• Title/Summary/Keyword: elemental analysis

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Preparation and Charecterization of Bromofullerenes in New Stoichiometry

  • Mehrotra, Reema;Lal, Darshan;Tripathi, V.S.;Mathur, G.N.
    • Carbon letters
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    • v.4 no.4
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    • pp.175-179
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    • 2003
  • It is well established that halogenated fullerene derivatives act as synthetic intermediates for further substitution via replacement with nucleophlies. In the present work, systematic studies were carried out on the synthesis of bromofullerenes under different experimental conditions. The effect of reaction time on the product formed was observed. We observed the formation of new compound of bromofullerenes in a different stoichiometric ratio i.e., $C_{60}Br_{14}$; in addition to previous reported bromofullerenes in the stoichiometric ratio of $C_{60}Br_6$, $C_{60}Br_8$, and $C_{60}Br_{24}$. The new derivative of bromofullerene was isolated and well characterized by various analytical techniques like FT-IR, TGA, DSC, and elemental analysis. In this paper, detail of the synthesis and characterization of the bromofullerene prepared are described. The yields obtained were better than those reported previously.

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Synthesis of Silver Nanoparticles from the Decomposition of Silver(I) [bis(alkylthio)methylene]malonate Complexes

  • Lee, Euy-Jin;Piao, Longhai;Kim, Jin-Kwon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.1
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    • pp.60-64
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    • 2012
  • Silver(I) [bis(alkylthio)methylene]malonates were synthesized from the reaction of silver nitrate and potassium [bis(alkylthio)methylene]malonates. The structures of the Ag complexes were characterized with nuclear magnetic resonance (NMR), inductively coupled plasma atomic emission spectrometry (ICP-AES) and elemental analysis. Ag nanoparticles (NPs) were obtained from the decomposition of the Ag complexes in 1,2-dichlorobenzene at $110^{\circ}C$ without an additional surfactant. The average sizes of the Ag NPs are in the range of 5.1-6.3 nm and could be controlled by varying the length of the alkyl chain. The optical properties, crystalline structure and surface composition of Ag NPs were characterized with ultraviolet-visible (UV-visible) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), gas chromatography-mass spectrometry (GC-MS), X-ray Photoelectron Spectroscopy (XPS) and thermal gravimetric analysis (TGA).

Using Microwave Irradiation to Prepare New Poly(amide-imide)s Containing Tetrahydropyrimidinone, Tetrahydro-2-thioxopyrimidine, and Trimellitic Rings in Their Main Chains: Synthesis and Characterization

  • Faghihi Khalil;Hagibeygi Mohsen
    • Macromolecular Research
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    • v.13 no.1
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    • pp.14-18
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    • 2005
  • Under irradiation in a microwave oven, six novel poly(amide-imide)s containing tetrahydropyrimidinone, tetrahydro-2-thioxopyrimidine moieties and trimellitic rings in their main chains were synthesized through the polycondensation reaction of N,N'-(4,4'-diphenylether)bis(trimellitimide) diacid chloride with six different derivatives of tetrahydropyrimidinone and tetrahydro-2-thioxopyrimidine in the presence of a small amount of a polar organic medium, such as o-cresol. The polycondensation proceeded rapidly and completed within 7-9 min, producing a series of new poly(amide-imide)s in high yield that showed inherent viscosities in the range 0.33-0.52 dL/g. These poly(amide-imide)s were characterized by elemental analysis, viscosity measurement, thermal gravimetric analysis, solubility test, and FT-IR spectroscopy. All of the polymers were soluble at room temperature in polar solvents such as N,N-dimethylacetamide, N,N-dimethylformamide, dimethylsulfoxide, tetrahydrofuran, and N-methyl-2-pyrrolidone.

Synthesis, Characterization and Enhanced Selectivity in RP-HPLC of Polar Carbonyl Group Embedded Poly (Vinyl Octadecanoate) Grafted Stationary Phase by Simple Heterogeneous "Graft from" Technique

  • Rana, Ashequl A.;Karim, Mohammad Mainul;Takafuji, Makoto
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.77-82
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    • 2011
  • A new high performance liquid chromatograpgy (HPLC) stationary phase that possesses an internal carbonyl functional group is synthesized by heterogeneous "graft from" method. This new stationary phase, poly (vinyl octadecanoate) grafted silica (Sil-2) is then characterized by different physico-chemical methods such as diffuse reflectance infrared fourier transform, suspension state $^1H$ NMR, solid state $^{13}C$ CP/MAS NMR, $^{29}Si$ CP/MAS NMR, elemental analysis and thermogravimetric analysis. Chromatographic properties of Sil-2 were evaluated under reversed phase condition by separating polycyclic aromatic hydrocarbons (PAHs) and comparing the chromatographic results with those on polymeric as well as monomeric octadecylated silica stationary phases.

Facile mass production of thermally reduced graphene oxide

  • Lee, Seung-Jun;Park, Sung-Jin
    • Carbon letters
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    • v.13 no.1
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    • pp.48-50
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    • 2012
  • Mass production of graphene-based materials, which have high specific surface area, is of importance for industrial applications. Herein, we report on a facile approach to produce thermally modified graphene oxide (TMG) in large quantities. We performed this experiment with a hot plate under environments that have relatively low temperature and no using inert gas. TMG materials showed a high specific surface area (430 $m^2g^{-1}$). Successful reduction was confirmed by elemental analysis, X-ray photoelectron spectroscopy, thermogravimetic analysis, and X-ray diffraction. The resulting materials might be useful for various applications such as in rechargeable batteries, as hydrogen storage materials, as nano-fillers in composites, in ultracapacitors, and in chemical/bio sensors.

