• Title/Summary/Keyword: M-ICP

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Kinetics and Mechanism of the Oxidation of Substituted Benzyl Alcohols by Cr(VI)-4,4'-Bipyridine Complex (크롬(VI)-4,4'-Bipyridine 착물에 의한 치환 벤질 알코올류의 산화반응 속도론과 메카니즘)

  • Kim, Young-Sik;Park, Young-Cho
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.13 no.1
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    • pp.462-469
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    • 2012
  • Cr(VI)-4,4'-bipyridine complex(4,4'-bipyridinium dichromate) was synthesized by the reaction of 4,4'-bipyridine with chromium trioxide in H2O, and characterized by IR, ICP. The oxidation of benzyl alcohol using 4,4'-bipyridinium dichromate in various solvents showed that the reactivity increased with the increase of the dielectric constant(${\varepsilon}$), in the order: cyclohexene$CH_3$, H, m-Br, m-$NO_2$) smoothly in N,N'-dimethylformamide. Electron-donating substituents accelerated the reaction, whereas electron acceptor groups retarded the reaction. The Hammett reaction constant(${\rho}$) was -0.63(303K). The observed experimental data have been rationalized as follows; the proton transfer occurs after the prior formation of a chromate ester in the rate determining step.

A Study for Mechanism and Oxidation Reaction of Substituted Benzyl Alcohols using Cr(VI)-Heterocyclic Complex[Cr(VI)-2-methylpyrazine] (Cr(VI)-헤테로고리 착물[Cr(VI)-2-methylpyrazine]를 이용한 치환 벤질 알코올류의 산화반응과 메카니즘에 관한 연구)

  • Kim, Young-Sik;Park, Young-Cho
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.14 no.11
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    • pp.6039-6046
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    • 2013
  • Cr(VI)-heterocyclic complex[Cr(VI)-2-methylpyrazine] was synthesized by the reaction between of heterocyclic compound(2-methylpyrazine) and chromium trioxide, and characterized by IR and ICP analysis. The oxidation of benzyl alcohol using Cr(VI)-2-methylpyrazine in various solvents showed that the reactivity increased with the increase of the dielectric constant(${\varepsilon}$), in the order : cyclohexene${\rho}$) was Cr(VI)-2-methylpyrazine= -0.65(308K). The observed experimental data have been ratiolized. The hydride ion transfer causes the prior formation of a chromate ester in the rate-determining step.

Plasma control by tuning network modification in 4MHz ionized-physical vapor deposition (4MHz I-PVD장치에서 정합회로를 이용한 플라즈마 제어)

  • 주정훈
    • Journal of the Korean Vacuum Society
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    • v.8 no.1
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    • pp.75-82
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    • 1999
  • Ion energy is one of the crucial property in thin film deposition by internal ICP assisted I-PVD. As ion energy is determined by the difference between the plasma potential and the substrate bias potential, ICP excitation frequency was tested with medium frequency of 4 MHz and two types of tuning circuits, alternate and floating LC network with a biasing resistor, were tested. The results showed that plasma potential was less than 5 V in a range of Ar pressures, 5mTorr to 30 mTorr, at 4 MHz RF 600 W and 60 V of maximum RF antenna voltage was maintained either at RF input or output terminal. By proper control of RLC circuit installed after after RF antenna, 50V of RF induced voltage on RF antenna was obtained at 500W input power. The total impedance of RF antenna and plasma was around 10$\Omega$, and minimum RF voltage was obtained with a condition of lowest reactance at most 0.05$\Omega$.

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Kinetics and Mechanism of the Oxidation of Substituted Benzyl Alcohols by Cr(VI)-Heterocyclic Complex (2,4'-Bipyridinium Chlorochromate) (크롬(VI)-헤테로고리 착물(2,4'-비피리디늄 클로로크로메이트)에 의한 치환 벤질 알코올류의 산화반응에서 속도론과 메카니즘)

  • Park, Young Cho;Kim, Young Sik
    • Applied Chemistry for Engineering
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    • v.25 no.6
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    • pp.648-653
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    • 2014
  • Cr(VI)-heterocyclic complex (2,4'-bipyridinium chlorochromate) was synthesized by the reaction between heterocyclic compound(2,4'-bipyridine) and chromium trioxide, and characterized by IR and ICP analysis. The oxidation of benzyl alcohol using 2,4'-bipyridinium chlorochromate in various solvents showed that the reactivity increased with the increase of the dielectric constant (${\varepsilon}$), in the order : N,N-dimet-hylformamide (DMF) > acetone > chloroform > cyclohexene. In the presence of DMF solvent with acidic catalyst such as hydrochloric acid (HCl solution), 2,4'-bipyridinium chlorochromate oxidized benzyl alcohol (H) and its derivatives (p-$CH_3$, m-Br, m-$NO_2$). Electron-donating substituents accelerated the reaction rate, whereas electron acceptor groups retarded the reaction rate. The Hammett reaction constant (${\rho}$) was -0.67 (303 K). The observed experimental data have been rationalize the proton transfer occurred followed the formation of a chromate ester in the rate-determining step.

