[화학]사과 중 Nuarimol의 잔류성 분석

김일광(Il Kwang Kim),한성수(Seong Soo Han),김윤근(Youn Geun Kim),김해진(Hea Jin Kim) 한국분석과학회 1993 분석과학 Vol.6 No.3

네모파 산화전극벗김 전압전류법을 이용한 생체시료 중의 미량 수은 분석

김일광,박성우,한종현,김윤근,천현자,박경옥,Kim Il Kwang,Park Sung Woo,Han Jong Hyun,Kim Youn Geun,Chun Hyun Ja,Park Kyung Ok 대한화학회 1993 대한화학회지 Vol.37 No.5

생체시료 중의 미량수은정량을 glassy carbon 전극을 사용하는 네모파 산화전극벗김 전압전류법으로 연구하였다. 생체시료는 분석에 들어가기 전에 질산과 황산 그리고 과망간산 칼륨으로 충분히 온침시켰다. 수은의 검출한계는 석출시간, 석출전위, pH, 그리고 저어줌속도 등에 의하여 크게 영향을 받았다. -1.0 volts에서 240초간 400rpm으로 저어주면서 수은을 석출하였을 때 검출한계는 $0.5\;ppb\;(2.5{\times}10^{-9} M)$이하였다. 이 방법은 분석시간이 짧고 감도가 높기 때문에 생체시료 중의 미량수은 분석에 유용하였다. The determination of trace level mercury in bio-materials has been investigated by the square wave anodic stripping voltammetry (ASV)-technique at glassy carbon electrode. Prior to analysis, the bio-materials were digested with HNO3/H2SO4 mixture and KMnO4 was added to complete the oxidation. The detection limit of the mercury varied greatly with deposition time, deposition potential, pH and stirring rate. When deposition is carried out for 240 sec with 400 rpm stirring at -1.0 volts vs. Ag/AgCl, the detection limit was below $0.5\;ppb\;(2.5{\times}10^{-9} M)$. The method is recommended for trace level mercury analysis of biomaterials because this procedure is time saving and has higher sensitivity.

${\alpha},{\beta}$-Dibenzyl N-Benzylidene L-Aspartate 의 Imino 기에 대한 선택적 전해환원반응

김일광,김윤근,이영행,채규윤,Kim, Il-Kwang,Kim, Youn-Geun,Lee, Young-Haeng,Chai, Kyu-Yun 대한화학회 1989 대한화학회지 Vol.33 No.6

0.1M LiCl의 ethanol 용액에서 ${\alpha},{\beta}$-dibenzyl N-benzylidene L-aspartate의 전기화학적 환원을 direct current, differential pulse polarography, cyclic voltammetry 그리고 controlled potential coulometry 방법으로 연구하였다. ${\alpha},{\beta}$-dibenzyl N-benzylidene L-aspartate의 환원과정은 1단계(-0.92 volts vs. Ag-AgCl)에서 양성자 첨가와 2전자이동에 의한 완전 비가역의 CEC 혹은 CE 반응기구로 진행되었으며 ${\alpha},{\beta}$-dibenzyl N-benzyl L-aspartate가 생성되었다. 계면활성제가 포함된 용액에서 polarography 환원파는 전체적으로 약간 억제되었으며 Triton X-100의 농도가 진해질수록 비가역성을 증가시키는 것으로 나타났다. 생성물 분석과 pH 변화에 따른 전극환원과정에 대한 고찰로 전기화학적 반응기구를 제안하였다. The electrochemical reduction of ${\alpha},{\beta}$-dibenzyl N-benzylidene L-aspartate in 0.1M LiCl ethanol solution was investigated by direct current (DC), differential pulse (DP) polarography, cyclic voltammetry and controlled potential coulometry(CPC). The irreversible reductive amination of imino group proceeded to form ${\alpha},{\beta}$-dibenyl N-benzyl L-aspartate by CEC or CE electrochemical reaction mechanism at the first reduction step (-0.92 volts vs. Ag-AgCl). The polarographic reduction wave was slightly suppressed due to inhibitory effect of micelle, while the irreversibility was increased according to the increase of Triton X-100 concentration. Upon the basis of product analysis and polarogram interpretation with pH change, possible CE electrode reaction mechanism was suggested.

