• Journal of Korean Society of Environmental Engineers
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• v.32 no.4
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• pp.349-356
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• 2010

Ion chromatography (IC) coupled with conductivity detector (CD) is a common system for the determination of perchlorate in water samples. Although the IC method with CD has been widely used for the determination of trace level perchlorate ion in water, sensitivity decreases dramatically as the complexity of the matrices increases. Here we proposed the application of ion chromatography coupled with mass spectrometry (IC-MS/MS) to significantly improve selectivity of perchlorate. The mean recovery of the method was 104.4 ${\pm}$ 5.7% and the relative standard deviation (RSD%) was 1.9 ${\pm}$ 1.3%. The alculated method detection limit (MDL) was 0.0207 ${\pm}$ 0.0099 ${\mu}g/L$. The concentrations of perchlorate were minimum <0.1 ${\mu}g/L$ and maximum 18.3 ${\mu}g/L$ in source water (Namhan, Bukhan and Han River). Hongreung showed higher concentrations ($1^{st}$-14.3 ${\mu}g/L$, $2^{st}$-18.3 ${\mu}g/L$) than the other places. And the concentrations of perchlorate were 0.18~0.34 ${\mu}g/L$ in the samples taken from the six water treatment plants and six intake stations in Seoul.

• Analytical Science and Technology
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• v.23 no.6
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• pp.560-565
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• 2010

Perchlorate ion ($ClO_4^-$) has been widely used as oxidizing agent in military weapon system such as rocket and missile fuel propellant. So it has been challenging to remove the pollutant of perchlorate ion. nanoscale zero valence iron (nZVI) particles are widely employing reduction catalyst for decomposition of perchlorate ion. nZVI particles has increasingly been utilized in groundwater purification and waste water treatment. But it have strong tendency of aggregation, rapid sedimentation and limited mobility. In this study, we focused on reduction of perchlorate ion using nZVI particles immobilized in alginate polymer bead for stabilization. The stabilized nZVI particles displayed much greater surface area, and much faster reaction rates of reduction of perchlorate ion. In this study, an efficient way to immobilize nZVI particles in a support material, alginate bead, was developed by using $Ca^{2+}$ as the cross-linking cations. The efficiency and reusability of the immobilized Fe-alginate beads on the reduction of perchlorate was tested at various temperature conditions.

• Journal of the Korean Chemical Society
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• v.27 no.1
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• pp.18-23
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• 1983

To understand the abnormal absorption behavior of rare earths in cation exchange resins, the absorption for Ce(III), Tb(III) and $Cl^-$ ions in Dowex 50W-X2 have been investigated by spectrophotometry in the concentration range of $1{\sim}12$ M HCI and $HCl-HClO_4$ mixed solutions. The amount of $Cl^-$ ion absorbed shows that the ratio of amount of $Cl^-$ ions to that of rare earths does not exceed 10% in the concentration range of $6{\sim}8M$ HCl and decreased gradually to 3% at 2M HCl and 6% at 12M HCl. The ratio is further decreased with the fraction of $HClO_4$ in $HCl-HClO_4$ mixed solutions and the decrease is presumably due to the weak tendency to form a complex between rare earths and $Cl^-$ ions in a cation exchange resin. The effect of $ClO_4^-$ is expected to play a more important role than that of $Cl^-$ ions in the large absorption of rare earths.

• Analytical Science and Technology
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• v.26 no.1
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• pp.11-18
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• 2013

Perchlorate ($ClO{_4}^-$) is the material that is used as propellants of rockets and material of explosive as a form of ammonium perchlorate salts. Ammonium perchlorate solution of high concentration is recovered from expired rocket through demilitarization process by the water-jet method. If people take perchlorate in food and water, it interferes with adsorption of iodide which is the substance needed to synthesize thyroid hormone in the thyroid gland. It has an bad influence upon disturbing pregnancy and synthesis of growth hormone. So the effective method is necessary to remove perchlorate anion in water. By considering economic aspect, we studied effective desorption (regeneration) of perchlorate anion from adsorbent with studies on removal and adsorption of perchlorate anion. Desorption experiment was conducted as batch type. Depending on various conditions (concentration, pH, cation anion form) elution, we evaluated amount, efficiency of desorption(amount of adsorption/desorption ${\times}$ 100). Also, research confirmed the efficiency of mixed resins between anion exchange resin and activated carbon and expected synergic effect from advantages of both adsorbents.

• Proceedings of the Membrane Society of Korea Conference
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• 1998.04a
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• pp.49-52
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• 1998

1. 서론 : 화약이나 고체 충진제, 고체로\ulcorner 추진제의 산화제, slurry blasting agent 및 동물사료의 식품첨가제로 사용되고 있는 과염소산은 발화나 폭발성이 매우 강한 산화제로 정확한 순도를 측정하는 것은 중요하다. 용량분석법과 중량분석법에 비교하여 조작이 간단하고 편리한 과염소산이온의 농도를 직접 측정할 수 있는 PVC막 전극에 대한 많은 연구가 진행되고 있다. (생략)

• Journal of the Korean Electrochemical Society
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• v.19 no.3
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• pp.95-100
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• 2016

A method for electrochemical degradation of the perchlorate anion ($ClO_4{^-}$) using mercury film electrode has been studied. Electrochemical method has relatively simple pre-treatment. However, electrochemical method should avoid interference from hydrogen evolution at the applied potential to degradation of perchlorate ion, and thus applied electrode should have large hydrogen overvoltage which suppressed the hydrogen evolution at the working reduction potential to prevent hydrogen evolution. In this study, we used mercury film electrode as a working electrode which has a large overvoltage. Ag / AgCl (sat. NaCl) was used as a reference electrode, and platinum was used as a counter electrode. Mercury film electrode was made by cyclic voltammetry (CV) method. The deposition time was decided as 10 minute, and the stability of the mercury electrode in perchlorate solution was confirmed by CV. The reduction potential of perchlorate was checked by using CV method, and decomposition of perchlorate was performed by using chronoamperometric (CA) method. Also, ion chromatography (IC) was used to confirm the degradation rates of perchlorate.

