• Journal of the Korean Chemical Society
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• v.38 no.7
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• pp.485-495
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• 1994

Several new symmetric and asymmetric homo and hetero dinuclear complexes of the type $[Cl(dppp)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$ and $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$(M,M'= Mo or W; phen = 1,10-phenanthroline; dppp = 1,3-bis(diphenylphosphino)propane; pyz = 1,4-pyrazine) were synthesized in three-steps starting from $[M(NO)_2Cl_2]_n(M = Mo, W)$. The final products were purified by eluting it through silica gel column ($2{\times}20$ cm) with acetone as the eluent. Characterization of these complexes and some related complexes was accomplished through UV-vis., $^1H$-NMR, $^{13}C$-NMR and IR spectroscopies as well as elemental analysis. The infrared spectra indicate that the NO groups occupy cis-positions of the octahedral. The $^1H$ and $^{13}C-NMR$ data for the new compounds revealed a dimeric structures with bridged pyz.

• Journal of the Korean Chemical Society
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• v.33 no.1
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• pp.46-54
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• 1989

The extraction method and quantitative analysis for the fat-soluble vitamins present in food stuffs and vitamin products have been investigated. The simultaneous separation and analysis of the vitamins by reverse phase high performance liquid chromatographic method was conducted using an isocratic elution with methanol : water (95 : 5) eluent on a Novapak $C_{18}$ column. The detection of vitamins was achieved by a variable wavelength UV detector. To improve the detection sensitivity detection wavelengths were set at the highest absorption bands such as 330, 265, 285, and 290nm for the respective vitamins. The analysis for the fat-soluble vitamins was finished within 40 minutes. Alkaline hydrolysis and enzymatic hydrolysis were investigated for the sample preparation; and liquid-liquid extraction and liquid-solid extraction were attempted for the extraction of vitamins. Both hydrolysis methods were turned out to be appropriate for the analysis for vitamins A, D, and E, while for the analysis of vitamin K the enzymatic hydrolysis method demonstrated better results. Diethyl ether, pentane, and n-hexane were found to give higher recovery for the liquid-liquid extraction and silica cartridge for the liquid-solid extraction.

• Journal of Food Hygiene and Safety
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• v.3 no.4
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• pp.211-215
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• 1988

Anion chromatographic (lC) method was developed for the determination of sulfites infoods. Sulfites refer to sulfur dioxide that was separated from a food sample by addition of acid and heating, and carried into a trapping solution by distillation. The trapping solution was applied to IC system. Sulfites was separated on an anionic separator column, HPIC-AS4A with 0.75mM $NAHCO_3/2.25mM\;Na_2CO_3$ as the eluent and determined by the use of conductivity detector. The recoveries of sulfites added to water, carrot and apple at level of 1 ppm were 99.8%, 91.6% and 83.5%, respectively. The detection limit was 0.2 ppm in the case of a 10 g sample size. All experiment could be finished within 20 minutes

• Bulletin of the Korean Chemical Society
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• v.22 no.8
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• pp.801-806
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• 2001

A study has been carried out on the separation of gold, iridium, palladium, rhodium, ruthenium and platinum in chromite samples and their quantitative determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution condition of the minerals by fusion with sodium peroxide was optimized and chromatographic elution behaviour of the rare metals was investigated by anion exchange chromatography. Spectral interference of chromium, a matrix of the minerals, was investigated on determination of gold. Chromium interfered on determination of gold at the concentration of 500 mg/L and higher. Gold plus trace amounts of iridium, palladium, rhodium and ruthenium, which must be preconcentrated before ICP-AES was separated by anion exchange chromatography after reducing Cr(Ⅵ) to Cr(III) by H2O2. AuCl4- retained on the resin column was selectively eluted with acetone- HNO3-H2O as an eluent. In addition, iridium, palladium, rhodium and ruthenium remaining on the resin column were eluted as a group with concentrated HCl. However, platinum was eluted with concentrated HNO3. The recovery yield of gold with acetone-HNO3-H2O was 100.7 ${\pm}2.0%$, and the yields of palladium and platinum with concentrated HCl and HNO3 were 96.1 ${\pm}1.8%$ and 96.6 ${\pm}1.3%$, respectively. The contents of gold and platinum in a Mongolian chromite sample were 32.6 ${\pm}$ 2.2 ${\mu}g$/g and 1.6 $\pm$ 0.14 ${\mu}g$/g, respectively. Palladium was not detected.