3-Phenyl-4-Nitrosydnone의 전기화학적 연구

김일광,김윤근,한순종,Il-Kwang Kim,Youn-Geun Kim,Soon-Jong Han 대한화학회 1988 대한화학회지 Vol.32 No.3

An electrochemical reduction on the 3-phenyl-4-nitrosydnone in acetonitrile solution has been studied by direct current, differential pulse polarography, cyclic voltammetry and controlled potential coulometry. Before the cleavage of phenyl-N single bond a irreversible electron transfer-chemical reaction(EC) mechanism of nitro functional group proceeded to form amino (or-hydroxylamino) group by multielectron transfer which is followed to give phenyl hydrazine by single electron transfer-chemical reaction at the 2nd and 3rd irreversible reduction wave of high negative potential region. The cathodic half-wave potentials shown to be shift negative due to inhibitory effect of cetyl-trimethyl ammonium bromide micelle while reversible anodic peaks on the 2nd and 3rd reduction waves in the presence of NaLS at high negative potential region. Acetonitrile 용액중에서 3-phenyl-4-nitrosydnone의 전기화학전 환원을 direct current, differential pulse polarography, cyclic voltammetry 그리고 controlled potential coulometry 방법으로 연구하였다. Phenyl-N 단일 결합의 분리 이전에 nitro 기능기의 비가역적 전자 전달-화학반응(EC)기구의 진행으로 다전자 이동에 의한 amino(또한 hydroxylamino)기를 형성하고, 높은 음 전위 영역에서 2,3 비가역성 환원파의 일전자전달-화학반응에 의한 phenyl hydrazine을 생성하였다. 음극 반파 전위들은 cetyltrimethyl ammonium bromide의 억제 효과에 의해 음의 값으로 이동하였고 한편, sodium lauryl sulfate micelle은 높은 음전위 영역에서 제 2,3 환원파의 가역성산화 peaks를 보였다.

Acetonitrile 용액중에서 살충제 O, O-Dimethyl-O-(3-Methyl-4-Nitrophenyl)-Phosphorothioate (Fenitrothion)의 전기화학적 환원

김일광,김윤근,천현자,Il-Kwang Kim,Youn-Geun Kim,Hyun-Ja Chun 대한화학회 1988 대한화학회지 Vol.32 No.3

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. The electrochemical reduction of O,O-dimethyl-O-(3-methyl-4-nitrophenyl)-phosphorothioate (Fenitrothion) has been studied in acetonitrile solution containing surfactant micelle by direct current (DC)-differential pulse (DP) polarography, cyclic voltammetry (CV) and controlled potential coulometry (CPC). The partially reversible electron transfer-chemical reaction(EC, EC mechanism) of fenitrothion reduction proceeded by four electron transfer to form O,O-dimethyl-O-(3-methyl-4-hydroxyaminophenyl)-phosphorothioate which undergoes single bond of the phosphorus atom and phenoxy group cleaves to give p-amino-m-cresol and dimethyl thiophosphinic acid as major product by two electron transfer-protonation at higher negative potential. The polarograpic reduction waves shown to suppressed due to inhibitory effect of sodium lauryl sulfate micelle solution and split up on selectivity of anionic micelle effect in two step at the first reduction peak.

3-Phenyl-4-nitrosydnone의 전기화학적 연구

金日光,金潤根 圓光大學校 基礎自然科學硏究所 1986 基礎科學硏究誌 Vol.5 No.2

An electrochemical reduction on the 3-phenyl-4-nitrosydnone in acetonitrile solution has been studied by direct current differential pulse polarography, cyclic voltammetry and controlled potential coulometry. Before the cleavage of phengl-N single bond a reversible electron transferchemical reaction (EC) mechanism of nitro functional group proceeded to form amino (orhydroxylamino) group by multielectron transfer which is followed to give phenyl glycine (or phenyl hydrazine) by single electron transfer-chemical reaction at the 2nd and 3rd irreversible reduction wave of high negative potential region. The cathodic half-wave potentials shown to be negative shift due to inhibition effect of cetyl-trimethyl ammonium bromide micelle while the sodium lauryl sulfate micelle showed reversible anodic peaks on the 2nd, 3rd reduction waves at high negative potential region.

수용액에서 연료용 수소를 얻기 위한 MgFe_2O_4 광반도성 전극의 제조와 특성에 대하여

김일광,이홍,최창진,김윤근,천현자 圓光大學校 基礎自然科學硏究所 1987 基礎科學硏究誌 Vol.6 No.2

In the light of the rarity of p-type semiconducting oxides and the unusual properties of the magnesium-iron-oxygen system, it is worthwhile to examine the solied state and photoelectrochemical properties of these materials more closely. This work presented an investigation of the preparation and characterization of magnesium-substituted ironoxid ceramics. Sintered discs of magnesium substituted ironoxides were prepared by conventional powder state mixing techniques. X-ray diffraction and scanning electron microscopy experiments showed that these materials are multiphase, containing both MgFe_2O_4 corundum phase and a spinel phase. More important, photoelectrochemical experiments using the ceramic discs as photoelectrodes showed both cathodic photocurrents and anodic photocurrents under illumination. Photochemical and electrochemcal techniques have been used to show that the inhomogeneities of these materials in the near surface region may be related to the photoelectrochemical properties of the magnesium substituted ironoxide bi-type photoelectrodes.

