JP5736732B2 - Chromatography column and its movable stopper - Google Patents

Description

  The present invention relates to a movable stopper used in a column for liquid chromatography (hereinafter sometimes referred to as a chromatography column), and a chromatography column using the movable stopper.

  Liquid chromatography is widely used as a means for separating and purifying target substances in natural products, fermentation products, cultured products by gene recombination and the like, and synthesis reaction products at a target purity and purification rate.

  Conventionally, packing of a packing material into a column for liquid chromatography has been performed by a method as shown in FIG.

  That is, first, as shown in FIG. 6 (a), a slurry prepared by using a column 2 equipped with a movable stopper 1 and mixing a filler with a solvent in this column 2 as shown in FIG. 6 (b). 3 is thrown. Then, as shown in FIG. 6 (c), a solvent outlet is provided at the upper part of the column, and an upper lid 4 having a porous plate for preventing the outflow of the packing material is attached. Extruding from the solvent outlet, as shown in FIG. 6 (d), the packed bed 5 of filler is formed under pressure. That is, the movement of the movable stopper 1 causes a uniform filling layer to be laminated from the side opposite to the movable stopper. After the filling is completed, the pressure of the filling layer 5 by the movable stopper 1 is maintained. This packing apparatus is widely known as an axial compression type column.

  A seal structure is provided between the movable stopper and the inner peripheral surface of the column so that the liquid and the packing material are not leaked.

  Conventional seal structures between the movable stopper and the inner peripheral surface of the column include, for example, an O-ring seal and a seal that removes and seals compressed air after the movable stopper has moved to a predetermined position (Japanese Patent No. 4098342). is there.

  However, the O-ring seal has a gap between the O-ring seal portion and the inner wall surface of the column main body, and not only is it easy to vent air from the gap portion, but it also becomes a filler and a liquid pool, resulting in contamination and purification efficiency. Causes a drop.

  In addition, the sealing structure of the above-mentioned Patent No. 4098342 is applied with a compression medium, the seal part is moved backward to loosen, the movable stopper is moved to a predetermined position in the column, and thereafter the pressure by the compression medium is removed. The sealing material is pressed and sealed by the acting force of the spring. In this method, in order to move the movable stopper after loosening the seal, when the packing is filled in the column in advance, when the movable stopper is brought into contact with the surface of the packed bed, the slurry-like filler is sealed. In addition to entering the inner wall surface of the column due to capillary action, the sealing state deteriorates, and the gap formed becomes a liquid pool, causing contamination and reducing chromatographic separation and purification efficiency. Further, the pressing force of the spring varies with the elapsed time due to deterioration of the spring repulsive force, and it is difficult to maintain a certain sealing accuracy. Furthermore, in order to prevent the filler slurry from entering between the seal part and the inner wall surface of the column, when the movable stopper is moved with little or no loosening of the seal, it is not easy to move the seal. However, it is difficult to predict the replacement time, and the replacement time, labor, and cost of the sealing material are required. Not economical.

  Therefore, the inventors previously filed an application for the movable stopper shown in FIG. 7 (Japanese Patent Application No. 2010-059392). The movable stopper 110 of FIG. 7 surrounds the outer periphery of the movable stopper core, the annular scraper 130, the base 140 having the recess 141 in which the proximal end of the movable stopper core is fitted. The packing 150 includes packing adapters 151 and 152 on both upper and lower sides thereof, and a bolt 160 that attracts the movable plug core 120. The scraper 130 is engaged with the flange portion 122 of the movable plug core. A tapered surface is provided on the flange portion 122 of the scraper 130 and the movable plug core 120.

  In the movable plug 110 of FIG. 7, the movable plug core 120 is attracted to the base 140 side by rotating the bolt 160, and the V packing 150 is sandwiched between the scraper 130 and the base 140. It bulges in the direction of diameter expansion. When the V packing 150 abuts on the inner peripheral surface of the chromatography column, the V packing 150 and the inner peripheral surface of the column are sealed.

  However, in the movable stopper 110 of FIG. 7, since sealing is mainly performed between the V packing 150 and the inner peripheral surface of the column, the gap between the scraper 130 and the inner peripheral surface of the column above the V packing 150 is between. There is a risk of fillers and liquids entering. In addition, if the outer diameter of the scraper 130 before inserting the column is sufficiently larger than the inner diameter of the column to prevent such intrusion, the movable stopper 10 is not easily moved, and the scraper 130 is heavily worn. The life of the scraper 130 is shortened and needs to be replaced frequently.

