EP0961647A1 - Method for charging the particle bed space of a chromatograph - Google Patents

Method for charging the particle bed space of a chromatograph

Info

Publication number
EP0961647A1
EP0961647A1 EP98958722A EP98958722A EP0961647A1 EP 0961647 A1 EP0961647 A1 EP 0961647A1 EP 98958722 A EP98958722 A EP 98958722A EP 98958722 A EP98958722 A EP 98958722A EP 0961647 A1 EP0961647 A1 EP 0961647A1
Authority
EP
European Patent Office
Prior art keywords
particle
bed space
particle bed
suspension
slip ring
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP98958722A
Other languages
German (de)
French (fr)
Inventor
Adalbert Prior
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Prior Separation Technology GmbH
Original Assignee
Prior Separation Technology GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Prior Separation Technology GmbH filed Critical Prior Separation Technology GmbH
Publication of EP0961647A1 publication Critical patent/EP0961647A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • 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

Definitions

  • the invention relates to a method for loading the particle bed space of an annular chromatograph with a filling.
  • the particle bed in an annular chromatograph should be isotropic in order to achieve a sharp web separation, that is to say it should have the same bulk density, in other words the same number of particles per unit volume. This is only reproducibly possible as a so-called dense packing, that is to say the particles are packed tightly together without any gaps that are not conditional on the particle shape.
  • the particle material is introduced as a suspension in a liquid under pressure and the particle bed space is shaken, preferably intermittently.
  • the suspension can be introduced evenly over the entire circumference of the particle bed space or at one or more selected points on the circumference, with the particle space being rotated faster (one feed point) or slower (several feed points) in the latter two cases.
  • oscillating heads e.g. electromechanical vibrations or sound generators.
  • the suspension feed is preferably not interrupted during the shaking - the shaking frequency and the shaking times are matched to the particle suspension.
  • Shaking or reciprocating is preferably carried out at a frequency up to approximately 2.5 kHz, in particular at 10 Hz to 1.5 kHz, the limits of the back and forth movement being set by the inertia. This also applies to their angular range, which is below 30 °, preferably 1 -1 5 °.
  • the feed is started so that the particle bed space is kept filled with liquid.
  • the flow resistance increases due to the increasing particle bed, so that a preferred procedure consists in that a suspension with constant particle content is used to achieve a uniform bed density and the suspension is force-controlled controlled. In other words, a constant volume per unit time is loaded regardless of the back pressure.
  • the suspension liquid for the particle material should be one in which swelling does not occur, preferably a liquid which causes shrinkage of the particle material.
  • the slip ring In the case of an annular chromatograph with eluate removal via a slip ring, the slip ring is either sagged or moved together with the particle bed space during loading, so that no wear occurs during shaking.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (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)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The invention relates to a method for charging the space of a particle bed in an annular chromatograph. Said method is characterised in that the particulate material is fed as a suspension in a fluid under pressure and in that the bed particle space is vibrated, preferably in an intermittent manner.

