• Title/Summary/Keyword: chemical ionization

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An ESR Study of Amino Acid and Protein Free Radicals in Solution Part Ⅲ. ESR Study of Lysozyme Free Radical Produced by $Ti-H_2O_2$ Flow System (용액에서의 아미노산 및 단백질 자유기에 관한 ESR 연구 제3보 $Ti-H_2O_2$ Flow System으로 만든 Lysozyme 자유기의 ESR 연구)

  • Hong, Sun-Joo;Piette, L.H.
    • Journal of the Korean Chemical Society
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    • v.15 no.4
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    • pp.177-181
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    • 1971
  • Free radicals of lysozyme produced by $Ti-H_2O_2$ system were studied in aqueous solution at room temperature using ESR with a continuous flow-mixing. The spectra, each consisting of a doublet with 5.5 G splitting and a broad resonance covering 80 G splitting are closely similar in shape to that for solid irradiated in vacuum at $77^{\circ}K$ and observed at room temperature immediately on warming. The result is assumed to indicate that the secondary protein radical components formed within 0.01 second, dead time of the mixing chamber, and initiated by hydrogen atom abstraction at ${\alpha}$-carbon atom of peptide chain in liquid solution at room temperature are identical to those resulting from the initial formation of a mixture of positive holes and negative ions by ionization processes as well as radical fragments by the rupture of chemical bonds in the solid during similar time at the same temperature. A broad resonance is observed with considerable amplitude on the high field side of the doublet, which is quite dissimilar to the spectra of irradiated solid lysozyme. This resonance was tentatively attributed to the polypeptide free radical in which unpaired electrons are localized on side chain.

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Indium and Gallium-Mediated Addition Reactions

  • Lee, Phil-Ho
    • Bulletin of the Korean Chemical Society
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    • v.28 no.1
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    • pp.17-28
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    • 2007
  • Indium and gallium have emerged as useful metals in organic synthesis as a result of its intriguing chemical properties of reactivity, selectivity, and low toxicity. Although indium belongs to a main metal in group 13, its first ionization potential energy is very low and stable in H2O and O2. Therefore, indium-mediated organic reactions are of our current interest. On the basis of these properties of indium, many efficient indium-mediated organic reactions have been recently developed, such as the addition reactions of allylindium to carbonyl and iminium groups, the indium-mediated synthesis of 2-(2-hydroxyethyl)homoallenylsilanes, the indiummediated allylation of keto esters with allyl halides, sonochemical Reformatsky reaction using indium, the indium-mediated selective introduction of allenyl and propargyl groups at C-4 position of 2-azetidinones, the indium-mediated Michael addition and Hosomi-Sakurai reactions, the indium-mediated β-allylation, β- propargylation and β-allenylation onto α,β-unsaturated ketones, the highly efficient 1,4-addition of 1,3-diesters to conjugated enones by indium and TMSCl, and the intramolecular carboindation reactions. Also, we found gallium-mediated organic reactions such as addition reactions of propargylgallium to carbonyl group and regioselective allylgallation of terminal alkynes.

The Improvement of the Ionization on Micro Mass Spectrometer using Carbon Nanotube Emitter (탄소나노튜브 방출원을 통한 초소형 질량분석기의 이온화 향상)

  • Song, S.H.;Han, Kyu-Sung;Hong, Nguyen Tuan;Lee, S.I.;Yang, Sang-Sik
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.58 no.5
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    • pp.1004-1009
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    • 2009
  • Recently, mass spectrometers are widely used for in-situ chemical analysis. It has rapid response and high sensitivity. In this paper, we present the fabrication and test of a cold cathode emitter for micro mass spectrometer using CNTs(Carbon nano tubes). The CNTs have good mechanical, electrical and chemical characteristics. So they have a long life time and strong robustness. The micro mass spectrometer is composed of the glass substrate and the silicon substrate. The glass substrate is constructed by electrodes for TOF(Time-of-flight) which analyze an ion with mass to charge ratio as ion separator. The silicon substrate is highly doped wafer which is patterned for gate electrode and then 100 11m dry etching to grow the CNTs as the electron emitter. The CNTs are grown by HFCVD(Hot filament chemical vapor deposition) with sputtering the catalyst. We successfully attained to grow the CNTs and to test the characteristics.

