• Title/Summary/Keyword: column clean-up

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Comparative Study on the HPLC Determination of Aflatoxins Coupled with Extraction and Clean-up Methods (Aflatoxin 분석법에 관한연구;추출 및 정제방법의 비교)

  • 김종규
    • Journal of Food Hygiene and Safety
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    • v.8 no.4
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    • pp.251-254
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    • 1993
  • Extraction and Clean-up procedures coupled with quantitation by high performance liquid chromatography(HPLC) was evaluated for the detection of 4 aflatoxins, B1, B2, G1 and G2, in peanut butter. The Sep-pak clean-up method showed poorer separation and repeatability than did the modified DeVries' and an immunoaffinity column clean-up methods. No significant difference of detected aflatoxins between the affinity column clean-up and modified DeVries' method. The coefficients of variation for the 4 aflatoxins were ranging from 6.3∼32.3 by the modified DeVries' method and 5.3∼9.8 by the affinity column clean-up.

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The Effect of Partitioning Porous Plate on Bubble Behavior and Gas Hold-up in a Bench Scale (0.36 m × 22 m) Trayed Bubble Column (벤치스케일(0.36 m × 22 m) 다단형 기포탑에서 다공판이 기포의 거동 및 기체 체류량에 미치는 영향)

  • Yang, Jung Hoon;Hur, Young Gul;Lee, Ho-Tae;Yang, Jung-Il;Kim, Hak-Joo;Chun, Dong Hyun;Park, Ji Chan;Jung, Heon
    • Korean Chemical Engineering Research
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    • v.50 no.3
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    • pp.505-510
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    • 2012
  • The gas hold-up has a strong relationship with the size distribution and rising velocities of bubbles in a bubble column. Therefore, many previous researchers have studied on the hydrodynamics focusing on the bubble size variation in bubble column. In this study, the bubble behavior was influenced by partitioning porous plates installed at a certain height in a trayed bubble column. The gas hold-up was increased in non-sparging region (H/D > 5) as well as sparging region. We identified the effect of the partitioning porous plate using three trayed bubble columns with different reactor geometries. Furthermore, the bubble break-up frequency and size distribution were observed before and after individual bubbles penetrated through the plate. The arrangement of the plates was also investigated using a 0.15-m-in-diameter bubble column. Based on the result, we applied this design concept to a 0.36-m-in-diameter, 22 m tall trayed bubble column and identified the effect of the partitioning porous plate on the gas hold-up increase.

Column regeneration for Partisil/Partisphere ion-exchange columns (Partisil/Partisphere 이온 교환 컬럼 재생 가이드)

  • Mark Fever;Gemma Howse
    • FOCUS: LIFE SCIENCE
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    • no.1
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    • pp.5.1-5.3
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    • 2024
  • The document discusses the regeneration of Partisil/Partisphere ion-exchange columns in chromatography. It mentions that column efficiency can diminish with use due to the accumulation of sample and/or mobile phase impurities at the head of the column. This can lead to a change in back pressure, lower column efficiency, and sometimes a change in selectivity. The document outlines a procedure that may restore column performance. The document also provides everyday practices to enhance the lifetime of a column. These include using only high-purity HPLC solvents and buffers, using freshly prepared mobile phases and buffers, filtering mobile phases to remove particulates, using appropriate sample clean-up procedures, using a guard column or pre-column filter, and working within the pressure and flow rate limitations of the column. For the regeneration of Partisil/Partisphere SAX, SCX, WAX, and WCX columns, the document suggests passing 20 column volumes of various mobile phases through the column. These include a buffer wash, distilled water, an acid wash, a chelating wash, a methanol wash, and a buffer for separation. The document emphasizes that not all of these wash steps are required for every column clean-up and that some chromatographers require only a combination of certain steps.

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A Synthesis of Optically Active cis and trans 2-(5-Hydroxypoperidin-2-yl)acetates

  • P.N. Reddy;한상수;정교현
    • Bulletin of the Korean Chemical Society
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    • v.19 no.6
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    • pp.617-618
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBs) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

Analytical Method for Dioxin and Organo-Chlorinated Compounds : (I) Pretreatment of Milk Samples for Dioxin Analysis

  • 양정수;김진영;최용욱;이대운
    • Bulletin of the Korean Chemical Society
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    • v.19 no.6
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    • pp.619-624
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBS) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

Determination of Thiamin by Gas-chromatography (기체크로마토그래피법에 의한 티아민 분석)

  • Yoo, Ji-Sang;Moon, Dong-Cheul;Hong, Sung-Hwa;Han, Kun;Kim, Bak-Kwang
    • YAKHAK HOEJI
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    • v.33 no.3
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    • pp.156-160
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    • 1989
  • A gas-chromatographic determination method of thiamin which use a quantitative cleavage of thiamin to 4-methyl-5-(2-hydroxyethyl)thiazol [I] and solvent extraction of the analyte prior to GC injection was modified. A column chromatographic procedure using a reversed phase, high capacity solid phase cartridge was applied to the clean-up of the analyte. Thiazol derivative[I] was quantitatively recovered upon the column method. Acetanilide, an internal standard, has a good recovery through the analytical procedure. The method has analytical precision of 2% or less in the coefficient of variation.

