• Title/Summary/Keyword: XAD-4

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Study on Characterization of Hydrophilic and Hydrophobic Fractions of Water-soluble Organic Carbon with a XAD Resin (XAD 수지에 의한 친수성 및 소수성 수용성 유기탄소의 특성조사)

  • Jeong, Jae-Uk;Kim, Ja-Hyun;Park, Seung-Shik;Moon, Kwang-Joo;Lee, Seok-Jo
    • Journal of Korean Society for Atmospheric Environment
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    • v.27 no.3
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    • pp.337-346
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    • 2011
  • 24-hr integrated measurements of water-soluble organic carbon (WSOC) in PM2.5 were made between May 5 and September 25, 2010, on a six-day interval basis, at the Metropolitan Area Air Pollution Monitoring Supersite. A macro-porous XAD7HP resin was used to separate hydrophilic and hydrophobic WSOC. Compounds that penetrate the XAD7HP column are referred to hydrophilic WSOC, while those retained by the column are defined as hydrophobic WSOC. Laboratory calibrations using organic standards suggest that hydrophilic WSOC includes lowmolecular aliphatic dicarboxylic acids and carbonyls with less than 4 or 5 carbons, amines, and saccharides. While the hydrophobic WSOC is composed of compounds of aliphatic dicarboxylic acids with carbon numbers larger than 4~5, phenols, aromatic acids, cyclic acid, and humic-like Suwannee River fulvic acid. Over the entire study period, total WSOC accounted for on average 48% of OC, ranging from 32 to 65%, and hydrophilic WSOC accounted for on average 30.5% (9.3~66.7%) of the total WSOC. Based on the previous results, our measurement result suggests that significant amounts of hydrophobic WSOC during the study period were probably from primary combustion sources. However, on June 9 when 1-hr highest ozone concentration of 130 ppb was observed, WSOC to OC was 0.61, driven by increases in the hydrophilic WSOC. This result also suggests that processes, such as secondary organic aerosol formation, produce significant levels of hydrophilic WSOC compounds that add substantially to the fine particle fraction of the organic aerosol.

Liquid Chromatographic Separation of Salicylic Acid and Its Derivatives Using Amberlite XAD-Copolymers (Amberlite XAD-공중합체를 이용한 살리실산 및 크로마토그래피적 분리 그 유도체들의 액체)

  • Yong Soon Chung;Taik Hyuk Lee;Young Ja Moon;Dai Woon Lee
    • Journal of the Korean Chemical Society
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    • v.33 no.1
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    • pp.70-81
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    • 1989
  • Reverse phase liquid chromatographic elution behaviors of salicylic acid and its derivatives were studied with classical and modern high-performance liquid chromatography(HPLC) using Amberlite XAD-4 and XAD-7 resin packed columns. Capacity factors(k') were determined in the comparatively high concentration(from 0. 010F to 0. 150F) of ferric nitrate-50% methanol solution to elucidate the elution behaviors with classical method. On the other hand, k's were measured in the various concentrations of methanol and ferric nitrate(from $2.5{\times}10^{-4}F\;to\;1.0{\times}10^{-3}F$) solution of pH 2. 25 and 293K with HPLC to explain the elution mechanism of them, and to find their optimum separation condition. As a result, it was found that log k's of salicylic acid and its derivatives were decreased with increasing the concentration of ferric ion, and the decreasing slopes of the compounds on the increasing ferric ion concentrations were related with each stability constant of ferric salicylates. Some isomers of derivatives of salicylic acid could be separated in the optimum condition.

