• Bulletin of the Korean Chemical Society
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• v.31 no.7
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• pp.1907-1914
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• 2010

A novel catalytic kinetic method is proposed for the determination of Se(IV), Se(VI) and total inorganic selenium in water based on the catalytic effect of Se(IV) on the reduction of bromate by p-nitrophenylhydrazine at pH 3.0. The generated bromine, $Br_2$ or $Cl_2$ plus $Br_2$ in 0.1 M NaCl (or NaBr) environment efficiently decolorized Calmagite and the reaction was monitored spectrophotometrically at 523 nm as a function of time. In this indicator reaction, bromide acted as an activator for the catalysis of selenium (IV) and a reducing agent for selenium (VI) at pH 3.0, which allowed the determination of total selenium. The fixed time method was adopted for the determination and speciation of inorganic selenium. Under the optimum conditions, the calibration graph are linear in the range 1 - 35 ${\mu}gL^{-1}$ of Se(IV) for the fixed time method at $25^{\circ}C$. The detection limit based on statistical $3S_{blank}$/m-criterion was 0.215 ${\mu}gL^{-1}$ for the fixed time method (7 min). All of the variables that affect the sensitivity at 523 nm were investigated, and the optimum conditions were established. The interference effect of various cations and anions on the Se (IV) determination was also studied. The selectivity of the selenium determination was greatly improved with the use of the strongly cation exchange resin such as Amberlite IR120 plus. The proposed kinetic method was validated statistically and through recovery studies in natural water samples. The RSDs for ten replicate measurements of 5, 15 and 25 ${\mu}gL^{-1}$ of Se(IV) and Se(VI) was changed between 2.1 - 4.85%. Analyses of a certified standard reference material (NIST SRM 1643e) for selenium using the fixed-time method showed that the proposed kinetic method has good accuracy. Se(IV), Se(VI) and total inorganic selenium in environmental water samples have been successfully determined by this method after selective reduction of Se(VI) to Se(IV).

• Bulletin of the Korean Chemical Society
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• v.25 no.10
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• pp.1508-1512
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• 2004

A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry.

• Proceedings of the Korean Society for Applied Microbiology Conference
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• 2002.10a
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• pp.101-101
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• 2002

• Journal of the Korean Chemical Society
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• v.25 no.1
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• pp.54-616
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• 1981

• Bulletin of the Korean Chemical Society
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• v.26 no.6
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• pp.998-1000
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• 2005

• Bulletin of the Korean Chemical Society
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• v.25 no.7
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• pp.1019-1024
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• 2004

The present paper is focused on simultaneous sorption concentration of gold (III) and silver (I) from thiocyanate solutions using high-selective anion exchanger AN-25 and subsequent separation of these ions at various concentrations of thiocarbamide (eluent). As a result, silver (I) ions are completely eluted from AN-25 and gold (III) ions remain in the resin phase and can be determined directly in the solid phase by diffuse reflection spectroscopy. It is proposed to use the sorption-spectroscopic method for Au(III) determination in aqueous solutions. The calibration curve is linear in the concentration range of 1-19 mg/L (sample volume is 10.0 mL) and the detection limit is 0.05 ${\mu}g/mL$. The presence of Cu(II), Co(II), Fe(II) do not hinder this determination. Au(III) was determined in industrial solutions.

• Bulletin of the Korean Chemical Society
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• v.35 no.1
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• pp.204-210
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• 2014

The nitrogen doped porous carbon nanopolyhedrons (N-PCNPs)-multi-walled carbon nanotubes (MWCNTs) hybrid materials were prepared for the first time. Combining the excellent catalytic activities, good electrical conductivities and high surface areas of N-PCNPs and MWCNTs, the simultaneous determination of hydroquinone (HQ), catechol (CC) and resorcinol (RE) with good analytical performance was achieved at the N-PCNPs-MWCNTs modified electrode. The linear response ranges for HQ, CC and RE are 0.2-455 ${\mu}M$, 0.7-440 ${\mu}M$ and 3.0-365 ${\mu}M$, respectively, and the detection limits (S/N = 3) are $0.03{\mu}M$, $0.11{\mu}M$ and $0.38{\mu}M$, respectively. These results are much better than that obtained on some graphene or CNTs-based materials modified electrodes. Furthermore, the developed sensor was successfully applied to simultaneously detect HQ, CC and RE in the local river water samples.

• Bulletin of the Korean Chemical Society
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• v.27 no.6
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• pp.875-880
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• 2006

A new, simple and fast flow injection analysis (FIA) method has been developed for the indirect determination of nitrite. The proposed indirect automatic method is based on the oxidation of nitrite to nitrate using a lead(IV) dioxide oxidant microcolumn where the flow of the sample through the microcolumn reduces the $PbO_2$ solid phase reagent to Pb(II), which is measured by flame atomic absorption spectrometry. The absorbance of Pb(II) are proportional to the concentration of nitrite in the samples. The calibration curve was linear up to 30 mg $L ^{-1}$, with a detection limit of 0.11 mg $L ^{-1}$ for a 400 mL injected sample volume and a sampling rate of about 80 $h ^{-1}$. The results exhibit no interference from the presence of large amounts of ions. The developed procedure was found to be suitable for the determination of nitrite in foodstuffs and wastewaters. A relative standard deviation better than 0.9% was obtained in a repeatability study. The reliability of the method was established by parallel determination against the standard method.

• Bulletin of the Korean Chemical Society
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• v.32 no.5
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• pp.1564-1568
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• 2011

A solvent extraction separation, preconcentration and determination of thorium with a new crown, 2-ethyl-N-benzyl-4,7,10,13,16-pentaoxa-1-azacyclooctadecane (MACE), is described in the study. The amount of thorium in the aqueous phase and organic phase was determined by Inductively Coupled Plasma-Optical Emission Spectroscopy and Ultraviolet-Visible, respectively. Thorium loaded organic phase was quantitatively stripped in a stage by using 1.0 M $HNO_3$. Thorium was effectively extracted with MACE in the pH range of 6-7 to produce a 3:2 complex ratio in the chloroform. A highly sensitive and rapid spectrophotometric method was described for determination of trace amounts of thorium with MACE. The effective molar absorption coefficient at 281 nm is $1.98{\times}10^3\;mol^{-1}cm^{-1}$, and the system complies with Beer's law in the range from 0.464 to 2.32 ${\mu}gm\;L^{-1}$ of thorium. Thorium was also determined in standard and environmental samples.

• Bulletin of the Korean Chemical Society
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• v.24 no.9
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• pp.1324-1328
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• 2003

The simultaneous determination of anions ($SO_4 ^{2-},\;Cl^-,\;and\;NO_3^-$) and cations ($Na^+,\;NH^{4+},\;K^+,\;Mg^{2+},\;and\;Ca^{2+}$) in natural water obtained by Nakdong River waters system in Korea were performed by ion-exclusion/cationexchange chromatography with conductimetric detection. The stationary phase was a polymethacrylate-based weakly acidic cation-exchange resin column in the $H^+$-form and a weak-acid eluent. When using only a 1.4 mM sulfosalicylic acid/6 mM 18-crown-6 ether as an eluent, good resolution of both anions and cations, minimum time required for the separation, and satisfactory detection sensitivity were obtained in a reasonable time. The method was successfully applied to the simultaneous determination of anions and cations in natural waters.