• Analytical Science and Technology
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• v.8 no.4
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• pp.539-543
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• 1995

The on-line SPE-HPLC coupling system was developed for the efficient separation and determination of trace pesticides, such as phenoxyacetic acids and esters, and triazines in aqueous solutions. By using the developed SPE-HPLC on-line system, the band broadening usually observed in single precolumn switching mode was greatly reduced, consequently, the quantitative determination of trace pesticides could be achieved, Besides, since most of the analytes preconcentrated by SPE column could be injected directly into HPLC system, the limit of detection can be improved down to ppt level.

• Nuclear Engineering and Technology
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• v.13 no.4
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• pp.237-244
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• 1981

The preliminary concentration of trace elements in uranium dioxide using an anion exchange resin is presented for neutron activation analysis. The uranyl solution in sulfuric acid is adjusted to the acidity of about pH 2.7 and loaded on a column of the anion exchange resin. An appropriate volume of eluates obtained from the column shows good recoveries of trace elements. By combining this preconcentration with a radiochemical separation scheme, which was developed for the determinations of impurities in aluminum, it is possible to determine 21 trace elements in reactor grade uranium dioxide.

• Carbon letters
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• v.26
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• pp.43-50
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• 2018

In this research, a novel and efficient quinoline thioacetamide functionalized magnetic graphene oxide composite ($GO@Fe_3O_4@QTA$) was synthesized and utilized for dispersive magnetic solid phase preconcentration of Cd(II) and Ni(II) ions in urine and various food samples. A number of diverse methods were employed for characterization of the new nanosorbent. The design of experiments approach and response surface methodology were applied to monitor and find the parameters that affect the extraction performance. After sorption and elution steps, the concentrations of target analytes were measured by employing FAAS. The highest extraction performance was achieved under the following experimental conditions: pH, 5.8; sorption time, 6.0 min; $GO@Fe_3O_4@QTA$ amount, 17 mg; 2.4 mL $1.1mol\;L^{-l}$ $HNO_3$ solution as the eluent and elution time, 13.0 min. The detection limit is 0.02 and $0.2ng\;mL^{-1}$ for Cd(II), and Ni(II) ions, respectively. The accuracy of the new method was investigated by analyzing two certified reference materials (sea food mix, Seronorm LOT NO 2525 urine powder). The interfering study revealed that there are no interferences from commonly occurring ions on the extractability of target ions. Finally, the new method was satisfactorily employed for rapid extraction and determination of target ions in urine and various food samples.

• Analytical Science and Technology
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• v.11 no.3
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• pp.174-178
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• 1998

A chelating resin was prepared by the reaction of formaldehyde and resorcinol. It possesses high adsorption selectivity for transition metal ions such as Pb(II) and Ni(II). The adsorption and desorption yields of Pb(II), Ni(II), Co(II), Fe(II) and Zn(II) were determined using batch method. The significant characteristics of the chelating resin is the exchange processes between its hydrogen and metal ions. The mechanism of metal adsorption and desorption seems to be the competing protonation and complexation reaction of the functional group of the resin. This resin was applied to the rapid concentration of trace amounts of these metal ions and to the separation of Pb(II) from other metal ions in bulk solution.

• Journal of the Korean Chemical Society
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• v.39 no.8
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• pp.635-642
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• 1995

Improved sample introduction system has been investigated for the determination of volatile organic compounds in water using a purge & trap preconcentration apparatus and a capillary gas chromatography/mass spectrometry. The present limitations associated with the moisture control module and cryorefocusing system suggested by EPA were discussed. To solve the problems such as improper separation of peaks due to the adsorption of water and contamination of purge & trap system, a more efficient connection system between the purge & trap apparatus and the gas chromatograph was introduced and the optimum operational conditions were suggested. A carbopack B/carboxen 1000 and 1001 trap was used for the purge & trap procedure and a custom made crosslinked dimethyldiphenylpolysiloxane capillary column was used for the separation of compounds. Accuracy and precision of the method suggested in this report were examined and the method detection limit of each compound was proposed for the simultaneous determination of 54 volatile organic compounds in water.

• Bulletin of the Korean Chemical Society
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• v.26 no.5
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• pp.781-785
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• 2005

A fast and reliable method for the selective separation and preconcentration of $Cu^{2+}$ ions using homogeneous liquid-liquid extraction was developed. A new $\alpha$-dioxime derivative (2H-1,4-benzothioazine-2,3(4H)dionedioxime, Dioxime I) was synthesized and investigated as a suitable selective complexing ligand for $Cu^{2+}$ ions. Zonyl FSA (FSA) was applied as a phase-separator agent under the slightly acidic pH conditions. Under the optimal experimental conditions ([FSA] = 3.2% w/v, [THF] = 19.5% v/v, [Dioxime I] = 1.9 ${\times}\;10^{-3}$ M, and pH = 4.7), 10 ${\mu}g\;of\;Cu^{2+}$ in 5.2 mL aqueous phase could be extracted quantitatively into 80 $\mu$L of the sedimented phase. The maximum concentration factor was 65-fold. The limit of detection of the proposed method was 0.005 ng $mL^{-1}$. The reproducibility of the proposed method, on the 10 replicate measurements, was 1.3%. The influence of the pH, type and volume of the water-miscible organic solvent, concentration of FSA, concentration of the complexing ligand and the effect of different diverse ions on the extraction and determination of $Cu^{2+}$ ions were investigated. The proposed method was applied to the extraction and determination of $Cu^{2+}$ ion in different synthetic and natural water samples.

