• Title/Summary/Keyword: elemental analysis

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Sythesis and Characterization of Transition Metal(II) Complexes with $NOTDH_2$ Schiff Base ($NOTDH_2$ Schiff Base를 가진 전이금속(II) 착물의 합성과 구조분석)

  • Oh, Jeong-Geun;Choi, Yong-Kook
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.498-503
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    • 1999
  • Co(II), Ni(II), and Cu(II) complexes with tetradentate schiff base-$NOTDH_2$, were synthesized. The structures of these complexes were characterized by elemental analysis, IR, UV-visible, NMR spectra, and thermogravimetric analysis. The mole ratio of schiff base($NOTDH_2$) to the metal(II) at complexes was found to be 1:1. Cu(II) complexes were four-coordinated configuration, while Co(II) and Ni(II) complexes were hexacoordinated configuration containing two water molecules and all complexes were non-ionic compounds.

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An Orchestrated Attempt to Determine the Chemical Properties of Asian Dust Particles by PIXE and XRF Techniques

  • Ma, Chang-Jin;Kim, Ki-Hyun;Choi, Sung-Boo;Kasahara, Mikio;Tohno, Susumu
    • Asian Journal of Atmospheric Environment
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    • v.4 no.3
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    • pp.189-197
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    • 2010
  • An orchestrated attempt was made to analyze samples of bulk and individual particulate matters (PM) collected at the Gosan ground-based station on the west coast of Jeju, Korea. A two-stage filter pack sampler was operated to collect particles in both large (> $1.2\;{\mu}m$) and small size fractions (< $1.2\;{\mu}m$) between the Asian dust (hereafter called "AD") storm event and non-Asian dust period. Elemental components in bulk and individual particles were determined by PIXE and synchrotron XRF analysis systems, respectively. To assess the transport pathways of air parcels and to determine the spatial distribution of PM, the backward trajectories of the Meteorological Data Explorer (Center for Global Environmental Research, 2010) and the NOAA's HYSPLIT dispersion-trajectory models were applied. In line with general expectations, Si and other crustal elements in large size particles showed considerably higher mass loading on AD days in comparison with non-AD days. Computation of the crustal enrichment factors [(Z/Si)$_{particle}$/(Z/Si)$_{desert}$ sand] of elements in large size particles (> $1.2\;{\mu}m$) allowed us to estimate the source profile and chemical aging of AD particles as well as to classify the soil-origin elements. On the basis of a single particle analysis, individual AD particles are classified into three distinct groups (neutralized mineral particles, S-rich mineral particles, and imperfectly neutralized particles).

The Syntheses, Characterizations, and Photocatalytic Activities of Silver, Platinum, and Gold Doped TiO2 Nanoparticles

  • Loganathan, Kumaresan;Bommusamy, Palanisamy;Muthaiahpillai, Palanichamy;Velayutham, Murugesan
    • Environmental Engineering Research
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    • v.16 no.2
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    • pp.81-90
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    • 2011
  • Different weight percentages of Ag, Pt, and Au doped nano $TiO_2$ were synthesized using the acetic acid hydrolyzed sol-gel method. The crystallite phase, surface morphology combined with elemental composition and light absorption properties of the doped nano $TiO_2$ were comprehensively examined using X-ray diffraction (XRD), $N_2$ sorption analysis, transmission electron microscopic (TEM), energy dispersive X-ray, and DRS UV-vis analysis. The doping of noble metals stabilized the anatase phase, without conversion to rutile phase. The formation of gold nano particles in Au doped nano $TiO_2$ was confirmed from the XRD patterns for gold. The specific surface area was found to be in the range 50 to 85 $m^2$/g. TEM images confirmed the formation a hexagonal plate like morphology of nano $TiO_2$. The photocatalytic activity of doped nano $TiO_2$ was evaluated using 4-chlorophenol as the model pollutant. Au doped (0.5 wt %) nano $TiO_2$ was found to exhibit higher photocatalytic activity than the other noble metal doped nano $TiO_2$, pure nano $TiO_2$ and commercial $TiO_2$ (Degussa P-25). This enhanced photocatalytic activity was due to the cathodic influence of gold in suppressing the electron-hole recombination during the reaction.

