• Bulletin of the Korean Chemical Society
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• v.32 no.2
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• pp.444-450
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• 2011

A novel method that utilizes poly(5-methyl-2-thiozyl methacrylamide-co-2-acrylamido-2-methyl-1-propanesulfonic acid-co-divinylbenzene) [MTMAAm/AMPS/DVB] as a solid-phase extractant was developed for simultaneous preconcentration of trace Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Ni(II), Pb(II), and Zn(II) prior to the measurement by flame atomic absorpiton spectrometry (FAAS). Experimental conditions for effective adsorption of the metal ions were optimized using column procedures. The optimum pH value for the simultaneously separation of the metal ions on the new adsorbent was 2.5. Effects of concentration and volume of elution solution, sample flow rate, sample volume and interfering ions on the recovery of the analytes were investigated. A high preconcentration factor, 100, and low relative standard deviation values, $\leq$1.5% (n = 10), were obtained. The detection limits (${\mu}gL^{-1}$) based on the 3s criterion were 0.18 for Cd(II), 0.11 for Co(II), 0.07 for Cr(III), 0.12 for Cu(II), 0.18 for Fe(III), 0.67 for Mn(II), 0.13 for Ni(II), 0.06 for Pb(II), and 0.09 for Zn(II). The validation of the procedure was performed by the analysis of two certified reference materials. The presented method was applied to the determination of the analytes in various environmental samples with satisfactory results.

• 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.

• Proceedings of the Korean Environmental Sciences Society Conference
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• 2005.05a
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• pp.327-328
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• 2005

Trace anions in high-sulfate wastewater from mainly derelict mines were determined by ion chromatography with on-line preconcentration and preelution technique. As the sample was preconcentrated and more strongly held ions were preeluted to the principal separation system, this approach was highly effective in removing large concentration of sulfate in high-sulfate wastewater. With this practical on-line preelution treatment, the peaks of fluoride and chloride showed good resolution even when the sulfate concentration was as high as 2000 mg/L and the analyzed total metal concentration was above 500 mg/L.

• Analytical Science and Technology
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• v.17 no.6
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• pp.532-535
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• 2004

A method on the determination of Co(II) after adsorbing of Co(II) on 2-mercaptobenzothiazole-loaded silica gel was studied. The conditions on the separation of Co(II) such as pH of solution, the amount of 2-mercaptobenzothiazole, the flow rate for adsorption, and the desorption solvent were optimized to 9.0, 0.05 g, $10mL\;min^{-1}$ and 1 M $HNO_3$ in ethanol, respectively. Under these optimum conditions, the calibration curve of Co(II) was obtained over concentration range of $2{\sim}120ng\;mL^{-1}$. The detection limit was $0.6ng\;mL^{-1}$. Recovery yields of Co(II) in various natural water samples were more than 90%.

• Bulletin of the Korean Chemical Society
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• v.35 no.1
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• pp.45-50
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• 2014

A fully packed capillary electrochromatographic (CEC) microchip with an on-column micro-solid phase extraction (SPE) bed for the preconcentration and separation of organic analytes was prepared. A linear microchannel with monodisperse colloidal silica packing was formed on a cyclic olefinic copolymer microchip with two reservoirs on both ends. Silver-cemented silica packing frit structure was formed at the entrance of the microchannel by electroless plating treatment as a base layer. A gold coating was formed on it by reducing $Au^{3+}$ to gold with hydroxylamine. Finally micro-SPE bed was formed by self-assembly adsorption of 1-dodecanethiol on it. Micro-SPE beds were about 100-150 ${\mu}m$ long. Approximately $10^3$ fold sensitivity enhancements for Sulforhodamine B, and Fluorescein in nM concentration levels were possible with 80 s preconcentration. Basic extraction characteristics were studied.

• Journal of the Korean Chemical Society
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• v.31 no.1
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• pp.45-54
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• 1987

Dowex 1-X8 resin ion exchanged with calcon carboxylic acid (CCA-Dowex 1-X8) and 2-methyl-8-hydroxyquinoline(MHQ) impregnated-Amberlite XAD-4 resin (MHQ-XAD-4) were examined for the separation and preconcentration of ferric ion from the various matrices. The stabilities of these resins were investigated, and their capacities on ferric ion were also measured. The effect of pH on the adsorption of ferric ion and matrix ions, such as Al(Ⅲ) and Ca(Ⅱ), was investigated to determine the optimun pH ranges. Separation and preconcentration of iron in aluminium foil and mineral water samples were studied by elution method with these resin columns. The recovered ions by 10ml of 2F nitric acid was determined by flame atomic spectrophotometry. SP-Sephadex C-25 column was used to separate ferrous and ferric ion in mineral water by stepwise elution with ferrozine and 1 % ascorbic acid-ferrozine solution. The concentrated and separated each ion could be determined spectrophotometrically at the analytical wavelenth of Fe(Ⅱ)-ferrozine complex (562nm).

