• Journal of the Korean Chemical Society
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• v.37 no.3
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• pp.327-333
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• 1993

A method was developed for the determination of trace elements in seawater by precipitate flotation preconcentration and subsequent flame atomic absorption detection. In order to quantitatively coprecipitate trace ions such as Cd(II), CuI(II), Fe(III), Mn(II), Pb(II) and Pd(II), 2.0 ml of 1.0M cerium(III) solution was added to 1.0l of seawater and the pH was adjusted to 9.5 with 5.0 M sodium hydroxide solution while stirring with a magnetic stirrer. The precipitate was floated with the aid of surfactant solution (1.0 ml of 0.3% sodium oleate) by bubbling nitrogen gas through a porous (No. 4) fritted glass disk. The floats was collected in a small Erlenmeyer flask by suction. The washed precipitate was dissolved in 8.0 M nitric acid and marked with deionized water in the volumetric flask of 10.0 ml. The analyte was determined by measuring the atomic absorbances in 100-fold concentrated solution. Above all analytes in Kangnung (East Sea) and Kanghwado (West Sea) sea waters were found to be under the detection limit of this method. The recoveries of over 92% for all analytes spiked into seawater samples showed that this method was applicable to the analysis of real seawater.

• Analytical Science and Technology
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• v.19 no.4
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• pp.290-300
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• 2006

Disinfection by-products(DBPs), such as volatile trihalomethanes and the nonvolatile organochlorine acids, created by chlorination have been extensively studied. However MX which contributes 20-50% of the mutagenic activity in drinking water began to people's attention since 1990. Its chemical name is 3-chloro-4-dichloromethyl-5-hydroxy-2(5H)-furanone. According to WHO guidelines its concentration should be controlled, but its value has not been set up. Due to analytical difficulties in measuring this compound at such a low concentrations and lack of information on toxicity to human. Because concentration (ng/L) of MX in drinking water is low traditional testing methods are ineffective. Therefore this study compared LLE and SPE and have chosen SPE to improve preconcentration. MX has been identified in chlorinated drinking water samples in several countries but not in korea Therefore this study analyzed concentration of MX in different water sources and in spring water. This study examined the causes of changing MX content. Chlorine dosage, seasons, water temperature and distance from the source was all discoverd to be relavant. MX was analyzed in various treatment to find optimum disinfection methods. The outcome was that the concentration of MX was minimized when using biological activated carbon-O3 and granular activated carbon.

• 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.

• 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.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.242-256
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• 2012

QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.