• Title/Summary/Keyword: Eluent Concentration

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Separation of Chromium(III) and Chromium(VI) by Carboxymethylated Polyamine-Polyurea Resin Column (카르복시메틸화된 폴리아민-폴리우레아 수지관에 의한 3가와 6가 크롬의 분리)

  • Chung, Yong Soon;Lee, Kang Woo;Hwang, Jong Youn;Lee, Yong Moon
    • Analytical Science and Technology
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    • v.7 no.2
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    • pp.205-211
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    • 1994
  • Acetic acid and succinic acid bonded polyamine-polyurea(CPPI and SAPPI) resins were synthesized from the reaction of polyethylenimine-polymethylenepolyphenylene isocyanate(PPI) resin as matrix polymer and chloroacetic acid and chlorosuccinic acid respectively. These resins were confirmed with infrared spectrometry and elemental analysis. The adsorption characteristics of the chromium(III) and dichromate(or chromate) ions on the resins were studied by measuring distribution coefficients($K_d$) with changing pH of the solution. It was thought that these ions were adsorbed by ion exchange mechanism. Chromium(III) and dichromate ion could be separated with stepwise elution method by changing pH of the eluent using SAPPI resin packed column($0.6cm(i.\;d.){\times}10cm(L.)$). Also, dichromate ion could be preconecntrated with CPPI resin column by a concentration factor of 50.

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Separation Study of Cytosine and Guanine by HPLC and Aspen Chromatography (Aspen Chromatography 전산모사와 HPLC를 이용한 구아닌 시토신의 분리특성연구)

  • Park, Moon Bae;Kim, In Ho
    • Korean Chemical Engineering Research
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    • v.48 no.1
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    • pp.88-92
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    • 2010
  • DNA structure studies attract many interests in pharmaceutical, biochemical and medical disciplines. Among them, base pairs play a vital role in biological information transfer. Therefore, they need to be analyzed in various ways and the pair of guaninine and cytosine is the present analytical object. Separation of guanine and cytosine was researched by Aspen chromatography simulator and HPLC(High Performance Liquid Chromatography) experiments. Aspen chromatography simulation resulted in various chromatograms with changes of sample concentration, eluent flow rate and number of plate. The resolutions and yields of guanine and cytosine were calculated to obtain a best separation condition. $C_{18}$ HPLC column and water/methanol/acetic acid mixture(90/10/0.2) were used for separation of guanine and cytosine. HPLC parameters(resolution and number of theoretical plate) were calculated under different flow rates and sample concentrations. Aspen chromatography simulation and HPLC experimental results were compared with fair agreement.

Study on the Separation and Determination of Pure Rare Earth Oxides by Anion Exchange Resin (음이온 교환수지에 의한 고순도 희토류산화물의 분리 및 정량에 관한 연구)

  • Cha, Gi Won;Ham, Yun Beom
    • Journal of the Korean Chemical Society
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    • v.34 no.6
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    • pp.606-615
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    • 1990
  • The purity of CeO$_2$, Sm$_2$O$^{3+}$ and La2O$^{3+}$ have been determinated by separating the impurity of rare earth-elements in those oxides with anion exchange resin and measuring the absorbance of the separated element with MTB. 1 ml of the mixture solution containing each 1 mg/ml of Y$^{3+}$, Yb$^{3+}$, Eu$^{3+}$, Sm$^{3+}$, Nd$^{3+}$, Pr$^{3+}$, Ce$^{4+}$and La$^{3+}$ is loaded in top layer of anion exchange resin column, Amberlite CG400 and separated with the mixture solution of the various concentration of methyl alcohol and nitric acid as an eluent. Using the result, the impure rare earth elements in pure CeO$_2$, Sm$_2$O$^{3+}$ and La$_2$O$^{3+}$ are determinated.

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Separation of Goid, Palladium and Platinum in Chromite by Anion Exchange Chromatography for Inductively Coupled Plasma Atomic Emission Spectrometric Analysis

  • Choe, Gwang Sun;Lee, Chang Hyeon;Park, Yeong Jae;Jo, Gi Su;Kim, Won Ho
    • 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.

The Application of Ion Chromatographic Method for Bioavailability and Stability Test of Iron Preparations

  • Kim, Young-Ok;Chung, Hye-Joo;Kong, Hak-Soo;Choi, Dong-Woong;Cho, Dae-Hyun
    • 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.

