• Journal of Ginseng Research
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• v.32 no.4
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• pp.291-299
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• 2008

The fresh ginseng roots were extracted in aqueous methanol (MeOH), and the obtained extracts were partitioned using ethyl acetate (EtOA), n-butanol (n-BuOH), and water, successively. The repeated silica gel column chromatography for n-BuOH fraction afforded a purified ginsenoside $Rg_1$. The physico-chemical, spectroscopic and chromatographic data of ginsenoside $Rg_1$, such as crystallization characteristics, melting point, specific rotation, infrared spectrometry (IR) data, fast atom bombardment/mass spectrometry (FAB/MS) data, nuclear magnetic resonance (NMR) data, retention factor (Rf) in thin layer chromatography (TLC) experiment, and retention time (r.t.) in HPLC analysis, were measured and compared with those reported in literatures. Especially, the previous literatures reported different data for ginsenoside $Rg_1$ in the $^{1}H-$ and $^{13}C$-NMR experiments. This paper gives the exactly assigned NMR data through 2D-NMR experiments, such as $^{1}H-^{1}H$ correlation spectroscopy (COSY), hetero nuclear single quantum correlation (HSQC), and hetero nuclear multiple bond connectivity (HMBC).

• Journal of the Korean Institute of Illuminating and Electrical Installation Engineers
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• v.20 no.7
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• pp.46-52
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• 2006

The effects of surface treatment on the hydrogen storage properties of a $Mg_2Ni$ alloy particle were investigated by the microvoltammetric technique, in which a carbon-filament microelectrode was manipulated to make electrical contact with the particle in a KOH aqueous solution. It was found that the hydrogen storage properties of $Mg_2Ni$ at room temperature were improved by the surface treatment with a nickel plating solution. The sodium salts(sodium phosphate and sodium dihydrogen citrate) contained in the nickel plating solution made the alloy form an amorphous-like state, resulting in an improved hydrogen charge/discharge capacity at room temperature as high as about 150[mAh/g] from the original value of 17[mAh/g]. Potential-step experiment was carried out to determine the apparent chemical diffusion coefficient of hydrogen atom($D_{app}$) in the alloy. Since the alloy particle we used here was a dense, conductive sphere, the spherical diffusion model was employed for data analysis. $D_{app}$ was found to vary the order between $10^{-8}{\sim}10^{-9}[cm^2/s]$ over the course of hydrogenation and dehydrogenation process.

• Journal of the Korean Magnetics Society
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• v.10 no.5
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• pp.225-231
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• 2000

The crystallographic and magnetic properties of the sample F $e_{0.8}$ $Co_{0.18}$(BN)$_{0.02}$ synthesized by microwave arc-melting with the maximum power of 3.5 kW have been studied by the methods of an X-ray diffraction and the measurement of the magnetic hysteresis using the vibrating sample magnetometer at room temperature. The samples were prepared in a form of pellet pressed under the pressure of 9,000 N/c $m^2$, rolled coldly, and treated with the different temperatures. The X-ray diffraction pattern of pelleted sample shows that the crystal structure of the sample is bcc as same as that of Fe with a good uniformity. The X-ray diffraction pattern shows that a residual stress, which exists in the sample, is eliminated by final 90$0^{\circ}C$ annealing. As rolling rate and heat treatment temperature increases, the saturation magnetization and the remanence of the samples increase whereas the coercivity of the samples shows decrease. Also the saturation magnetization and the remanence of the samples were affected by rolling rate and rolling direction than heat treatment temperature, but the coercivity of the samples was affected by rolling rate and direction as well as heat treatment temperature. This means that a domain wall motion is easy due to elimination of a residual stress and an inclusion which exists in the sample by rolling and heat treatment and a local induced-magnetization easy axis was also formed to parallel to the rolling direction due to creation of the like-atom pairs across the slip plane by rolling......

• Journal of the Korean Institute of Telematics and Electronics C
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• v.35C no.10
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• pp.1-11
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• 1998

This paper presents a new implementation method of the pulsed NMR(nuclear magnetic resonance) apparatus, which contains a single coil in a magnet console, to detect a NMR signal. Applying an RF magnetic field of 5MHz to the magnet console which is designed to have Larmor frequency of 5MHz for hydrogen atom, the hydrogen NMR signal was obtained from the glycerin which was put in the magnet console as a sample. The DC magnetic field in the magnet console was implemented with a permanent magnet of 1168 gauss and the RF magnetic field was generated appling an RF signal with the frequency of 5MHz and the current magnitude of 8A to a coil of 5.73${\mu}$H. The magnitude of the NMR signal was maximum when the RF magnetic field was generated for 2.8 ${\mu}$sec, and the period of generating the RF magnetic field was designed to 100msec for detecting the NMR signal repeatedly. The NMR signal, radiated from the sample in the magnetic console, was appeared as an amplitude-modulated signal with a frequency equal to the Larmor frequency. The signal, induced in the coil, was amplified in the tx/rx separation circuit, preamplifier and intermediate amplifier by a factor of 20.7dB, 36dB and 40dB, respectively, and the signal was detected by a synchronous detection circuits, then the NMR signal was obtained.

