JP5458581B2 - Liquid chromatography device - Google Patents

Description

The present invention relates to a liquid chromatography apparatus, and more particularly to a liquid chromatography apparatus with improved liquid dispersibility from an inlet .

  In order to separate and purify each component from a mixed solution containing a plurality of substances, a liquid chromatography apparatus is used. In a liquid chromatography apparatus, a packing material is held inside a cylindrical column, and porous plate-like members called filters or frit are arranged at both ends of the column. This filter or frit (hereinafter referred to as a filter) has a function of holding the packing material inside the column so as not to leak out of the column. In addition, this filter disperses the liquid sample to be separated and purified in the column cross section (that is, the cross section in the direction perpendicular to the column stretching direction), and the liquid sample moves from one end side to the other end side in the column. It has the function of allowing it to flow with piston flow without backflow.

  The material constituting the filter is generally a metal such as stainless steel or a resin such as high-density polyethylene. Since a resin filter is inferior in strength to a metal filter, a metal filter is used in a high-pressure chromatography apparatus in which the inside of the column is at a high pressure. As a metal filter, JP-A-7-260763 discloses a sintered metal filter obtained by laminating and sintering stainless steel fibers.

  Japanese Patent Application Laid-Open No. 2004-525384 discloses a plate-like main body, an inflow port provided at the center of the plate-like main body, and a lower surface of the plate-like main body as liquid distribution members arranged above the filter. It has been described with a disk facing the entrance. The liquid that has flowed in from the inflow port (“exit-side connecting portion” in the same publication) is applied to the upper surface of the filter (“perforated plate” in the same publication) after striking the disk and being dispersed in the radial direction, Pass the filter through the filter. In this way, by disposing the disk below the inlet and distributing the liquid from the inlet in the radial direction, the supply of the influent to the filler layer is equalized.

JP-A-7-260763 JP 2004-525384 A

  In the liquid chromatography apparatus disclosed in JP-A-2004-525384, since a separate disk is provided, the number of parts is large.

An object of the present invention is to provide a liquid chromatography apparatus capable of dispersing and supplying liquid from an inlet to a filter with a simple configuration .

The liquid chromatography apparatus according to claim 1 has a first lid attached to one end of a column packed with a packing material, a second lid attached to the other end, and a central portion of the first lid. Is provided with a liquid inlet, a liquid outlet is provided at the center of the second lid, and a porous plate-like filter is disposed between the first lid and the filler. in the liquid chromatography apparatus, which is, in the inlet near portions of the opposing surfaces of the first lid of the filter, formed by adhering the lower sheet or thin liquid-permeable than the filter TeiTorueki In the case where one end of the column is the upper end and the other end is the lower end, a recess is provided on the lower surface of the first lid body in almost the entire area except for the outer peripheral edge. A plurality of ridges extending radially from the vicinity of the inlet are provided on the ceiling surface, Centripetal direction of the distal end of the strip, said those characterized that you located inside the outer periphery of the low liquid permeable portion.

  A liquid chromatography apparatus according to a second aspect is the liquid chromatography apparatus according to the first aspect, wherein the thin plate or the thin film is welded to a vicinity of the inlet of the filter.

  A liquid chromatography apparatus according to a third aspect is the liquid crystal chromatography apparatus according to the first or second aspect, wherein the thin plate or the thin film is made of a pore sheet.

  According to a fourth aspect of the present invention, there is provided the liquid chromatography apparatus according to any one of the first to third aspects, wherein the filter is formed of a mesh welded body.

  In the liquid chromatography apparatus of the present invention, the liquid that has flowed in through the inlet of the lid spreads widely along the filter upon hitting the low-permeability thin plate or thin film of the filter, and then passes through the filter. In contact with the filler.

  In the liquid chromatography apparatus of the present invention, a thin plate or thin film with low liquid permeability is attached to the surface of the filter facing the lid, and a separate disk as described in Patent Document 2 is not necessary.

  In order to adhere a thin plate or thin film having a low liquid permeability to the vicinity of the inlet of the opposed surface of the filter, it is convenient and preferable to deposit the thin plate or thin film. Further, when this thin plate or thin film is welded, since no adhesive is used, there is no elution of adhesive components from the adhesive, and contamination of the liquid is prevented.

It is a longitudinal cross-sectional view of the liquid chromatography apparatus which concerns on embodiment. It is a disassembled perspective view which shows an upper cover body and a filter. It is an enlarged view of the inflow port part of FIG. It is an example of a chromatogram.

  Hereinafter, embodiments will be described with reference to the drawings.

