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EP1064542A1 - Annular chromatograph - Google Patents

Annular chromatograph

Info

Publication number
EP1064542A1
EP1064542A1 EP99908668A EP99908668A EP1064542A1 EP 1064542 A1 EP1064542 A1 EP 1064542A1 EP 99908668 A EP99908668 A EP 99908668A EP 99908668 A EP99908668 A EP 99908668A EP 1064542 A1 EP1064542 A1 EP 1064542A1
Authority
EP
European Patent Office
Prior art keywords
annular chromatograph
cylinder jacket
cylinder
chromatograph according
annular
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Withdrawn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
EP99908668A
Other languages
German (de)
French (fr)
Inventor
Adalbert Prior
Jürgen Wolfgang
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 EP1064542A1 publication Critical patent/EP1064542A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • G01N30/58—Conditioning of the sorbent material or stationary liquid the sorbent moving as a whole
    • 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
    • G01N30/58—Conditioning of the sorbent material or stationary liquid the sorbent moving as a whole
    • G01N2030/582—Conditioning of the sorbent material or stationary liquid the sorbent moving as a whole micellar electrokinetic capillary chromatography [MECC]
    • 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
    • G01N30/58—Conditioning of the sorbent material or stationary liquid the sorbent moving as a whole
    • G01N2030/587—Continuous annular chromatography

Definitions

  • the invention relates to annular chromatographs with a particle bed rotating relative to a stationary base and a stationary feeder head with continuous feeder lines on a turntable with eluate discharges, which is formed between an inner cylinder and a cylinder jacket.
  • the task was to create an annular chromatograph construction that can be tailored to the tasks to be solved not only by selecting the suitable particle bed material / materials, but also constructively, in particular as regards the particle bed height but also the particle bed density.
  • This object is achieved according to the invention by a type of modular system, in which different, especially different height, inner cylinder / jacket cylinder pairs can be displaced relative to one another and / or used together.
  • a central column is provided on the turntable, onto which all components to be arranged above the turntable are threaded, so to speak.
  • An annular chromatograph according to the invention is accordingly primarily characterized in that a central column is provided on the turntable, which extends upwards through the feeder head and on which a clamping device for pressing the feeder head onto the cylinder jacket is arranged.
  • either the clamping device has spacer sleeves or the central column has extension pieces for adapting to cylinder jackets of different lengths.
  • the annular chromatograph according to the invention can easily be equipped with cylinder jackets of different heights.
  • cylinder sleeves that can be stacked on one another, preferably those with different inner diameters and / or inner cylinders
  • Composite bodies of this type preferably contain a fixed particle bed filling, in particular in the form of a porous matrix obtained by polymerizing prepolymer particles in contact with the inner cylinder and cylinder jacket.
  • a prefabricated matrix is easy to clean / rinse after use and is then reusable, which significantly reduces the need for particle bed material and the time required for numerous successive ring chromatographic separations, since the column does not need to be lulled again after each separation, a large one Number of separations can be carried out one after the other but in continuous operation and the conversion of the annular chromatograph to different particle bed materials can be carried out extremely quickly.
  • annular chromatographs In preferred annular chromatographs according to the invention, two or more concentric cylinder jackets can be provided, between each of which a particle bed is arranged, the turntable having corresponding rows of eluate drains.
  • a particularly preferred embodiment of the annular chromatograph according to the present invention has feeder head passages for the feeder lines, into which the feeder lines can be inserted and passed from the interior of the core / jacket arrangement.
  • An annular chromatograph according to the invention can additionally comprise a temperature control, for example by providing heat exchangers for eluents and / or feed, which in a preferred embodiment have an inner cylinder and / or cylinder. coat associated are provided. This enables the particle bed for the separation processes to be brought to a higher operating temperature or the heat released, if appropriate, by removal or desorption processes to be removed.
