• Bulletin of the Korean Chemical Society
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• v.24 no.2
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• pp.173-177
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• 2003

The present work is focused on the preconcentration of nickel and its determination by means of diffuse reflection spectroscopy. The preconcentration of nickel was carried out by sorption on macroporous aminocarboxylic amphoteric resin ANKB-35. Based on this collector, a method to determine nickel in wastes of heat power industry was worked out using solid-phase spectroscopy. The colored surface compound to be determined was obtained by a preceding nickel sorption on the resin and by subsequent treatment of the concentrate obtained with definite amounts of 1-(2-pyridilazo)-2-naphtol (PAN). The Ni calibration curve is linear in the concentration range of 0.5-20.0 mg/L (sample volume is 200.0 mL) and the detection limit is 0.05 mg/L. The presence of $Cu^{2+},\;Fe^{3+},\;Co^{2+}$ ions as well as macrocomponents of natural water $(Na^+,\;K^+,\;Ca^{2+},\;Mg^{2+})$ do not hinder the solid-phase spectroscopy determination of nickel. The nickel determination by diffuse reflection spectroscopy was carried out in model solutions as well as in solutions obtained after the dissolution of wastes of heat power industry.

• Bulletin of the Korean Chemical Society
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• v.29 no.10
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• pp.1932-1936
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• 2008

A new analytical method using 1-(2-pyridylazo)-2-naphthol modified $SiO_2$ nanoparticles as solid-phase extractant has been developed for the preconcentration of trace amounts of mercury(II) in different water samples. Conditions of the analysis such as preconcentration time, effect of pH, sample volumes, shaking time, elution conditions and effects of interfering ions for the recovery of analyte were investigated. The adsorption capacity of nanometer $SiO_2$-PAN was found to be 260 ${\mu}molg^{-1}$ at optimum pH and the detection limit (3$\sigma$) was 0.48 ${\mu}gL^{-1}$. The extractant showed rapid kinetic sorption. The adsorption equilibrium of mercury(II) on nanometer $SiO_2$-PAN was achieved just in 5 mins. Adsorbed mercury(II) was easily eluted with 5 mL of 6 M hydrochloric acid. The maximum preconcentration factor was 50. The method was applied for the determination of trace amounts of mercury(II) in various water samples and industrial effluents.

• Advances in environmental research
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• v.2 no.4
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• pp.309-321
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• 2013

High AA new high capacity sorbent for preconcentration and determination of nickel in environmental samples was synthesized. The sorbent was synthesized by copolymerization of allyl glaycidyl ether / imminodiacetic acid with N,N-dimethylacrylamide as functional monomers in the presence of N,N-bismethylenacryl amid as cross linker and characterized by Fourier transform infra red spectroscopy, elemental analysis, thermogravimetric analysis and scanning electron microscopy. A recovery of 93.6% was obtained for the metal ion with 0.1 M, sulfuric acid as the eluting agent. The sorption capacity of the functionalized sorbent was 55.9 $mgg^{-1}$. The equilibrium sorption data of Ni(II) on polymeric sorbent were analyzed using Langmuir, Freundlich, Temkin and Redlich.Peterson models. Based on equilibrium adsorption data the Langmuir, Freundlich and Temkin constants were determined 0.87 (L mg-1), 25.87 ($mgg^{-1}$) $(Lmg^{-1})^{1/n}$ and 171.4 ($Jmol^{-1}$) respectively at pH 4.5 and $20^{\circ}C$.

• Journal of the Korean Chemical Society
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• v.52 no.2
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• pp.155-163
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• 2008

.A simple and reproducible method for the rapid extraction and determination of trace amounts of copper(II) ions using mesoporous organo-silicas mesoporous silica and atomic absorption spectrometry is presented. Common coexisting ions did not interfere with the separation and determination. The preconcentration factor was 100 (1 ml elution volume) for a 100 ml sample volume. The limit of detection of the proposed method is 1.0 ng ml-1. The maximum sorption capacity of sorbent under optimum conditions has been found to be 5mg of copper per gram of sorbent. The relative standard deviation under optimum conditions was 2.8% (n=10). Accuracy and application of the method was estimated by using test samples of natural and synthetic water spiked with different amounts of copper(II) ion.

• 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.

• Journal of the Korean Chemical Society
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• v.43 no.6
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• pp.651-655
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• 1999

Xylenol Orange was bonded on an anion-exchange resin (Amberlite lRA 400, in $Cl^-$form) by batch equilibration. The resin was proved to be stable in acidic solutions of about 0.1 M HCl, $HNO_3$ or $H_2SO_4$. Sorption capacities for the metal ions on the Amberlite IRA 400 bonded with xylenol orange have been measured by batch method. The result showed that Fe(III) is higher than any other metals for sorption capacity. The preconcentration and the separation of Fe(lll) from the mixture soIution, therefore, were carried out with the 0.1 M sulfosalicylic acid as an eluent.

