• Title/Summary/Keyword: spectroscopic method

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Dehydration effects on spectroscopic properties of $Er^{+3}$ doped phosphate laser Glass ($Er^{+3}$ 첨가된 인산염 레이저 유리의 탈 수산기 영향에 관한 분광학적 특성)

  • Cho, Kou-Sung;Park, Wan-Soo;Kim, Jong-Su;Kim, Chong-Don
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.335-335
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    • 2008
  • Phosphate glass samples with various $Cr_2O_3$ and $Er_2O_3$ contents based upon $55P_2O_5\cdot24BaO\cdot10K_2O\cdot4Al_2O_3\cdot6Yb_2O_3$ were prepared. The prepared glass compositions are dehydrated using gas bubble flow method in open system and investigated the effects of the eliminating of OH groups from the glass melts with bubbling time. It was found that the probability of $Er^{+3}$ fluorescence quenching by OH groups oscillations linear depends upon the OH groups absorption coefficients in the maximum of the stretch vibrations band at $3500cm^{-1}$ while $Er^{+3}$ concentration range is between $1.6\times10^{19}$ and $21.2\times10^{19}$ ion/$cm^3$.

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Graphene/Multi-Walled Carbon Nanotubes Hybrid Materials for Supercapacitors

  • Lee, Bo-Reum;Chang, Dong Wook
    • Clean Technology
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    • v.21 no.1
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    • pp.62-67
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    • 2015
  • We have developed a versatile method for the preparation of chemically linked graphene/multi-walled carbon nanotubes (MWNTs) hybrid materials via simple acid-catalyzed dehydration reaction between graphene oxide (GO) and amine-functionalized MWNTs (af-MWNTs). In this condition, ketone (-C=O) groups in GO and primary amine (-NH2) moieties in af-MWNTs readily react to form imine (-C=N-) linkage. The chemical structures of graphene/MWNTs hybrid materials have been investigated using various microscopic and spectroscopic measurements. As a result of the synergetic effects of hybrid materials such as improved surface area and the superior structural restoration of graphitic networks, the hybrid materials demonstrate improved capacitance with excellent long-term stability. Furthermore, controlled experiments were conducted to optimize the weight ratio of graphene/MWNTs in hybrid materials. The highest capacitance of 132.4 F/g was obtained from the GM7.5 material, in which the weight ratio between graphene and MWNTs was adjusted to 7.5/1, in 1M KOH electrolyte at a scan rate of 100 mV/s.

Change of Flavonoid Composition in Scutellaria baicalensis by Processing (수치에 의한 황금의 성분변화)

  • 김장희;양기숙;김태희
    • YAKHAK HOEJI
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    • v.43 no.1
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    • pp.16-22
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    • 1999
  • Scutellaria baicalensis Georgi (Labiatae) has been extensively used in treatment of diarrhea, conjunctivitis, gastritis, enteritis and skin disease. As instructed in old description, the Scutellariae Radix should sometimes be processed before use. To 노디 light on the changes of chemical compositions by processing as well as processing method-activity relationships, Scutellariae Radix was heated at 16$0^{\circ}C$-20$0^{\circ}C$ for 30 min. in furnace or soaked with 20% EtOH (SPE) and boy's urine(SPU), respectively, which are one of processing methods and then heated at 17$0^{\circ}C$ for 30 min. To isolate the chemical components, Scutellariae Radix with/without processing were extracted with EtOH and EtOH extract was fractionated with ether, ethyl acetate and butanol to give respective fractions. Ether and EtOAc fractions obtained from the processed drug with urine (SPU) were subjected to chromatography to obtainsix components, oroxylin A, Wogonin, chrysin, baicalein, baicalein 7-O-$\beta$-D-glucopyranoside and $\beta$-sitosterol 3-O-$\beta$-D-glucopyranoside. All the isolated compounds were identified by means of physicochemical and spectroscopic methods (IR, $^1H-NMR,{\;}^13C-NMR$, Mass). By HPLC determination, the changes of the contents for each isolated components from SPE and SPU samples were observed. It was found that the content of nonglycosidic flavones such as oroxylin A, wogonin, chrysin and baicalein was increased markedly, whereas the content of baicalin and baicalein 7-O-$\beta$-D-glucopyranoside was significantly decreased in both samples as compared with those of Scutellariae Radix. When the sample was soaked with boy's urine, the total amount of nonglycosidic flavones was higher than that of processing with 20% EtOH.

