• Bulletin of the Korean Chemical Society
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• v.22 no.8
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• pp.821-826
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• 2001

Solvent sublation has been studied for the separation and determination of trace Zn(Ⅱ) and Pb(Ⅱ) in water samples. A synergy producing method was utilized to improve the efficiency of extraction in the sublation using an ion-pair of metal-naphth oate {M-(Nph)3- } complexes and tetra-n-butylammonium (TBA+ ) ion. After the M-(Nph)3- complexes were formed by adding 1-naphthoic acid to the sample solution, tetra-n-butylammonium bromide was added in the solution to form the ion-pair. And sodium lauryl sulfate (SLS) was added to make the ion-pair hydrophobic. The ion-pairs of the metal complexes were floated and extracted into methylisobutyl ketone (MIBK) from the aqueous solution by bubbling with nitrogen gas in a flotation cell. Metal ions in MIBK solution were measured by graphite furnace-AAS. Experimental conditions were optimized as follow so. After the pH of a 1.0 L water sample was adjusted to 5.0, 6.0 mL of 0.1 M 1-HNph and 10 mL of 0.03 M TBA-bromide were added to the sample to form ion-pairs, and 2.0 mL of 0.2%(w/v) SLS was added to make the ion-pairs hydrophobic. The solution was bubbled with 30 mL/min N2 gas for 5 minutes in a flotation cell. Linear calibration curves were obtained for the determination of Zn(Ⅱ) and Pb(Ⅱ) in several water samples. Reproducible results of showing a relative standard deviation of < 10% and recoveries of 80-100% could be obtained.

• Applied Chemistry for Engineering
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• v.23 no.5
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• pp.505-509
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• 2012

In this study, we investigate the use of new carbon nanotube paste electrode (CNPE) for promoting the detection of lead (Pb) heavy metal in the a drinkable water, which negatively affects human brain and nerve system. For the evaluations, CNPE is served as a working electrode, while sensitivity and limit of detection (LOD) of Pb are measured in DI and tap water based electrolytes using squarewave anodic stripping voltammetry (SWASV). As a result of that, in the 25~150 ppb range of $Pb^{2+}$ ions, its sensitivity and calculated LOD are $12.85\;{\mu}A/{\mu}M$ and 26 ppb in DI water based 0.1 M $H_{2}SO_{4}$ electrolyte while they are $10.36\;{\mu}A/{\mu}M$ and 38 ppb electrolytes respectively. In addition, experimentally measured LOD values of Pb are 4 ppb and 10 ppb in the two water electrolytes. The stripping of $Pb^{2+}$ ion is also controlled by surface reaction. Our experimental data are then compared with those of other already published references. With the comparison, it is proved that our electrode outperforms other electrodes in terms of the sensitivity and LOD of trace Pb metal.

• Analytical Science and Technology
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• v.11 no.4
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• pp.281-291
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• 1998

An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in blood and urine has been investigated by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Microwave oven was used for the pretreatment of blood samples using nitric acid and hydrogen peroxide in a closedvessel digestion system with 1 mL whole blood for 8 minutes. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Detection limits for Cu, Sn, and Bi by this method were 0.000375 ng/mL, 0.000297 ng/mL, and 0.000174 ng/mL, respectively. Recoveries of 99.1% for Cu, 102.5% for Sn, and 98.4% for Bi were obtained for the standard spiked NIST SRM 955a blood sample. The developed method was applied for whole real blood and urine samples.

• Journal of the Korean Chemical Society
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• v.39 no.1
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• pp.35-39
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• 1995

Simultaneous measurements of trace platinum and rhodium, based on catalytic reduction of protons by the adsorbed Pt-formazone and Rh-formaldehyde complexes formed in formaldehyde-hydrazine-sulfuric acid medium, were demonstrated. The conditions for the measurements of Pt and Rh both present at trace levels (>10-10 M) were 0.004% (w/v) formaldehyde-0.0012% (w/v) hydrazine-0.75 M sulfuric acid. In this medium method detection limits are 7.3${\times}$10-11 M Pt and 3.2${\times}$10-11 M Rh. And dynamic ranges are 5${\times}$10-10~6${\times}$10-8 M and 1${\times}$10-10∼2${\times}$10-8 M for platinum and rhodium respectively. In the linear dynamic ranges, Rh and Ir interfere platinum in the presence of only 10 and 100 times that of Pt respectively. There are no interferences from other platinum group metal ions for rhodium even in the presence of a 500-fold excess of Ir(IV), a hundredfold excess of platinum.

• Bulletin of the Korean Chemical Society
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• v.27 no.11
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• pp.1757-1762
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• 2006

A solvent sublation using salphen as a ligand was studied and applied for the determination of trace Ni(II), Co(II) and Cu(II) in water samples. The fundamental study was investigated by a solvent extraction process because the solvent sublation was done by extracting the floated analytes into an organic solvent from the aqueous solution. The salphen complexes of Ni(II), Co(II) and Cu(II) ions were formed in an alkaline solution of more than pH 8 and then they were extracted into m-xylene. It was known that the each metallic ion formed 1 : 1 complex with the salphen and the logarithmic values of extraction constants for the complexes were 3.3 5.1 as an average value. Based on the preliminary study, the procedure was fixed for the separation and concentration of the analytes in samples. Various conditions such as the pH of solutions, the influence of $NaClO_4$, the bubbling rate and time of $N_2$ gas, and the type of organic solvent were optimized. The metal-salphen complexes could be extracted into m-xylene from the solution of more than pH 8, but the pH could be shifted to acidic solution of pH 6 by the addition of $NaClO_4$. In addition, the solvent sublation efficiency of the analytes was increased by adding $NaClO_4$. The recovery of 97-115% was obtained in the spiked samples in which given amounts of 0.3 mg/L Ni(II), 0.8 mg/L Co(II) and 0.04 mg/L Cu(II) were added.

