• 제목/요약/키워드: Polarography

검색결과 93건 처리시간 0.029초

물아닌 용매속에서의 요오드의 전기화학적 환원 (Electrochemical Reduction of Iodine in Non-aqueous Solvents)

  • 박두원;최원형
    • 대한화학회지
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    • 제19권2호
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    • pp.104-115
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    • 1975
  • 요오드의 전기화학적 환원과정을 여러가지 특성을 가진 물아닌 용매 속에서 polarography, chronopotentiometry, cyclic voltammetry, controlled potential coulometry 등의 전기분석적 방법을 이용하여 적하수은전극, 백금, 금 및 백금아말감전극등을 사용하여 상세히 조사하였다. 메탄올, 에탄올, 이소프로판올 및 피리딘과 같은 양쪽성 용매 속에서는 $I_2{\longrightarrow}I^-$의 I단계 환원과정을 거치며 아세톤, 디메틸포름아미드, 메틸에틸케톤, 디메틸술폭시드, 아세토니릴과 같은 반양성자 용매속에서는 $I_2{\longrightarrow}I_3^-{\longrightarrow}I^-$의 2단계 환원과정을 거쳤다. 적하수은전극, 고인 수은전극, 백금, 금 그리고 백금아말감전극등 전극조건을 다르게 하였을 때에도 $^'I_2$의 환원과정은 같았으며 사용한 모든 전극에서 확산지배적이었다. 반양성자용매에 물을 첨가하여 그 영향을 걸토한 결과 물의 첨가량이 약 $50v/v{\%}$ 이상일때 2단계의 환원과정이 1단계의 환원과정으로 줄어들었다. 또 chronopotentiometric data와 Send의 식으로부터 계산한 각 용매 속에서의 요오드의 확산계수는 $D_{I2}^{AN}=5.96{\times}10^{-6}cm^2/sec,\;D_{13-}^{AN}=9.63{\times}10^{-6}cm^2/sec,\;D_{I2}^{MeOH}=5.30{\times}10^{-6}cm^2/sec$이였다. 전기화학적 환원과정의 stoichiometry를 알아 보고저 controlled potential coulometry로 使用하였으며, 얻은 생성물은 은법적정으로 확인 및 정량하였다.

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1-Benzyl-4-Iodomethyl-2-Azetidinone의 합성과 Iodo기에 대한 전기화학적 환원반응 (Synthesis of 1-Benzyl-4-Iodomethyl-2-Azetidinone and Electrochemical Reduction on the Iodo Group)

  • 김일광;이영행;이채호;채규윤;김윤근
    • 대한화학회지
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    • 제35권1호
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    • pp.70-77
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    • 1991
  • 1-Benzyl-4-iodomethyl-2-azetidinone(BIMA)을 합성하여 iodomethyl기에 대한 전기화학적 환원을 direct current, differential pulse polarography, cyclic voltammetry 그리고 controlled potential coulometry 방법으로 연구하였다. BIMA의 환원과정은 1단계(-1.35 volts vs. Ag-AgCl)에서 완전비가역과 2전자이동후에 양성자가 첨가되는 EEC 반응기구로 진행되었으며 1-benzyl-4-methyl-2-azetidinone이 생성되었다. 양이온 계면활성제(cetyltrimethylammonium bromide)의 농도가 진하여질수록 양전위 이동이 있었으나 음이온 계면활성제(sodium lauryl sulfate)의 경우에는 2단계로 세분화되는 현상이 나타났다. pH변화에 따른 전극환원과정과 생성물 분석의 결과를 바탕으로 전기화학적 반응기구를 제안하였다.

