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Arylation of Styrene by Palladium Acetate-Phosphine Complexes

  • 황박영애;황성원
    • Bulletin of the Korean Chemical Society
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    • v.18 no.2
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    • pp.218-221
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    • 1997
  • When phenylation of styrene was carried out in the presence of Pd(OAc)2 and PPh3 in benzene, trans-stilbene was obtained in good yield (566%) with high selectivity (98%) under mild condition (55 ℃, 50 psi O2, 20 h). Since trans-stilbene could be produced not only from benzene but also from phenyl group of PPh3 by migration of its phenyl group to Pd, the competitiveness of benzene and the migratory aptitude of aryl group of triarylphosphine toward styrene has been investigated with various phosphines (PR3: P(p-C6H4CH3)3, P(p-C6H4OCH3)3, P(p-C6H4F)3, P(p-C6H4Cl)3, P(C6H5)3, P(C6H11)3, P(OC4H9n)3, P(CH2C6H5)3 and P(C6F5)3). The yield and selectivity toward trans-stilbene are increased as the basicity of the phosphines increases. The composition of arylated olefin from arylphosphine, in turn, increases as the electronegativity of the substituent on the aryl group of arylphosphines increases.

A Study on Synthesis and Magnetic Properties of Soft Magnetic Materials Sintered at Low Temperature (저온 소결용 연자성 물질의 합성 및 자기적 특성 연구)

  • Koh Jae Gu
    • Resources Recycling
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    • v.12 no.6
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    • pp.13-18
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    • 2003
  • The initial NiCuZn synthetic ferrite were acquired from thermally decomposing the metal nitrates Fe($NO_3$)$_3$$9H_2$O, Zn($NO_3$)$_2$$6H_2$O, Ni($NO_3$3)$_2$$6H_2$O and Cu(NO$_3$)$_2$$3H_2$O at 1$50^{\circ}C$ for 24 hours and was calcined at $500^{\circ}C$. Each of those was pulverized for 3 and 9 hours in a steel ball mill and was sintered between $700^{\circ}C$ and $1,000^{\circ}C$ for 1 hour, and then their microstructures and magnetic properties were examined. We could make the initial specimens chemically bonded in liquid at the temperature as low as $150 ^{\circ}C$, by using the melting points less than $ 200^{\circ}C$ of the metal nitrates instead of the mechanical ball milling, then narrowed a distance between the particles into a molecular level, and thus lowed sintering temperature by at least $200 ^{\circ}C$ to $300^{\circ}C$ Their initial permeability was 50 to 490 and their saturation magnetic induction density and coercive force 2,400G and 0.3 Oe to 1.2 Oe each, which were similar to those of NiCuZn ferrite synthesized in the conventional process.

Kinetics of pH Changes during Thermal Degradation of MSG under Model System (Model System 하에서 MSG 열분해 중 pH 변화의 속도론적 연구)

  • Cha, Bo-Sook;Han, Min-Soo;Kim, Woo-Jung
    • Korean Journal of Food Science and Technology
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    • v.24 no.3
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    • pp.232-235
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    • 1992
  • Effect of temperature and initial pH were studied on the pH change of MSG solution during heating. The heating temperature and initial pH of 2% MSG solution were in the range of $100{\sim}120^{\circ}C$ and $pH\;2{\sim}9$, respectively. The results showed that the pH of MSG solution was more rapidly decreased as the temperature increased and the initial pH decreased due to pyroglutamic acid formation from MSG thermal degradation. A linear relationship was obtained between pH decreased and logarithmic value of heating time and the decreasing rate constant of pH were calculated from the slope. The pH decreased$({\Delta}pH)$ after 3 hrs of heating was 1.2 at the initial pH 4 and $120^{\circ}C$ and 0.33 at pH 5 and $120^{\circ}C$ while little pH change measured at the range of $pH\;6{\sim}9$. Activation energy calculated for pH decrease during heating was 11.77 and 22.26 kcal/mole at pH 4 and pH 5, respectively.

