• Title/Summary/Keyword: solvent extractions

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Comparison of Static and Dynamic Solvent Extraction of Polychlorinated Dibenzofurans from Fly Ash

  • Yang, Jeong Soo;Jeong, Jang Hwan;Yu, Euy Kyung
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.295-301
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    • 2004
  • In this study, static and dynamic solvent extractions are compared for more efficient extraction of polychlorinated dibenzofurans (PCDFs) from fly ash. Static solvent extraction rather than dynamic extraction showed a higher recovery of PCDFs, which was adsorbed strongly with fly ash. The effects of parameters, such as temperature, toluene-isopropyl alcohol mixture, static and dynamic time flow rate, and solvent volume on the extraction were investigated and the variations in average recoveries of PCDFs were explained. In both extractions, temperature was an effective parameter because the higher temperature gave the higher recoveries. In dynamic solvent extraction, dynamic time was more effective than flow rate and solvent volume for the extraction of PCDFs from fly ash. Multi-layer column chromatography on neutral and acidic silica gel with n-hexane was used for cleaning up the extracts. The quantification of the PCDFs extracted was performed using HPLC-UV.

Introduction of Modifying Solvents to Carbon Dioxide in Supercritical Extractions

  • 이정미정;David J. Chesney
    • Bulletin of the Korean Chemical Society
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    • v.19 no.12
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    • pp.1351-1355
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    • 1998
  • A simple apparatus for adding a modifying solvent to supercritical CO2 extractant was described. Small, fixed volumes (typically 100 μL) of liquid modifying solvents were delivered during the extraction process by use of an in-line high pressure loop injector and an air pump. Without disconnecting the extraction cell from the supercritical fluid extraction system, the modifying solvent was repeatedly delivered. The solvent modification device was optimized during the extraction of carbaryl and bis(acetylacetonato) copper(Ⅱ). Extraction recoveries from spiked filter paper and soil samples ranged between 22% and 109%, depending on the analyte and matrix components. The addition of polar modifying solvents were necessary to improve the extractability of the nonpolar CO2.

Analytical Method for Dioxin and Organo-Chlorinated Compounds: (Ⅱ) Comparison and Extraction Methods of Dioxins from XAD-2 Adsorbent

  • 양정수;이성광;박영훈;이대운
    • Bulletin of the Korean Chemical Society
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    • v.20 no.6
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    • pp.689-695
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    • 1999
  • Supercritical fluid extraction (SFE), ultrasonic extraction (USE), and accelerated solvent extraction (ASE) were compared with the well known Soxhlet extraction for the extraction of polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins(PCDDs) from the XAD-2 resin which was used to adsorb PCDDs in the atmosphere. XAD-2 resin spiked with five PCDDs was chosen as a sample. The optimum conditions for the extraction of PCDDs by SFE were turned out to be the use of CO2 modified with 10% toluene at 100 ℃ and 350 atm, with 5 min static extraction followed by 20 min dynamic extraction. SFE gave a good extraction rate with good reproducibility for PCDDs ranging from 68 to 98%. The ultrasonic extraction of PCDDs from XAD-2 was investigated and compared with other extractions. A probe type method was compared with a bath type. Two extraction solvents, toluene and acetone were compared with their mixture. The use of their mixture in probe type, with 9 minutes of extraction time, was found to be the optimum condition. The average recovery of the five PCDDs for USE was 82-93%. Accelerated solvent extraction (ASE) with a liquid solvent, a new technique for sample preparation, was performed under elevated temperatures and pressures. The effect of tem-perature on the efficiency of ASE was investigated. The extraction time for a 10 g sample was less than 15 min, when the organic solvent was n-hexaneacetone mixture (1 : 1, v/v). Using ASE, the average recoveries of five PCDDs ranged from 90 to 103%. SFE, USE, and ASE were faster and less laborious than Soxhlet extraction. The former three methods required less solvent than Soxhlet extraction. SFE required no concentration of the solvent extracts. SFE and ASE failed to perform simultaneous parallel extractions because of instrumental limitations.

