• Title/Summary/Keyword: voltammetric analysis

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Determination of Hg22+ Ions Using a Modified Glassy Carbon Electrode with 2,2':6':2''-Terpyridine

  • Kong, Young-Tae;Bae, Yun-Jung;Shim, Yoon-Bo
    • Bulletin of the Korean Chemical Society
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    • v.23 no.2
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    • pp.346-350
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    • 2002
  • A glassy carbon electrode (GCE) modified with 2,2':6':2”-terpyridine (2,2':6':2”-TPR) using a spin coating method was applied for the highly selective and sensitive analysis of a trace amount of $Hg_2^{2+}$ ions. Various experimental parameters, which influenced the response of the 2,2':6':2”-TPR modified electrode to $Hg_2^{2+}$ ions, were optimized. The linear sweep and differential pulse voltammograms for the 2,2':6':2”-TPR modified electrode deposited with Hg show a well-defined anodic peak at +0.65 V (vs. Ag|AgCl). After a 25 min preconcentration time in an $Hg_2^{2+}$ ion solution (0.1 M acetate buffer, pH 5.0), differential pulse voltammetry(DPV) with 2,2':6':2”-TPR modified electrode shows a linear response between $1.0\;{\times}\;10^{-6}M\;and\;2.0\;{\times}\;10^{-7}M$. The least-square treatment of these data produce an equation of I[${\mu}A$] = 0.031 + 0.005C with r = 0.980(n = 5). The detection limit of this electrode with linear sweep voltammetry and differential pulse anodic voltammetry were $2.0\;{\times}\;10^{-6}M\;and\;8.0\;{\times}\;10^{-8}M$, respectively. The presence of Pb, Fe, Cd, Ti, Ni, Co, Mg, Al, Mn, and Zn did not interfere in the analysis of the $Hg_2^{2+}$ ion. The 2,2':6':2”-TPR modified GCE has been successfully applied in determination trace amounts of Hg in a human urine sample.

Synthesis of Tridentate Schiff base Molybdenum(Ⅴ) Complexes and Their Electrochemical Properties in Aprotic Solvents (세자리 Schiff base 몰리브데늄(Ⅴ) 착물들의 합성과 비수용매에서의 전기화학적 성질)

  • Choi, Young-Kook;Song, Mi-Sook;Rim, Chae-Pyeong;Chjo, Ki-Hyung
    • Journal of the Korean Chemical Society
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    • v.39 no.1
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    • pp.47-56
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    • 1995
  • Tridentate Schiff base molybdenum(V) complexes such as [Mo(Ⅴ)2O(SOHB)4], [Mo(Ⅴ)2O3(SOIP)2(NCS)2] and [Mo(Ⅴ)2O3(SOTB)2(H20)2](SOHB: Salicylidene-o-imino hydroxybenzene, SOIP; Salicylidene-o-imino pyridine, SOTB; Salicylidene-o-imino thiolbenzene) were synthesized and identified by elemental analysis, spectroscopy, and thermogravimetric analysis (TGA). It was found that the mole ratio of Schiff base ligand to the metal in these complexes is 1 : 1 or 1 : 2. The redox processes of the complexes were investigated by cyclic voltammetric and differential pulse polarographic techniques in nonaquous solvent containing 0.1 M tetraethylammonium perchlorate (TEAP) as supporting electrolyte at glassy carbon electrode. It was found that diffusion controlled reduction processes with one electron were Mo(Ⅴ)Mo(Ⅴ)e-→ Mo(Ⅴ)Mo(Ⅳ)e-→Mo(Ⅳ)Mo(Ⅳ)e-→Mo(Ⅳ)Mo(Ⅲ).

