JP2008102077A - Cartridge column and column module - Google Patents

Abstract

A highly reliable cartridge column using a vitreous porous material as a separating material and a column module using the same are provided.
A cartridge column according to the present invention includes a columnar separating material, a deformable tube arranged to cover an outer peripheral surface of the separating material, and a housing holding the separating material and the deformed tube. . The separating material 10 includes a columnar vitreous porous body 11 and a heat shrinkable tube 12 that covers the outer peripheral surface of the vitreous porous body 11. The deformation tube 21 is a tube whose compression rate at 25 ° C. is in the range of 5% to 90%, or is an elastomer tube.
[Selection] Figure 3

Description

  The present invention relates to a cartridge column used for chromatography and a column module using the same.

  In recent years, as a column for chromatography, a column using an integral porous body made of porous silica or the like instead of a powdery separating material has been proposed. As one of such columns, a column using an inorganic porous material (separation material) formed by a sol-gel method has been proposed (see, for example, Patent Documents 1 and 2). A column using an integral inorganic porous body has features such as high separation performance, small variation in separation characteristics, and excellent stability. Such a porous body can be used for high-precision analysis and high-speed separation of DNA.

As one of the columns using an integrated porous body, a column in which the outer peripheral surface of the porous body is protected by a cylinder including a heat shrinkable tube and a thermoplastic resin layer has been proposed (see Patent Document 3).
JP-A-6-265534 JP 7-41374 A JP-A-10-197508

  However, in the case of a column whose outer peripheral surface is protected only by a hard resin, when the column is set in a measuring device or a housing, the separation target may leak at the end or outer peripheral portion of the column. If the separation target leaks, the reproducibility and accuracy of the separation will decrease.

  Under such circumstances, an object of the present invention is to provide a highly reliable cartridge column using a vitreous porous material as a separating material, and a column module using the same.

  In order to achieve the above object, a first cartridge column of the present invention includes a columnar separation material, a tube disposed so as to cover an outer peripheral surface of the separation material, a housing for holding the separation material and the tube, And the compression ratio at 25 ° C. of the tube is in the range of 5% to 90%, and the separating material includes a columnar vitreous porous body and a heat shrinkable tube covering the outer peripheral surface of the vitreous porous body. .

  In addition, the compression rate of a tube is a value when the compression rate of the sheet | seat which consists of the same material is measured at 25 degreeC according to the specification of JIS-R3453.

  The second cartridge column of the present invention includes a columnar separation member, a tube disposed so as to cover an outer peripheral surface of the separation member, and a housing that holds the separation member and the tube, and the tube Is an elastomer tube, and the separating material includes a columnar vitreous porous body and a heat shrinkable tube covering an outer peripheral surface of the vitreous porous body.

  The column module of the present invention is a column module comprising a container that can be filled with a pressurized fluid, and a cartridge column that is disposed in the container. In the first or second cartridge column of the invention, the housing of the cartridge column is configured so that the pressure of the fluid is transmitted to the tube.

  In the cartridge column of the present invention, the outer peripheral surface of the separation material is covered with a tube that deforms greatly, and the separation material and the tube are held by the housing. Therefore, according to this invention, it can suppress that a separation target object leaks in the outer peripheral surface of a vitreous porous body. Moreover, since the outer peripheral surface of a vitreous porous body is protected by the heat-shrinkable tube, it can suppress that a vitreous porous body is damaged. Moreover, according to the column module of the present invention, the separation object can be separated with good reproducibility.

  Embodiments of the present invention will be described below. In the following description, the present invention may be described with specific examples, but the present invention is not limited to the specific examples described below.

[Cartridge column]
The cartridge column of the present invention can be used for chromatography. This cartridge column can be used for separation of substances and extraction of substances.

  Two types of cartridge columns will be described below as the cartridge column of the present invention.

  The first cartridge column of the present invention includes a columnar separating material, a tube disposed so as to cover the outer peripheral surface of the separating material, and a housing for holding the separating material and the tube. Hereinafter, the tube covering the outer peripheral surface of the separation material in the first cartridge column may be referred to as “soft tube”.

  The separating material includes a columnar vitreous porous body and a heat-shrinkable tube that covers the outer peripheral surface of the vitreous porous body. The separating material can be formed by applying heat to the tube and shrinking it in a state where the columnar vitreous porous body is disposed in the non-shrinkable tube. Usually, the thickness of the heat-shrinkable tube is thin, for example, in the range of 0.08 mm to 5 mm (preferably in the range of 0.1 mm to 2.5 mm).

