• Title/Summary/Keyword: Mass spectroscopy

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Identification of New Urinary Metabolites of Byakangelicin, a Component of Angelicae dahuricae Radix, in Rats

  • Kwon, Oh-Seung;Song, Yun-Seon;Shin, Kuk-Hyun;Ryu, Jae-Chun
    • Archives of Pharmacal Research
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    • v.26 no.8
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    • pp.606-611
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    • 2003
  • Byakangelicin, 9-(2,3-dihydroxy-2-methylbutoxy)-4-methoxy-7H- furo[3,2-g][l]benzopyran-7-one (BKG), a component of Angelicae dahuricae Radix, is considered to be an inhibitor of aldose reductase for the treatment of diabetic cataract. An analytical method for the isolation of BKG developed by high-performance liquid chromatography has been reported. No literature on the metabolism of BKG, however, has been found. With the purpose of identifying new metabolites of BKG, BKG (100 mg/kg) was orally administered to Sprague-Dawley rats via a gavage. Using a metabolic cage, urine was collected for 24 h, and the urine samples were extracted by liquid-liquid extraction. For structural identification of new urinary metabolites of BKG, various instrumental analyses were conducted by gas-chromatography/mass spectrometry, high-performance liquid chromatography/diode array detector, liquid chromatography/mass spectroscopy with thermospray interface and $^1H$ nuclear magnetic resonance spectroscopy. Two metabolites produced from the Ο-demethylation or Ο-dealkylation of BKG were newly identified, and another new but unknown metabolite was assumed to be the hydroxylated form of BKG. These results indicate that the major metabolic products of BKG are formed by Ο-demethylation or Ο-dealkylation of BKG side chains.

Synthesis of LaMnO3-Diamond Composites and Their Photocatalytic Activity in the Degradation of Weak Acid Red C-3GN

  • Huang, Hao;Lu, Benqian;Liu, Yuanyuan;Wang, Xeuqian;Hu, Jie
    • Nano
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    • v.13 no.10
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    • pp.1850121.1-1850121.11
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    • 2018
  • In this study, a series of $LaMnO_3$-diamond composites with varied $LaMnO_3$ mass contents supported on micro-diamond have been synthesized using a sol-gel method. The as-prepared composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and the Fourier transform infrared spectra (FTIR). Meanwhile, the photocatalytic performances were also tested by photoluminescence (PL) spectroscopy, ultraviolet-visible diffuse reflection spectra (UV-Vis DRS) and the degradation of weak acid red C-3GN (RC-3GN). Results show that the peak position of $LaMnO_3$ is shifted to low angle after the introduction of diamond, and perovskite particles uniformly distributed on the surface of diamond, forming a network structure, which can increase the active sites and the absorption of dye molecules. When the mass ratio of $LaMnO_3$ and diamond is 1:2 (LMO-Dia-2), the composite shows the most excellent photocatalytic activity. This result offers a sample route to enlarge the range of the application of micro-diamond and provide a new carrier for perovskite photocatalysts.

Structural and component characterization of the B4C neutron conversion layer deposited by magnetron sputtering

  • Jingtao Zhu;Yang Liu;Jianrong Zhou;Zehua Yang;Hangyu Zhu;Xiaojuan Zhou;Jinhao Tan;Mingqi Cui;Zhijia Sun
    • Nuclear Engineering and Technology
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    • v.55 no.9
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    • pp.3121-3125
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    • 2023
  • Neutron conversion detectors that use 10B-enriched boron carbide are feasible alternatives to 3He-based detectors. We prepared boron carbide films at micron-scale thickness using direct-current magnetron sputtering. The structural characteristics of natural B4C films, including density, roughness, crystallization, and purity, were analyzed using grazing incidence X-ray reflectivity, X-ray diffraction, X-ray photoelectron spectroscopy, time-of-flight secondary ion mass spectrometry, and scanning electron microscopy. A beam profile test was conducted to verify the practicality of the 10B-enriched B4C neutron conversion layer. A clear profile indicated the high quality of the neutron conversion of the boron carbide layer.

