• Title/Summary/Keyword: Fourier transform mass spectrometry

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Catalytic oxidation kinetics of iron-containing carbon particles generated from diesel-sprayed hydrogen-air diffusion flame (디젤-분무 수소-공기 확산화염에서 생성된 철-함유 탄소입자의 촉매 산화반응 특성)

  • Kim, Yongho;Kim, Yong-Tae;Kim, Soo Hyung;Lee, Donggeun
    • Particle and aerosol research
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    • v.4 no.2
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    • pp.51-67
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    • 2008
  • In this study, we devoted to kinetic measurement of the catalytic oxidation of iron-containing flame soot particles and better understanding the role of catalytic particles on carbon oxidation in particular at low temperature, targeting on autothermal regeneration of diesel particulate filter by diesel exhaust gas. Carbon-based Fe-containing particles generated by spraying ferrocene-doped diesel fuel in an oxy-hydrogen flame are tested and compared with a commercial carbon black powder for thermogravimetric analysis (TGA), secondary ion mass spectrometry (SIMS), Fourier-transform infrared spectroscopy (FTIR), Induced coupled plasma-Atomic emission spectroscopy (ICP-AES), and High-resolution transmission electron microscopy (HR-TEM). As a result, we found that a small amount of the ferrocene addition led to significant reductions in a on-set temperature and an activation energy of the carbon oxidation as well. An oxygenated surface complex forming at the particle surface could be thought as active species that would be readily consumed in particular at low temperature.

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Proton Transfer Reactions and Ion-Molecule Reactions of Ionized XCH2CH2Y (X and Y = OH or NH2)

  • Choi, Sung-Seen;So, Hun-Young
    • Bulletin of the Korean Chemical Society
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    • v.27 no.4
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    • pp.539-544
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    • 2006
  • Proton transfer reactions and ion-molecule reactions of bifunctional ethanes of $H_2NCH_2CH_2NH_2$, $H_2NCH_2CH_2OH$, and $HOCH_2CH_2OH$ were studied using Fourier transform mass spectrometry (FTMS). The rate constants for proton transfer reactions between the fragment ions and neutral molecules were obtained from the temporal variation of the ion abundances. The rate constants were consistent with the heats of reaction. The fastest proton transfer reactions were the reactions of $CH_2N^+$, $CHO^+$, and $CH_3O^+$ for $H_2NCH_2CH_2NH_2$, $H_2NCH_2CH_2OH$, and $HOCH_2CH_2OH$, respectively. The $[M+13]^+$ ion was formed by the ion-molecule reaction between $H_2C=NH_2 ^+$ or $H_2C=OH^+$ and the neutral molecule. The major product ions generated from the ion-molecule reactions between the protonated molecule and neutral molecule were $[2M+H]^+$, $[M+27]^+$, and $[M+15]^+$.

Synthesis and Application of Metal Doped Silica Particles for Adsorptive Desulphurization of Fuels

  • Jabeen, Bushra;Rafique, Uzaira
    • Environmental Engineering Research
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    • v.19 no.3
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    • pp.205-214
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    • 2014
  • Petroleum a vital commodity affecting every aspect of 21st century. Toxicity and adverse effects of sulphur as catalyst in petroleum products is of great concern required development of techniques for desulphurization in compliance with the International standards. Installation of desulphurizing units costs over $200 million per unit placing economic burden on developing countries like Pakistan. Present study analysis of commercial fuels (station petrol and jet fuel JP8) on gas chromatography-mass spectrometry (GC-MS) identified sulphur concentration of 19.94 mg/L and 21.75 mg/L, respectively. This scenario urged the researcher to attempt synthesis of material that is likely to offer good adsorption capacity for sulphur. Following protocol of sol-gel method, transition metals (Ni, Cu, Zn) solution is gelated with tetraethoxysilane (TEOS; silica precursor) using glycerol. Fourier transform infrared spectroscopy (FTIR) spectra revealed bonding of Zn-O, Cu-O, and Ni-O by stretching vibrations at $468cm^{-1}$, $617cm^{-1}$, and $468cm^{-1}$, respectively. Thiophene and Benzothiophene mixed in n-heptane and benzene (4:1) for preparation of Model Fuels I and II, respectively. Each of silica based metal was applied as adsorbent in batch mode to assess the removal efficiency. Results demonstrated optimal desulphurization of more than 90% following efficacy order as Si-Ni > Si-Zn > Si-Cu based adsorbents. Proposed multilayered (Freundlich) adsorption mechanism follows ${\pi}$-complexation with pseudo secnd order kinetics.

