• Journal of the Korean Chemical Society
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• v.33 no.2
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• pp.215-224
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• 1989

Electrochemical reductions of $trans-[Co(en)_2X_2](ClO_4)_n$ (where X is cyanide, nitrite, ammonia, and isothiocyanate) were investigated by cyclic voltammetry and polarography at mercury and glassy carbon electrode. $trans-[Co(en)_2(CN)_2]ClO_4$ was reduced to Co(II) complex followed by adsorption to the mercury electrode. Cyanide ion was not released from the reduced Co(II) complex but the cyanide and (en) were released after the reduction to metallic cobalt. The other complexes except $trans-[Co(en)_2(CN)_2]ClO_4$ were reduced to cobalt(II) complexes followed by release of monodendate ligand, and (en) was released at the reduction step to metallic cobalt. $trans-[Co(en)_2(NO_2)_2]ClO_4$ was reduced to cobalt(Ⅱ) complex, and $NO_2^-$ ion was released followed by electroreduction through ECE mechanism at pH 2. On glassy carbon electrode, all complexes of Co(III) were reduced to Co(II) complexes with irreversible one-electron diffusion controlled reaction in which (en) was not released at this step. Increasing absorption wave number of complexes caused to negative shift of peak potential.

• Analytical Science and Technology
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• v.23 no.1
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• pp.68-73
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• 2010

In order to develop the square wave voltammetric method determining cimetidine in an ampoule for injection, $5.00{\times}10^{-4}\;M$ cimetidine HCl solutions prepared with phosphate buffers of various pH values (3.01~8.97) were investigated by SWV. The well defined single peak due to the electrochemical reduction of -C=N-C$\equiv$N- in the structure of cimetidine moved towards the cathodic direction by -0.051V/pH as the pH values were increased indicating the involvement of hydrogen in its reduction. The calibration curves of cimetidine HCl in the concentration range between $1.00{\times}10^{-5}\;M$ and $5.00{\times}10^{-3}\;M$ prepared using three phosphate buffers yielded the slopes of 127,407nA/M (pH 3.01), 115,125nA/M (pH 5.00) and 111,287nA/M(pH 7.00) with excellent linearities of $R^2{\geqq}0.9997$. When one ampoule of Tagma Inj.$^{(R)}$ was analyzed by standard addition method by SWV, the within-day precision study (n=4) on the day of sample preparation resulted in the contents of cimetidine as $203{\pm}3.8\;mg$ (102% of the specified contents, RSD of 1.9%) and the inter-day precision (n=4) through 5 days was reasonable as 1.3% of RSD.

• Transactions of the Korean hydrogen and new energy society
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• v.19 no.1
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• pp.18-25
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• 2008

The membrane electrode assembly(MEA) was prepared by a nonequilibrium impregnation- reduction (I-R) method. Nafion 117 and covalently cross-linked sulfonated polyetherether with tungsto- phosphoric acid (CL-SPEEK/TPA30) prepared by our laboratory, were chosen as polymer electrolyte membrane(PEM). $Pt(NH_3)_4Cl_2$, $RuCl_3$ and reducing agent $(NaBH_4)$ were used as electrocatalytic materials. Electrochemical activity surface area(ESA) and specific surface area(SSA) of Pt cathodic electrode with Nafion 117 were $22.48m^2/g$ and $23.50m^2/g$ respectively under the condition of 0.8 M $NaBH_4$. But Pt electrode prepared by CL-SPEEK/TPA30 membrane exhibited higher ESA $23.46m^2/g$ than that of Nafion 117. In case of Pt-Ru anodic electrode, the higher concentration of Ru was, the lower potential of oxygen reduction and region of hydrogen desorption was, and Pt-Ru electrode using 10 mM $RuCl_3$ showed best properties of SSA $34.09m^2/g$ with Nafion 117. In water electrolysis performance, the cell voltage of Pt/PEM/Pt-Ru MEA with Nafion 117 showed cell property of 1.75 V at $1A/cm^2$ and $80{\circ}C$. On the same condition, the cell voltage with CL-SPEEK/TPA30 was the best of 1.73 V at $1A/cm^2$.

