US3487678A - Sample loading apparatus - Google Patents

Description

Jan. 6, 1970 A. R. THOMSON ET AL 3,487,678

SAMPLE LOADING APPARATUS Filed Dec. 16. 1966 United States Patent 3,487,678 SAMPLE LOADING APPARATUS Alan Russell Thomson, Abingdon, and John William Eveleigh, Wantage, England, assignors to United Kingdom Atomic Energy Authority, London, England Filed Dec. 16, 1966, Ser. No. 602,267 Claims priority, application Great Britain, Mar. 25, 1966, 13,440/ 66 Int. 'Cl. G01n 1/00 US. Cl. 73--61.1 20 Claims ABSTRACT OF THE DISCLOSURE Apparatus for automatically loading samples for analysis on to a chromatography column has a transfer member that is stepwise moved along a path. A plurality of sample locating chambers are located in a spaced relationship on the transfer member and extend through the member. A fluid inlet duct and a fluid outlet duct are located relative to the transfer member so that as each chamber is, in turn, registered with the ducts, the ducts are connected with each successive chamber. The ducts are connected by sealing to opposite sides of a fluid passageway through a given chamber, such that fluid can flow from the inlet duct through the given chamber and out the outlet duct leading to a column.

This invention relates to analysing equipment and is particularly, but not exclusively, concerned with equipment suitable for use in column chromatography.

Determination of protein and polynucleotide structures require large numbers of quantitative analyses of mixtures of amino acids and nucleotides. Recent advances in column chromatography have significantly reduced the time required for one analysis e.g. for amino acids from 24 to 2 hrs. and since suitable automatic systems are now available it is desirable that means he provided whereby a predetermined number of samples for analysis may be automatically loaded, in turn, and at preselected times onto a column.

According to the invention means for automatically loading samples for analysis on to a chromatography column comprises a transfer member, a plurality of sample locating chambers located in a spaced relationship on said transfer member, a fluid inlet duct and a fluid outlet duct connectable with said chamber, said fluid outlet duct leading to said column and means for stepwise moving the transfer member such that each chamber is, in turn, simultaneously registerable with said inlet and outlet ducts.

Preferably fluid sealing means are provided to seal the sample chamber to the ducts.

According to a further aspect of the invention, means for automatically loading samples for analysis onto a chromatography column comprises a transfer member, a plurality of apertures in a spaced relationship in said member, means for locating a sample in each aperture, means for stepwise moving the member such that each aperture is held in exclusive register with fluid inlet and outlet ducts and fluid sealing means between the member and each of the said ducts.

The sealing means may incorporate a cam associated and operable with the transfer member moving means such a sealing pressure applied by said cam is operable when one of the sample holding apertures is in register with the said ducts.

In a preferred form of the invention, the transfer member comprises a block having a plurality of apertures arranged in a spaced linear relationship and the samples are located in containers positionable in each aperture.

To enable the nature of the invention to be more readily understood, an embodiment of the invention will now be described, solely by way of example with reference to the accompanying drawing. In the drawing FIG. 1 is a sectional elevation of a sampling loading device.

FIG. 2 is a sectional end elevation on the line 11 of FIG. 1.

Referring to the drawing the sample loading device comprises a rectangular block incorporating a plurality of sample containers 2, the block being arranged to slide longitudinally on guide rails 3 whereby each sample container may be moved in a pre-determined sequence to register with inlet and outlet ducts 4 and 5, the inlet duct connecting with an eluent pump (not shown) and the outlet duct leading to an analytical column (not shown).

The block 1 is provided with a plurality of equally spaced vertical apertures 6, said apertures being dimensioned to easily receive the sample containers 2. Each aperture is shaped to support the flanged upper end of a sample container. The containers are tubular, having an internal shoulder 7 at the lower end arranged to support a porous disc 8. A resilient O-ring located in an annular groove on the outer surface of the container acts as a seal between the block and the container. The interior of the container is partly filled with a sample support material 9, for example, a resin or other absorbent bed material.

With some sample materials it is desirable to exclude the atmosphere while awaiting analysis and a cover 33 is provided, for this purpose, above the movable block. The cover is resiliently secured to a pair of side plates 12 such that the block may freely move under the cover.

The block 1 is basically rectangular inshape having a bottom flange or extension 10 at each lower longitudinal edge. Each upper longitudinal edge is provided with a series of vertical grooves 11 which extend into the block to form a rack. The grooves 11 are spaced mid-Way between the container locating apertures 6.