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1D Proton NMR Spectroscopic Determination of Ethanol and Ethyl Glucuronide in Human Urine

  • Kim, Siwon;Lee, Minji;Yoon, Dahye;Lee, Dong-Kye;Choi, Hye-Jin;Kim, Suhkmann
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2413-2418
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    • 2013
  • Forensic and legal medicine require reliable data to indicate excessive alcohol consumption. Ethanol is oxidatively metabolized to acetate by alcohol dehydrogenase and non-oxidatively metabolized to ethyl glucuronide (EtG), ethyl sulfate (EtS), phosphatidylethanol, or fatty acid ethyl esters (FAEE). Oxidative metabolism is too rapid to provide biomarkers for the detection of ethanol ingestion. However, the non-oxidative metabolite EtG is a useful biomarker because it is stable, non-volatile, water soluble, highly sensitive, and is detected in body fluid, hair, and tissues. EtG analysis methods such as mass spectroscopy, chromatography, or enzyme-linked immunosorbent assay techniques are currently in use. We suggest that nuclear magnetic resonance (NMR) spectroscopy could be used to monitor ethanol intake. As with current conventional methods, NMR spectroscopy doesn't require complicated pretreatments or sample separation. This method has the advantages of short acquisition time, simple sample preparation, reproducibility, and accuracy. In addition, all proton-containing compounds can be detected. In this study, we performed $^1H$ NMR analyses of urine to monitor the ethanol and EtG. Urinary samples were collected over time from 5 male volunteers. We confirmed that ethanol and EtG signals could be detected with NMR spectroscopy. Ethanol signals increased immediately upon alcohol intake, but decreased sharply over time. In contrast, EtG signal increased and reached a maximum about 9 h later, after which the EtG signal decreased gradually and remained detectable after 20-25 h. Based on these results, we suggest that $^1H$ NMR spectroscopy may be used to identify ethanol non-oxidative metabolites without the need for sample pretreatment.

Preparation of Anatase TiO2 Thin Films with (OiPr)2Ti(CH3COCHCONEt2)2 Precursor by MOCVD

  • Bae, Byoung-Jae;Lee, Kwang-Yeol;Seo, Won-Seok;Miah, Md. Arzu;Kim, Keun-Chong;Park, Joon T.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.11
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    • pp.1661-1666
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    • 2004
  • The reaction of titanium tetraisopropoxide with 2 equiv of N,N-diethyl acetoacetamide affords Ti($O^iPr)_2(CH_3COCHCONEt_2)_2$ (1) as colorless crystals in 80% yield. Compound 1 is characterized by spectroscopic (Mass and $^1H/^{13}C$ NMR) and microanalytical data. Molecular structure of 1 has been determined by a single crystal X-ray diffraction study, which reveals that it is a monomeric, cis-diisopropoxide and contains a six coordinate Ti(IV) atom with a cis($CONEt_2$), trans($COCH_3$) configuration (1a) in a distorted octahedral environment. Variable-temperature $^1H$ NMR spectra of 1 indicate that it exists as an equilibrium mixture of cis, trans (1a) and cis, cis (1b) isomers in a 0.57 : 0.43 ratio at -20$^{\circ}C$ in toluene-$d_8$ solution. Thermal properties of 1 as a MOCVD precursor for titanium dioxide films have been evaluated by thermal gravimetric analysis and vapor pressure measurement. Thin films of pure anatase titanium dioxide (after annealing above 500$^{\circ}C$ under oxygen) have been grown on Si(100) with precursor 1 in the substrate temperature range of 350- 500$^{\circ}$ using a bubbler-based MOCVD method.