  • FIGS. 1 to 4 are each schematic side sectional views. 1 and 4 are overall views and FIGS. 2 and 3 are partial views of annular chromatographs according to the invention, the head construction of the annular chromatograph in FIGS. 1 and 2 being different from that in FIGS. 3 and 4.
  • a base plate 1 which e.g. can be screwed onto a laboratory table and in which a drive shaft 2 is rotatably mounted.
  • a turntable 3 is wedged onto the drive shaft 2 and has continuous eluate take-off channels along a circumference, below which a non-rotatable eluate receiving cup 5 is provided for the drive shaft 2 on the bearing connecting piece 4 formed integrally with the base plate 1.
  • a hollow cylinder 6 is bolted on as a jacket cylinder at 7, which has a retracted roof 8 which runs parallel to the turntable 3 in FIGS. 1 and 2 and which is connected via a ball bearing 9 to a feed sleeve 10 which is opposite in operation the base plate 1 does not move and is penetrated by supply channels to the interior of the hollow cylinder 6 for feed, eluate, for loading with particle bed material, etc., two of which are denoted by 1 1 and 12.
  • an inner cylinder 1 3 is plugged onto the drive shaft 2 and is seated on the turntable 3, with the hollow cylinder 6 and
  • the inner cylinder 1 3 has on the upper side facing away from the turntable 3 a roof with an upwardly directed guide flange 1 5, with which it sits on the drive shaft 2 and on which a coil spring 16 engages, which presses the inner cylinder 13 on the turntable 3
  • the abutment door spring 1 6 is a clamping sleeve 1 7, which is counter-screwed so far onto the drive shaft 2 that a rotary flange 18 of the clamping sleeve 1 7, which carries a ball bearing 1 9, with its free bearing ring on the feed sleeve 10, is conclusive There is thus a storage of the feed sleeve 10 both with respect to the roof 8 of the hollow cylinder 6 and with respect to the clamping sleeve 1 7, so that the feed sleeve 1 0 can be easily tested against the rotating parts of the annular chromatograph
  • each matched clamping sleeves 1 7, inner cylinder 1 3 and hollow cylinder 6 can be varied.
  • the particle bed space can be varied by coordinating the diameters of hollow cylinder 6 and inner cylinder 13
  • FIG. 3 which also relates to another head construction, it is shown by way of example that feed tubes 20 are guided through the feed channels, specifically from the interior of the annular chromatograph to the outside.
  • a distributor block 21 is screwed onto the feed sleeve 10, which has bores corresponding to the feed channels, which have shoulders for engaging an annular flange arranged at the end of the feed tube 20.
  • the feed tube 20 is pushed upwards into the distributor head until it is with its ring flange on the school
  • a sealing nipple 22 is screwed in, to which a distributor tube 24 is fastened via a knurled nut 23, which projects into the annular gap 14 between the hollow cylinder 6 and the inner cylinder 1 3 and ends above the particle bed (not shown).
  • the particle bed rotates relative to the distributor pipe 24.
  • a split plug 25 is used, which only has the purpose of centering the feed pipe 20.
  • With 26 a screw for venting the interior of the annular chromatograph is designated.
  • both the inner cylinder 13 and the hollow cylinder 6 are screwed onto the turntable from below.
  • Fig. 4 further shows a similar annular chromatograph construction to that in Fig. 3, however the drive shaft in this embodiment is made in two parts, the upper shaft part 2 'having a smaller diameter being pushed into the lower part 2 and being in the overlap region 27, e.g. via a screw or detent, is fixed to it.
  • the upper shaft part 2 ' can be inserted over a part of the total length of the shaft into the lower one, so that the length of the shaft can be adapted to different heights of the jacket cylinder / inner cylinder pairs 6, 1 3 and thus to different parti bed heights.
  • tempering liquid enters the lower part of the drive shaft 2 at the inlet connection 28 (arrow A), is guided inside the shaft to the connection 29, where it emerges from the shaft and into the interior of the inner cylinder 1 3 enters (arrow B) in order to maintain the temperature (heating or cooling) of the particle bed.
  • the further flow path takes place via outlet 30 out of the cylinder interior and again into the shaft - in this case in its upper part 2 '- (arrow C) until the bath liquid finally leaves the annular chromatograph at outlet port 31 (arrow D).
  • the temperature control liquid is preferably conducted in a closed circuit by passing it through a heat exchanger (not shown) at 31 and, at a corresponding temperature, entering the chromatograph again at 28