이온 에너지 분석을 통한 저손상 그래핀 클리닝 연구

  • Kim, Gi-Seok;Min, Gyeong-Seok;Yeom, Geun-Yeong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.218.2-218.2
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    • 2014
  • 그래핀은 높은 전기 전도도와 열전도도, 기계적 강도를 가지고 있고 동시에 높은 전자이동도($200,000cm^2{\cdot}V{\cdot}^1{\cdot}s{\cdot}^1$) 특성을 갖는 물질로써 차세대 소재로 각광받고 있다. 하지만 그래핀을 소자에 응용하기 위해서는 전사공정과 lithography 공정 과정에서 발생되는 PMMA(Poly methyl methacrylate) residue를 완벽하게 제거해야 하는 문제점이 있다. 특히, lithography 공정 중 완벽하게 PMMA residue 가 제거되지 않고 잔류해 있을 경우에 소자의 life time, performance에 악영향을 준다는 보고가 있다. 이와같은 문제를 해결하기 위해 화학적 cleaning, 열처리를 통한 cleaning, 전류 인가에 의한 cleaning과 같은 방법들을 이용하여 그래핀의 PMMA residue를 제거하는 공정들이 보고되고 있지만, 화학적 cleaning 방법의 경우 chloroform 이라는 독성물질 사용으로 인해 산업적으로 응용이 어렵고, 열처리 방법은 전극 등의 금속이 $200^{\circ}C$ 이상의 높은 온도에서 장시간 노출될 경우 쉽게 손상을 입으며, 전류 인가에 의한 cleaning 방법은 국부적으로만 효과를 볼 수 있기 때문에 lithography 공정 후 PMMA residue를 효과적으로 제거하기에는 한계를 보이고 있다. 본 연구에서는 Ar을 이용하는 Ion beam 시스템을 통해 beam energy를 제어함으로써 PMMA residue를 효과적으로 제거하는 연구를 진행하였다. 최적화된 플라즈마 발생 조건을 찾기 위해 QMS(Quadrupole Mass Spectrometer)를 이용하여 입사하는 ion energy와 flux 양을 컨트롤 하였고, 250 W에서 최적화된 ion energy distribution 영역이 존재한다는 것을 확인할 수 있었다. 또한, 25 Gauss 정도의 electro-magnetic field를 이용하여 Ar의 ion energy를 10 eV 이하로 낮추어 damage를 최소화함으로써 효과적으로 그래핀을 cleaning 할 수 있었다. Cleaning과정에서 ion bombardment에 의해 발생한 damage는 $250^{\circ}C$에서 6시간 동안 annealing 공정을 거치면서 회복되는 것을 Raman spectroscopy의 D peak ($1335cm{\cdot}^1$) / G peak ($1572cm{\cdot}^1$) ratio 로 확인할 수 있었고, PMMA residue의 cleaning 여부는 G peak ($1580cm{\cdot}^1$)의 blue shift와 2D peak ($2670cm{\cdot}^1$)의 red shift를 통해 확인하였다. 그리고 AFM (Atomic Force Microscopy)을 이용하여 cleaning 공정과정에서 RMS roughness가 4.99 nm에서 2.01 nm로 감소하는 것을 관찰하였다. 마지막으로, PMMA residue의 cleaning 정도를 정량적으로 분석하기 위해 XPS (X-ray Photoelectron Spectroscopy)를 이용하여 sp2 C-C bonding이 74.96%에서 87.66%로 증가함을 확인을 할 수 있었다.

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Etching Mechanism of $YMnO_3$ Thin Films in High Density $CF_4$/Ar Plasma ($CF_4$/Ar 가스 플라즈마를 이용한 $YMnO_3$ 박막의 식각 반응연구)

  • 김동표;김창일;이철인
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.14 no.12
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    • pp.959-964
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    • 2001
  • We investigated the etching characteristics of YMnO$_3$ thin films in high-density plasma etching system. In this study, YMnO$_3$ thin films were etched with CF$_4$/Ar gas chemistries in inductively coupled plasma(ICP). Etch rates of YMnO$_3$ increased up to 20% CF$_4$ in CF$_4$/(CF$_4$+Ar), but decreased with furthermore increasing CF$_4$ in CF$_4$/(CF$_4$+Ar). In optical emission spectroscopy (OES) analysis, F radical and Ar* ions in plasma at various gas chemistries decreased with increasing CF$_4$ content. Chemical states of YMnO$_3$ films exposed in plasma were investigated with x-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS). There is a chemical reaction between metal (Y, Mn) and F and metal-fluorides were removed effectively by Ar ion sputtering. YF$_{x}$, MnF$_{x}$ such as YF, YF$_2$, YF$_3$ and MnF$_3$ were detected using SIMS analysis. The etch slope is about 65$^{\circ}$ and cleasn surface. surface of the etched YMnO$_3$ thin films was investigated with X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS). The etch profile was also investigated by scanning electron microscopy (SEM).EM).