  FIG. 1 is a longitudinal sectional view of a liquid chromatography apparatus according to an embodiment, FIG. 2 is an exploded perspective view showing an upper lid and a filter, and FIG. 3 is an enlarged view of an inlet portion of FIG.

  The liquid chromatography apparatus 1 includes a cylindrical column 2, a packing 3 packed in the column 2, an upper lid 4 disposed on the upper end side of the column 2, and a lower lid disposed on the lower end side. A body 5, an upper filter 6 disposed on the lower side of the upper lid body 4, and a lower filter 7 disposed on the upper side of the lower lid body 5 are provided.

  The lids 4 and 5 are both disc-shaped, and an inflow port 8 is provided at the center of the lid 4 so as to penetrate the disc in the thickness direction, and the outflow port 12 is provided at the center of the lid 5. Is provided.

  A circular recess 4 a is provided on the lower surface of the lid 4. The recess 4 a is provided in almost the entire region other than the outer peripheral edge of the lower surface of the lid 4. A plurality of streaks (projections) 9 extending in the radial direction from the vicinity of the inflow port 8 are provided on the ceiling surface 13 of the recess 4a. The streaks 9 protrude from the ceiling surface 13 with a height of preferably about 1 to 10 mm, particularly preferably about 2 to 6 mm, and between the streaks 9 are streaks extending in the radial direction on the outer peripheral side of the lid body 4. (Projections) 10 is provided. The height of the muscle 10 is the same as that of the muscle 9.

  On the upper surface of the lower lid 5, a disc-shaped recess 5 a is provided. On the bottom surface 14 of the recess 5a, a streak 11 extending in the radial direction from the vicinity of the outlet 12 is provided so as to protrude from the bottom surface preferably at a height of about 1 to 10 mm, particularly preferably about 2 to 6 mm. Between the muscles 11, a muscle (not shown) similar to the muscle 10 is provided that extends radially on the outer peripheral side of the lid 5. Note that the recess 5 a has the same diameter as the inner diameter of the column 2.

  The tips of the muscles 9 and 11 in the centripetal direction (opposite to the radial direction) are preferably separated from the inlet 8 or the outlet 12 by 300 mm or less, particularly about 5 to 250 mm.

Centripetal direction of the distal end of the muscle 9,11, low liquid permeability portion 6a will be described later, is preferably located on the inner side (center side of the filter 6, 7) than the outer periphery of 7a, but is not limited thereto.

The radial tips of the streaks 9 to 11 preferably reach the peripheral wall surfaces of the recesses 4a and 5a, but may be slightly separated (for example, about 2 mm or less) from the peripheral wall surfaces. The total number of the streaks 9, 10 is preferably about 3 to 300, particularly about 4 to 150 . The same applies to the number of lines of the lid 5.

  The filter 6 has a disk shape having a diameter equal to the diameter of the recess 4a, and the filter 7 has a disk shape having a diameter equal to the diameter of the recess 5a.

  In this embodiment, each of the filters 6 and 7 is preferably made of a laminated welded body in which a plurality of meshes, preferably metal meshes (metal mesh), are laminated and welded at least on the outer peripheral side. You may comprise by the porous body etc. which were shape | molded and sintered to plate shape. In order to weld metal meshes together, it is preferable to perform heat welding, high frequency welding, or ultrasonic welding.

  The wire diameter of the metal mesh is preferably about 0.01 to 3 mm, and the opening is preferably about 10 to 3000 mesh, but is not limited thereto. The thickness of the filters 6 and 7 is preferably about 2 to 10 mm, but is not limited thereto.

  In the center of the upper surface of the filter 6 and the center of the lower surface of the filter 7, low liquid-permeable portions 6a and 7a are provided, respectively. The low liquid permeability portions 6a and 7a are formed by attaching, preferably welding, a thin plate or thin film having low liquid permeability to the center of the filters 6 and 7. The filter and the thin plate or thin film are welded only on the outer periphery of the thin plate or thin film. To weld the thin plate or thin film to the filters 6 and 7, it is preferable to perform heat welding, high frequency welding, or ultrasonic welding. The thickness of the thin plate or thin film is preferably 5 mm or less, particularly preferably about 1 to 2 mm. The thin plate or thin film may be a non-porous plate or membrane, or may be a pore sheet having fine pores.

  As materials for the filters 6 and 7 and the low liquid-permeable portions 6a and 7a, it is preferable to use metals having low elution and high strength, such as stainless steel, nickel chromium, and titanium. Stainless steel is particularly preferable because it can be used at a lower cost than nickel chromium or titanium.

