• Analytical Science and Technology
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• v.13 no.5
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• pp.608-615
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• 2000

A determination method of trace nickel and cobalt in water samples was studied and developed by adsorbing their complexes on ion exchange resin suspension. The analytical ions were formed as complexes with a ligand of APDC (ammonium pyrrolidinedithiocarbamate) and adsorbed on anion exchange resin of Dowex 2-X8. After the suspension was filtered out with membrane filter, the complexes were dissolved in HCl solution by an ultrasonic vibrator for ET-AAS determination. Several conditions were optimized as followings. pH of sample solution: 5.0, amount of ligand APDC: more than 430 times in mole ratio, the type and concentration of acid: 0.1 M HCl, and vibration time: 7 minutes. The addition of palladium in the HCl solution could improve the reproducibility and sensitivity by a matrix modification in the absorbance measurement. This procedure was applied for the analysis of three kinds of real water samples. The detection limits equivalent to 3 times standard deviation of blank were Co 0.36 ng/mL and Ni 0.27 ng/mL and recoveries in spiked samples were 99-102% for cobalt and 100-105% for nickel.

• Analytical Science and Technology
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• v.7 no.1
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• pp.33-39
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• 1994

The purpose on this study was to develop a new improved chromatographic method for determination of trace phenols from environmental waste water. The research was carried out with selected 8 phenols, and solid-phase extraction was employed as sample pretreatment method. The coupling of XAD-4 and Dowex $1{\times}8$ resin as preconcentration column increased the selectivities toward interferences coexisted in matrix. Automation was accomplished with on-line process of pretreatment and HPLC system. After elution of sample through XAD-4 column, phenols were adsorbed by dispersion force, then displaced from it by ACN basified, simultaneously and selectively readsorbed via anion exchange on Dowex $1{\times}8$. Dowex $1{\times}8$ column was washed by water. Phenols readsorbed were removed from Dowex $1{\times}8$ column by a minimum volumn of methanol containing HCl. Each pretreatment step was connected by switching valves and the eluate was directly on-line injected to obtain fast and reliable results into the HPLC. Recovery of phenols was greater than 90%. To examine utility of this method, analysis of phenols from laboratory waste water sample which was added some organic pollutants to find with phenols on environmental waste water were also accomplished without their interference effects.

• 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.

• Bulletin of the Korean Chemical Society
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• v.26 no.10
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• pp.1529-1532
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• 2005

A simple and cost effective method for separation and preconcentration of Ag(I) at the $10^{-7}\;mol\;L^{-1}$ level in the environmental and mineral samples is present. The method is based on the flotation of Ag(I)-iodide complex as an ion-associate with ferroin in pH of 4 from a large volume of an aqueous solution (500 mL) using nheptane. The floated layer was then dissolved in dimethylsulfoxide (DMSO) for the subsequent spectrophotometric determination. Beer's law was obeyed over a range of 2.0 ${\times}$ $10^{-7}$-4.0 ${\times}$ $10^{-6}$ mol $L^{-1}$ with the apparent molar absorptivity of 2.67 ${\times}$ $10^5$ L $mol^{-1}\;cm^{-1}$. The detection limit (n = 5) was 4 ${\times}$ $10^{-8}$ mol $L^{-1}$, and RSD (n = 5) obtained for 2.0 ${\times}$ $10^{-6}$ mol $L^{-1}$ of Ag(I) was 2.2%. The interference effects of a number of elements was studied and found that only $Hg^{2+}$ at low concentration, and $Pb^{2+}$, $Cd^{2+}$, $Cu^{2+}$, and $Fe^{3+}$ ions at moderately high concentrations were interfered. To overcome on these interference effects, the solution was treated with EDTA at a buffering pH of 4 and passed through a column containing Amberlite IR-120 ionexchanger resin, just before the flotation process. The proposed method was applied to determine of Ag(I) in a synthetic waste water, a photographic washing sample and a geological sample and the results was compared with those obtained from the flame atomic absorption spectrometry. The results were satisfactorily comparable with together, so that the applicability of the proposed method was confirmed in encountering with the real samples.

