• Title/Summary/Keyword: $^{13}C-NMR$ Analysis

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토양-휴민의 물리화학적 특성 및 PAHs의 결합 특성 연구

  • Im Dong-Min;Sin Hyeon-Sang
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2006.04a
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    • pp.16-19
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    • 2006
  • 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, do-ashed humin was isolated from a soil sample after removing free lipid and alkali-soluble humic fractions followed by dissolution of mineral matrix with 2% HF, and characterized by elemental analysis, C-13 NMR spectroscopic method. Sorption behavior of 1-naphthol with humin was also investigated from aqueous solution. C-13 NMR spectra indicate that humin molecules are mainly made up of aliphatic carbon including carbohydrate, methylene chain etc.. Sorption intensity for 1-naphthol was increased as organic carbon content of humin increased and log Koc values for the 1-naphthol sorption were determined to be ${\sim}3.12$

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Structural Investigation of Lignins in Three Different Ferns (Pteridopbytes)

  • Choi, Joon-Weon
    • Journal of the Korean Wood Science and Technology
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    • v.29 no.3
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    • pp.83-91
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    • 2001
  • This paper examines the structural characteristics of fern lignins (deer fern (Blechnum spicant), sword fern (Polystichum munitum) and maidenhair fern (Adiantum pedatum)) by chemical degradation methods of thioacidolysis and nitrobenzene oxidation as well as 13C NMR. Phloroglucinol-HCI staining indicates that the lignins are specifically accumulated at the sclerenchyma cells beneath the epidermis and vascular bundles. The fern lignins consist of only guaiacyl units. Remarkably, the frequency of the -O-4 linkages is extremely low in fern lignins (only 9 to 11 %). Furthermore, the presence of lignin is ambiguous in maidenhair fern, due to very rare amount of -O-4 linkage. Biphenyl (5-5) and 1,2 bis arylpropane (-1) are main condensed dimeric substructures in fern lignins over 70%. In addition, 13C NMR analysis strongly evidenced the integration of phenolics or their derivatives into the fern lignins.

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Oxidative Addition Reaction of Mono(aryl)cyanoplatinum(Ⅱ) Complex with Two Amino Ligands with the Dihalogens

  • Ko Jaejung;Kim Moonsik;Kim Seho;Shin Yookil
    • Bulletin of the Korean Chemical Society
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    • v.13 no.2
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    • pp.135-139
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    • 1992
  • The mono(aryl)cyanoplatinum(II) complex $[Pt(CN)(C_6H_3{CH_2NMe_2}_2-26)]$, reacts with the dihalogens to yield the mono(aryl)cyanoplatinum complexes $[PtX_2(CN)(C_6H_3{CH_2NMe_2}_2-26)]$, (X = Cl, Br, I). The structural configuration of the two halogen atoms for a square planar platinum complex was studied by 1H-NMR spectroscopy and led to a mixture of trans and cis orientation. The trans orientation was found to be more stable in energy (1.33 kcal/mol) than the cis orientation by means of Extended H ckel calculations. On the base of a combination of the analysis of $^1H-NMR$, $^{13}C-NMR spectra and computational calculations it is assumed that the intermediate consists of an initial attack in the linear transition state, leading to the $S_{N}2$ type mechanism.

NMR Spectroscopy and Mass Spectrometry of Benzyl Alcohol Galactoside synthesized using β-Galactosidase (베타-갈락토시데이즈를 이용하여 합성된 Benzyl Alcohol Galactoside의 NMR Spectroscopy 및 Mass spectrometry)

  • Lee, Hyang-Yeol;Jung, Kyung-Hwan
    • Journal of the Korean Applied Science and Technology
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    • v.36 no.1
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    • pp.84-89
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    • 2019
  • To characterize the molecular structure of BzO-gal synthesized using Escherichia coli ${\beta}$-gal, NMR ($^1H$- and $^{13}C$-) spectroscopy and mass spectrometry of BzO-gal were conducted. $^1H$ NMR spectrum of BzO-gal showed multiple peaks corresponding to the galactosyl group, which is an evidence of galactosylation on BzOH. Five proton peaks around the aromatic region at ${\delta}_H$ 7.43 ~ 7.24 ppm and 2 peaks from ${\delta}_H$ 4.93 and 4.67 ppm were evidence of the presence of the benzyl group. Seven proton peaks at ${\delta}_H$ 4.32 ~ 3.46 ppm showed the presence of a monosaccharide and were indicative of galactosylation on BzOH. $^{13}C$ NMR spectrum also revealed the presence of 11 carbons suggestive of BzO-gal. The mass value (sodium adduct ion of BzO-gal, m/z = 293.0994) from mass spectrometry analysis of BzO-gal, and $^1H$ and $^{13}C$ NMR spectral data were in good agreement with the expecting structure of BzO-gal. We are expecting that through future study it will eventually be able to develop a new additive of low cytotoxicity.

Syntheses and Spectroscopic Studies of [$Cp_2ZrR]_2Fe(CO)_4$

  • Ko, Jae-Jung
    • Bulletin of the Korean Chemical Society
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    • v.7 no.6
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    • pp.413-421
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    • 1986
  • Hydrocarbon solution of $Cp_2Zr(CH_3)Cl$ react rapidly with $Na_2Fe(CO)_4$ (1/2 equiv.) to yield $[Cp_2Zr(CH_3)]_2Fe(CO)_4$ and NaCl. The more soluble metal-metal bonded complex $[Cp_2ZrC_8H_{17}]_2Fe(CO)_2$ has also been prepared through the reaction of $Cp_2Zr(C_8H_{17})BF_4$ and $Na_2Fe(CO)_4 (1/2 equiv.). The complexes were characterized by IR, $^1H$ NMR, ^{13}C$ NMR, and elemental analysis. The infrared spectrum of $[Cp_2ZrR]_2Fe(CO)_4$ shows four bands, which is indicative of a cis-structure. The $^{13}C$ NMR spectrum provides evidence for the cis-structure.

