• Title/Summary/Keyword: methanol separation column

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Burnup Measurement of Irradiated Uranium Dioxide Fuel by Chemical Methods (화학적 방법에 의한 핵연료의 연소도 측정)

  • Kim, Jung-Suk;Han, Sun-Ho;Suh, Moo-Yul;Joe, Kih-Soo;Eom, Tae-Yoon
    • Nuclear Engineering and Technology
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    • v.21 no.4
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    • pp.277-286
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    • 1989
  • Destructive methods are used for the turnup determination of an irradiated PWR fuel. One of the methods includes U, Pu, Nd-148 and Nd-(145+146) determination by an isotope dilution mass spectrometry using triple spikes (U-233, Pu-242 and Nd-150). The method involves two sequential ion exchange resin separation procedures. Pu is eluted from the first anion exchange resin column (Dowex AG 1$\times$8) with 12 M HCl-0.1 M HI mixed solution, followed by U elution with 0.1 M HCl. Nd is isolated from other fission products on the second anion exchange resin column (Dowex AG 1$\times$4) with a nitric acid-methanol eluent. Each fraction is analysed by thermal ionization mass spectrometry. The difference between Nd-148 and Nd-(145+146) method is found with an average 2.07%. The results are compared with those by the heavy element method using U and Pu isotopes and by the destructive y-spectrometric measurement of Cs-137. The dependences of isotope composition of U and Pu on burn-up, and correlation between those isotopes are illustrated graphically.

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Isolation and Characterization of Allelopathic Substances from Sorghum Stem (수수 줄기에 함유(含有)된 타감물질(他感物質)의 분리(分離) 및 특성(特性) 구명(究明))

  • Kim, S.Y.;De Datta, S.K.;Robles, R.P.;Kim, K.U.;Lee, S.C.;Shin, D.H.
    • Korean Journal of Weed Science
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    • v.14 no.2
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    • pp.156-162
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    • 1994
  • To better understand the exact nature of the major toxic compound responsible for phytotoxicity of sorghum stem, the most toxic compound from the stem extract was isolated by rapid chromatography and subsequently purified by thin-layer chromatography(TLC) and high pressure liquid chromatography(HPLC). Of the eight fractions isolated by rapid chromatography, the fraction with solvent combinations of butanol (8) : acetic acid (1) : water (1) had the highest toxicity. Further separation of the fraction by TLC in a solvent mixture of butanol (24) : acetic acid (16.4) : water (7) : propanol (1) showed that the spot with an $R_f$ 0.71 had one major peak with retention time of 20.40 minutes. Upon subjecting gas chromatography and the HPLC fraction to the mass spectrometry, the toxic compound is probably one of the four compounds ; 1-methyl-1-(2-propynyl)-hydrazine, 1-aziridineethanol, 5-chloro-2-pentanone, and 2-(methylseleno)-ethanamine.

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A Study on the Separation of Neodymium from the Simulated Solution of $U_3Si/Al$ Spent Nuclear Fuel (모의 사용후분산핵연료($U_3Si/Al$) 용해용액으로부터 네오디뮴 분리에 관한 연구)

  • Choi, Kwang Soon;Kim, Jung Suk;Han, Sun Ho;Park, Soon Dal;Park, Yeong Jae;Joe, Kih Soo;Kim, Won Ho
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.584-591
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    • 2000
  • The separation of Nd from the simulated $U_3Si/Al$ spent fuel solution with sequential two-step anion exchange separation has been studied. To prepare the simulated $U_3Si/Al$ spent nuclear fuel, unirradiated $U_3Si/Al$ whose composition consists of small $U_3Si$ particle dispersed in an Al matrix with Al cladding was dissolved with a mixture of 4 M HCl and 10 M $HNO_3$ and 8 or 15 fission product elements were added to the dissolved solution. The trace amount of silica in the solutions was removed by evaporating to dryness with HF and the U was adsorbed on the first anion exchange resin. Neodymium can be purely isolated from the fission product elements with a methanol-nitric acid eluent using the second anion exchange resin. A large excess of Al didn't influence on the elution velocity of Nd, but reduced the eluted contents of Nd, Al, Eu, Gd, Sm and Sr, A large amount of Al was removed first from the column with 3 mL of loading solution (0.8 M $HNO_3$/99.8% MeOH) before Nd elution by the eluent [0.04 M $HNO_3$-99.8% MeOH(1:9)]. The recovery of Nd was more than 94%, regardless of Al contents. Taking the 9 to 13 mL fraction of eluate was effective to purely isolate Nd.