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A Simple and Effective Purification Method for Removal of U(VI) from Soil-Flushing Effluent Using Precipitation: Distillation Process for Clearance

  • Hyun-Kyu Lee;Ilgook Kim;In-Ho Yoon;Wooshin Park;Seeun Chang;Hongrae Jeon;Sungbin Park
    • 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.

Determination of 3-phenoxybenzoic Acid in Urine and Exposure Assessment of Pyrethroid Insecticides to Human Being (요중 3-phenoxybenzoic acid 미량 분석 및 pyrethroid계 살포자 노출 평가)

  • Seo, Jong-Chul;Song, Jae-Seok;Choi, Hong-Soon
    • The Korean Journal of Pesticide Science
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    • v.11 no.2
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    • pp.87-94
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    • 2007
  • Pyrethroid insecticide have widely been used for agricultural sector and residential environments. To assess the exposure of insecticide which is absorbed through skin the analysis of urinary metabolite is essential. At present, the urinary 3-PBA was analyzed using liquid-phase extraction. But LPE have many limitations, such as long pre-treatment time and low recovery. So, this study was conducted to determine the optimum conditions for analysing 3-PBA in urine using solid phase extraction. Furthermore, this study intend to investigate the relation of concentrations of pyrethroid, deltamethrin in air and 3-PBA in urine. The optimum condition for hydrolysis was found to be done with hydrochloric acid for one hour. The recovery rates of 3-PBA were $84.6%{\pm}1.2%$, $54.8{\pm}0.9%$, $99.8{\pm}1.2%$ with XAD-2, XAD-7, XAD-16 using as the aborbents and acetone as eluents respectively. But acetonitrle and methanol gave low recovery rate and methyl cellosolve could not elute the compound. The amount of acetone for elution were 6mL, 9mL, 3mL for XAD-2, XAD-7, XAD-16 as absorbents respectively. The non-absorbed rates was $0.8{\pm}0.5%$, and $0.7{\pm}0.3%$ under XAD-16, mesh size 140-200, amount of resin 1.4g and the flow rate of eluent was 0.1mL/min. In the concentration process, we obtained 11 times higher concentration of material. The amounts of urinary 3-PBA were. The LODs of 3-PBA and deltamethrin were 0.004 mg/L, 0.038 mg/L, respectively. The further research of minute monitoring which include spray pattern, environmental condition is needed And more research about the relation between total pyrethroid exposure and urinary various metabolite are also necessary.

Preparation of $Gal^3Man_4(6^3-mono-{\alpha}-D-galacto-pyranosyl-{\beta}-mannotetraose)$ by Bacillus sp. ${\beta}-mannanase$ and Growth Activity to Intestinal Bacteria (Bacillus sp.유래 ${\beta}-mannanase$에 의한 $Gal^3Man_4(6^3-mono-{\alpha}-D-galacto-pyranosyl-{\beta}-mannotetraose)$ 조제 및 장내세균에 대한 생육활성)

  • Kim, Sang-Woo;Park, Gwi-Gun
    • Applied Biological Chemistry
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    • v.47 no.4
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    • pp.379-383
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    • 2004
  • For the elucidation of substrate specificity to the brown copra meal by Bacillus sp. ${\beta}-mannanase.$, the enzymatic hydrolysate after 24 hr of reaction was heated in a boiling water bath for 10 min, and then centrifuged to remove the insoluble materials from hydrolysates. The major hydrolysates composed of D.P 5 and 7 galactosyl mannooligosaccharides. For the separate of galactosyl mannooligosaccharides, the supernatant solution of 150 ml was put on a first activated carbon column. The column was then washed with 5 l of water to remove mannose and salts. The oligosaccharides in the column were eluted by a liner gradient of $0{\sim}30%$ ethanol, at the flow rate of 250 ml per hour. The sugar composition in each fraction tubes was examined by TLC and FACE analysis. The combined fraction from F3 was concentrated to 30 ml by vacuum evaporator. Then put on a second activated carbon column. The oligosaccharides in the column were eluted by a liner gradient of $0{\sim}30%$ ethanol (total volume: 5 l), at the flow rate of 250 ml per hour. The eluent was collected in 8 ml fraction tubes, and the total sugar concentration was measured by method of phenol-sulfuric acid. The major component of F2 separated by 2nd activated carbon column chromatography were identified $Gal^3Man_4(6^3-mono-{\alpha}-D-galactopyranosyl-{\beta}-mannotetraose)$. To investigate the effects of brown copra meal galactomannooligosaccharides on growth of Bifidobacterium longum, B. bifidum were cultivated individually on the modified-MRS medium containing carbon source such as $Gal^3Man_4$, compared to those of standard MRS medium.

