• Title/Summary/Keyword: Solid-phase reagent

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Characterization of Synthesized WS$_2$ Solid Lubricant (합성 WS$_2$ 고체윤활제의 특성 분석)

  • 신동우;윤대현;최인혁;김인섭
    • Proceedings of the Korean Society of Tribologists and Lubrication Engineers Conference
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    • 1997.10a
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    • pp.211-216
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    • 1997
  • The tungsten disulfide (WS$_2$) solid lubricant was synthesized by two different reaction processes, and the chemical and physical characteristics of synthesized WS$_2$ powder were analyzed in terms of the average particle size, morphology, crystalline phase. The solid WO$_3$ powder with the average size of 0.2 $\mu$m was reacted with CS$_2$ gas flowed with N$_2$ or 96% N$_2$ + 4% H$_2$ forming gas for 36 h and 24 h at 900$\circ$C respectively. In the case of vapour phase transport method, the 3.5 wt% iodine was added as a vapour transport reagent into the composition of tungsten and sulfur powders maintaining a constant molar ratio of W : S = 1 : 2.2. The mixture was then heat treated at 850$\circ$C for 2 weeks in vacuum The reaction product obtained showed the average size of 12 $\mu$m and the hexagonal plate shape of typical solid lubricant with 2H-WS$_2$ crystalline phase.

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Synthesis of $WS_2$ Solid Lubricant ($WS_2$ 고체 윤활제의 합성)

  • 신동우;윤대현;황영주;김성진;김인섭
    • Tribology and Lubricants
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    • v.13 no.4
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    • pp.60-65
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    • 1997
  • The tungsten disulfide $(WS_2)$ solid lubricant was synthesized by two different reaction processes, i.e., the reaction between $CS_2$ gas phase and solid $WO_3$powder, and the vapour phase transport method of tungsten and sulfur in a high vacuum. The chemical and physical characteristics of synthesized $WS_2$powder were analyzed in terms of the average particle size, morphology, crystalline phase etc. in comparison with those of commercial $WS_2$powder. The solid $WO_3$ powder with the average size of 0.2 ${\mu}{\textrm}{m}$ was reacted with $CS_2$gas flowed with$N_2$or 96%$N_2{\times}4%H_2$forming gas for 36 h and 24 h at 90$0^{\circ}C$ respectively. $WS_2$ crystalline phase was then formed through the intermediate phase of .$W_{20}O_{58}$ In the case of vapour phase transport method, the 3.5 wt% iodine was added as a vapour transport reagent into the composition of tungsten and sulfur powders maintaining a constant molar ratio of W:S=1:2.2. The mixture was then heat treated at 85$0^{\circ}C$ for 2 weeks in vacuum. The reaction product obtained showed the average size of 12 ${\mu}{\textrm}{m}$ and the hexagonal plate shape of typical solid lubricant with 2H-$WS_2$crystalline phase.

The Evaluation of Solid-Phase Microextraction(SPME) Techniques for Analyzing Mixed Fuel Oxygenates and Products

  • 이재선;이시진;장순웅
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.09a
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    • pp.458-461
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    • 2003
  • Solid-phase microextraction (SPME) and gas chromatography/headspace techniques(HS) and flame ionization detection (GC/FID) have been combined for determination of very polar compounds in water, including the widely used gasoline oxygenates and by-products. A relatively simple extraction method using a CAR/PDMS(75${\mu}{\textrm}{m}$) SPME fiber was optimized for the routine analysis of gasoline oxygenates and by-products in groundwater and reagent water. A sodium chloride concentration of 25%(w/w) combined with an extraction time of 20 min provided the greatest sensitivity while maintaining analytical efficiency Replicate analyses in fortified reagent and groundwater spiked with microgram per liter concentrations of gasoline oxygenates and by-products indicate quantitative and reproducible recovery of these and related oxygenate compounds. Method dynamic range was 50$\mu\textrm{g}$ L-1 to 3000$\mu\textrm{g}$ L-1 for gasoline oxygenates and by-products.

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Application of BMPI / HOBT Reagent in Solid-Phase Peptide Synthesis

  • Hong Nam Joo;Choi Soo Kwan;Koock Soon Uoong
    • Bulletin of the Korean Chemical Society
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    • v.10 no.1
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    • pp.19-22
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    • 1989
  • The suitability of BMPI (2-bromo-N-methyl pyridinium iodide) for solid-phase peptide synthesis was investigated. The coupling rate of BMPI/HOBT procedure. BMPI/HOBT was superior to DCC/HOBT couplings using the solid-phase peptide bond formation proceeded to a greater degree of completion than DCC/HOBT method did. Double couplings with 2 equiv. of Bocamino acids and 1.5 equiv. of BMPI and $NEt_3$ and 2 equiv. of HOBT in DMF/MC (1:1 v/v) gave the best result for the preparation of a model compound. Stepwise solid phase peptide synthesis using BMPI/HOBT procedure was successfully utilized for the preparation of $(D-Ala)^2$-dynorphine A. BMPI/HOBT procedure for the synthesis of $(D-Ala)^2$-dynorphine gave better yield (20%) than DCC/HOBT procedure did.

