• Journal of the Korean Chemical Society
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• v.56 no.2
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• pp.228-235
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• 2012

A $N_2O_2$ Schiff base ligand, N,N'-bis(4-methoxysalicylidene)phenylendiamine (4-$CH_3O$-salphen) was synthesized. Using the 4-$CH_3O$-salphen, the spectrophoto-metric quantitative analysis of Cu(II) ion in aqueous solution was performed. The optimum condition for the quantitative analysis of Cu(II) ion was determined as the following; the concentration of 4-$CH_3O$-salphen is $2.0{\times}10^{-4}\;mol/L$, ratio between solvent DMSO and water is 50/50(v/v), pH is 5.5. After 1 hr water incubation at $55^{\circ}C$ and then the absorbance measurements at 388 nm, a calibration curve (${\varepsilon}=3.6{\times}10^4\;mol^{-1}cm^{-1}$) with a correlation coefficient ($R^2$=0.9963) was obtained in this condition. Using this optimized condition, the quantitative analysis of Cu(II) ion was performed with various samples such as hot spring water, semiconductor factory waste water and treated water from sewage treatment plant. The average value of the measured values agreed well with standard value with a range of 0.6~5.4%. The limit of determination was 31.77 ng/mL ($5.0{\times}10^{-7}\;mol/L$).

• Journal of the Korean Chemical Society
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• v.37 no.8
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• pp.723-729
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• 1993

Cu(II) ion-responsive chemically modifed electrodes (CMEs) were constructed by incorporating 1-(2-pyridylazo)-2-naphthol (PAN) into a conventional carbon-paste mixture of graphite powder and Nujol oil. Cu(II) ion was chemically deposited on the surface of the PAN-chemically modified electrode in the absence of an applied potential by immersion of the electrode in a buffer solution (pH 3.2) containing Cu(II) ion, and then reduced at a constant potential in 0.1 M KNO$_3$. And a well-defined voltammetric peak could be obtained by scanning the potential to the positive direction. The electrode surface could be regenerated with exposure to acid solution and reused for the determination of Cu(II) ion. In 5 deposition / measurement / regeneration cycles, the response could be reproduced with 6.1${\%}$ relative standard deviation. In case of using the differential pulse voltammetry, the calibration curve for Cu(II) was linear over the range of 2.0 ${times}$ 10$^{-7}$ ∼ 1.0 ${times}$ 10$^{-6}$ M. And the detection limit was 6.0 ${times}$ 10$^{-8}$ M. Studies of the effect of diverse ions showed that Co, Ni, Zn, Pb, Mg and Ag ions added 10 times more than Cu(II) ion did not influence on the determination of Cu(II) ion, except EDTA and oxalate ions.

• Journal of the Korean Chemical Society
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• v.53 no.1
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• pp.27-33
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• 2009

A sensitive technique for the determination of trace Cd(II) in various real samples after preconcentration onto microcrystalline p-dichlorobenzene loaded with 2-mercaptobenzothiazole was developed. Several experimental conditions such as the pH of the sample solution, the amount of chelating agent 2-mercaptobenzothiazole, the amount of adsorbent p-dichlorobenzene-2-MBT, and the flow rate of sample solution were optimized. The interfering effects of various concomitant ions were investigated. Cu(II) interfered with more seriously than any other ions. However, the interference by Cu(II) could be overcome sufficiently by adjusting tartrate ion concentration to be 0.01M or by controlling the amount of 2-mercaptobenzothiazole contained in 0.20 g p-dichlorobenzene to be 0.12 g. The dynamic range, the correlation coefficient ($R^2$) and the detection limit obtained by this proposed technique were $0.5{\sim}30$ ng $mL^{-1}$, 0.9962, and 0.39 ng $mL^{-1}$, respectively. Thus, good results were obtained by the use of p-dichlorobenze as adsorbent matrix. For validating this proposed technique, the aqueous samples(wastewater, stream water, and reservoir water) and the plastic sample were used. Recovery yields of $93{\sim}104$ % were obtained. By F test, these measured data were not different from ICP-MS data at 95 % confidence level. Based on the results from the experiment, it was found that this proposed technique could be applied to the preconcentration and determination of Cd(II) in various real samples.

• Analytical Science and Technology
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• v.23 no.3
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• pp.240-246
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• 2010

A technique for the determination of trace Cu(II) in various real samples by FAAS after the column preconcentration onto p-dichlorobenzene-SA adsorbent, which is microcrystalline p-dichlorobenzene loaded with salicylaldoxime (SA) has been developed. Several experimental conditions such as pH of the sample solution, the amount of chelating agent salicylaldoxime, the amount of adsorbent p-dichlorobenzene-SA, and flow rate of sample solution were optimized. The interfering effects of various concomitant ions were investigated. $CN^-$ interfered more seriously than any other ions. However, the interference by $1\;{\mu}g\;mL^{-1}\;CN^-$ could be overcome completely by controlling the concentration of Ni(II) to $20\;{\mu}g\;mL^{-1}$. The linear range, correlation coefficient ($R^2$) and detection limit obtained by this technique were $3.0\sim100\;ng\;mL^{-1}$, 0.9901, and $3.1\;ng\;mL^{-1}$, respectively. For validating this technique, the aqueous samples (wastewater, reservoir water and stream water) and the food samples (orange juice, fresh egg and skim milk) were used. Recovery yields of 93~104% were obtained. These measured mean values were not differents from ICP-MS data at 95% confidence level. The good results were obtained from the experiments using the rice flour certified reference material (CRM) sample. Based on the experimental results, it was found that this technique could be applied to the preconcentration and determination of Cu(II) for various real samples.

• Journal of the Korean Chemical Society
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• v.43 no.4
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• pp.423-429
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• 1999

A spectrofluorimetric method for the determination of Fe(III) in aqueous solution with 4,5-dihydroxy-1,3-benzenedisulfonic acid(Tiron) as a fluorimetric reporter was developed. Tiron, which is very soluble in water,is a good fluorimetric reagent. However, when Tiron was complexed with Fe(III), the fluorescent intensity was decreased proportionally with the concentration of Fe(III) by a quenching effect. The excitation and fluorescene wavelength of Tiron showing the quenching effect by Fe(III) at pH 4.5 were 312 nm and 341 nm, respectively. The highest sensitivities were shown at Tiron concentration of $1.0{\times}10^{-2}M$. To enhance the quenching effect, the Fe(III)-Tiron complex solution was heated to 80$^{\circ}C$ for 90 minutes. As for Fe(III), the most interfering ion was Cu(II). The interference effects could be mostly eliminated by pH adjustment or by adding EDTA. The concentration ranges showing the linear response to Fe(III) was from $5.0{\times}10^{-7}M\;to\;6.0{\times}10^{-5}M$ With this proposed method, the detection limits of Fe(III) was $2.8{\times}10^{-6}M$. Recovery of Fe(lII) in a synthetic sample was almost quantitative. Based on experimental results, it is proposed that the above technique can be applied to the practical determination of Fe(III).