• Title/Summary/Keyword: Carbon 13 NMR

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Synthesis and Analytical Application of Piperidine Dithiocarbamate Complex of Copper(II) (피페리딘 디티오카바메이트의 구리(II)의 착물합성과 분석적 응용)

  • Kim, Chan-Woo;Kim, Chang-Su
    • Analytical Science and Technology
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    • v.12 no.1
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    • pp.1-6
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    • 1999
  • Copper(II) complex of piperidine dithiocarbamate (Pipdtc) was synthesized from the reaction of Cu(II) and piperidine dithiocarbamate. The possible structure of the complex was proposed on the basis of elemental analysis, molar conductivity, infrared spectroscopy, electronic absorption spectroscopy, and $^{13}C-NMR$ studies. The extraction of copper(II)-Pipdtc complex by carbon tetrachloride can be achieved in the pH range of 6.0~10. The solution of copper(II) with piperidine dithiocarbamate was bey Beer's law in the concentration up to ${\sim}8.0{\times}10^{-5}M$ at pH 9.0.

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Equimolar Carbon Dioxide Absorption by Ether Functionalized Imidazolium Ionic Liquids

  • Sharma, Pankaj;Park, Sang-Do;Park, Ki-Tae;Jeong, Soon-Kwan;Nam, Sung-Chan;Baek, Il-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2325-2332
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    • 2012
  • A series $[C_3Omim]$[X] of imidazolium cation-based ILs, with ether functional group on the alkyl side-chain have been synthesized and structure of the materials were confirmed by various techniques like $^1H$, $^{13}C$ NMR spectroscopy, MS-ESI, FTIR spectroscopy and EA. More specifically, the influence of changing the anion with same cation is carried out. The absorption capacity of $CO_2$ for ILs were evaluated at 30 and $50^{\circ}C$ at ambient pressure (0-1.6 bar). Ether functionalized ILs shows significantly high absorption capacity for $CO_2$. In general, the $CO_2$ absorption capacity of ILs increased with a rise in pressure and decreased when temperature was raised. The obtained results showed that absorption capacity reached about 0.9 mol $CO_2$ per mol of IL at $30^{\circ}C$. The most probable mechanism of interaction of $CO_2$ with ILs were investigated using FTIR spectroscopy, $^{13}C$ NMR spectroscopy and result shows that the absorption of $CO_2$ in ether functionalized ILs is a chemical process. The $CO_2$ absorption results and detailed study indicates the predominance of 1:1 mechanism, where the $CO_2$ reacts with one IL to form a carbamic acid. The $CO_2$ absorption capacity of ILs for different anions follows the trend: $BF_4$ < DCA < $PF_6$ < TfO < $Tf_2N$. Moreover, the as-synthesized ILs is selective, thermally stable, long life operational and can be recycled at a temperature of $70^{\circ}C$ or under vacuum and can be used repeatedly.

A Study on the Correlations between Molecular Structures of Soil Humins and Sorption Properties of Phenanthrene (토양 휴민(Humin)의 분자구조 특성과 Phenanthrene 흡착상수와의 상관관계에 대한 연구)

  • Lee, Doo-Hee;Eom, Won-Suk;Shin, Hyun-Sang
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.12
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    • pp.897-905
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    • 2013
  • In this study, sorption coefficients (${\log}K_{OC}$, n) for the binding of phenanthrene (PHE) to soil humins, insoluble fraction of soil humc substances (HS), were determined and relationship between the sorption coefficients and structural characteristics of the soil humins were investigated. The soil humins used in the present study were isolated from 7 different soils including 5 domestic soils, an IHSS standard and a peat soil, and characterized by elemental analysis and CPMAS $^{13}C$ NMR method. $^{13}C$ NMR spectral features indicate that the soil humins are mainly made up of aliphatic carbons (57.1~72.3% in total carbon) with high alkyl-C moiety, and the alkyl-C contents ($C_{Al-H,C}$, %) was in order of granite soil Hu (26~42%) > volcanic ash soil, HL Hu (23.9%) > Peat Hu (14.0%). The results of correlation study show that a positive relationship ($r^2$ = 0.77, p < 0.05) between organic carbon normalized-sorption coefficients ($K_{OC}$, mL/g) and alkyl-C contents($C_{Al-H,C}$, %), while negative relationship ($r^2$ = (-)0.74, p < 0.05) between Freundlich sorption parameter (n) and H,C-substituted aromatic carbon contents ($C_{Ar-H,C}$, %). The magnitude of $K_{OC}$ values are also negatively well correlated with polarity index (e.g., PI, N + O)/C) ($r^2$ = (-)0.74, p < 0.1). These results suggest that the binding capacity (e.g., $K_{OC}$) for PHE is increased in soil humin molecules having high contents of alkyl-C or lower polarity, and nonlinear sorption for PHE increased as the H,C-substituted aromatic carbon contents ($C_{Ar-H,C}$, %) in the soil humins increased. The PHE sorption characteristics on soil humins are discussed based on the dual reactive mode of sorption model.