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (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)

Abstract

The invention relates to an annular chromatograph comprising a particle bed which rotates on a rotary plate (3), said plate having eluate drainage lines, with regard to a stationary base and a stationary feeder head (10) with continuous feeder lines. Said particle bed is configured between an inner cylinder (13) and a cylinder sleeve (6). The invention is characterized in that a central column (2) is provided on the rotary plate (3) and extends upwards and through the feeder head (10). In addition, a tightening device (16, 17) for pressing the feeder head (10) on the cylinder sleeve (6) is arranged on said column.

Description

AnnularchromatographAnnular chromatograph
Die Erfindung betrifft Annularchromatographen mit gegenüber einer stationären Basis und einem stationären Feederkopf mit durchgehenden Feederleitungen auf einem Drehteller mit Eluatableitungen rotierendem Teilchenbett, das zwischen einem Innenzylinder und einem Zylindermantel ausgebildet ist.The invention relates to annular chromatographs with a particle bed rotating relative to a stationary base and a stationary feeder head with continuous feeder lines on a turntable with eluate discharges, which is formed between an inner cylinder and a cylinder jacket.
Es bestand die Aufgabe, eine Annularchromatographen-Konstruktion zu schaffen, die auf die zu lösenden Aufgaben nicht nur durch Auswahl des/der geeigneten Teilchenbett- Materials/Materialien abstimmbar ist, sondern auch konstruktiv, insbesondere was die Teilchenbetthöhe, aber auch die Teilchenbettdichte betrifft.The task was to create an annular chromatograph construction that can be tailored to the tasks to be solved not only by selecting the suitable particle bed material / materials, but also constructively, in particular as regards the particle bed height but also the particle bed density.
Diese Aufgabe ist erfindungsgemäß durch eine Art Baukastensystem gelöst, bei dem verschiedene, vor allem verschieden hohe, Innenzylinder/Mantelzylinder-Paare gegeneinander verschiebbar und/oder zusammen verwendbar sind. Dazu wird eine Zentralsäule am Drehteller vorgesehen, auf die alle oberhalb des Drehtellers anzuordnenden Bauteile sozusagen aufgefädelt werden.This object is achieved according to the invention by a type of modular system, in which different, especially different height, inner cylinder / jacket cylinder pairs can be displaced relative to one another and / or used together. For this purpose, a central column is provided on the turntable, onto which all components to be arranged above the turntable are threaded, so to speak.
Ein erfindungsgemäßer Annularchromatograph ist dementsprechend vor allem dadurch gekennzeichnet, daß am Drehteller eine Zentralsäule vorgesehen ist, die sich nach oben bis durch den Feederkopf hindurch erstreckt und auf der eine Spannvorrichtung zum Andrücken des Feederkopfs an den Zylindermantel angeordnet ist.An annular chromatograph according to the invention is accordingly primarily characterized in that a central column is provided on the turntable, which extends upwards through the feeder head and on which a clamping device for pressing the feeder head onto the cylinder jacket is arranged.
In bevorzugten Ausführungsformen weist entweder die Spannvorrichtung Distanzhülsen oder aber die Zentralsäule Verlängerungsstücke zur Anpassung an Zylindermäntel verschiedener Länge auf. In beiden Fällen kann der erfindungsgemäße Annularchromatograph problemlos mit unterschiedlich hohen Zylindermänteln ausgerüstet werden.In preferred embodiments, either the clamping device has spacer sleeves or the central column has extension pieces for adapting to cylinder jackets of different lengths. In both cases, the annular chromatograph according to the invention can easily be equipped with cylinder jackets of different heights.
In einer weiteren bevorzugten Ausführungsform sind aufeinandersetzbare Zylindermäntel, vorzugsweise solche mit unterschiedlichen Innendurchmessern und/oder Innenzy-In a further preferred embodiment, cylinder sleeves that can be stacked on one another, preferably those with different inner diameters and / or inner cylinders
- 1 - Iinder/Zvlindermantel-Paare, die insbesondere als Verbundkorper ausgebildet sind, vorgesehen Dadurch können mehrere Teilchenbetten - übereinander bzw. einander umgebend - gleichzeitig zur chromatographischen Trennung herangezogen werden- 1 - Iinder / Zindlindermantel pairs, which are designed in particular as a composite, provided. This allows several particle beds - one above the other or surrounding each other - can be used simultaneously for the chromatographic separation