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Study of the Separation and Elution Behavior of Phenols as Priority Pollutants in Reversed Phase Liquid Chromatography (역상 액체 크로마토그래피에서 유기오염물질로서의 페놀류들의 분리 및 용리거동에 관한 연구)

  • Dai Woon Lee;Sun Kyung Lee;Keun Sung Yook;Won Lee
    • Journal of the Korean Chemical Society
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    • v.33 no.3
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    • pp.287-294
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    • 1989
  • The optimum condition for the separation of priority pollutant phenols using isocratic elution has been determined. The elution behavior of eleven phenols has been also studied to interpret the retention. The reversed phase liquid chromatographic methods were performed on a ${\mu}$-Bondapak $C_{18}$ column with methanol-water, acetonitrile-water, and THF water mixtures as mobile phases. The COF method, where Snyder's solvent triangle concept was combined with a mixture-design statistical technique, was used to optimize the strength and selectivity of solvents for the separation of phenols. The optimum solvent composition, which gives a complete separation of eleven phenols, was found to be $MeOH:ACN:H_2O$ = 7:40:53. The plots of ln k' vs. -${\Delta}H^{\circ}$ and ${\Sigma}{\pi}$ of phenols showed relatively good linearities. Effect of van der Waals volume, pi-energy and hydrogen bonding on the retention of phenols were investigated. The following equation with the correlation coefficient of 0.9927 for ACN-water solvent system was obtained; $log^{k'}=2.515{\times}10^{-2}VWV-1.301{\times}10^{-1}E-3.674{\times}10^{-1}$

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A Study on the Development of Analytical Methods and Behaviors of Environmental Pollutants(III) : On-Line System for Preconcentration and Separation of Trace Phenols by HPLC (환경 오염물질의 정량법 개발과 거동에 관한 연구(III) : 미량 페놀류의 HPLC 정량을 위한 온 라인 농축)

  • Lee, Dai Woon;Kim, Jin Young;Park, Young Hun;Moon, Myeong Hee
    • Analytical Science and Technology
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    • v.7 no.1
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    • pp.33-39
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    • 1994
  • The purpose on this study was to develop a new improved chromatographic method for determination of trace phenols from environmental waste water. The research was carried out with selected 8 phenols, and solid-phase extraction was employed as sample pretreatment method. The coupling of XAD-4 and Dowex $1{\times}8$ resin as preconcentration column increased the selectivities toward interferences coexisted in matrix. Automation was accomplished with on-line process of pretreatment and HPLC system. After elution of sample through XAD-4 column, phenols were adsorbed by dispersion force, then displaced from it by ACN basified, simultaneously and selectively readsorbed via anion exchange on Dowex $1{\times}8$. Dowex $1{\times}8$ column was washed by water. Phenols readsorbed were removed from Dowex $1{\times}8$ column by a minimum volumn of methanol containing HCl. Each pretreatment step was connected by switching valves and the eluate was directly on-line injected to obtain fast and reliable results into the HPLC. Recovery of phenols was greater than 90%. To examine utility of this method, analysis of phenols from laboratory waste water sample which was added some organic pollutants to find with phenols on environmental waste water were also accomplished without their interference effects.

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Polyacetylene Compounds from Panax ginseng C.A. Meyer (인삼의 Polyacetylene 화합물)

