• Title/Summary/Keyword: 0.1N HCl

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Synthesis and Characterization of New Polyaza Macrocyclic Nickel(Ⅱ) and Copper(Ⅱ) Complexes Two Nitrile or Imidate Ester Pendant Arms: Metal-Mediated Hydrolysis and Alcoholysis of the Nitrile Groups

  • Kang, Shin-Geol;Song, Jeong-Hoon;Jeong, Jong-Hwa
    • Bulletin of the Korean Chemical Society
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    • v.23 no.6
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    • pp.824-829
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    • 2002
  • New di-N-cyanomethylated tetraaza macrocycle 2.13-bis(cyanomethyl)-5.16-dimethyl-2,6,13,17-tetraazatricyclo[$16.4.0.0^7.12$]docosane $(L^2)$ has been prepared by the reaction of 3, 14-dimethyl-2,6,13,17-tetraazatricyclo $(L^1)$ with bromoacetonitrile. The square-planar complexes $[ML^2](ClO_4)_2(M=Ni(II)$ or Cu(II) can be prepared by the reaction of $L^2$ with the corresponding metal ion in acetonitrile. The cyanomethyl groups of $[ML^2](ClO_4)_2readily$ react with water to $yield[ML^3](ClO_4)_2$ containing pendant amide groups. The trans-octahedral complexes $[ML^4](ClO_4)_2$, in which two imidate ester groups are coordinated to the metal ion, can be also prepared by the reaction of $[ML^2](ClO_4)_2with$ methanol under mild conditions. The hydrolysis and alcoholysis reactions of $[ML^2](ClO_4)_2are$ promoted by the central metal ion, in spite of the fact that the cyanomethyl group is not involved in intramolecular coordination. The reactions are also promoted by a base such as triethylamine but are retarded by an $acid(HClO_4).Interestingly$, the imidate ester groups of $[ML^4]^2$ are unusually resistant to hydrolysis even in 0.1 M $HCIO_4$ or 0.1 M NaOH aqueous solution. Crystal structure of $[NiL^4](ClO_4)_2shows$ that the Ni-N (pendant imidate ester group) bond is rlatively strong; the Ni-N bond distance is shorter then the Ni-N(tertiary) distance and is similar to the Ni-N (secondary) distance.

Synthesis of a Di-N-cyanoethylated Tetraaza Macrocycle Containing Eight C-Methyl Groups and Its Nickel(II) Complex: Effects of the Methyl Groups on Their Properties

  • Kang, Shin-Geol;Ryu, Ki-Seok;Kim, Jin-Kwon
    • Bulletin of the Korean Chemical Society
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    • v.23 no.1
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    • pp.81-85
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    • 2002
  • A new di-N-cyanoethylated 14-membered tetraaza macrocycle 1,8-bis(2-cyanoethyl)-3,5,7,7,10,12,14,14-octamethyl-1,4,8,11-tetraazacyclotetradecane $(L^2)$ and its nickel(II) complex $[NiL^2(OAc)]^+$ have been prepared. The square-planar complex $[NiL^2](C IO_4)_2$ can be prepared by addition of $HClO_4$ to a hot aqueous solution of $[NiL^2(OAc)]^+$ The Ni-N (tertiary amino group) bond distances $(2.008{\AA})$ of $[NiL^2](C IO_4)_2$ are relatively long, and the complex exhibits a d-d transition band at unusually long wavelength (ca. 515 nm). The complex $[NiL^2](C IO_4)_2$ rapidly reacts with acetate ion or ethylenediamine (en) to produce $[NiL^2(OAc)]^+$ or [Ni(en)_3]^{2+}$, respectively, and is readily decomposed in NaOH (0.01 M) solution. The chemical properties of $[NiL^2]^{2+}$ as well as its synthetic procedure are quite different from those for other related 14-membered tetraaza macrocyclic complexes. Effects of the N-cyanoethyl and C-methyl groups on the properties of $L^2$.