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Host-Guest Interactions Between Macrocycles and Methylsubstituted Anilinium Ions

  • Lee, Shim-Sung;Jung, Jong-Hwa;Chang, Duk-Jin;Lee, Bu-Yong;Kim, Si-Joong
    • Bulletin of the Korean Chemical Society
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    • 제11권6호
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    • pp.521-527
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    • 1990
  • The binding characteristics and analytical applications of anilinium ion complexes with 18-crown-6 were studied by polarography and NMR. First, the electrochemical reduction of the 10 species of mono and dimethylsubstituted anilinium ion complexes with 18-crown-6 as host in methanol are examined. The addition of 18-crown-6 to anilinium guest solution the polarographic waves remain well defined but shifted toward more negative potentials, indicating the complex formation. The values of formation constants, log Κ for 10 species of methylsubstituted anilinium ion complexes with 18-crown-6 varies from 2.7 to 4.8 in methanol at $25^{\circ}C$. The stability order of complexes for 18-crown-6 is anilinilum > 4-methyl > 3,4-dimethyl > 3-methyl > 3,5-dimethyl > 2,4-dimethyl > 2,5-dimethyl > 2,3-dimethyl > 2-methyl > 2,6-dimethylanilinium ion. The steric hindrance shows significant effect. Second, Proton NMR was used to elucidate their interaction characteristics. From the results of so called NMR titration techniques, the behaviors of binding sites on complexation, and the stoichiometry and stability order of complex were obtained. And the later results show the satisfactory agreement with the quantitative values obtained by polarography. Finally, the individual determinations of anilinium ion mixtures were also accomplished by addition of 18-crown-6. In some mixtures of methyl or dimethylanilinium ions the reduction peaks of differential pulse method appeared into one unresolved wave attributed to the small difference of half-wave potential, ${\Delta}E_{1/2}$. In the presence of 18-crown-6, the polarographic waves were resolved into individual maxima because of the shift toward more negative direction by the difference of selectivity of anilinium ions with 18-crown-6. It may be concluded that quantitative analysis of methylanilinium ion mixture make possible because the half-wave potential shift by the selectivity difference due to the steric hindrance between methyl group and 18-crown-6 on complexation.

Azo계 유기화합물의 폴라로그래프법적 거동 (제3보). 아세토니트릴중에서 Benzeneazoresorcinol의 환원 (Polarographic Behavior of Azo Series Organic Compounds (III). Reduction of Benzeneazoresorcinol in Acetonitrile)

  • 이흥락;배준웅
    • 대한화학회지
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    • 제28권2호
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    • pp.130-134
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    • 1984
  • 반양성자성 용매인 아세토니트릴 중에서 benzeneazoresorcinol (BAR)의 폴라로그래프법적 거동을 직류 폴라로그래프법과 정전위전기량법으로 조사하였다. $1.0{\times} 10^{-2}$몰농도의 과염소산 테트라에틸암모늄의 아세토니트릴 용액 중에서 BAR은 1전자 4단계의 환원과정을 거쳐 아민 화합물로 환원되었다. 각 환원파는 비교적 확산 지배적이었고, 가역성은 나쁜 편이었다

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Study on Electrochemical Properties of TBT(Tributyltin)

  • Park, Chil-Nam;Yang, Hyo-Kyung
    • Environmental Sciences Bulletin of The Korean Environmental Sciences Society
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    • 제10권S_4호
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    • pp.173-179
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    • 2001
  • The chemical behavior and properties of the redox state of environmental pollutants was investigated using electrochemical methods. The purpose was to measure the variations in the redox reaction of differential pulse polarograms and cyclic voltammograms. The results observed the influences on redox potential and current of various factors including concentration, temperature, salt, and pH. These were established factors as the effect of the redox reaction. It can be clearly recognized that the electrode reaction are from reversible to irreversible processes. Also, it was mixing with reaction current controlled.

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Polarography에 依한 Nitrosophenylhydroxylamine에 關한 硏究 (Polarographic Study of Nitrosophenylhydroxylamine)

  • 황정의;정종재;손무용
    • 대한화학회지
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    • 제13권4호
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    • pp.303-307
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    • 1969
  • 酸性溶液中에서 重金屬 이온의 沈澱劑로 널리 使用되는 Nitrosophenyhydroxylamine(Cupferron)의 非可逆電極反應의 電流電壓曲線과 酸性 및 알카리性에서의 還元反應機構 및 反應速度 그리고 pH變化에 따른 관여전자수, 活性化 energy를 Delahay 方法을 利用하여 구하였다.