• Journal of the Korean institute of surface engineering
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• v.13 no.3
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• pp.146-154
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• 1980

The effects of various electrodeposition conditions (deposition temperature and cathode current density) on preferred orientation and microhardness of electrodeposited Ni-Sn and Sn-Zn alloys were studied. At deposition temperatures from 25$^{\circ}$ to 95$^{\circ}C$ and constant cathode current density of 270 and 530 A/$m^2$ Ni-Sn and Sn-Zn were codeposited in chloride-fluoride acid and stannate-cyanide alkaline electrolyte bath respectively. Ni-Sn alloy deposited at temperatures from 25$^{\circ}$ to 35$^{\circ}C$ was composed of single phase of $Ni_3Sn_4$ with 73 wt.% Sn and the one deposited at temperatures from 45$^{\circ}$ to 95$^{\circ}C$ was made of multiphase mixture of NiSn, $Ni_3Sn_2$ and $Ni_3Sn_4$ with nearly equiatomic composition (65.5 wt.% Sn). The random orientation of thermody-namically metastable NiSn phase (hexagonal structure) predominated at deposition temperature range 25$^{\circ}$-45$^{\circ}C$, and the strong (110) preferred orientation was found at 65$^{\circ}$-85$^{\circ}C$ and then disappeared again at 95$^{\circ}C$. The microhardness of Ni-Sn deposits increased with deposition temperature up to 85$^{\circ}C$, and then decreased at constant cathode current density. The preferred orientation and the maximum microhardness were discussed in terms of lattice contractile stress which result from desorption of hydrogen atom absorbed in deposit lattice. The Sn content of Sn-Zn alloy deposits increased with deposition temperature up to 75$^{\circ}C$, and then decreased at constant cathode current density of 530 A/$m^2$. It also decreased with cathode current density up to 530 A/$m^2$, and then increased at constant deposition temperature of 25$^{\circ}C$. Sn-Zn alloy deposits were composed of two-phase mixture of ${beta}$-Sn and Zn. The preferred orientations of ${beta}$-Sn (tetragonal structure) changed with deposition temperature. The microhardness of Sn-Zn deposits decreased with deposition temperature. It also increased with cathode density up to 530 A/$m^2$, and then decreased at constant deposition temperature of 25$^{\circ}C$. The microhardness of Sn-Zn deposits was observed to be determinded more by the Sn content than by the preferred orientation.

• Proceedings of the Korean Vacuum Society Conference
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• 2000.02a
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• pp.77-77
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• 2000

Titanium oxide (TiO2) thin films have valuable properties such as a high refractive index, excellent transmittance in the visible and near-IR frequency, and high chemical stability. Therefore it is extensively used in anti-reflection coating, sensor, and photocatalysis as electrical and optical applications. Specially, TiO2 have a high dielectric constant of 180 along the c axis and 90 along the a axis, so it is highlighted in fabricating dielectric capacitors in micro electronic devices. A variety of methods have been used to produce patterned self-assembled monolayers (SAMs), including microcontact printing ($\mu$CP), UV-photolithotgraphy, e-beam lithography, scanned-probe based micro-machining, and atom-lithography. Above all, thin film fabrication on $\mu$CP modified surface is a potentially low-cost, high-throughput method, because it does not require expensive photolithographic equipment, and it produce micrometer scale patterns in thin film materials. The patterned SAMs were used as thin resists, to transfer patterns onto thin films either by chemical etching or by selective deposition. In this study, we deposited TiO2 thin films on Si (1000 substrateds using titanium (IV) isopropoxide ([Ti(O(C3H7)4)] ; TIP as a single molecular precursor at deposition temperature in the range of 300-$700^{\circ}C$ without any carrier and bubbler gas. Crack-free, highly oriented TiO2 polycrystalline thin films with anatase phase and stoichimetric ratio of Ti and O were successfully deposited on Si(100) at temperature as low as 50$0^{\circ}C$. XRD and TED data showed that below 50$0^{\circ}C$, the TiO2 thin films were dominantly grown on Si(100) surfaces in the [211] direction, whereas with increasing the deposition temperature to $700^{\circ}C$, the main films growth direction was changed to be [200]. Two distinct growth behaviors were observed from the Arhenius plots. In addition to deposition of THe TiO2 thin films on Si(100) substrates, patterning of TiO2 thin films was also performed at grown temperature in the range of 300-50$0^{\circ}C$ by MOCVD onto the Si(100) substrates of which surface was modified by organic thin film template. The organic thin film of SAm is obtained by the $\mu$CP method. Alpha-step profile and optical microscope images showed that the boundaries between SAMs areas and selectively deposited TiO2 thin film areas are very definite and sharp. Capacitance - Voltage measurements made on TiO2 films gave a dielectric constant of 29, suggesting a possibility of electronic material applications.