Mossbauer Spectroscopic Study of La2-2xSr2xCu1-xFexO4-y(0≤x≤0.5) Solid-solution

  • Park, Jung-Chul;Byeon, Song-Ho;Kim, Don;Lee, Choong-Sub
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.97-100
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    • 2004
  • Tetragonal $K_2NiF_4$-type $La_{2-2x}Sr_{2x}Cu_{1-x}Fe_xO_{4-y}$ solid-solution have been synthesized by citrate based sol-gel method. The valence state of iron was determined by Mossbauer spectroscopy and subsequent iodometric titration clearly showed that the copper ions in this solid-solution are in the mixed valence state Cu(II/III). When x ${\geq}$ 0.3, Fe(III) is competing with the mixture of Cu(II) and Cu(III) and $La_{2-2x}Sr_{2x}Cu_{1-x}Fe_xO_{4-y}$ exhibits a metallic character. No evidence for Cu(II)-O-Fe(IV) ${\leftrightarrow}$ Cu(III)-O-Fe(III) valence degeneracy was observed. In contrast, a small amount of Fe(IV) is observed with increasing x (x = 0.4 and 0.5), revealing a semiconducting behavior. These results suggest that the electronic interaction of Cu(III)-O-Fe(III) contributes greatly to the metallic character, while the electronic interaction of Cu(II)-O-Fe(IV) deteriorates the metallic character of $La_{2-2x}Sr_{2x}Cu_{1-x}Fe_xO_{4-y}$.

Study on optical emission spectroscopic method for measuring OH radical distribution in rocket plume (로켓 플룸 내부 OH 라디칼 공간분포 계측을 위한 발광 분광 기법에 관한 연구)

  • Han, Kiwook;Hahn, Jae W.
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2017.05a
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    • pp.1135-1139
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    • 2017
  • Spatial distribution of chemical species in flame is a important indicator understanding the flame structure and combustion characteristics, and optical emission spectroscopy has been widely used for the measurement because of its simple and non-intrusive methodology. In this study, we suggest the feasibility of the measurement of chemical species (OH radical) distribution in rocket plume using optical emission spectrometer which was developed for the spatially resolved measurement along the line-of-sight. In order to predict the ground state concentration of species from the measured emission intensity by optical emission spectrometer, we consider thermal and chemical excitation mechanisms in flame, and assume thermodynamic equilibrium for the thermally excited species. We also present the spatial resolution and the correction of collection characteristics of the optical emission spectrometer depending on object distance.

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Effect of Thermal Imidization and Curing on Fluorescence Behavior of a Phenylethynyl-Terminated Poly(amic acid)

  • Cho, Donghwan;Yang, Gyeongmo;Drzal, Lawrence T.
    • Macromolecular Research
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    • v.11 no.5
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    • pp.297-302
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    • 2003
  • The imidization and cure reaction of a thermosetting phenylethynyl-terminated amic acid (LaRC PETI-5) in film form have been monitored as a function of temperature by means of a steady-state fluorescence technique using a front-face illumination method. The variation of the fluorescence emission spectra of LaRC PETI-5 can be divided into four temperature regions; Region I: below 15$0^{\circ}C$, Region II: 150-25$0^{\circ}C$, Region III: 250-35$0^{\circ}C$, and Region IV: above 35$0^{\circ}C$. The fluorescence spectra in Region I are largely influenced by residual N-methyl-2pyrrolidinone in the polymer and also slightly by partial imidization of the polymer. There is a combined effect of imidization and solvent removal on the fluorescence behavior in Region II. The spectra in Regions III and IV are due significantly to the cure reaction of LaRC PETI-5 and to a post-cure effect of the polyimide, respectively. This spectroscopic evidence indicating the transformation of the amic acid imide oligomer into the corresponding polyimide via imidization and cure, agrees well with thermal analysis results obtained previously. The intermediate stage of cure in the range of 250-30$0^{\circ}C$ predominantly influences the change of the fluorescence intensity. The later stage above 30$0^{\circ}C$ significantly influences the position of the spectrum. This fluorescence study also supports the mechanism proposed in earlier work that the crosslinking reaction takes place at the reaction sites in the conjugated polyene and the phenylethynyl end group in the polyimide chain.

