DE2263770C2 - Fraction collector for column chromatographs - Google Patents

Description

The invention relates to a fraction collector for connection to the separation column of a liquid chromatograph, with an effort to divert the fractions of interest into the appropriate Collecting vessels, the collecting devices being arranged in a circle and at a distance from one another are, a with the separation column connectable delivery device and a motor that intermittently the The delivery device and one of the collecting devices connects.

Such fraction collectors are used in the preparative Liquid chroniatography for this, intermittent from the separation column of a chromatograph released, liquid fractions of interest individually and separated from the intermediate fractions catch and collect in containers.

It is already a fraction collector of the aforementioned Type known, in which üie different collecting containers in a circle on a turntable are arranged. A motor is intermittently operated by a control device such that it in each case one collecting container is carried out one after the other under the outlet line of the separation column.

This fraction collector brings with it considerable drive problems and becomes device-related expensive if several or larger collection containers and, moreover, at ever shorter intervals and are to be moved cyclically by the motor in a precisely timed manner. The drive problem increases further if, for example, small test tubes in one case and in the other In contrast, containers with several liters of content are to be filled. In addition, it follows that the Distribution of the fractions hardly with the exclusion of oxygen or moisture or in a protective gas atmosphere, since then the entire turntable with a large one, too moving chamber would be surrounded. On the other hand, fraction collectors are known where switching is carried out from one collecting vessel to the next with the help of a multi-way valve. However, such arrangements have the disadvantage that a pressure surge occurs with every switching operation, which can lead to interference with the detector signal.

The invention is based on the object of providing a fraction collector of the type described at the beginning in particular to be trained in such a way that both smaller and larger quantities of

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the fractions can be distributed to collecting tanks without affecting the overall device cerätetechnisch is more complex or any drive problems occur and that switching from one collecting vessel to the next without a pressure surge.

To solve this problem, the invention provides that the collecting devices are stationary are arranged, a support member for the dispensing device is provided above the holder, the dispensing device a connection for a line connectable to the separation column, one end of which attached to the support member and a hollow manifold finger with an outlet nozzle having the rotatably and centrally mounted to the collecting devices on the support member and with this line as well a parallel connection for a detector can be connected is, a driver driven by the motor is the distributor finger and thus its outlet nozzle each of the fall arrest devices rotating? the motor intermittently via a control device can be actuated and a drain collecting duct absorbs the intermediate fractions which emerge from the outlet nozzle of the distributor finger when they is located between the collection facilities for the fractions of interest. This will If possible, a much simpler structure is sufficient, wfii no longer has a large number of collecting bins must be moved and braked stötfweise, but only a comparatively with extremely ed: i [> er mass inertia afflicted distributor finger dr ht will. Furthermore, the drive device can be independent of the size of the individual collective breeder be dimensioned.

According to a preferred embodiment of the Invention can be provided that the holder one-n interchangeable insert with circular next to one another arranged recesses, to which output lines for those of interest Fractions are releasably connected. In this way a variable number of collecting containers can be used Any size can be spatially separated, which is also for safety reasons can be beneficial

If fractions - with the exclusion of oxygen or moisture in a protective gas atmosphere are to be distributed to the collecting container, the fraction collector can expediently be designed in such a way that an externally circumferential annular shoulder is formed on the holder and a cylinder made of transparent SrT chemically between this and the holder inert material can be used with the formation of a protective gas _{chamber and this chamber has} a closure for a protective gas line

The following are preferred embodiments, pie, dg invention to H-nd the drawing and connected to a hollow price increase. the Washer is by means of three knurled nuts 5β, so

screwed-on webs 6a, 6b arranged at a distance above the annular shoulder 7 of a holder 8 and is used

in turn as a support member for the distributor finger, which is centrally and rotatably mounted on this. The top The end of the distributor finger is connected to the discharge line, while the other end is connected to the outlet nozzle is provided. ,.

There is a parallel to the output line 1 a Connection Ic for a detector or its supply line. The length of this lead is on the length matched the flow path up to an outlet nozzle 9 on the distributor finger.

Below the outlet nozzle on the generated by rotation of the nozzle about its axis are circular in gieichen distances from each other through holes 10a, 10b for accommodating test tubes 11 ", 11 b provided in the holder. The holder is cylindrical

designed so drisch and e>; holds a ^{collecting drainage channel} 12 at the bottom, to which an outlet line for the intermediate fractions can be connected.