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Clean-up of Contaminated Groundwater by Permeable Reactive Barrier (투수성 반응벽에 의한 오염지하수 복원효과 분석)

  • 정하익;김상근
    • Proceedings of the Korean Geotechical Society Conference
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    • 2000.03b
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    • pp.542-547
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    • 2000
  • It has become interested in the concept of permeable barriers for the containment and/or destruction of contaminated groundwater. The purpose of these trench-like barriers is to provide in situ capture and possibly destruction of the contaminant while preserving groundwater flow to uncontaminated zones. For instance, a trichloreethylene(TCE) plume may be contained by a permeable in which reactive iron reduces TCE to ethylene and ethane, compounds which can be easily biodegraded. The objective of this research is to examine the feasibility of using zero-valent iron as a clean-up media in permeable reactive barrier system. A series of laboratory column tests are performed. The concentration of influent and effluent water and the rate of clean up are analysed from these test results. The experimental result shows that the majority of the contamination in groundwater is removed in the reactor. And it shows the corresponding increase in the concentration of chloride ions through the reactor. Results from this study indicate that permeable reactive barrier containing admixtures of zero-valent iron and other materials can effectively clean up groundwater contaminated with organic compounds.

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폐기물 매립지 토양에서의 PCBs 분석법

  • Lee Jeong-Hwa;Jeon Chi-Wan;Jeong Yeong-Uk
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2005.04a
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    • pp.199-201
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    • 2005
  • This paper describes a simple procedure for the quantitative analysis of 7 PCBs (polychlorinated biphenyls) in soils on the waste reclaimed land, The procedure involved sample clean up using silicagel column, acetonitrile partition and sulfuric acid procedures. The instrumental technique is applied GC/PDD(gas chromatography/pulsed discharge detector) and GC/ECD(gas chromatography/electron capture detector). Concentration of $sub-{\mu}g/g$ level was attainable with 20g soils on the waste reclaimed land.

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An effective immunoaffinity clean-up method for multi-DDT residue analysis

  • Hong, Ji-Youn;Hong, Jee-Eun;Lee, Eun-Ah;Park, Song-Ja;Lho, Dong-Seok;Kim, Jong-Hyun;Choi, Myung-Ja
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.290.3-291
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    • 2003
  • To increase detection sensitivity for multi-DDT residues (o,p-/p,p-DDT, o,p-/p,p-DDE, o,o-/o,p-DDD) analysis, a highly selective sample clean-up method was introduced prior to GC/MS analysis using immunoaffinity column. The immunoaffinity matrix was prepared by coupling IgG fraction of DDT antiserum to cyanogens bromide activated Sepharose 4B. Three DDT antisera (DDA-1, DDHP-2, DDCP-3) were test for affinity column ligand that obtained by imunizing respective DDT immunogen to rabbits, and IgG was purified using protein A affinity purification. (omitted)

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Development of Analytical Method for Polychlorinated Biphenyls and Organochlorine Pesticides in Air (대기 중 PCBs와 유기염소계 살충제의 정량을 위한 분석 방법 개발)

  • 최민규;여현규;김태욱;천만영;선우영
    • Journal of Korean Society for Atmospheric Environment
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    • v.18 no.6
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    • pp.475-485
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    • 2002
  • An analytical method was investigated for the meaiiurement of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) concentrations in air samples. Procedures required for column chromatographic clean up. silicagel (stage I) and gel permeation chromatography (stage II), were discussed. Identification and quantification of PCBs and OCPs were performed using a combination of gas chromatography/mass spectrometry/ selected ion monitoring. Recovery tests calculated from six samples are 68∼137% for PCBs and 58∼130% for OCPs except for endrin aldehyde. Instrumental detection limits determined for the PCBs and OCPs varied from 0.05 to 0.18 pg/m3 and from 0.71 to 16.82 pg/㎥, respectively. The method has been applied to the analysis of air samples collected at Ansung city, Kyonggi province, Korea. This method may serve as a screening protocol for the simultaneous determination of PCBs and OCPs in air.