• Title/Summary/Keyword: M-ICP

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Electrochemical Properties of Zr0.8Ti0.2Mn0.4V0.6Ni1-xFex Alloy Electrodes (Zr0.8Ti0.2Mn0.4V0.6Ni1-xFex 합금 전극의 전기화학적 특성)

  • Song, MyoungYoup;Kwon, IkHyun;Lee, DongSub
    • Transactions of the Korean hydrogen and new energy society
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    • v.13 no.3
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    • pp.181-189
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    • 2002
  • A series of multicomponent $Zr_{0.8}Ti_{0.2}Mn_{0.4}V_{0.6}Ni_{1-x}Fe_{x}$ (x=0.00, 0.08, 0.15, 0.22, and 0.30) alloys are prepared and their oystal structure and P-C-T curves are examined. The electrochemical properties of these allqys such as activation conditions, discharge capacity, cycling performance are also investigated. $Zr_{0.8}Ti_{0.2}Mn_{0.4}V_{0.6}Ni_{1-x}Fe_{x}$ (x=0.00, 0.08, 0.15, 0.22 and 0.30) have the C14 Laves phase hexagonal structure. The electrode was activated by the hot-charging treatment. The best activation conditions were the current density 120 mA/g and the hot-charging time 12h at $80^{\circ}C$ in the case of the alloy with x=0.00. The discharge capacity increased rapidly until the fourth cycle and then decreased. The discharge capacity increased again from the 13th cycle, arriving at 234 mAh/g at the 50th cycle. The discharge capacily just after activation decreases with the increase in the amount of the substituted Fe but the cycling performance is improved. The discharge capacity after activation of the alloy with x=0.00 is 157 mAh/g at the current density 120 mA/g. $Zr_{0.8}Ti_{0.2}Mn_{0.4}V_{0.6}Ni_{0.85}Fe_{0.15}$ is a good composition with a medium quantity of discharge capacities and a good cycling performance. The ICP analysis of the electrolyte for these electrodes after 50 charge-discharge cycles shows that the concentrations of V and Zr are relatively high. Another series of multicomponent $Zr_{0.8}Ti_{0.2}Mn_{0.4}V_{0.6}Ni_{0.85}M_{0.15}$ (M = Fe, Co, Cu, Mo and Al) alloys are prepared. They also have the C14 Laves phase hexagonal structure. The alloys with M = Co and Fe have relatively larger hydrogen storage capacities. The discharge capacities just after activation are relatively large in the case of the alloys with M = Al and Cu. They are 212 and 170 mAh/g, respectivety, at the current density 120mA/g. The $Zr_{0.8}Ti_{0.2}Mn_{0.4}V_{0.6}Ni_{0.85}Co_{0.15}$ alloy is the best one with a relatively large discharge capacity and a good cycling performance.

A Study for Kinetics and Oxidation Reaction of Alcohols by Cr(VI)-4-(Dimethylamino)pyridine (크롬(VI)-4-(Dimethylamino)pyridine에 의한 알코올류의 산화반응과 반응속도에 관한 연구)

  • Kim, Young-Sik;Park, Young-Cho;Kim, Young Jun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.14 no.1
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    • pp.499-505
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    • 2013
  • Cr(VI)-4-(dimethylamino)pyridine[4-(dimethylamino)pyridinium chlorochromate] was synthesized by the reaction of 4-(dimethylamino)pyridine with chromium trioxide in 6M-HCl, and characterized by IR, ICP. The oxidation of benzyl alcohol using 4-(dimethylamino)pyridinium chlorochromate in various solvents showed that the reactivity increased with the increase of the dielectric constant(${\varepsilon}$), in the order: cyclohexene$H_2SO_4$ solution), 4-(dimethylamino)pyridinium chlorochromate oxidized benzyl alcohol and its derivatives(p-$OCH_3$, m-$CH_3$, H, m-$OCH_3$, m-Cl, m-$NO_2$) smoothly in DMF. Electron-donating substituents accelerated the reaction, whereas electron acceptor groups retarded the reaction. The Hammett reaction constant(${\rho}$) was -0.68(303K). The observed experimental data was used to rationalize the hydride ion transfer in the rate-determining step.

grid를 이용한 plasma parameter control

  • 배근희;김성식;홍정인;장홍영
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.181-181
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    • 2000
  • 최근 반도체 공정에 있어 0.2$\mu\textrm{m}$ 이하의 미세 공정에 필요해짐에 따라 plasma를 이용한 공정이 필요하게 되었다. 그러나 ICP를 이용하여 SiO2를 etching 할 경우, SiO2/Si 선택비를 높이기 우해 전자 온도 제어가 필요하다. grid를 이용하여 전자 온도를 제어할 경우 plasma potential이 plasma 변수 제어에 중요한 역할을 하게 된다. 이번 실험에서는 grid를 이용하여 plasma potential를 변화시켜 주면서 생기는 플라즈마 변수 변화에 대해 연구하였다.

