• Bulletin of the Korean Chemical Society
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• 제31권12호
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• pp.3549-3552
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• 2010

The complex formation between diazocalix[4]dipropyl (1) and diazocalix[4]crown-6 ether (2) with alkali, alkaline earth and transition metal ions was investigated by voltammetry. Electrochemical properties of compounds 1 and 2 and their selectivity toward metal ions were evaluated in $CH_3CN$ solution by comparison of voltammetric behaviors of two phenols in each compound. Compounds 1 and 2 showed almost same voltammetric behavior which is two irreversible oxidation peaks caused by intramolecular hydrogen bonding between two phenols in 1 and 2. While, however, upon interacting with various metal ions, 1 with two propyl ether groups showed no significant changes in voltammetry, 2 with crown ether group caused significant voltammetric changes upon the addition of $Ba^{2+}$ to 2. Their behavior is closely related to the complex formation by entrapment of metal ion into crown ether cavity, and ion-dipole interaction between metal ion and two phenolic groups in calix[4]crown-6.

• 전기화학회지
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• 제11권1호
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• pp.59-63
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• 2008

Poly (vinylchloride) (PVC) membrane electrodes based on neutral carrier, tetracycline was prepared as an active sensor for Hg(II) ion, and tested in different contents of the potassium tetrakis (4-chlorophenyl) borate (KTpClPB) as lipophilic salt. Bis (2-ethylhexyl) sebacate (DOS), bis(l-butylpentyl) adipate (BBPA), 2-nitrophenyl octyl ether (NPOE) and dibutyl phthalate (DBP) were used as diverse plasticizing solvent mediators. This electrode shows excellent potentiometric response characteristics and display good linearity with log $[Hg^{+2}]$ versus EMF response, over a range of concentrations between $10^{-7}$ and $10^{-3}M$. With 30.8mV/decade Nernstian slope, the detection limit was $6.9{\times}10^{-9}M$ and the response time was less than 20s. The proposed electrode yields very good selectivity for mercury (II) ion over many cations such as alkali, alkaline earth, transition and heavy metal ions. And it shows a very stable potential values in a wide pH range. This reliable electrode prepared was kept at least a month without considerable alteration in their response to Hg (II) ion.

• Bulletin of the Korean Chemical Society
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• 제29권5호
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• pp.969-973
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• 2008

Solvent extraction using a Schiff-base, salen$(NEt_2)_2$, as a chelating agent has been conducted on several water samples to study the determination of trace Cu(II), Mn(II) and Zn(II). Experimental conditions for the formation and extraction of metal complexes were optimized with an aqueous solution similar in composition to the samples. The matrix difference between the sample and standard solutions was approximately matched, and the pH of each sample solution was adjusted to 9.5 with $NaHCO_3/NaOH$ buffer. The concentration of salen$(NEt_2)_2$ was $7.3\;{\times}\;10^{-3}$ mol/L, and the complexes were extracted into MIBK solvent followed by the measurement of AAS absorbance. The potential interference of concomitant ions was investigated, but no interference from alkaline and alkali earth ions was shown in this procedure. The given procedure is precise, as judged from the relative standard deviation of less than 5% for five measured data. The recovery of 93-103% shows that this method is quantitative for such trace metal analysis.

• Bulletin of the Korean Chemical Society
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• 제25권10호
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• pp.1465-1470
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• 2004

A short and efficient synthesis, solvent extraction and potentiometric measurements of new thiazole-containing naphtho-crown ethers are reported. The naphthalene moiety enhances the ammonium ion selectivity over potassium ion. The selectivity of ${NH_4}^+/K^+$ follows the trend $3\;{\approx}\;2\;>\;1$, indicating that the differences in conformational changes of 2 and 3 in forming ammonium complexes affect little on the resulting ammonium/potassium extraction selectivity ratio. The ammonium ion-selective electrodes were prepared with noctylphenyl ether plasticized poly(vinyl chloride) membranes containing 1-4 the effect of one naphthalene unit introduced on either right (2) or left (3) side of thiazolo-crown ether on their potentiometric properties (e.g., ammonium ion selectivity over other cations, response slopes, and detection limits) were not apparent. However, the ammonium ion selectivity of 1, 2 and 3 over other alkali metal and alkaline earth metal cations is 10-100 times higher than that of nonactin.

• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3592-3596
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• 2011

A novel poly(vinylchloride)-based membrane sensor using $N^1$,$N^3$,$N^5$-tris(2-(2,3-dihydroxybenzylamino)-ethyl)cyclohexane-1,3,5-tricarboxamide (CYCOENCAT, L) as ionophore has been prepared and explored as $Fe^{3+}$ selective electrode. The membrane electrode composed of ionophore, poly(vinylchloride) and o-nitropheyloctyl ether in the optimum ratio 4:33:63 gave excellent potentiometric response characteristics, and displayed a linear log[$Fe^{3+}$] versus EMF response over a wide concentration range of $1.0{\times}10^{-5}-1.0{\times}10^{-1}$ M with super nernstian slope of 28.0 mV/decade and the detection limit of $8.0{\times}10^{-6}$ M. The proposed ion selective electrode showed fast response time (< 15 s), wide pH range (3.0-7.0), high non-aqueous tolerance (up to 20%) and adequate long life time (120 days). It also exhibited very good selectivity for $Fe^{3+}$ relative to a wide variety of alkali, alkaline earth, transition and heavy metal ions. Further, the analytical applicability of the sensor was tested as an indicator electrode in the potentiometric titration of $Fe^{3+}$ with EDTA.