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Various Temperatures Affecting Characteristics of Pt/C Cathode Catalysts for Polymer Electrolyte Membrane Fuel Cells (Polymer Electrolyte Membrane Fuel Cells용 Pt/C 캐소드 전극촉매 특성에 미치는 반응 온도)

  • Yoo, Sung-Yeol;Kang, Suk-Min;Lee, Jin-A;Rhee, Choong-Kyun;Ryu, Ho-Jin
    • Korean Journal of Materials Research
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    • v.21 no.3
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    • pp.180-185
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    • 2011
  • This study is aimed to increase the activity of cathodic catalysts for PEMFCs(Polymer Electrolyte Membrane Fuel Cells). we investigated the temperature effect of 20wt% Pt/C catalysts at five different temperatures. The catalysts were synthesized by using chemical reduction method. Before adding the formaldehyde as reducing agent, process was undergone for 2 hours at the room temperature (RT), $40^{\circ}C$, $60^{\circ}C$, $80^{\circ}C$ and $100^{\circ}C$, respectively. The performances of synthesize catalysts are compared. The electrochemical oxygen reduction reaction (ORR) was studied on 20wt% Pt/C catalysts by using a glassy carbon electrode through cyclic voltammetric curves (CV) in a 1M H2SO4 solution. The ORR specific activities of 20wt% Pt/C catalysts increased to give a relative ORR catalytic activity ordering of $80^{\circ}C$ > $100^{\circ}C$ > $60^{\circ}C$ > $40^{\circ}C$ > RT. Electrochemical active surface area (EAS) was calculated with cyclic voltammetry analysis. Prepared Pt/C (at $80^{\circ}C$, $100^{\circ}C$) catalysts has higher ESA than other catalysts. Physical characterization was made by using X-ray diffraction (XRD) and transmission electron microscope (TEM). The TEM images of the carbon supported platinum electrocatalysts ($80^{\circ}C$, $100^{\circ}C$) showed homogenous particle distribution with particle size of about 2~3.5 nm. We found that a higher reaction temperature resulted in more uniform particle distribution than lower reaction temperature and then the XRD results showed that the crystalline structure of the synthesized catalysts are seen FCC structure.

Photoelectrochemical Cell Study on Closely Arranged Vertical Nanorod Bundles of CdSe and Zn doped CdSe Films

  • Soundararajan, D.;Yoon, J.K.;Kwon, J.S.;Kim, Y.I.;Kim, S.H.;Park, J.H.;Kim, Y.J.;Park, D.Y.;Kim, B.C.;Wallac, G.G.;Ko, J.M.
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2185-2189
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    • 2010
  • Closely arranged CdSe and Zn doped CdSe vertical nanorod bundles were grown directly on FTO coated glass by using electrodeposition method. Structural analysis by XRD showed the hexagonal phase without any precipitates related to Zn. FE-SEM image showed end capped vertically aligned nanorods arranged closely. From the UV-vis transmittance spectra, band gap energy was found to vary between 1.94 and 1.98 eV due to the incorporation of Zn. Solar cell parameters were obtained by assembling photoelectrochemical cells using CdSe and CdSe:Zn photoanodes, Pt cathode and polysulfide (1M $Na_2S$ + 1M S + 1M NaOH) electrolyte. The efficiency was found to increase from 0.16 to 0.22 upon Zn doping. Electrochemical impedance spectra (EIS) indicate that the charge-transfer resistance on the FTO/CdSe/polysulfide interface was greater than on FTO/CdSe:Zn/polysulfide. Cyclic voltammetry results also indicate that the FTO/CdSe:Zn/polysulfide showed higher activity towards polysulfide redox reaction than that of FTO/CdSe/polysulfide.

Electrochemical Behaviors of N'-phenyl-N-(2-chloroethyl)-N-nitrosourea Analogous and Synthesis of N-aminourea (N'-phenyl-N-(2-chloroethyl)-N-nitrosourea 유사체의 전기화학적 거동 및 N-aminourea의 합성)