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Determination of Isotopic Ratios for Ca in Inductively Coupled Plasma Mass Spectrometry (ICPMS) by Removing Water Related Molecules

  • 박용남;S. R. Koirtyohann
    • Bulletin of the Korean Chemical Society
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    • v.18 no.11
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    • pp.1172-1175
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    • 1997
  • Calcium isotopic ratios are precisely measured by removing isobaric interferences originated from water in the plasma. Liquid Ar cryogenic trap combined with membrane desolvator could eliminate backgrounds at m/z 42 and 44. Slow drift of ICP-MS is corrected by the frequent running of the standards. It is found necessary to separate Ca from the sample matrix using Ca oxalate precipitation technique. Currently, the RSD is 0.5-1.0% for 2 minutes of measurement but is expected to be improved if the measurement time is increased. The technique was applied to 42Ca enriched baby fecal samples and successfully determined 42Ca/44Ca ratio changes.

High aspect ratio 10:1 Via formation and Seed layer sputtering (고종횡비 10:1 Via 가공 및 Seed layer 스퍼터링 공정 연구)

  • Song, Yeong-Sik;Han, Yun-Ho;Eom, Ho-Gyeong;Im, Tae-Hong;Kim, Jong-Ryeol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2012.11a
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    • pp.141-141
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    • 2012
  • 고종횡비 10:1 비아를 Si wafer 상에 형성하기 위해 $7{\mu}m$ 직경의 마스크로 포토작업하여 Cr층을 100nm 스퍼터링하여 PR(photo resistor) 대신의 에칭 barrier 막으로 사용하였다. 얼라인, 노광, 현상을 거쳐 Cr에칭, PR 제거후 ICP(inductively coupled plasma) 공정으로 Si deep etching하여 via 직경 $10.16{\mu}m$, 깊이 $102.5{\mu}m$의 고종횡비 비아를 형성하였다. 구리필링도금을 위해서 필수적인 seed layer는 단층 또는 다층의 금속막을 스퍼터링 법으로 형성하였다. 형성된 seed layer 단면을 FE-SEM(Field emission scanning electron microscope)으로 관찰하여 내부에 seed 층의 형성 유무를 확인하였다.

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Determination of selenium in grains by hydride generation-ICP/MS (수소화물발생-유도결합플라즈마 질량분석법(HG-ICP/MS)을 이용한 곡류 중 셀레늄의 정량분석)

  • Kim, Minkyung;Jung, Jinok;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.26 no.2
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    • pp.135-141
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    • 2013
  • The purpose of this study is to determine the quantity of selenium in grains by hydride generation-inductively coupled plasma mass spectrometry. Two sample preparation methods, beaker and microwave digestions, are compared and the former shows better result. The optimum condition for hydride generation is 4.0 M for HCl, 3% for $NaBH_4$ with the sample flow of 0.6 mL/min. The detection limit is 0.02 ${\mu}g/kg$($3{\sigma}$) and improved by 10 times. Isobaric interferences on Se is removed by Octopole Reactoin Cell and $H_2$ (3.8 mL/min) shows better performance over He. However, in case Br exists in a matrix, $H_2$ could induce interferences on m/z 80 and 82 ($^{80}[BrH]^+$ and $^{82}[BrH]^+$). The accuracy of this experiment is examined successfully by analyzing several reference materials. The results for several domestic grain analysis show that the concentrations are between 12.7 ${\mu}g/kg$ and 29.6 ${\mu}g/kg$.