• Korean Chemical Engineering Research
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• v.52 no.2
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• pp.247-255
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• 2014

$La_{0.8}Sr_{0.2}CuO_3$ powder with the perovskite structure was prepared as electrode catalyst using citrate method. Porous electrode was made with as-prepared catalyst, carbon as supporter and polytetrafluoroethylene (PTFE) as hydrophobic binder. As results of potentiostatic electrolysis with potential of -1.5~-2.5 V vs. Ag/AgCl in 0.1, 0.5 and 1.0 M KOH at 5 and $10^{\circ}C$ on the porous electrode, liquid products were methanol, ethanol, 2-propanol and 1, 2-butanol regardless reaction temperature, while gas products were methane, ethane and ethylene at $5^{\circ}C$, and methane, ethane and propane at $10^{\circ}C$ respectively. Optimal potentials for $CO_2$ reduction in the view of over all faradic efficiency were high values (-2.0 and -2.2 V) for gas products whereas low potential (-1.5 V) for liquid products regardless of concentration and temperature.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.13 no.3
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• pp.229-233
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• 2015

Developing novel anode materials to replace the Pt anode currently used in electrolytic reduction is an important issue on pyroprocessing. In this study, the electrochemical behavior of TiN was investigated as the conductive ceramic anode which evolves O₂ gas during the reaction. The feasibility and stability of the TiN anode was examined during the electrolytic reduction of UO₂. The TiN anode could electrochemically convert UO₂ to metallic U in a LiCl–Li₂O molten salt electrolyte. No oxidation of TiN was observed during the reaction; however, the formation of voids in the bulk section appeared to limit the lifetime of the TiN anode.

• Restorative Dentistry and Endodontics
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• v.18 no.2
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• pp.431-445
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• 1993

The purpose of this study was to observe corrosion characteristics of six dental amalgams and was to analyse corrosion products electrochemically. After each amalgam alloy and Hg was triturated as the direction of the manufacturer by using mechanical amalgamator, the triturated mass was inserted into the cylinderical metal mold ($12{\times}10mm$) and was condensed with 160kg/$cm^2$ by using the hydrolic press. The specimen was removed from the mold and was stored at room temperature for 1 week, and was polished with amalgam polishing kit. The anodic and cathodic polarization curve was obtained by using cyclic voltammetric method with 3-electrode potentiostat in saline for each amalgam and Ag, Sn, Cu plate specimen at $37{\pm}0.5^{\circ}C$. The potential sweep range was -1.7V~0. 4V(vs SCE) in working electrode and scan rate was 50mV/s and the exposed surface area of each specimen to the electrolytic solution was $0.79cm^2$. The results were as follows. 1. In anodic-cathodic polarization curve of amalgam specimens, two anodic current rising areas and two cathodic current peaks were obtained at the low Cu amalgam(CF, CS) specimen and three anodic current rising areas and three cathodic current peaks were obtained at the high Cu amalgam (TY, DS, HV) specimen. 2. As this compared with the anodic and cathodic current peak potentials of Sn, Cu and Ag specimen, the first cathodic current peak I c was caused by the reduction of divalent tin salt, second cathodic current peak IIIc results from the reduction of quadravalent tin salt, and third cathodic current peak me results from the reduction of copper salt. 3. As reverse potential sweeping was done repeatedly, anodic current was decreased slightly in all amalgam specimens.

• Journal of the Korean Chemical Society
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• v.21 no.6
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• pp.404-412
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• 1977

Electrochemical reduction of nitrobenzene (${\phi}NO_2$) and its derivatives on Pb electrode was studied by means of galvanostatic measurements and coulometric electrolysis in ethanol-water solvent. In acidic solutions phenylhydroxyl amine and aniline ethanol-water solvent. In acidic solutions phenylhydroxyl amine and aniline were produced while nitrosobenzene and coupled products such as azo-and hydrazobenzene were produced in basic solutions. Nitrosobenzene (${\phi}NO$) was not found to be an intermediate in the reduction reactions of ${\phi}NO_2$ in acidic solutions. No direct coupling between ${\phi}NO\;and\;{\phi}NHOH$ was observed to occur in the electrolyte solutions used. Mechanisms of the production of phenylhydroxylamine and nitrosobenzene are deduced from Tafel slope, pH dependence and reaction order with respect to nitrobenzene. Mechanism for the reduction of substituted nitrobenzenes seems to be identical to that of nitrobenzene.