Derartige Verbundkorper enthalten vorzugsweise eine fixierte Teilchenbettfullung, insbesondere in Form einer durch Durchpolymeπsieren von Vorpolymerteilchen in Kontakt mit Innenzylinder und Zylindermantel erhaltenen porösen Matrix. Eine solche vorgefertigte Matrix ist nach Verwendung leicht zu reinigen/spulen und ist anschließend wiederverwendbar, was den Bedarf an Teilchenbettmateπal wie auch den zeitlichen Aufwand für zahlreiche aufeinanderfolgende annularchromatographische Trennungen erheblich senkt, da die Säule nicht nach jeder Trennung erneut gelullt zu werden braucht, eine große Anzahl von Trennungen nacheinander aber im kontinuierlichen Betrieb durchgeführt werden kann und die Umrüstung des Annularchromatographen auf unterschiedliche Teilchenbettmateπalien äußerst rasch vonstatten gehen kann.Composite bodies of this type preferably contain a fixed particle bed filling, in particular in the form of a porous matrix obtained by polymerizing prepolymer particles in contact with the inner cylinder and cylinder jacket. Such a prefabricated matrix is easy to clean / rinse after use and is then reusable, which significantly reduces the need for particle bed material and the time required for numerous successive ring chromatographic separations, since the column does not need to be lulled again after each separation, a large one Number of separations can be carried out one after the other but in continuous operation and the conversion of the annular chromatograph to different particle bed materials can be carried out extremely quickly.
In bevorzugten erfindungsgemaßen Annularchromatographen können zwei oder mehrere konzentrische Zylindermantel vorgesehen sein, zwischen denen jeweils ein Teilchen- bett angeordnet ist, wobei der Drehteller korrespondierende Reihen von Eluatableitungen autweist. Dadurch können mehrere annularchromatographische Trennungen gleichzeitig in einer einzigen Anlage durchgeführt und weitaus höhere Durchsatze des Annularchromatographen erzielt werdenIn preferred annular chromatographs according to the invention, two or more concentric cylinder jackets can be provided, between each of which a particle bed is arranged, the turntable having corresponding rows of eluate drains. As a result, several annular chromatographic separations can be carried out simultaneously in a single system and much higher throughputs of the annular chromatograph can be achieved
Eine besonders bevorzugte Ausfuhrungsform der Annularchromatographen gemäß vorliegender Erfindung weist der Feederkopf Durchgange für die Feederleitungen auf, in die die Feederleitungen vom Innenraum der Kern-Mantelanordnung her einsetz- und hindurchfuhrbar sind.A particularly preferred embodiment of the annular chromatograph according to the present invention has feeder head passages for the feeder lines, into which the feeder lines can be inserted and passed from the interior of the core / jacket arrangement.
Ein erfindungsgemaßer Annularchromatograph kann zusätzlich eine Temperatursteuerung umfassen, z.B. indem Wärmetauscher für Eluenten und/oder Feed vorgesehen sind, die in einer bevorzugten Λusfuhrungsform mit Innenzylinder und/oder Zylinder- mantel assoziiert vorgesehen sind. Dies ermöglicht, daß das Teilchenbett für die Trennprozesse auf höhere Betriebstemperatur gebracht bzw. die gegebenenfalls durch Ab- oder Desorptionsvorgänge freiwerdende Wärme abgeführt werden kann Die Wärmetauscher zur Temperaturerhöhung können dabei an sich bekannte Heizeinrichtungen und jene zur Temperatursenkung bekannte nach dem Durchflußprinzip arbeitende Kühler sein.An annular chromatograph according to the invention can additionally comprise a temperature control, for example by providing heat exchangers for eluents and / or feed, which in a preferred embodiment have an inner cylinder and / or cylinder. coat associated are provided. This enables the particle bed for the separation processes to be brought to a higher operating temperature or the heat released, if appropriate, by removal or desorption processes to be removed.
Es folgt nun eine detailliertere Beschreibung der Erfindung unter Bezugnahme auf die beigelegten Zeichnungen, wobei die Fig. 1 bis 4 jeweils schematische Seitenschnitt- ansichten sind. Davon sind die Fig. 1 und 4 Gesamtansichten und die Fig. 2 und 3 Teilansichten von erfindungsgemäßen Annularchromatographen, wobei sich die Kopfkonstruktion des Annularchromatographen in den Fig. 1 und 2 von jener in den den Fig. 3 und 4 unterscheidet.There now follows a more detailed description of the invention with reference to the accompanying drawings, wherein FIGS. 1 to 4 are each schematic side sectional views. 1 and 4 are overall views and FIGS. 2 and 3 are partial views of annular chromatographs according to the invention, the head construction of the annular chromatograph in FIGS. 1 and 2 being different from that in FIGS. 3 and 4.
In Fig. 1 erkennt man eine Grundplatte 1 , die z.B. auf einen Labortisch aufschraubbar ist und in der eine Antriebswelle 2 drehbar gelagert ist. Auf die Antriebswelle 2 ist ein Drehteller 3 aufgekeilt, der entlang eines Kreisumfangs nicht näher bezeichnete durchgehende Eluatabnahmekanäle aufweist, unterhalb denen am einstückig mit der Grundplatte 1 ausgebildeten Lagerstutzen 4 für die Antriebswelle 2 eine nichtdrehbare Eluat- aufnahmetasse 5 vorgesehen ist.1 shows a base plate 1 which e.g. can be screwed onto a laboratory table and in which a drive shaft 2 is rotatably mounted. A turntable 3 is wedged onto the drive shaft 2 and has continuous eluate take-off channels along a circumference, below which a non-rotatable eluate receiving cup 5 is provided for the drive shaft 2 on the bearing connecting piece 4 formed integrally with the base plate 1.