The Effect of Temperature and Flow Rate of Eluent on the Separation of Adjacent Lanthanides (La : Ce, Ce : Pr, Pr : Nd) with Displacement Chromatography (치환크로마토그래피에서 온도와 용리액의 흐름속도가 란탄족 원소들 (La : Ce, Ce : Pr, Pr : Nd) 의 분리에 미치는 영향)

  • Ha, Yeong Gu;Song, Gi Hun
    • Journal of the Korean Chemical Society
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    • v.38 no.9
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    • pp.660-666
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    • 1994
  • The effects of temperature and flow rate of eluent on the separation of adjacent lighter lanthanide pairs (La : Ce, Ce : Pr, Pr: Nd) have been studied with displacement chromatography. Two serial columns packed with Amberlite 120 cation exchange resin are used for loading and separation. The retaining ion is $H^+$ ion and the eluent is 0.012M and 0.015M of EDTA solution. The columns and the eluent are maintained at the temperature of 90$^{\circ}C$ and pressurized to reduce vaporizing in the ion-exchange resin column. The eluated solution is analyzed directly with ICP-AES. The separation factors of the lanthanide pairs, La: Ce, Ce :Pr, and Pr: Nd, are 4.6, 2.8, and 1.9, respectively and are higher than that from theoretical calculation at 25$^{\circ}C$. When the flow rate is reduced from 2.5 ml/min to 1.5 ml/min, the HETP is reduced from 1.60 cm to 0.88 cm. The separation efficency can be improved at lower flow rate of eluent and higher operating temperature. The recoveries of pure lanthanides than 99.9% are 49∼77% from this separation.

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A Study on the Cation Extraction and Separation in Cement Industrial By-products for Applications to the Carbonation Process (탄산화 공정 적용을 위한 시멘트 산업부산물 내 양이온 추출 및 분리 연구)

  • Lee, Ye Hwan;Han, Dong Hee;Lee, Sang Moon;Eom, Han Ki;Kim, Sung Su
    • Applied Chemistry for Engineering
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    • v.30 no.1
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    • pp.34-38
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    • 2019
  • A cement industrial by-product was used as a Ca source for the carbonation process. It was confirmed that the most of cement industrial by-products was composed of CaO and KCl through ICP and XRD analyses. The optimal extractant type and concentration was 1.5 M of hydrochloric acid, and the solid/liquid ratio was 0.1 g/mL. It was assumed that the cation extraction efficiency was dependent of the pair ions and their binding formation and also the solubility from extraction efficiency results by varing extractants. After extraction process, it was also confirmed that the cation could be selectively separated from the solution with respect to the kind of additives and the injection order. When NaOH was injected into the solution to control pH values ranging from 9.5 and 13, impurities and $Ca(OH)_2$ were precipitated, whereas the separated K ion was precipitated in the form of KCl under the injected $C_2H_5OH$.

A Study for Kinetics and Oxidation Reaction of Substituted Benzyl Alcohols Using 2,4'-Bipyridinium Dichromate (2,4'-Bipyridinium Dichromate를 이용한 치환 벤질 알코올류의 산화반응과 반응속도에 관한 연구)

  • Kim, Young Sik;Park, Young Cho
    • Applied Chemistry for Engineering
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    • v.22 no.6
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    • pp.718-722
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    • 2011
  • 2,4'-Bipyridinium dichromate [$(C_{10}H_8N_2H)_2Cr_2O_7$] was synthesized by the reaction of 2,4'-bipyridinie with chromium trioxide in $H_2O$. The structure was characterized by IR and ICP analysis. The oxidation of benzyl alcohol using 2,4'-bipyridinium dichromate in various solvents showed that the reactivity increased with the increase in the order of the dielectric constant (${\varepsilon}$), in the order : cyclohexene < chloroform < acetone < N,N'-dimethylformamide. In the presence of hydrochloric acid, 2,4'-bipyridinium dichromate effectively oxidized benzyl alcohol and its derivatives ($p-CH_3$, H, m-Br, $m-NO_2$) in N,N'-dimethylformamide. Electron-donating substituents accelerated the reaction, whereas electron acceptor groups retarded the reaction. The Hammett reaction constant (${\rho}$) was -0.65 at 303 K. The observed experimental data was used to rationalize the hydride ion transfer in the rate-determining step.