Synthesis and Electro-optical Properties of π-Conjugated Polymer Based on 10-Hexylphenothiazine and Aromatic 1,2,4-Triazole

  • Choi, Ji-Young;Kim, Dong-Han;Lee, Bong;Kim, Joo-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.9
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    • pp.1933-1938
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    • 2009
  • New $\pi$-conjugated polymer with vinylene linkage, poly((10-hexyl-3,7-phenothiazine)-alt-(4-(4-butyl-phenyl)- 3,5-diphenyl-4H-[1,2,4]triazole)-3,5-vinylene) (PTV-TAZ) was synthesized by the Heck coupling reaction. The photoluminescence (PL) maximum wavelength and the band gap energy of PTV-TAZ film were 555 nm and 2.41 eV, respectively. The HOMO energy level of PTV-TAZ was -4.99 eV, which was slightly lower than that of PTV (-4.89 eV). Electron deficient aromatic 1,2,4-triazole (TAZ) in the polymer backbone does not affect the HOMO energy level significantly. The maximum efficiency and brightness of double layer structured electroluminescent (EL) device (ITO/PEDOT (30 nm)/PTV-TAZ (60 nm)/Al) were 0.247 cd/A and 553 cd/$m^2$, respectively, which were significantly higher than those of the device based PTV (1.65 ${\times}\;10^{-4}$ cd/A and 4.3 cd/$m^2$). This is due to that TAZ unit improves electron transporting ability in the emissive layer. The turn-on voltage (defined as the voltage required to give a luminescence of 1 cd/$m^2$) of brightness of the device based on PTV-TAZ was 12.0 V, which was similar to that the based on PTV (11.5 V). This is due to that the ionization potential of PTV-TAZ is very similar to that of PTV.

Quantitative Analysis of Cinnamaldehyde, Cinnamylalcohol and Salicylaldehyde in Commercial Biopesticides Containing Cinnamon Extract Using Gas Chromatography - Flame Ionization Detector

  • Lim, Sung-Jin;Lee, Ji-Hye;Kim, Jin-Hyo;Choi, Geun-Hyoung;Cho, Nam-Jun;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.33 no.3
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    • pp.213-219
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    • 2014
  • BACKGROUND: In an environment-friendly agriculture, plant extracts have been perceived as alternatives of synthetic pesticides. The Environment-friendly Agriculture Promotion Act of Korea has approved cinnamon extract as a matter for the production of commercial biopesticides. Thirteen commercial biopesticides containing cinnamon extract have been marketed locally. However, the analytical method for the quality control of these biopesticides containing cinnamon extract has not been studied. METHODS AND RESULTS: Cartridge clean-up method for the determination of cinnamaldehyde, cinnamylalcohol and salicylaldehyde in biopesticides containing cinnamon extract was developed and validated by gas chromatography (GC). The clean-up method was optimized with HLB SPE cartridges for the bioactive substance in biopesticides containing cinnamon extract, and the eluate was analyzed by GC. The developed method was validated, and the LOQ and recovery rates of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were 0.139, 0.067 and $0.062mgL^{-1}$ and 84.2, 86.5 and 82.1%, respectively. The contents of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were analyzed using the developed method in the 13 commercial biopesticides. Results showed 0.06-17.37%,

A Study on the Treatment of Heavy Metal in Wastewater by Redox Reaction of Cu-Zn Metal Alloy and Adsorption reaction of Al-Silicate (Cu-Zn 금속합금의 산화 환원반응과 Al-Silicate의 흡착반응을 이용한 폐수 중 중금속처리에 관한 연구)