Am Drehteller 3 ist ein Hohlzylinder 6 als Mantelzylinder bei 7 angebolzt, der ein eingezogenes, in Fig. 1 und Fig. 2 parallel zum Drehteller 3 verlaufendes Dach 8 aufweist, das über eine Kugellagerung 9 mit einer Anspeisungshülse 10 verbunden ist, die im Betrieb gegenüber der Grundplatte 1 nicht bewegt und von Zufuhrkanälen zum Innenraum des Hohlzylinders 6 für Feed, Eluate, zum Beschicken mit Teilchenbettmaterial etc. durchsetzt wird, von denen zwei mit 1 1 und 12 bezeichnet sind.On the turntable 3, a hollow cylinder 6 is bolted on as a jacket cylinder at 7, which has a retracted roof 8 which runs parallel to the turntable 3 in FIGS. 1 and 2 and which is connected via a ball bearing 9 to a feed sleeve 10 which is opposite in operation the base plate 1 does not move and is penetrated by supply channels to the interior of the hollow cylinder 6 for feed, eluate, for loading with particle bed material, etc., two of which are denoted by 1 1 and 12.
Im Innenraum des Hohlzylinders 6 ist auf die Antriebswelle 2 ein Innenzylinder 1 3 aufgesteckt und sitzt am Drehteller 3 auf, wobei zwischen Hohlzylinder 6 undIn the interior of the hollow cylinder 6, an inner cylinder 1 3 is plugged onto the drive shaft 2 and is seated on the turntable 3, with the hollow cylinder 6 and
- 3 Innenzvlinder 1 3 ein zv ndermantelformiger Teilchenbettraum 14 verbleibt, der bis zur gewünschten Hohe gleichmäßig mit teilchenformigem Bettmaterial gefüllt wird. Der Innenzvlinder 1 3 weist an der dem Drehteller 3 abgewandten Oberseite ein Dach mit nach oben gerichtetem Fuhrungsflansch 1 5 auf, mit dem es auf der Antriebswelle 2 sitzt und an dem eine Spiralfeder 16 angreift, die den Innenzylinder 13 an den Drehteller 3 druckt- 3rd Inside Zvlinder 1 3 a zv ndermantel-shaped particle bed space 14 remains, which is evenly filled with particulate bed material to the desired height. The inner cylinder 1 3 has on the upper side facing away from the turntable 3 a roof with an upwardly directed guide flange 1 5, with which it sits on the drive shaft 2 and on which a coil spring 16 engages, which presses the inner cylinder 13 on the turntable 3
Das Widerlager tur die Feder 1 6 ist eine Spannhulse 1 7, die gekontert soweit auf die Antriebswelle 2 autgeschraubt ist, daß ein Drehflansch 18 der Spannhulse 1 7, der ein Kugellager 1 9 tragt, mit dessen freiem Lagerring an der Anspeisungshulse 10 kratt- schlussig anliegt Somit besteht eine Lagerung der Anspeisungshulse 10 sowohl gegenüber dem Dach 8 des Hohlzylinders 6 als auch gegenüber der Spannhulse 1 7, sodaß die Anspeisungshulse 1 0 gegenüber den rotierenden Teilen des Annularchromatographen ohne weiteres testgehalten werden kannThe abutment door spring 1 6 is a clamping sleeve 1 7, which is counter-screwed so far onto the drive shaft 2 that a rotary flange 18 of the clamping sleeve 1 7, which carries a ball bearing 1 9, with its free bearing ring on the feed sleeve 10, is conclusive There is thus a storage of the feed sleeve 10 both with respect to the roof 8 of the hollow cylinder 6 and with respect to the clamping sleeve 1 7, so that the feed sleeve 1 0 can be easily tested against the rotating parts of the annular chromatograph
Bei einem Vergleich der Fig. 1 und 2 erkennt man, daß durch Zubehorteilsatze, die jeweils aufeinander abgestimmte Spannhulse 1 7, Innenzylinder 1 3 und Hohlzylinder 6 autweisen, die Tei lchenbettraumhohe variiert werden kann. Ebenso kann die Teilchen- bettraumtiete durch Abstimmen der Durchmesser von Hohlzylinder 6 und Innenzylinder 1 3 variiert werdenIn a comparison of FIGS. 1 and 2 it can be seen that by accessories sets, each matched clamping sleeves 1 7, inner cylinder 1 3 and hollow cylinder 6, the Tei lchenbettraumhehe can be varied. Likewise, the particle bed space can be varied by coordinating the diameters of hollow cylinder 6 and inner cylinder 13
Aus den Fig. 1 und 2 ist lediglich zu erkennen, daß die Zufuhrkanale 1 1 und 12 an bestimmten Stellen oberhalb des Innenzylinders 13 munden; in Fig. 3, die auch eine andere Koptkonstruktion betrifft, ist beispielhaft gezeigt, daß Zufuhrrohre 20 durch die Zufuhrkanale hindurchgefuhrt werden, und zwar vom Innenraum des Annularchromatographen nach außen. Dazu ist an die Anspeisungshulse 10 ein Verteilerblock 21 angeschraubt, der mit den Zufuhrkanalen korrespondierende Bohrungen aufweist, die Schultern zur Anlage eines am Ende des Zufuhrrohrs 20 angeordneten Ringflanschs aufweisen Das Zufuhrrohr 20 wird vor dem Zusammenbau des Chromatographen in den Verteilerkopt nach oben eingeschoben, bis es mit seinem Ringflansch an der Schul-From Figures 1 and 2 it can only be seen that the feed channels 1 1 and 12 mouth at certain points above the inner cylinder 13; In FIG. 3, which also relates to another head construction, it is shown by way of example that feed tubes 20 are guided through the feed channels, specifically from the interior of the annular chromatograph to the outside. For this purpose, a distributor block 21 is screwed onto the feed sleeve 10, which has bores corresponding to the feed channels, which have shoulders for engaging an annular flange arranged at the end of the feed tube 20. Before the chromatograph is assembled, the feed tube 20 is pushed upwards into the distributor head until it is with its ring flange on the school