  • Shim Sang Chul;Chang Suk-Ku
    • Proceedings of the Ginseng society Conference
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    • 1988.08a
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    • pp.122-128
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    • 1988
  • Several major polyacetylene compounds were isolated from the petroleum-ether fraction of fresh Korean ginseng roots through solvent fractionation. partition and silica gel column chromatography. Further separation of acetylenic compounds was accomplished by bonded normal phase HPLC utilizing a moderately nonpolar microparticulate column. The preparative separation for the various spectral measurements was carried out by low pressure preparative liquid chromatography. The chemical structure of these polyacetylenes separated was determined by UV. IR/FTIR. $^{1}H$ NMR. mass spectral and elemental analysis. These are identified to be heptadeca-1-en-4.6-diyn-3.9.l0.-triol [1] heptadeca-1.9-dien-4.6-diyn-3-ol. heptadeca-1.8-dien-4.6-diyn-3.10-diol and the 4th was denatured polyacetylene. heptadeca-1.4-dien-6.8-diyn-3.10-diol. Two different p-substituted benzoates of panaxynol were synthesized for the determination of exciton chirality. The circular dichroism spectra in the UV region show that panaxynol p-bromobenzoate and p-dimethyl-aminobenzoate constitute negative exciton chirality [2]. Isolated major polyacetylene compounds were irradiated in aerated solution with 300 nm UV light to obtain the oxidized product at the allylic alcohol center to corresponding carbonyl compounds such as heptadeca-1-en-4.6-diyn-9.10-diol-3-one and heptadeca-1.9-dien-4.6-diyn-3-one. These photooxidation compounds have en-on-diyne chromophore and undergo nucleophilic addition reaction with methanol to yield ${\beta}-methoxy$ carbonyl compounds such as heptadeca-9-en-4.6-diyn-1-methoxy-3-one and heptadeca-4.6-diyn-1-methoxy-9.10-diol-3-one.

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Impurities formed from ethanol fermentation process among different materials and it′s effective separation in large scale (대규모의 주정발효 과정에서 생성된 불순물과 그 효율적 분리)

  • 류병호;김운식;남기두;이인기;하미숙
    • Microbiology and Biotechnology Letters
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    • v.14 no.5
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    • pp.371-376
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    • 1986
  • This study to elucidate concentrations of impurities such as methanol and fusel oil formed during fermentation process among the different materials and has been applied technical seperation for processing improvement by continuous distillation of super-allospas type. Methanol was formed high concentrations of cutting dried sweet potato and tapioca in order among the different materials during fermentation process. n-Propanol oil was formed high concentration of rice, cutting dried sweet potato, corn, naked barley and tapioca in order among the those materials. I-Buthanol showed high concentration of tapioca, corn, rice, cutting dried sweet potato and naked barley in order and isoamyl-alcohol showed high concentration of tapioca, rice, cutting dried sweet potato, corn and naked barley in order. Using the continuous distillation of super-allospas type, the following are collection ratios of n-propanol, iso-butanol, n-butanol and iso-amylalcohol: 37.9%, 28.6%, 37.4%, and 56.1% when 78.25% (v/v), 68.54% (viv), 50.0% (viv), and 50.0% (v/v) alcohol are used, respectively. Fusel oil and bad alcohol put into the recovery column and then seperated directly by side cut of fusel oil partially from plate of tower bottom after concentration again. Extra impurities seperated by fusel oil seperator when 20 % (v/v) alcohol adjusted with water.

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Influence of Ionic Liquid for Separation of D-tryptophan and N-CBZ-D-phenylalanine (D-tryptophan과 N-CBZ-D-phenylalanine의 분리에서 이온성 액체의 영향)

  • Jin, Yinzhe;Zheng, Jinzhu;Polyakova, Yulia;Koo, Yoon Mo;Row, Kyung Ho
    • Korean Chemical Engineering Research
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    • v.44 no.5
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    • pp.453-459
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    • 2006
  • D-tryptophan and N-CBZ-D-phenylalanine were separated using ionic liquid as additives for the mobile phase in high performance liquid chromatography (HPLC). The ionic liquid of 1-butyl-3- methylimidazolium tetrafluoroborate (${[BMIm]}^+{[BF_4]}^-$) was used. Mobile phases were 65%, 70%, and 80% methanol in water with addition of different concentrations (0.5, 1.0, 1.5, 2.0, 4.0, 6.0, 8.0, 10.0, 12.0, and 15.0 mmol/L) of the ionic liquid. The experiments were performed on stainless steel column, $3.9{\times}300mm$ i.d., packed with $15{\mu}m$ octadecyl-bonded silica gel at laboratory.The retention factor of D-tryptophan was not negligibly changed while that of N-CBZ-D-phenylalanine was decreased. The resolution between the two components were affected by the contents of methanol and ionic liquid in the mobile phase. With the small content of methanol and the high concentration of ionic liquid, the resolution was improved.

