• Title/Summary/Keyword: Electrochemical Determination

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Determination of Ag(Ⅰ) Ion with a Chemically Modified Carbon Paste Electrode Containing Cinchonidine (Cinchonidine으로 변성된 Carbon Paste 전극을 사용한 은이온의 정량)

  • Kim, Sin Hui;Won, Mi Suk;Sim, Yun Bo
    • Journal of the Korean Chemical Society
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    • v.38 no.10
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    • pp.734-740
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    • 1994
  • Electrochemical determination of Ag(I) ion was carried out by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) with the carbon paste electrode (CPE) containing cinchonidine. The detection limit for Ag(I) ion was shown to be $1.0 {\times}10^{-6}$ M in conventional CV and up to $8.0{\times}10^{-9}$ M (${\pm}$0.6%) using DPV. The optimum analytical condition of Ag(I) ion was determined as follows: pH 7, 20 minutes of deposition time, and 50% (w/w) cinchonidine to carbon powder composition of electrode. The interference effect of various metal ions added to the deposition solution was also studied. The peak current of Ag(I) ion except Hg(II) ion was decreased roughly 25% compare to Ag(I) ion only. When Mn(II) ion was present in sample solution at pH 9, shown a large interference effect.

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Amperometric Enzyme Electrode for the Determination of $NH_4^+$ ($NH_4^+$ 정량을 위한 Amperometric Enzyme Electrode)

  • Moo Lyong Seo;Jae Sang Kim;Shim Sung Lee;Zun Ung Bae;Heung Lark Lee;Tae Myung Park
    • Journal of the Korean Chemical Society
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    • v.37 no.11
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    • pp.937-942
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    • 1993
  • Enzyme electrodes for amperometric measurement of ammonia was prepared by immobilization of L-glutamate dehydrogenase on an Immobilon-AV Affinity membrane and attachment to a glassy carbon electrode. Reduced nicotinamide adenine dinucleotide (NADH) was used as the electroactive species. The electrochemical oxidation of NADH was monitored at +1.0 volt vs. Ag/AgCl. Response was linear from $4.0\;{\times}\;10^{-5}\;to\;4.0\;{\times}\;10^{-4}$ M. The detection limit was 2.0 ${\times}\;10^{-6}$ M. Response time, the optimum pH and life time of enzyme immobilized membrane were 2 min, pH 7.3∼7.6 (Dulbecco's buffer solution) and about 25 days respectively. When the enzyme electrode was applied to the $NH_4^+$ determination with amperometric method, other physiological materials had no interference.

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Studies on Electrochemical Behavior of Some Light Lanthanide Ions in Nonaqueous Solution, Flow Injection Determination and Photochemical Characterization of Heavy Metal Ion Chelate Eight Coordinated Complexes. (Part 2) (비수용액에서 가벼운 란탄족 이온의 전기화학적 거동, 흐름 주입법에 의한 정량 및 중금속 이온의 킬레이트형 8-배위 착물의 광화학적 특성 연구 (제 2 보) : 계면활성제 존재하에서 Chromeazurol S를 사용하여 몇 가지 란탄이온의 흐름주입법에 의한 정량)

  • Gang, Sam U;Jang, Ju Hwan;Kim, Il Gwang;Han, Hong Seok;Jo, Gwang Hui
    • Journal of the Korean Chemical Society
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    • v.38 no.1
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    • pp.50-54
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    • 1994
  • Spectrophotometric determination of some light lanthanide ions by flow injection method is described. Chromeazurol S forms water soluble complex with lanthanide ions in the presence of DTAB. The absorption maximum of the complexes are from 650 nm to 655 nm and the molar absorptivities were ca. $1.8{\times}10^5\;L mol^{-1}cm^{-1}$ on Tris buffer (pH 10.5). The calibration curves for Nd(III), Eu(III) and Sm(III) obtained by FIA are over the range of 0.1 to 0.6 ppm and the correlation coefficient were ca. 0.9993. The detection limits (S/N) were from 10 ppb for Nd(III) and Eu(III) to 20 ppb for Sm(III). The relative standard deviations was ${\pm}$.2% for 0.4 ppm sample. The samples throughput was ca. $50\;cm^{-1}$.

