• Bulletin of the Korean Chemical Society
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• 제33권3호
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• pp.790-794
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• 2012

Trace metal ions such as $Cd^{2+}$, $Ni^{2+}$, and $Zn^{2+}$ in a highly saline sample were subjected to on-line complexation with 4-(2-thiazolylazo) resorcinol (TAR) dissolved in a background electrolyte (BGE) under transient isotachophoresis (TITP) conditions. A long plug of the saline sample, containing the trace metal ions but devoid of TAR, was injected into a coated capillary filled with a BGE composed of 150 mM 2-(cyclohexylamino) ethanesulfonic acid (CHES) and 110 mM triethylamine (TEA) at pH 9.7. Since the electrophoretic mobility of TAR fell between the mobilities of the anionic leading electrolyte ($Cl^-$ in the sample) and the anionic terminating background electrolyte ($CHES^-$), a highly concentrated zone of TAR from the BGE was formed at the rear of the sample matrix and then the metal cations toward the cathode were swept by isotachophoretically assisted on-line complexation (IAOC) between the metal ions and the isotachophoretically stacked TAR. As a result, anionic metal-TAR complexes were formed efficiently, which satisfy the TITP conditions between $Cl^-$ and $CHES^-$. The enrichment factors of metal ions including $Cd^{2+}$ were up to 780-fold compared to a conventional CZE mode using absorbance detection. The detection limits were 17 nM, 15 nM, and 27 nM for $Ni^{2+}$, $Zn^{2+}$, and $Cd^{2+}$ in a 250 mM NaCl matrix, respectively. Our method was successfully applied to the analysis of urine samples without desalting.

• 분석과학
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• 제17권1호
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• pp.82-84
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• 2004

The quantitative trace analysis of ions could be deteriorated by filter papers because of the effect of adsorption. Generally the adsorption of anions on filter paper did not occurred. Instead, $Cl^-$ and $NO{_3}^-$ ions were extracted from the filter papers. However, most metal ions were adsorbed on the filter papers by the formation of hydroxide in neutral solution. The adsorption of metal ions except $Ag^+$ ion could be avoided depend on the acid concentrations.

• Bulletin of the Korean Chemical Society
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• 제27권10호
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• pp.1557-1561
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• 2006

The use of chemically modified silica-salen$(NEt_2)_2$ was studied for the separation and concentration of the metal ions from an aqueous solution by a solid phase extraction. After the salen(NEt2)2 was synthesized, it was chemically bonded to silica gel by a diazonium coupling reaction. The adsorption capacities and binding constants were obtained with respect to Cu(II), Mn(II), Pb(II) and Zn(II) by a graphical method. Some experimental conditions were optimized for the determination of the trace elements. After the silica-salen(NEt2)2 was pulverized in a sample solution of which the pH was adjusted, the solution was stirred to pre-concentrate the metal ions. The metal ions adsorbed were desorbed with nitric acid solution. And the concentrated analytes were determined by a flame AAS. The method proposed here was so rarely influenced by a sample matrix that the procedure was applied to 3 types of water samples. The reproducible results of less than 10% RSD were obtained at the concentration level of ca. 100 ng/mL and the recoveries of 95-109% were obtained in the spiked samples in which given amounts of analytes were added.

• Bulletin of the Korean Chemical Society
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• 제23권8호
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• pp.1067-1072
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• 2002

A new polystyrene-divinylbenzene resin containing 2-(2-thiazolylazo)-5-dimethylamino-phenol (TAM) functional groups has been synthesized and its sorption behavior for nineteen metal ions, including Zr(Ⅳ),Hf(Ⅳ) and U(Ⅵ) has been investigated by batch and column methods. The chelating resin showed high sorption affinity for Zr(Ⅳ) at pH 1-5 and U(Ⅵ) at pH 4. Some parameters affecting the sorption of the metal ions have been detailed. The breakthrough and overall capacities were measured under optimized conditions. The overall capacities of Zr(Ⅳ), Th(Ⅳ) and U(Ⅵ), which showed higher than the other metal ions, were 0.90,0.84 and 0.80 mmol/g, respectively. The elution order of metal ions at pH 4 was evaluated as Zr(Ⅳ) > Th(Ⅳ) > U(Ⅵ) > Cu(Ⅱ) > Hf(Ⅳ) > W(Ⅵ) > Mo(Ⅵ) > In(Ⅲ) > Sn(Ⅳ) > Cr(Ⅲ) > V(Ⅴ) > Fe(Ⅲ). Quantitative recovery of most metal ions except Zr(Ⅳ) was achieved using 2M HNO3. Desorption and recovery of Zr(Ⅳ) was successfully performed with 2 M HClO4 and 2 M HCl.

• Bulletin of the Korean Chemical Society
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• 제31권1호
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• pp.140-145
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• 2010

The simultaneous detection of Cd (II), Pb (II), Cu (II), and Hg (II) ions in aqueous medium using a BDD electrode with DPASV is described. XPS was used to characterize the chemical states of trace metal ions deposited on the BDD electrode surface. Experimental parameters that affect response, such as pH, deposition time, deposition potential, and pulse amplitude were carefully optimized. The detection limits for Cd (II), Pb (II), Cu (II), and Hg (II) ions were 3.5 ppb, 2.0 ppb, 0.1 ppb and 0.7 ppb, respectively. The application of the BDD electrode on the electrochemical pretreatment for the simultaneous metal detection in the dye waste water was also investigated.