Antibacterial Effect of Porous Glass Ceramics as Ag Ion Exchange in Phosphate System (Phosphate계 다공성 글라스 세라믹스의 $Ag^+$ 이온교환에 따른 항균 효과)

  • 윤영진;이용수;강원호
    • Journal of the Korean Ceramic Society
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    • v.38 no.11
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    • pp.1055-1059
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    • 2001
  • Porous glass ceramics composed of Li$_2$O.-Ti $O_2$-P$_2$ $O_{5}$ -CaO were prepared by melting and 2 step heat treatment for nucleation at 61$0^{\circ}C$ and crystallization at 78$0^{\circ}C$. subsequently $\beta$-Ca$_3$(P $O_4$)$_2$crystal phase was selectively leached out in 1N-HC1 solution for 3 days, leaving Li $Ti_2$(P $O_4$)$_3$crystal phases. prepared porous glass ceramics were immersed in 1M AgN $O_3$solution for ion exchange. Staphylococcus aureus and salmonella typhi were used in this study. It was found taht the resultant porous glas ceramics show excellent bacteriostatic properties.

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GaN 위에 electron beam evaporator로 증착시킨 ITO contactd의 구조적 특성 및 전기적 특성 평가

  • 김동우;성연준;이재원;박용조;김태일;김현수;염근영
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.33-33
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    • 2000
  • 일반적으로 GaN-based light emitting diodes(LEDs)는 Top layer위에 금속박막으로 contact을 형성하고 있으며 광소자 구성에 있어 빛은 이러한 금속 contact을 통과할 수 없다. 그러나 만약 이러한 contact이 투명전도막으로 구성될 수 있다면 보다 효율적인 광소자의 구성이 기대되어진다. 특히 GaN photodetector, GaN-based LEDs, GaN vertical cavity surface emitting lasers(VCSELs)등의 소자형성에 있어 투명전도막 contact은 매우 중요하며 그 응용에 앞서 기본적인 구조적, 전기적, 광학적 특성에 대한 연구가 반드시 선행되어져야 한다. 따라서 본 실험에서는 이러한 투명전도막으로써 Indium Tin Oxide(ITO)를 사용하였으며 박막형태의 contact으로 제조하여 n-GaN, p-GaN와 corning glass위에 e-beam evaporation법로써 제조하였다. 또한 각 n-, p-type과 corning glass위에 증착된 ITO박막의 구조적 특성을 분석하기 위하여 x-ray diffractometry(XRD)와 Auger electron spectroscopy(AES)등을 사용하였으며 전기적 특성을 측정하기 위하여 four point probe를 사용하였고 그들의 I-V 곡선을 측정하였다. 또한 UV spectrometry를 사용하여 그들의 광학적 특성을 측정하고자 하였다. ITO 박막의 제조에 있어 기판은 초음파 유기세정 후 HCl과 H2O2(1:1)의 혼합용액을 사용하여 GaO2를 제거하고자 하였으며 이후 초순수로 세척하여 사용하였다. 초기 진공도는 3$\times$10-5 Torr이하였으며 기판온도 50$0^{\circ}C$에서 0.6 /s의 증착속도로 약 2000 증착하였다. 이렇게 제조된 ITO 박막은 5$\times$10-5 Torr이하의 진공분위기에서 $600^{\circ}C$로 열처리를 실시하였으며 열처리 시간의 변화에 따른 그들의 전기적, 구조적, 광학적 특성을 측정하였다. 열처리 과정을 통한 ITO박막은 투과도는 420nm의 영역에서 80%이상을 나타내었으며 이때의 면저항은 약 50ohm/ 이었다. 또한 I-V 곡선 측정에 의한 contact특성의 측정결과 열처리 전의 ITO contact은 n-GaN와 n-GaN에 대해 각각 ohmic과 schottky contact의 일반적인 contact 특성을 나타내었다. 그러나 이러한 contact 특성은 열처리 시간의 변화에 따라 변화하는 것을 확인할 수 있었다.