Patent No. 4098342 Japanese Patent Application No. 2010-059392

  The present invention solves the above-mentioned conventional problems, and provides a movable stopper capable of improving the operability, reliability, economy and separation / purification efficiency of liquid chromatography, and a chromatography column equipped with this movable stopper. For the purpose.

The movable stopper of the present invention (first aspect) is a movable stopper arranged in a liquid chromatography column, the tip of the movable stopper faces the packing material, and the axial center of the movable stopper extends in the axial direction of the column. A movable stopper core, an annular scraper externally fitted to the outer periphery of the distal end side of the movable stopper core, a base having a recess in which a proximal end side of the movable stopper core is internally fitted, and the scraper and the base A scraper pressing means provided therebetween, and a pulling means for pulling the movable plug core in the direction of pushing the movable plug core into the recess of the base. The scraper is engaged with the flange portion, and the scraper can be deformed in the diameter increasing direction when sandwiched between the scraper pressing means and the flange portion. Is.

The movable stopper of the second aspect is the first aspect , wherein the flange portion has a tapered surface having a diameter that is enlarged toward the distal end side of the movable stopper core, and the inner peripheral surface of the scraper is It has the taper surface which overlaps with the taper surface of a stopper core, It is characterized by the above-mentioned.

The movable stopper of the third aspect is characterized in that, in the second aspect , a space for receiving the proximal end side of the tapered surface of the flange portion at the time of the clamping is provided on the distal end side of the scraper pressing means. Is.

In the movable plug of the fourth aspect according to the second or third aspect , the movable plug core has the flange portion and a cylindrical portion connected to the proximal end portion of the flange portion, and the cylindrical portion is the flange portion. The taper surface has a smaller diameter than the base end portion, and the boundary between the tip end portion of the cylindrical portion and the base end portion of the taper surface of the flange portion is a stepped portion, and the base end portion of the scraper is Further, the step extends to the base end side of the movable plug core from the stepped portion.

In any one of the first to fourth aspects, the movable stopper according to the fifth aspect is characterized in that the scraper pressing means has a flexibility that can be deformed during the clamping .

Movable plug of the sixth aspect, in any one aspect of the first to fifth, wherein the attracting means, characterized in that through said base is a bolt which is screwed into the movable plug core is there.

Column of the onset Ming liquid chromatography is one in which movable plug according to any one aspect of the first through 6 disposed therein.

In the movable stopper of the present invention and the chromatographic column equipped with this movable stopper, the scraper is clamped by the scraper pressing means and the flange portion by attracting the movable stopper core to the base, and the scraper itself expands in diameter. Contact the peripheral surface. Thereby, the fine particles and fine particle slurry in the column are prevented from entering between the scraper and the inner peripheral surface of the column.

In the movable stopper of the second aspect , when the movable stopper core is attracted to the base, the scraper moves along the taper surface of the flange portion, so that the diameter of the scraper is well expanded and contacts the inner peripheral surface of the column. To do.

In the movable plug of the third aspect , when the movable plug core is attracted to the base, a part of the proximal end side of the tapered surface of the flange portion is accommodated in the space of the scraper pressing means. Until this housing is completed, the scraper pressing means can reliably press the scraper without being obstructed by the tapered surface of the flange portion.

In the movable stopper of the fourth aspect , the scraper extends from the stepped portion to the proximal end side of the movable core. Accordingly, the scraper pressing means can reliably press the scraper without being obstructed by the tapered surface over a distance extending from at least the stepped portion.

The scraper pressing means may have a flexibility that can be deformed during clamping . In this case, the scraper pressing means can be deformed to give a good pressing force to the scraper.

  The means for pulling the movable plug core toward the base may be a bolt. Although not shown, the movable stopper core and the base may be screwed together.

It is sectional drawing of the movable stopper which concerns on 1st Embodiment. It is sectional drawing of the movable stopper which concerns on 2nd Embodiment. It is sectional drawing of the movable stopper which concerns on 3rd Embodiment. It is sectional drawing of the movable stopper which concerns on 4th Embodiment. It is sectional drawing of the movable stopper which concerns on 5th Embodiment. It is sectional drawing which shows a prior art example. It is sectional drawing which shows another prior art example.