• 대한화학회지
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• 제32권3호
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• pp.211-226
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• 1988

역상 액체 크로마토그래피에 의하여 몇 가지 금속-dithiocarbamate(DTC) 킬레이트의 용리거동을 Novapak $C_{18}$과 {\mu}$-Bondapak $C_{18}$ 분리관을 사용하여 연구하고, 아울러 동시 분리정량에 미치는 pH, 진탕시간, 흐름속도, 추출용매 종류 및 이동상의 세기등 여러가지 인자들의 영향을 조사 검토하였다. 미량 금속-DTC 킬레이트들은 Novapak $C_{18}$ 분리관에서 acetonitrile/methanol/water 또는 acetonitrile/water의 용리액을 사용하여 성공적으로 분리되었다. 모든 금속-DTC 킬레이트의 용매세기 인자는 $0{\leqq}log\;k'{\leqq}1$ 의 범위임을 확인하였고, 회수율을 97.0-106.7 %, coefficient of variation은 0.98-3.41%이었다. 최적 분석 조건에서 합성 시료중에 있는 혼합 금속 이온들은 상대 오차 ${\pm}$6.7 % 이내에서 동시 분리정량이 가능하였다.

• 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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• 제16권5호
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• pp.422-427
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• 1995

In a stream of water sample, trace metal ions are quantitatively coprecipitated with Indium hydroxide and filtered. The filtered precipitate is continuously dissolved in 3 M nitric acid and introduced to ICP directly. The lead, cadmium, and copper are concentrated more than 10-fold and determined with ICP-AES at a sampling frequency of 10/hour. The detection limits are 2.89, 1.43,0.52 ppb for lead, cadmium, and copper respectively. Recoveries of lead, cadmium, and copper are 98.7, 94.3, and 104.5% respectively. The RSD values for three elements are about 3-5% currently.

• 분석과학
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• 제11권3호
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• pp.174-178
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• 1998

Formaldehyde와 resorcinol을 반응시켜 chelating 수지를 제조하였다. 이 수지는 Pb(II)나 Ni(II)와 같은 전이금속에 대해 높은 흡착능을 나타내었다. Pb(II), Ni(II), Co(II), Fe(II)와 Zn(II)의 흡착과 탈착율을 batch법으로 구하였다. 이 수지의 중요한 특성은 금속 이온과 수지의 수소 이온간의 교환과정이다. 금속이온의 흡착과 탈착의 메카니즘은 수지의 작용기인 수소 이온의 탈착과 금속 이온간의 교환반응으로 생각된다. 이 수지를 이용하여 전이금속을 농축시키고, 다른 이온들로부터 Pb(II)를 분리하는데 적용해 보았다.

• 한국광물학회지
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• 제11권1호
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• pp.20-31
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• 1998

Adsorption of metal elements onto illite and halloysite was investigated at $25^{\circ}C$ using pollutant water collected from the gold-bearing metal mine. Incipient solution of pH 3.19 was reacted with clay minerals as a function of time: 10 minute, 30 minute, 1 hour, 12 hour, 24 hour, 1 day, 2 day, 1 week, and 2 week. Twenty-seven cations and six anions from solutions were analyzed by AAs (atomic absorption spectrometer), ICP(induced-coupled plasma), and IC (ion chromatography). Speciation and saturation index of solutions were calculated by WATEQ4F and MINTEQA2 codes, indicating that most of metal ions exist as free ions and that there is little difference in chemical species and relative abundances between initial solution and reacted solutions. The adsorption results showed that the adsorption extent of elements varies depending on mineral types and reaction time. As for illite, adsorption after 1 hour-reaction occurs in the order of As>Pb>Ge>Li>Co, Pb, Cr, Ba>Cs for trace elements and Fe>K>Na>Mn>Al>Ca>Si for major elements, respectively. As for halloysite, adsorption after 1 hour-reaction occurs in the order of Cu>Pb>Li>Ge>Cr>Zn>As>Ba>Ti>Cd>Co for trace elements and Fe>K>Mn>Ca>Al>Na>Si for major elements, respectively. After 2 week-reaction, the adsorption occurs in the order of Cu>As>Zn>Li>Ge>Co>Ti>Ba>Ni>Pb>Cr>Cd>Se for trace elements and Fe>K>Mn>Al, Mg>Ca>Na, Si for major elements, respectively. No significant adsorption as well as selectivity was found for anions. Although halloysite has a 1:1 layer structure, its capacity of adsorption is greater than that of illite with 2:1 structure, probably due to its peculiar mineralogical characteristics. According to FTIR (Fourier transform infrared spectroscopy) results, there was no shift in the OH-stretching bond for illite, but the ν1 bond at 3695 cm-1 for halloysite was found to be stronger. In the viewpoint of adsorption, illite is characterized by an inner-sphere complex, whereas halloysite by an outer-sphere complex, respectively. Initial ion activity and dissociation constant of metal elements are regarded as the main factors that control the adsorption behaviors in a natural system containing multicomponents at the acidic condition.