• Archives of Pharmacal Research
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• v.22 no.3
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• pp.288-293
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• 1999

Postabsorptive serum iron level was determined after oral administration of the compounds to human. In serum and whole blood, $Fe^{3+}$ was measured by ion chromatography (IC) using a pyridine-2,6-dicarboxylic acid (PDCA) as an eluent. The serum sample solutions were pretreated with I N HCI and 50% TCA. The whole blood sample solutions were treated with 3 N HCI for 30 min at $125^{\circ}C$. The limit of detection (LOD) of the IC technique is $0.2 {\mu}M$ for$Fe^{2+}$and 0.1 $\mu$M for $Fe^{3+}$. The area under concentration (AUC) can be obtained by the above analytical condition. In addition, to compare the stability of $Fe^{2+}$ to that of $Fe^{3+}$ in pharamaceutical preparations, accelerated stability test was carried out. After storing the samples under $40^{\circ}C$, 75%RH in light-resistant container for various time intervals, the contents of iron of different valencies were determined separately by the IC technique and the change and/or the interchange of among those iron species in preparations was investigated. Iron raw materials are stable, but $Fe^{2+}$ in$Fe^{3+}$ source materials was slightly converted to $Fe^{3+}$ by oxidation. $Fe^{2+}$ in$Fe^{3+}$ source raw materials and $Fe^{3+}$ in $Fe^{2+}$ raw materials are determined as impurities. Therefore, IC technique is found to be an appropriate method for comparative evaluation of dissimilar bioavailability of $Fe^{2+}$ and $Fe^{3+}$, stability of $Fe^{2+}$ and $Fe^{3+}$ raw materials and preparations.

• Journal of the Korean Wood Science and Technology
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• v.32 no.1
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• pp.59-66
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• 2004

The dried neeldes(1.5 kg) of Juniperus rigida were ground, extracted with acetone-H₂O(7:3, v/v), concentrated, and fractionated with a series of hexane, CH₂Cl₂, EtOAc and water on a separatory funnel. Each fraction was freeze dried to give dark-brown powder and EtOAc and water soluble fractions were chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluent. Spectrometric analysis such as NMR and FAB or EI-MS including TLC were performed to characterize the structures of the isolated compounds. The needles of Juniperus rigida contained a large amount of (+)-catechin, quercetin-3-O-α-L-rhamnopyranoside and isoconiferin, in addition to a small amount of umbelliferone and quercetin-3-O-β-D-rutinoside. The antioxidative activities of each fraction and isolated compounds were tested by DPPH radical scavenging method, and EtOAc soluble fraction, (+)-catechin and quercetin-3-O-α-L-rhamnopyranoside were effective.

• Journal of Radiation Protection and Research
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• v.48 no.2
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• pp.77-83
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• 2023

Background: The purpose of this study is to purify uranium (U[VI])-contaminated soil-flushing effluent using the precipitation-distillation process for clearance. Precipitation and distillation are commonly used techniques for water treatment. We propose using a combination of these methods for the simple and effective removal of U(VI) ions from soil-flushing effluents. In addition, the U concentration (Bq/g) of solid waste generated in the proposed treatment process was analyzed to confirm whether it satisfies the clearance level. Materials and Methods: Uranium-contaminated soil was decontaminated by soil-flushing using 0.5 M sulfuric acid. The soil-flushing effluent was treated with sodium hydroxide powder to precipitate U(VI) ions, and the remaining U(VI) ions were removed by phosphate addition. The effluent from which U(VI) ions were removed was distilled for reuse as a soil-flushing eluent. Results and Discussion: The purification method using the precipitation-distillation process proposed in this study effectively removes U(VI) ions from U-contaminated soil-flushing effluent. In addition, most of the solid waste generated in the purification process satisfied the clearance level. Conclusion: The proposed purification process is considered to have potential as a soil-flushing effluent treatment method to reduce the amount of radioactive waste generated.