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Selective Separation and Determination of Iron with Ion-Exchange Resins (이온교환수지에 의한 철의 선택적 분리 및 정량)

  • Yong Soon Chung;Dong Won Kim;Seung Ho Kim;Dai Woon Lee
    • Journal of the Korean Chemical Society
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    • v.31 no.1
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    • pp.45-54
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    • 1987
  • Dowex 1-X8 resin ion exchanged with calcon carboxylic acid (CCA-Dowex 1-X8) and 2-methyl-8-hydroxyquinoline(MHQ) impregnated-Amberlite XAD-4 resin (MHQ-XAD-4) were examined for the separation and preconcentration of ferric ion from the various matrices. The stabilities of these resins were investigated, and their capacities on ferric ion were also measured. The effect of pH on the adsorption of ferric ion and matrix ions, such as Al(Ⅲ) and Ca(Ⅱ), was investigated to determine the optimun pH ranges. Separation and preconcentration of iron in aluminium foil and mineral water samples were studied by elution method with these resin columns. The recovered ions by 10ml of 2F nitric acid was determined by flame atomic spectrophotometry. SP-Sephadex C-25 column was used to separate ferrous and ferric ion in mineral water by stepwise elution with ferrozine and 1 % ascorbic acid-ferrozine solution. The concentrated and separated each ion could be determined spectrophotometrically at the analytical wavelenth of Fe(Ⅱ)-ferrozine complex (562nm).

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Oxidative Decomposition of 2, 4, 6-Trichlorophenol Catalyzed by Polymer Supported Metalloporphyins (고분자결합 금속포르피린을 촉매로 한 2, 4, 6-트리클로로페놀의 산화 분해반응)

  • Park, Hye-Ok;Lee, Bo-Young;Rhee Paeng, Insook
    • Analytical Science and Technology
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    • v.14 no.1
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    • pp.72-79
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    • 2001
  • Oxidative decomposition of 2, 4, 6-trichlorophenol(TCP) was studied in aqueous solution. Iron and manganese protoporphyrin [or tetrakis(p-carboxyphenylporphyrin)] and their polymer supported derivatives were used as catalysts, and $KHSO_5$ and tert-butyldroperoxide(TBHP) as oxidants. Metalloporphyrin itself shows very poor catalytic activity in oxidative decomposition of TCP with oxidant. However, very high catalytic activity was observed when metalloporphyrin was chemically bound to newly synthesized polymers or XAD2 resin. Additionally, it revealed much higher catalytic activity in the presence of water-soluble polymers having a electron-donating axial ligand such as pyridine and immidazole. Maleic acid and chloromaleic acid were found in the resulting solution by ESI-MS. Especially, XAD2-supported metalloporphyrins can be reused as catalysts due to insolubility to solvent, and stability against oxidant.

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Furfural Production and Recovery by Two-stage Acid Treatment of Lignocellulosic Biomass (Two-stage 산 처리에 의한 목질계 바이오매스로부터 푸르푸랄 생산과 회수)

  • Shin, Gyeong-Jin;Jeong, So-Yeon;Lee, Hong-Joo;Lee, Jae-Won
    • Journal of the Korean Wood Science and Technology
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    • v.43 no.1
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    • pp.76-85
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    • 2015
  • In this study, we investigated optimal reaction conditions for furfural production from lignocellulosic biomass by two-stage acid treatment. Furfural produced by this method was recovered using XAD-4 resin. Oxalic and sulfuric acid were used as catalysts for the first stage of treatment. The concentration of xylose in the hydrolysate obtained from the first stage was $18.86g/{\ell}$ with oxalic acid and $19.35g/{\ell}$ with sulfuric acid. The concentration of oligosaccharide was relatively high when sulfuric acid was used. Maximum yield of furfural, that is, 55.10% ($6.71g/{\ell}$), was obtained when oxalic acid was used for the first stage and $0.1m{\ell}$ of sulfuric acid was used for the second stage of treatment for 90 min. Furfural production yield increased with increasing the reaction time. Most of the furfural produced by this two-stage treatment method was recovered using XAD-4 resin.

Solid-Phase Extraction of L-Muscone from Aqueous Samples with Amberlite XAD-4 for Gas Chromatographic Assay