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LONG-SLIT SPECTROSCOPY OF PARSEC-SCALE JETS FROM DG TAURI

  • Oh, Heeyoung;Pyo, Tae-Soo;Yuk, In-Soo;Park, Byeong-Gon
    • Journal of The Korean Astronomical Society
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    • v.48 no.2
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    • pp.113-123
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    • 2015
  • We present observational results from optical long-slit spectroscopy of parsec-scale jets of DG Tau. From HH 158 and HH 702, the optical emission lines of Hα, [O i] λλ6300, 6363, [N ii] λλ6548, 6584, and [S ii] λλ6716, 6731 are obtained. The kinematics and physical properties (i.e., electron density, electron temperature, ionization fraction, and mass-loss rate) are investigated along the blueshifted jet up to 650′′ distance from the source. For HH 158, the radial velocity ranges from −50 to −250 km s−1. The proper motion of the knots is 0.′′196 − 0.′′272 yr−1. The electron density is ∼104 cm−3 close to the star, and decreases to ∼102 cm−3 at 14′′ away from the star. Ionization fraction indicates that the gas is almost neutral in the vicinity of the source. It increases up to over 0.4 along the distance. HH 702 is located at 650′′ from the source. It shows ∼ −80 km s−1 in the radial velocity. Its line ratios are similar to those at knot C of HH 158. The mass-loss rate is estimated to be about ∼ 10−7 M yr−1, which is similar to values obtained from previous studies.

Photovoltaic Performance of Crystalline Silicon Recovered from Solar Cell Using Various Chemical Concentrations in a Multi-Stage Process (습식 화학 공정에 의한 태양전지로부터 고순도 실리콘 회수 및 이를 이용한 태양전지 재제조)

  • Noh, Min-Ho;Lee, Jun-Kyu;Ahn, Young-Soo;Yeo, Jeong-Gu;Lee, Jin-Seok;Kang, Gi-Hwan;Cho, Churl-Hee
    • Korean Journal of Materials Research
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    • v.29 no.11
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    • pp.697-702
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    • 2019
  • In this study, using a wet chemical process, we evaluate the effectiveness of different solution concentrations in removing layers from a solar cell, which is necessary for recovery of high-purity silicon. A 4-step wet etching process is applied to a 6-inch back surface field(BSF) solar cell. The metal electrode is removed in the first and second steps of the process, and the anti-reflection coating(ARC) is removed in the third step. In the fourth step, high purity silicon is recovered by simultaneously removing the emitter and the BSF layer from the solar cell. It is confirmed by inductively coupled plasma mass spectroscopy(ICP-MS) and secondary ion mass spectroscopy(SIMS) analyses that the effectiveness of layer removal increases with increasing chemical concentrations. The purity of silicon recovered through the process, using the optimal concentration for each process, is analyzed using inductively coupled plasma atomic emission spectroscopy(ICP-AES). In addition, the silicon wafer is recovered through optimum etching conditions for silicon recovery, and the solar cell is remanufactured using this recovered silicon wafer. The efficiency of the remanufactured solar cell is very similar to that of a commercial wafer-based solar cell, and sufficient for use in the PV industry.

NMR Spectroscopy and Mass Spectrometry of 1, 2-Hexanediol Galactoside synthesized using Escherichia coli β-Galactosidase (대장균 베타-갈락토시데이즈를 이용하여 합성된 1, 2-Hexanediol Galactoside의 NMR Spectroscopy 및 Mass spectrometry)