• Analytical Science and Technology
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• v.9 no.3
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• pp.279-291
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• 1996

The new chelating resins, XAD-2, 4, 16-TAC and XAD-2, 4, 16-TAO were synthesized by Amberlite XAD-2, XAD-4, and XAD-16 macroreticular resins with 2-(2-thiazolylazo)-p-cresol(TAC) and 4-(2-thiazolylazo)orcinol(TAO) as functional groups and were characterized by elemental analysis and FT-IR spectrometry. It was found that the content of functional group in chelating resin was 0.60mmol/g in XAD-16-TAC and 0.68mmol/g in XAD-16-TAO respectively. The chelating resins were stable in acidic and alkaline solution and can be reused over 10 times. The sorption behavior of some metalions to two chelating resins was investigated by batch method, which included batch equilibrium, effect of pH, coexisting ions and masking agent. For the optimum condition of sorption, the time required for equilibrium was about 1 hour and optimum pH was 5. In the presence of anions such as ${SO_4}^{2-}$ and $CH_3COO^-$, the sorption of U(VI) ion was slightly reduced but other anions such as $Cl^-$ and $NO{_3}^-$ revealed no interference effect. Also, sorption capacity of U(VI) ion was decreased by addition of $CO{_3}^{2-}$ ion because of complex formation of $[UO_2(CO_3)_3]^{4-}$, but alkali metals and alkali earth metals including Na(I), K(I), Mg(II), and Ca(II) were not affected for the sorption extent. Masking agent, NTA showed better separation efficiency of U(VI) ion from coexisting metal ions such as Th(IV), Zr(IV), Hf(IV), Cu(II), Cd(II), Pb(II), Ni(II), Zn(II) and Mn(II) than EDTA, CDTA.

• Journal of the Korean Chemical Society
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• v.48 no.6
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• pp.590-598
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• 2004

The preconcentration and determination of trace Cu(II) and Pb(II) on calcium alginate beads in aqueous solution were studied. A calcium alginate beads were prepared by adding an alginic acid to sample solution contained Ca(II). Some following conditions were optimized: the pH of sample solution, amount of alginic acid, and stirring time for effective adsorption; the type and concentration of acid, and sonication time in an ultrasonic vibrator for the perfect de-sorption. A sample solution was prepared with Cu(II) and Pb(II) in DI water. And Ca(II) and ethanol was added into the sample solution. The pH of the final sample solution was controlled with buffer solution. The alginic acid were dispersed in the sample solution by a magnetic stirrer. This mixture was stored in room temperature for 30 min to form a calcium alginate. After the beads were filtered and washed on a membrane filter, the analytes were redissolved from the beads by an ultrasonic vibration of 10 minutes in 1.0M $HNO_3$ solution. The effect of diverse ions on the adsorption of analytes were studied. This procedure was applied for the analysis of two real samples. The recoveries in spiked samples were $90.4{\sim}104.3%$ for analytes.

• Analytical Science and Technology
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• v.17 no.3
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• pp.199-210
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• 2004

A new polystyrene-divinylbenzene chelating resin containing 4,5-dihydroxy-naphthalene-2,7-disulfonic acid (chromotropic acid : CTA) as functional group has been synthesized and characterized. The sorption and desorption properties of this chelating resin for Cr(III) ion and Cr(VI) ion including nine metal bloodstain. As a results, FOB test kit could be effectively applied to identification of human blood at chelating resin was stable in acidic and alkaline solution. The Cr(VI) ion is selectively separated from Cr (III) ion at pH 2 and the maximum sorption capacity of Cr(VI) ion is 1.2 mmol/g. In the presence of anions such as $F^-$, $SO{_4}^{2-}$, $CN^-$, $CH_3COO^-$, $NO{_3}^-$, the sorption of Cr(VI) ion was reduced but anions such as $PO{_4}^{3-}$ and $Cl^-$ revealed no interference effect. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 2 was Cr(VI)>Sn(II)>Fe(III)>Cu(II)>Cd(II)${\simeq}Pb(II){\simeq}Cr(III){\simeq}Mn(II){\simeq}Ni(II){\simeq}Al(III)$. Desorption characteristics for Cr(VI) ion was investigated with desorption agents such as $HNO_3$, HCl, and $H_2SO_4$. It was found that the ion showed high desorption efficiency with 3 M HCl. As the result, the chelating resin, XAD-16-CTA was successfully applied to separation and preconcentration of Cr (VI) ion from several metal ions in metal finishing works.

• 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%.