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Characteristics of Optimized Analytical Method of Hydrogen Cyanide in Cigarette Mainstream Smoke by Using Continuous Flow Analyzer(CFA) (Continuous Flow Analyzer(CFA)를 이용한 담배 주류연 중 Hydrogen Cyanide(HCN)의 최적 분석방법 구명)

  • Na, Seung-Ju;Eo, Sung-Je;Kim, Do-Yeon;Bock, Jin-Young;Hwang, Keon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.31 no.1
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    • pp.39-44
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    • 2009
  • Hydrogen cyanide (HCN) is present in both the particulate and vapor phase of cigarette mainstream smoke. It is one of the 44 harmful substances on Hoffmann's list and is known to be a major ciliatoxic agent in cigarette mainstream smoke. Typically the determination of HCN in cigarette mainstream smoke has been done through colorimetric and electrochemical techniques, such as UV-spectrophotometry (UV), continuous flow analyzer (CFA), ion chromatography (IC) and capillary GC-ECD. In particular, CFA commonly has been using analysis hydrogen cyanide in cigarette smoke and the basic principle is pyridine-pyrazolone reaction. In this study, the more optimized analytical method is suggested isonicotinic acid-pyrazolone reaction method than previous pyridine-pyrazolone reaction method, a commonly used method for the determination of cyanide in water and air, by CFA. Sample collection was optimized by trapping particulate and vapor phase of smoke separately. The optimum NaOH concentration of the trapping solution was shown to be 0.2 M. HCN was stable up to 6 hours in this concentration but only 3 hours in 0.1 M solution. The sensitivity of this method was fairly good and it might be used in analysis of HCN in cigarette mainstream smoke.

Electroanalytical Applications Based on Carbon Nanotube/Prussian Blue Screen-printable Composite

  • Shim, Jun-Ho;Lee, Jae-Seon;Cha, Geun-Sig;Nam, Hak-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.31 no.6
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    • pp.1583-1588
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    • 2010
  • A single step fabrication process of carbon nanotube/Prussian Blue (CNT/PB) paste electrodes based on screen printing technology has been studied as an amperometric sensor for the determination of hydrogen peroxide and free chlorine. Compared to the classical carbon paste (CP) electrode, the CNT paste electrode greatly enhanced the response in the presence of hydrogen peroxide due to the electrocatalytic activity of the CNT. Based on the CNT/binder paste, PB was also incorporated into a network of CNT paste and characterized. The best electroanalytical properties of PB-mixed sensors to hydrogen peroxide were obtained with PB ratio of 10 wt % composition, which showed fast response time ($t_{90}{\leq}5$ s; 0.2 - 0.3 mM), low detection limit of 1.0 ${\mu}M$, good linear response in the range from $5.0{\times}10^{-5}$ - $1.0{\times}10^{-3}$ mol $L^{-1}$ ($r^2$ = 0.9998), and high sensitivity of -8.21 ${\mu}AmM^{-1}$. In order to confirm the enhanced electrochemical properties of CNT/PB electrode, the sensor was further applied for the determination of chlorine in water, which exhibited a linear response behavior in the range of 50 - 2000 ppb for chlorine with a slope of 1.10 ${\mu}Appm^{-1}$ ($r^2$ = 9971).

Determination of the Langmuir and Temkin Adsorption Isotherms of H for the Cathodic H2 Evolution Reaction at a Pt/KOH Solution Interface Using the Phase-Shift Method

  • Chun Jang-H.;Jeon Sang-K.;Chun Jin-Y.
    • Journal of the Korean Electrochemical Society
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    • v.9 no.1
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    • pp.19-28
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    • 2006
  • The phase-shift method for determining the Langmuir, Frumkin, and Temkin adsorption isotherms ($\theta_H\;vs.\;E$) of H for the cathodic $H_2$ evolution reaction (HER) at a Pt/0.1 M KOH solution interface has been proposed and verified using cyclic voltammetric, differential pulse voltammetric, and electrochemical impedance techniques. At the Pt/0.1 M KOH solution interface, the Langmuir and Temkin adsorption isotherms ($\theta_H\;vs.\;E$), the equilibrium constants ($K_H=2.9X10^{-4}mol^{-1}$ for the Langmuir and $K_H=2.9X10^{-3}\exp(-4.6\theta_H)mol^{-1}$ for the Temkin adsorption isotherm), the interaction parameters (g=0 far the Langmuir and g=4.6 for the Temkin adsorption isotherm), the rate of change of the standard free energy of $\theta_H\;with\;\theta_H$ (r=11.4 kJ $mol^{-1}$ for g=4.6), and the standard free energies (${\Delta}G_{ads}^{\circ}=20.2kJ\;mol^{-1}$ for $k_H=2.9\times10^{-4}mol^{-1}$, i.e., the Langmuir adsorption isotherm, and $16.7<{\Delta}G_\theta^{\circ}<23.6kJ\;mol^{-1}$ for $K_H=2.9\times10^{-3}\exp(-4.6\theta_H)mol^{-1}$ and $0.2<\theta_H<0.8$, i.e., the Temkin adsorption isotherm) of H for the cathodic HER are determined using the phase-shift method. At intermediate values of $\theta_H$, i.e., $0.2<\theta_H<0.8$, the Temkin adsorption isotherm ($\theta_H\;vs.\;E$) corresponding to the Langmuir adsorption isotherm ($\theta_H\;vs.\;E$), and vice versa, is readily determined using the constant conversion factors. The phase-shift method and constant conversion factors are useful and effective for determining the Langmuir, Frumkin, and Temkin adsorption isotherms of intermediates for sequential reactions and related electrode kinetic and thermodynamic data at electrode catalyst interfaces.