  • Lee, Soo-Jeong;Kim, Jong Hwa;Song, Ju Yeong
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.3
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    • pp.441-448
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    • 2016
  • Heavy metal removal study is conducted from synthetic waste water by reduction and oxidation(redox) reaction of Cu-Zn metal alloy and adsorption reaction of aluminium silicate. Heavy metal whose ionization tendency is smaller than zinc are reducted in an aqueous solution, and the concentration of ionized zinc is reduced by adsorption reaction. The average diameter of metal alloy micro fiber is about $200{\mu}m$, and the surface area is wide enough to get equilibrium in a single cycle treatment. A single cycle treatment of redox reaction of Cu-Zn metal alloy, could remove 100.0 % of Cr(III), 98.0 % of Hg, 92.0 % of Sn and 91.4 % of Cu respectively. An ionization tendency of chromium is very close to zinc, but removal efficiency of chromium by redox reaction is significant. This result shows that trivalent chromium ion is expected to generate hydroxide precipitation with $OH^-$ ion generated by redox reaction. Zinc ion generated by redox reaction is readily removed by adsorption reaction of aluminium silicate in a single cycle treatment. Other heavy metal components which are not perfectly removed by redox reaction also showed very high removal efficiency of 98.0 % or more by adsorption reaction. Aluminium ion is not increased by adsorption reaction of aluminium silicate. That means heavy metal ion removal mechanism by adsorption reaction is turned out to be not an ion exchange reaction, but an adsorption reaction.

PEMOCVD of Ti(C,N) Thin Films on D2 Steel and Si(100) Substrates at Low Growth Temperatures

  • Kim, Myung-Chan;Heo, Cheol-Ho;Boo, Jin-Hyo;Cho,Yong-Ki;Han, Jeon-Geon
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.211-211
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    • 1999
  • Titanium nitride (TiN) thin films have useful properties including high hardness, good electrical conductivity, high melting point, and chemical inertness. The applications have included wear-resistant hard coatings on machine tools and bearings, decorative coating making use of the golden color, thermal control coatings for widows, and erosion resistant coatings for spacecraft plasma probes. For all these applications as feature sizes shrink and aspect ratios grow, the issue of good step coverage becomes increasingly important. It is therefore essential to manufacture conformal coatings of TiN. The growth of TiN thin films by chemical vapor deposition (CVD) is of great interest for achieving conformal deposition. The most widely used precursor for TiN is TiCl4 and NH3. However, chlorine impurity in the as-grown films and relatively high deposition temperature (>$600^{\circ}C$) are considered major drawbacks from actual device fabrication. To overcome these problems, recently, MOCVD processes including plasma assisted have been suggested. In this study, therefore, we have doposited Ti(C, N) thin films on Si(100) and D2 steel substrates in the temperature range of 150-30$0^{\circ}C$ using tetrakis diethylamido titanium (TDEAT) and titanium isopropoxide (TIP) by pulsed DC plamsa enhanced metal-organic chemical vapor deposition (PEMOCVD) method. Polycrystalline Ti(C, N) thin films were successfully grown on either D2 steel or Si(100) surfaces at temperature as low as 15$0^{\circ}C$. Compositions of the as-grown films were determined with XPS and RBS. From XPS analysis, thin films of Ti(C, N) with low oxygen concentration were obtained. RBS data were also confirmed the changes of stoichiometry and microhardness of our films. Radical formation and ionization behaviors in plasma are analyzed by optical emission spectroscopy (OES) at various pulsed bias and gases conditions. H2 and He+H2 gases are used as carrier gases to compare plasma parameter and the effect of N2 and NH3 gases as reactive gas is also evaluated in reduction of C content of the films. In this study, we fond that He and H2 mixture gas is very effective in enhancing ionization of radicals, especially N resulting is high hardness. The higher hardness of film is obtained to be ca. 1700 HK 0.01 but it depends on gas species and bias voltage. The proper process is evident for H and N2 gas atmosphere and bias voltage of 600V. However, NH3 gas highly reduces formation of CN radical, thereby decreasing C content of Ti(C, N) thin films in a great deal. Compared to PVD TiN films, the Ti(C, N) film grown by PEMOCVD has very good conformability; the step coverage exceeds 85% with an aspect ratio of more than 3.