  • Won, Mi-Sook;Kim, Jeong-Gyun;Sim, Yoon-Bo
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.707-712
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    • 1991
  • N'-phenyl-N-(2-chloroethyl)-N-aminourea has been prepared from N'-phenyl-N-(2-chloroethyl)-N-nitrosourea by means of the electrochemical reduction with the mercury pool electrolytic cell. In order to find out the optimum condition of the reaction, the voltammetric behaviors for N'-aryl-N-(2-chloroethyl)-N-nitrosourea derivatives have been investigated by the cyclic voltammetry and polarography. The peak potentials was shifted to the negative direction as the pH value of the solution decrease. The substituent effects of phenyl ring on the peak potential were not observed in this case. (5:3) EtOH/4 N-HCl mixed solution was employed for the electrolysis. The applied potential was -0.7 V vs. Ag/AgCl/4 N-HCl electrode. The number of electrons participated to the reduction process was 4, respectively. The product was identified by FT-IR, NMR, mass and/or elemental analysis data.

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Electricity Generation from Dairy Wastewater Using Microbial Fuel Cell (미생물연료전지를 이용한 유가공 폐수로부터 전기생산)

  • Roh, Sung-Hee;Lee, Sung-Wook;Kim, Kyung-Ryang;Kim, Sun-Il
    • Applied Chemistry for Engineering
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    • v.23 no.3
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    • pp.297-301
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    • 2012
  • Microbial fuel cell (MFC) is the major of bio-electrochemical system which can convert biomass spontaneously into electricity through the metabolic activity of the microorganisms. In this study, we used an activated sludge as a microbial inoculum and then investigated the feasibility of using dairy wastewater as a possible substrate for generating electricity in MFC. To examine the performance of MFC as power generator, the characteristics on cell potentials, power density, cyclic voltammetric analysis and sustainable power estimation were evaluated for dairy wastewater. The maximum power density of $40\;mW/m^2$was achieved when the dairy wastewater containing 2650 mg/L COD was used, leading to the removal of 88% of the COD. The results from this study demonstrate the feasibility of using MFC technology to generate electricity while simultaneously treating dairy wastewater effectively.

Use of hybrid materials in the trace determination of As(V) from aqueous solutions: An electrochemical study

  • Tiwari, Diwakar;Jamsheera, A.;Zirlianngura, Zirlianngura;Lee, Seung Mok
    • Environmental Engineering Research
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    • v.22 no.2
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    • pp.186-192
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    • 2017
  • The carbon paste electrode (CPE) was modified with the pristine bentonite and hybrid material (HDTMA-modified bentonite). The modified-CPEs are then employed as working electrode in an electrochemical detection of As(V) from aqueous solutions using the cyclic voltammetric measurements. Cyclic voltammograms revealed that As(V) showed reversible behavior onto the working electrode. The hybrid material-modified carbon paste electrode showed significantly enhanced electrochemical signal which was then utilized in the low level detection of As(V). Moreover, the studies were conducted at neutral pH conditions. The electrochemical studies were conducted with scan rates (20 to 200 mV/s) to deduce the mechanism of redox processes involved at the electrode surface. The anodic current was linearly increased, increasing the concentration of As(V) from 5.0 to $35.0{\mu}g/g$ using the hybrid material-modified electrode. This provided fairly a good calibration line for As(V) detection. The presence of varied concentrations of As(III) in the determination of total arsenic was studied. The influence of several cations and anions viz., Cu(II), Mn(II), Zn(II), Pb(II), Cd(II), Fe(III), $Cl^-$, $NO_3{^-}$, $PO_4{^{3-}}$, EDTA and glycine in the detection of As(V) from aqueous solution was also studied. Further, in an attempt to simulate the real matrix analysis, the tap water sample was spiked with As(V) and subjected for As(V) detection using the modified-CPE.

