• Journal of the Korean Chemical Society
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• v.48 no.1
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• pp.46-52
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• 2004

The effect of crystallinity on the structural stability of layered manganese oxide has been systematically investigated. While well-crystalline manganate was prepared by solid-state reaction-ion exchange method, nanocrystalline one was obtained by Chimie-Douce reaction at room temperature. According to micro-Raman and Mn K-edge X-ray absorption spectroscopic results, manganese ions in both the manganese oxides are stabilized in the octahedral sites of the layered lattice consisting of edge-shared MnO6 octahedra. The differential potential plot clarifies that the layered structure of nanocrystalline material is well maintained during electrochemical cycling, in contrast to the well-crystalline homologue. From the micro-Raman results, it was found that delithiation-relithiation process for well-crystalline material gives rise to the structural transition from layered to spinel-type structure. On the basis of the present experimental findings, it can be concluded that nanocrystalline nature plays an important role in enhancing the structural stability of layered manganese oxides.

• Journal of Environmental Health Sciences
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• v.29 no.2
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• pp.62-68
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• 2003

Differential pulse voltammetry (DPV) using nafion-coated glassy carbon electrodes modified with Tetren(tetraethylene pentamine)-glycerol showed sensitivity for determining lead (II) at low concentration. The Lead (II) was accumulated on the electrode surface by the formation of the complex in an open circuit, and the resulting surface was characterized by medium exchange, electrochemical reduction, and differential pulse voltammetry. Various experimental parameters, such as the composition of modifier, preconcentration time, pH of electrolyte (0.1 M acetate buffer), and parameters of differential pulse voltammetry, were optimized. The initial potential was applied for 50 s, the electrode was scanned from -0.9 to -0.3 V, and the anodic peak current was measured at -0.604 V $\pm$ 0.015 V (vs. Ag/AgCl). The calibration plot was obtained in the range 1.0$\times$10$^{-8}$ M~l.0$\times$10$^{-6}$ M with pH 4.5 buffer solution. The detection limit (3$\sigma$) it as low as 5.0$\times$ 10$^{-9}$ M. This method is applied to the determination of lead(II) in a certified reference material and the result agrees satisfactorily with the certified value.

• Archives of Pharmacal Research
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• v.24 no.2
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• pp.100-104
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• 2001

Differential pulse polarographic(DPP) analytical procedure for the rifampicin antibiotic, which can be applied to monitor its synthetic process from the starting antibiotic of rifamycin B or rifamycin SV has been developed based on the electrochemical reduction of an azomethine group. Rifampicin exhibited a cathodic peak due to the azomethine group in the side chain of 3-[(4-methyl-1-piperazinyl)imino]methyl moiety and another cathodic peak due to the carbonyl group in rifamycin SV by DPP. The experimental peak potential shift of an azomethine reduction was -73 mV/pH in the pH range between 3.0 and 7.5, agreeing with involvement of 4 e-and 5 $H^5$ in its reduction. By the cyclic voltammetric(CV) studies, the azomethine and the carbonyl reductions in rifampicin were processed irreversibly on the mercury electrode. The plot of peak currents vs. concentrations of rifampicin ranging $1.0{\times}10^{-7} M~$1.0{\times}10^{-5} M yielded a straight line with a correlation coefficient of 0.9996. The detection limit was $1.0{\times}10^{-8} M with a modulation amplitude of 50 mV DPP has been successfully applied for the determination of rifampicin in the pharmaceutical preparations.