  The compressibility of the flexible tube at 25 ° C. is in the range of 5% to 90%. By using a deformable soft tube, it is possible to press the outer peripheral surface of the separating material so as to correspond to the unevenness of the outer peripheral surface of the separating material. As a result, the separation target can be prevented from leaking on the outer peripheral surface of the vitreous porous body. As described in the description of the second cartridge column of the present invention, the soft tube may be an elastomer tube.

  The compressibility of the flexible tube at 25 ° C. may be in the range of 10% to 88%, for example, in the range of 20% to 60%. Examples of the soft tube include soft polytetrafluoroethylene (hereinafter sometimes referred to as “soft PTFE”). Examples of commercially available soft PTFE include Hyper Sheet (registered trademark) manufactured by Japan Gore-Tex Corporation.

  In the soft tube as an example, the thickness (wall thickness: difference between the outer diameter and the inner diameter) t of the soft tube is in the range of 1.0 mm to 30 mm, and the compressibility at 25 ° C. is in the range of 45% to 67%. .

  The second cartridge column of the present invention includes a columnar separating material, a tube disposed so as to cover the outer peripheral surface of the separating material, and a housing for holding the separating material and the tube. The tube that covers the outer peripheral surface of the separating material is an elastomer tube. The separating material includes a columnar vitreous porous body and a heat-shrinkable tube that covers the outer peripheral surface of the vitreous porous body.

  The elastomer tube is a tube made of an elastomer. An elastomer is a polymer substance having rubber-like elasticity, and a typical example is rubber. The elastomer tube may be a rubber tube. In the following description, elastomer can be read as rubber.

  The elastomer tube may be made of, for example, fluorine rubber, or may be made of silicone rubber or petroleum synthetic rubber. Examples of petroleum synthetic rubber include nitrile rubber (NBR), styrene / butadiene copolymer rubber (SBR), acrylic rubber (ACM), chloroprene rubber (CR), ethylene / propylene rubber (EP), and isobutylene / isoprene copolymer rubber. (IIR). A fluorine-based elastomer (for example, fluororubber) is preferable in terms of high chemical resistance and heat resistance. Examples of the fluororubber include vinylidene fluoride rubber, tetrafluoroethylene-propylene rubber, tetrafluoroethylene-perfluoromethyl vinyl ether rubber (FFKM), and the like. Moreover, as another fluorine-type elastomer, a perfluoroelastomer is mentioned, for example. Among these, perfluoroelastomer and FFKM are preferable because of high chemical resistance and heat resistance.

  The preferred hardness of the elastomer tube varies depending on the thickness t of the elastomer tube. For example, the hardness measured according to a durometer type hardness meter (JIS-K-6253) is in the range of A / 20 to A / 100 (for example, A / 40 to A / 90) or a range of D / 60 or less.

  In the example of the elastomer tube, the thickness (wall thickness) t of the elastomer tube is in the range of 2 mm to 4 mm, and the hardness (JIS-K-6253) is in the range of A / 50 to A / 80.

  The elastomer tube is required to have high elasticity. Therefore, a tube formed of a resin having no rubber-like elasticity such as hard Teflon (registered trademark) or polyether ether ketone (PEEK) cannot be used.

  Hereinafter, the above-described soft tube and elastomer tube may be collectively referred to as “deformed tube”.

  If the thickness (wall thickness) of the deformed tube is too thin, the characteristics of the tube cannot be exhibited sufficiently. Therefore, it is preferable that the thickness t of the deformed tube in the portion where the separating material is accommodated is a certain thickness or more. In one example, the thickness t of the deformed tube in a normal state (a state where no external force is applied) may be 0.1 mm or more (for example, 0.5 mm or more, and 2.5 mm or more in one example). The upper limit of the thickness t is not particularly limited, and may be 20 mm or less, for example.

  The deformation tube usually covers the entire outer peripheral surface of the separating material. However, as long as the effect of the present invention is obtained, the deformable tube may cover substantially the entire outer peripheral surface of the separating material. For example, as long as the effect of the present invention is obtained, the outermost end portion of the separating material may be covered with the deformation tube, or the outermost end region of the separating material may not be covered.

  A heat-shrinkable tube is a tube that does not have rubber-like elasticity. Examples of the heat shrinkable tube include a tube made of a fluorine resin or an olefin resin. Examples of commercially available heat shrinkable tubes include fluororesin pen tubes (manufactured by Pennitto Co., Ltd.). Depending on the object to be separated, the heat-shrinkable tube is preferably formed of a material having high chemical resistance.

  In the cartridge column of the present invention, the vitreous porous body and the heat shrinkable tube are fixed by being in close contact with each other. The separating material may be fixed to the deformable tube in a non-detachable manner, but is usually inserted in a removable manner.