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Effect of Polar Organic Substance on Cutting Mechanism (極性有機物質이 切削機構에 미치는 影響)

  • 서남섭;양균의
    • Transactions of the Korean Society of Mechanical Engineers
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    • v.10 no.1
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    • pp.131-137
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    • 1986
  • Cutting oil cools the chip and a tool as well as lubricates the chip-tool interface, the flank and machined surface. Rehbinder effect has been known as a phenomenon, the reduction of mechanical strength, when the metal is exposed to a polar organic environment or the surface of metal is coated with some polar organic substances. About the cause of Rehbinder effect there have been many different ideas by Rehbinder, Shaw, Barlow, Sakida and etc. In this report, the efect of polar organic substance( $C_{6}$ $H_{5}$C $H_{3}$+ $C_{6}$ $H_{4}$(C $H_{3}$)$_{2}$+ $C_{4}$ $H_{9}$OH+ $C_{6}$ $H_{12}$ $O_{2}$) (magic ink) upon the mechanism of chip formation on the orthogonal cutting of copper and mechanical properties of the work material are experimentally discussed with various rake angles. As expected no lubrication action could be noticed, but the shear angle increased and the cutting force and shear strain on the shear plane decreased, therefore the work material must be embrittled under polar organic substance.substance.

Variation in the Nanostructural Features of the nc-Si:H Thin Films with Substrate Temperature (수소화된 나노결정 실리콘 박막의 기판온도에 따른 나노구조 변화)

  • Nam, Hee-Jong;Son, Jong-Ick;Cho, Nam-Hee
    • Korean Journal of Materials Research
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    • v.23 no.7
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    • pp.359-365
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    • 2013
  • We investigated the nanostructural, chemical and optical properties of nc-Si:H films according to deposition conditions. Plasma enhanced chemical vapor deposition(PECVD) techniques were used to produce nc-Si:H thin films. The hydrogen dilution ratio in the precursors, [$SiH_4/H_2$], was fixed at 0.03; the substrate temperature was varied from room temperature to $600^{\circ}C$. By raising the substrates temperature up to $400^{\circ}C$, the nanocrystalite size was increased from ~2 to ~7 nm and the Si crystal volume fraction was varied from ~9 to ~45% to reach their maximum values. In high-resolution transmission electron microscopy(HRTEM) images, Si nanocrystallites were observed and the crystallite size appeared to correspond to the crystal size values obtained by X-ray diffraction(XRD) and Raman Spectroscopy. The intensity of high-resolution electron energy loss spectroscopy(EELS) peaks at ~99.9 eV(Si $L_{2,3}$ edge) was sensitively varied depending on the formation of Si nanocrystallites in the films. With increasing substrate temperatures, from room temperature to $600^{\circ}C$, the optical band gap of the nc-Si:H films was decreased from 2.4 to 1.9 eV, and the relative fraction of Si-H bonds in the films was increased from 19.9 to 32.9%. The variation in the nanostructural as well as chemical features of the films with substrate temperature appears to be well related to the results of the differential scanning calorimeter measurements, in which heat-absorption started at a substrate temperature of $180^{\circ}C$ and the maximum peak was observed at ${\sim}370^{\circ}C$.

Characterization of Bacteriocin from Bacillus subtilis cx 1 (Bacillus subtilis cx1이 생산하는 박테리오신의 특성)

  • 김수인;장지윤;김인철;장해춘
    • Microbiology and Biotechnology Letters
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    • v.29 no.1
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    • pp.50-55
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    • 2001
  • A new bacteriocin produced by Bacillus subtilis cx1, was partially purified and characterized. The bactericoin from B. subtilis cx1 was stable in the range of pH 2.5-9.5. B. subtilis csx1 retained its antimicrobial activity to long-term exposure at $-20^{\circ}C$ and $-70^{\circ}C$. However, B. subtilis cx1 was inactivated completely within 15 min over $60^{\circ}C$ and lost 50% of its antimicrobial activity within 15 min at $50^{\circ}C$, B. subtilis cx1 was inactivated by protease, trypsin, proteinase K and carboxypeptidase, which indi-cates its protein nature. Direct detection of the antimicrobial activity on Tricine -SDS-PAGE suggested an apparent molecular mass of about 9,500 dalton.

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Discovery of C2 Swan Band and CN emission in Spark Discharge Experiment

  • Song, In-Ok;Mo, Younghoon;Ryu, Jein;Chang, Hoyon;Hwang, Ki-Wook;Chun, Man-Seog;Oh, Jinho;Hahn, Sangjoon
    • The Bulletin of The Korean Astronomical Society
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    • v.46 no.2
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    • pp.74.1-74.1
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    • 2021
  • 밀러-유리 실험으로 알려진 전기방전 실험은 지구초기대기를 모사하여 아미노산을 합성하여, 지구에서 생명의 기원을 연구하는 실험중의 하나이다. 메탄(CH4), 암모니아(NH3), 질소(N2) 가스를 주입하고 전기방전으로 에너지를 가했다. 그 결과 용액에서는 아미노산인 글라이신(C2H5NO2), 알라닌(C3H7NO2), 히스티딘(C6H9N3O2), 프롤린(C5H9NO2), 발린(C5H11NO2)이 검출되었고, 기존 Miller 1953과 Parker et al. 2014의 결과와 비교하였다. 전기방전에서는 C2 Swan Band 와 CN emission을 발견하였다. 이 두 방출선들은 혜성에서도 일반적으로 보여지는 방출선들이다.