Synthesis and Antimicrobial Evaluation of Some Novel 2-(4-Chlorophenylimino) thiazolidin-4-one Derivatives

  • B'Bhatt, H.;Sharma, S.
    • Journal of the Korean Chemical Society
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    • v.56 no.3
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    • pp.341-347
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    • 2012
  • A series of 2-(4-chlorophenylimino)-5-((3-(p-substituted phenyl)-1-phenyl-1H-pyrazol-4-yl) methylene) thiazolidin-4-one ($\mathbf{3a-h}$) compounds were prepared from the 2-(4-chlorophenylimino) thiazolidin-4-one ($\mathbf{1}$) and 1-phenyl-3-(p-substituted phenyl)-1H-pyrazole-4-carbaldehyde ($\mathbf{2a-h}$). All compounds were characterized by elemental (C, H, N) analysis and spectral (FT-IR, $^1H$ NMR and GC-MS) analysis. These newly synthesized compounds were screened for their antibacterial and antifungal activities. Antimicrobial activity was observed and evaluated against the bacterial strains like Eschericha coli (MTCC 443), Pseudomonas aeruginosa (MTCC 1688), Staphylococcus aureus (MTCC 96), Streptococcus pyogenes (MTCC 442) and against the fungal strains like Candida albicans (MTCC 227), Aspergillus niger (MTCC 282) and Aspergillus clavatus (MTCC 1323). All the synthesized compounds were found to possess moderate to excellent antimicrobial activity against above selected strains.

Synthesis and Characterization of Transition Metal Complexes with Benzimidazolyl-2-hydrazones of o-anisaldehyde and Furfural

  • Mohapatra, R.K.;Mishra, U.K.;Mishra, S.K.;Mahapatra, A.;Dash, D.C.
    • Journal of the Korean Chemical Society
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    • v.55 no.6
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    • pp.926-931
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    • 2011
  • A series of complexes of the type [$ML_2Cl_2$], where L=2-(o-anisylidene-2'-imino) amino benzimidazole (AIAB) and 2-(furfurylidene imino) amino benzimidazole (FIAB), M=Cu(II), Co(II), Ni(II) and Zn(II), have been synthesized and characterized on the basis of elemental analysis, thermal analysis, molar conductivity, magnetic moment, electronic, infrared, $^1H$-NMR spectral studies. The results are in consistent with bidentate chelation of ligand with azomethine nitrogen and ring nitrogen donors. All these Schiff bases and their complexes have also been screened for their antibacterial (Bacillus subtilis, Bacillus stearothermophilus, Escherichia coli and Salmonella typhi) and antifungal activities (Aspergillus niger and Aspergillus flavus).

Synthesis and Structure of Benzotriazolyl Fluorenes

  • KohPark, Kwang-Hee;Jung, Hye-Mi;Lee, Tae-Woo;Kang, Sung-Kwon
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.984-988
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    • 2010
  • 1-(Fluoren-2-yl)-benzo[d][1,2,3]triazoles 5a-b were synthesized starting from 2-nitrofluorene. 2-Nitrofluorenes 1a-b were reduced by catalytic hydrogenation, reacted with 2,4-dinitrofluorobenzene followed by catalytic hydrogenation to afford 2-(N-2,4-diaminophenyl)aminofluorenes 4a-b. Diazotization of 4a-b with $NaNO_2/H_2SO_4$ followed by treatment with $H_3PO_2$ gave 5a-b. Sulfonation of 5a-b yielded 7-benzotriazol-1-yl-fluorene-2-sulfonic acids 6a-b. The structures of 5b and 6b were firmly identified by X-ray crystal analysis in addition to $^1H$ NMR, $^{13}C$ NMR, and elemental analysis.

State-space formulation for simultaneous identification of both damage and input force from response sensitivity

  • Lu, Z.R.;Huang, M.;Liu, J.K.
    • Smart Structures and Systems
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    • v.8 no.2
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    • pp.157-172
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    • 2011
  • A new method for both local damage(s) identification and input excitation force identification of beam structures is presented using the dynamic response sensitivity-based finite element model updating method. The state-space approach is used to calculate both the structural dynamic responses and the responses sensitivities with respect to structural physical parameters such as elemental flexural rigidity and with respect to the force parameters as well. The sensitivities of displacement and acceleration responses with respect to structural physical parameters are calculated in time domain and compared to those by using Newmark method in the forward analysis. In the inverse analysis, both the input excitation force and the local damage are identified from only several acceleration measurements. Local damages and the input excitation force are identified in a gradient-based model updating method based on dynamic response sensitivity. Both computation simulations and the laboratory work illustrate the effectiveness and robustness of the proposed method.

Resolution Analysis of Axially Distributed Image Sensing Systems under Equally Constrained Resources

  • Cho, Myungjin;Shin, Donghak
    • Journal of the Optical Society of Korea
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    • v.17 no.5
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    • pp.405-409
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    • 2013
  • In this paper, a unifying framework to evaluate the depth resolution of axially distributed image sensing (ADS) systems under fixed resource constraints is proposed. The proposed framework enables one to evaluate the system performance as a function of system parameters such as the number of cameras, the number of pixels, pixel size, and so on. The Monte Carlo simulations are carried out to evaluate ADS system performance as a function of system parameters. To the best of our knowledge, this is the first report on quantitative analysis of ADS systems under fixed resource constraints.