  The length of one deformation tube (the length in the central axis direction of the tube) is usually 1 mm or more (for example, 2 mm or more), and is usually 200 mm or less (for example, 100 mm or less).

  In addition, you may cover the outer peripheral surface of one separating material with a some deformation | transformation tube. In this case, it becomes easy to insert the separating material into the deformable tube. A plurality of separation materials may be arranged in one deformation tube. In addition, a plurality of separation members and a plurality of deformation tubes may be disposed in the housing.

  The vitreous porous body of the separating material is a columnar integrated (monolith type) separating medium, unlike the powdered separating medium. The shape of the vitreous porous body is, for example, a columnar shape (including a disk shape), and a typical shape is a column whose cross-sectional shape is a perfect circle. However, the vitreous porous body may not have a perfect cross-sectional shape, and the end surface may not be a flat surface. For example, the end surface may be a curved surface. The cross-sectional shape of the vitreous porous body of the present invention may be a circular shape obtained by rounding square corners.

  For the glassy porous material (substantially inorganic porous material, including glass and glass ceramics) as a separating material, a vitreous porous material formed by using a sol-gel method, specifically, sol- A porous gel obtained by using a gel method or a porous material obtained by heat-treating the gel can be used. For example, a vitreous porous body formed by a known sol-gel method using a metal alkoxide (for example, alkoxysilane) or a metal halide as a starting material can be used. Note that the vitreous porous body of the separating material may be a vitreous porous body containing an organic component formed using a metal alkoxide or metal halide to which an organic group is bonded as one of the starting materials.

  The vitreous porous body may be modified on the surface in order to increase the separation ability. For example, a functional group or an organic molecule may be bonded to the surface of the vitreous porous body. An organic molecule having a functional group may be bonded to the surface of the vitreous porous body. The functional group or organic molecule that modifies the surface of the vitreous porous body is selected according to the required resolution. For these, known materials used for separation materials can be applied, and for example, hexyl group, octyl group, other alkyl groups, octadecylsilane, octadecyl group, phenyl group, trimethylsilyl group, cyano group, and amino group can be applied.

  A typical example of the vitreous porous body is a porous body containing silicon oxide as a main component (50 mass% or more), for example, porous silica glass. However, a vitreous porous body containing an oxide other than silicon oxide (inorganic porous body) or a vitreous porous body containing an oxide other than silicon oxide as a main component (inorganic porous body) may be used. A monolith type gel (vitreous porous material) formed by a sol-gel method is preferable in that the control of the porosity and the pore diameter is relatively easy and the variation in the separation ability is small.

  A commercially available vitreous porous body may be used as the vitreous porous body of the separating material. The vitreous porous body may be formed using a known sol-gel method. For example, you may form by the method described in Unexamined-Japanese-Patent No. 6-265534 and Unexamined-Japanese-Patent No. 7-41374. According to these methods, it is possible to form cylindrical porous silica glass (porous silica gel).

As the vitreous porous body of the separating material, a mixture of through holes having a relatively large pore diameter and pores having a small pore diameter may be used. For example, a vitreous porous body produced by the production method described in JP-A-6-265534, specifically, a large number of through holes having a pore diameter of 500 nm to several tens of μm (for example, 30 μm), and a pore diameter of 5 nm to A vitreous porous body in which a large number of pores of 100 nm are formed may be used. The total volume of the pores of the vitreous porous body, for example, in the range of ^{0.001m 3 /kg~0.01m 3 / kg (1m} 3 / t~10m 3 / t).

  The separability of the vitreous porous body varies depending on the pore diameter, porosity, specific surface area, and the like of the porous body. Therefore, those values are controlled according to the required resolution. These values can be controlled by changing the production conditions of the porous body, particularly the conditions of the sol-gel method.

  In the present invention, a vitreous porous body having a diameter of 1 mm or more (for example, 1.6 mm or more) and a length of 2 mm or more (for example, 20 mm or more) may be used. An example vitreous porous body has a diameter in the range of 1.6 mm to 300 mm and a length in the range of 2 mm to 200 mm.

  The housing may include a holder into which the separating material and the deformation tube are inserted. The holder is usually cylindrical.

  The housing may further include a cylindrical spacer disposed between the deformation tube and the holder. In this case, the spacer may be separable into two semi-cylindrical members. If the outer diameter of the separating material is approximately the same as or larger than the inner diameter of the spacer, it may be difficult to insert the separating material into the spacer, especially if the separating material is long (eg, the length is 2 cm or more). Even in such a case, by using a separable spacer, the separating material can be easily arranged in the spacer.