  The low liquid permeability portions 6a and 7a are circular regions, and the diameter of the low liquid permeability portion 6a is preferably 1 to 10 times, particularly 2 to 5 times the diameter of the inflow port 8. The diameter of the low liquid permeability portion 7a is preferably 1 to 10 times, particularly 2 to 5 times the diameter of the outlet 12.

  The water permeation rate at the center of the filter provided with the low liquid permeation portions 6a, 7a may be 50% or less, particularly 3-30%, of the water permeation rate at the filter outer peripheral portion where the low liquid permeation portions 6a, 7a are not provided. preferable. The amount of water permeation of the low liquid permeable portions 6a and 7a is preferably less than 0 because it is easy to equalize the amount of liquid outflow on the entire surface of the filter.

  The lid body 4 has a piston shape fitted inside the column 2. The lid 5 is fixedly connected to the lower end of the column 2. By pressing the lid 4 downward, the filler 3 is densified and a uniform filler layer is formed.

  In the liquid chromatography apparatus 1 configured as described above, the liquid to be processed is supplied from the inlet 8 to the inside. As shown in FIG. 3, this liquid strikes the low liquid permeability portion 6a facing the inlet 8 and changes its direction in the radial direction. The liquid is guided by the streaks 9 and 10 and spreads over the entire upper surface of the filter 6. It permeates, contacts with the filler 3 and is subjected to chromatographic separation. The liquid that has passed through the filler 3 flows out through the filter 7 and the outlet 12.

  In this embodiment, since the filter 6 is provided with the low liquid permeability 6a, the liquid from the inlet 8 is widely dispersed in the radial direction. Moreover, since the low liquid-permeability part 7a is provided also in the center part of the filter 7 facing the outflow port 12, the liquid which descend | falls in the layer of the filler 3 also distributes the whole region of the filter 7 equally. After permeation, it passes through the muscles 11 and is collected at the outlet 12. Therefore, chromatographic processing with high separation performance can be performed. FIG. 4 shows a chromatogram of a dye predicted using a CFD (Computational Fluid Dynamics) analysis technique. Compared with “Without low liquid permeability”, “With low liquid permeability” according to the present invention, the liquid flowing in from the inlet spreads quickly and is uniformly dispersed in the packing layer. It is recognized that a sharp chromatogram is shown.

  In this embodiment, the low liquid-permeability portions 6a and 7a are formed by welding thin plates or thin films to the filters 6 and 7, the configuration is simple, and the apparatus cost is low.

DESCRIPTION OF SYMBOLS 1 Liquid chromatography apparatus 2 Column 3 Packing agent 4,5 Cover body 6,7 Filter 6a, 7a Low liquid permeability part 8 Inflow port 9,10,11 Muscle

Claims (5)

A first lid is attached to one end of the column filled with packing material, and a second lid is attached to the other end,
A liquid inlet is provided at the center of the first lid, and a liquid outlet is provided at the center of the second lid.
In the liquid chromatography apparatus in which a porous plate-like filter is disposed between the first lid and the filler,
A low liquid permeable portion formed by adhering a thin plate or a thin film having a lower liquid permeability than the filter is provided in the vicinity of the inlet of the surface facing the first lid of the filter,
When one end of the column is the upper end and the other end is the lower end, a concave portion is provided on the lower surface of the first lid body except for the outer peripheral edge thereof, and the inlet of the inlet is formed on the ceiling surface of the concave portion. A liquid chromatography apparatus, wherein a plurality of ridges extending radially from the vicinity are provided, and the tips of the ridges in the centripetal direction are located inside the outer periphery of the low liquid permeability portion.   2. The liquid chromatography apparatus according to claim 1, wherein the thin plate or the thin film is welded to a vicinity of the inlet of the filter.   3. The liquid chromatography apparatus according to claim 1, wherein the thin plate or the thin film is made of a pore sheet.   4. The liquid chromatography apparatus according to claim 1, wherein the filter is a mesh welded body. 5. The column according to claim 1, wherein the column has a cylindrical shape, the first lid and the second lid have a disk shape, and the filter has the concave portion of the first lid. A plurality of first ridges extending in the radial direction from the vicinity of the inflow port on the ceiling surface of the concave portion, and having a diameter of 1 to 10 mm from the ceiling surface. Protruding at a height, and between the first ridges, a second ridge extending in the radial direction on the outer peripheral side of the lid is provided protruding at a height of 1 to 10 mm. And
The tip of the first ridge in the centripetal direction is separated from the inflow port by 5 to 250 mm,
The radial tips of the first and second ridges reach the peripheral wall surface of the recess,
The liquid chromatographic apparatus, wherein the low liquid permeability portion is a circular region, and the diameter of the low liquid permeability portion is 1 to 10 times the diameter of the inlet.

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