CN1252010A - 填充色谱颗粒层空间的方法 - Google Patents

填充色谱颗粒层空间的方法 Download PDF

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Publication number
CN1252010A
CN1252010A CN98804059A CN98804059A CN1252010A CN 1252010 A CN1252010 A CN 1252010A CN 98804059 A CN98804059 A CN 98804059A CN 98804059 A CN98804059 A CN 98804059A CN 1252010 A CN1252010 A CN 1252010A
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space
stratum granulosum
liquid
slip ring
suspension
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A·普赖尔
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Prior Separation Technology GmbH
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Prior Separation Technology GmbH
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
    • B01D15/206—Packing or coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/18—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
    • B01D15/1892—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns the sorbent material moving as a whole, e.g. continuous annular chromatography, true moving beds
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/50—Conditioning of the sorbent material or stationary liquid
    • G01N30/56—Packing methods or coating methods
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/50—Conditioning of the sorbent material or stationary liquid
    • G01N30/56—Packing methods or coating methods
    • G01N2030/562—Packing methods or coating methods packing
    • G01N2030/565—Packing methods or coating methods packing slurry packing

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

本发明涉及填充环状色谱中颗粒层空间的方法。所说的方法特征为颗粒材料是在加压下以液体中悬浮物的形式进料的,并且层中颗粒空间最好以间歇的方式被振动。

Description

填充色谱颗粒层空间的方法
本发明涉及一种用填料填充环状色谱颗粒层空间的方法。
在环状色谱中颗粒层应该是各向同性的以达到径迹的尖锐分离，即应有相同的堆积密度，换言之，每单位体积中应存在相同的颗粒数目。为达到可能的重现性，需要进行所谓紧密装填，即尽可能使颗粒紧密并置不留空隙，而不管颗粒的形状。
按照本发明，这可以通过在加压下以在液体中的悬浮物的形式引入颗粒材料，并振动、最好间歇地振动颗粒层空间来达到。
为此，悬浮物可以均匀的方式沿着整个颗粒层空间的周围引入，或在沿周围的一个或一些选定的地点引入，在后面两种情况下可以更快(对一个引入点)或更慢(对一些引入点)地旋转颗粒空间。
振动可通过应用一个或一些振荡装置，例如电磁振荡子或音频发生器来产生。在环形色谱被旋转的装填方法中，最好是在振动过程中颗粒层空间的旋转运动被与旋转方向相同和相反的往返运动所替代。
在振动时最好不要中断悬浮物的引入过程，同时振动的频率和持续时间应适应于颗粒悬浮物的情况。
振动或往返运动的频率最好高至约2.5千赫，具体为10赫兹至1.5千赫，同时物质的惯性当然会是往返运动的一个限制因素。对角度运动程度也是这样，它应小于30°，最好是1至15°。
装填以这样的方式开始，即这时颗粒层空间应被液体所充满。在填充时由于颗粒层变得愈来愈高，流动的阻力增加，在优选的操作方式中，为达到均匀的层密度，应使用具有恒定颗粒级分的悬浮物并把悬浮物以控制的方式强迫进料。换言之，无论反压力的大小，每单位时间应引入恒定的体积。
在环状色谱的颗粒层空间是用与液体接触时发生溶胀的材料来填充的情况下，用于颗粒材料的悬浮液体应该是在其中不发生溶胀的液体，最好是能引起这种颗粒材料收缩的液体。
依赖于颗粒层所需的渗透性，决定了可以允许发生收缩的程度，因为当颗粒层空间被填充后颗粒膨胀时颗粒会变形并使间隙减小。
在带有经滑动环回收洗脱液装置的环状色谱的情况下，滑动环可以在填充过程中从颗粒层空间移开，也可以和它一起运动，从而使振动操作不产生损耗。

Claims (9)

1.把填料填充到环状色谱中颗粒层空间的方法，其特征为这种颗粒材料是在加压下以在液体中悬浮物的形式引入的，并且颗粒空间最好间歇地振动。
2.权利要求1的方法，其特征为在振动过程中颗粒层空间的旋转运动被与旋转方向相同和相反的往返运动所代替。
3.权利要求1或2的方法，其特征为振动或往返运动发生的频率为至高约2.5千赫，优选10赫兹到1.5千赫。
4.权利要求2或3的方法，其特征为往返运动发生的角度范围小于30°，优选1至15°。
5.权利要求1至4中之一的方法，其特征为在开始填充过程前颗粒层空间是保持被液体所充满的。
6.权利要求1至5中之一的方法，其特征为在使用可溶胀颗粒材料的情况下要使用一种在其中不发生溶胀的液体，最好是一种可引起颗粒材料收缩的液体。
7.权利要求1至6中之一的方法，其特征为使用具有恒定颗粒级分的悬浮物，并强迫悬浮物以可控制的方式进料以达到均匀的层密度。
8.权利要求1至7中之一的方法，其特征为在带有经滑动环回收洗脱液装置的环状色谱的情况下，在填充过程中滑动环被从颗粒层空间移开。
9.权利要求1至7中之一的方法，其特征为在带有经滑动环回收洗脱液装置的环状色谱的情况下，在填充过程中滑动环与颗粒层空间一起运动。
CN98804059A 1997-12-10 1998-12-10 填充色谱颗粒层空间的方法 Pending CN1252010A (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ATGM768/97 1997-12-10
AT76897 1997-12-10

Publications (1)

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CN1252010A true CN1252010A (zh) 2000-05-03

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CN98804059A Pending CN1252010A (zh) 1997-12-10 1998-12-10 填充色谱颗粒层空间的方法

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EP (1) EP0961647A1 (zh)
JP (1) JP2001511070A (zh)
CN (1) CN1252010A (zh)
AU (1) AU1474899A (zh)
BR (1) BR9807208A (zh)
CA (1) CA2279944A1 (zh)
EA (1) EA199900731A1 (zh)
WO (1) WO1999029389A1 (zh)

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1457273A (en) * 1973-05-23 1976-12-01 Wellcome Found Column packing device
US4175037A (en) * 1978-04-10 1979-11-20 Whatman Inc. Process for packing chromatographic columns
DE2943982A1 (de) * 1979-10-31 1981-05-14 Josef E. Dipl.-Chem. 5000 Köln Moch Verbesserte drehvorrichtung zum gleichmaessigen packen von chromatographiesaeulen mit dextrangelen
US4305275A (en) * 1980-05-27 1981-12-15 Applied Plastics Co., Inc. Chromatographic apparatus and method of operation
FR2533836B1 (fr) * 1982-10-05 1988-01-22 Elf Aquitaine Procede et dispositif de remplissage de colonnes chromatographiques
WO1991014490A1 (en) * 1990-03-29 1991-10-03 Ht Chemicals Inc. Slurry compressor, apparatus for guiding compressor, and method for packing slurry in column
JPH08145973A (ja) * 1994-11-18 1996-06-07 Mitsui Eng & Shipbuild Co Ltd 円環クロマト装置の樹脂充填装置及び充填方法

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EP0961647A1 (de) 1999-12-08
AU1474899A (en) 1999-06-28
JP2001511070A (ja) 2001-08-07
EA199900731A1 (ru) 2000-02-28
WO1999029389A1 (de) 1999-06-17
BR9807208A (pt) 2000-05-23
CA2279944A1 (en) 1999-06-17

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