4 - ter der Bohrung im Verteilerkopf 21 anliegt; dann wird ein Dichtnippel 22 eingeschraubt, an dem über eine Rändelmutter 23 ein Verteilerrohr 24 befestigt wird, das in den Ringspalt 14 zwischen Hohlzylinder 6 und innenzylinder 1 3 hineinragt und oberhalb des nicht gezeigten Teilchenbetts endet. Im Betrieb dreht sich also das Teilchenbett gegenüber dem Verteilerrohr 24. An der Stelle, wo das Zufuhrrohr 20 aus der Anspeisungshulse 10 austritt, ist ein geteilter Stopfen 25 eingesetzt, der nur den Sinn hat, das Zufuhrrohr 20 zu zentrieren. Mit 26 ist eine Schraube zum Entlüften des Innenraums des Annularchromatographen bezeichnet.4 - ter of the bore in the distributor head 21; then a sealing nipple 22 is screwed in, to which a distributor tube 24 is fastened via a knurled nut 23, which projects into the annular gap 14 between the hollow cylinder 6 and the inner cylinder 1 3 and ends above the particle bed (not shown). In operation, the particle bed rotates relative to the distributor pipe 24. At the point where the feed pipe 20 emerges from the feed sleeve 10, a split plug 25 is used, which only has the purpose of centering the feed pipe 20. With 26 a screw for venting the interior of the annular chromatograph is designated.
Bei der in Fig. 3 dargestellten Konstruktion wird sowohl der Innenzylinder 13 als auch der Hohlzylinder 6 von unterhalb des Drehtellers an diesem angeschraubt.In the construction shown in FIG. 3, both the inner cylinder 13 and the hollow cylinder 6 are screwed onto the turntable from below.
Weiters zeigt Fig. 4 eine ähnliche Annularchromatographen-Konstruktion zu jener in Fig. 3, allerdings ist die Antriebswelle in dieser Ausführungsform zweiteilig ausgeführt, wobei der obere Wellenteil 2' mit geringerem Durchmesser in den unteren Teil 2 eingeschoben und im Überlappungsbereich 27, z.B. über eine Schraub- oder Rastsicherung, an diesem fixiert ist. Der obere Wellenteil 2' ist über einen Teil der Gesamtlänge der Welle in den unteren einschiebbar, um so die Länge der Welle an verschiedene Höhen der Mantelzylinder/Innenzylinder-Paare 6, 1 3 und damit an unterschiedliche Teiichen- betthöhen anpassen zu können.Fig. 4 further shows a similar annular chromatograph construction to that in Fig. 3, however the drive shaft in this embodiment is made in two parts, the upper shaft part 2 'having a smaller diameter being pushed into the lower part 2 and being in the overlap region 27, e.g. via a screw or detent, is fixed to it. The upper shaft part 2 'can be inserted over a part of the total length of the shaft into the lower one, so that the length of the shaft can be adapted to different heights of the jacket cylinder / inner cylinder pairs 6, 1 3 and thus to different parti bed heights.
Zusätzlich ist in Fig. 4 der Strömungsweg eines in dieser Ausführungsform vorgesehenen Durchfluß-Temperiersystems eingezeichnet. Dabei tritt Temperierflüssigkeit (d.h. Heiz- oder Kühlflüssigkeit) an Einlaßstutzen 28 in den unteren Teil der Antriebswelle 2 ein (Pfeil A), wird innerhalb der Welle zum Stutzen 29 geführt, wo sie aus der Welle aus- und in den Innenraum des Innenzylinders 1 3 eintritt (Pfeil B), um dort für die Temperierung (Heizung bzw. Kühlung) des Teilchenbetts zu sorgen. Der weitere Strömungsweg erfolgt über Auslaß 30 aus dem Zylinderinnenraum heraus und erneut in die Welle - in diesem Fall in deren oberen Teil 2' - hinein (Pfeil C), bis die Temperierflüssigkeit schließlich am Auslaßstutzen 31 den Annularchromatographen verläßt (Pfeil D).In addition, the flow path of a flow temperature control system provided in this embodiment is shown in FIG. 4. Thereby tempering liquid (ie heating or cooling liquid) enters the lower part of the drive shaft 2 at the inlet connection 28 (arrow A), is guided inside the shaft to the connection 29, where it emerges from the shaft and into the interior of the inner cylinder 1 3 enters (arrow B) in order to maintain the temperature (heating or cooling) of the particle bed. The further flow path takes place via outlet 30 out of the cylinder interior and again into the shaft - in this case in its upper part 2 '- (arrow C) until the bath liquid finally leaves the annular chromatograph at outlet port 31 (arrow D).
- 5 Vorzugsweise wird die Temperierflussigkeit in einem geschlossenen Kreislauf gefuhrt, indem diese nach ihrem Austritt an 31 einen (nicht dargestellten) Wärmetauscher passiert und - entsprechend temperiert - an 28 wieder in den Chromatographen eintritt- 5th The temperature control liquid is preferably conducted in a closed circuit by passing it through a heat exchanger (not shown) at 31 and, at a corresponding temperature, entering the chromatograph again at 28
Obwohl die Erfindung anhand von konkreten Ausfuhrungsformen beschrieben wurde, versteht sich von selbst, daß daran von Fachleuten zahlreiche Variationen und Modifikationen vorgenommen werden können, die auch allesamt im durch die zugehörigen Ansprüche definierten Schutzumtang der Erfindung liegen.Although the invention has been described on the basis of specific embodiments, it goes without saying that numerous variations and modifications can be made to it by experts, all of which are within the scope of protection of the invention defined by the associated claims.
- 6 - 6th