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

  FIG. 1 (a) is a sectional view in the axial center direction of the movable stopper according to the first embodiment, and FIG. 1 (b) is a sectional view of a state in which a porous plate is attached to the tip of the movable stopper. .

  The movable stopper 10 includes a movable stopper core 20, a scraper 30, a base 40, a seal ring (scraper pressing means) 50, and the like. This movable stopper 10 is arranged so that the tip side (the upper end side in the figure) is in contact with the packing material in the column. The movable plug core 20 is formed of a substantially cylindrical body that extends from the distal end of the movable plug 10 in the axial direction. From the middle of the movable plug core 20 to the base end side (the lower end side in the figure) is a cylindrical portion 21 having an equal diameter. Above the cylindrical portion 21 is a flange portion 22.

  The lower surface of the flange portion 22 is a tapered surface 22a whose diameter increases toward the top. A shallow circular recess 23 is provided on the upper end surface of the movable plug core 20, and an enlarged diameter step portion 24 is formed on the upper side of the side peripheral surface of the recess 23. By engaging with the stepped portion 24, the porous plate 25 is attached to the distal end surface of the movable plug core 20, and between the porous plate 25 and the bottom surface of the recess 23, the liquid is supplied and collected or discharged. Vacancy is formed.

  A communication hole 26 for supplying or discharging the liquid is provided so as to penetrate from the center of the bottom surface of the recess 23 to the center of the bottom surface of the movable plug core 20.

  A female screw hole 27 into which a bolt 60 described later is screwed is provided on the bottom surface of the movable plug core 20 in a direction parallel to the axis of the movable plug 10.

  The scraper 30 is an annular member fitted to the outer periphery of the flange portion 22. The outer peripheral surface of the scraper 30 is a cylindrical surface having an equal diameter. The inner peripheral surface of the scraper 30 includes a tapered surface 31 that overlaps the tapered surface 22a. The bottom surface of the scraper 30 is perpendicular to the axis of the movable stopper 10. The sectional shape of the annular scraper 30 in the direction orthogonal to the circumferential direction is a right triangle. The base end surface of the scraper 30 has the same height as the lower end of the tapered surface 22a.

  Although the base 40 has a substantially cylindrical shape, a concave portion 41 into which the lower portion of the movable plug core 20 is fitted is provided at the center of the upper surface. A liquid circulation hole 42 is provided to circulate from the bottom surface of the recess 41 to the bottom surface of the base 40. In this embodiment, the base 40 is provided with an insertion hole 43 for the bolt 60.

  The seal ring 50 is provided so as to go around the movable stopper core 20 between the scraper 30 and the base 40. The cross-sectional shape of the seal ring 50 is not particularly limited, and may be an O-ring having a circular or elliptical cross-sectional shape. The cross-sectional shape may be a triangle, quadrangle, pentagon, hexagon, heptagon, octagon, or the like. It may be a square shape, a star shape, a four-leaf shape, or the like. The shape of the seal ring 50 is not limited to a ring shape (circular shape), and may be provided so as to go around one or more string shapes, and can be practically used in a large column having a column diameter of about several meters.

  The bolt 60 is screwed into the female screw hole 27 through the insertion hole 43. After the head portion of the bolt 60 comes into contact with the bottom surface of the base 40, the movable plug core 20 is attracted to the base 40 side by further rotating the bolt 60.

In the movable stopper 10, the outer diameter of the scraper 30 before inserting the column is equal to or slightly larger than the inner diameter of the column in the state before the above-mentioned pulling, and the outer peripheral surface of the scraper 30 is made to be It is preferable to press against the inner peripheral surface. More specifically, the inner diameter of the column and _{d 1,} if the outer diameter of the scraper 30 (diameter) was _{d 2, d 2} -d ₁ is less than 3%, especially 2% larger and _{d 1} than 0 among others 1 % Or less is preferable.

  The taper angle θ (see FIG. 1 (a)) of the taper surfaces 31 and 22a of the scraper 30 and the flange portion 22 is preferably 5 ° or more and less than 90 °, particularly about 15 to 60 °.