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A Study for Kinetics and Oxidation Reaction of Alcohols by Cr(VI)-4-(Dimethylamino)pyridine (크롬(VI)-4-(Dimethylamino)pyridine에 의한 알코올류의 산화반응과 반응속도에 관한 연구)

  • Kim, Young-Sik;Park, Young-Cho;Kim, Young Jun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.14 no.1
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    • pp.499-505
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    • 2013
  • Cr(VI)-4-(dimethylamino)pyridine[4-(dimethylamino)pyridinium chlorochromate] was synthesized by the reaction of 4-(dimethylamino)pyridine with chromium trioxide in 6M-HCl, and characterized by IR, ICP. The oxidation of benzyl alcohol using 4-(dimethylamino)pyridinium chlorochromate in various solvents showed that the reactivity increased with the increase of the dielectric constant(${\varepsilon}$), in the order: cyclohexene$H_2SO_4$ solution), 4-(dimethylamino)pyridinium chlorochromate oxidized benzyl alcohol and its derivatives(p-$OCH_3$, m-$CH_3$, H, m-$OCH_3$, m-Cl, m-$NO_2$) smoothly in DMF. Electron-donating substituents accelerated the reaction, whereas electron acceptor groups retarded the reaction. The Hammett reaction constant(${\rho}$) was -0.68(303K). The observed experimental data was used to rationalize the hydride ion transfer in the rate-determining step.

The Acid Sensitivity of Gulose and Mannose in Chemically-Reduced Alginates Obtained from Pseudomonas syringae

  • Ashby, Richard D.;Day, Donal F.;Kim, Du-Woon
    • Food Science and Biotechnology
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    • v.15 no.4
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    • pp.555-558
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    • 2006
  • The chemical reduction of Pseudomonas syringae subsp. phaseolicola alginates produces neutral polymers of D-mannose and L-gulose in source specific ratios. L-Gulose was highly sensitive to degradation by 1N HCl at $100^{\circ}C$. As hydrolysis time increased, gulose recovery decreased to 22% after 4 hr, whereas 98% of the D-mannose was recovered under the same conditions. Thin layer chromatography showed the formation of a second product upon L-gulose acid hydrolysis. This new product had a rate of flow (Rf) value of 0.58, identical to that of 1,6 anhydro-${\beta}$-D-mannopyranose and very close to that of 1,6 anhydro-${\beta}$-D-glucopyranose (Rf=0.60). Because of the difference in acid sensitivity between L-gulose and D-mannose, normal acid hydrolytic techniques applied to reduced alginates produces erroneous mannuronic acid (M): guluronic acid (G) ratio's unless one accounts for the differential rates of destruction of each sugar.

Purification and Chemical Characterisation of Laminaran from Eisenia bicyclis in Korea (대황(Eisenia bicyclis)으로부터 Laminaran의 정제 및 화학적 특성)

  • Kim, Young-Myoung;Choi, Yong-Seok;Park, Jong-Hyuk
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.35 no.1
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    • pp.78-86
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    • 2006
  • Laminarans with different purity were prepared from Eisenia bicyclis and their structures were characterized. Crude laminaran was successively extracted two times at room temperature for 2 hr with 0.09 N HCl, and partially purified laminaran was isolated using cetylpyridinium chloride (CPC). Crude laminaran accounted for $14.5\%$ of the dry seaweed weight and contained $8.4\%$ protein, $7.6\%$ sulfate and $68.2\%$ polysaccharide. Partially purified laminaran accounted for $6.5\%$ of the dry algal weight and composed of $3.8\%$ protein, $3.2\%$ sulfate and $74.7\%$ total sugar, which is mainly composed of glucose $(83.3\%)$, indicating that partially purified laminaran was more purified polysaccharide than crude laminaran. Purified laminaran was fractionated into one fractions by Sephacryl S-300 HR column chromatography and this fraction was analysed by FT-IR, $^{13}C$ NMR, methylation and gel filtration chromatography. Purified laminaran showed $\beta-configuration$ $(^{13}C:103.0ppm,\;FT-IR:888cm^{-1})$ in the anomerization of the glycosidic linkages and was $(1\rightarrow3),\;(1\rightarrow6)$ linked $\beta-glucan$. The average molecular weight of purified laminaran was 12,600 dalton.