• Journal of the Korean Chemical Society
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• v.17 no.5
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• pp.346-352
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• 1973

The quantitative separations of a mixture containing equal amounts of each cation such as Mn(Ⅱ), Cr(Ⅲ), V(Ⅴ), Cu(Ⅱ), Ni(Ⅱ), Co(Ⅱ), and Fe(Ⅲ) are carried out by the elution through $35cm{\times}3.14cm^2$ column of cation exchange resin, $Dowex 50w{\times}12$. The eluents are a mixture of 0.6 M sodium chloride and 0.1 M sodium tartrate (pH = 2.00 and 4.50) for Fe(Ⅲ), V(Ⅴ), Cu(Ⅱ), Ni(Ⅱ) and Co(Ⅱ), and a mixture of 3 M sodium chloride and 0.1 M sodium tartrate (pH = 4.50) or a mixture of 0.7 M sodium chloride and 0.5 M sodium oxalate (pH = 4.50 and 5.00) for Mn(Ⅱ) and Cr(Ⅲ). The subsidiary cations in a standard iron mixture such as V(Ⅴ), Cu(Ⅱ), Ni(Ⅱ), Mn(Ⅱ) and Cr(Ⅲ) are separated together from the large amount of Fe(Ⅲ) through $15cm{\times}3.14cm^2$ column of the resin, $Dowex 1{\times}8$, by elution with the eluent of 4.0 M hydrochloric acid. A small amount of Fe(Ⅲ), however, is eluted together with Cu(Ⅱ). V(Ⅴ), Ni(Ⅱ), Mn(Ⅱ) and Cr(Ⅲ) eluted together are separated quantitatively through $10cm{\times}3.14cm^2$ column of the resin,$Dowex 50w{\times}12$. Cu (Ⅱ) and a small amount of Fe(Ⅲ) are separated quantitatively through $10cm{\times}3.14cm^2$ column of the resin, $Dowex 50w{\times}12$, by the elution with a mixture of 0.6 M sodium chloride and 0.1 M sodium tartrate (pH = 2.00 and 4.50) as an eluent. By the conditions obtained in the separations of the standard iron mixture, Fe(Ⅲ) and all of the subsidiary cations in steel are quantitatively separated.

• Journal of the Korean Chemical Society
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• v.17 no.1
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• pp.20-24
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• 1973

The average fission neutron cross sections were determined for the following reactions, $^{93}Nb(n,\alpha)^{90}Y$, $^{90}Zr(n,p)^{90}Y$,$^{93}Nb(n,\alpha)^{90m}Y$and$^{90}Zr(n,p)^{90m}Y$. The cation exchange column was used for the quantitative separation of the product nuclides using $\alpha-$hydroxyisobutyric acid as the eluent. The absolute activites of $^{90m}Y$ and $^{90}Y$were determined by the gamma ray spectrometry and a calibrated $2\pi$gas flow counter, respectively. The cross sections of $^{93}Nb(n,\alpha)^{90}Y$, $^{90}Zr(n,p)^{90}Y$,$^{93}Nb(n,\alpha)^{90m}Y$and $^{90}Zr(n,p)^{90m}Y$ reactions were found to be$0.14\pm0.01mb$, $0.83\pm0.02mb$, $0.018\pm0.02mb$ and $0.33\pm0.02mb$, respectively. The possible use of $^{90m}Y$ instead of $^{90}Y$ was discussed as a better means for the determination of niobium.

• Journal of the Korean Chemical Society
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• v.58 no.2
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• pp.179-185
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• 2014

Commercial (S)-naproxen was racemized under strong basic condition. After checking the peak position of (R)- and (S)-naproxen by analysis the recemized naproxen, optical purity of 19 commercialized naproxens sold in 2013 in Korea were examined by chiral HPLC. The Chiralcel OD-H column, ChiralHyun-LE(S)-1 column and LUX-Cellulose-1 column were used as chiral stationary phases and the mixed eluent of hexane:isopropanol:acetic acid as 100:1:0.1 was used as a mobile phase with a flow rate of 1.0 mL/min. Each data was obtained from an average value of at least three different experiments for each sample and the relative standard deviation of them appeared very small. The average optical purity values obtained from three different chiral columns were very similar and the total average optical purity value (99.32%) of nineteen commercialized naproxens used in this study were larger than those of three years ago (98.17%).