• Bulletin of the Korean Chemical Society
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• 제28권1호
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• pp.68-72
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• 2007

A new PVC membrane potentiometric sensor that is highly selective to Hg2+ ions was prepared, using bis(2-hydroxybenzophenone) butane-2,3-dihydrazone (HBBD) as an excellent hexadendates neutral carrier. The sensor works satisfactorily in the concentration range of 1.0 × 10-6 to 1.0 × 10-1 mol L-1 (detection limit 4 × 10-7 mol L-1) with a Nernstian slope of 29.7 mV per decade. This electrode showed a fast response time (~8 s) and was used for at least 12 weeks without any divergence. The sensor exhibits good Hg2+ selectivity for a broad range of common alkali, alkaline earth, transition and heavy metal ions (lithium, sodium, potassium, magnesium, calcium, copper, nickel, cobalt, zinc, cadmium, lead and lanthanum). The electrode response is pH independent in the range of 1.5-4.0. Furthermore, the developed sensor was successfully used as an indicator electrode in the potentiometric titration of mercury ions with potassium iodide and the direct determination of mercury in some binary and ternary mixtures.

• Bulletin of the Korean Chemical Society
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• 제26권6호
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• pp.882-886
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• 2005

Copper(II) ion-selective PVC membrane electrode based on 2-mercaptobenzoxazole as a new ionophore and o-nitrophenyl octyl ether (o-NPOE) as plasticizer is proposed. This electrode revealed good selectivity for $Cu^{2+}$ over a wide variety of other metal ions. Effects of experimental parameters such as membrane composition, nature and amount of plasticizer, and concentration of internal solution on the potential response of $Cu^{2+}$ sensor were investigated. The electrode exhibits good response for $Cu^{2+}$ in a wide linear range of 5.0 ${\times}$ 10−.6-1.6 ${\times}$ $10^{-2}$ mol/L with a slope of 29.2 ${\pm}$ 2.0 mV/decade. The response time of the sensor is less than 10 s, and the detection limit is 2.0 ${\times}$ $10^{-6}$ mol/L. The electrode response was stable in pH range of 4-6. The lifetime of the electrode was about 2 months. The electrode revealed comparatively good selectivities with respect to many alkali, alkaline earth, and transition metal ions.

• Bulletin of the Korean Chemical Society
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• 제24권11호
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• pp.1585-1589
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• 2003

A PVC-based membrane electrode for thallium(I) ions based on 1,21,23,25-tetramethyl-2,20: 3,19-dimetheno-[H, 2] H, 23H, 25H-bis-[1,3] dioxocino[5,4-i:5',4'-i] benzo [1,2-d: 5.4-d'] bis [1,3] benzodioxocin(II) has been prepared. The electrode displays a linear dynamic range of $1.0{\times}10^{-1}-1.0{\times}10^{-5}$ M, with a Nernstian slope of $59.8{\pm}0.2\;mV\;{decad^-1}$, and a detection limit $5.0{\times}10^{-6}$ M. It has a very fast response time of<10 s and can be used for at least ten weeks without a considerable divergence in potentials. This electrode revealed comparatively good selectivity with respect to alkali, alkaline earth, and some transition and heavy metal ions and was effective in a pH range of 2.0-10.0. It was used as an indicator electrode in potentiometric titration of thallium ion with sulfide ion.

• 대한화학회지
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• 제39권7호
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• pp.524-529
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• 1995

pH 1에서 15-crown-5(SGBM)을 결합시킨 silica gel를 고정상으로 하는 액체 크로마토그래피을 이용하여 혼합 금속이온 용액으로부터 금속이온들의 분리효율을 결정하였다. 여러가지 SGBM-금속이온들간의 결합상수 및 분리인자들을 측정한 결과 그 순위는 Li(Ⅰ) < Sr(Ⅱ) < Na(Ⅰ) < Cu(Ⅱ) < Mg(Ⅱ) < K(Ⅰ) < Ca(Ⅱ) < Bi(Ⅲ) < Sb(Ⅲ)로 나타났다. 이러한 사실은 금속이온의 크기 효과 및 전자 밀도 효과에 의해서 결정됨을 알 수 있었으며, 또한 알칼리, 알칼리 토금속이온 및 $Cu^{2+}$이 혼합된 용액에서 $Sb^{3+}$의 분리효율이 다른 이온들에 비해서 훨씬 좋게 나타남을 알았다.

• 분석과학
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• 제5권1호
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• pp.33-39
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• 1992

리튬이온의 새로운 중성운반체로서 tetrahydrofuran 단위의 16고리형 crown-4를 퓨란과 아세톤으로부터 산 촉매하에서 합성하여 수소화시킨 후 리튬-이온과의 착물형성반응을 Li-7 NMR과 전기전도도법으로 조사했다. 합성한 리간드를 PVC-액체막 전극에 사용하여 분리용액법에 의한 리튬이온의 선택성을 결정하였다. 막용매, tris(2-ethylhexyl) phosphate에서 리튬이온의 선택계수는 알칼리금속이온 및 알칼리토금속이온에 대해 $2.4{\times}10^{-1}$에서 $2.3{\times}10^{-4}$ 범위의 값을 가졌으며, 산성용액(pH=2 이하, 0.1M LiCl)에서 액체막은 $H^+$ 이온의 방해로 불안정하였다.