• Title/Summary/Keyword: magnetic susceptibility analysis

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Synthesis and Characterization of Some Transition Metal Complexes of Unsymmetrical Tetradentate Schiff Base Ligand (비대칭 Tetradentate Schiff 염기 리간드의 전이금속 착물에 대한 합성 및 특성)

  • Munde, A. S.;Jagdale, A. N.;Jadhav, S. M.;Chondhekar, T. K.
    • Journal of the Korean Chemical Society
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    • v.53 no.4
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    • pp.407-414
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    • 2009
  • The solid complexes of Cu(II), Ni(II), Co(II), Mn(II) and Fe(III) with 4-hydroxy-3-(1-{2-(2-hydroxybenzylidene)- amino phenylimino}-ethyl)-6-methy-pyran-2-one (H2L) derived from o-phenylenediamine, 3-acetyl- 6-methyl-(2H) pyran, 2,4 (3H)-dione (dehydroacetic acid or DHA) and salicylic aldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, IR, $^1H$-NMR spectra, X-ray diffraction, thermal analysis, and screened for antimicrobial activity. The IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests square planar geometry for Cu(II) and Ni(II) complexes and octahedral geometry for Co(II), Mn(II) and Fe(III) complexes. The x-ray differaction data suggests orthorhombic crystal system for Cu(II) complex, monoclinic crystal system for Ni(II), Co(II) and Fe(III) and tetragonal crystal system for Mn(II) complex. Thermal behaviour (TG/DTA) of the complexes was studied and kinetic parameters were determined by Coats-Redfern method. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus Niger and Trichoderma.

Synthesis and Characterization of Tetradentate N2O2 Schiff Base Ligand and its Rare Earth Metal Complexes (사배위 N2O2 Schiff 염기 리간드와 그 희토류 금속착물의 합성 및 특성)

  • Shelke, Vinod A.;Jadhav, Sarika M.;Shankarwar, Sunil G.;Munde, chut S.;Chondhekar, Trimbak K.
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.436-443
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    • 2011
  • The solid complexes of La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) with 4-hydroxy-3-(1-{2-(2,4-dihydroxy-benzylidene)-amino phenylimino}-ethyl)-6-methyl-pyran-2-one ($H_2$L) derived from o-phenylenediamine, 3-acetyl-6-methyl-(2H)pyran,2,4(3H)-dione (dehydroacetic acid or DHA) and 2, 4-dihydroxy benzaldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, FT-IR, $^1H$-NMR, X-ray diffraction, thermal analysis study, and screened for antimicrobial activity. The FT-IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests distorted octahedral geometry for La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) complexes. The X-ray diffraction data suggests monoclinic crystal system for La(III) and Ce(III) and orthorombic crystal system for Pr(III) and Nd(III) complexes. Thermal behavior (TG/DTA) of the complexes was studied and kinetic parameters were determined by Horowitz-Metzger and Coats-Redfern methods. The ligand and its metal complexes were screened for antibacterial activity against Staphylococcus aureus, Escherichia coli, Bacillus Sp. and fungicidal activity against Aspergillus Niger, Trichoderma and Fusarium oxysporum.

Complex Formation of Transition and Post-Transition Metal Ions with 1,15-Diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacyclooctadecane (전이 및 중금속이온과 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxa-cyclooctadecane과의 착물형성)

  • Kim, Si-Joong;Lee, Myung-Jae;Koo, Chang-Hyung;Woo, Kyoun-Ja
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.645-652
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    • 1991
  • The stability constants$(K_f)$ of the complexes of some transition and post-transition metal ions (Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ), Zn(Ⅱ), Cd(Ⅱ), Pb(Ⅱ), Hg(Ⅱ)) with $N_2O_3$-donor macrocyclic ligand, 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacyclooctadecane ($NtnOdienH_4$), have been determined by potentiometry in aqueous solution at $25^{\circ}C$. Log $K_f$ values of the complexes were : Co(Ⅱ): 3.83, Ni(Ⅱ) : 4.56, Cu(Ⅱ) : 7.74, Zn(Ⅱ) : 4.98, Cd(Ⅱ) : 3.91, Pb(Ⅱ) : 6.65, and Hg(Ⅱ) : 14.87. The order of stabilities of transition metal complexes was the same as the natural order of stability proposed by Williams-Irving. In post-transition metal complexes, the order of stabilities was Cd(Ⅱ) < Pb(Ⅱ) < Hg(Ⅱ), and the covalent character in metal ion-donor atoms bonds appeared a dominant factor in the stability. In methanol solution, each metal ion forms 1 : 1 complex, while Ni(Ⅱ) ion forms both 1 : 1 and 1 : 2 complexes. It was confirmed by $^1H-$ and $^{13}C-$NMR spectral study that the nitrogen atoms in the ligand were major contributors for the complexation of post-transition metal ions with the ligand. It was shown, by elementry analysis, electrical conductivity and magnetic susceptibility measurements, and spectral analysis, that solid Cu(Ⅱ)-and Zn(Ⅱ)-complexes have a distorted octahedral and a tetrahedral structure, respectively.