3-Phenyl-4-Nitrosydone의 전기화학적 연구

金日光,金潤根,韓順鍾 圓光大學校 基礎自然科學硏究所 1989 基礎科學硏究誌 Vol.8 No.3

Aretonitrile 용액중에서 3-phenyl-4-nitrosydnone의 전기화학적 환원을 direct current,differential Pulse polarography, cyclic voltammetry 그리고 controlled potential coulometry 방법으로연구하였다. Phenyl-N 단일 결합의 분리 이전에 nitro 기능기의 비가역적 전자전달-화학반응(EC)기구의 진행으로 다전자 이동에 의한 amino(또는 hydroxylamino)기를 형성하고, 높은 음전위 영역에서 제 2,3 비가역성 환원파의 일전자전달-화학반응에 의한 phenyl hydrazine을 생성하였다. 음극 반파 전위들은 cetyltrimethyl ammonium bromide의 억제효과에 의해 음의 값으로 이동하였고한편, sodium lauryl sulfate micelle은 높은 음전위 영역에서 제 2,3 환원파의 가역성산화 peaks를보였다. An electrochemical reduction on the 3-phenyl-4-nitrosydnone in acetonitrile solu-tion has been studied by direct current, differential pulse polarography, cyclic voltammetry andcontrolled potential coulometry. Before the cleavage of phenyl-N single bond a irreversible elect-ron transfer-chemical reaction(EC) mechanism of nitro fuctional group proceeded to form amino(or-hydroxylamino) group by multielectron transfer whick is followed to give phenyl hydrazineby single electron transfer-chemica1 reaction at the 2nd and 3rd irreversible reduction wave of highnegative potential region. The cathodic half-wave potentials shown to be shift negative due toinhibitory effect of cetyl-trimethyl ammonium bromide micelle whi1e reversible anodic peaks onthe 2nd and 3rd reduction waves in the presence of NaLS at high negative potential region.

Acetonitrile 용액중에서 살충제 O, O-Dimethyl-O-(3-Methyl-4-Nitrophenyl)-Phosphorothioate (Fenitrothion)의 전기화학적 환원

金日光,金潤根,千賢子 圓光大學校 基礎自然科學硏究所 1989 基礎科學硏究誌 Vol.8 No.3

계민활성 micelle을 형성하는 acetonitrile 용액에서 O,O-dimethyl-O-(3-methyl-4-nitrophenyl)-phosphorothioat(Fenitrothion)의 전기화학적 환원을 direct current 및 differential pulasepolarography, cyclic voltammetry 그리고 controlled potential coulometry 방법으로 연구하였다. Fenitrothion의 환원 과정은 1단계로 4 전자 이동에 의한 부분 가역적 전자이동 화학반응 (EC, EC)기구로 O,O-dimethyl-O-(3-metbyl-4-hydroxyaminophenyl)-Phosphorothioate를 형성하고, 더 높은 음전위에서 2 전자 이동에 따른 양성자 반응으로 phosphorus 원자와 phenoxy group의 단일 결합이끊어지면서 주생성물인 P-amino-m-cresol과 dimethyl thiophosphinic acid를 생성하였다. Sodiumlauryl sulfate micelle 용액에서 polarography 환원파는 전체적으로 억제 되었으며 특히 1차 환원파는 음이온 micelle의 선택적 작용으로 2단계로 분리되었다. The electrochemical reduction of O,O-dimethyl-O-(3-methyl-4-nitropheny1)-phos-phorothioate(Fenitrothion) has been studied in acetonitrile solution containing surfactant micelleby direct current (DC)-differential pulse (DP) polarography, cyclic voltammetry (CV) and controlled potential coulometry (CPC). The partially reversible clectron transfer-chemical reaction(EC,EC mechanism) of fenitrothion reduction proceeded by four electron transfer to form O.0-dimethyl-O-(3-methyl-4-hydroxyaminophenyl)-phosphorothioate which undergoes sing1e bond of the phosphorus atom and phenoxy group cleaves to give p-amino-m-cresol and dimethyl thiophosphinic acid as major product by two electron transfer-protonation at higher negative potential. The polarograpic reduction waves shown to suppressed due to inhibitory effect of sodium lauryl sulfate micelle solution and split up on selectivity of anionic micelle effect in two step at the first reduction peak.

Chromium(Ⅲ)의 전기화학적 환원에 관한 연구

김일광,김윤근,김세봉 圓光大學校 基礎自然科學硏究所 1987 基礎科學硏究誌 Vol.6 No.1

The electrochemical reduction of chromium(Ⅲ)in 1×10exp(-1)M sodium perchlorate and 1×10exp(-2)M sulfuric acid aqueous solution has been examined by polarography and cyclic voltammetry. The cyclovoltammetric results showed quasirreversible electrode processes that reduction of chromium(Ⅲ) proceeds by two electron transfer at first reduction step and second reduction step of one electron transfer followed to form chromium metallic state although the direct current polarogram shown to be a three electron transfer process in one reduction step. The height of reduction wave was suppresed and strongly shifted to the more negative potential in cationic surfactant(CTABr), nonionic surfactant triton x-100 and EDTA effects. In anionic surfactant NaLS solution, the height was increased while the half-wave potential shifted to the height negative potential.