• Title/Summary/Keyword: $HfCl_4$

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Simultaneous Determination of Tetracycline Antibiotics by 3-Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME) and HPLC-UV/Vis (3-상 속빈 섬유-액체상 미량추출법(HF-LPME)과 HPLC-UV/Vis을 이용한 Tetracycline류 항생제 동시분석)

  • Oh, Woong Kyo;Myung, Seung-Woon
    • Journal of the Korean Chemical Society
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    • v.58 no.6
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    • pp.535-542
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    • 2014
  • A simple and efficient preconcentration method was developed using three-phase liquid phase microextraction prior to HPLC-UV for simultaneous extraction and determination of tetracycline antibiotics (tetracycline, oxytetracycline, and chlortetracycline). The tetracycline antibiotics were separated simultaneously on a column ($C_8$, $3.0{\times}150mm$, $3{\mu}m$) with high selectivity and sensitivity using gradient elution. Under optimized conditions (extraction solvent, heptanal; pH of donor, 9.0; pH of acceptor, 1.0; stirring speed, 700 rpm; NaCl salt, 0%; and extraction time, 60 min), enrichment factors (EF) were between 5.6 and 22.3. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of $0.08{\sim}0.8{\mu}g/mL$ and $0.4{\sim}1.6{\mu}g/mL$, respectively. The calibration curves were linear within the range of $0.1{\sim}32{\mu}g/mL$ with the square of the correlation coefficient being more than 0.995. The precision (as a relative standard deviation, RSD) and accuracy (as a relative recovery) within working range were 1.3~9.1% and 84~118%, respectively.

Impedance Parameters of Electrical Double Layer I. A Determination Method of Electrolytic Cell Impedance Parameter on the Platinum Electrode (전기이중층의 임피던스 파라미터 I. 백금전극을 사용한 전해쎌 임피던스 파라미터의 결정방법)

  • Kum-Sho Hwang;Un-Sik Kim
    • Journal of the Korean Chemical Society
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    • v.30 no.3
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    • pp.273-281
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    • 1986
  • This study is focused on the correct measurement of the equations for the determination of the impedance parameters-the differential capacity of the double layer $C_d$, solution resistance $R_Q$, transfer resitance $R_i$, and adsorption pseudcapacity $C_{\phi}$/ The application of only an imaginary part of complex function of ${\omega}$ at the sinusoidal steady state indicates the following equations of total impedance: at low frequency $|Z_{LF}|=1/{\omega}_1\;C_{\phi}\;{\sqrt{1+{{\omega}_1}^2/{\omega}^2}$, at high frequency $|Z_{HF}|={\omega}_2/({\omega}_1{\omega}_3C{\phi})({\omega}^2+{{\omega}_2}^2)\;{\sqrt{{({\omega}^2+{\omega}_2{\omega}_3)}^2+{({\omega}_2{\omega}-{\omega_3{\omega})^2}}$. The values of the total impedance of cell, phase angle, and cell current that are necessary for the calculations of impedance parameters were experimentally measured from 200 to 6000Hz for the following supporting electrolytes, 0.5M $Na_2SO_4$, 1M NaCl, 19.373% sea water, 1M HCl, 1M $KNO_3$ and for $10^{-2}M$ KI and 60mM DBNA (Di-iso-Butylnitrosoamine) in these supporting electrolytes. The derived equations in this study shows that the values of impedance parameters of $C_d,\;C_{\phi},\;R_i\;and\;R_Q\;are\;15{\sim}40\;{\mu}F/cm^2,\;162{\sim}758\;{\mu}F/cm^2\;11.5{\sim}57.6\;ohm{\cdot}cm^2\;and\;0.5{\times}10^{-2}{\sim}4.1{\times}10^{-2}\;ohm{\cdot}cm^2$ respectively.

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Hafnium Oxide Nano-Film Deposited on Poly-Si by Atomic Layer Deposition

  • Wei, Hung-Wen;Ting, Hung-Che;Chang, Chung-Shu
    • 한국정보디스플레이학회:학술대회논문집
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    • 2005.07a
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    • pp.496-498
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    • 2005
  • We reported that high dielectric hafnium oxide nano-film deposited by thermal atomic layer deposition on the poly-silicon film (poly-Si). The poly -Si film was produced by plasma enhanced chemical vapor deposition and excimer laser annealing. We used the hafniu m chloride ($HfCl_4$) and water as the precursors and analyzed the hafnium oxide film by transmission electron microscope and secondary ion mass spectrometer. Hafnium oxide produced by the ALD method showed very good coverage on the rough surface of poly-Si film. While deposited with 200 cycles, these hafnium oxide films revealed a relatively smooth surface and good uniformity, but the cumulative roughness produced by the incomplete reaction was apparent when the amount of deposition cycle increased to 600 cycles.