Study of Macrophage Activation and Structural Characteristics of Purified Polysaccharides from the Fruiting Body of Hericium erinaceus

  • Lee, Jong-Seok;Min, Kyoung-Min;Cho, Jae-Youl;Hong, Eock-Kee
    • Journal of Microbiology and Biotechnology
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    • v.19 no.9
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    • pp.951-959
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    • 2009
  • Most, if not all, Basidiomycetes mushrooms have biologically active polysaccharides showing potent antitumor activity with immunomodulating properties. These polysaccharides have various chemical compositions and belong primarily to the $\beta$-glucan group. In this study, the crude water-soluble polysaccharide HEF-P, which was obtained from the fruiting body of Hericium erinaceus by hot water extraction and ethanol precipitation, was fractionated by DEAE-cellulose and Sepharose CL-6B column chromatographies. This process resulted in four polysaccharide fractions, named HEF-NP Fr I, HEF-NP Fr II, HEF-AP Fr I, and HEF-AP Fr II. Of these fractions, HEF-AP Fr II was able to upregulate the functional events mediated by activated macrophages, such as production of nitric oxide and expression ofcytokines (IL-1${\beta}$ and TNF-${\alpha}$). The molecular mass of HEF-AP Fr II was estimated by gel filtration to be 13 kDa. Its structural characteristics were investigated by a combination of chemical and instrumental analyses, including methylation, reductive cleavage, acetylation, Fourier transform infrared spectroscopy (FT-IR), and gas chromatography-mass spectrometry (GC-MS). Results indicate that HEF-AP Fr II is a low-molecular-mass polysaccharide with a laminarin-like triple helix conformation of a ${\beta}$-1,3-branched-${\beta}$-1,6-glucan.

Quantitative Mass Spectrometric Analysis of Mixed Self-Assembled Monolayers for Biochips

  • Son, Jin Gyeong;Shon, Hyun Kyong;Hong, Daewha;Choi, Changrok;Han, Sang Woo;Choi, Insung S.;Lee, Tae Geol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.275-275
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    • 2013
  • Formation and characterization of self-assembled monolayers (SAMs) on various surfaces are the essential basis for many other applications, including molecular switches, biosensors, microfluidics, and fundamental studies in surfaces and interfaces. To improve the performance at these applications, it is a key to control the quantity of each molecule in various mixed SAMs on the surface. In this study, using mixed SAM of carbamate-based hydroquinone (HQ)-PhBr and11-mercaptoundecanol, the quantitative mass spectrometric method of mixed SAM was developed based on comparison study with XPS and FT-IR methods. In addition, our method was applied to another mixed SAM of biotinylated PEG alkane thiol and 11-mercaptoundecanol for verification purpose. Time-of-flight secondary mass spectrometry (ToF-SIMS) analysis was performed to identify and quantify each molecule of mixed SAM along with principal component analysis (PCA). Since there is no matrix effect in the X-ray photoelectron spectroscopy (XPS) and Fourier transform-infrared (FT-IR) techniques, we compared ToF-SIMS results with XPS and FT-IR results. Because PCA results from ToF-SIMS analysis are well matched with XPS and FT-IR results from both mixed SAMs, we are expecting that our method will be useful to identify and quantify each molecule in various mixed SAMs.

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Analysis of Heavy Metal Toxic Ions by Adsorption onto Amino-functionalized Ordered Mesoporous Silica

  • Showkat, Ali Md;Zhang, Yu-Ping;Kim, Min-Seok;Gopalan, Anantha Iyengar;Reddy, Kakarla Raghava;Lee, Kwang-Pill
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.1985-1992
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    • 2007
  • Ordered mesoporous silica (MCM-41) materials with different textural properties were prepared using alkyl (dodecyl, cetyl, eicosane) trimethyl ammonium bromide (DTAB, CTAB, ETAB, respectively) as structure directing surfactants, functionalized with amine groups and used as adsorbent for the toxic metal ions, Cr (VI), As (V), Pb (II) and Hg (II). Amino functionalization of mesoporous MCM-41 was achieved by cocondensation of N-[3-(trimethoxysilyl)-propyl] aniline with tetraethyl orthosilicate. Adsorption isotherm and adsorption capacity of the amine functionalized materials for Cr (VI), As (V), Pb (II) and Hg (II) ions were followed by inductively coupled plasma mass spectrometry (ICP-MS). Results demonstrate that amine functionalized MCM-41 prepared with ETAB showed higher adsorption capacity for Cr (VI), As (V), Pb (II) and Hg (II) ions in comparison to MCM-41 prepared with CTAB and DTAB. The higher adsorption capacity for MCM-41(ETAB) was correlated with amine content in the material (determined by CHN analysis) and relative decrease in pore volume and pore diameter. X-ray diffraction (XRD) analysis, nitrogen adsorptiondesorption measurements and Fourier Transform infrared spectrometry (FTIR) were used to follow the changes in the textural parameters and surface properties of the mesoporous materials as a result of amine functionalization to correlate with the adsorption characteristics. The adsorption process was found to depend on the pH of the medium.