• Bulletin of the Korean Chemical Society
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• v.15 no.1
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• pp.37-45
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• 1994

$(NH_4)_{4.5}[H_{3.5}{\alpha}-PtMo_6O_{24}]{\cdot}1.5\;H_2O(A),\;(NH_4)_4[H_4{\beta}-PtMo_6O_{24}]{\cdot}1.5\;H_2O(B),\;and\;K_{3.5}[H_{4.5}{\alpha}-PtMo_6O_{24}]{\cdot}3\;H_2O(C)$ have been synthesized and their molecular structures have been also determined by single-crystal X-ray diffraction technique. The space groups, unit cell parameters, and R factors are as follows: Compound A, monoclinic, $A_{2/a}$, a= 19.074 (3), b=21.490 (3), c=15.183 (2) ${\AA};\;{\beta}$=109.67 (1) ${\AA}$; z=8; R=0.075($IF_0I>4{\sigma}(IF_0I);$ Compound B, triclinic, P$bar{1}$, a=10.776 (2), b=15.174 (4), c=10.697 (3) ${\AA};\;{\alpha}$ =126.29 (2), ${\beta}$=111.55 (2), ${\gamma}$=93.18 (2) ${\AA}$; Z=2; R=0.046($IF_0I>3{\sigma}(IF_0I);$): Compound C, triclinic, Pl, a=12.426 (2), b=13.884 (2), c=10.089 (1) ${\AA}$; ${\alpha}$=102.59 (2), ${\beta}$=110.73 (1), ${\gamma}$=53.93 (1) ${\AA}$; Z=2; R=0.074 ($IF_0I>3{\sigma}(IF_0I)$. Compounds A and C contain the well-known Anderson structure (planar structure) heteropoly oxometalate having approximate $bar{3}_m(D_{3d})$ symmetry, while compound B contains the bent structure heteropoly oxometalate having appproximate $2_{mm}(C2_v)$ symmetry. The bent structure and the planar one are geometrical isomers. These compounds are rot only novel heteroply molybdates containing platinate(IV) but also the first example of geometrical isomerism in the hexamolybdoheteropoly oxometalates. That isomerization surprisingly occurred because of the change of only 0.5 non-acidic hydrogen atom attached to the polyanion such as $[H_{3.5}{\alpha} -PtMo_6O_{24}]^{4.5-}{\to}[H_4{\beta}-PtMo_6O_{24}]^{4-}{\to}[H_{4.5}{\alpha} -PtMo_6O_{24}]^{3.5-}$. It seems that the gradual protonation of the polyanion plays an important role in that isomerism. These heteropolyanions form dimers by strong hydrogen bonds between two heteropolyanions in the respective crystal system.

• Bulletin of the Korean Chemical Society
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• v.14 no.5
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• pp.603-610
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• 1993

The crystal structure of dehydrated $Ag_{5.6}K_{6.4}-A$, zeolite A ion-exchanged with $K^+\;and\;Ag^+$ as indicated and dehydrated at 360$^{\circ}$C, has been determined by single-crystal X-ray diffraction techniques. Also determined were the structures of the products of the reactions of this zeolite with 0.1 Torr of Cs vapor at 250$^{\circ}$C for 48 h and 72 h, and with 0.1 Torr of Rb vapor at 250$^{\circ}$C for 24 h. The structures were solved and refined in the cubic space group Pm3m at 21(l)$^{\circ}$C (a= 12.255(l) ${\AA}$ , 12.367(l) ${\AA}$, 12.350(l) ${\AA}$, and 12.263(l) ${\AA}$, respectively). Dehydrated $Ag_{5.6}K_{6.4}$-A was refined to the final error indices $R_1= 0.044\;and\;R_2=0.037$ with 202 reflections for which I>3${\sigma}$(I). The crystal structures of the reaction products were refined to $R_1=0.087\;and\;R_2= 0.089$ with 157 reflections, $R_1=0.080\;and\;R_2= 0.087$ with 161 reflections, and $R_1= 0.071\;and\;R_2=0.061$ with 88 reflections, respectively. In the structure of $Ag_{5.6}K_{6.4}-A,\;K^+$ ions block all 8-oxygen rings, and one reduced Ag atom is found per sodalite cavity. Also, ca. 4.6 $Ag^+ ions\;and\;3.4 K^+ ions$ are found at 6-ring sites in the large cavity. The crystal structures of the reaction products show that all $K^+$ and $Ag^+$ ions have been reduced, and that all K^+$ atoms have left the zeolite. Cs or Rb species are found at three different crystallographic sites: 3.0 $Cs^+\;or\;3.0Rb^+$ ions per unit cell occupy 8-ring centers, ca. 8.0 $Cs^+ ions\;or\;5.7 Rb^+$ ions, are found on threefold axes opposite 6-rings deep in the large cavity, and ca. 2.5 $Cs^+\;or\;2.3 Rb^+ ions are found on threefold axes in the sodalite unit. Also, 1 $Rb^+$ ion lies opposite a 4-ring. Silver atoms, corresponding to 75% or 40% occupancy of hexasilver clusters stabilized by coordination to $Cs^+\;or\;Rb^+$ ions, are found at the centers of the large cavities. In the crystal structures of dehydrated Ag_{5.6}K_{6.4}-A$ reacted with Cs vapor, excess Cs atoms are absorbed and these form (locally) cationic clusters such as $(Cs_4)3^+\;and\;(Cs_6)4^+$.