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Low resistivity Ohmic Co/Si/Co contacts to n-type 4H-SiC (낮은 접촉 저항을 갖는 Co/Si/co n형 4H-SiC의 오옴성 접합)

  • Kim, C.K.;Yang, S.J.;Lee, J.H.;Cho, N.I.;Jung, K.H.;Kim, N.K.;Kim, E.D.;Kim, D.H.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.07b
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    • pp.764-768
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    • 2002
  • Characteristics of ohmic Co/Si/Co contacts to n-type 4H-SiC are investigated systematically. The ohmic contacts were formed by annealing Co/Si/Co sputtered sequentially. The annealings were performed at $800^{\circ}C$ using RTP in vacuum ambient and $Ar:H_2$(9:1) ambient, respectively. The specific contact resistivity$(\rho_c)$, sheet resistance$(R_s)$, contact resistance$(R_c)$, transfer length$(L_T)$ were calculated from resistance$(R_T)$ versus contact spacing(d) measurements obtained from TLM(transmission line method) structure. While the resulting measurement values of sample annealed at vacuum ambient were $\rho_c=1.0{\tiimes}10^{-5}{\Omega}cm^2$, $R_c=20{\Omega}$ and $L_T$ = 6.0 those of sample annealed at $Ar:H_2$(9:1) ambient were $\rho_c=4.0{\tiimes}10^{-6}{\Omega}cm^2$, $R_c=4.0{\Omega}$ and $L_T$ = 2.0. The physical properties of contacts were examined using XRD and AES. The results showed that cobalt silicide was formed on SiC and Co was migrated into SiC.

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Histopathological study of acute toxicity of ammonia to the eel, Anguilla japonica in high temperature and pH levels (고수온(高水溫) 고(高)pH에서 뱀장어에 미치는 암모니아 급성독성(急性毒性)의 병리조직학적(病理組織學的) 연구(硏究))

  • Kim, Min-Soo;Yang, Han-Choon
    • Journal of fish pathology
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    • v.9 no.2
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    • pp.147-155
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    • 1996
  • This study was carried out to examine the acute toxic effects of ammonia to the eel, Anguilla japonica in high temperature and pH levels by histopathological observations. The eels of 40 g average body weight were exposed to 4 different concentrations of total ammonia (0, 10, 20, 30 mg/$\ell$) for 24~120 hours. Each concentration was treated under 4 different levels of pH (7.5, 8.0, 8.5, 9.0) and each of these treatments was tested at 2 different temperatures ($27^{\circ}C$, $32^{\circ}C$). Histopathological changes in gill tissues were observed by hematoxylin-eosin stain. As increasing of pH (from 7.5 to 9.0), water temperature (from $27^{\circ}C$ to $32^{\circ}C$), total ammonia concentration (from 0 mg/$\ell$ to 30 mg/$\ell$) and exposure time (from 24 hours to 120 hours), gill discolorated to dark brown with the naked eye and gill tissues showed hypertrophy of gill lamellae, winding of the secondary gill lamellae, epitherial separation and necrosis histopathologically. When gill lamellae epithelium was separated from the blood vessels, gill discolorated to dark brown with the naked eye.

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The Crystal and Molecular Structure of Fenothiocarb, $C_{13}H_{19}NO_2S$. (Fenothiocarb, $C_{13}H_{19}NO_2S$의 결정 및 분자구조)

  • 박권일;조성일
    • Korean Journal of Crystallography
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    • v.6 no.2
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    • pp.63-68
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    • 1995
  • The crystal structure of fenothiocarb(S-4-phenoxybutyl dimethylthiocarbamate), C13H19NO2S is monoclinic, space group P21/c, a=9.045(1)Å, b=14.577(2)Å, c=10.727(2)Å, β=103.56(1)°, Z=4, V=1375.20(6)Å3, Dc=1.23g/cm3, λ(Mo-Kα)=0.71069Å, μ=2.3cm-1, F(000)=544, temperature : 293±3K, R=0.049 for 1543 unique observed reflections. The structure was determined by direct method and refined by full-matrix least squares method. The molecules are contacted to the c axis with two fold screw and van der Waales force.

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