Construction of 19F-13C Solid-State NMR Probe for 400MHz Wide-Bore Magnet

  • Jeong, Ji-Ho;Park, Yu-Geun;Choi, Sung-Sub;Kim, Yongae
    • Journal of the Korean Magnetic Resonance Society
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    • v.17 no.2
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    • pp.81-85
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    • 2013
  • Various fluorine-containing materials are used in electronic devices like LCD display panels and Li-ion batteries. The structural conformation of fluorine in fluorinated materials is an important contributing factor that influences the chemical and physical properties. The conformation can be changed by heat and stress during manufacture or use. Understanding the conformational changes is critical for understanding the performance and durability of electronic devices. Solid-state NMR spectroscopy could be widely used for the analysis of various fluorine-containing materials for electronic devices. However, conventional CPMAS probes cannot be used for in-situ analysis of fluorine-containing electronic devices like LCD panels and Li-ion batteries. In this paper, we show the design, construction, and optimization of a $^{19}F-^{13}C$ double-resonance solid-state NMR probe for a 400MHz wide-bore magnet with a flat square coil for in-situ analysis of fluorine-containing electronic devices without observing fluorine background signals. This custom-built probe does not show any fluorine background signals, and can have higher efficiency for lossy samples.

Nuclear Magnetic Resonance (NMR)-Based Quantification on Flavor-Active and Bioactive Compounds and Application for Distinguishment of Chicken Breeds

  • Kim, Hyun Cheol;Yim, Dong-Gyun;Kim, Ji Won;Lee, Dongheon;Jo, Cheorun
    • Food Science of Animal Resources
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    • v.41 no.2
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    • pp.312-323
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    • 2021
  • The purpose of this study was to use 1H nuclear magnetic resonance (1H NMR) to quantify taste-active and bioactive compounds in chicken breasts and thighs from Korean native chicken (KNC) [newly developed KNCs (KNC-A, -C, and -D) and commercial KNC-H] and white-semi broiler (WSB) used in Samgye. Further, each breed was differentiated using multivariate analyses, including a machine learning algorithm designed to use metabolic information from each type of chicken obtained using 1H-13C heteronuclear single quantum coherence (2D NMR). Breast meat from KNC-D chickens were superior to those of conventional KNC-H and WSB chickens in terms of both taste-active and bioactive compounds. In the multivariate analysis, meat portions (breast and thigh) and chicken breeds (KNCs and WSB) could be clearly distinguished based on the outcomes of the principal component analysis and partial least square-discriminant analysis (R2=0.945; Q2=0.901). Based on this, we determined the receiver operating characteristic (ROC) curve for each of these components. AUC analysis identified 10 features which could be consistently applied to distinguish between all KNCs and WSB chickens in both breast (0.988) and thigh (1.000) meat without error. Here, both 1H NMR and 2D NMR could successfully quantify various target metabolites which could be used to distinguish between different chicken breeds based on their metabolic profile.

Complete assignments of $^{1}H$ and $^{13}C NMR$ spectra of Chivosazole F

  • Park, Jung-Rae;Jongheonn Shin;Kim, Jin-Cheol;Ahn, Jong-Woong
    • Journal of the Korean Magnetic Resonance Society
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    • v.5 no.2
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    • pp.91-98
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    • 2001
  • The $^1$H and $^{13}$ C NMR spectra of chivosazole F from Sorangium cellulosum were completely assigned by a combination of ID and 2D NMR techniques. The configurations of double bonds were confirmed from the ROESY spectra. The stereochemistry at asymmetric carboncenters was partially assigned on the basis of the results of NOE analysis.

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Pharmaceutical Application of FT-NMR (FT-NMR의 약학적(藥學的) 응용(應用))

  • Yu, Byung-Sul
    • Korean Journal of Pharmacognosy
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    • v.9 no.1
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    • pp.1-9
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    • 1978
  • The principle of Fourier Transform Nuclear Magnetic Resonance and its usefulness in the fields of pharmacy and biological sciences are described. 1. The $^1H\;and\;^{13}C$ NMR spectra of triostin A and its mixture with purine derivatives were taken. From the analysis of the spectra it has established that triostin A, which exists in two symmetric conformers in chloroform solution, forms complexes only with purine derivatives by the participation of one of the conformers. 2. Also, the $^{13}C$ NMR spectra of "intact" substances in the field of pharmacognosy were taken. From the spectra it was suggested that the method is very useful for natural product research in cooperation with the chemical method.

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Discoloration and the Effect of Antioxidants on Thermo-Oxidative Degradation of Polyamide 6 (폴리아미드 6의 열 산화반응에 의한 황변 현상과 산화방지제의 효과)

  • ;;;T. Mori
    • Polymer(Korea)
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    • v.26 no.4
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    • pp.452-461
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    • 2002
  • In this study, the effect of various concentrations of antioxidants on thermo-oxidative degradation of polyamide 6 was investigated. Unstabilized and stabilized polyamides 6 were subjected to long-term oven aging in ambient atmosphere at 70~$160^{\circ}C$. All of specimens were discolored within 100 hr at temperature range of 70~$160^{\circ}C$. Optimum antioxidant concentration was determined from the data of mechanical properties, yellowness index and relative viscosity. The synergistic effect of each primary and secondary antioxidant concentrations was not observed. Yellowing phenomenon was explained by using NMR, IR and EA. Different carbonyl groups were detected by $^{13}C$/NMR. During thermooxidative degradation, oxygen consumptions were determined by EA. The lifetime after long-term aging was predicted using Arrhenius equation.