradually weakening with increasing the concentration of EG in DESs by forming of hydrogen bond interaction of $O-H{\cdots}Cl^-$, resulting in a decrease of ${\rho}$, ${\eta}$, u, $n_D$, and $T_d$ of DESs, and hindering the charge-transfer interaction of $SO_2$ with $Cl^-$ and deceasing $SO_2$ capture capacity. Moreover, the $SO_2$ absorption capacity of DESs is proportional to their ${\rho}$ and $E_{\eta}$, respectively.

유기태양전지를 위한 작은 밴드갭 고분자의 합성과 광전특성 (Synthesis and Photovoltaic Properties of a Low Band Gap Polymer for Organic Solar Cell)

  • 우용호;이효상;박성남;최이준;김봉수
    • 폴리머
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    • 제39권1호
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    • pp.71-77
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    • 2015
  • 본 연구에서는 전자가 풍부한 구조단위(dithienosilole 및 benzodithiophene)와 전자가 부족한 구조단위(difluorobenzothiadiazole)를 주사슬에 교대로 갖는 작은 밴드갭 공중합체를 Stille 짝지움 반응을 이용하여 합성하였다. $^1H$ NMR을 통하여 각 단계별 화합물과 고분자의 구조를 확인하였다. GPC, TGA, UV-vis 분광분석기 및 cyclic voltammetry를 이용하여 합성한 고분자의 특성을 조사하였다. 합성한 공액고분자와 $PC_{70}BM$을 1:1.5, 1:2, 1:3, 1:3.5 및 1:4의 중량비로 혼합하여 ITO/PEDOT:PSS/polymer:$PC_{70}BM/Al$의 구조로 유기태양전지 소자를 제작하여 그 광전특성을 조사하였다. 고분자:$PC_{70}BM$의 혼합비율이 1:3에서 최고 1.0%의 광전변환효율이 달성되었다. TEM 실험을 통하여 1:3 혼합비율에서 유기태양전지에 가장 적합한 나노규모로 상분리가 일어났으며, 다른 혼합비율에서는 고분자와 $PC_{70}BM$의 뭉침현상에 기인하여 태양전지 특성이 낮아졌다.

Comparison of Organic Carbon Composition in Profile by Using Solid 13C CPNMR Spectroscopy in Volcanic Ash Soil

  • Sonn, Yeon Kyu;Kang, Seong Soo;Ha, Sang Keun;Kim, Yoo Hak;Lee, Chang Hoon
    • 한국토양비료학회지
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    • 제46권5호
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    • pp.391-398
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    • 2013
  • Soil organic carbon (SOC) has the potential to promote the soil quality for sustainability and mitigation of global warming. There is little information on organic carbon composition despite of having resistance of carbon degradation in soil. In this study, to understand the effect of volcanic ash on organic carbon composition and quantity in soil, we investigated characteristics of volcanic soil and compared organic carbon composition of soil and humic extract by using $^{13}C$-CPMAS-NMR spectra under soil profiles of Namweon series in Jeju. SOC contents of inner soil profiles were 134.8, 101.3, and 27.4 g C $kg^{-1}$ at the layer of depth 10-20, 70-80 and 90-100 cm, respectively. These layers were significantly different to soil pH, oxalate Al contents, and soil moisture contents. Alkyl C/O-alkyl C ratio in soil was higher than that of humic extracts, which was decreased below soil depth. Aromaticity of soil and humic extract was ranged from 29-38 and 24-32%, which was highest at the humic extract of 70-80 cm in soil depth. These results indicate that the changes of SOC in volcanic ash soil resulted from alteration of organic composition by pyrolysis and stability of organic carbon by allophane in volcanic ash soil.