• Journal of the Korean Chemical Society
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• v.25 no.6
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• pp.383-389
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• 1981

Thianthrene cation radical perchlorate reacts with N-arylsulfonamides such as p-toluenesulfonanilide, benzenesulfonanilide, N-(2-methylphenyl)benzenesulfonamide, and N-phenyl-p-toluenesulfonanilide to give 5-(p-N-p-toluenesulfonamidophenyl)-(1a), 5-(p-N-benzenesulfonamidophenyl)-(1b), 5-(4-N-benzenesulfonamido-3-methylphenyl)-(1c), and 5-(p-N-phenyl-N-p-toluenesulfonamidophenyl thianthrenium perchlorate (1d), respectively. In the meantime, 1d reacts further with thiathrene cation ratical to form diperchlorate(1e). The structure of 1a~1e is very similar to 5-(p-acetamidophenyl) thianthrenium perchlorate which has been obtained from the reaction with acetanilide. However, the discrepancy in the stoichiometry between two reactions indicates that the reaction with sulfonamide appears not to proceed with a single mechanism.

• Journal of the Korean Chemical Society
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• v.21 no.5
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• pp.320-329
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• 1977

p-Phenylenediamine dihydroperchlorate, $C_6H_4N_2H_4{\cdot}2HC1O_4$, crystallizes in space group $P\={1}$ with $a=4.79{\pm}0.02,\;b=9.03{\pm}0.02,\;c=7.12{\pm}0.03{\AA},\;{\alpha}=109.4{\pm}0.2,\;{\beta}=79.6{\pm}0.2,\;r=104.6{\pm}0.2^{\circ},\;Z=1$. The structure has been solved by the Patterson and Fourier methods. The refinement by block-diagonal least-squares cycles gives R = 0.13 for 387 observed reflexions collected on equi-inclination Weissenberg photographs with CuK${\alpha}$ radiation. There are two different types of five hydrogen bonds. The first type consists of one trifurcated N${\cdot}{\cdot}{\cdot}$O hydrogen bond and the second of two normal N${\cdot}{\cdot}{\cdot}$O hydrogen bonds, both of which exist between the amino group and the perchlorate, groups. A p-phenylenediamine group is approximately planar within an experimental error and bonded to twelve perchlorates: ten perchlorates forming hydrogen bonds and two being contacted with the van der Waals forces. A perchlorate group is surrounded by six p-phenylenediamines and four perchlorates; among the six p-phenylenediamines, five of them are hydrogen-bonded, and the rest contacted with the van der Waals force.ce anaysis of our samples and investigated the variarions in the values of parameters obtained through fitting the theoretical impedance to the experimental impedance. The characters of the dielectric constant and the impedance showed abnormal variations for the 0.2 at K-doped NSBN ceramics, which we were able to interpret in terms of the variations in the number A-site vacancies with the K doping ratio. From these results, A-site vacancies are thought to be space charges that influence the ferroelectric properties of NSBN ceramics.

• Analytical Science and Technology
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• v.25 no.6
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• pp.435-440
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• 2012

A liquid chromatography-electrospray ionization-tandem mass spectrometry method (LC-ESI-MS/MS) was used for determining perchlorate in the Gum-River surface water. Sample was directly injected into LC-ESI-MS/MS after the filtrations using PTFE filter paper. The coefficient of variation of perchlorate was less than 3% and the limit of quantification was 0.17 ${\mu}g/L$. Water samples were collected from thirty-five basins of Gum-River on February, April and June 2012, respectively. As a result, perchlorate was detected in the concentration range of 0.23-3.73 ${\mu}g/L$ (mean 0.20 ${\mu}g/L$) in the frequency of 15% in general surface water and in the concentration range of 0.36-25.10 ${\mu}g/L$ (mean 1.69 ${\mu}g/L$) in the frequency of 36% in surface water samples near industry area.

• Analytical Science and Technology
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• v.23 no.5
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• pp.429-436
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• 2010

The present research evaluates the efficiency of mixed resins between anion exchange resin and active carbon. We expected synergic effect from advantages of both adsorbents. Especially, this research focused on the removal of high cencentrated perchlorate ion from demilitarization solution. The total amount of the adsorbed perchlorate ion is increased considerably with mixed resins between mono functional anion exchange resin and granular active carbon from a single adsorbent. Results demonstated that this process not only improve the efficiency of adsorbing perchlorate, but save the time, space and cost for treating perchlotrate waste solution, because of reducing organic contaminant removing process. The interference effects from coexisting anions are not significant and can successfully applied to real demilitarization sample.