Combinatorial Solid Phase Peptide Synthesis and Bioassays

  • Shin, Dong-Sik;Kim, Do-Hyun;Chung, Woo-Jae;Lee, Yoon-Sik
    • BMB Reports
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    • v.38 no.5
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    • pp.517-525
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    • 2005
  • Solid phase peptide synthesis method, which was introduced by Merrifield in 1963, has spawned the concept of combinatorial chemistry. In this review, we summarize the present technologies of solid phase peptide synthesis (SPPS) that are related to combinatorial chemistry. The conventional methods of peptide library synthesis on polymer support are parallel synthesis, split and mix synthesis and reagent mixture synthesis. Combining surface chemistry with the recent technology of microelectronic semiconductor fabrication system, the peptide microarray synthesis methods on a planar solid support are developed, which leads to spatially addressable peptide library. There are two kinds of peptide microarray synthesis methodologies: pre-synthesized peptide immobilization onto a glass or membrane substrate and in situ peptide synthesis by a photolithography or the SPOT method. This review also discusses the application of peptide libraries for high-throughput bioassays, for example, peptide ligand screening for antibody or cell signaling, enzyme substrate and inhibitor screening as well as other applications.

Numerical Analysis of Solid Propellant Ignition ~Numerical Formulation Assessment~

  • Shimada, Toru;Novozhilov, Boris V.
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2004.03a
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    • pp.528-531
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    • 2004
  • For a simple one-dimensional ignition problem a mathematical model is described to investigate the difficulties in numerical simulations. Some computation results are obtained and comparison is made with analytical solution. Discussions are made on topics such as 1) coordinate transformation, 2) gas-phase and solid-phase analysis; (divergence form of the governing system, a finite-volume discretization, implicit time integration, upwind split flux, spatial accuracy improvement are described. Mass, reagent mass, and energy conservations are solved.), and 3) method to determine quantities on the burning surface (matching). Results obtained for small values of the non-dimensional pressure show a steady-combustion and good agreement with the analytical solution. Numerical instability appeared for larger values of the pressure, discussion on the cause of the problem is made. This effort is a part of a study of flame spread phenomena on solid propellant surface.

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Indirect Determination of Nitrite by Flame Atomic Absorption Spectrometry Using a Lead(IV) Dioxide Oxidant Microcolumn

  • Noroozifar, Meissam;Khorasani Motlagh, Mozhgan;Taheri, Aboozar;Homayoonfard, Marjan
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.875-880
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    • 2006
  • A new, simple and fast flow injection analysis (FIA) method has been developed for the indirect determination of nitrite. The proposed indirect automatic method is based on the oxidation of nitrite to nitrate using a lead(IV) dioxide oxidant microcolumn where the flow of the sample through the microcolumn reduces the $PbO_2$ solid phase reagent to Pb(II), which is measured by flame atomic absorption spectrometry. The absorbance of Pb(II) are proportional to the concentration of nitrite in the samples. The calibration curve was linear up to 30 mg $L ^{-1}$, with a detection limit of 0.11 mg $L ^{-1}$ for a 400 mL injected sample volume and a sampling rate of about 80 $h ^{-1}$. The results exhibit no interference from the presence of large amounts of ions. The developed procedure was found to be suitable for the determination of nitrite in foodstuffs and wastewaters. A relative standard deviation better than 0.9% was obtained in a repeatability study. The reliability of the method was established by parallel determination against the standard method.

Nano-particles of Mechanochemical Synthesis

  • Urakaev, Farit Kh.
    • Journal of the Speleological Society of Korea
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    • no.71
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    • pp.5-11
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    • 2006
  • A theoretical investigation of the solid phase mechanochemical synthesis of nano sized target product on the basis of dilution of the initial powdered reagent mixture by another product of an exchange reaction is presented. On the basis of the proposed 3 mode particle size distribution in mechanically activated mixture, optimal molar ratios of the components in mixture are calculated, providing the occurrence of impact friction contacts of reagent particles and excluding aggregation of the nanosized particles of the target reaction product. Derivation of kinetic equations for mechanochemical synthesis of nanoscale particles by the final product dilution method in the systems of exchange reactions is submitted. On the basis of obtained equations the necessary times of mechanical activation for complete course of mechanochemical reactions are designed. Kinetics of solid phase mechanosynthesis of nano TlCl by dilution of initial (2NaCl+$Tl_2SO_4$) mixture with the exchange reaction product (diluent,$zNa_2SO_4$, z=z*=11.25) was studied experimentally. Some peculiar features of the reaction mechanism were found. Parameters of the kinetic curve of nano TlCl obtained experimentally were compared with those for the model reaction KBr+TlCl+zKCl=(z+1) KCl+TlBr (z=z1*=13.5), and for the first time the value of mass transfer coefficient in a mechanochemical reactor with mobile milling balls was evaluated. Dynamics of the size change was followed for nanoparticle reaction product as a function of mechanical activation time.

Comparison of Liquid-Liquid Extraction and Solid-Phase Extraction Coupled with GC/MS for Determination of Priority Pollutants in Water (액체 추출법과 고체상 추출법에 의한 수질 중 유해물질 농축법 비교)

  • Yook, Keun-Sung;Hong, Sa-Moon;Kim, Jong-Ho
    • Analytical Science and Technology
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    • v.7 no.4
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    • pp.441-453
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    • 1994
  • Two extraction methods, liquid-liquid extraction(LLE) and solid-phase extraction(SPE), coupled with GC/MS were compared as preconcentration procedures for priority pollutants in water. Among the semi-volatile priority pollutants, 11 acid and 44 base/neutral compounds were spiked in reagent water. With LLE, which is a modification of EPA Method 625, the overall mean recovery of the 54 compounds was 91% with a mean relative standard deviation(RSD) of 4.6%. With SPE, the overall mean recovery of the 52 compounds was 53% with a mean RSD of 8.9%. The detection limits of both methods were in the range of $1{\sim}5{\mu}g/l$.

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