Characterization of Size Distribution and Water Solubility of 15 Elements in Atmospheric Aerosols

  • Park, Jeong-Ho;Sun, Jeong-Min;Park, Kum-Chan
    • Journal of Korean Society for Atmospheric Environment
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    • v.17 no.E1
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    • pp.1-7
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    • 2001
  • The elemental characteristics of atmospheric aerosols were investigated as a function of particle size and water solubility. The aerosol particles were samples at 12 individual size ranges between 0.01 and 30㎛. Collected aerosol particles were separated into both soluble and insoluble components. The concentrations of 15 elements in both components were determined by a PIXE analysis using a 2.0 MeV-proton beam. In general, the mass size distribution of particulate matter was represented as a bimodal distribution. The maximum rations of S in July and December were 5.5 and 3.8 %, and they appeared in the size range of 0.47∼1.17㎛(stage No. 6 or 7) . The ratios of a S at non-separated size were 3.1 and 2.2 % in July and December, respectively, On the other hand, the maximum rations of Si in July and December were 7.0 and 5.4% and they appeared in the size range of 5.1∼30㎛(stage No. 0∼2). The ratios of Si at the non-separated size were 2.1 and 1.8% in July and December, respectively, The mass diameter of 12 elements ranged between 0.59㎛ of S and 3.20 of Fe. More than 90% of atmospheric aerosols consisted of the light elements such as C, N, O, H and Al. The soluble component was dominant in the smaller size range and the insoluble component in the larger size range. Large portions of Si. Ti and Fe existed in insoluble state. By contrast, S, Cl, Ca, Zn and Br were dissolved in water.

According to the type of commercial antifreeze experimental study of vehicle emissions (상용부동액 종류에 따른 자동차 배출가스의 실험적 연구)

  • Hong, Sung-In
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.15 no.6
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    • pp.4002-4006
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    • 2014
  • The automotive exhaust gases generated by the vehicles containing carbon monoxide, hydrocarbons and lead, is a large concern because of their harm to human health or the living environment. To reduce exhaust gas, it is important to develop a variety of techniques that are currently being used by elemental analysis to determine the optimal conditions. In this study, the anti-freeze coolant contained in the exhaust gas was examined, which can affect the emissions. The effects of the commercially available coolant from five domestic companies on the HC, NOx and $CO_2$ emissions were analyzed to determine the optimal amount of antifreeze. In addition, antifreeze products from the five companies were analyzed with respect to driving time of the cooling fan and the correlation of the NOx emission analysis. The temperature of the engine oil was matched using a manual gear of small passenger inspection standard speed $40{\pm}2Km/h$ so the vehicle could meet the specifications for inspection $90{\sim}93^{\circ}C$. The Company D fan operation time resulted in the shortest antifreeze, $CO_2$ and NOx emissions.

${\alpha},{\omega}$-Bis[4-(4'(S)-(+)-2-methylbutylbiphenyl-4-carboxy)phenoxy]alkanes-Synthesis and Liquid Crystalline Properties of New Dimesogenic Compounds (${\alpha},{\omega}$-비스[4-(4'-(S)-(+)-2-메틸부틸비페닐-4-카르복시)페녹시]알칸 -새로운 디메소겐 화합물의 합성 및 액정성)