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Ab initio Nuclear Shielding Calculations for Some X-Substituted Silatranes Using Gauge-Including Atomic Orbitals

  • 김동희;이미정
    • Bulletin of the Korean Chemical Society
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    • v.18 no.9
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    • pp.981-985
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    • 1997
  • 13C, 15N, and 29Si NMR chemical shifts have been computed for selected X-substituted silatranes (X=Cl, F, H, CH3) using Gauge-Including Atomic Orbitals (GIAO) at the Hartree-Fock level of theory. The isotropic 13C chemical shifts are largely insensitive to substituent-induced structural changes. In this study, the isotropic 13C chemical shifts between 1-methyl- and 1-hydrogensilatranes by GIAO-SCF calculation at the HF/6-31G level are very similar. But the results of 1-chloro- and 1-fluorosilatranes are about 4 ppm different from the experimental values. In contrast, the isotropic 15N and 29Si chemical shifts and the chemical shielding tensors are quite sensitive to substituent-induced structural changes. These trends are consistent with those of the experiment. The isotropic 15N chemical shift demonstrates a very clear correlation with Si-N distance. But in case of 29Si the correlations are not as clean as for the 15N chemical shift; the calculated variation in the 29Si chemical shift is much larger.

Characteristic Effects of 4,5-Disubstituted Pyridazin-3-one Derivatives with Various Functional Groups: Ab initio Study

  • Yoon, Yong-Jin;Koo, In-Sun;Park, Jong-Keun
    • Bulletin of the Korean Chemical Society
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    • v.28 no.8
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    • pp.1363-1370
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    • 2007
  • The geometrical structures of pyridazin-3-one derivatives (4,5-dihalopyridazin-3-one and 4-halo-5- alkoxypyridazin-3-one) with various functional and substituent groups were fully optimized using the ab initio Hartree-Fock (HF) and second order Moller-Plesset perturbation (MP2) methods. At the N2-, C4-, and C5- positions on the pyridazin-3-one rings, the structural and electronic features pertaining to the variations of the functional and substituent groups were analyzed, respectively. The trends in the variation of the bond lengths, atomic charges, and energetics (relative energy, binding energy) of the derivatives induced by changing the electron donating functional groups (X1 = OMe, OEt) to electron withdrawing groups (X1 = Cl, NO2) were examined. The variations of the bond lengths, atomic charges, and binding energies with the electron withdrawing strength of the substituent groups (Y = Me → F) were also investigated.

Liquid-liquid Distribution of the Tetravalent Zirconium, Hafnium and Thorium with a New Tetradentate Naphthol-derivative Schiff Base

  • Saberyan, Kamal;Shamsipur, Mojtaba;Zolfonoun, Ehsan;Salavati-Niasari, Masoud
    • Bulletin of the Korean Chemical Society
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    • v.29 no.1
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    • pp.94-98
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    • 2008
  • A fundamental study was developed concerning the novel solvent extraction of the tetravalent metal ions; zirconium(IV), hafnium(IV) and thorium(IV). Their extraction behavior in toluene was investigated with a recently synthesized naphthol-derivative Schiff base, 1-({[4-(4-{[(E)-1-(2-hydroxy-1-naphthyl)methyliden]amino}phenoxy) phenyl]imino}methyl)-2-naphthol (HAPMN). The spectrophotometrical examination of the complex formation between HAPMN and the Zr(IV), Hf(IV) and Th(IV) ions in acetonitrile revealed the formation of stable 1:1 complexes in the solution. After the thorium extraction in toluene, it was found that [Th(OH)3HA] was the respective deriving substance. While, in the case of zirconium and hafnium extraction, the extracted adduct was found to be [M4(OH)8(H2O)16Cl62HA]. The stoichiometric coefficients of these extracted species were determined by the slope analysis method. The extraction reaction followed a cation exchange mechanism.

The Effect of Heat Treatment on the Corrosion-Resistance for Ti-6Al-4V Alloy (Ti-6Al-4V합금의 열처리가 내식성에 미치는 영향)

  • 백신영;나은영
    • Journal of Advanced Marine Engineering and Technology
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    • v.27 no.3
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    • pp.453-459
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    • 2003
  • In this study, the effect of heat treatment to the electrochemical polarization resistance for the Ti-6Al-4V alloy was measured. The solution heat treatments were carried out at $1066^{circ}E, 966^{\circ}$E$, followed by aging heat treated $550^{circ}E, 600^{circ}E, and 650^{circ}E$. The electrochemical polarization resistance behavior was measured by potentio-dynamic polarization in the 1N $HNO_3$ + 15ppm HF solution. The obtained results were as follows. 1. As solution heat temperature increased. the corrosion potential was increased, whereas passive current density and critical current density were decreased. 2. As aging heat temperature increased, the corrosion potential was almost constant, but passive current density was decreased 3. The results of composition test measured by EDS at grain boundary and near $\gamma'$ precipitates indicated that S, Cl. and Si which originated from base metal were segregated at the grain boundaries Al and Ti which were the main alloying element in $\gamma'$ were depleted at the $\gamma'$ precipitated. The depletion of Al and Ti in $\gamma'$ was caused to early breakdown of passive film.