Claims

Ansprüche: Expectations:
1 . Annularchromatograph mit gegenüber einer stationären Basis und einem stationären Feederkopt mit duigehenden Feederleitungen aut einem Drehteller mit Eluatableitungen rotierendem Tei lchenbett, das zwischen einem Innenzylinder und einem Zylindermantel ausgebildet ist, dadurch gekennzeichnet, daß am Drehteller (3) eine Zentralsaule (2) vorgesehen ist, die sich nach oben bis durch den Feederkopf (10) hindurch erstreckt und auf der eine Spannvorrichtung (1 6, 1 7) zum Andrucken des Feederkopfs (10) an den Zylindermantel (6) angeordnet ist.1 . Annular chromatograph with a stationary base and a stationary feederkopt with duigehende feeder lines aut a rotary bed with eluent drainage rotating Tei lchenbett, which is formed between an inner cylinder and a cylinder jacket, characterized in that a central column (2) is provided on the turntable (3), the extends upwards through the feeder head (10) and on which a tensioning device (1 6, 1 7) for pressing the feeder head (10) onto the cylinder jacket (6) is arranged.
2. Annularchromatograph nach Anspruch 1 , dadurch gekennzeichnet, daß die Spannvorrichtung (16, 1 7) Distanzhulsen (1 7) zur Anpassung an Zylindermantel (6) verschiedener Lange autweist2. Annular chromatograph according to claim 1, characterized in that the clamping device (16, 1 7) spacer sleeves (1 7) for adaptation to the cylinder jacket (6) has different lengths
3. Annularchromatograph nach Anspruch 1 , dadurch gekennzeichnet, daß die Zentralsaule (2) Verlängerungsstücke (2') zur Anpassung an Zylindermantel (6) verschiedener Lange aufweist.3. Annular chromatograph according to claim 1, characterized in that the central column (2) has extension pieces (2 ') for adaptation to the cylinder jacket (6) of different lengths.
4. Annularchromatograph nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß aufemandersetzbare Zylindermantel (6) vorgesehen sind.4. Annular chromatograph according to one of claims 1 to 3, characterized in that cylinder jacket (6) which can be fitted onto one another are provided.
5. Annularchromatograph nach Anspruch 4, dadurch gekennzeichnet, daß die Zylindermantel (6) unterschiedliche Innendurchmesser aufweisen.5. Annular chromatograph according to claim 4, characterized in that the cylinder jacket (6) have different inner diameters.
6. Annularchromatograph nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß Innenzyhnder/Zylindermantelpaare (1 3, 6) vorgesehen sind.6. Annular chromatograph according to one of claims 1 to 5, characterized in that inner cylinders / cylinder jacket pairs (1 3, 6) are provided.
7. Annularchromatograph nach Anspruch 6, dadurch gekennzeichnet, daß die Innen- zylinder/Zylindermantelpaare (1 3, 6) als Verbundkorper vorgesehen sind. 7. Annular chromatograph according to claim 6, characterized in that the inner cylinder / cylinder jacket pairs (1 3, 6) are provided as composite bodies.
8. Annularchromatograph nach Anspruch 7, dadurch gekennzeichnet, daß die Verbundkorper eine fixierte Teilchenbettfullung enthalten.8. Annular chromatograph according to claim 7, characterized in that the composite bodies contain a fixed particle bed filling.
9 Annularchromatograph nach Anspruch 8, dadurch gekennzeichnet, daß die fixierte Teilchenbettfullung eine durch Durchpolymerisieren von Vorpolymerteilchen in Kontakt mit Innenzylinder (1 3) und Zylindermantel (6) erhaltene poröse Matrix ist.9 Annularchromatograph according to claim 8, characterized in that the fixed particle bed filling is a porous matrix obtained by polymerizing through prepolymer particles in contact with the inner cylinder (1 3) and cylinder jacket (6).
10. Annularchromatograph nach einem der Ansprüche 1 bis 9, dadurch gekennzeichnet, daß zwei oder mehrere konzentrische Zylindermantel (6) vorgesehen sind, zwischen denen jeweils ein Teilchenbett angeordnet ist sowie der Drehteller (3) korrespondierende Reihen von Eluatableitungen aufweist.10. Annular chromatograph according to one of claims 1 to 9, characterized in that two or more concentric cylinder jacket (6) are provided, between each of which a particle bed is arranged and the turntable (3) has corresponding rows of eluate discharge lines.
1 1 Annularchromatograph nach einem der Ansprüche 1 bis 10, dadurch gekennzeichnet, daß der Feederkopf (10) Durchgange (1 1 , 1 2) für die Feederleitungen (20) aufweist, in die die Feederleitungen (20) vom Innenraum der Kern-Mantelanordnung her emsetz- und hindurchfuhrbar sind.1 1 Annularchromatograph according to one of claims 1 to 10, characterized in that the feeder head (10) has passages (1 1, 1 2) for the feeder lines (20) into which the feeder lines (20) from the interior of the core-jacket arrangement can be inserted and passed through.
1 2. Annularchromatograph nach einem der Ansprüche 1 bis 1 1 , dadurch gekennzeichnet, daß eine Temperatursteuerung vorgesehen ist.1 2. Annular chromatograph according to one of claims 1 to 1 1, characterized in that a temperature control is provided.
1 3. Annularchromatograph nach Anspruch 1 2, dadurch gekennzeichnet, daß Wärmetauscher für Eluenten und/oder Feed vorgesehen sind.1 3. Annularchromatograph according to claim 1 2, characterized in that heat exchangers are provided for eluents and / or feed.
14. Annularchromatograph nach Anspruch 12 oder 13, dadurch gekennzeichnet, daß Wärmetauscher assoziiert mit Innenzylinder und/oder Zylindermantel vorgesehen sind.14. Annular chromatograph according to claim 12 or 13, characterized in that heat exchangers associated with the inner cylinder and / or cylinder jacket are provided.
1 5 Annularchromatograph nach Anspruch 1 3 oder 14, dadurch gekennzeichnet, daß die Wärmetauscher zur Temperaturerhöhung an sich bekannte Heizeinrichtungen und jene zur Temperatursenkung bekannte Durchflußkuhler sind.1 5 Annularchromatograph according to claim 1 3 or 14, characterized in that the heat exchangers for increasing the temperature are known heating devices and those known for lowering the flow rate cooler.
- 8 - - 8th -
EP99908668A 1998-03-19 1999-03-19 Annular chromatograph Withdrawn EP1064542A1 (en)