  • Kim, Jae Hoon;Lee, Soo Min;Jin, Jung Il
    • Journal of the Korean Chemical Society
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    • v.42 no.6
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    • pp.679-695
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    • 1998
  • A series of ${\alpha}{\omega}-bis[4-(4'-(S)-(+)-2-methylbutylbiphenyl-4-carboxy)phenoxy]alkanes$, were synthesized, and their thermal and liquid crystalline properties were studied. The chain length of the central polymethylene spacers, x, of the chiral twin compounds was varied from 3 to 12. These compounds were characterized by elemental analysis, IR and NMR spectroscopy, differential thermal analysis (DSC), and crosspolarized microscopy. All compounds were found to be enantiotropic liquid crystalline, and the values of melting $(T_m)$ and isotropization temperature $(T_i)$ as well as ${\delta}H_I$ and ${\delta}S_I$ decreased in a zig-zag fashion, revealing the so called odd-even effect as x increased. Their mesomorphic properties fell into four categories depending upon x; (a) compounds with x=3, 4 and 5 formed only a cholesteric phase on heating, while on cooling they went through two transitions of isotropic (I)-to-cholesteric (Ch) and Ch-to-smectic $A\;(S_A)$ phases before crystallization. (b) compounds with x=6, 8 and 10 exhibited only a cholesteric phase both on heating and on cooling. (c) compounds with x=7 and 9 went through three transitions of crystal $(C)-to-S_A,\;S_A-to-Ch,$ and Ch-to-I phases on heating while on cooling they went through four transitions of I-to-Ch, $Ch-to-S_A,\;S_A-to-Smectic\;C\;(S_C),\;and\;S_c-to-C$ phases in that order, and (d) compounds with x=11 and 12 went reversibly through four transitions of $C-to-S_C,\;S_C-to-S_A,\;S_A-to-Ch,$ and Ch-to-I phases.

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Cr(III)-Tetraaza Macrocyclic Complexes Containing Auxiliary Ligands (Part IV); Synthesis and Characterization of Cr(III)-Acetylacetonato, -Malonato and -Oxalato Macrocyclic Complexes

  • Byun, Jong-Chul;Han, Chung-Hun
    • Bulletin of the Korean Chemical Society
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    • v.26 no.9
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    • pp.1395-1402
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    • 2005
  • The reaction of cis-[Cr([14]-decane)$(OH)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = acetylacetonate (acac), oxalate (ox) or malonate (mal)} leads to a new cis-[Cr([14]-decane)(acac)]$(ClO_4)_2{\cdot}(1/2)H_2O\;(1),\;cis-[Cr([14]-decane)(ox)]ClO_4{\cdot}(1/2)H_2O\;(2)\;or\;cis-[Cr([14]-decane)(mal)]ClO_4{\cdot}(1/4)H_2O\;(3)$. These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[Cr([14]-decane)(acac)]$(ClO_4)_2{\cdot}(1/2)H_2O$ reveals that central chromium(III) has a distorted octahedral coordination environment and two acetylacetonate-oxygen atoms are bonded to the chromium(III) ion in the cis positions. The angle $N_{axial}-Cr-N_{axial}$ deviates by $11^{\circ}$ from the ideal value of $180^{\circ}$ for a perfect octahedron. The bond angle O-Cr-O between the chromium(III) ion and the two acetylacetonate-oxygen atoms is close to $90^{\circ}$. The bond lengths of Cr-O between the chromium and the acetylacetonate-oxygen atoms are 1.950(3) and 1.954(2) $\AA$. They are shorter than those between chromium and nitrogen atoms of the macrocycle. The IR spectra of 1, 2 and 3 display bands at 1560 {ν (C=O)}, 1710 {${\nu}_{as}$(OCO)} and 1660 $cm^{-1}$ {${\nu}_{as}$(OCO)} attributed to the acac, ox and mal auxiliary ligands stretching vibrations, respectively.

Cr(III)-Tetraaza Macrocyclic Complexes Containing Auxiliary Ligands (Part II); Synthesis and Characterization of Cr(III)-Citrato Macrocyclic Complex

