• 제목/요약/키워드: Differential Pulse Voltammetry

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Synthesis and Electrochemical Studies of Cu(II) and Ni(II) Complexes with Tetradentate Schiff Base Ligands

  • 조기형;정병구;김정희;전승원;임채평;최용국
    • Bulletin of the Korean Chemical Society
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    • 제18권8호
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    • pp.850-856
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    • 1997
  • A series of tetradentate Schiff-base ligands; 1,3-bis(salicylideneimino) propane, 1,4-bis(salicylideneimino)butane, and 1,5-bis(salicylideneimino)pentane, and their Cu(Ⅱ) and Ni(Ⅱ) complexes have been synthesized. The properties of ligands and complexes have been characterized by elemental analysis, IR, NMR, UV-Vis spectra, molar conductance, and thermogravimetric anaylsis. The mole ratio of Schiff base to metal at complexes was found to be 1 : 1. All complexes were four-coordinated configuration and non-ionic compound. The electrochemical redox processes of the ligands and their complexes in DMF solution containing 0.1 M TEAP as supporting electrolyte have been investigated by cyclic voltammetry, chronoamperometry, differential pulse voltammetry at glassy carbon electrode, and by controlled potential coulometry at platinum gauze electrode. The redox process of the ligands was highly irreversible, whereas redox process of Cu(Ⅱ) and Ni(Ⅱ) complexes was observed as one electron transfer process of quasi-reversible and diffusion-controlled reaction. Also the electrochemical redox potentials of complexes were affected by chelate ring size of ligands. The diffusion coefficients of Cu(Ⅱ) and Ni(Ⅱ) complexes in DMF solution were determined to be 4.2-6.6×10-6 cm2/sec. Also the exchange rate constants were determined to be 3.6-9.7×10-2 cm/sec.

Synthesis and Electrochemical Studies of Ni(Ⅱ) Complexes with Tetradentate Schiff Base Ligands

  • 정병구;임채평;국성근;조기형;최용국
    • Bulletin of the Korean Chemical Society
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    • 제17권2호
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    • pp.173-179
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    • 1996
  • A series of tetradentate Schiff base ligands; [1,2-bis(naphthylideneimino)ethane, 1,3-bis(naphthylideneimino)propane, 1,4-bis(naphthylideneimino)butane, and 1,5-bis(naphthylideneimino)pentane] and their Ni(Ⅱ) complexes have been synthesized. The properties of these ligands and their Ni(Ⅱ) complexes have been characterized by elemental analysis, IR, NMR, UV-vis spectra, molar conductance, and thermogravimetric analysis. The mole ratio of Schiff base to Ni(Ⅱ) metal was found to be 1:1. The electrochemical redox process of the ligands and their Ni(Ⅱ) complexes in DMF and DMSO solution containing 0.1 M tetraethyl ammonium perchlorate (TEAP) as a supporting electrolyte have been investigated by cyclic voltammetry, chronoamperometry, differential pulse voltammetry, and controlled potential coulometry at glassy carbon electrode. The redox process of the ligands was highly irreversible, whereas redox process of Ni(Ⅱ) complexes were observed as one electron transfer process in quasi-reversible and diffusion-controlled reaction. The electrochemical redox potentials of the Ni(Ⅱ) complexes were affected by the chelate ring size of ligands. The diffusion coefficients of Ni(Ⅱ) complexes containing 0.1 M TEAP in DMSO solution were determined to be 5.7-6.9 × 10-6 cm2/sec. Also the exchange rate constants were determined to be 1.8-9.5 × 10-2 cm2/sec. These values were affected by the chelate ring size of ligands.