As the material of the scraper 30, a material that can be deformed in the diameter increasing direction when sandwiched between the seal ring (scraper pressing means) 50 and the tapered surface 22 a of the flange portion 22 is used. The material of the scraper 30 is preferably rubber such as natural rubber, EPDM rubber, urethane rubber, chloroprene rubber, nitrile rubber, butyl rubber, or fluororubber. Further, fluorinated resins such as polytetrafluoroethylene, partially fluorinated resins such as polychlorotrifluoroethylene, polyvinylidene fluoride, polyvinyl fluoride and fluorinated resin copolymers such as perfluoroalkoxy fluororesin, four Preferred are a fluorinated ethylene-hexafluoropropylene copolymer and an ethylene-tetrafluorinated ethylene copolymer. In addition to these, a fluorinated resin, a partially fluorinated resin, a rubber coated with a fluorinated resin copolymer, and the like can also be applied.

  The material of the movable plug core 20 is preferably a corrosion-resistant metal such as stainless steel, titanium, or hastelloy, but may be a synthetic resin such as fluororesin, polypropylene, polyethylene, polysulfone, acrylic, or methylpentene.

A preferable material of the base 40 is exemplified by the same material as that of the movable plug core 20, but is not limited thereto. It is preferable the outer diameter of the base 40 is smaller than the inner diameter d ₁ of the column is preferred, and more intermediate values of the inner and outer diameters of the packing adapter 52.

  The material of the seal ring 50 is exemplified by the same material as that of the scraper 30, but is not limited thereto.

  When the movable stopper 10 configured as described above is mounted in the column, the movable stopper 10 is inserted into the column and disposed at a desired position, and then the bolt 60 is rotated. As a result, the scraper 30 is clamped by the seal ring (scraper pressing means) 50 and the taper surface 22a of the movable plug core 20, and the scraper 30 is moved upward along the taper surface 22a relative to the taper surface 22a. The scraper 30 expands in diameter. The scraper 30 having an enlarged diameter is pressed against the inner peripheral surface of the column, whereby the scraper 30 and the inner peripheral surface of the column are firmly sealed. Thereby, a filler and a liquid do not enter between the scraper 30 and the inner peripheral surface of the column, and a liquid pool does not occur. As a result, the purification and separation efficiency is improved.

  In the present embodiment, the seal ring 50 is also pinched by the scraper 30 and the base 40 when the bolt 60 is rotated, and is deformed in the diameter increasing direction. The expanded seal ring 50 is pressed against the inner peripheral surface of the column, whereby the seal ring 50 and the inner peripheral surface of the column are firmly sealed. However, the seal ring 50 may not be pressed against the inner peripheral surface of the column when the bolt 60 rotates.

  In the chromatographic column in which the movable stopper 10 is inserted, the liquid is introduced into or out of the column through the holes 42 and 26 and the perforated plate 25. Since the packing material in the column does not enter between the movable stopper 10 and the inner peripheral surface of the column, the chromatographic separation and purification efficiency is high.

  In the movable stopper 10, the scraper 30 and the seal ring 50 can be easily replaced by removing the bolt 60 and separating the base 40 and the movable stopper core 20.

  When the movable stopper 10 in the seal is moved to the packing material side (upward in FIG. 1), the scraper 30 is forced to move downward along the tapered surface 22a by the frictional force from the inner circumferential surface of the column. Will be added. However, a pressing force is applied to the scraper 30 from the seal ring 50. The balance between the frictional force and the pressing force prevents the filler from entering between the scraper 30 and the inner circumferential surface of the column, while the movable stopper 10 smoothly moves toward the filler (upward in FIG. 1). Move to. On the other hand, when the movable stopper 10 in the seal is moved to the side opposite to the packing material (downward in FIG. 1), the scraper 30 moves upward along the tapered surface 22a by the frictional force from the inner circumferential surface of the column. Force is applied in the direction. However, the tapered surface 31 of the scraper 30 is supported by the tapered surface 22a of the flange portion 22, and a pressing force is applied from the tapered surface 22a. The balance between the frictional force and the pressing force prevents the packing material from entering between the scraper 30 and the inner circumferential surface of the column, while the movable stopper 10 is opposite to the packing material (lower side in FIG. 1). To move smoothly.

  The movable stopper according to the second to fifth embodiments will be described with reference to FIGS.

