JP2010078419A - Liquid chromatographic apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a liquid chromatographic apparatus capable of preventing a liquid from staying at a column corner, and equalizing liquid flows in the column. <P>SOLUTION: The liquid chromatographic apparatus 1 includes a cylindrical column 2, a filler 3 filling the column 2, a cover 4 located on the upper end of the column 2, a cover 5 located on the lower end, an upper filter 6 located on the lower side of the cover 4, and a lower filter 7 located on the upper side of the lower cover 5. A tapered circular 4b is provided on the undersurface circumference of the cover 4. A tapered circular 2b is provided on the lower internal-circumference of the column 2. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a liquid chromatography apparatus, and more particularly to a liquid chromatography apparatus configured to uniformize the flow of liquid in a column.

  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 lids are provided at both ends of the column.

  The inflow side cover body is provided with an inflow hole, and a flow path for distributing the liquid flowing in from the inflow hole in the radial direction of the cover body. The lid on the outflow side is provided with an outflow hole and a liquid collecting flow path for collecting the liquid flowing through the filler in the centripetal direction toward the outflow hole.

  On the filler side of these lids, porous plate-like members called filters, screens or frit are arranged, respectively. This filter, screen 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. This filter also disperses the liquid sample to be used for separation / purification in the column cross-sectional direction and allows the liquid sample to flow in the piston flow without backflowing from one end to the other. Have

  An example of such a liquid chromatography apparatus (Japanese Patent Laid-Open No. 2000-65813) is shown in FIG.

  A first lid 21 is provided at the upper end of the cylindrical column 20, and a second lid 22 is provided at the lower end.

  The inflow liquid from the inflow hole 21a of the lid 21 passes through the tapered distribution chamber 21b, the support disk 23, and the screen (filter) 24, descends in the packing layer in the column 20, and is chromatographed.

This liquid is taken out through the lower screen 24, the support disk 23, the tapered liquid collection chamber 22b, and the outflow hole 22a.
JP 2000-65813 A

  In the liquid chromatography apparatus disclosed in Japanese Patent Application Laid-Open No. 2000-65813, the liquid tends to stay near the corner portion C between the screen 24 and the inner peripheral surface of the column 20, and the uniform flow of the liquid in the column is hindered. The

  An object of the present invention is to provide a liquid chromatography apparatus capable of preventing the liquid from staying at the column corner and making the liquid flow in the column uniform.

  In the liquid chromatography apparatus according to claim 1, a first lid is attached to one end of a column packed with a packing material, and a second lid is attached to the other end. In the liquid chromatography apparatus provided with an inflow port, and provided with a liquid outflow port in the second lid, at the corner between the packing-side surface of the first lid and the inner circumferential surface of the column, A taper-shaped cross-sectional first annular portion having an inner diameter that increases with distance from the first lid is provided.

  A liquid chromatography apparatus according to a second aspect of the present invention is the liquid chromatography apparatus according to the first aspect, wherein the inner diameter increases as the distance from the second lid body increases in the corner portion between the packing-side surface of the second lid body and the inner circumferential surface of the column. A second annular portion having a tapered cross-sectional shape is provided.

  A liquid chromatography apparatus according to a third aspect is characterized in that, in the first or second aspect, the annular portion is provided integrally with the lid.

  A liquid chromatography apparatus according to a fourth aspect is the liquid chromatography apparatus according to the first or second aspect, wherein the annular portion is provided integrally with the column.

  In the liquid chromatography apparatus of the present invention, the annular portion having the tapered cross-sectional shape is provided at the corner portion between the first lid body on the inflow side and the inner peripheral surface of the column. And the flow of the liquid in the filler layer becomes uniform.

  In the liquid chromatography apparatus of the present invention, by providing an annular portion having a tapered cross-sectional shape at the corner portion between the second lid and the inner peripheral surface of the column, liquid retention at the corner portion is prevented, and the filler layer The flow of liquid inside becomes uniform.

  The annular portion may be provided integrally with the lid or may be provided integrally with the column.

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

  1 (a) is a longitudinal sectional view of a liquid chromatography apparatus according to an embodiment, FIG. 1 (b) is an enlarged view of the lower part thereof, FIG. 2 is an exploded perspective view showing a lid and a filter, and FIG. The figure is an enlarged view of the inlet portion of FIG. FIG. 4 is a sectional view showing another embodiment.

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

  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 9 extending in the radial direction from the inflow port 8 are provided on the ceiling surface of the recess 4a, and between the streaks 9 extend radially in the outer peripheral side of the lid body 4. An existing muscle 10 is provided. These lines 9 and 10 protrude at a height of about 2 mm from the ceiling surface of the recess 4a.