Isolation of Alliin in Garlic and Its Quantitative Determination by High Performance Liquid Chromatography and Studies on the Antimicrobial Efforts of Alliin and Ethanol Extracts from Korean Garlic(Alliium sativum L.) (마늘 중 고속 액체 크로마토그래피에 의한 알린의 분리 및 정량과 Alliin과 에탄올 추출물의 항균효과에 관한 연구)

  • 위성언
    • The Korean Journal of Food And Nutrition
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    • v.16 no.4
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    • pp.296-302
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    • 2003
  • First. the purification and analysis of alliin in garlic from different origins by alliin-HPLC determination method were studied. Allinase in garlic was inactivated by heating in boiling water followed by extraction of alliin in garlic with 80% methanol. To remove free amino acids and alliin homologs in garlic, garlic extract was separated by cation exchange column which was packed with amberlite CG-120 resin using 40L d-water as eluent. Alliin in garlic extract was crystallized in a mixture of acetone (50$^{\circ}C$):H$_2$O:acetic acid=70:29:1 and then recrystallized in a mixture of acetone (50$^{\circ}C$):H$_2$O:acetic acid=75:24:1. Obtained alliin was identified by melting point. TLC, microscope observation and mass spectrometry. High performance liquid chromatography (HPLC) following pre-column derivatization of cystein derivatives with o-phthaldialdehyde/2-mercaptoethanol has succeessfully been applied to the analysis of various garlics. Each alliic of standard solution and garlic extract was derivatized to isoindole derivative by o-phthaldialdehyde /2-mercaptoethanol and then analyzed by HPLC. Six point calibration was done by using alliin peak area. Lineality was observed at 0 ∼ 1.0mg/ml of alliin concentration. Weighted regression line function was Y=6254X - 256077. By this function, alliin contents in various garlics were 0.34 ∼ 0.73% fresh weight. Second study was designed to evaluate the effects of garlic extracts of various concentrations on the growth of various pathogenes (Eubacterium limonsum, Bacteroides fragilis, Salmonella typhimurium, Salmonella typhi, Shigella sonnei, Kiebsiella pneumoniae, Enterobacter cloacae, Pserdomonas aeruginosa, Escherichia coli). For antimicrobial effects against microorganism, totally minimal inhibition concentrations (MIC) of alliin were from 5,000 to 20,000ppm. MIC of ethanol extract were 1,250 to 10,000ppm.

Studies on the Separation and Preconcentration of Metal Ions by XAD-16-[4-(2-thiazolylazo)] orcinol Chelating Resin (XAD-16-[4-(2-thiazolylazo)]orcinol 킬레이트 수지에 의한 금속이온의 분리 및 농축에 관한 연구)

  • Lee, Won;Seol, Kyung-Mi;An, Hye-Sook;Lee, Chang-Heon;Lim, Jae-Hee
    • Analytical Science and Technology
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    • v.10 no.4
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    • pp.282-290
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    • 1997
  • The sorption and desorption properties of U(VI), Th(IV), Zr(IV), Cu(II), Pb(II), Ni(II), Zn(II), Cd(II) and Mn(II) ions on XAD-16-[4-(2-thiazolylazo)orcinol] (TAO) chelating resin were studied by elution method. The effect was examined with respect to overall capacity of each metal ion, separation of mixed metal ions, flow rate and concentration of buffer solution for optimum condition of sorption. The overall capacities of some metal ions on this chelating resin were 0.35nmol U(VI)/g resin, 0.49nmol Th(IV)/g resin, 0.41nmol Cu(II)/g resin, and 0.31nmol Zr(IV)/g resin, respectively. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 5.0 was Th(IV)>Cu(II)>U(VI)>Zr(IV)>Pb(II)>Ni(II)>Zn(II)>Mn(II)>Cd(II). The group separation of mixed metal ions was possible by increasing pH in pH range 2~5 at a flow rate of 0.28mL/min. Characteristics of desorption were investigated with desorption agents such as $HNO_3$, HCl, $HClO_4$, $H_2SO_4$, and $Na_2CO_3$. It was found that 2M $HNO_3$ showed high desorption efficiency to most of metal ions except Zr(IV) ion. Also, desorption and recovery of Zr(IV) ion were successfully performed with 1M $H_2SO_4$. Recovery of trace amount of U(VI) ion from artificial sea water was over 94%. The chelating resin, XAD-16-TAO was successfully applied to group separation of rare earth metal ions from U(VI) by using 2M $HNO_3$ as an eluent.

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