  The movable stopper 11 in FIG. 2 uses a movable stopper core 20A having a long cylindrical portion 21A in the axial direction instead of the movable stopper core 20, and a seal ring 50, between the scraper 30 and the base 40, A disc-shaped partition plate 70 and a seal ring 50A are provided in this order from the top so as to go around the movable stopper core 20A.

  As described above, since the two seal rings 50 and 50A are partitioned by the partition plate 70, the seal rings 50 and 50A are appropriately deformed without being in contact with each other. As a result, the scraper 30 can be pressed well. . Further, since each of the seal rings 50 and 50A is appropriately deformed in the diameter increasing direction and pressed against the inner peripheral surface of the column, the seal rings 50 and 50A and the inner peripheral surface of the column are firmly sealed. Thereby, compared with the case where one seal ring 50 is used like the movable stopper 10 of FIG. 1, a sealing performance improves more. Furthermore, when the movable stopper 11 is moved into the column, the partition plate 70 prevents the seal rings 50 and 50A from being overlapped or entangled, so that the movable stopper 11 moves smoothly.

  The material of the partition plate 70 is preferably rubber such as natural rubber, EPDM rubber, urethane rubber, chloroprene rubber, nitrile rubber, butyl rubber, or fluororubber. Further, fluorinated resins such as polytetrafluoroethylene, partially fluorinated resins such as polychlorotrifluoroethylene, polyvinylidene fluoride, polyvinyl fluoride and fluorinated resin copolymers such as perfluoroalkoxy fluororesin, four Preferred are a fluorinated ethylene-hexafluoropropylene copolymer and an ethylene-tetrafluorinated ethylene copolymer. In addition to these, a fluorinated resin, a partially fluorinated resin, a rubber coated with a fluorinated resin copolymer, a synthetic resin such as polypropylene, acrylic, methylpentene, and polysulfone can also be applied. The thickness of the partition plate 70 is not particularly limited, but is preferably about 1/4 to 3 times the diameter of the seal rings 50 and 50A (the height in the vertical direction in FIG. 2). In FIG. 2, two seal rings 50 and 50A are used. However, this is an example when a plurality of seal rings are used, and three or more seal rings may be used. A partition plate is interposed between the seal rings. The number of seal rings is not limited, but is preferably 4 or less, particularly 2 or less. When the number is two or less, the pressing force from the base 40 can be satisfactorily transmitted from the uppermost seal ring to the scraper 30 via the seal ring and the partition plate 70.

  The movable stopper 12 shown in FIG. 3 is different from the movable stopper 11 shown in FIG. 2 in that two V packings 53 are arranged in a stacked manner in place of the seal ring 50A and the partition plate 70, and packing adapters (wearing rings) are arranged above and below, respectively. ) A laminate in which 51 and 52 are arranged is used. The V packing 53 and the packing adapters 51 and 52 have an inner diameter that is the same as or slightly larger than the outer diameter of the movable plug core 20, and the outer diameter is slightly smaller than the inner diameter of the scraper column. A notch 51a is provided around the inner peripheral surface of the packing adapter 51, and the notch 51a is a space. The V packing 53 and the packing adapters 51 and 52 are arranged on the scraper 30 side (upper side in FIG. 3) from the seal ring 50.

  3, when the bolt 60 is rotated, the packing adapter 51 is pushed upward through the base 40, the seal ring 50, the packing adapter 52, and the V packing 53. At this time, when the notch 51a receives the proximal end (lower end) of the tapered surface 22a of the flange 22, the packing adapter 51 moves relatively upward with respect to the movable plug core 20A. When the movement proceeds to some extent, the outer diameter of the tapered surface 22a received in the notch 51a becomes large, and no further reception becomes possible, and the movement stops.

  Thus, when the packing adapter 51 moves upward relative to the movable plug core 20A, the scraper 30 moves along the tapered surface 22a relative to the tapered surface 22a, The scraper 30 expands in diameter. The scraper 30 having an enlarged diameter is pressed against the inner peripheral surface of the column, whereby the scraper 30 and the inner peripheral surface of the column are firmly sealed. As described above, when the relative upward movement of the packing adapter 51 with respect to the movable plug core 20A stops, the movement of the scraper 30 also stops. Thus, the packing adapter 51 with the notch 51a has a function of limiting the moving distance of the scraper 30. Further, the V packing 53 is squeezed between the scraper 30 and the base 40 and bulges in the diameter increasing direction. When the V-packing 53 comes into contact with the inner peripheral surface of the chromatography column, the movable stopper 12 and the inner peripheral surface of the column are sealed.