Copper phthalocyanine conjugated PANI coated screen printed carbon electrode for electrochemical sensing of 4-NP

  • Ramalingam Manikandan;Jang-Hee Yoon;Seung-Cheol Chang
    • 한국표면공학회지
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    • 제56권1호
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    • pp.40-54
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    • 2023
  • In this work, we synthesized a novel electrochemical sensing materials based on tetracarboxylic copper phthalocyanine (TcCuPtc) conjugated PANI (TcCuPtc@PANI). The synthesized materials were employed to modify the screen-printed carbon electrode (SPCE) for the selective sensing of 4-nitrophenol. The TcCuPtc was conjugated with conducting polymer of PANI through the electrostatic interaction and π-π electron conjugation, the polymer film of PANI to inhibit the leakage of TcCuPtc from the surface of the electrode. The prepared TcCuPtc@PANI were characterized and confirmed by scanning electron microscopy (SEM) with EDX, ATR-IR, UV-vis absorption spectroscopy, cyclic voltammetry, and differential pulse voltammetry techniques. The prepared TcCuPtc@PANI/SPCE showed an excellent electrocatalytic sensing of 4-NP in the linear concentrations from 3 to 500 nM with a LOD of 0.03 nM and a sensitivity of 8.8294 ㎂/nM cm-2. However, the prepared TcCuPtc@PANI/SPCE showed selective sensing of 4-NP in the presence of other interfering species. The practical applicability of the TcCuPtc@PANI/SPCE was employed for the sensing of 4-NP in different water samples by standard addition method and showed satisfactory recovery results.

Voltammetric Determination of Copper(II) at Chemically Modified Carbon Paste Electrodes Containing Alga

  • Bae, Zun-Ung;Kim, Young-Lark;Chang, Hye-Young
    • 분석과학
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    • 제8권4호
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    • pp.611-615
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    • 1995
  • The design of appropriate chemically modified electrodes should allow development of new voltammetric measurement schemes with enhanced selectivity and sensitivity. Microorganism like algae has high ability to trap toxic and heavy metal ions and different affinities for metal ions. A copper(II) ion-selective carbon paste electrode was constructed by incorporating alga Anabaena into a conventional carbon paste mixture, and then the film of 10% Nafion was coated to avoid the swelling of the electrode surface. Copper ion could be deposited at the 25% algamodified electrode for 15 min without the applied potential while stirring the solution by only immersing the electrode in a buffer (pH 4.0) cot1taining copper(II). Temperature was controlled at $35^{\circ}C$. After preconcentration was carried out the electrode was transferred to a 0.1 M potassium chloride solution and was reduced at -0.6 volt at $25^{\circ}C$. The differential pulse anodic stripping voltammetry was employed. A well-defined oxidation peak could be obtained at -0.1 volt (vs SCE). In five deposition / measurement / regeneration cycles, the responses were reproducible and relative standard deviations were 3.3% for $8.0{\times}10^{-4}M$ copper(II). Calibration curve for copper was linear over the range from $2.0{\times}10^{-4}M$ to $1.0{\times}10^{-3}M$. The detection limit was $7.5{\times}10^{-5}M$. Studies of the effect of diverse ions showed that the coexisting metal ions had little or no effect for the determination of copper. But anions such as cyanide. oxalate and EDTA seriously interfered.

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Acetonitrile 용액중에서 살충제 O, O-Dimethyl-O-(3-Methyl-4-Nitrophenyl)-Phosphorothioate (Fenitrothion)의 전기화학적 환원 (On the Electrochemical Reduction of O, O-Dimethyl-O-(3-Methyl-4-Nitrophenyl)-Phosphorthioate (Fenitrothion) Pesticide in Acetonitrile Solution)

  • 김일광;김윤근;천현자
    • 대한화학회지
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    • 제32권3호
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    • pp.186-194
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    • 1988
  • 계면활성 micelle을 형성하는 acetonitrile 용액을 O,O-dimethyl-O-(3-methyl-4-nitrophenyl)-phosphorothioate (Fenitrothion)의 전기화학적 환원을 direct current 및 differential pulase polarography, cyclic voltammetry 그리고 controlled potential coulometry 방법으로 연구하였다. Fenitrothion의 환원과정은 1단계로 4 전자 이동에 의한 부분 가역적 전자이동 화학반응(EC, EC)기구로 O,O-dimethyl-O-(3-methyl-4-hydroxyaminophenyl)-phosphorothioate를 형성하고, 더 높은 음전위에서 2 전자 이동에 따른 양성자 반응으로 phosphorus 원자와 phenoxy group의 단일 결합이 끊어지면서 주 생성물인 p-amino-m-cresol과 dimethyl thiophosphinic acid를 생성하였다. Sodium lauryl sulfate micelle 용액에서 polarography 환원파는 전체적으로 억제 되었으며 특히 1차 환원파는 음이온 micelle의 선택적 작용으로 2단계로 분리되었다.

