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Reaction Conditions and Mechanism of Electrolytic Reduction of Nitrobenzene (니트로벤젠의 전해환원 반응 조건과 메카니즘)

  • Chon Jung Kyoon;Paik Woon Kie
    • 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.

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Natural isotopes and trace element analyses in glass samples (판유리 시료에서 동위원소 및 미량원소 분석법)

  • Min, Ji-Sook;Heo, Sangcheol;Kim, Jae-Guin;Kim, Eun-Ho;Kim, Dong-Wook;Chung, Hee-Sun
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.219-226
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    • 2007
  • Glass is frequently encountered as types of materials that are submitted to forensic science laboratories as a result of trace evidence transfers. The repeatability and the reproducibility of trace element analysis were presented. An analysis of variance (ANOVA) was performed on laser ablation inductively coupled plasma spectrometric analyses of the fragments to identify the source. Pairwise comparisons were completed for all samples. In a pairwise comparison, each sample was compared to each other for a possible [n(n-1)/2] (n : numbers of the samples) total comparison to associate/discriminate samples using Tukey's HSD method. The aim of this study was to determine the utility of LA-ICP-MS for multi-element analysis of forensic samples. The 12 glass fragments from two manufacturers were collected and analyzed to identify the source. An analysis of variance (ANOVA) was performed on 31 elements in NIST 612 Trace elements in Glass. Elements were classified into four categories defined by the combination of precision and variation of inter-samples. We selected 11 elements, 209Bi, 90Zr, 121Sb, 178Hf, 59Co, 238U, 208Pb, 140Ce, 118Sn, 49Ti and 137Ba. 6 pairs out of 66 possible pairs were not distinguished when compared by 137Ba (p<0.05). However, all samples were distinguished using both 49Ti and 137Ba (p<0.05). In conclusion, multi-elemental analysis with LA-ICP-MS is a potential tecnique for the discrimination of forensic samples.