Cystocin, a Novel Antibiotic, Produced by Streptomyces sp. GCA0001: Production and Characterization of Cystocin

  • Sohng, Jae-Kyung;Lee, Hei-Chan;Liou, Kwang-Kyoung;Lee, Eui-Bok;Kang, Sun-Yub;Woo, Jin-Suk
    • Journal of Microbiology and Biotechnology
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    • v.13 no.4
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    • pp.483-486
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    • 2003
  • 3'-[S-Methyl-cysteinyl]-3'-amino-3'-deoxy-N,N- dimethyl adenosine, cystocin, is a biosynthesized antibiotic material newly identified from Streptomyces sp. GCA0001. Its structure was found to be similar to puromycin, where the terminal tyrosine is replaced by a methyl cysteine. NMR data prove that the 3-ammo ribose is connected to dimethylaminopurine through the anomeric carbon at 1'-carbon. The methyl cysteinyl unit is connected to the amino unit of ribose by peptide bond. The verification of the structure was performed by comparing the puromycin nucleosides resulted from the hydrolysis of cystocin and puromycin, respectively. Antibiotic activity of cystocin against Streptococcus was found to be two times more potent than that of puromycin.

Penicillium sp.-L4의 균성장 및 효소작용을 억제하는 $\beta$-glucosidase inhibitor의 분리 및 특성

  • Kim, Moo-Sung;Ha, Sung-Yoon;Jeon, Gi-Boong;Lim, Dal-Taek;Park, Byung-Hwa;Lee, Bo-Seop;Lee, Sang-Rin;Choi, Yong-Keel
    • Microbiology and Biotechnology Letters
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    • v.25 no.2
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    • pp.189-196
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    • 1997
  • A producer of inhibitor against ${\beta}-glucosidase$ of Penicillium sp.-L4 was screened from Actinomycetes, and the isolated strain was identified as Streptomyces sp. The inhibitor produced was very stable against heat, acidic and alkaline conditions, proteolytic and amylolytic enzymes. The inhibotor was purified from culture broth through activated carbon treatment, ultrafiltration, anion and cation exchange, activated carbon columm, acetone precipitation and preparative HPLC. It showed inhibitory activities against a variety of dissacharide hydrolyzing enzymes produced by P.sp.-L4, and the mode of inhibition was competitive. Its structure and molecular formular was elucidated by IR, $^1H\;and\;^{13}C$ NMR and FAB/Mass spectrometry, which was identified as 1-deoxynojirimycin (dNM). dNM showed inhibitory effects on the cell growth and hydrolytic enzyme action of P.sp.-L4 on agar plate and infected lemon peel.

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New Cryptand Complexes of Lanthanides(Ⅲ) and Dioxouranium(Ⅵ) Nitrates

  • Oh-Jin Jung;Chil-Nam Choi;Hak-Jin Jung
    • Bulletin of the Korean Chemical Society
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    • v.12 no.2
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    • pp.130-137
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    • 1991
  • The following new cryptand 221 complexes of lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate have been synthesized: $(Ln(C_{16}H_{32}N_2O_5)(H_2O)_2(NO_3)_3\ and \((UO_2)_2(C_{16}H_{32}N_2O_5)(H_2O)_4(NO_3)_4$. These complexes have been identified by elemental analysis, moisture titration, conductivity measurements and various spectroscopic techniques. The proton and carbon-13 NMR as well as calorimetric measurements were used to study the interaction of cryptand 221 with La(Ⅲ), Pr(Ⅲ ), Ho(Ⅲ) and $UO_2(Ⅱ)$ ions in nonaqueous solvents. The bands of metal-oxygen atoms, metal-nitrogen atoms and O-U-O in the IR spectra shift upon complexation to lower frequencies, and the vibrational spectra ({\delta}NMN$) of metal-amide complexes in the crystalline state exhibit lattice vibrations below 300 $cm^{-1}$. The NMR spectra of the lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate complexes in nonaqueous solvents are quite different, indicating that the ligand exists in different conformation, and also the $^1H$ and $^{13}C-NMR$ studies indicated that the nitrogen atom of the ring has greater affinity to metal ions than does the oxygen atom, and the planalities of the ring are lost by complexation with metal ions. Calorimetric measurements show that cryptand 221 forms more stable complexes with $La^{3+}$ and $Pr^{3+}$ ions than with $UO^{22+}$ ion, and $La^{3+}/Pr^{3+}$ and $UO^{22+}/Pr^{3+}$ selectivity depends on the solvents. These changes on the stabilities are dependent on the basicity of the ligand and the size of the metal ions. The absorption band (230-260 nm) of the complex which arises from the direct interaction of macrocyclic donor atoms with the metal ion is due to n-{\delta}*$ transition and also that (640-675 nm) of $UO^{22+}$-cryptand 221 complex, which arises from interaction between two-dioxouranium(Ⅵ) ions in being out of cavity of the ligand ring is due to d-d* transition.