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Quantitative Determination of Ascaridole, Carvacrol and p-Cymene in the Biopesticides Products Derived from Chenopodium ambrosioides L. Extracts by Gas Chromatography

  • Yang, Ji-Yeon;Ryu, Song-Hee;Lim, Sung-Jin;Choi, Geun-Hyoung;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.35 no.3
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    • pp.211-215
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    • 2016
  • BACKGROUND: The commercial biopesticides containing Chenopodium ambrosioides L. extracts which have been registered as one of the ingredients of the commercial biopesticide by the organic agriculture materials, and have been widely used in Republic of Korea. However, the quantitative analysis method of the active substances for the commercial biopesticides containing C. ambrosioides L. extract has not been conducted.METHODS AND RESULTS: To analyze the quantitative analysis of ascaridole, carvacrol, and p-cymene as active substances of C. ambrosioides L. extract, hydrophilic lipophilic balance cartridge was used for solid phase extraction. The active substances were analyzed by the gas chromatography with flame ionization detector. The limit of quantitation values of ascaridole, carvacrol, and p-cymene were 10, 5, and 2 mg/L, and the recovery rates were 96.3, 84.0, and 82.5% in liquid products and 98.3, 99.1, and 97.3% in solid products, respectively. The total content of ascaridole, carvacrol, and p-cymene in the commercial biopesticides was ranged from 0.08 to 12.75%.CONCLUSION: From these results, this method was suitable for the quantitative analysis of the active substances of commercial biopesticides containing C. ambrosioides L. extract.

Determination of Lipid A Profile of Gram-Negative Bacteria from Arctic Soils Using Mass Spectrometric Approaches (질량분석 시스템을 이용한 극지 토양 유래 신규 미생물의 지질 A 화학적 구조 분석)

  • Hwang, Cheol-hwan;Park, Han-Gyu;Kim, Yun-Gon
    • KSBB Journal
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    • v.31 no.4
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    • pp.263-269
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    • 2016
  • For decades, the microorganisms in arctic soils have been newly discovered according to the climate change and global warming. In this study, the chemical structure of a lipid A molecule from Pseudomonas sp. strain PAMC 28615 which was newly discovered from arctic soils was characterized by mass spectrometric approaches such as matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) and MALDI multi-stage tandem mass spectrometry (MS). First, lipopolysaccharide (LPS) from Pseudomonas sp. strain PAMC 28615 was extracted and subsequently hydrolyzed to obtain the lipid A. The parent ion peak at m/z 1632 was determined by MALDI-TOF MS, which also can validate our lipid A purification method. For detailed structural determination, we performed the multiple-stage tandem mass analysis ($MS^4$) of the parent ion, and subsequently the abundant fragment ions in each MS stage are tested. The fragment ions in each MS stage were produced from the loss of phosphate groups and fatty acyl groups, which could be used to confirm the composition or the position of the lipid A components. Consequently, the mass spectrometry-based lipid A profiling method could provide the detail chemical structure of lipid A from the Pseudomonas sp. strain PAMC 28615 as an arctic bacterium from the frozen arctic soil.

Microbead based micro total analysis system for Hepatitis C detection (마이크로비드를 이용한 초소형 C형 간염 검출 시스템의 제작)

  • Sim, Tae-Seok;Lee, Bo-Rahm;Lee, Sang-Myung;Kim, Min-Soo;Lee, Yoon-Sik;Kim, Byung-Gee;Kim, Yong-Kweon
    • Proceedings of the KIEE Conference
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    • 2006.07c
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    • pp.1629-1630
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    • 2006
  • This paper describes a micro total analysis system ($\mu$ TAS) for detecting and digesting the target protein which includes a bead based temperature controllable microchip and computer based controllers for temperature and valve actuation. We firstly combined the temperature control function with a bead based microchip and realized the on-chip sequential reactions using two kinds of beads. The PEG-grafted bead, on which RNA aptamer was immobilized, was used for capturing and releasing the target protein. The target protein can be chosen by the type of RNA aptamer. In this paper, we used the RNA aptamer of HCV replicase. The trypsin coated bead was used for digesting the released protein prior to the matrix assisted laser desorption ionization time of flight mass spectrometer (MALDI TOF MS). Heat is applied for release of the captured protein binding on the bead, thermal denaturation and trypsin digestion. PDMS microchannel and PDMS micro pneumatic valves were also combined for the small volume liquid handling. The entire procedures for the detection and the digestion of the target protein were successfully carried out on a microchip without any other chemical treatment or off-chip handling using $20\;{\mu}l$ protein mixture within 20 min. We could acquire six matched peaks (7% sequence coverage) of HCV replicase.

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