Applications Claiming Priority (3)

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AT17098 1998-02-02
AT0017098U AT2578U1 (en) 1998-03-19 1998-03-19 ANNULAR CHROMATOGRAPH
PCT/AT1999/000075 WO1999047913A1 (en) 1998-03-19 1999-03-19 Annular chromatograph

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AT (1) AT2578U1 (en)
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EA (1) EA200000962A1 (en)
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DE50012916D1 (en) * 2000-03-07 2006-07-20 A L P Technology Ag Autoclavable Annular Chromatograph
DK1492623T3 (en) * 2002-04-05 2010-11-15 Dynamic Extractions Ltd Centrifuge
US8277650B2 (en) 2009-03-13 2012-10-02 Terrasep, Llc Methods and apparatus for centrifugal liquid chromatography

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US3077103A (en) 1958-02-10 1963-02-12 Gen Motors Corp Chromatographic method and apparatus
GB1350204A (en) * 1970-04-03 1974-04-18 Nat Res Dev Apparatus for use in continuous liquid chromatography
US3666105A (en) * 1970-08-04 1972-05-30 Us Agriculture Apparatus for continuous liquid-solid phase chromatography
EP0328146B1 (en) 1988-02-12 1995-09-20 The Perkin-Elmer Corporation A high pressure column assembly for a liquid chromatograph system
US5217608A (en) 1988-07-21 1993-06-08 The Research Foundation Of State University Of New York Multi-column planet centrifuge chromatograph
US5124023A (en) * 1988-11-28 1992-06-23 Union Oil Company Of California Continuous removal of polynuclear aromatics from hydrocarbon recycle oil
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US6464882B1 (en) 2002-10-15
WO1999047913A1 (en) 1999-09-23
AT2578U1 (en) 1999-01-25
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CA2329402A1 (en) 1999-09-23
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