• Bulletin of the Korean Chemical Society
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• v.28 no.3
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• pp.373-378
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• 2007

A micro organism Agrobacterium tumifacient as an immobilized cell on a solid support was presented as a new biosorbent in a simple and sensitive spectrophotometry determination of Ni(II) in various samples using 4-hydroxy benzaldehyde-4-bromophenyl hydrazone as a color developing agent (λmax 497 nm) at pH 4.0 ± 0.2. Beer's law was obeyed over the range of 0.01-0.1 μg L-1. The molar absorptivity and Sandell's sensitivity were 1.285 × 105 L mol-1cm-1 and 0.007245 μg cm-2 respectively. Under these conditions, the preconcentration factor obtained was 82, and the detection limit achieved was 0.05 μg L-1. The detailed study of various interfering ions made the method more sensitive and selective. The recovery of Ni(II) from various samples range from 97.75 to 99.35%. The present method was successfully applied for the determination of Ni(II) in spiked, natural water and alloy samples. The proposed method was compared with reported methods in terms of Student's ‘t'-test and Variance ratio ‘f'-test which indicates that there is no significant difference between proposed and literature method at 95% confidence level.

• Bulletin of the Korean Chemical Society
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• v.23 no.6
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• pp.861-865
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• 2002

A sensitive method for the determination of trace copper(II) after the preconcentration by adsorbing its cupferron complex onto microcrystalline benzophenone was developed.Several experimental conditions such as the pH of sample solution,concentration of cupferron, amount of benzophenone and atirring time were optimized. Trace compper(II) in 100mL solution was chelated with $3.0\;{\times}\;10^3$ M cupferron at pH 5.0. After 0.20g benzophenone, The benzophenone adsorbing Cu-cupferron complex was filtered and then Cu-cupferron complex was desorbed in 10 mL ethanol. Copper was determined by a flame atomic absorption spectrophotomethry. The interfering effects of diverse concomitant ions were investigated. Fe(III) interfered seriously with, but the interference by Fe(III) was completely eliminated by adjusting the concentration of copferron to $5.0\;{\times}\;10^3$ M. The detection limit of this method was 8.6${\times}$10 M(5.5 ngmL$^1$). Recoveries of 97% and 96% were obtained for Cu(II) in a stream water and a brass sample, respectively. Based on the results from the experiment. this proposed technique could be applied to the determination of copper(II) in real samples.

• 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 Environmental Health Sciences
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• v.26 no.4
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• pp.110-114
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• 2000

Determination of mercury(II) using Nafion-EDTA-modified glassy carbon electrodes is proposed. it is based on the chemical reactivity of an immobilized modifier, Nafion-EDTA. Differential pulse voltammetry is employed, and the oxidation of complexes, at +0.43V vs. Ag/AgCl, is observed. For a 5-min preconcentration period, a linear calibration curve is obtained for mercury(II) concentrations ranging from 1.0$\times$ 10$^{-8}$ to 1.0$\times$10$^{-6}$ M. Further, when an approximate amount of copper(II) is added to the test solution, We demonstrate that at a preconcentration time of 5 min the Nafion-EDTA-modified glassy carbon electrode has a dynamic range of 2 orders of magnitude(from 10$^{-10}$ to 10$^{-8}$ M) and the detection limit is as low as 0.5$\times$ 10$^{-10}$ M(0.01 ppb). This method is applied to the determination of mercury(II) in sea water(4.0$\times$10$^{-10}$ M, 0.08ppb). The result agrees satisfactorily with the value(below 0.1 ppb) measured by using ICP/MS.

• BioChip Journal
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• v.12 no.4
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• pp.317-325
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• 2018

This paper investigated the effects of ionic strength in the medium on a preconcentrator for a protein sample with low concentration. The preconcentration chip was designed and fabricated using a polydimethylsiloxane replica through standard lithophotography. A glass substrate is silanized prior to functionalizing the nanoparticles for self-assembly at a designed region. Due to the overlap of electrical double layers in a nanofluidic channel, a concentration polarization effect can be achieved using an electric field. A nonlinear electrokinetic flow is induced, resulting in the fast accumulation of proteins in front of the induced ionic depletion zone, so called exclusion-enrichment effect. Thus, the protein sample can be driven by electroosmotic flow and accumulated at a specific location. The chip is used to collect fluorescein isothiocyanate-labeled bovine serum albumin (FITC-BSA) diluted in phosphate-buffered saline (PBS) buffer solution. Different concentrations of the buffer media were studied herein. Fluorescence intensity images show that the buffer concentration of 4 mM is more appropriate than all the other ones. The sample of FITC-BSA with an initial concentration of $10{\mu}M$ in the 4 mM PBS solution increases its concentration at the desired region by up to 50 times within 30 min, demonstrating the results in this investigation.