  The number of stacked V packings 53 is preferably 2 or more, particularly about 4 to 8 sheets. The packing material is preferably, but not limited to, fluororesin, fluororubber, EPDM, urethane rubber, chloroprene rubber, nitrile rubber, butyl rubber, fluororesin-coated synthetic rubber, and the like.

  Examples of the material for the packing adapters 51 and 52 include fluorinated resins such as polytetrafluoroethylene and partially fluorinated resins such as polychlorotrifluoroethylene, polyvinylidene fluoride, polyvinyl fluoride and fluorinated resin copolymers, For example, a perfluoroalkoxy fluororesin, a tetrafluoroethylene-hexafluoropropylene copolymer, an ethylene-tetrafluorinated ethylene copolymer, and the like are preferable. In addition to these, a rubber coated with a fluorinated resin, a partially fluorinated resin, a fluorinated resin copolymer, a fluororubber, a urethane rubber, a chloroprene rubber, a nitrile rubber, a butyl rubber, EPDM, or the like can also be applied. However, in order to exhibit the function of limiting the moving distance of the scraper 30, the fluorinated resin, for example, polytetrafluoroethylene, or the partially fluorinated resin, for example, polychlorotrifluoroethylene, polyvinylidene fluoride, polyvinyl fluoride. And a hard material such as a perfluoroalkoxy fluororesin, a tetrafluoroethylene-hexafluoropropylene copolymer, an ethylene-tetrafluoroethylene copolymer, or the like is preferably used.

  In the movable stopper 12 of FIG. 3, a disc spring 61 is mounted between the base 40 and the head of the bolt 60. For this reason, elasticity occurs in the connection of the bolt 60. As a result, when an external force is generated in the V packing 53 and the scraper 30, not only the V packing 53 but also the disc spring 61 contracts or expands, and the degree of tightening of the bolt 60 is adjusted. And the deterioration of the V-packing 53 and the scraper 30 can be reduced. In FIG. 3, one disc spring 61 is installed, but the number is not limited, and may be 2 to 12, for example. When a plurality of disc springs are used, the disc springs 61 are overlapped so that the convex portions and convex portions of the pan or the concave portions and the concave portions face each other. The disc spring 61 can be applied as long as the movable plug core 20 is attracted to the base 40 by the bolt 60, and can be applied to other modes (the modes shown in FIGS. 1, 2, and 4).

  The movable stopper 13 of FIG. 4 uses the movable stopper core 20B instead of the movable stopper core 20A in the movable stopper 11 of FIG. 2, and the two V packings 53 are arranged in a laminated form instead of the partition plate 70. A laminated body in which packing adapters (wear rings) 51A and 52A are respectively arranged on the upper and lower sides is used. In the movable plug core 20B, in the movable plug core 20A, the diameter of the lower end of the tapered surface of the flange portion 22 is larger than the diameter of the cylindrical portion 21, and a step portion 22b is provided at the boundary between the tapered surface and the cylindrical portion 21. It is a thing. The lower part of the scraper 30 extends further downward than the stepped part 22b. Although the lower part of the scraper 30 is in contact with the outer peripheral surface of the cylindrical part 21, it may be separated.

  Even in the movable stopper 13 of FIG. 4, by rotating the bolt 60, the scraper 30 is clamped by the taper surface of the seal ring 50 and the movable stopper core 20B, and the scraper 30 is moved along the taper surface. The scraper 30 moves upward relative to the tapered surface, and the diameter of the scraper 30 is increased. The scraper 30 having an enlarged diameter is pressed against the inner peripheral surface of the column, whereby the scraper 30 and the inner peripheral surface of the column are firmly sealed. Further, the seal rings 50, 50A and the V packing 53 are expanded and pressed against the inner peripheral surface of the column, whereby the seal rings 50, 50A and the V packing 53 and the inner peripheral surface of the column are firmly sealed.