Selective Contact Hole Filling by electroless Ni Plating (무전해 Ni 도금에 의한 선택적 CONTACT HOLE 충전)

  • 우찬희;권용환;김영기;박종완;이원해
    • Journal of the Korean institute of surface engineering
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    • v.25 no.4
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    • pp.189-206
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    • 1992
  • The effect of activation and electroless nickel plating conditions on contact properties was investi-gated for selective electroless nickel plating of Si wafers in order to obtain an optimum condition of con-tact hole filling. According to RCA prosess, p-type silicon (100) surface was cleaned out and activated. The effects of temperature, DMAB concentration, time, and strirring were investigated for activation of p-type Si(100) surface. The optimal activation condition was 0.2M HF, 1mM PdCl2, 2mM EDTA,$ 70^{\circ}C$, and 90sec under ultrasonic vibration. In electroless nickel plating, the effect of temperature, DMAB concentra-tion, pH, and plating time were studied. The optimal plating condition found was 0.10M NiSO4.H2O, 0.11M Citrate, pH 6.8, $60^{\circ}C$, 30minutes. The contact resistance of films was comparatively low. It took 30minutes to obtain 1$\mu\textrm{m}$ thick film with 8mM DMAB concentration. The film surface roughness was improved with decreasing temperature and decreasing pH of the plating solution. The best quality of the film was obtained at the condition of temperature $60^{\circ}C$ and pH 6.0. The micro-vickers hardness of film was about 800Hv. Plating rate of nickel on the hole pattern was slower than that of nickel on the line pattern.

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An Influence of Additional Metals over Ni/SiO2 or Ni/Al2O3 on the Formation of CFC-1113 from CFC-113 (CFC-113로부터 CFC-1113의 합성시 Ni/SiO2(또는 Al2O3) 촉매상에서 다른 금속의 첨가효과)

  • Kim, JinHo;Park, Kun-You;Ha, Baik-Hyon
    • Applied Chemistry for Engineering
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    • v.10 no.2
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    • pp.237-241
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    • 1999
  • Nickel was impregnated on the $SiO_2$ and $Al_2O_3$ supports and applied to the reduction reaction of CFC-113 ($CF_2Cl$-$CFCl_2$) with hydrogen to 3FCl ($CF_2$=CFCl, CFC-1113). The conversion was rapidly declined on the Ni/$SiO_2$(or $Al_2O_3$) and the deactivation accelerated as the increase of Ni content. However, the selectivity of 3FCl was maintained at around 80% level. The simultaneous coprecipitation of copper and lithium on Ni/$Al_2O_3$ improved both the conversion and selectivity to 3FCl, but an excessive amount of lithium reduced the conversion as well as the selectivity of 3FCl. However, in the case of Ni/$SiO_2$, the conversion was greatly reduced possibly due to a loss of silica support with high surface area by the reaction of $SiO_2$ with HF. Such a reduction in conversion also can be ascribed to the decrease in active sites, caused by the addition of alkali metal compound, LiOH.

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Polymerization of Hydrosilanes and Vinyl Monomers in the Presence of Transition Metal Complex

  • Kim, Myoung-Hee;Lee, Jun;Cha, Hyo Chang;Shin, Joong-Hyeok;Woo, Hee-Gweon
    • Journal of Integrative Natural Science
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    • v.2 no.1
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    • pp.18-23
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    • 2009
  • This minireview provides the chosen examples of our recent discoveries in the polymerization of hydrosilanes, dihydrosilole, lactones, and vinyl derivatives using various catalysts. Hydrosilanes and lactones copolymerize to give poly(lactone-co-silane)s with $Cp_2MCl_2$/Red-Al (M = Ti, Zr, Hf) catalyst. Hydrosilanes (including dihydrosilole) reduce noble metal complexes (e.g., $AgNO_3$, $Ag_2SO_4$, $HAuCl_4$, $H_2PtCl_6$) to give nanoparticles along with silicon polymers such as polysilanes, polysilole, polysiloxanes (and silicas) depending on the reaction conditions. Interestingly, phenylsilane dehydrocoupled to polyphenylsilane in the inert nitrogen atmosphere while phenylsilane dehydrocoupled to silica in the ambient air atmosphere. $Cp_2M/CX_4$ (M = Fe, Co, Ni; X = Cl, Br, I) combination initiate the polymerization of vinyl monomers. In the photopolymerization of vinyl monomers using $Cp_2M/CCl_4$ (M = Fe, Co, Ni), the photopolymerization of MMA initiated by $Cp_2M/CCl_4$ (M = Fe, Co, Ni) shows while the polymerization yield decreases in the order $Cp_2Fe$ > $Cp_2Ni$ > $Cp_2Co$, the molecular weight decreases in the order $Cp_2Co$ > $Cp_2Ni$ > $Cp_2Fe$. For the photohomopolymerization and photocopolymerization of MA and AA, the similar trends were observed. The photopolymerizations are not living. Many exciting possibilities remain to be examined and some of them are demonstrated in the body of the minireview.

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