• Transactions of the Korean hydrogen and new energy society
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• v.29 no.5
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• pp.450-457
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• 2018

To design the practical core-shell electrocatalysts, combination of core and shell materials is important to meet catalytic activity and durability target. In general, Pd is considered as a good core material due to its best activity caused by strain/ligand effect. Preparing Pd nanoparticles can be a starting point in fabricating core-shell type electrocatalysts, much simplified Pd preparing process is suggested by using carbon monoxide (CO) as a reducing agent and/or capping agent. The solvent composition and reaction temperature can control to nanosheet, tetrahedron, and sphere without using additional stabilizer. Among them, Pd nanosheet which has mainly (111) plane showed about 3 times higher electrocatalytic activity for oxygen reduction reaction (ORR) to the spherical Pd nanoparticles. The enhanced ORR activity of Pd nanosheets can be attributed to the exposure of Pd (111) surface and the high electrochemical surface area. Therefore, we demonstrated that the shape of Pd nanomaterials is easily controlled via a facile reduction method using CO, and (111) plane-oriented Pd nanosheets can be a promising ORR catalysts and core material for polymer electrolyte fuel cells (PEFCs).

• Korean Chemical Engineering Research
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• v.61 no.4
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• pp.604-610
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• 2023

The nitrogen reduction reaction (NRR), which produces NH₃ by reducing N₂ under ambient conditions, is attracting attention as a promising technology that can reduce energy consumption in industrial processes. We investigated the adsorption behaviors at various active sites on the Ni (100) surface, which is widely used among catalytic metal surfaces capable of adsorbing and activating N₂, based on density-functional theory calculations. We also investigated two N₂ adsorption structures, so-called end-on and side-on structures. We find that for the end-on case, N₂ is adsorbed on a top site, and the reaction proceeded in a distal pathway, while for the side-on case, N₂ is adsorbed on a bridge site, and the reaction proceeded with enzymatic pathway. Finally, this study provides insight into the adsorption of metal catalyst surfaces for the NRR reactions based on the calculated Gibbs free energy profiles of the thermodynamically most favorable pathways.

• Journal of Powder Materials
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• v.13 no.5 s.58
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• pp.327-335
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• 2006

In the development of new hydrogen absorbing materials for a next generation of metal hydride electrodes for rechargeable batteries, metastable Mg-Ni-based compounds find currently special attention. Amor phous-nanocrystalline $Mg_{63}Ni_{30}Y_7$ and $Mg_{50}Ni_{30}Y_{20}$ alloys were produced by mechanical alloying and melt-spinning and characterized by means of XRD, TEM and DSC. On basis of mechanically alloyed Mg-Ni-Y powders, complex hydride electrodes were fabricated and their electrochemical behaviour in 6M KOH (pH=14,8) was investigated. The electrodes made from $Mg_{63}Ni_{30}Y_7$ powders, which were prepared under use of a SPEX shaker mill, with a major fraction of nanocrystalline phase reveal a higher electrochemical activity far hydrogen reduction and a higher maximum discharge capacity (247 mAh/g) than the electrodes from alloy powder with predominantly amorphous microstructure (216 mAh/g) obtained when using a Retsch planetary ball mill at low temperatures. Those discharge capacities are higher that those fur nanocrystalline $Mg_2Ni$ electrodes. However, the cyclic stability of those alloy powder electrodes was low. Therefore, fundamental stability studies were performed on $Mg_{63}Ni_{30}Y_7$ and $Mg_{50}Ni_{30}Y_{20}$ ribbon samples in the as-quenched state and after cathodic hydrogen charging by means of anodic and cathodic polarisation measurements. Gradual oxidation and dissolution of nickel governs the anodic behaviour before a passive state is attained. A stabilizing effect of higher fractions of yttrium in the alloy on the passivation was detected. During the cathodic hydrogen charging process the alloys exhibit a change in the surface state chemistry, i.e. an enrichment of nickel-species, causing preferential oxidation and dissolution during subsequent anodization. The effect of chemical pre-treatments in 1% HF and in $10\;mg/l\;YCl_3/1%\;H_2O_2$ solution on the surface degradation processes was investigated. A HF treatment can improve their anodic passivation behavior by inhibiting a preferential nickel oxidation-dissolution at low polarisation, whereas a $YCl_3/H_2O_2$ treatment has the opposite effect. Both pre-treatment methods lead to an enhancement of cathodically induced surface degradation processes.