Determination and preconcentration of Cu(II) using microcrystalline p-Dichlorobenzene loaded with salicylaldoxime (Salicylaldoxime이 내포된 p-Dichlorobenzene 미세결정을 이용한 Cu(II)의 예비농축 및 정량)

  • Lee, Ha-Na;Choi, Hee-Seon
    • Analytical Science and Technology
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    • v.23 no.3
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    • pp.240-246
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    • 2010
  • A technique for the determination of trace Cu(II) in various real samples by FAAS after the column preconcentration onto p-dichlorobenzene-SA adsorbent, which is microcrystalline p-dichlorobenzene loaded with salicylaldoxime (SA) has been developed. Several experimental conditions such as pH of the sample solution, the amount of chelating agent salicylaldoxime, the amount of adsorbent p-dichlorobenzene-SA, and flow rate of sample solution were optimized. The interfering effects of various concomitant ions were investigated. $CN^-$ interfered more seriously than any other ions. However, the interference by $1\;{\mu}g\;mL^{-1}\;CN^-$ could be overcome completely by controlling the concentration of Ni(II) to $20\;{\mu}g\;mL^{-1}$. The linear range, correlation coefficient ($R^2$) and detection limit obtained by this technique were $3.0\sim100\;ng\;mL^{-1}$, 0.9901, and $3.1\;ng\;mL^{-1}$, respectively. For validating this technique, the aqueous samples (wastewater, reservoir water and stream water) and the food samples (orange juice, fresh egg and skim milk) were used. Recovery yields of 93~104% were obtained. These measured mean values were not differents from ICP-MS data at 95% confidence level. The good results were obtained from the experiments using the rice flour certified reference material (CRM) sample. Based on the experimental results, it was found that this technique could be applied to the preconcentration and determination of Cu(II) for various real samples.

Evaluation of Chemical Pre-treatment for the Optimization of CO2 Fixatiom Using by Carbonation Reaction with Serpentine (이산화탄소 광물고정화 효율 증가를 위한 사문석의 화학적 전처리에 관한 연구)

  • Jang, Na Hyung;Shim, Hyun Min;Hua, Xu Li;Kim, Hyung Teak
    • Applied Chemistry for Engineering
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    • v.19 no.5
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    • pp.526-532
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    • 2008
  • The proposed $CO_2$ storage technology in the present study is a one-step sequestration process that stabilizes $CO_2$ in a reactor with Serpentine. The advantage of this technology is associated with its high stability of final product so that the entire system is recognized as permanent environment-friendly $CO_2$ removal method. Since the sequestration reaction mechanisms are generally understood that carbonation reaction proceeds with very slow rate, so that pretreatment method to increases reaction rate of $CO_2$ carbonation reaction should be developed. To increase the reactivity of Serpentine with $CO_2$, two different methods of pretreatment are carried out in the present investigation. One is heat-treatment, the other is chemical pretreatment. In this study, only chemical pretreatment is considered leaching method of magnesium from Serpentine using sulfuric acid at the various reaction temperatures, times, and acid concentrations. Experimental results illustrated that pretreatment by sulfuric acid increases surface area of serpentine from $11.1209m^2/g$ to $98.7903m^2/g$ and extracts magnesium compounds. Single variable experiment demonstrated the enhancements of magnesium extraction with increased reaction temperature and time. Amount of magnesium extraction is obtained by using the data of ICP-AES as maximum extraction condition of magnesium is 2 M acid solution, $75^{\circ}C$ and 1hr. After performing chemical pretreatment, carbonation yield increased from 23.24% to 46.30% of weight.

A study on the separation and determination of the rare earth Elements by the AG® 50W-X8 cation exchange resin (AG® 50W-X8 양이온교환수지를 이용한 희토류원소의 분리와 분석에 관한 연구)

  • Lee, Jung Sook;Choi, Beom Suk
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.272-278
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    • 2008
  • Methods to separate 14 rare earth elements (REEs) and yttrium by the $AG^{(R)}$ 50W-X8 cation exchange resin, and to determine REEs by inductively coupled plasma atomic emission spectrophotometry (ICP-AES) were described. Ion exchange capacities of REEs on the resin were so high that the REEs were quantitatively ion exchanged under the flow rate of 0.3~1.0 mL/min at pH 1~6. The breakthrough capacity curve of the REEs showed that ion exchange capacities of light REEs (Cerium group) were greater than that of the heavy REEs (Yttrium group). When $200{\mu}g$ of each REEs was ion exchanged on 100 mg of resin, most of the heavy REEs were quantitatively desorbed with 10 mL of 2.0 M of $HNO_3$, while most of the light REEs with 30 mL. The method was applied to the monazite sample. The REEs could be separated from matrix, since ion exchange capacities of matrix ions of Ca, Ti, Mg, Mn were much lower than that of the REEs. However the relative standard deviations of the analytical results by the present method were not improved, as high as 1~5%.