Study of Macrophage Activation and Structural Characteristics of Purified Polysaccharide from the Fruiting Body of Cordyceps militaris

  • Lee, Jong-Seok;Kwon, Jeong-Seok;Won, Dong-Pil;Lee, Jung-Hyun;Lee, Keun-Eok;Lee, Shin-Young;Hong, Eock-Kee
    • Journal of Microbiology and Biotechnology
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    • v.20 no.7
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    • pp.1053-1060
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    • 2010
  • Cordyceps militaris, an entomopathogenic fungus belonging to the class Ascomycetes, has been reported to have beneficial biological activities such as hypoglycemic, anti-inflammatory, antitumor, antimetastatic, hypolipidemic, immunomodulatory, and antioxidant effects. In this study, the crude water-soluble polysaccharide CMP, which was obtained from the fruiting body of C. militaris by hot water extraction and ethanol precipitation, was fractionated by DEAE-cellulose and Sepharose CL-6B column chromatographies. This process resulted in three polysaccharide fractions, termed CMP Fr I, CMP Fr II, and CMP Fr III. Of these fractions, CMP Fr II, with an average molecular mass of 127 kDa, was able to upregulate effectively the phenotypic functions of macrophages such as NO production and cytokine expression. The chemical property of the stimulatory polysaccharide, CMP Fr II, was determined based on its monosaccharide composition, which consisted of glucose (56.4%), galactose (26.4%), and mannose (17.2%). Its structural characteristics were investigated by a combination of chemical and instrumental analyses, including methylation, reductive cleavage, acetylation, Fourier transform infrared spectroscopy (FTIR), and gas chromatography-mass spectrometry (GCMS). Results indicated that CMP Fr II consisted of the (1${\rightarrow}$4) or (1${\rightarrow}$2) linked glucopyranosyl or galactopyranosyl residue with a (1${\rightarrow}$2) or (1${\rightarrow}$6) linked mannopyranosyl, glucopyranosyl, or galactopyranosyl residue as a side chain. The configuration of the ${\beta}$-linkage and random coil conformation of CMP Fr II were confirmed using a Fungi-Fluor kit and Congo red reagent, respectively.

Properties of a New Adhesive Composed of Gambir-Sucrose

  • SUCIPTO, Tito;WIDYORINI, Ragil;PRAYITNO, Tibertius Agus;LUKMANDARU, Ganis
    • Journal of the Korean Wood Science and Technology
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    • v.48 no.3
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    • pp.303-314
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    • 2020
  • Gambir is a non-wood forest product with a potential of being used as wood adhesive, due to about 33% catechin in it. Meanwhile, catechins and sucrose have not been studied as adhesives. Therefore, basic characteristics of gambir-sucrose adhesives were investigated. In this research, adhesives were prepared by dissolving gambir and sucrose in distilled water, at different blending ratios of the gambir/sucrose such as 100/0, 75/25, 50/50, and 25/75 wt%. Furthermore, gas chromatography-mass spectrometry (GC-MS) was employed to determine the gambir chemical compositions, and Fourier transform-infrared (FTIR) spectroscopy was carried out to identify chemical bonds. Particleboards with a target density of 0.8 g/㎤ were then manufactured by hot-pressing for 10 min at 200℃. The internal bond (IB) strength of particleboard was subsequently measured. Based on the GC-MS analysis, 31.11% of catechin was identified. In addition, the viscosity, density, solid content, and gelation time of the adhesives, and insoluble matter content (IMC) in boiling water were 7.30~33.24 mPa.s, 1.2~1.3 g/㎤, 25.56~28.44%, 73~420 min, and 29.75~62.10%, respectively. Adding sucrose to the adhesive was observed to raise the IMC from 49.05 to 62.10%, at 180℃ and 200℃. FT-IR analysis showed that the gambir absorption peaks occurred at approximately 1620 cm-1, assigned to the C=O stretching of 5-hydroxymethylfurfural, which tended to increase with the addition of sucrose. The reaction between gambir and sucrose was observed in the form of the dimethylene ether bridge. The 25/75 wt% gambir-sucrose adhesives and 200℃ hot-pressed temperature resulted in the highest IB strength (0.89 MPa), and met the requirement of JIS A5908-2003 type 18. Consequently, the gambir-sucrose adhesive could be used as a particleboard adhesive.