Determination of Adsorption Isotherms of Hydrogen on Zirconium in Sulfuric Acid Solution Using the Phase-Shift Method and Correlation Constants

  • Chun, Jang-H.;Chun, Jin-Y.
    • Journal of the Korean Electrochemical Society
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    • v.12 no.1
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    • pp.26-33
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    • 2009
  • The phase-shift method and correlation constants, i.e., the unique electrochemical impedance spectroscopy (EIS) techniques for studying the linear relationship between the behavior ($-{\varphi}$ vs. E) of the phase shift ($90^{\circ}{\geq}-{\varphi}{\geq}0^{\circ}$) for the optimum intermediate frequency and that ($\theta$ vs. E) of the fractional surface coverage ($0{\leq}{\theta}{\leq}1$), have been proposed and verified to determine the Langmuir, Frumkin, and Temkin adsorption isotherms of H and related electrode kinetic and thermodynamic parameters at noble metal (alloy)/aqueous solution interfaces. At a Zr/0.2 M ${H_2}{SO_4}$ aqueous solution interface, the Frumkin and Temkin adsorption isotherms ($\theta$ vs. E), equilibrium constants (K = $1.401{\times}10^{-17}\exp(-3.5{\theta})mol^{-1}$ for the Frumkin and K = $1.401{\times}10^{-16}\exp(8.1{\theta})mol^{-1}$ for the Temkin adsorption isotherm), interaction parameters (g = 3.5 for the Frumkin and g = 8.1 for the Temkin adsorption isotherm), rates of change of the standard free energy (r = $8.7\;kJ\;mol^{-1}$ for g = 3.5 and r = $20\;kJ\;mol^{-1}$ for g = 8.1) of H with $\theta$, and standard free energies ($96.13{\leq}{\Delta}G^0_{\theta}{\leq}104.8\;kJ\;mol^{-1}$ for K = $1.401{\times}10^{-17}\exp(-3.5{\theta})mol^{-1}$ and $0{\leq}{\theta}{\leq}1$ and ($94.44<{\Delta}G^0_{\theta}<106.5\;kJ\;mol^{-1}$ for K = $1.401{\times}10^{-16}\exp(-8.1{\theta})mol^{-1}$ and $0.2<{\theta}<0.8$) of H are determined using the phase-shift method and correlation constants. At 0.2 < $\theta$ < 0.8, the Temkin adsorption isotherm correlating with the Frumkin adsorption isotherm, and vice versa, is readily determined using the correlation constants. The phase-shift method and correlation constants are probably the most accurate, useful, and effective ways to determine the adsorption isotherms of H and related electrode kinetic and thermodynamic parameters at highly corrosion-resistant metal/aqueous solution interfaces.

A study on electrochemical protection diagrams of steel in nitric and sulfuric acid solutions (질산과 황산 용액중의 철강의 전기방식도에 관한 연구)