• The Journal of the Petrological Society of Korea
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• v.10 no.3
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• pp.179-189
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• 2001

The determination of trace concentration of U, Th and Pb was carried out for chemical dating of zircon and monazite by electron microprobe. Detection limit and error range should be considered to measure characteristic X-rays of M-line from those minerals, which are low in the ionization of atom and low peak intensity in the spectrum. The element of U, Th and Pb were simultaneously measured with 3 spectrometers equipped with PET crystal to reduce a total counting time and error due to drift of instrumental operating condition. Detection limit could be improved from increase of the peak/background ratio through adjusting pulse height analyzer about 1000 mv baseline. Under permissible maximum analytical conditions, theoretical detection limit of U, Th and Pb is down to 30 ppm (99% confidence level). The analytical result was maintained at a relative error $\pm$10% ($2{\sigma}$) in 800 ppm Pb, $\pm$5% ($2{\sigma}$) in 2330 ppm U and $\pm$10% ($2{\sigma}$) in dating from a single measurement of zircon at 15 keV and 100 nA. However, for the precise dating of zircon and monazite, if it is considered a 3 $\mu\textrm{m}$ spatial resolution, <100 ppm ($3{\sigma}$) detection limit and <$\pm$10% ($2{\sigma}$) relative error, optimum analytical conditions are given as 15~20 keV accelerating voltage, 100~200 nA beam current and 300~1200 sec total counting time. To reduce material damage by high current, there is need to be up to 3~5 $\mu\textrm{m}$ of electron beam diameter, or to use arithmetic average of multiple measuring at a shorter counting time. A younger or relatively low concentration rocks can be dated chemically by lower detection limit and improved precision resulted from increase of current and measuring time.

• Journal of the Korean Chemical Society
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• v.45 no.3
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• pp.242-246
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• 2001

The quaternary thiophosphates, $A_2NiP_2S_6$ (A=Rb, Cs), have been synthesized with halide fluxes and structurally characterized by single-crystal X-ray diffraction technique. These compounds crystallize in the space group $C_{2h}^5-P2_1/n$ of the monoclinic system with two formula units in a cell of dimensions a=5.960(2), b=12.323(4), $c=7.491(3)\AA$, $\beta=97.05(3)^{\circ}$, and $V=546.0(3)\AA^3$ for Rb2NiP2S6 and a=5.957(4), b=12.696(7), $c=7.679(4)\AA$, $b=93.60(5)^{\circ}$, and $V=579.7(5)\AA^3$ for $Cs_2NiP_2S_6.$ These compounds are isostructural. The structure of $Cs_2NiP_2S_6$ is made up of one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chains along the a axis and these chains are isolated by $Cs^+$ ions. The Ni atom is octahedrally coordinated by six S atoms. These Ni$S_6$ octahedral units are linked by sharing three m-S atoms of the $[P_2S_6^{4-}]$ anions to form the infinite one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chain. For $Cs_2NiP_2S_6$, the magnetic susceptibility reveals an antiferromagnetic exchange interaction below 8K,which corresponds to the Neel temperature ($T_N$). Above $T_N$, this compound obeys Curie-Weiss law. The magnetic moment, C, and ${\theta}forCs_2NiP_2S_6$ are 2.77 B.M., 0.9593 K, and -19.02 K, respectively. The effective magnetic moment obtained from the magnetic data is agreed with the spin-only value of $Ni^{2+}d^8$(2.83 B.M.) system.