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Synthesis, Potentiometric, Spectral Characterization and Microbial Studies of Transition Metal Complexes with Tridentate Ligand (세자리 리간드의 전이금속 착물에 대한 합성과 전위차 및 분광학적 확인 그리고 미생물학적 연구)

  • Jadhav, S.M.;Munde, A.S.;Shankarwar, S.G.;Patharkar, V.R.;Shelke, V.A.;Chondhekar, T.K.
    • Journal of the Korean Chemical Society
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    • v.54 no.5
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    • pp.515-522
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    • 2010
  • A relation between antimicrobial activities and the formation constants of solid complexes of Cu(II), Ni(II), Co(II), Mn(II) and Fe(III) with tridentate Schiff base ligand, 4-hydroxy-3(1-{2-(benzylideneamino)-phenylimino}-ethyl)-6-methyl-2Hpyran-2-one (HL) derived from o-phenylene diamines, dehydroacetic acid (DHA) and p-chloro benzaldehyde have been studied. The ligand and metal complexes were characterized by elemental analysis, conductivity, magnetic susceptibility, thermal analysis, X-ray diffraction, IR, $^1H$-NMR, UV-vis and mass spectra. From the analytical data, the stiochiometry of the complexes was found to be 1:2 (metal:ligand) with octahedral geometry. The molar conductance values suggest the nonelectrolytic nature of metal complexes. The X-ray diffraction data suggests monoclinic crystal system for Ni(II) and orthorhombic crystal system for Cu(II) and Co(II) complexes. The IR spectral data suggest that the ligand behaves as tridentate ligand with ONN donor atoms sequence towards central metal ion. Thermal behavior (TG/DTA) and kinetic parameters calculated by Coats-Redfern method suggests more ordered activated state in complex formation. The protonation constants of the complexes were determined potentiometrically in THF:water (60:40) medium at $25^{\circ}C$ and ionic strength ${\mu}=0.1\;M$ ($NaClO_4$). Antibacterial activities in vitro were performed against Staphylococcus aureu and Escherichia coli. Antifungal activities were studied against Aspergillus Niger and Trichoderma. The effect of the metal ions and stabilities of complexes on antimicrobial activities are discussed.

Petrological Classification and Provenance Interpretation of the Sungnyemun Stone Block Foundation, Korea PDF icon (숭례문 육축 구성석재의 암석학적 분류와 원산지 해석)

  • Jo, Young Hoon;Lee, Chan Hee;Yoo, Ji Hyun;Kang, Myeong Kyu;Kim, Duk Mun
    • Korean Journal of Heritage: History & Science
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    • v.45 no.3
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    • pp.174-193
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    • 2012
  • This study focused on distribution ratio of stone properties based on material characteristic analysis, provenance presumption and transportation route interpretation of the Sungnyemun stone block foundation. The stone block foundation is composed of pinkish granite (56.0%), reddish granite (4.5%) and leucocratic granite (26.2%) of original stones and pinkish granite of new stones(13.3%). The rock-forming minerals for granites are consisted mainly of quartz, alkali-feldspar, plagioclase and biotite, and are similar geochemical evolution trend of major, rare earth, compatible and incompatible elements. Therefore, it is clear that the rocks are genetically same origin. As a result of magnetic susceptibility measurement, the pinkish and reddish granite of original stones and pinkish granite of new stones showed normal distribution around about 4.00(${\times}10^{-3}SI\;unit$). But the leucocratic granite of original stones were confirmed ilmenite series under about 1.00(${\times}10^{-3}SI\;unit$). As a result of provenance interpretation and transportation route analysis based on the petrological results, the provenance of pinkish granite and reddish granite of original stones are presumed the north slope in Namsan mountain and Naksan mountain. Also, the leucocratic granite of original stones and the pinkish granite of new stones are strongly possible furnished from the south and north slope in Namsan mountain and Naksan mountain, respectively.