Solubility Enhancement of Flavonols in the Inclusion Complex with Thioether-bridged Dimeric β-Cyclodextrins

  • Cho, Eunae;Jeong, Daham;Paik, Hyun-Dong;Jung, Seunho
    • Bulletin of the Korean Chemical Society
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    • v.35 no.8
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    • pp.2487-2493
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    • 2014
  • Dimeric ${\beta}$-cyclodextrin linked by a thioether bridge was synthesized from a reaction of mono-6-iodo-6-deoxy-${\beta}$-cyclodextrin with sodium sulfide, and the structure was analyzed using nuclear magnetic resonance spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The effects of thioether-bridged dimeric ${\beta}$-CD on the aqueous solubility of flavonols (myricetin, quercetin, and kaempferol) were investigated by ultraviolet-visible spectroscopy. The aqueous solubility of myricetin, quercetin, and kaempferol were enhanced 33.6-, 12.4-, and 10.5-fold following the addition of 9 mM of thioether-bridged dimeric ${\beta}$-CD. In comparison, the aqueous solubility of myricetin, quercetin, and kaempferol were enhanced 5.4-, 3.3-, and 2.7-fold using the same concentration of monomeric ${\beta}$-cyclodextrin. Furthermore, the formation of flavonol/thioether-bridged dimeric ${\beta}$-CD inclusion complexes was confirmed with nuclear magnetic resonance, Fourier-transform infrared spectroscopy, differential scanning calorimetry, and scanning electron microscopy. The results showed that the nature of the complexes significantly differed from that of free flavonols. Herein, we suggest that the thioether-bridged dimeric ${\beta}$-CD can act as an effective complexing agent for flavonols.

Study of PSII-treated PMMA, PHEMA, and PHPMA ; Investigation of Their Surface Stabilities

  • Hyuneui Lim;Lee, Yeonhee;Seunghee Han;Jeonghee Cho;Moojin suh;Kem, Kang-Jin
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.204-204
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    • 1999
  • The plasma source ion implantation(PSII) technique which is a method using high negative voltage pulse in plasma system has the potential to change the surface properties of polymer. PSII technique increase the surface free energy by introducing polar functional groups on the surface so that it improves reactivity, hydrophilicity, adhension, biocompatability, etc. However, the mobility of polymer chains enables the modified surface layers to adapt their composition to interfacial force. This hydrophobic recovery interrupts the stability of modified surfaces to keep for the long time. In this study, poly(methyl methacrylate)(PMMA), poly(2-hydroxyethyl methacrylate)(PHEMA), and polu(2-hydroxypropyl methacylate)(PHPMA) for contact lens application, were modified to improve the wettability with PSII technique and were investigated the surface stabilities. Polymer film was prepared with solution casting(3 wt.% solution) and was annealed at 11$0^{\circ}C$ under vacuum oven to remove solvent completely and to eliminate physical ageing. The thickness of the film measured by scanning electron microscopy (SEM) and surface profilometer was about 10${\mu}{\textrm}{m}$. Polymers were treated with different kinds of gases, pulse frequency, pulse with, pulse voltage, and treatment time. Even though PMMA, PHEMA, and PHPMA have similar repeat unit structure, the optimal treatment conditions and the tendency to hydrophobic recovery were different. PHPMA, more hydrophilic polymer than PMMA and PHEMA showd better wettability and stability after mild treatment. Surface tensions were obtained by water and diiodomethane contact angle measurements to monitor the relation between hydrophobic recovery and polymer structure. Different ion species in plasma change the polar component and dispersion component of polymer surface. For better wettability surface, the increase of polar component was a dominant factor. We also characterized modified polymer surfaces using x-ray photoelectron spectroscopy(XPS), secondary ion mass spectrometry(SIMS), Fourier Transform infrared spectroscopy(FT-IR), and SEM.

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