  An annular portion 4 b projects from the outer peripheral edge of the lid 4 downward. The outer peripheral surface of the annular portion 4b is a straight cylindrical surface that overlaps with the inner peripheral surface of the column 2, but the inner peripheral surface is a tapered surface that approaches the inner peripheral surface of the column downward. Therefore, the annular portion 4b has a tapered cross-sectional shape in which the inner diameter increases toward the lower side.

  On the upper surface of the lower lid 5, a disc-shaped recess 5 a is provided. On the upper surface of the recess 5a, a streak 11 similar to the streak 9 extending in the radial direction from the outlet 12 is provided, and the outer peripheral side of the lid body 5 extends in the radial direction between the streaks 11. A muscle (not shown) similar to the muscle 10 is provided.

  The inner peripheral surface immediately above the lid 5 in the lower part of the column 2 is an annular portion 2b having a tapered cross-sectional shape with an inner diameter decreasing toward the lower side. The concave portion 5a has the same diameter as the inner diameter of the lower end of the annular portion 2b.

  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 made of a porous body obtained by laminating and sintering a metal mesh.

  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-permeable portions 6a and 7a are formed by cutting the central portions of the filters 6 and 7 and clogging the pores of the filters 6 and 7. This cutting process can be performed by rotating a grindstone or a drill or rotating a blade such as a sword. A grindstone or a cutting edge may be ultrasonically vibrated.

  The low liquid permeability portion may be formed by other means such as partial melting by laser irradiation.

  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 lid body 4 has a piston shape fitted inside the column 2. The lid 5 is fixedly connected to the flange 2 a at 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.

  A concave step 2c is provided along the inner periphery of the column 2 on the lower side of the inner periphery of the annular portion 2b. On the upper surface of the lid 5, a protrusion 5 b that engages with the recessed step 2 c is provided around. An O-ring receiving groove is provided around the upper end surface of the ridge 5b and the ceiling surface of the recessed step portion 2c, and the O-ring 12 is disposed.

  The taper angle θ of the annular portions 4b and 2b is preferably about 5 to 85 °, particularly about 20 to 70 °.

  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 passes through the filter 7, passes between the muscles 11, and flows out from the outlet 12.

  In this embodiment, since the annular portions 4b and 2b are provided, the retention of the liquid at the corner portion between the lids 4 and 5 and the inner peripheral surface of the column 2 is prevented, and the liquid in the layer of the filler 3 is prevented. The flow is uniform.

  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 passing through, it is guided by the muscle 11 and collected at the outlet 12. Therefore, chromatographic processing with high separation performance can be performed.

  In this embodiment, the ridge 5b and the recessed step 2c are engaged. And when the outer peripheral surface of the convex part 5b closely_contact | adheres to the vertical inner peripheral surface of the concave step part 2c, the hydraulic pressure applied to the O-ring 12 is reduced, and a sealing property becomes favorable.

[Another embodiment]
In the above embodiment, the lower (outflow side) annular portion 2 b is provided in the column 2, but the lid 5 may be provided with an annular portion. FIG. 4 shows an example thereof, and an annular portion 5c is provided on the upper surface of the lid 5A so as to stand along the inner peripheral surface of the column 2A. The inner peripheral surface above the filter 7 of the annular portion 5c is a tapered surface 5d whose inner diameter increases toward the upper side. The inner peripheral surface of the column 2A has a straight cylindrical shape.

  An O-ring 13 is disposed between the lower end surface of the column 2A and the outer peripheral side of the annular portion 5c of the lid 5A. Also in this case, since the outer peripheral surface of the annular portion 5c is in close contact with the inner peripheral surface of the column 2A, the hydraulic pressure applied to the O-ring 13 is reduced.

  Although illustration is omitted, a tapered annular portion may be provided on the column also on the upper end side of the column.

  In the above-described embodiment, the lid 4 is a piston-type movable type and the lids 5 and 5A are fixed types, but may be reversed. Further, both the upper and lower lids may be piston-type movable types, and both may be fixed types.

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

Explanation of symbols

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

Claims (4)

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,
In the liquid chromatography apparatus, wherein the first lid is provided with a liquid inlet, and the second lid is provided with a liquid outlet.
A first annular portion having a tapered cross-sectional shape having an inner diameter that increases with distance from the first lid is provided at a corner between the packing-side surface of the first lid and the inner circumferential surface of the column. A liquid chromatography apparatus characterized by the above.   2. The second annular shape according to claim 1, wherein the second cover body has a tapered cross-sectional shape with an inner diameter that increases with distance from the second cover body at a corner portion between the packing-side surface of the second cover body and the inner circumferential surface of the column. A liquid chromatography apparatus provided with a section.   3. The liquid chromatography apparatus according to claim 1, wherein the annular portion is provided integrally with the lid.   3. The liquid chromatography apparatus according to claim 1, wherein the annular portion is provided integrally with the column.

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