Differential Effects of Resveratrol and its Oligomers Isolated from Seeds of Paeonia lactiflora (Peony) on Proliferation of MCF-7 and ROS 17/2.8 Cells

  • Kim, Hyo-Jin;Lee, Won-Jung;Park, Yun-Hee;Cho, Sung-Hee;Park, Sang-Won
    • Preventive Nutrition and Food Science
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    • v.8 no.4
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    • pp.356-364
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    • 2003
  • A methanol extract from seeds of Paeonia lactiflora (Paeoniaceae, peony) was found to possess different antiproliferative activities against four different human cancer cell lines: Hela, MCF-7, HepG2 and HT-29. Furthermore, five different methanol (20, 40, 60, 80 and 100 % MeOH) fractions obtained by fractionation of the methanol extract of the seeds on a Diaion HP-20 column exhibited differential antiproliferative effects against the above four cancer cell lines. Among five fractions, the 60 % MeOH fraction showed relatively lower antiproliferative activity on MCF-7 estrogen-sensitive breast cancer cell than the other cancer cell lines. Systematic separation of 60% the MeOH fraction by silica gel and Sephadex LH-20 columns led to the isolation of four known stilbenes, trans-resveratrol (1), trans-(+)- $\varepsilon$ -viniferin (2), gnetin H (3) and suffruticosol B (4). The four stilbenes (1∼4) exerted differential biphasic effects on cell proliferation of MCF-7 cells in a similar manner as genistein, a soybean isoflavone used as a positive reference, in the concentration range from 1.0 to 200 $\mu$M. Three stilbenes (1 ∼ 3) weakly stimulated the proliferation of MCF -7 cells at doses below 10 JIM. However, strong antiproliferative effects on MCF-7 cell were exerted by extract 1 at a dose of 200 JIM, and by 2 and 3 at doses above 25 $\mu$M. In contrast, 4 inhibited the proliferation of MCF-7 cell at a dose below 25 $\mu$M, but stimulated cell proliferation at concentrations of 50 and 100 $\mu$M. All four stilbenes (1∼4) stimulated the proliferation of ROS 17/2.8 osteoblast-like cells in the range of 10$^{-10}$ ∼10$^{-1}$ $\mu$M. Compound 1 exhibited especially potent proliferative activity, although its activity was weaker than that of genistein. Additionally, three resveratrol oligomers (2∼4) also exhibited concentration-dependently moderate proliferative activity, but less than that of 1. These results suggest that resveratrol, and its dimer and trimers from the seeds of Paeonia lactiflora may act as a phytoestrogen, but in a somewhat different manner from that of genistein.

Characteristics of Nitrite Scavenger Derived from Seeds of Cassia tora L. (결명자 추출물의 아질산염 소거인자의 특성)

  • Park, Yeung-Beom;Lee, Tae-Gee;Kim, Oi-Kyung;Do, Jeong-Ryong;Yeo, Saeng-Gyu;Park, Yeung-Ho;Kim, Seon-Bong
    • Korean Journal of Food Science and Technology
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    • v.27 no.1
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    • pp.124-128
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    • 1995
  • The present study was conducted to elucidate nitrite scavenger derived from seeds of Cassia tora L. Methanolic extract of Cassia tora L was refractionated into ethyl ether, chloroform, ethyl acetate and water farction, and nitrite scavenging abilities of these fractions were investigated. Among these fractions, ethyl acetate fraction had the strongest nitrite scavenging ability(97%/2 mg). Therefore, to further investigate nitrite scavenger, ethyl acetate fraction was fractionated by silica gel column chromatography with a chloroform-methanol($10:0{\sim}0:10$) and then compound A and B were isolated. Compound A had a stronger nitrite-scavenging effect than compound B. Therefore the further separation of compound A was carried out by HPLC(32% acetonitrile. 1 ml/min) using ${\mu}Bondapak$C18 column$(3.9{\times}300 mm)$ and finally compound A-1 was obtained from compound A. Compound A-1 had by far nitrite-scavenging ability as compared with that of ascorbic acid. Compound A-1 was identified as $nor-rubrofusarin-6-{\beta}-mono-D-glucoside$ from the profiles of UV, IR and $^1H-NMR$.

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