Description

VERFAHREN ZUM BESCHICKEN DES TEILCHENBETTRAUMS EINES CHROMATOGRAPHENMETHOD FOR LOADING THE PARTICLE BED ROOM OF A CHROMATOGRAPH
Die Erfindung betrifft ein Verfahren zum Beschicken des Teilchenbettraums eines Annularchromatographen mit einer Füllung.The invention relates to a method for loading the particle bed space of an annular chromatograph with a filling.
Das Teilchenbett in einem Annularchromatographen sollte zur Erzielung einer scharfen Bahnentrennung isotrop sein, also die gleiche Schüttdichte aufweisen, mit anderen Worten sollten pro Volumseinheit gleich viele Teilchen vorliegen. Dies ist nur reproduzierbar möglich als sogenannte dichte Packung, also dichtes Aneinanderlagern der Teilchen möglichst ohne teilchenformnichtbedingte Zwischenräume.The particle bed in an annular chromatograph should be isotropic in order to achieve a sharp web separation, that is to say it should have the same bulk density, in other words the same number of particles per unit volume. This is only reproducibly possible as a so-called dense packing, that is to say the particles are packed tightly together without any gaps that are not conditional on the particle shape.
Erfindungsgemäß wird dies dadurch erzielt, daß das Teilchenmaterial als Suspension in einer Flüssigkeit unter Druck eingebracht und der Teilchenbettraum, vorzugsweise intermittierend, gerüttelt wird.This is achieved according to the invention in that the particle material is introduced as a suspension in a liquid under pressure and the particle bed space is shaken, preferably intermittently.
Dabei kann man die Suspension gleichmäßig über den gesamten Umfang des Teilchenbettraums einbringen oder an einer oder mehreren ausgewählten Stellen des Umfangs, wobei in den beiden letztgenannten Fällen der Teilchenraum schneller (eine Aufgabestelle) oder langsamer (mehrere Aufgabestellen) rotiert wird.The suspension can be introduced evenly over the entire circumference of the particle bed space or at one or more selected points on the circumference, with the particle space being rotated faster (one feed point) or slower (several feed points) in the latter two cases.
Gerüttelt kann durch Anlegen eines oder mehrerer Schwingköpfe von z.B. elektromechanischen Schwingen oder Schallgeneratoren erfolgen. Bei Beschickungen, wo der Annularchromatograph gedreht wird, ist bevorzugt, daß beim Rütteln eine Rotationsbewegung des Teilchenbettraums durch eine Hin- und Her-Bewegung in der und gegen die Rotationsrichtung abgelöst wird.Can be shaken by applying one or more oscillating heads of e.g. electromechanical vibrations or sound generators. In the case of feeds where the annular chromatograph is rotated, it is preferred that, when shaking, a rotational movement of the particle bed space is replaced by a back and forth movement in and against the direction of rotation.
Während des Rütteins wird die Suspensionszufuhr vorzugsweise nicht unterbrochen - die Rüttelfrequenz und die Rüttelzeiten werden auf die Teilchensuspension abgestimmt. Vorzugsweise wird mit einer Frequenz bis hinauf zu etwa 2,5 kHz, insbesondere bei 10 Hz bis 1 ,5 kHz gerüttelt bzw. hin- und herbewegt, wobei natürlich der Hin- und Herbewegung Grenzen durch die Massenträgheit gesetzt sind. Dies betrifft auch deren Winkelbereich, der unter 30°, vorzugsweise bei 1 -1 5° liegt.The suspension feed is preferably not interrupted during the shaking - the shaking frequency and the shaking times are matched to the particle suspension. Shaking or reciprocating is preferably carried out at a frequency up to approximately 2.5 kHz, in particular at 10 Hz to 1.5 kHz, the limits of the back and forth movement being set by the inertia. This also applies to their angular range, which is below 30 °, preferably 1 -1 5 °.
Die Beschickung wird so begonnen, daß der Teilchenbettraum mit Flüssigkeit gefüllt gehalten wird. Während des Beschickens steigt der Durchflußwiderstand infolge des höher werdenden Teilchenbetts an, sodaß eine bevorzugte Vorgangsweise darin besteht, daß zur Erzielung einheitlicher Bettdichte eine Suspension mit konstantem Teilchenanteil eingesetzt und die Suspension gesteuert zwangsgefördert wird. Mit anderen Worten wird unabhängig vom Gegendruck mit konstantem Volumen pro Zeiteinheit beschickt.The feed is started so that the particle bed space is kept filled with liquid. During loading, the flow resistance increases due to the increasing particle bed, so that a preferred procedure consists in that a suspension with constant particle content is used to achieve a uniform bed density and the suspension is force-controlled controlled. In other words, a constant volume per unit time is loaded regardless of the back pressure.
Im Falle der Teilchenbettraum des Annularchromatographen mit einem Material beschickt werden soll, das in Kontakt mit Flüssigkeiten aufquillt, sollte als die Suspensionsflüssigkeit für das Teilchenmaterial eine solche verwendet werden, in der Quellung nicht auftritt, vorzugsweise eine Flüssigkeit, die Schrumpfung des Teilchenmaterials verursacht.In the case of the particle bed space of the annular chromatograph to be charged with a material which swells in contact with liquids, the suspension liquid for the particle material should be one in which swelling does not occur, preferably a liquid which causes shrinkage of the particle material.
Wie stark diese Schrumpfung sein darf, hängt von der geforderten Durchlässigkeit des Teilchenbetts ab, da bei der Expansion der Teilchen nach Beschickung des Teilchenbettraums Teilchenverformung unter Zwischenraumverkleinerung auftritt.How much this shrinkage may be depends on the required permeability of the particle bed, since when the particles expand after the particle bed space has been charged, particle deformation occurs with a reduction in the gap.
Bei einem Annularchromatographen mit Eluatabnahme über einen Schleifring wird während der Beschickung der Schleifring gegenüber dem Teilchenbettraum entweder abgesackt oder zusammen mit ihm bewegt, sodaß beim Rütteln keine Abnützung auftritt. In the case of an annular chromatograph with eluate removal via a slip ring, the slip ring is either sagged or moved together with the particle bed space during loading, so that no wear occurs during shaking.