Engraftment of Human Mesenchymal Stem Cells in a Rat Photothrombotic Cerebral Infarction Model : Comparison of Intra-Arterial and Intravenous Infusion Using MRI and Histological Analysis

  • Byun, Jun Soo;Kwak, Byung Kook;Kim, Jae Kyun;Jung, Jisung;Ha, Bon Chul;Park, Serah
    • Journal of Korean Neurosurgical Society
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    • v.54 no.6
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    • pp.467-476
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    • 2013
  • Objective : This study aimed to evaluate the hypotheses that administration routes [intra-arterial (IA) vs. intravenous (IV)] affect the early stage migration of transplanted human bone marrow-derived mesenchymal stem cells (hBM-MSCs) in acute brain infarction. Methods : Male Sprague-Dawley rats (n=40) were subjected to photothrombotic infarction. Three days after photothrombotic infarction, rats were randomly allocated to one of four experimental groups [IA group : n=12, IV group : n=12, superparamagnetic iron oxide (SPIO) group : n=8, control group : n=8]. All groups were subdivided into 1, 6, 24, and 48 hours groups according to time point of sacrifice. Magnetic resonance imaging (MRI) consisting of T2 weighted image (T2WI), $T2^*$ weighted image ($T2^*WI$), susceptibility weighted image (SWI), and diffusion weighted image of rat brain were obtained prior to and at 1, 6, 24, and 48 hours post-implantation. After final MRI, rats were sacrificed and grafted cells were analyzed in brain and lung specimen using Prussian blue and immunohistochemical staining. Results : Grafted cells appeared as dark signal intensity regions at the peri-lesional zone. In IA group, dark signals in peri-lesional zone were more prominent compared with IV group. SWI showed largest dark signal followed by $T2^*WI$ and T2WI in both IA and IV groups. On Prussian blue staining, IA administration showed substantially increased migration and a large number of transplanted hBM-MSCs in the target brain than IV administration. The Prussian blue-positive cells were not detected in SPIO and control groups. Conclusion : In a rat photothrombotic model of ischemic stroke, selective IA administration of human mesenchymal stem cells is more effective than IV administration. MRI and histological analyses revealed the time course of cell migration, and the numbers and distribution of hBM-MSCs delivered into the brain.

Material Characteristics and Clay Source Interpretation of Crucibles in Baekje Kingdom Excavated from the Ssangbukri Site in Buyeo, Korea (부여 쌍북리 유적 출토 백제 도가니의 재료학적 특성과 원료의 산지해석)

  • Kim, Ji-Young;Park, Jin-Young;Park, Dae-Sun;Lee, Chan-Hee
    • Journal of Conservation Science
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    • v.26 no.1
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    • pp.1-12
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    • 2010
  • The crucibles of Baekje Kingdom from the Ssangbukri Site which were used for glass and metal melting had light brown, grayish blue and grayish brown colored bodies. In thin section, the crucibles contained numerous quartz grains and pottery fragments. The surface was covered with fine grained quartz for thermal resistance. Based on decomposition of mica group minerals and formation of mullite detected by X-ray diffraction analysis, it was inferred that all crucibles have been fired over $1,000^{\circ}C$. It was also found that firing temperature has exceeded $1,100^{\circ}C$ in some crucibles because feldspar was not detected. The maximum temperature was assumed at $1,200^{\circ}C$. The magnetic susceptibility values and geochemical characteristics sorted out the crucibles into two groups that differed from the characteristics of the local soils. This reflected geological setting of the site where the alluvium was formed from two kinds of surrounding rock masses, granite gneiss and biotite granite. However, the local soils had similarities with the crucibles in weathering degree and geochemical behavior of major elements. In consequence, it was considered that the raw clay of the crucibles was supplied from the local area of the site.