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비수용매에서 Schiff Base를 가진 Cobalt(II) 착물들의 전기화학적 성질 (Electrochemical Properties of Cobalt(II) Schiff Base Complexes in Nonaqueous Solvent)

  • 오정근;최용국
    • 분석과학
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    • 제15권2호
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    • pp.97-101
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    • 2002
  • Co(II)착물들을 세자리 Schiff base-NOIPH, 네자리 Schiff base-$NOTDH_2$$TNBPH_4$ 로부터 합성하였으며, 이 착물들의 산화-환원 과정 mecanism을 지지 전해질로서 0.1 M TBAP를 포함한 DMF용액에서 작업전극으로 유리질 탄소전극을 사용하여 순환 전압-전류법과 펄스 차이 전압-전류법에 의해서 알아 보았다. [Co(II)$(NOIP)_2$]와 [Co(II)(NOTD)$(H_2O)_2$] 착물의 환원은 Co(III)/Co(II)의 반응이 비가역적으로 진행되고 Co(II)/Co(I)의 반응이 준가역적으로 진행되는 일전자의 2단계반응이 확산 지배적으로 일어났다. 반면에 [$Co(II)_2$(TNBP)] 착물의 환원반응은 $Co(II)_2$가 Co(II)/Co(I)로 진행되는 준가역적이며 일전자 일단계의 반응이 확산지배적으로 일어났다.

Determination of Ascorbic Acid, Acetaminophen, and Caffeine in Urine, Blood Serum by Electrochemical Sensor Based on ZnO-Zn2SnO4-SnO2 Nanocomposite and Graphene

  • Nikpanje, Elham;Bahmaei, Manochehr;Sharif, Amirabdolah Mehrdad
    • Journal of Electrochemical Science and Technology
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    • 제12권2호
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    • pp.173-187
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    • 2021
  • In the present research, a simple electrochemical sensor based on a carbon paste electrode (CPE) modified with ZnO-Zn2SnO4-SnO2 and graphene (ZnO-Zn2SnO4-SnO2/Gr/CPE) was developed for the direct, simultaneous and individual electrochemical measurement of Acetaminophen (AC), Caffeine (Caf) and Ascorbic acid (AA). The synthesized nano-materials were investigated using scanning electron microscopy, X-ray Diffraction, Fourier-transform infrared spectroscopy, and electrochemical impedance spectroscopy techniques. Cyclic voltammetry and differential pulse voltammetry were applied for electrochemical investigation ZnO-Zn2SnO4-SnO2/Gr/CPE, and the impact of scan rate and the concentration of H+ on the electrode's responses were investigated. The voltammograms showed a linear relationship between the response of the electrode for individual oxidation of AA, AC and, Caf in the range of 0.021-120, 0.018-85.3, and 0.02-97.51 μM with the detection limit of 8.94, 6.66 and 7.09 nM (S/N = 3), respectively. Also, the amperometric technique was applied for the measuring of the target molecules in the range of 0.013-16, 0.008-12 and, 0.01-14 μM for AA, AC and, Caf with the detection limit of 6.28, 3.64 and 3.85 nM, respectively. Besides, the ZnO-Zn2SnO4-SnO2/Gr/CPE shows an excellent selectivity, stability, repeatability, and reproducibility for the determination of AA, AC and, Caf. Finally, the proposed sensor was successfully used to show the amount of AA, AC and, Caf in urine, blood serum samples with recoveries ranging between 95.8% and 104.06%.