  • Kim, Yi-Ok;Lee, Hyang-Yeol;Jung, Kyung-Hwan
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.2
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    • pp.286-292
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    • 2016
  • 1, 2-Hexanediol galactoside (HD-gal) has been synthesized from 1, 2-hexanediol (HD), a cosmetic preservative, using recombinant Escherichia coli ${\beta}$-galactosidase (${\beta}$-gal) at the high lactose concentration (300 g/l). To confirm the molecular structure of synthesized HD-gal, NMR ($^1H$- and $^{13}C$-) spectroscopy and mass spectrometry of HD-gal were conducted. $^1H$ NMR spectrum of HD-gal showed multiple peaks corresponding to the galactocyl group, which is an evidence of galactocylation on HD. Downfield proton peaks at ${\delta}_H$ 4.44 ppm and multiple peaks from ${\delta}_H$3.96~3.58 ppm were indicative of galactocylation on HD. Up field proton peaks at ${\delta}_H$ 1.60~1.35 ppm and 0.92 ppm showed the presence of $CH_2$ and $CH_3$ protons of HD. $^{13}C$ NMR spectrum revealed the presence of 21 carbons suggestive of ${\alpha}$- and ${\beta}$-anomers of HD-gal. Among 12 carbon peaks from each anomers, the 3 peaks at dC 68.6, 60.9 and 13.2 ppm were assigned to be overlapped showing only 21 peaks out of total 24 peaks. The mass value (protonated HD-gal, m/z = 281.1601) from mass spectrometry analysis of HD-gal, and $^1H$ and $^{13}C$ NMR spectral data were in well agreement with the expecting structure of HD-gal. For further study, the minimum inhibitory concentrations (MICs) of HD-gal against bacteria will be investigated, and, in addition, cytotoxicity to human skin cells of HD-gal will be examined. It is expected that it will eventually be able to develop a new cosmetic preservative, which have low cytotoxicity against human skin cell and maintains antimicrobial effect.

NMR Spectroscopy and Mass Spectrometry of Phenylethanol Galactoside synthesized using Escherichia coli 𝛽-Galactosidase (대장균 베타-갈락토시데이즈를 이용하여 합성된 Phenylethanol 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.37 no.5
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    • pp.1323-1329
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    • 2020
  • To characterize the molecular structure of PhE-gal synthesized using Escherichia coli 𝛽-gal, NMR (1H- and 13C-) spectroscopy and mass spectrometry of PhE-gal were conducted. 1H NMR spectrum of PhE-gal showed multiple peaks corresponding to the galactosyl group, which is an evidence of galactosylation on 2-phenylethanol (PhE). Downfield proton peaks at 𝛿H 7.30~7.21 ppm showed the presence of aromatic protons of PhE as well as benzyl CH2 protons at 𝛿H 2.88 ppm. Up field proton peaks at 𝛿H 4.31 ppm, 4.07 ppm and multiple peaks from 𝛿H 3.86~3.38 ppm are indicative of galactocylation on PhE. 13C NMR spectrum revealed the presence of 12 carbons suggestive of PhE-gal. Among 12 carbon peaks from PhE-gal, the four peaks at 138.7, 129.0, 128.6 and 126.5 were assigned aromatic carbons in the phenyl ring. Three peaks at 129.0, 128.6 and 126.5 showed high intensities, indicating CH aromatic carbons. 13C NMR data of PhE-gal showed 6 monosaccharide peaks from galactose and 2 peaks from aliphatic chain of PhE, indicating that PhE-gal was galactosyl PhE. The mass value (sodium adduct ion of PhE-gal, m/z = 307.1181) from mass spectrometry analysis of PhE-gal, and 1H and 13C NMR spectral data were in good agreement with the expecting structure of PhE-gal. We are expecting that through future study it will eventually be able to develop a new additive with low cytotoxicity.

Electron Impact Ionization Mass Spectra of 3-Substituted-2-hydroxy-4(3H)-quinazolinones

  • El Deen, I.M.;Abd El Fattah, M.E.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.4
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    • pp.473-478
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    • 2003
  • 3-Amino-2-hydroxy-4(3H)-quinazolinone (3) was prepared via condensation of 1 with hydrazine hydrate. Treatment of 3 with appropriate acid in $POCl_3$, ethyl chloroacetate and activated olefinic compounds in DMF yielded the corresponding 3-(substituted)amino-2-hydroxy-4(3H)-quinazolinones 4, 5 and 6. The electron impact ionization mass spectra of compounds 3 and 4 show a weak molecular ion peak and a base peak of m/z 146 resulting from a cleavage fragmentation. The compounds 5 and 6 give a characteristic fragmentation pattern with a very stable fragment of benzopyrazolone (m/z 132).