The Comparative Study of Anti-inflammation and Anti-oxidation in Accodance with Extraction Solvents of Jeondo-san (전도산(顚倒散)의 추출용매에 따른 항염 및 항산화 비교 연구)

  • Seo, Hyung-Sik
    • The Journal of Korean Medicine Ophthalmology and Otolaryngology and Dermatology
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    • v.23 no.2
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    • pp.69-80
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    • 2010
  • Objective : The purpose of this study was to compare anti-Inflammation and anti-oxidation of Jeondo-San(JDS) extracted with two kinds of solvents, ethanol and water. Methods : Two kinds of JDS extractions were prepared 20, 50, $100\;{\mu}g/mg$. The Cytotoxicity was measured by MTT assay in Raw 264.7 cell. The anti-inflammation effects were measured by inhibitory efficacy on $PGE_2$, NO, TNF-$\alpha$, COX-2 and iNOS in Raw 264.7 cell. The anti-oxidation effects were measured by ROS inhibitory efficacy, intracellular GSH synthesis and DPPH Radical scavenging in HaCaT cell. Results : 1. All of JDS extraction groups had no cytotoxicity in Raw 264.7 cell. 2. All of JDS extraction groups showed significantly inhibitory effect on production of $PGE_2$. Inhibitory efficacy increased in accodance with concentration. 3. All of JDS extraction groups showed significantly inhibitory effect on production of NO. Inhibitory efficacy increased in accodance with concentration. 4. All of JDS extraction groups did not show significantly inhibitory effect on production of TNF-$\alpha$. 5. $100\;{\mu}g/ml$ JDS extracted with ethanol and $50\;{\mu}g/ml$, $100\;{\mu}g/ml$ JDS extracted with water showed inhibitory effect on iNOS expression. 6. All of JDS extraction groups showed significantly inhibitory effect on production of ROS. Inhibitory efficacy increased in accodance with concentration. Ethanol extractions were better than water extractions. 7. $100\;{\mu}g/ml$ JDS extracted with ethanol only produced GSH of $32{\pm}5.2%$. 8. All of JDS extraction groups showed significantly scavenging effect of DPPH radicals. Inhibitory efficacy increased in accodance with concentration. Ethanol extractions were better than water extractions. Conclusion : Two kinds of JDS extractions have not cytotoxicity and inhibit production of NO. JDS extracted with water was effective in anti-inflammation, JDS extracted with ethanol was effective in anti-oxidation.

Extraction Methods of Organic Components from Rubber Composites and Analysis of the Extract Using Gas Chromatography/Mass Spectrometry

  • Chae, Eunji;Choi, Sung-Seen
    • Elastomers and Composites
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    • v.54 no.3
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    • pp.188-200
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    • 2019
  • Rubber articles contain various organic additives such as antidegradants, curing agents, and processing aids. It is important to extract and analyze these organic additives. In this paper, various extraction methods of organic additives present in rubber composites were introduced (solvent extraction, Soxhlet extraction, headspace extraction, and solid-phase microextraction), and the extracts were characterized using gas chromatography/mass spectrometry (GC/MS). Solvent and Soxhlet extractions are easy-to-perform and commonly used methods. Efficiency of solvent extraction varies according to the type of solvent used and the extraction conditions. Soxhlet extraction requires a large volume of solvent. Headspace sampling is suitable for extracting volatile organic compounds, while solid-phase extraction is suitable for extracting specific chemicals. GC/MS is generally used for characterizing the extract of a rubber composite because most components of the extract are volatile and have low molecular weights. Identification methods of chemical structures of the components separated by GC column were also introduced.

Structure Optimization of Di-ionizable Calixarene Nano-baskets for Competitive Solvent Extraction of Alkali and Alkaline Earth Metals

  • Mokhtari, Bahram;Pourabdollah, Kobra
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.3855-3860
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    • 2011
  • The competitive solvent extractions of alkali and alkaline earth metals by di-ionizable calix[4]arene nano-baskets were studied using nine conformers of calix[4]arene nano-baskets. The objective of this work is to assess the variation of macrocycle conformation, orientation and position of pendant moieties upon the extraction parameters (efficiency, selectivity and $pH_{1/2}$) of the complexes. The results revealed that alternation of ring conformation in calixarene scaffold affects the solvent extraction parameters towards alkali and alkaline earth metals, while changing the orientation of pendant moieties from ortho- to para- as well as cis- to trans-analogues depicted no changes in those extraction parameters.

Competitive Solvent Extractions of Alkaline Earth Metal Cations by Crown Ether Phosphonic Acid Monoethyl Esters (크라운에테르 포스포닉산 모노에틸 에스테르에 의한 알칼리 토금속 양이온의 경쟁 용매추출)

  • Chung, Yeong-Jin
    • Journal of the Korean Applied Science and Technology
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    • v.22 no.1
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    • pp.9-14
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    • 2005
  • Competitive solvent extraction of alkaline earth metal cations from water into organic solvent containing the carboxylic acid crown ether and analogous crown ether phosphonic acid monoethyl esters were investigated. sym-(n-Decyldibenzo)-16-crown-5xyacetic acid $\underline{1}$ and monoethyl sym-(n-decyldibenzo)-16-crown-5-oxymethylphosphonic acid $\underline{3}$ are structurally identical except for the ionizable groups. Both of them provide similar extraction behavior in terms of efficiency and selectivity, but monoethyl sym-(n-decyldibenzo)-16-crown-5-oxymethylphosphonic acid $\underline{3}$ showed higher alkaline earth metals loadings at acidic or neutral media. Monoethylsym-(n-octyldibenzo)-16-rown-5-oxymethylphosphonic acid $\underline{2}$ showed better selectivity and alkaline earth metals loading than did the analogous sym-(n-octyldibenzo)-16-crown-5-oxymethyldiphosphonic acid $\underline{6}$.