Each block flange 10 rests on a guide rail 3 and each guide is resiliently secured to a side plate 12 by two screws 13 and soft rubber members 14. The side plates are spaced apart on a base plate 15 which also forms a locating base for a conventional electric drive motor (not shown).

A drive shaft 16 coupleable to the motor is journalled on ball or roller bearings 17 and extends between the side plates. The shaft supports and drives a pair of discs 18 and a central cam 19. Each disc is provided with a'projecting peg 20 arranged to engage the rack grooves 11 on each side of the block 1 such that rotation of the disc by the drive motor, acting through shaft 16, moves the block relative to the slides.

A union or sealing member 21 is interposed between the top of the block and the cam 19 the said member having the form of a flat disc pivotally supported on a stirrup shaped strap 22. A passage way 23 formed within the disc connects with inlet duct 4 and communicates with a central opening 24 in the lower face of the disc. An annular groove 25 and O-ring 26 contained therein provide a high pressure seal between the upper surface of the block 1 and the disc. The upper face of the disc is centrally recessed to accept a slightly resilient circular pad 27. Pad 27 may be formed of nylon. The strap 22 is itself pivoted on a cross bar 28 extending between the side plates, such that rotation of the cam 19 pushes the disc into abutment with the upper surface of the block.

The outlet duct 5 connects with a centrally apertured bottom connector piece 29 located vertically below the sealing number 21. The upper face 30 of the connector piece is provided with an annular groove 31 containing an O-ring 32. O-ring 32 lightly contacts the under surface of the block 1 when the block is being moved on the guide rails.

In operation, the block having a number of sample containers located in the appropriate apertures is moved by energising the drive motor to rotate the disc 18 in a step-wise fashion. The projecting peg on each disc engages a groove 11 in the block and the block moves through one increment equal to the spacing distance between each sample container. Initial setting of the disc position ensures that each sample container is moved into accurate register with the upper sealing member 21 and the bottom connector 29. The cam 19 is arranged such that pressure is applied to the upper sealing member 21 via the resilient pad 27 when the sample container is correctly positioned in relation to the inlet and outlet and the sealing member is then pressed downwards on to the block. Due to the resilience of the guide rail mountings, the block and guide rail mountings deflect slightly and apply a pressure to the connector block. Since both the O-rings 26 and 32 are partially deformed by the pressure applied by the cam the sample container is effectively connected in a leak tight manner with the ducts leading from an eluent supply line or pump and the analytical column.

The samples are preferably absorbed on an ion exchange media held in the sample containers and regeneration and re-equilibration are carried out at the end of each analytical cycle before the next sample is brought on line. The apparatus operates automatically being controlled by a simple program.

The motor drive may be programmed or controlled in any conventional manner which permits a time-controlled stepwise operation and in a preferred arrangement the flow of eluent through the sample is controlled by a selector valve also operated in accordance with the desired program. For example, the cam 19 can be arranged to open and close a valve (not shown) in the eluent supply line.

It will be appreciated that the invention is in no way limited to the embodiment shown. For example, other forms of transfer member can be envisaged, i.e. a turntable, driving or roller chain or belt may be used, the stepwise motion being suitably arranged in association with the desired sample spacing.

We claim:

1. Apparatus for automatically loading samples for analysis on to a chromatography column comprising a transfer member movable along a path, a plurality of sample locating chambers located in a spaced relationship on said transfer member and extending through said member, a fluid inlet duct and a fluid outlet duct, said fluid outlet duct leading to said column, said ducts being located, relative to said transfer member to be connected with successive chambers, means for sealing both ducts to opposite sides of a fluid passageway through a given chamber with which the ducts are connected, such that fluid can flow from said inlet duct through the given chamber and through the outlet duct, and means for stepwise moving the transfer member such that each chamber is, in turn, simultaneously registerable with said inlet and outlet ducts.

2. Apparatus for automatically loading samples for analysis on to a chromatography column comprising a transfer member movable along a path, a plurality of apertures in a spaced relationship in said member and extending through said member, sample support means for locating and supporting sample in each aperture, means for stepwise moving the member such that each sample support means in each aperture is held in exclusive register with fluid inlet and outlet ducts and fluid sealing means between the member and each of the said ducts for sealing the ducts to opposite sides of a fluid passage way through the sample support means in exclusive register with h duc 41911 hat fluids flow from said inlet duct through the sample support means and through the outlet duct.