Development of Gold Amalgam Voltametric Microelectrode for the Quantification of O2, Fe2+, Mn2+, and HS- (퇴적물 공극수내 O2, Fe2+, Mn2+ 및 HS- 센싱을 위한 금아말감 미세전극 개발)

  • Kwon, Soongil;Park, Donggeun;Choi, Geunyoung;Sung, Jaebin;Kim, Hyunsoo;Lee, Jae Woo;Hong, Yongseok
    • Journal of Korean Society on Water Environment
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    • v.38 no.2
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    • pp.103-112
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    • 2022
  • A gold amalgam voltammetric microelectrode (GAVM) system was developed for the quantification of dissolved biogeochemical species, such as O2, Fe2+, Mn2+, and HS- in sediment porewater. Commercially available Ag/AgCl and platinum electrodes were used as the reference and counter electrode, respectively, and a gold amalgam microelectrode was fabricated in the laboratory using 150-um diameter gold wire and a borosilicate capillary tube with a 1.6-mm diameter. A portable potentiostat (Metrohm, DropSens) was used for the application of voltage sweeping and to acquire the electric current. For sediment profiling, a commercially available actuator was customized and modified. The analysis method used in the system used the most widely used analysis method among the electrochemical analysis currently used The GAVM system was successively calibrated with the species and applied to estuarine sediments. The porewater analysis showed that the oxygen concentration was decreased to zero at a depth of 0.6 mm, and maximum Mn2+ and Fe2+ concentrations of 50 uM and 20 uM were detected at 2 and 3-cm depths, respectively. Maximum HS- concentrations of 10 uM were detected at 4 cm in the deeper sediments. The GAVM system was successfully developed and applied to the sediment and can be used to better understand biogeochemical reactions.

Analysis on the Langmuir Adsorption Isotherm of the Over-Potentially Deposited Hydrogen (OPD H) at the Polycrystalline Au|Acidic Aqueous Electrolyte Interface Using the Phase-Shift Method

  • Chun Jang H.;Jeon Sang K.
    • Journal of the Korean Electrochemical Society
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    • v.4 no.3
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    • pp.118-124
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    • 2001
  • The Langmuir adsorption isotherm of the over-potentially deposited hydrogen (OPD H) for the cathodic $H_2$ evolution reaction (HER) at the $poly-Au|0.5M\;H_2SO_4$ aqueous electrolyte interface has been studied using cyclic voltammetric and ac impedance techniques. The behavior of the phase shift $(0^{\circ}\leq{-\phi}\leq90^{\circ})$ for the optimum intermediate frequency corresponds well to that of the fractional surface coverage $(1\geq{\theta}\geq0)$ at the interface. The phase-shift profile $({-\phi}\;vs.\;E)$ for the optimum intermediate frequency, i.e., the phase-shift method, can be used as a new method to estimate the Langmuir adsorption isotherm $(\theta\;vs.\;E)$ of the OPD H for the cathodic HER at the interface. At the poly-$Au|0.5M\;H_2SO_4$ electrolyte interface, the equilibrium constant (K) and standard free energy $({\Delta}G_{ads})$ of the OPD H are $2.3\times10^{-6}\;and\;32.2\;kJ\;mol^{-1}$, respectively.

Electrochemical Analysis of Alkylammonium Halides by Addition of Crown Ether (크라운 에테르첨가에 의한 할로겐화 알킬암모늄의 전기화학적 분석)

  • Chong Min Park;Myung Yong Park
    • Journal of the Korean Chemical Society
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    • v.33 no.1
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    • pp.37-45
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    • 1989
  • Voltammetric behavior of alkylammonium ion was studied in the absence and in the presence of crown ether in propylene carbonate as solvent. The peak potentials and the peak currents, their dependency on the concentrations, the reversibility of the electrode reactions are described. In the presence of crown ether chemical reaction might be preceeded before the electron-transfer process, the peak potential for the reduction shifts at the negative direction as the concentration of crown ether to the electrolyte solution increases. The addition of crown ether(20mM 18CR6)to the electrolyte solution made it possible to determine voltammetrically the dialkylammonium ions($Me_2NH^{+}_{2};O.6{\sim}0.8mM$) in the presence of the monoalkylammonium ions ($EtNH^{+}_{3} ;1.6mM$) and the monoalkylammonium ions ($EtNH^{+}_{3} ; 0.5{\sim}2.5mM$) in the presence of the dialkylammonium ions($Me_2NH^{+}_{2};0.5mM$)

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