• Advances in nano research
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• v.10 no.3
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• pp.295-312
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• 2021

A new ionic liquid functionalized magnetic silica nanoparticle was synthesized and characterized and tested as an adsorbent. The adsorbent was used for magnetic solid phase extraction on ICP-MS method. Simultaneous determination of precious metal Au has been addressed. The method is simple and fast and has been applied to standard water and surface water analysis. A new method for separation/analysis of trace precious metal Au by Magnetron Solid Phase Extraction (MSPE) combined with ICP-MS. The element to be tested is rapidly adsorbed on CoFe2O4@SiO2@[BMIM]PF6 composite nano-adsorbent and eluted with thiourea. The method has a preconcentration factor of 9.5-fold. This method has been successfully applied to the determination of gold in actual water samples. Hydrophobic Ionic Liquids (ILs) 1-butyl-3-methylimidazole hexafluorophosphate ([BMIM]PF6) coated CoFe2O4@SiO2 nanoparticles with core-shell structure to prepare magnetic solid phase extraction agent (CoFe2O4@SiO2@ILs) and establish a new method of MSPE coupled with inductively coupled plasma mass spectrometry for separation/analysis of trace gold. The results showed that trace gold was adsorbed rapidly by CoFe2O4@SiO2@[BMIM]PF6 and eluanted by thiourea. Under the optimal conditions, preconcentration factor of the proposed method was 9.5-fold. The linear range, detection limit, correlation coefficient (R) and relative standard deviation (RSD) were found to be 0.01~1000.00 ng·mL-1, 0.001 ng·mL-1, 0.9990 and 3.4% (n = 11, c = 4.5 ng·mL-1). The CoFe2O4@SiO2 nanoparticles could be used repeatedly for 8 times. This proposed method has been successfully applied to the determination of trace gold in water samples.

• Bulletin of the Korean Chemical Society
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• v.31 no.10
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• pp.2813-2818
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• 2010

A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion ($TBA^+$)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a $100\;{\mu}L$ micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = $1.0{\times}10^{-4}\;M$, [$TBA^+$] = $2.0{\times}10^{-2}\;M$, [$CHCl_3$] = $100.0\;{\mu}L$ and [$ClO_4$] = $2.0{\times}10{-2}\;M$, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results.

• Bulletin of the Korean Chemical Society
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• v.34 no.11
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• pp.3362-3366
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• 2013

A simple and quick separation technique for selenite in natural water was developed using $TiO_2$@$SiO_2/Fe_3O_4$ nanoparticles. For the synthesis of nanoparticles, a polymer-assisted sol-gel method using hydroxypropyl cellulose (HPC) was developed to control particle dispersion in the synthetic procedure. In addition, titanium butoxide (TBT) precursor, instead of the typical titanium tetra isopropoxide, was used for the formation of the $TiO_2$ shell. The synthesized nanoparticles were used to separate selenite ($Se^{4+}$) in the presence of $Se^{6+}$ or selenium anions for the photocatalytic reduction to $Se^0$ atom on the $TiO_2$ shell, followed by magnetic separation using $Fe_3O_4$ nanoparticles. The reduction efficiency of the photocatalytic reaction was 81.4% at a UV power of 6W for 3 h with a dark adsorption of 17.5% to the nanoparticles, as determined by inductively coupled plasma-mass spectrometry (ICP-MS). The developed separation method can be used for the speciation and preconcentration of selenium cations in environmental and biological analysis.

• Bulletin of the Korean Chemical Society
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• v.27 no.9
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• pp.1293-1296
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• 2006

In this study, a solid phase extraction method has been developed for the preconcentration and separation of the elements Cr(III), Fe(III), Co(II) and Pb(II) at trace levels by using a column packed with Amberlite XAD-1180 resin loaded with 4-(2-pyridylazo)-resorcinol (PAR) reagent. After preconcentrating, the metals retained on the column were eluted with 20 mL of 3 mol/L $HNO_3$ and then determined by flame atomic absorption spectrometry (FAAS). The factors affecting the recovery of the elements, such as pH, type and concentration of eluent, volume of sample and elution solution, and matrix components, were also ascertained. The recoveries of Cr(III), Fe(III), Co(II) and Pb(II) were found to be $99\;{\pm}\;4,\;97\;{\pm}\;3,\;95\;{\pm}\;3$ and $98\;{\pm}\;4$%, respectively, under the optimum conditions at 95% confidence level and the relative standard deviations found by analyzing of nine replicates were $\leq4.4$%. The preconcentration factors for Cr(III), Fe(III), Co(II) and Pb(II) were found as 75, 125, 50 and 75 respectively. The detection limits (DL, 3s/b) were 3.0 $\mu g/L$ for Cr(III), 1.25 $\mu g/L$ for Fe(III), 3.3 $\mu g/L$ for Co(II), and 7.2 $\mu g/L$ for Pb(II). The recoveries achieved by adding of metals at known concentrations to samples and the analysis results of Buffalo river sediment (RM 8704) show that the described method has a good accuracy. The proposed method was applied to tap water, stream water, salt and street dust samples.