3. Apparatus according to claim 2, wherein the transfer member is resiliently supported and cam means are provided to depress the transfer member on said supports, a sealing member incorporating one of said fluid ducts and a deformable fluid sealing means interposed between the cam and one face of the transfer member and second deformable fluid sealing means interposed between the other fluid duct and a face of the transfer member such that movement of the cam clamps the transfer member between the fluid ducts and deforms the sealing means.

4. Apparatus according to claim 2 wherein the transfer member comprises a turntable having the said chambers arranged in spaced relationship around a circle.

5. Apparatus according to claim 2 wherein the transfer member is a belt having said chambers in spaced relationship along said belt.

6. An apparatus according to claim 2 wherein a sample support material is inserted in at least one of said sample support means.

7. An apparatus according to claim 6 wherein said sample support material is an absorbent material.

8. An apparatus according to claim 7 wherein said absorbent material is an ion exchange medium.

9. An apparatus according to claim 7 wherein said absorbent material is a resin.

10. Apparatus for automatically loading samples for analysis on to a chromatography column comprising a resiliently supported transfer member, a plurality of sample locating chambers located in spaced relationship in said transfer member, means for stepwise moving the member such that each chamber is held in exclusive register with fluid inlet and outlet ducts, fluid sealing means between the transfer member and each of said ducts, and cam means to depress the said transfer member on said supports and clamp the transfer member between the fluid ducts.

11. Apparatus according to claim 10 wherein the transfer member comprises a rectangular block having a plurality of apertures arranged in a spaced linear relationship and the sample locating means include a container positionable in each aperture.

12. Apparatus according to claim 11 wherein the block is slidably mounted on guide rails and each upper longitudinal edge of the block is provided with a series of vertical grooves forming a toothed rack and the drive means for the block include a pair of spaced discs, each disc having a projecting peg engageable with said rack.

13. Apparatus according to claim 12 wherein the cam and said discs are mounted on a common drive shaft.

14. Apparatus for automatically loading samples for analysis onto a chromatography column comprising a transfer member having a plurality of sample locating chambers located in spaced relationship in said transfer member, each chamber being in the form of a bore extending through the transfer member, a fluid flow assembly including a fluid inlet duct and a fluid outlet duct, the two said ducts being located to be simultaneously registerable with a given chamber sealing the two ducts to' the chamber such that fluid can flow from said inlet duct through the chamber to said outlet duct, said transfer member and said fluid flow assembly being relatively movable such that the two said ducts can register, in turn, with successive chambers of said transfer member.

15. An apparatus according to claim 14 including a force exerting means for causing at least one of said fluid ducts to be located against and away from said transfer member, such that the said relative movement between the transfer member and the fluid flow assembly takes place when the said at least one fluid duct is in its position away from the transfer member, and such that fluid flow through that chamber in register with the ducts takes place when the said one duct is in its position against the transfer member.

16. A apparatus according to claim 15 wherein said force exerting means comprises a resilient transfer member supporting structure permitting limited resilient movement of said transfer member towards and away from said at least one fluid duct, and including sealing means between each of said fluid ducts and the chamber in register therewith, and a pressure exerting member for forcing into fluid tight engagement with each other the ducts and the chamber in register there with, to form a closed fluid flow path between the ducts through the chamber.

17. An apparatus according to claim 15 including drive means for moving the said transfer member while the said fluid flow assembly is held generally stationary, such that successive chambers are moved into registry with said fluid flow assembly.

18. An apparatus according to claim 17 wherein said drive means includes a member which, while moving continuously, moves the said transfer member in steps.

19. An apparatus according to claim 18 wherein each of said ducts includes sealing means for sealing the ducts to the chambers of the transfer member in register with the said ducts.

20. An apparatus as claimed in claim 19 wherein the transfer member is resiliently supported for movement towards and away from said at least one fluid flow duct, and including a force exerting means operable in timed relationship with said drive means for forcing into fluid tight engagement with each other the ducts and the chamber in refister with the ducts.

References Cited UNITED STATES PATENTS 3,240,068 3/ 1966 Horeth et al 73--421.5 3,038,340 6/1962 Isreeli.

3,162,050 12/1964 MacDonald et a1.

3,239,312 3/1964 Bell et al.

LOUIS R. PRINCE, Primary Examiner HARRY C. POST, Assistant Examiner US. Cl. X.R.

Images