Pullulan Production from Starch Hydrolysate by Aureobasidium pullulans SH8646

  • Shin, Yong-Chul;Kim, Tae-Un
    • Journal of Microbiology and Biotechnology
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    • v.3 no.4
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    • pp.298-302
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    • 1993
  • Pullulan was produced from starch hydrolysate with Aureobasidium pullulans SH8646. We could measure the correct amount of pullulan produced without the interference of starch from the culture supernatant by using a bacterial $\alpha$-amylase treatment and ethanol: acetone (1:1) precipitation. When 5% acid-hydrolyzed starch was used as a carbon source, the dry cell weights obtained were similar irrespective of DE values of starch hydrolysates. The dry cell weights of those on the starch hydrolysate media prepared with 0.1 N HC1 treatment, were slightly higher (9.5~10.5 g/l) than those on the starch hydrolysate media prepared with 1.0 N HCl (8.5~9.5 g/l). And among the starch hydrolysates showing DE values lower than 50, maximum pullulan production of 15 g/l was obtained at DE 30~40 starch hydrolysate but those showing DE values higher than 50, the pullulan production was increased with the increase of the DE value of starch hydrolysates. From the media containing 5%, 10%, and 15% starch hydrolysate (DE 25, 45, and 75), about 20~34% pullulan yield was obtained and the maximum pullulan yield of 34% (17g/l) was obtained from 5% DE 75 starch hydrolysate. The pullulan yields from starch hydrolysate media were much lower than those from glucose, maltose, maltotriose, and sucrose media.

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The measurement of dicamba in soil and plants (토양 및 식물 중 디캄바 측정법에 대한 연구)

  • Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.480-487
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    • 2009
  • The herbicide dicamba (2-methoxy-3,6-dichlorobenzoic acid) in soil and plants was determined by gas chromatography-mass spectrometry (GC/MS). The samples were extracted with diethyl ether at pH 2, and washed with 0.1 N HCl, and then dried. The dried residue was derivatized in 1 mL of 10% $H_2SO_4$-MeOH for 2 hr at $80^{\circ}C$. The reaction mixture was neutralized with 4 mL of sodium bicarbonate solution and reextracted with 5 mL of diethyl ether. After the extract was concentrated, dicamba was determined by GC/MS-SIM mode. There was good linearity above 0.999 in the ranges of the $1.0{\sim}100{\mu}g/kg$. Total 42 sample including 32 soil samples and 10 plants samples were analyzed by developed method. Dicamba was detected in the concentration range of $2.9-123.9{\mu}g/kg$ in 15 samples among 32 soil samples and in the concentration range of $43-33,252{\mu}g/kg$ in 5 samples among 10 plants samples. A cause of the wither and die of the pine trees is suspected to spray dicamba around or directly to them.

Relationship between pH and colloidal stability of three Hawaii soils (3종류의 하와이 토양의 pH와 토양분산도와의 관계)

  • Lim, Soo-Kil H.
    • Korean Journal of Soil Science and Fertilizer
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    • v.24 no.2
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    • pp.95-101
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    • 1991
  • The results of relationships between colloidal stability and soil pH on three Hawaii's volcanic ash soils developed under the three different rainfall conditions can be summarized as follows: 1. The Hilo soil only revealed the increase of colloidal stability by becoming for from Z.P.C point to either side of pH. 2. Hilo and Kawaihae soils, however, showed the increase of colloidal stability only in the higher pH range than their Z.P.C. 3. $P_2O_5$ drying procers decreased colloidal stability kof these soils because of so called irreversible drying characteristics of amorphous materials and the decrement was in order of: Akaka>Hilo>Kawaihae expressing positive correlation with content of amorphous materials in them. 4. The difference of colloidal stability curves among three soils can easily be interpreted by DLVO theory considering 0.1N-HCl amount added to decrease their soil pH, respectively. The addition of large amount of 0.1N-HCl into Akaka and Kawaihae soils did not effectively develop the positive charge but resulted in the shrink of diffuse double layer thickness inducing large attraction forces among soil particles.

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