Solvent-free determination of BTEX in water using repetitive membrane extraction followed by GC-MS (반복적인 막 추출과 GC-MS를 이용한 물 중 BTEX의 분석)

  • Kim, He-Kap;Kim, Se-Young;Lee, Soo-Hyung
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.352-359
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    • 2011
  • An analytical method for solvent-free determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using repetitive membrane extractions coupled to cryofocusing and GC-MS was derived. BTEX compounds that permeated through a nonporous silicone membrane from the aqueous phase and evaporated into the acceptor phase were purged into a cryofocusing trap ($-100^{\circ}C$) with helium gas. The BTEX compounds, thus enriched in the trap, were thermally desorbed into a capillary column GC and detected using an MS. The flow rate of the donor phase (30 mL water) was set at 10 mL/min, and membrane extractions, accomplished by returning the water drained from the extraction module to the sample container, were repeated three times at $20{\pm}2^{\circ}C$. Although recoveries (%) were variable, from the highest for benzene (approximately 80%) to the lowest for ethylbenzene and xylenes (3.5-10%), the method showed satisfactory precision (RSD 2.2-10%) with good-linearity calibration curves ($r^2$ 0.9976-0.9997 in 1-100 ${\mu}g$/L range) for all of the compounds. The method detection limits (MDLs) ranged from 0.16 to 1.8 ${\mu}g$/L. The results showed the method's advantages such as short analysis time and overall simplicity without solvent compared to the conventional techniques.

Solvent Extractions of Alkali Metal Cations and Alkaline Earth Cations by Ionizable Crown Ether Phosphonic Acids (이온성 크라운에테르 포스포닉산에 의한 알칼리 금속 양이온과 알칼리 토금속 양이온의 용매추출)

  • Chung, Yeong-Jin
    • Journal of the Korean Applied Science and Technology
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    • v.22 no.1
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    • pp.50-55
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    • 2005
  • A comparison of alkali metal cation and alkaline earth cation solvent extraction was made for three additional monoionizable crown ethers and one diionizable crown ether. sym-(n-Octyldibenzo)-16-crown-5-oxyacetic acid $\underline{1}$ exhibited high efficiency and selecvity in solvent extraction of alkali metal cations with respect to that observed with alkaline earth cations. Sizes of $Na^+$ and $Ca^{2+}$ appropriately match with the cavity size of monoethyl sym-bis[4(5)-tert-butylbenzo]-16-crown-5-oxymethylphosphonic acid $\underline{3}$. As the result, $Na^+$ and $Ca^{2+}$ are the best extracted. sym-(n-Octyldibenzo)-16-crown-5-oxymethyldiphosphonic acid $\underline{4}$was found to be somewhat selective for $Na^+$ over $Li^+$ and other alkaline earth metal cations. In the complexation of alklaine earth cations by crown ether diphosphonic acid $\underline{4}$, $Ca^{2+}$ and $Sr^{2+}$ are the appropriate sizes, but lager $Ba^{2+}$ may be due to favorable formation of a sandwich type complex between the crown ether cavity and the dianion of the deprotonated crown ether phoaphonic acid moiety.

Effect of Crown Ring Size and Upper Moiety on the Extraction of s-Block Metals by Ionizable Calixcrown Nano-baskets

  • Mokhtari, Bahram;Pourabdollah, Kobra
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.3979-3990
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    • 2011
  • Eight ionizable nano-baskets of cone 25,26-di(carboxymethoxy)calix[4]arene-crown-3,4,5,6 were synthesized and were verified by $^1H$ and $^{13}C$ NMR spectroscopy, IR spectroscopy and elemental analysis. The competitive solvent extractions of alkali and alkaline earth metal cations were studied using such nano-baskets. The novelty of this study is including three binding units of calixarene's bowl, crown ether's ring and electron-donor ionizable moieties in a unique scaffold to assess the binding tendency towards the cations. The objective of this work is to study the extraction efficiency, selectivity and $pH_{1/2}$ of such complexes. The result of solvent extraction experiments indicated that these compounds were effective extractants of alkali and alkaline earth metal cations. Their selectivities were greatly influenced by the acidity of solution and the conformations of the calixcrown. One conformer was selective to $Na^+$ in pH ${\geq}$ 4, while the other was highly selective to $Ba^{2+}$ in pH 6 and upper.