• Journal of the Korean Chemical Society
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• v.41 no.8
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• pp.392-398
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• 1997

A method of selective determination of inorganic and organic mercury compounds has been described. The $CHCl_3$ solution of a high molecular quaternary alkylammonium salt, Aliquat 336 was used for the simultaneous preconcentration of both inorganic, $Hg^{2+}$ as its thiocyanate complex, and organic mercury compounds, $CH_3HgCl$ and $C_2H_3O_2$ $HgC_6H_5$ by extraction from their aqueous solution. Selective separation of the inorganic mercury from the extract was followed by stripping with 3 M $HClO_4 $ solution for the subsequent determination by CVAAS. Organic mercury was also determined by CVAAS after removal of $CHCl_3solvent$ from the extract and decomposition of the residue with 4% $KMnO_4 $-1 MH_2$S0_4$. The mixtures of inorganic and organic mercury compounds contained 1.0 $\mug$ as Hg in 50 mL of sample solution(0.02 ${\mu}gHg/mL$) were analysed within ${\pm}6%$ by absolute errors.

• 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.10 no.4
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• pp.282-290
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• 1997

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-[4-(2-thiazolylazo)orcinol] (TAO) chelating resin were studied by elution method. The effect was examined with respect to overall capacity of each metal ion, separation of mixed metal ions, flow rate and concentration of buffer solution for optimum condition of sorption. The overall capacities of some metal ions on this chelating resin were 0.35nmol U(VI)/g resin, 0.49nmol Th(IV)/g resin, 0.41nmol Cu(II)/g resin, and 0.31nmol Zr(IV)/g resin, respectively. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 5.0 was Th(IV)>Cu(II)>U(VI)>Zr(IV)>Pb(II)>Ni(II)>Zn(II)>Mn(II)>Cd(II). The group separation of mixed metal ions was possible by increasing pH in pH range 2~5 at a flow rate of 0.28mL/min. Characteristics of desorption were investigated with desorption agents such as $HNO_3$, HCl, $HClO_4$, $H_2SO_4$, and $Na_2CO_3$. It was found that 2M $HNO_3$ showed high desorption efficiency to most of metal ions except Zr(IV) ion. Also, desorption and recovery of Zr(IV) ion were successfully performed with 1M $H_2SO_4$. Recovery of trace amount of U(VI) ion from artificial sea water was over 94%. The chelating resin, XAD-16-TAO was successfully applied to group separation of rare earth metal ions from U(VI) by using 2M $HNO_3$ as an eluent.

• Journal of the Korean Chemical Society
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• v.35 no.4
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• pp.355-361
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• 1991

The separative preconcentration of trace mercury[Hg(II)] in a water sample was studied by a coprecipitation flotation technique. The trace Hg(II) was precipitated together with Ce(OH)$_3$ by adding 3.0 ml of 0.1M Ce$^{3+}$ solution to 1,000 ml of water sample and adjusting pH to 11.0 with 1.0M NaOH solution. The hydrophobic precipitate[Ce(OH)$_3$-Hg(OH)$_2$], which was formed by adding 2.0 ml of 0.1${\%}$ ethanolic sodium oleate solution, were floated on the surface with an aid of tiny nitrogen gas bubbles. The floated materials were quatitatively collected in a suction flask and dissolved with 5.0 ml of 2.0M HNO$_3$. The solution was marked to 25.00 ml with a deionized water. The content of Hg(II) was determined by cold vapor atomic absorption spectrophotometry. Any interferences of concomitants such as Ag$^+$, Br$^-$, I$^- $, etc. were not observed on the whole procedure. The analytical result showed that Hg(II) found in the wastewater of Seochang Campus, Korea University was 1.98 ng/ml with the relative standard deviation of 3.6${\%}$. And recoveries of Hg(II) in the wastewater into which 1.0 ng/ml and 2.0 ng/ml were added were 95${\%}$ and 91${\%}$, respectively. From such results, this procedure could be concluded to be tolerably accurate and reproducible for the determination of trace mercury in a water sample.

• Analytical Science and Technology
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• v.21 no.5
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• pp.412-423
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• 2008

A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.