  • Paik, Man-Jeong;Kim, Kyoung-Rae
    • Archives of Pharmacal Research
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    • v.27 no.5
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    • pp.539-543
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    • 2004
  • An efficient analytical method was devised for the accurate L-muscone assay in aqueous samples. It involves solid-phase extraction of L-muscone in adsorption mode using XAD-4 as the sorbent and dichloromethane modified with 10% (v/v) methanol as the eluting solvent. The gas chromatographic analysis of the eluate residue dissolved in toluene on a DB-5MS capillary column provided complete resolution of L-muscone from the co-extracted interferences. The overall method showed excellent linearity ($r^2{\geq}$ 0.9994) in the range of 0.1 to 2.0 $\mu\textrm{g}$/mL with good intra- and inter-day precisions (% RSD = 2.5~7.3) and with high extraction recovery rates ($\geq$ 98.1 %). When the present method was applied to a L-muscone herbal drink product, the within-batch RE (%) in the labeled concentration (1.5 $\mu\textrm{g}$/mL) for the three randomly chosen bottles were -2.4, -1.3 and -3.3 with high precision (% RSD $\leq$ 3.1). The present method is considered to be suitable for quality control evaluation on liquid drinks and other complex formulations fortified with L-muscone.

Organic Compounds in the Nak Dong River and Its Toxicity (낙동강 수질중 유기물질과 독성)

  • 류병호;심종환;최진택;조현철;정종순
    • Journal of Environmental Health Sciences
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    • v.20 no.1
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    • pp.39-53
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    • 1994
  • This study aims to investigate organic compounds and its toxicity by Ames test and chromosomal aberration in the water of the Nak Dong River. Six sampling sites such as Goryung, Hagueun, Maelie, Duksan, Haedong and Myungiang were selected for these pur15oses. 200 l water samples were absorbed on XAD-2 resin columns (2.5X30cm), eluted with organic solvents mixture of acetone: cyclohexane and then dried under vacuum condition. The extracts from the XAD-2 resin was injected into GC/MS and 184 organic compounds were identified such as aldehydes, aromatic compounds, ketones, phenols, hydrocarbons, alcohols, carboxylic acids, alkanes and some unknowns. The US EPA priority pollutants such as naphthlene, bis(2-ethylhexyl)phthalate and other pollutants, 1,2-diethyl benzene, 1,2,3,4-tetrahydronaphthalene and cyclohexanol were detected in these samples. The concentration of chemical pollutants such as 1,2-diethyl benzene, nephthalene, 1,2,3,4-tetrahydronaphthalene, bis(2-ethylhexyl)phthalate and cyclohexanol were ranged into 1.228 $\mu$g/l, 298 $\mu$g/l, 30.191 $\mu$g/l, 1.147 $\mu$g/l and 2.839 $\mu$g/l, respectively. The mutagenic activity of XAD-2 extracts were tested on Salmonella typhimurium TA 98, TA 100, TA 1535 and TA 1537 and then exhibited strong mutagenic activity against S. typhimurium TA 98 and TA 100 in the presence of S$_9$. Amon them, bis(2-ethylhexyl)phtalate and 1,2-diethyl benzene showed the most strongest mutagenic activity against S. typhimurium TA 98 and TA 100 in the presence of S$_9$. On the other hands, chromosomal aberration of XAD-2 extracts in the human blood cells were not occurred by the sampling water at Goryung, Hagueun, Maelie and Duksan, Chromosomal aberration were also not occurred by the each concentration of 0.05, 0.1 amd 0.3 mg/l of each 1,2-diethyl benzol, bis(2-ethylhexyl)phthalate, naphthalene, phenol, cyclohexanol and benzothiazol test solution.

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Studies on the Selective Separation and Preconcentration of Cr(VI) Ion by XAD-16-Chromotropic Acid Chelating Resin (XAD-16-Chromotropic Acid 킬레이트 수지에 의한 몇 가지 금속이온의 선택적 분리 및 농축에 관한 연구)

