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4-(2-Thiazolylazo)-resorcinol 을 킬레이트제로 사용한 Ni(Ⅱ)의 鹽析抽出定量
裵俊雄,李興洛,張惠榮,徐戊龍 경북대학교 1987 論文集 Vol.43 No.-
As a part of analytical application of 4-(2-thiazolylazo)-resorcinol(TAR), the extraction method with salting-out technique was applied to the determination of nickel(Ⅱ) ion in aqueous solution. After nickel(Ⅱ) was extracted from the buffered aqueous solution into accetonitrile layer as a Ni(Ⅱ)-TAR chelate by salting-out technique, the visible absorption spectrum was recorded. In this experiment ammonium sulfate was used as a salting-out reagent. The effects of amount of ammonium sulfate and extracting reagent TAR on the extractability, the relationship between pH of the aqueous phase and the extractability of Ni(Ⅱ)-TAR chelate, and the calibration curve for the determination of Ni(Ⅱ) by spectrophotometry has been evaluated. And the effects of diverse ion on the determination of Ni(Ⅱ) by this method have been investigated.
黃正儀,裵俊雄,鄭倧在,鄭在元,張景喜 慶北大學校 物理化學硏究所 1986 硏究論文集 Vol.7 No.-
치환나프톨류(4-Cl-1-Naphthol, 6-Br-2-Naphthol, 8-NH_2-2-Naphthol)의 해리상수를 온도(25∼40℃)와 압력(1∼2000 bar)을 변화시키면서 분광학적 방법으로 측정했다. 이들의 해리상수는 치환기가 들어가므로서 모두 감소했다. 이것은 치환기의 I-효과로서 설명이 가능했으며 또 온도와 압력이 증가하면 해리상수도 증가하였다. 이들 해리상수로부터 반응의 열역학적 성질을 계산하여 반응의 성질을 알아보았다. The dissociation constants of 4-Cl-1-naphthol, 6-Br-2-naphthol, 8-NH_2-2-naphthol in aqueous solution were measured by spectroscopic method in the temperature range from 25 to 40℃ and pressure up to 2000bar. The dissociation constants were decreased as the substituents were inserted in naphthol from 4.4×10 exp(-10) to 5.82×10 exp(-11) as chloride compound and 2.5×10 exp(-10) to 3.44×10 exp(-11) or 4.21×10 exp(-11) as bromine or amino compounds, respectively. This decrease can be explained with the I- or R-effects of substituents. From the dissociation constants various thermodynamic properties were claculated and discussed the characteristics of the dissociation reaction.
아세토니트릴 용매 중에서 Copper-1,5,9,13-Tetrathiacyclohexadecane 착물의 전기화학적 거동과 그 분석적 응용
徐戊龍,李富永,崔明子,裵俊雄,朴泰明 慶尙大學校 기초과학연구소 1992 基礎科學硏究所報 Vol.8 No.-
비수용매인 아세토니트릴 중에서 Cu(Ⅱ)dhk 1,5,9,13-tetrathiacyclohexadecane[16-ane-S_4]의 착물에 대한 전기화학적 거동으로서 직류폴라로그램과 미분펄스폴라로그램으로부터 환원전류의 유형과 가역성을 조사하고, 이들 화합물의 분석적 응용으로서 수용액에 있는 Cu(Ⅱ) 이온을 염석추출법으로 정량하였다. 또한 아세토니트릴 용매 중에서 착물의 안정도상수를 구하고, 분석적 응용으로 수용액 중의 Cu(Ⅱ)를 염석추출법으로 정량하기 위하여 추출 조건 곧 킬레이트와 염석제의 효과, pH 범위를 구하고 또한 Cu(Ⅱ)이온을 정량하는데 있어서의 검량성과 공존이온 효과를 조사하였다. 실험결과로부터 환원 과정은 비가역적이었으며 환원전류는 확산지배적임을 알았다. 또한 아세토닐트릴 용매 중에서 착물의 log K_f 값은 3.51이었으며 Cu(Ⅱ) 이온을 정량하는데 있어서 공존하는 이온의 영향을 별로 받지 않아 선택성이 좋았으며 본 실험방법에 의한 정량한계는 60ppb 이었다. The electrochemical behaviors and analytical application of copper-1,5,9,13-tetrathiacyc-lohexadecane[16-ane-S_4] complex in acetonitrile(AN) solution have been investigated by the use of Dc polarogaphy and differential pulse polarography. Thus the formation constant of copper complex was 10^3.51. Copper (Ⅱ) ion was found to form complex of 1-to-1 composition with [16-ane-S_4]. In addition, reduction step was irreversible and the reduction current was diffusin controlled. And the effect of concentration of the salting-out reagent and chelating agent and pH of aqueous phase on the determination of copper(Ⅱ) was investigated and diverse ion effect was discussed. By salting-out extraction technique, we can be determined until the concentration of cooper (Ⅱ) of 60 ppb.
Electrochemical Behaviors of 4-(2-thiazolylazo)-resorcinol in Acetonitrile
Bae, Zun-Ung,Lee, Heung-Lark,Seo, Moo-Lyung Korean Chemical Society 1989 Bulletin of the Korean Chemical Society Vol.10 No.3
The electrochemical behaviors of 4-(2)-thiazolylazo)-resorcinol (TAR) in acetonitrile solution was studied by DC polarography, cyclic voltammetry, controlled-potential coulometry and UV-Vis spectroscopy. The electrochemical reduction of TAR occurs in four-one electron reduction steps in acetonitrile solution. The products of the first and the third electron transfer are speculated to be a relatively stable anion radical. The second electron transfer to the dianion is followed by a chemical reaction producing a protonated species. The product of the fourth electron transfer also produces the corresponding amine compounds with a following reaction. Also every reduction wave was diffusion controlled. The first reduction wave is considerably reversible and the other waves are less reversible.
Bae, Zun-Ung,Kim, Young-Lark,Chang, Hye-Young 한국분석과학회 1995 분석과학 Vol.8 No.4
The design of appropriate chemically modified electrodes should allow development of new voltammetric measurement schemes with enhanced selectivity and sensitivity. Microorganism like algae has high ability to trap toxic and heavy metal ions and different affinities for metal ions. A copper(II) ion-selective carbon paste electrode was constructed by incorporating alga Anabaena into a conventional carbon paste mixture, and then the film of 10% Nafion was coated to avoid the swelling of the electrode surface. Copper ion could be deposited at the 25% algamodified electrode for 15 min without the applied potential while stirring the solution by only immersing the electrode in a buffer (pH 4.0) cot1taining copper(II). Temperature was controlled at $35^{\circ}C$. After preconcentration was carried out the electrode was transferred to a 0.1 M potassium chloride solution and was reduced at -0.6 volt at $25^{\circ}C$. The differential pulse anodic stripping voltammetry was employed. A well-defined oxidation peak could be obtained at -0.1 volt (vs SCE). In five deposition / measurement / regeneration cycles, the responses were reproducible and relative standard deviations were 3.3% for $8.0{\times}10^{-4}M$ copper(II). Calibration curve for copper was linear over the range from $2.0{\times}10^{-4}M$ to $1.0{\times}10^{-3}M$. The detection limit was $7.5{\times}10^{-5}M$. Studies of the effect of diverse ions showed that the coexisting metal ions had little or no effect for the determination of copper. But anions such as cyanide. oxalate and EDTA seriously interfered.