  • Byun, Jong-Chul;Park, Yu-Chul;Youn, Jeung-Su;Han, Chung-Hun;Lee, Nam-Ho
    • Bulletin of the Korean Chemical Society
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    • v.26 no.4
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    • pp.634-640
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    • 2005
  • The reaction of cis-[Cr([14]-decane)(OH$_2)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = citrate(cit)} leads to a new dimeric complex cis-[{Cr([14]-decane)($\mu$-cit)}$_2](ClO_4)_2$. This binuclear complex has been structurally characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[{Cr([14]-decane)($\mu$-cit)})($_2]^+$ reveals that each chromium has a distorted octahedral coordination environment and citrato ligands are monodentate to the two chromium atoms via the carboxyl groups. For dimeric complex the bridging geometry is as follows: Cr$\ldots$Cr = 7.361 $\AA$; Cr-O(average) = 1.958 (8) $\AA$; Cr-N range = 2.108 (9)-2.147(9) $\AA$; N(1)-Cr-N(3) (equatorial position) = 98.0(4)$^{\circ}$; N(2)-Cr-N(4) (axial position) = 166.4(4)$^{\circ}$; O(1)-Cr-N(2) = 98.1(4)$^{\circ}$; O(3)-Cr-N(4) = 96.6(3)$^{\circ}$; O(1)-Cr-O(3) = 90.4$^{\circ}$. The FAB mass spectrum of the dimeric complex displays peak due to the molecular ions cis-[{Cr([14]-decane)($\mu$-cit)})($_2]^+$ at m/z 1053.

Crystal Structure, Fluorescence Property and Theoretical Calculation of the Zn(II) Complex with o-Aminobenzoic Acid and 1,10-Phenanthroline

  • Zhang, Zhongyu;Bi, Caifeng;Fan, Yuhua;Zhang, Xia;Zhang, Nan;Yan, Xingchen;Zuo, Jian
    • Bulletin of the Korean Chemical Society
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    • v.35 no.6
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    • pp.1697-1702
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    • 2014
  • A novel complex [$Zn(phen)(o-AB)_2$] [phen: 1,10-phenanthroline o-AB: o-aminobenzoic acid] was synthesized and characterized by elemental analysis and X-ray diffraction single-crystal analysis. The crystal crystallizes in monoclinic, space group P2(1)/c with $a=7.6397(6){\AA}$, $b=16.8761(18){\AA}$, $c=17.7713(19){\AA}$, ${\alpha}=90^{\circ}$, ${\beta}=98.9570(10)^{\circ}$, ${\gamma}=90^{\circ}$, $V=2.2633(4)nm^3$, Z = 4, F(000) = 1064, S = 1.058, $Dc=1.520g{\cdot}cm^{-3}$, $R_1=0.0412$, $wR_2=0.0948$, ${\mu}=1.128mm^{-1}$. The Zn(II) is six coordinated by two nitrogen and four oxygen atoms from the 1,10-phenanthroline and o-aminobenzoic acid to furnish a distorted octahedron geometry. The complex exhibits intense fluorescence at room temperature. Theoretical studies of the title complex were carried out by density functional theory (DFT) B3LYP method. CCDC: 898291.

Influence of Preparation Conditions on the Formation of Copper (II) Architectures with Pyrazine-2,3,5-tricarboxylic Acid

  • Wang, Feng-Qin;Lin, Shu;Guo, Ming-Lin;Xu, Jun-Jian;Wang, Xiao-Qing;Zhao, Yong-Nan
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2351-2357
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    • 2011
  • Three new metal-organic copper(II) complexes, $[Cu(H_2PZTC)_2]_n{\cdot}2nH_2O$ (1), $[Cu(HPZTC){\cdot}2H_2O]_n{\cdot}2nH_2O$ (2), and $Cu_2[(PZHD)(OH)(H_2O)_2]_n$ (3) ($H_3PZTC$ = pyrazine-2,3,5-tricarboxylic acid, $PZHD^{3-}$ = 2-hydroxypyrazine-3,5-dicarboxylate), have been synthesized from $Cu(II)/H_3PZTC$ system under different synthetic conditions, and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy and thermogravimetric analysis. In complexes 1 and 2, $H_3PZTC$ ligands loose one and two protons, which were transformed into $H_2PZTC^-$ anion and $HPZTC^{2-}$ dianion under different preparation condition, respectively. Furthermore, two ligands coordinate with Cu(II) cations in different modes, leading to the formation of the different chain structures. In complex 3, $H_3PZTC$ ligand was converted into a new ligand-PZHD by in situ decarboxylation and hydroxylation under a higher pH value than that for complexes 1 and 2. PZHD ligands link the Cu(II) cations to form a 2D layer structure. These results demonstrate that the preparation conditions, including pH value and reaction temperature etc, play an important role in the construction of complexes based on $H_3PZTC$ ligand.