Six new dammarane-type triterpene saponins from Panax ginseng flower buds and their cytotoxicity

  • Li, Ke-Ke;Li, Sha-Sha;Xu, Fei;Gong, Xiao-Jie
    • Journal of Ginseng Research
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    • v.44 no.2
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    • pp.215-221
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    • 2020
  • Background: Panax ginseng has been used for a variety of medical purposes in eastern countries for more than two thousand years. From the extensive experiences accumulated in its long medication use history and the substantial strong evidence in modern research studies, we know that ginseng has various pharmacological activities, such as antitumor, antidiabetic, antioxidant, and cardiovascular system-protective effects. The active chemical constituents of ginseng, ginsenosides, are rich in structural diversity and exhibit a wide range of biological activities. Methods: Ginsenoside constituents from P. ginseng flower buds were isolated and purified by various chromatographic methods, and their structures were identified by spectroscopic analysis and comparison with the reported data. The 3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H- tetrazolium bromide method was used to test their cytotoxic effects on three human cancer cell lines. Results: Six ginsenosides, namely 6'-malonyl formyl ginsenoside F1 (1), 3β-acetoxyl ginsenoside F1 (2), ginsenoside Rh24 (6), ginsenoside Rh25 (7), 7β-hydroxyl ginsenoside Rd (8) and ginsenoside Rh26 (10) were isolated and elucidated as new compounds, together with four known compounds (3-5 and 9). In addition, the cytotoxicity of these isolated compounds was shown as half inhibitory concentration values, a tentative structure-activity relationship was also discussed based on the results of our bioassay. Conclusion: The study of chemical constituents was useful for the quality control of P. ginseng flower buds. The study on antitumor activities showed that new Compound 1 exhibited moderate cytotoxic activities against HL-60, MGC80-3 and Hep-G2 with half inhibitory concentration values of 16.74, 29.51 and 20.48 μM, respectively.

The Magnetic Properties of Polycrystalline Yttrium Iron Garnet by Ferromagnetic Resonance (강자성공명 현상을 이용한 YIG의 자기적 특성 연구)

  • 김기현;이대하;김영호
    • Journal of the Korean Magnetics Society
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    • v.9 no.1
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    • pp.7-16
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    • 1999
  • Stoichiometric and nonstoichiometric $Y_{3-x}Fe_{5+x}O_{12})$ polycrystalline samples (x=0.00, 0.05, 0.10, 0.30, -0.05, -0.10, -0.30) were prepared by solid state reaction method. The magnetic properties of the sample were investigated by FMR (ferromagnetic resonance) technique at microwave frequency 5.11 GHz (G-band) and 23.39 GHz (K-band) respectively. The spectroscopic splitting factor g were estimated to be 2.04~2.35 from the derivative absorption lines. As the samples became yttrium $(Y^{3+})$ excess and iron $(Fe^{3+})$ excess, Magnetizations were decreased. But resonance linewidth were increased. To investigate the anisotropy, the angular dependence of resonance magnetic fields were measured. Angular dependence of effective magnetizations were measured by FMR from 77 K to 300 K at K-band microwave frequency (23.39 GHz) and the saturation magnetizations were measured by VSM. The Bloch coefficients B and C were determined by fitting. $M_{eff}(0)$ was obtained by the extrapolation from 80 K. From this result, the spin wave stiffness constant D $(about\; 162~206 \;eV{\AA}^2)$and average square range of exchange interaction $$$(about \;5.84~12.13\;{\AA}^2)$ were determined.

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