Characterization of Glycine Metal Salts for $CO_2$ Absorption (이산화탄소 흡수를 위한 글리신 금속염의 특성 연구)

  • Lim, Yun-Hui;Park, Young Koo;Jo, Young-Min
    • Applied Chemistry for Engineering
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    • v.23 no.3
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    • pp.284-288
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    • 2012
  • This work deals with the chemical characterization of glycine aqueous solution in $CO_2$ absorption. Three alkali elements were impregnated into the glycine in order to facilitate the formation of amino functionalities. The analysis by IR revealed the transformation of ammonium ions to the amino group. In addition, the NMR analysis showed that the substitution of metal cations to the chemical shift of hydrogen and carbon atoms in glycine; in order of lithium glycinate, sodium glycinate and potassium glycinate depending on the electro negativity. Meanwhile, the $CO_2$ absorption at room temperature was the highest in primary amine solution, but at the increasing temperature sodium glycinate could capture more $CO_2$ than that of the pure amine solution.

Sorption of PAHs by Soil Humins and Effect of Soil Inorganic Matrixs (PAHs의 토양휴민과의 흡착특성 및 토양 무기물의 영향 해석)

  • Lim, Dong-Min;Lee, Seung-Sik;Shin, Hyun-Sang
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.12
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    • pp.1337-1346
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    • 2006
  • Soil humin is the insoluble fraction of humic materials and play an important roles in the irreversible sorption of hydrophobic organic contaminants onto soil particles. However, there have been limited knowledge about the sorption and chemical properties of humin due to the difficulties in its separation from the inorganic matrix(mainly clays and oxides). In this study, de-ashed soil humins($Hu_1-Hu_6$) were isolated from a soil residues(Crude Hu) after removing alkali-soluble organic fractions followed by consecutive dissolution of the mineral matrix with 2%-HF for 2 hr. The humin samples were characterized by elemental analysis and $^{13}C$ NMR spectroscopic method and their sorption-desorption behavior for 1-naphthol were investigated from aqueous solution. The results were compared one another and that with peat humin. $^{13}C$ NMR spectra features indicate that the soil humin molecules are mainly made up of aliphatic carbons(>80% in total carbon) including carbohydrate, methylene chain. Freundlich sorption parameter, n was increased from 0.538 to 0.697 and organic carbon-normalized sorption coefficient(log $K_{OC}$) values also increased from 2.43 to 2.74 as inorganic matrix of the soil humin removed by HF de-ashing. The results suggest that inorganic phase in humin plays an important, indirect role in 1-naphthol sorption and the effects on the sorption non-linearity and intensity are analyzed by comparison between the results of soil humin and peat humin. Sorption-desorption hysteresis were also observed in all the humin samples and hysteresis index(HI) at low solute concentration($C_e$=0.1 mg/L) are in order of Peat humin(2.67)>De-ashed humin(0.74)>Crude Hu(0.59).

Study of CO2 Absorption Characteristic and Synthesis of 1-(2-methoxyethyl)-3-methylimidazoLium Methanesulfonate Ionic Liquid (1-(2-methoxyethyl)-3-methylimidazolium Methanesulfonate 이온성 액체 합성 및 CO2 흡수 특성 연구)

  • Jin, Yu Ran;Jung, Yoon Ho;Park, So Jin;Baek, Il Hyun
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.35-40
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    • 2012
  • In this study, 1-(2-methoxyethyl)-3-methylimidazolium methanesulfonate ionic liquid has been synthesized, characterized and tested with respect to carbon dioxide absorption with the aim to use it as advanced absorbent materials in fossil fuel processing. The ionic liquid was synthesized by a one step method, low cost. The thermal and chemical stability of selected ionic liquid has been investigated by DSC, TGA and the structure was verified by $^1H$-NMR spectroscopy. The solubility of carbon dioxide in the methanesulfonate-based ionic liquids were measured using a high-pressure equilibrium apparatus equipped with a variable-volume view cell at 30, 50 and $70^{\circ}C$ and pressure up to 195 bar. The results show that carbon dioxide solubilities of 1-(2-methoxyethyl)-3-methylimidazolium methanesulfonate increased with pressure increasing and temperature decreasing, and the carbon dioxide absorption capacity showed 27.6 $CO_2/IL$(g/kg) at $30^{\circ}C$, 13 bar.

$^{13}C$ Spin-Lattice Relaxation Study of Segmental Motions in n-alkanes: n-Undecane and n-Dodecane

  • Min, Buem-Chan;Lee, Jo-Woong
    • Journal of the Korean Magnetic Resonance Society
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    • v.2 no.1
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    • pp.1-23
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    • 1998
  • The motions of carbon-chain backbone in n-undecance and n-dodecane dissolved in CDCl3 are investigated by 13C NMR relaxation study. For this purpose a model of C - C backbone motions for these molecules is introduced that takes into account the cooperativities between rotations about two $\beta$-coupled C - C bonds. In this model it is assumed that the major conformational interconversions occurring in the inner part of the chain involve the type II jumps only, although at terminal part of the chain both type II and type III motions are assumed to take place. Information of the rate constants of these conformational transitions could be extracted by comparing the T1's calculated on the basis of the assumed model with those observed over the temperature range of 248 - 308 K. The calculations were performed according to the method proposed by Wittebort and Szabo. The activation energies, ranging from ca 12 to 20 kJ/mol, could be obtained from the Arrhenius plots of these calculated rate constants.

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