• Journal of the Korean Chemical Society
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• v.40 no.12
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• pp.724-732
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• 1996

The organic precipitate flotation using Cu(II)-pyrrolidinedithiocarbamate complex as a coprecipitant was studied for the preconcentration and determination of trace Cd, Pb, Bi and Co in several water samples. Experimental conditions such as pH of solution, amounts of Cu(II) and ammonium pyrrolidinedithiocarbamate(APDC), stirring time, the type and amount of surfactant, etc. were optimized for the effective flotation of analytes. After 3.0 mL of 1,000 ${\mu}g/mL$ Cu(II) solution was added to 1.00 L water sample, the pH of the solution was adjusted to 2.5 with HNO3 solution. Trace amounts of analytes were coprecipitated by adding 2.0% APDC solution. And the precipitates were flotated onto the surface of solution with the aid of nitrogen gas and sodium lauryl sulfate. The floats were collected from mother liquor, and filtered through the micropore glass filter by suction. The precipitates were dissolved with 4 mL conc. HNO3, and then diluted to 25.00 mL with deionized water. The analytes were determined by graphite furnace atomic absorption spectrophotometry. This flotation technique was applied to the analysis of some water samples, and the 90 to 120% of recoveries were obtained from the spiked samples, this procedure could be concluded to be simple and applicable for the trace element analysis in various kinds of water.

• Analytical Science and Technology
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• v.13 no.2
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• pp.173-178
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• 2000

A new open-chain ligand containing two phenol groups, 1, 14-Bis (2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane(bsated) was synthesized as its tetrahydrochloride salt and characterized by elemental analysis, mass, infrared and NMR. Its proton dissociation constants ($logK^n{_H}$) and stability constants ($logK_{ML}$) toward $Co^{2+}$, $Ni^{2+}$, $Cu^{2+}$ and $Zn^{2+}$ were determined at $25^{\circ}C$ and 0.10M($KNO_3$) ionic strength in aqueous solution by potentiometry. The X-ray structure of its copper (II) complex [Cu(bsated)]$(ClO_4)_2$ was reported: Monoclinic space group $P2_1/n$, $a=17.856(4){\AA}$, $b=17.709(1){\AA}$, $c=8.539(2){\AA}$, $V=2700(2){\AA}$ with Z=4. Electrochemical studies of [Cu(bsated)]$(ClO_4)_2$ complex in dimethyl sulfoxide (DMSO) solution containing tetrabutylammonium perchlorate (supporting electrolyte) were carried out by cyclic voltammograms (CV) and normal pulse voltammetry (NPV).

• Journal of the Korean Chemical Society
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• v.50 no.1
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• pp.23-31
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• 2006

carbon modified methods were used for the preconcentration and determination of copper in some real samples using the flame atomic absorption spectrometry. The copper ions was adsorbed quantitatively on the activated carbon due to their complexation with 4- amino-2, 3-dimethyl-1-phenyl-3-pyrazoline (ADMPP) or 4-(4- methoxybenzylidenimin) thiophenole (MBITP). The adsorbed copper on solid phase was eluted quantitatively using small amount of nitric acid. The influence of important parameters including pH, amount of carrier, flow rate, amount of activated carbon and type and concentration of eluting agent for obtaining maximum recovery were investigated. The methods based on ADMPP and MBITP at optimum conditions is linear over concentration range of 0.05-1.5 g mL-1 and 0.05-1.2 g mL-1 of copper with correlation coefficient of 0.9997 and 0.9994 and both detection limit of 1.4 ng mL-1, respectively. The preconcentration leads to enrichment factor of 310 and break through volume of 1550 mL for both ligands. The method has a good tolerance limit of interfering ion and a selectivity that has been successfully applied for the determination of copper content in real sample such as tap, spring, river and waste water.