The holder is screwed by screws 13 ″, 136 to a ₅ eaiem stand 14, which is fastened to a base plate 15 and receives a stepper motor 16 indicated by a block an insert 19 protrudes and is sealed against it.

On the extension shaft 18 is em driver 20 attached in the form of a bracket which includes the distributor finger and in accordance with the engine rotations leads.

In operation, the fraction collector emerging from the separation column eluate is the one hand, the fraction collector and secondly via the on-circuit Ib to a small Te "a UeteKtor zugeführt.Durch the interaction of the detector and a not shown and not part oer invention forming 'Steuereinncntung is It is important that the motor 16 rotates the valve finger 4 intermittently over the test glasses 11 ', 116 by means of the driver 20 so that the correct fractions are repeatedly directed into the test glasses. ^ a the eluate continuously borrowed through the constantly open starting nozzle 'of the distributor f ^ * ^^^ ** " detector acting 5 ^^ _ah 7

It goes without saying that erne multiplicity Λ

Changes or additions to mogl.ch d without to adopt the basic idea of the invention

can be in a hurry.

Screen 21

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which collecting openings are provided that are closed with.

To be able to change the lines leading to these, the holder can have an interchangeable insert have the appropriate shape. Radial and / or axial recesses can be provided in the insert in which the collecting devices can be slidably attached.

According to Fig. 2, the insert 19 ⁷ recesses 23, which are connected to receiving lines 24, with further recesses in the form of voi blind holes 25 are located between these recesses, which is connected to a collecting line 27 for the intermediate fractions via a collecting outlet 26 with a collecting line 27. The through-holes and blind holes are expediently bevelled in a funnel-shaped manner in the upper circumferential section and arranged directly next to one another in order to achieve a sharper separation of individual "peaks" in the chromate gram.

1 sheet of drawings

Claims (10)

Patent claims: 1. Fraction collector for connection to the separation column of a liquid chromatograph, with a holder for holding collecting devices for the fractions of interest, the collecting devices being arranged in a circle and at a distance from one another, a delivery device that can be connected to the separation column and a motor that intermittently controls the delivery device and one of the collecting devices, characterized in that the collecting devices (11a, Ufa or 24) are arranged stationary, a support member (2) is provided for the dispensing device above the holder (8), the dispensing device has a connection (1 ti) for a with the separating column connectable line (la), one end of which is attached to the ao support member, and a hollow distributor finger (4) with an outlet nozzle (9) which is rotatably and centrally mounted to the collecting devices on the support member and with this line as well a parallel connection (1 c) for a detector verbi A driver (20) driven by the motor (16) rotates the distributor finger and thus its outlet nozzle via one of the collecting devices, the motor can be operated intermittently via a control device and a drainage channel (12) receives the intermediate fractions, which emerge from the outlet nozzle of the distributor finger when this is located between the collecting devices for the fractions of interest. 2. Fraction collector according to claim 1, characterized in that the support member has a disc which is lifted by webs (6 a, 6 ti) at a distance from the holder (8). 3. Fraction collector according to claim 1 or 2, 4η characterized in that an externally encircling annular shoulder (7) is formed on the holder is and between this and the holder a cylinder (21) made of transparent, chemically inert Material can be used to form a protective gas chamber and this chamber has a connection (22) for a protective gas line. 4. Fraction collector according to one of claims 1 to 3, characterized in that the holder is circular and arranged at a distance from one another * has through holes (10 a, 10 ti) into which collecting containers (11 a, lib) can be used. 5. fraction collector according to one of claims 1 to 4, characterized in that the Holder just exchangeable insert (19) with recesses arranged in a circle next to one another (23) to which output lines (24) for the fractions of interest are releasably connected. 6. fraction collector according to claim 5, characterized in that the upper edges of the Recesses (23) are beveled and further recesses (25) through a common one Drainage channel (26) for the intermediate fractions are connected. 7. Fraction collector according to one of claims 1 to 4, characterized in that the collecting devices (Ha, 11 b; 24) are arranged radially displaceably in the recesses. 8. fraction collector according to one of claims 4 to 7, characterized in that the Collecting devices are arranged axially displaceably in the recesses and the outlet nozzle (9) of the distributor finger (4) is mounted adjustable in the axial direction. 9. fraction collector according to one of claims 1 to 8, characterized in that the Distributor finger (4) is mounted on the support member (2) above the outlet nozzle (9). 10. Fraction collector according to one of claims 1 to 9, characterized in that the Motor (16) is arranged in the stator (14) of the device and the driver (20) is coaxial with it the distributor finger (4) and above the outlet nozzle (9).