  • Lee, Won;Lee, Chang-Youl;Kim, Mi-Kyoung;Kim, In-Whan
    • Analytical Science and Technology
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    • v.17 no.3
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    • pp.199-210
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    • 2004
  • A new polystyrene-divinylbenzene chelating resin containing 4,5-dihydroxy-naphthalene-2,7-disulfonic acid (chromotropic acid : CTA) as functional group has been synthesized and characterized. The sorption and desorption properties of this chelating resin for Cr(III) ion and Cr(VI) ion including nine metal bloodstain. As a results, FOB test kit could be effectively applied to identification of human blood at chelating resin was stable in acidic and alkaline solution. The Cr(VI) ion is selectively separated from Cr (III) ion at pH 2 and the maximum sorption capacity of Cr(VI) ion is 1.2 mmol/g. In the presence of anions such as $F^-$, $SO{_4}^{2-}$, $CN^-$, $CH_3COO^-$, $NO{_3}^-$, the sorption of Cr(VI) ion was reduced but anions such as $PO{_4}^{3-}$ and $Cl^-$ revealed no interference effect. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 2 was Cr(VI)>Sn(II)>Fe(III)>Cu(II)>Cd(II)${\simeq}Pb(II){\simeq}Cr(III){\simeq}Mn(II){\simeq}Ni(II){\simeq}Al(III)$. Desorption characteristics for Cr(VI) ion was investigated with desorption agents such as $HNO_3$, HCl, and $H_2SO_4$. It was found that the ion showed high desorption efficiency with 3 M HCl. As the result, the chelating resin, XAD-16-CTA was successfully applied to separation and preconcentration of Cr (VI) ion from several metal ions in metal finishing works.

Separation of Fission Product Elements from Synthetic Dissolver Solutions of Spent Pressurized Water Reactor Fuels by $TBP/XAD-16/HNO_3$Extraction Chromatography ($TBP/XAD-16/HNO_3$추출 크로마토그래피에 의한 모의 사용후핵연료 용해용액 중 미량 핵분열생성물 원소의 분리)

  • Lee, Chang Heon;Choi, Kwang Soon;Kim, Jung Suk;Choi, Ke Chon;Jee, Kwang Yong;Kim, Won Ho
    • Journal of the Korean Chemical Society
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    • v.45 no.4
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    • pp.304-311
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    • 2001
  • A study has been carried out on the extraction chromatographic separation of fission products from spent pressurized water reactor (PWR) fuels for inductively coupled plasma atomic emission spectrometric analysis. Impregnation capacity of tri-n-butyl phosphate (TBP), which is well known as an extractant in the field of uranium separation from various nuclear grade materials, on Amberlite XAD polymeric macroporous support materials was measured. Amberlite XAD-16 of which the surface area is the highest was selected as a support material because its TBP impregnation capacity was the largest in Amberlite XADs. Sorption behaviour of this TBP impregnated resin was investigated for the fission product elements using acidic solutions simulated for dissolver solutions of spent PWR fuels. The parameters affecting the performance of the separation system were optimized. The fission product elements studied excluding Pd and Ru were quantitatively recovered with the precision of less than 3.1%.

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수돗물 중 강력한 돌연변이유발물질인 MX에 대한 분석

  • 권오영;김희갑
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2002.10a
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    • pp.153-153
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    • 2002
  • 수돗물의 염소소독 과정에서 부식질의 초기 분해생성물인 MX(Mutagen X)는 수돗물의 전체 돌연변이유발성의 최고 60%까지 차지하는 것으로 알려져 있다. 그러나 존재하는 농도는 수 ng/L로 정량분석을 위해서는 resin을 사용하여 10 ~ 20L의 물을 농축하여야 한다. 이 연구에서 MX의 농축에 사용된 resin은 XAD-4와 XAD-7HP의 1:1 mixture이었으며, 사용 전에 Soxhlet extractor를 사용하여 ethyl acetate와 methanol로 각각 12시간씩 세척하였다. 15L의 물 시료는 37%의 염산으로 pH 2에 맞춘 후 직경 2cm의 유리관에 15cm의 높이로 채워진 resin을 40mL/min의 유속으로 통과시켰다. 유리관에 잔류하는 물은 질소가스로 대부분 불어 제거한 후 ethyl acetate 200mL를 가해 1mL/min의 유속으로 흘려주어 MX를 용출시킨 후 회전증발기로 5mL의 부피까지 농축시키고 10% H$_2$SO$_4$ in MeOH 0.1mL를 가하여 6$0^{\circ}C$에서 methyl ester화하였다. 과포화된 $Na_2$SO$_4$ 수용액 0.3ml를 가한 후 MTBE 0.3mL로 추출하고 GC/ECD로 분석하였다. MX의 회수율은 60% 이상이었으며 일부수돗물 시료에 대해 분석하였다.

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