• Journal of Korean Society of Environmental Engineers
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• v.30 no.3
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• pp.345-351
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• 2008

Fe-impregnated activated carbon(Fe-AC) was prepared by Fe(III) loading on activated carbon(AC) in various preparation pH. In order to evaluate the stability of Fe-AC, dissolution of iron from Fe-AC in acidic conditions was measured. In addition, batch experiments were conducted to monitor the removal efficiency of copper by Fe-AC. Results of stability test for Fe-AC showed that the amount of extracted iron increased with contact time but decreased with increasing solution pH. The dissolved amount of iron gradually increased at solution pH 2 and finally 13% of the total iron loaded on activated carbon was extracted after 12 hr. However dissolution of iron was negligible over solution pH 3. Removal of Cu(II) by Fe-AC was greatly affected by solution pH and was decreased as solution pH increased as well as initial Cu(II) concentration decreased. Surface complexation modeling was performed by considering inner-sphere complexation reaction and using the diffuse layer model with MINTEQA2 program.

• Journal of Environmental Science International
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• v.16 no.10
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• pp.1111-1118
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• 2007

A bismuth-coated carbon fiber microelectrode was prepared using cyclic voltammetry (CV). An analytical application was performed for the copper analysis with Square Wave Stripping Voltammetry (SWSV). Gallic acid n-propyl ester (PG) was used for the complex formation with a copper ion, and electrochemical measurements were performed with a pre-amplifier of a low-current module for nano am per detection. The effects of various parameters on the response were optimized. Analytical working ranges of $0.03-25.9\;{\mu}gl^{-1}$ and $0-25\'mgl^{-1}$ Cu(II) were obtained. The relative standard deviation at $13\;mgl^{-1}$ Cu was 0.9% (n = 12) in optimum conditions. The detection limit was found to have been $0.019\;{\mu}gl^{-1}$, with a 30-sec accumulation time. The developed methods were applied to a copper assay in water samples.

• Journal of the Korean Chemical Society
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• v.36 no.6
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• pp.796-801
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• 1992

An empirical Lewis basicity, DN, for eight mixed methanol solvents has been measured by the solvatochromic behavior of the [Cu(tmen)(acac)]$CIO_4$. The change of DN in mixed methanol solvents is not correlated with composition of the mixtures and divided into three groups: (1) dipolar aprotic solvents contribute mainly to the solvation of solute (MeOH-DMSO, MeOH-PY, MeOH-DMF), (2) two components of mixture contribute equally to the solvation of solute (MeOH-MeCN, MeOH-dioxane, MeOH-AC) and (3) methanol contributes entirely to the solvation of solute (MeOH-DCE, MeOH-TCE). The relationship between DN and Kamlet-Taft's $B_{KT}$ for mixed methanol solvents was found to agree well. These DN values also were a useful factor to analysis of reactivity for mixed methanol solvents.

• Analytical Science and Technology
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• v.9 no.4
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• pp.336-344
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• 1996

The extraction of trace cobalt, copper, nickel, cadmium, lead and zinc in urine samples of organic and alkali metal matrix into chloroform by the complex with a dithizone was studied for graphite furnace AAS determination. Various experimental conditions such as the pretreatment of urine, the pH of sample solution, and dithizone concentration in a solvent were optimized for the effective extraction, and some essential conditions were also studied for the back-extraction and digestion as well. All organic materials in 100 mL urine were destructed by the digestion with conc. $HNO_3$ 30 mL and 30% $H_2O_2$ 50 mL. Here, $H_2O_2$ was added dropwise with each 5.0 mL, serially. Analytes were extracted into 15.0 mL chloroform of 0.1% dithizone from the digested urine at pH 8.0 by shaking for 90 minutes. The pH was adjusted with a commercial buffer solution. Among analytes, cadmium, lead and zinc were back-extracted to 10.00 mL of 0.2 M $HNO_3$ from the solvent for the determination, and after the organic solvent was evaporated, others were dissolved with $HNO_3-H_2O_2$ and diluted to 10.00 mL with a deionized water. Synthetic digested urines were used to obtain optimum conditions and to plot calibration-eurves. Average recoveries of 77 to 109% for each element were obtained in sample solutions in which given amounts of analytes were added, and detection limits were Cd 0.09, Pb 0.59, Zn 0.18, Co 0.24, Cu 1.3 and Ni 1.7 ng/mL, respectively. It was concluded that this method could be applied for the determination of heavy elements in urine samples without any interferences of organic materials and major alkaline elements.