• Journal of Environmental Health Sciences
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• v.27 no.4
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• pp.63-71
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• 2001

PM 2.5/ samples were measured at two sites, Hadan(suburban site) and Anrak (roadside site) in Busan area. PM 2.5/ sampling was performed for 24-hour intervals by the FH9.5 particulate sampler. Aerosol samples were collected on PTFE filter. A total of 60 particulate samples were collected, dad samples were measured for Particulate mass concentration, metallic elements (Cr, Mn, Ni. Cu. Se, Fe, Pb, and Zn) and waer-soluble elements (C $l^{[-10]}$ , N $O_{3}$$^{[-10]}$ ,S $O_{4}$$^{2-}$, N $H_{4}$$^{+}$, $Ca_{2}$$^{+}$, $Mg_{2}$$^{+}$ and $^{+}$.Mass concentration in Hadan ranged 24.23~57.12 $\mu\textrm{g}$/㎥ and 60.22~72.12 $\mu\textrm{g}$/㎥m Yellow Sand Events. Major cations in Hadan and Anrak site is N $H_{4}$$^{+}$and N $a^{+}$ respectively. SO42$^{[-10]}$ was the abundant specie in the PM 2.5 fraction for Hadan site an dAnrak site. Hadan site showed igher concentration in S $O_{4}$$^{2.1}$ and N $H_{4}$ $^{+}$ In Anrak site the concentration of S $O_{4}$/sip 2-/and N $a^{+}$ was higher than other ions Prominent metallic elements were Fe and Pb in two sites. Principal component analysis showed that main source of PM 2.5 aerosol particles was non-metal related source which was resulted in relating elements as Cr, Ni, and Pb at Hadan site, Anrak site also has resulted PM2.5 aerosol paricles source, which was related its element like Zn, and Ni,. The SAS package analysis also showed that long-range transport effect at Hadan area due to Yellow Sand Event by the prevailing weaterlies.ling weaterlies.

• Journal of the Korean Chemical Society
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• v.43 no.1
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• pp.36-41
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• 1999

The adsorptive stripping voltammetric determination method of trace germanium (IV) using mercaptoacetic acid as a ligand was studied. Optimal conditions were found to be 0.25 M NaCl solution (pH 6.0) containing mercaptoacetic acid concentration of $5.0{\times}10^{-6}M$. The peak potential appeared at - 1.402 V vs. Ag/AgCl. Effects of sodium chloride concentration, mercaptoacetic acid concentration, and accumulation time for the complex of Ge(IV)-Mercaptoacetic acid on the peak current were studied. Amberlite IRC-718 chelating resin was applied to the separation of Ge(IV) from other metal ions.

• Analytical Science and Technology
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• v.6 no.3
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• pp.247-254
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• 1993

Strontium can not be determined by conventional dc polarography method since it is very difficult to be reduced at the drop mercury electrode(DME) in aqueous solution. However the analytical sensitivity was improved by adsorptive stripping voltammetry in which electro-reduction of ligand in a complex formed between strontium and o-cresolphthaleoxone was performed. Strontium could be determined in range of $5{\sim}30{\mu}g/L$ concentration. This method was affected by coexistent alkali earth metal ions. Consequently ion exchange separation is recommended to analyze strontium in samples.

• Journal of the Korean Vacuum Society
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• v.12 no.S1
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• pp.7-9
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• 2003

Solid-state reactions in Ni/Si multilayered films (MLF) with an overall stoichiometry of $Ni_2Si$, NiSi and $NiSi_2$, induced by ion-beam mixing (IBM) and thermal annealing, were studied by using spectroscopic ellipsometry and magneto-optical spectroscopy as well as x-ray diffraction (XRD). The mixing was performed with Ar+ ions of an energy of 80 keV and a dose of $1.5 x\times10^{16}$ $Ar^+$/$\textrm{cm}^2$. It was shown that the IBM induces structural changes in the Ni/Si MLF, which cannot be detected by XRD but are confidently recognized by the optical method. A thermal annealing at 673 K of the Ni/Si MLF with an overall stoichiometry of NiSi and $NiSi_2$ causes formation of the first η -NiSi phase. The first trace for $NiSi_2$ phase on the background of NiSi one was detected by XRD after an annealing at 1073 K while, according to the optical results, $NiSi_2$ turns out be the dominant phase for the annealed Ni/Si MLF with an overall stoichiometry of $NiSi_2$.

• Journal of the Korean Chemical Society
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• v.19 no.6
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• pp.428-433
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• 1975

500 ml of a sample water was extracted with 10 ml of 0.01 % dithizone-$CHCl_3$three times. When $CHCl_3$ layer was back extracted with 10 ml of 0.1 N HCl containing mercuric ion, the free metal ions come into aqueous layer. The aqueous layer was added with 2 ml of 2 N KCl and was washed with 10 ㎖ of $CHCl_3$two times in order to remove the trace dithizone, and then was recorded square wave polarogram. The concentration of copper, lead and cadmium can be determined up to 3 ppb and that of zinc up to 14 ppb with an error of 10 %.