REE Mineralization of Quy Hop Area in Nghe An Province, Northern Vietnam (베트남 북부 네안성 뀌홉지역 희토류 광화작용)

  • Lee, Jae-Ho;Jin, Kwang-Min;Heo, Chul-Ho
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.3
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    • pp.193-213
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    • 2018
  • Soil geochemical exploration to check anomalies related to mineralization was carried out targeting around Quy Hop area within Nghe An province, Northern Vietnam. The interval of sampling are horizontal 250 m with 13 line and longitudinal 300 m with 25 line, resulting in 325 soil samples. Based on the result of soil geochemical exploration, the pitting survey was carried out targeting the grid point with high TREO content, resulting in 73 soil samples within 8 pits. The geology of the survey area are consisted of Ban Chieng biotite granite complex intruding Bu Khang formation comprising of schist, gneiss and limestone. In order to elucidate the source rock of monazite and xenotime confirmed from heavy sand, soil geochemical exploration was carried out. By ICP-MS result of soil samples, total REE oxide content of background amount is about 1.4 times of crustal abundance, depleting the light rare earth (about 0.2 times) and enriching the heavy rare earth (about 1.5 times). By ICP-MS result of pit soil samples, we identified TREO more than 1,000 ppm in 6 pits. It may be considered that REE ore bodies may develop in NE-SW direction, compared with the geochemical results of Quy Chau area.

Distribution Characteristics of Heavy Metals in the Ambient Air of Ulsan Area (울산 대기 중 중금속 분포특성)

  • Moon, Ji-Yong;Kim, Young-Bok;Lee, Ji-Young;Jeong, Gi Ho
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.442-450
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    • 2001
  • In this study, we collected PM10(particulate matter less than $10{\mu}m$) by using a high volume air sampler from March 2000 to September 2000 to investigate the contamination level and the distribution characteristics of heavy metals in the ambient air in Ulsan area. Samples were pretreated by the microwave extraction methods, and heaby metals (Cr, Cu, Zn, Cd, Ni, As, and Pb) were quantified by using and ICP-MS system. The highest PM10 concentrations in the ambient air were $85.6{\mu}g/m^3$ and the aberage value was $37.1{\mu}g/m^3$. The maximum levels of each heavy metal were as follows: $2.5{\mu}g/m^3$ for Fe(Yeocheon-dong), $0.41{\mu}g/m^3$ for Zn(Nammok-2-dong), $0.061{\mu}g/m^3$ for Cd(Yeocheon-dong), $0.20{\mu}g/m^3$ for Pb(Yeocheon-dong), $0.037{\mu}g/m^3$ for Ni(Yeoncheon-dong), $0.88{\mu}g/m^3$ for Cu(Yaeum-dong), $0.042{\mu}g/m^3$ for Cr(Yaeum-dong), and $0.015{\mu}g/m^3$ for As(Onsan). Among concentration of heavy metals, Ni and Zn compounds were highly correlated with a correlation coefficient of 0.87 at Nammok-2-dong.

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Quantitative Speciation of Selenium in Human Blood Serum and Urine with AE- RP- and AF-HPLC-ICP/MS

  • Jeong, Ji-Sun;Lee, Jonghae;Pak, Yong-Nam
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3817-3824
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    • 2013
  • Various separation modes in HPLC, such as anion exchange (AE), reversed-phase (RP), and affinity (AF) chromatography were examined for the separation of selenium species in human blood serum and urine. While RP- and AE-HPLC were mainly used for the separation of small molecular selenium species, double column AF-HPLC achieved the separation of selenoproteins in blood serum efficiently. Further, the effluent of AF-HPLC was enzymatically hydrolyzed and then analyzed with RP HPLC for selenoamino acid study. The versatility of the hybrid technique makes the in-depth study of selenium species possible. For quantification, post column isotope dilution (ID) with $^{78}Se$ spike was performed. ORC ICP/MS (octapole reaction cell inductively coupled plasma/mass spectrometry) was used with 4 mL $min^{-1}$ Hydrogen as reaction gas. In urine sample, inorganic selenium and SeCys were identified. In blood serum, selenoproteins GPx, SelP and SeAlb were detected and quantified. The concentration for GPx, SelP and SeAlb was $22.8{\pm}3.4\;ng\;g^{-1}$, $45.2{\pm}1.7\;ng\;g^{-1}$, and $16.1{\pm}2.2\;ng\;g^{-1}$, respectively when $^{80}Se/^{78}Se$ was used. The sum of these selenoproteins ($84.1{\pm}4.4\;ng\;g^{-1}$) agrees well with the total selenium concentration measured with the ID method of $87.0{\pm}3.0\;ng\;g^{-1}$. Enzymatic hydrolysis of each selenium proteins revealed that SeCys is the major amino acid for all three proteins and SeMet is contained in SeAlb only.