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희토류금속 착물의 합성과 전기화학적 거동 (제 2 보) (Synthesis and Electrochemical Behavior of Rare Earths Metal Complexes)

  • 최칠남;정오진;윤석진;김준태
    • 대한화학회지
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    • 제34권3호
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    • pp.280-287
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    • 1990
  • 란탄나이드 3가 [Sm(Ⅲ), Tb(Ⅲ), and Yb(Ⅲ)]와 유기리간드들의 착물을 비수용매 속에서 전기화학적인 DC 및 DP 폴라로그래피 그리고 CV방법으로 조사하였다. 란탄나이드 3가 착물들은 Ag/AgCl 전극에서 이들 환원 peak는$ E_{pc}$ = -0.16 V, -0.35 V, -0.14 V와 그리고 -0.03 V의 비가역적인 일전자환원 과정이었고, 무거운 란탄나이드의 거동은 원자번호가 증가함에 따라서 안정도상수는 Sm > Tb > Ho > Yb순서로 감소하였다

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EDTA 및 NTA 支指電解質중 Thallium (I) 의 Polarography 에 關한 硏究 (Study on the Polarographic Behaviors of Tl(I) in EDTA and NTA as Supporting Electrolytes)

  • 김황암;김영태
    • 대한화학회지
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    • 제6권1호
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    • pp.61-63
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    • 1962
  • The polarographic behaviors of Tl(I) was investigated in EDTA and NTA as supporting electrolytes for determination of Tl(I). A base solution containing 0.005 % gelatine, 0.1 M EDTA, and 0.05 M NTA was used. The halfwave potential of Tl(I) determined is -0.495 V v.s. S.C.E. in 0.1 M EDTA at pH 4.1 and -0.520V v.s. S.C.E. in 0.05 M NTA at pH 6.3. In this paper, the effects of gelatine concentration and pH values was investigated. The half-wave potentials of common elements was determined and compared with the half-wave potential of Tl(I).

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Polarography에 依한 Titanium Oxalato 및 Oxalatous Complex에 關한 硏究 (Polarographic Study of Titanium Oxalato and Oxalatous Complex)

  • 김황암;한동진
    • 대한화학회지
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    • 제9권2호
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    • pp.71-74
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    • 1965
  • Reduction of Ti(Ⅳ)-oxalate complex on dropping mercury electrode has been studied as a function of oxalate concentration and of pH varied with HCl. Assuming there are equilibrium $TiO(C_2O_4)_2= \;+\;2H^+\;=\;Ti^{+4}\;+\;2C_2O_4\;=\;+\;H_2O,\;K_4$ in addition to $TiO(C_2O_4)_2\;^=\;=\;TiO^{++}\;+\;2C_2O_4=\;K_2\;Ti(C_2O_4)_2\;^-\;=\;Ti^{+3}\;+\;2C_2O_4=\;K_3$ in the system cathodic wave has been well explained for that pH is higher than 0.5. The equilibrium constants $K_2,\;K_3$ and $K_4$ have been to be $2{\times}10^{-12},\;5{\times}10^{-13}$ and $10^{-11}$, respectively. The reduction of Ti(Ⅳ)-oxalate system is $Ti^{+4}\;+\;e\;{\to}\;Ti^{+3}$ in the concentration of hydrochloric acid, higher than 3M.

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Chemical Properties of Co(II) Compound Containing Endocrine Disrupter, Bis-Phenol A

  • Park, Chil-Nam
    • 한국환경과학회지
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    • 제11권2호
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    • pp.131-137
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    • 2002
  • The chemical behavior and properties on the redox state of environmental pollutant has been investigated by electrochemical methods. We carried out to measure the variations in the redox reaction of differential pulse polarogram and cyclic voltammogram. The results observed the influences on redox potential and current of various factors with temperature and pH. These were established factors as the effect of the redox reaction. It can be clearly recognized that the electrode reaction are from qusi-reversible to irreversible processes. Also, it was mixing with reaction current controlled. The bits-phenol A in the waste water was made to compound with cobalt ion and it take away from the separation into compound. The $Co(BPA)_2$ compound was not found to be dissociation in waste water. However, this compound is avery unstable(K=1.02) and for a while, it was to be a dissociation. Therefore, we believed that it was likely to a toxic substance.