Study on Material Characteristics and Firing Temperature of Jar Coffins from Oryang-dong Kiln Site and Jeongchon Tomb, Naju, Korea (나주 오량동 유적 및 정촌 고분 출토 옹관의 재료적 특성 및 소성온도 연구)

  • Kim, Su Kyoung;Jin, Hong Ju;Jang, Sungyoon
    • Journal of Conservation Science
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    • v.34 no.3
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    • pp.179-193
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    • 2018
  • This study is aimed to investigate the provenance of raw materials and firing temperature of jar coffins excavated from the Oryang-dong kiln site and Jeonchon tomb site, Naju, Korea. Most of jar coffin samples shows same range of magnetic susceptibility and have gray color, while 404 and 405 of Jeongchon site are reddish yellow. In some samples fired at high temperature, the water absorption at the mouth rim and body part of same jar coffin were 3.50% and 7.56% respectively. It means that heat transfer and equilibrium in the kiln was not properly continued and the heat energy transferred to the mouth rim and the body part was different. In the petrographic analysis, As a tempering materials, biotite, weathered quartz and feldspar were added in the jar coffins of Oryang-dong site, and biotite, polycrystalline quartz and feldspar in it of Jeongchon site. Tempering materials were found more in the body than in the mouth rim of same jar coffin of Oryang-dong site. It seemed that some samples were fired at over 1,000 to $1,100^{\circ}C$, which showed vitrified texture in the scanning electron images and the rest of samples were fired at below $900^{\circ}C$. Due to similarity of chemical compositions, it is estimated that jar coffins of Jeongchon tomb were produced and supplied from Oryang-dong kiln site. However, the slight difference of some trace elements distribution of samples is attributed to the selection of clay depending on the location.

Material Analysis and Surface Condition Monitoring of Standing Buddha Statue in the Gwanchoksa Temple, Nonsan, Korea (논산 관촉사 석조미륵보살입상의 재질분석과 표면상태 변화 모니터링)

  • Lee, Myeong Seong;Choie, Myoungju;Yoo, Ji Hyun;Ahn, Yu Bin
    • The Journal of the Petrological Society of Korea
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    • v.28 no.4
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    • pp.227-236
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    • 2019
  • Medium to coarse-grained biotite granodiorite was used to build the Standing Buddha Statue in the Gwanchoksa temple. An ancient document revealed the period and place of constructing the statue: it was made in the northwest of Mt. Banyasan and then moved eastward. Also, the comparison of standing Buddha statue and basement rock in terms of texture, magnetic susceptibility, and gamma spectrometer shows that they have similar characteristics, which is considered to be the same provenance rock. The damage caused by surface contaminants observed in the statue seems to be a combined effect of environmental factors and aging of the epoxy resin. After removal of the contaminants in 2007, the contamination has resumed, and continuous monitoring is necessary. Algal engraftment becomes faster when biological contamination occurs on the surface of stone cultural heritage. Since the secondary lichen growth forms a symbiosis with mold, it is necessary to observe the spatial and distributional changes. Also, the aging epoxy resin may cause secondary damage due to contaminants generated due to the determination of salts, and deterioration of bonding strength due to breaking out. Thus it is desirable to secure stability through proper conservation management.

Synthesis, Magneto-Spectral, Electrochemical, Thermal Characterization and Antimicrobial Investigations of Some Nickel(II) Complexes of Hydrazones of Isoniazid (Isoniazid의 hydrazone을 갖는 몇 가지 니켈(II) 착물들의 합성, 자기적 및 전기적 성질, 열적 특성과 항균성에 대한 연구)

  • Prasad, Surendra;Agarwal, Ram K.
    • Journal of the Korean Chemical Society
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    • v.53 no.6
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    • pp.683-692
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    • 2009
  • The synthesis of a novel series of nickel(II) complexes with new ligands derived from hydrazones of isoniazid have been reported in present work. The complexes have general compositions [$Ni(L)_2X_2$] or $[Ni(L)_3](ClO_4)_2$ {L = N-isonicotinamido-furfuraldimine (INH-FFL), N-isonicotinamido-3',4',5'-trimethoxybenzaldimine (INH-TMB) or N-isonicotinamido-cinnamalidene (INH-CIN) and X = $Cl^-$, ${NO_3}^-$, $ NCS^-$ or $CH_3COO^-$}. The ligands hydrazones behave as neutral bidentates (N and O donor) through the carbonyl oxygen and azomethine nitrogen. The new complexes with octahedral geometry have been characterized by elemental analysis, molecular weight determinations, magnetic susceptibility/moment, thermogravimetric, electrochemical and spectroscopic studies viz. infrared and electronic spectra. On the basis of conductivity measurements in nitrobenzene ($PhNO_2$) solution the [$Ni(L)_2X_2$] and $[Ni(L)_3](ClO_4)_2$ complexes have been found to be non-electrolytes and 1:2 electrolytes, respectively. Thermal properties have also been investigated, which support the geometry of the complexes. Antibacterial and antifungal properties of nickel(II) complexes and few standard drugs have also been examined and it has been observed that the complexes have moderate antibacterial activities.