  • 전대희;김진경
    • Journal of Advanced Marine Engineering and Technology
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    • v.13 no.2
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    • pp.43-63
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    • 1989
  • Various kinds of corrosion prevention methods have been developed. It is known that the method of electrochemical protection is more effective and economical than any other method on the large scale metal structures in corrosive solutions. Strong acid solutions such as nitric and sulfuric acid solutions are often used in industries, and the expensive stainless steel is almost exclusively used for the equipment that comes in contact with such acid solutions. However, it is more reasonable that carbon steel is used rather than stainless steel depending upon concentration of those acid solutions from the economical viewpoint. In this study, the typical strong acid solution such as nitric and sulfuric acid solutions are chosen for the experiment and the selected materials of specimen are the stainless steels of SUS 304L and SUS 316L, the carbon steels of SS 41, SM 50 and RA 32, and highly pure lead. Electrochemical protection diagrams can be drawn with data from the external cathodic and anodic polarization curves of SUS 304L, SUS 316L and SM 50 steels in 5-60% nitric acid solutions and from those polarization curves of SS 41, RA 32, SM 50 and SUS 316L steels, and highly pure lead in 2.5-98% sulfuric acid solutions at the slow scanning rate. The data obtained with using the determination method of the optimum cathodic protection potential, the Tafel extrapolation method and the characteristics of anodic polarization curves. The main results obtained from the diagrams are as follows: 1) In nitric acid solution : (1) Corrosion potentials exist in each of those corrosion zones on the stainless steels in the lower concentration than about 12% solutions and on the high tensile strength steels in the lower concentration than about 30% solutions, but the corrosion current (density) in each zone is small on the above mentioned former steels and large on the latter ones. (2) The stainless steels can be self-passivated in the higher concentration than 15% solutions, and the high tensile strength steels gives rise to the same phenomenon in the higher concentration than 35% solutions. (3) The stainless steels in the lower concentration than 60% solutions and the high tensile strength steels in the higher concentration than 35% solutions can be used without protection, but the latter steels must ve protected anodically in the lower conccentration than about 30% solutions. 2) In sufuric acid solution : (1) The carbon steels can be self-passivated in the higher concentration than 45% solutions, and the SUS 316L steel in higher concentration than 75% solutions and the lead in all concentration solutions also gives rise to the same phenomenon. (2) The lead in the lower concentration than 80% solutions and the SUS 316L steel in the higher concentration than 80% solutions can be used without protection. (3) The carbon steels in the higher concentration than 50% solutions also can be used without protecting economically, but the SUS 316L steel in the 20-70% solutions are considerably corrosive without protecting anodically.

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Influence of Polarization Behaviors on the ECM Characteristics of SnPb Solder Alloys in PCB (PCB에서의 ECM 특성에 미치는 SnPb 솔더 합금의 분극거동의 영향)

  • Lee Shin-Bok;Yoo Young-Ran;Jung Ja-Young;Park Young-Bae;Kim Young-Sik;Joo Young-Chang
    • Journal of the Microelectronics and Packaging Society
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    • v.12 no.2 s.35
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    • pp.167-174
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    • 2005
  • Smaller size and higher integration of electronic components make smaller gap between metal conducting layers in electronic package. Under harsh environmental conditions (high temperature/humidity), electronic component respond to applied voltages by electrochemically ionization of metal and metal filament formation, which lead to short failure and this phenomenon is termed electrochemical migration(ECM). In this work, printed circuit board(PCB) is used for determination of ECM characteristics. Copper leads of PCB are soldered by eutectic solder alloys. Insulation breakdown time is measured at $85^{\circ}C,\;85{\%}RH$. CAF is the main mechanism of ECM at PCB. Pb is more susceptible to CAF rather than Sn, which corresponds well to the corrosion resistance of solder materials in aqueous environment. Polarization tests in chloride or chloride-free solutions fur pure metal and eutectic solder alloys are performed to understand ECM characteristics. Lifetime results show well defined log-normal distribution which resulted in biased voltage factor(n=2) by voltage scaling. Details on migration mechanism and lifetime statistics will be presented and discussed.

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A Study of Liquid Chromatographic Detection Method for Thiocarbamates by Using Photochemical Reaction (광화학 반응을 이용한 티오카바메이트류의 액체 크로마토그래피 검출법에 관한 연구)

  • Dai Woon Lee;Young Hun Park;Yong Wook Choi
    • Journal of the Korean Chemical Society
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    • v.37 no.4
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    • pp.453-461
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    • 1993
  • Detection method was developed using a simply designed photochemical reactor made of teflon coil and low pressure mercury lamp. This method of UV photolysis of analytes followed by UV, fluorescence and electrochemical detection was found to be useful for four thiocarbamates. Analytes eluting from the column are irradiated with a high flux of 254 nm UV light, so that they change to either fluorescent active forms or highly electrochemically sensitive products. Appling this technique to the UV detection, thiocarbamates were converted into long wavelength absorbing products upon UV irradiation. In fluorescence detector four thiocarbamates are not detected at nonirradiated condition but fluorescence signals of MPTC, CPTC photolysates are appeared after irradiation with UV light. The electrochemical detection for the determination of thiocarbamates was enhanced up to 5∼20 fold signal after UV irradiation, compared to that of the nonirradiated. The detection limit of thiocarbamates on electrochemical detector was 13.3∼0.02 ng under pH 7.0, ionic strength $0.5{\times}10^{-2}$ M, phosphate buffer solution. Adducts produced by reaction of photolysates and OPA-MERC in the reaction coil were monitored at 425 nm with fluorescence detector, and one of the photolysates was primary amine.

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