• Analytical Science and Technology
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• v.20 no.1
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• pp.55-60
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• 2007

A sensitive technique for the determination of trace Cu(II) in various samples after the column preconcentration by adsorbing its N-benzoylphenylhydroxylamine (BPHA) onto benzophenone was developed. Several experimental conditions such as the pH of the sample solution, the amount of chelating agent, the amount of benzophenone, and the flowrate of sample solution and so forth were optimized. The interfering effects of diverse concomitant ions were investigated. Fe(III) and $CN^-$ interfered with more seriously than any other ions. However, the interference by these ions could be overcome sufficiently by adjusting the added volume of 0.01M BPHA to 10 mL. The dynamic range, the correlation coefficient ($r^2$) and the detection limit obtained by this proposed technique were 5.0~120 ng/mL, 0.9974, and 2.1 ng/mL, respectively. For validating this proposed technique, the aqueous samples (stream water, reservoir water, and wastewater), the plastic sample and the diluted brass sample were used. Recovery yields of 93~102% were obtained. These measured data were not different from ICP-MS data at 95% confidence level. This method was also validated by the rice flour CRM (normal, fortified) samples. Based on the results from the experiment, it was found that this proposed technique could be applied to the determination of Cu(II) in various real samples.

• Journal of the Korean Chemical Society
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• v.37 no.5
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• pp.513-522
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• 1993

The purpose of this study is to optimize the selectivity of mobile phase solvents for separation of 25 phenols in reversed phase liquid chromatography and to accomplish the simultaneous preconcentration and separation of trace phenols from water samples. Phenols used in this study were classified into three groups, chloro-, methyl-, and nitrophenols. Quaternary solvent mobile phases were employed to improve the selectivity. Overlapping resolution maps(ORM) as a statistical simplex techniques was used to predict the optimum solvent system. Additional criterion such as pH and temperature were also investigated. In order to improve the resolution and decrease the analysis time, isoselective multisolvent gradient elution system was employed with ORM-Prism method. The simultaneous preconcentration and separation of trace phenols from water samples were performed by using XAD-2/Dowex 1-X8 tandem column. When the extraction efficiency was evaluated by sampling up to 1 L of distilled water, recovery of the phenols, except phenol, was above 90% and the limit of detection of the phenols was 5 ppb. The XAD-2/Dowex 1-X8 method was superior to C18 cartridge in terms of recovery and selectivity.

• Journal of the Korean Chemical Society
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• v.50 no.1
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• pp.23-31
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• 2006

carbon modified methods were used for the preconcentration and determination of copper in some real samples using the flame atomic absorption spectrometry. The copper ions was adsorbed quantitatively on the activated carbon due to their complexation with 4- amino-2, 3-dimethyl-1-phenyl-3-pyrazoline (ADMPP) or 4-(4- methoxybenzylidenimin) thiophenole (MBITP). The adsorbed copper on solid phase was eluted quantitatively using small amount of nitric acid. The influence of important parameters including pH, amount of carrier, flow rate, amount of activated carbon and type and concentration of eluting agent for obtaining maximum recovery were investigated. The methods based on ADMPP and MBITP at optimum conditions is linear over concentration range of 0.05-1.5 g mL-1 and 0.05-1.2 g mL-1 of copper with correlation coefficient of 0.9997 and 0.9994 and both detection limit of 1.4 ng mL-1, respectively. The preconcentration leads to enrichment factor of 310 and break through volume of 1550 mL for both ligands. The method has a good tolerance limit of interfering ion and a selectivity that has been successfully applied for the determination of copper content in real sample such as tap, spring, river and waste water.

• 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.

• Bulletin of the Korean Chemical Society
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• v.15 no.12
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• pp.1045-1049
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• 1994

A simple and fast ion chromatographic method is developed for the determination of transition metals such as Fe, Cu, Ni, Zn and Co in atmospheric particulates. The method involves acid digestion, on-column preconcentration, and subsequent ion chromatogaphic detection. The precision of the method is less than 3${\%}$ RSD at parts per billion level for the metals studied. No significant interferences are observed. The results obtained with this method agree well with those by ICP-AES.