Claims

Ansprüche: Expectations:
1 . Verfahren zum Beschicken des Teilchenbettraums eines Annularchromatographen mit einer Füllung, dadurch gekennzeichnet, daß das Teilchenmaterial als Suspension in einer Flüssigkeit unter Druck eingebracht und der Teilchenbettraum, vorzugsweise intermittierend, gerüttelt wird.1 . A process for loading the particle bed space of an annular chromatograph with a filling, characterized in that the particle material is introduced as a suspension in a liquid under pressure and the particle bed space is shaken, preferably intermittently.
2. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, daß beim Rütteln eine Rotationsbewegung des Teilchenbettraums durch eine Hin- und Her-Bewegung in der und gegen die Rotationsrichtung abgelöst wird.2. The method according to claim 1, characterized in that when shaking a rotational movement of the particle bed space is replaced by a back and forth movement in and against the direction of rotation.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß mit einer Frequenz von bis hinauf zu etwa 2,5 kHz, vorzugsweise 10 Hz bis 1 ,5 kHz, gerüttelt bzw. hin- und herbewegt wird.3. The method according to claim 1 or 2, characterized in that with a frequency of up to about 2.5 kHz, preferably 10 Hz to 1.5 kHz, is shaken or moved back and forth.
4. Verfahren nach Anspruch 2 oder 3, dadurch gekennzeichnet, daß über einen Winkelbereich von unter 30°, vorzugsweise 1-15°, hin- und herbewegt wird.4. The method according to claim 2 or 3, characterized in that over an angular range of less than 30 °, preferably 1-15 °, is moved back and forth.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß vor dem Beginn des Beschickens der Teilchenbettraum mit Flüssigkeit gefüllt gehalten wird.5. The method according to any one of claims 1 to 4, characterized in that the particle bed space is kept filled with liquid before the start of loading.
6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß bei quellbarem Teilchenmaterial eine Flüssigkeit verwendet wird, in der Quellung nicht eintritt, vorzugsweise eine Flüssigkeit, die Schrumpfung des Teilchenmaterials verursacht.6. The method according to any one of claims 1 to 5, characterized in that in the case of swellable particle material, a liquid is used in which swelling does not occur, preferably a liquid which causes shrinkage of the particle material.
7. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß zur Erzielung einheitlicher Bettdichte eine Suspension mit konstantem Teilchenanteil eingesetzt und die Suspension gesteuert zwangsgefördert wird. 7. The method according to any one of claims 1 to 6, characterized in that a suspension with a constant particle content is used to achieve uniform bed density and the suspension is force-controlled controlled.
8. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß bei einem Annularchromatographen mit Schleifringeluatabnahme der Schleifring während des Beschickens gegenüber dem Teilchenbettraum abgesackt wird.8. The method according to any one of claims 1 to 7, characterized in that in an annular chromatograph with slip ring eluate decrease the slip ring is bagged against the particle bed space during loading.
9. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß bei einem Annularchromatographen mit Schleifringeluatabnahme der Schleifring während des Beschickens mit dem Teilchenbettraum mitbewegt wird. 9. The method according to any one of claims 1 to 7, characterized in that the slip ring is moved during loading with the particle bed space in an annular chromatograph with slip ring eluate.
EP98958722A 1997-12-10 1998-12-10 Method for charging the particle bed space of a chromatograph Withdrawn EP0961647A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT76897 1997-12-10
AT76897 1997-12-10
PCT/AT1998/000300 WO1999029389A1 (en) 1997-12-10 1998-12-10 Method for charging the particle bed space of a chromatograph

Publications (1)

Publication Number Publication Date
EP0961647A1 true EP0961647A1 (en) 1999-12-08

Family

ID=3499257

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98958722A Withdrawn EP0961647A1 (en) 1997-12-10 1998-12-10 Method for charging the particle bed space of a chromatograph

Country Status (8)

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

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 (en) * 1979-10-31 1981-05-14 Josef E. Dipl.-Chem. 5000 Köln Moch Filling of chromatography column with gel - where column is rotated by motor to ensure uniform packing, esp. when filling long column with dextran gel
US4305275A (en) * 1980-05-27 1981-12-15 Applied Plastics Co., Inc. Chromatographic apparatus and method of operation
FR2533836B1 (en) * 1982-10-05 1988-01-22 Elf Aquitaine METHOD AND DEVICE FOR FILLING CHROMATOGRAPHIC COLUMNS
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 (en) * 1994-11-18 1996-06-07 Mitsui Eng & Shipbuild Co Ltd Apparatus and method for filling resin of circular chromatograph

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9929389A1 *

Also Published As

Publication number Publication date
JP2001511070A (en) 2001-08-07
WO1999029389A1 (en) 1999-06-17
AU1474899A (en) 1999-06-28
CN1252010A (en) 2000-05-03
CA2279944A1 (en) 1999-06-17
BR9807208A (en) 2000-05-23
EA199900731A1 (en) 2000-02-28

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