Electrochemical Detection of Hydroxychloroquine Sulphate Drug using CuO/GO Nanocomposite Modified Carbon Paste Electrode and its Photocatalytic Degradation

  • G. S. Shaila;Dinesh Patil;Naeemakhtar Momin;J. Manjanna
    • 전기화학회지
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    • 제27권1호
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    • pp.15-31
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    • 2024
  • The antimalarial drug hydroxychloroquine sulphate (HCQ) has taken much attention during the first COVID-19 pandemic phase for the treatment of severe acute respiratory infection (SARI) patients. Hence it is interest to study the electrochemical properties and photocatalytic degradation of the HCQ drug. Copper oxide (CuO) nanoparticles, graphene oxide (GO) and CuO/GO NC (nanocomposite) modified carbon paste electrodes (MCPE) are used for the detection of HCQ in an aqueous medium. Electrochemical behaviour of HCQ (20 μM) was observed using CuO/MCPE, GO/MCPE and CuO/GO NC/MCPE in 0.1 M phosphate buffer at pH 7 with a scan rate of 20 to 120 mV s-1 by cyclic voltammetry (CV). Differential pulse voltammetry (DPV) of HCQ was performed for 0.6 to 16 μM HCQ. The CuO/GO NC/MCPE showed a reasonably good sensitivity of 0.33 to 0.44 μA μM cm-2 with LOD of 69 to 92 nM for HCQ. Furthermore, the CuO/GO NC was used as a catalyst for the photodegradation of HCQ by monitoring its UV-Vis absorption spectra. About 98% was degraded in about 34 min under visible light and after 4 cycles it was 87%. The improved photocatalytic activity may be attributed to decrease in bandgap energy and enhanced ability for the electrons to migrate. Thus, CuO/GO NC showed good results for both sensing and degradation applications as well as reproducibility.

Simultaneous Detection of Cd (II), Pb (II), Cu (II), and Hg (II) Ions in Dye Waste Water Using a Boron Doped Diamond Electrode with DPASV

  • Yoon, Jang-Hee;Yang, Jee-Eun;Kim, Jong-Phil;Bae, Jong-Seong;Shim, Yoon-Bo;Won, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • 제31권1호
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    • pp.140-145
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    • 2010
  • The simultaneous detection of Cd (II), Pb (II), Cu (II), and Hg (II) ions in aqueous medium using a BDD electrode with DPASV is described. XPS was used to characterize the chemical states of trace metal ions deposited on the BDD electrode surface. Experimental parameters that affect response, such as pH, deposition time, deposition potential, and pulse amplitude were carefully optimized. The detection limits for Cd (II), Pb (II), Cu (II), and Hg (II) ions were 3.5 ppb, 2.0 ppb, 0.1 ppb and 0.7 ppb, respectively. The application of the BDD electrode on the electrochemical pretreatment for the simultaneous metal detection in the dye waste water was also investigated.

Determination of Lead(II) at Nafion-DTPA-Glycerol-Modified Glassy Carbon Electrodes

  • Park, Eun-Heui;Park, Chan-Ju;Chung, Keun-Ho
    • 한국환경보건학회:학술대회논문집
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    • 한국환경보건학회 2003년도 Challenges and Achievements in Environmental Health
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    • pp.204-207
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    • 2003
  • Determination of Lead(II) using nafion-DTPA (diethylene triamine pentaacetic acid)-glycerol-modified glassy carbon electrodes is described. Lead(II) is accumulated at the electrode by complexing with the DTPA, reduced, and detected by differential pulse voltammetry. In this study, we demonstrate that at a preconcentration time of 5min the nafion-DTPA-glycerol-modified glassy carbon electrode has a linear calibration curve at range 1.0${\times}$10$\^$-9/M∼1.0${\times}$10$\^$-7/M in pH 4.0 buffer solution. The detection limit(3$\sigma$) is as low as 5.0${\times}$10$\^$-6/M. This method is applied to the determination of lead(II) in certified reference material and the result agrees satisfactorily with the certified value.

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