• Bulletin of the Korean Chemical Society
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• v.25 no.8
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• pp.1133-1136
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• 2004

The need for highly reliable methods for the determination of trace metals is recognized in analytical chemistry and environmental science. A method based on the cloud-point extraction (CPE) technique for the trace analysis of Pb and Cu in water samples is described in this study. The analytes in the initial aqueous solution are complexed with pyrogallol, and 0.1%(w/v) Triton X-114 is added as surfactant. Following phase separation at $50^{\circ}C$, based on the cloud point of the mixture and dilution of the surfactant-rich phase with acidified methanolic solution, the enriched analytes are determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions, the enrichment factors of Pb and Cu were found to be 72 and 85, respectively. Under optimum conditions, the preconcentration of 60 mL of samples in the presence of 0.1%(w/v) Triton X-114 permitted the detection of 0.4 ${\mu}gL^{?1}$ of Pb and 0.05 ${\mu}gL^{?1}$ of Cu. The proposed method was applied successfully to the determination of Pb and Cu in water samples.

• Analytical Science and Technology
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• v.10 no.1
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• pp.31-34
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• 1997

Barium titanyl oxalate which is a precursor of barium titanate has been precipitated at pH 4~5 by a rapid addition of aqueous titanyl oxalate solution to artificial environmental water samples containing equivalent weight of $Ba^{2+}$ ions. Quantitative recoveries of $Cd^{2+}$ and $Pb^{2+}$ from the water samples has been confirmed and found to be usable as a possible method of preconcentration for their determination.

• Analytical Science and Technology
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• v.9 no.4
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• pp.364-372
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• 1996

The sorption and desorption properties of U(VI), Th(IV), Zr(IV), Cu(II), Pb(II), Ni(II), Zn(II), Cd(II) and Mn(II) ions on XAD-16-[2-(2-thiazolylazo)-p-cresol](TAC) chelating resin were studied by elution method for selective separation, concentration and recovery of trace metal ions in sea water. The optimum conditions for the sorption of metal ions were examined with respect to flow rate, pH and concentration of buffer solution. The overall capacities of some metal ions on this chelating resin were 0.41mmol U(VI)/g resin, 0.55mmol Th(IV)/g resin, 0.43mmol Cu(II)/g resin, and 0.32mmol Zr(IV)/g resin, respectively. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 5.0 was found as Th(IV)>Cu(II)>U(VI)>Zr(IV)>Pb(II)>Ni(II)>Zn(II)>Cd(II)>Mn(II). Desorption of characteristics for metal ions were investigated with desorption agents such as $HNO_3$, HCl, $HClO_4$, $H_2SO_4$, and $Na_2CO_3$. It was found that most of metal ions except Zr(IV) showed high desorption efficiency with 2M $HNO_3$. But, desorption and recovery of Zr(IV) ion were successfully performed with 1M $H_2SO_4$. The resin was applied for separation and preconcentration of trace amount of U(VI) ion from artificial sea water and the recovery of U(IV) was over 96%.

• Analytical Science and Technology
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• v.13 no.3
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• pp.323-331
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• 2000

Two chelating resins, XAD-16-TAC and XAD-16-TAO were synthesized by Amberlite XAD-16 macroreticular resin with 2-(2-thiazolylazo)-p-cresol (TAC) and 4-(2-thiazolylazo)-orcinol (TAO) as functional groups. The sorption behaviour of Zr(IV), Th(IV) and U(VI) with two chelating resins were examined with respect to the effect of pH and masking agent by batch methods. It was obtained that the optimum pH was in the range of 5-6, and two chelating resins showed good separation efficiency of Zr(IV) or Th(IV) by using $NH_4F$ as a masking agent. Characteristics of desorption were investigated with 0.1-2 M $HNO_3$ as desorption agent. It was found that 2 M $HNO_3$ showed high desorption efficiency to most of metal ions except Zr(IV). XAD-16-TAC resin is applied to separation and preconcentration of trace Zr(IV) from mixed metal ions. Also, Th(IV) ion can be successfully separated from U(VI) and Zr(IV) ion by using XAD-16- TAO resin.