  The step 22b in FIG. 4 can be applied to other modes (the modes in FIGS. 1 to 3). For example, in FIG. 3, the movable stopper core 20B may be used instead of the movable stopper core 20A, and the notch 51a may be omitted. In this case, the stepped portion 22b exhibits the function of limiting the moving distance of the scraper 30. Specifically, when the bolt 60 is rotated, the packing adapter 51 moves upward with respect to the movable plug core 20B, but when the bolt 60 is moved upward to some extent, the stepped portion 22b prevents further upward movement. Thus, when the packing adapter 51 moves upward by a predetermined distance, the scraper 30 moves upward by a predetermined distance, and the scraper 30 is expanded in diameter and pressed against the inner peripheral surface of the column. In the case where the notch 51a is not omitted, both the notch 51a and the step 22b exhibit the function of limiting the moving distance of the scraper 30.

  In FIG. 3, the scraper 30 and the packing adapter 51 may be integrally formed. By doing so, it is preferable that no liquid pool is formed between the scraper 30 and the packing adapter 51.

In the movable plugs 10 to 13 shown in FIGS. 1 to 4, the tapered surface 22a is connected directly from the peripheral edge of the upper surface of the flange portion 22. However, as shown in FIG. The peripheral edge may be continuous with the tapered surface 22a via the cylindrical outer peripheral surface 22c. Further, the scraper 30 may also be provided with a cylindrical surface 32 that continues to the upper end of the tapered surface 31. The cylindrical outer peripheral surface 22 c of the flange portion 22 is engaged with the cylindrical surface 32. The height of the cylindrical surface 32 of the cylindrical outer peripheral surface 22c and the scraper 30 of the movable plug core 20 h is preferably at 1/400 or more particularly 1/250 or more inner diameter _{d 1} of the column. Further, h is preferably 20 mm or less, particularly preferably 10 mm or less. Thickness t of the cylindrical surface 32 portion of the scraper 30 is 1/15 of _{d 2,} particularly 1/20 or less.

  The above-described embodiment is an example of the present invention, and the present invention may be configured other than illustrated.

  The movable stopper of the present invention can be applied to a metal column such as stainless steel and a plastic column such as transparent acrylic. In particular, the plastic column has lower processing accuracy than the metal column and may have irregularities on the inner peripheral surface. However, according to the movable stopper of the present invention, the plastic column has good irregularities. Sealing can be performed.

10-13 Movable plug 20, 20A, 20B Movable plug core 22b Stepped portion 30 Scraper 40 Base 50, 50A Seal ring 51, 51A, 52, 52A Packing adapter 51a Notch 53 V packing 60 Bolt 70 Partition plate

Claims (3)

In a movable stopper placed in a liquid chromatography column,
A movable plug core with the tip facing the packing material and extending the axial center of the movable plug in the axial direction of the column;
An annular scraper fitted around the outer periphery of the distal end side of the movable plug core;
A base having a recess in which the proximal end side of the movable plug core is fitted,
Scraper pressing means provided between the scraper and the base;
A pulling means for pulling the movable plug core in a direction of pushing into the recess of the base;
A flange portion is provided on the outer peripheral portion on the distal end side of the movable plug core, and the scraper is engaged with the flange portion,
The scraper is a movable stopper that can be deformed in the diameter increasing direction when sandwiched between the scraper pressing means and the flange portion,
The flange portion has a tapered surface that has a shape whose diameter increases toward the distal end side of the movable plug core,
The inner peripheral surface of the scraper has a tapered surface overlapping the tapered surface of the movable plug core,
The scraper has an outer peripheral surface made of a cylindrical surface, the tapered surface (22a), and a bottom surface perpendicular to the axis of the movable stopper, and has a cross-sectional shape perpendicular to the circumferential direction of the scraper (30). A right triangle,
The movable plug core has the flange portion and a columnar portion connected to the proximal end portion of the flange portion,
The cylindrical portion has a smaller diameter than the proximal end portion of the tapered surface of the flange portion, and the boundary between the distal end portion of the cylindrical portion and the proximal end portion of the tapered surface of the flange portion is a stepped portion (22b). And
The movable stopper characterized by the base end part of the said scraper (30) extending to the base end side of this movable stopper core rather than this level | step-difference part (22b).   2. The movable stopper according to claim 1, wherein the attracting means is a bolt that penetrates the base and is screwed to the movable stopper core.   A liquid chromatography column in which the movable stopper according to claim 1 is disposed.

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