  The housing may further include two pressing members movable so as to press each of the two end faces of the deformable tube. The pressing member may be movable without rotating with respect to the end face of the deformable tube. In this case, the housing may include a rotation suppressing means for preventing the pressing member from rotating. The rotation suppressing means is not particularly limited, and for example, a groove and a rib fitted to the groove may be formed on the pressing member and the holder (or spacer). Moreover, you may form a recessed part and the processus | protrusion fitted to it in a press member and a holder (or spacer).

  The housing may hold the separating material and the deforming tube while pressing the two end surfaces and the outer peripheral surface of the deforming tube. According to this structure, it can suppress that a separation target object flows through parts other than a vitreous porous body. In a typical example, the two end surfaces of the deformation tube are pressed by a pressing member, and the outer peripheral surface of the deformation tube is pressed by a holder or a spacer.

  There is no particular limitation on the material of the housing, and the housing can be formed of a material having an appropriate strength. Usually, the structural member of the housing (excluding the O-ring) is made of a material having no elasticity (plastomer). The constituent members of the housing (excluding the O-ring) may be formed of, for example, a material having a Rockwell hardness (ASTM D 785) and an R scale of 15 or more. Examples of such materials include nylon, polyphenylene sulfide (PPS), liquid crystal polymer (LCP), polyester, polyphenylene oxide (PPO), acrylic, polypropylene (PP), ABS resin, polyether ether ketone (PEEK), and fluorine resin. , Silicone resins, and resins containing various fillers. The constituent member of the housing may be formed of one type of material or a plurality of types of materials. Moreover, a part or all of the structural members (except for the O-ring) of the housing may be formed of metal. In addition, as long as the effect of this invention is acquired, the structural member of a housing may be formed with the material which has elasticity.

  In the cartridge column of the present invention, the deformation tube may be compressed in the direction along the central axis in the housing. The elastomer tube compressed in the direction along the central axis has a smaller inner diameter than usual and an outer diameter larger than usual. As a result, the adhesion between the deformed tube and the separating material is increased. The compressible length of the deformation tube in the housing may be 0.1% to 50% (for example, 1.5% to 25%) of the length of the deformation tube in a normal state.

[Column module]
The column module of the present invention includes a container capable of filling a pressurized fluid therein, and a cartridge column disposed in the container. The cartridge column is the above-described first or second cartridge column of the present invention, that is, a cartridge column using a deformed tube (soft tube or elastomer tube). The housing of the cartridge column is configured so that the fluid pressure is transmitted to the deformation tube. Except for the fact that the housing is configured so that the pressure of the fluid is transmitted to the deformable tube, the same members as those of the cartridge column of the present invention described above can be applied to the components of the cartridge column of the column module.

  In the column module of the present invention, when the pressure of the fluid is transmitted to the deformation tube, the outer peripheral surface of the separation material is pressed by the inner peripheral surface of the deformation tube. As a result, the separation object can be prevented from flowing on the outer peripheral surface of the vitreous porous body.

  The fluid to be pressurized may be a gas or a liquid, but a liquid (for example, water) is usually used. Since the first and second cartridge columns have been described above, redundant description will be omitted.

  When the housing includes a cylindrical holder, an opening through which fluid can pass may be formed on the side wall of the holder. According to this configuration, the pressure of the fluid is transmitted to the deformation tube. Similarly, when the housing includes a cylindrical spacer, an opening through which fluid can pass may be formed on the side wall of the spacer.

[Example of cartridge column]
Hereinafter, an example of the cartridge column of the present invention will be described. FIG. 1A shows a cross-sectional view along the central axis of an example of the separating material used in the cartridge column of the present invention, and FIG. 1B shows a cross-sectional view taken along line Ib-Ib in FIG. Show.

  1A and 1B is composed of a cylindrical vitreous porous body 11 and a heat shrinkable tube 12. The heat shrinkable tube 12 covers the entire outer peripheral surface of the porous body 11. The separating material 10 can be formed by inserting the porous body 11 into the tube before shrinkage and then thermally shrinking the tube. The contracted tube is in close contact with the outer peripheral surface of the porous body 11.

  The separating material 10 is inserted into a cylindrical deformation tube 21. FIG. 2A shows a cross-sectional view of an example of the separating material 10 whose outer peripheral surface is covered with the deformable tube 21. Further, a cross-sectional view taken along line IIb-IIb in FIG. 2A is shown in FIG. FIG. 3 shows an exploded perspective view of an example of a cartridge column using the separating material 10 and the deformable tube 21.

  The cartridge column 20 in FIG. 3 includes a separating material 10, a deformation tube 21, and a housing 30. The separating material 10 is inserted into the deformation tube 21.

  The housing 30 includes a cylindrical spacer 31, a cylindrical holder 32, two O-rings 33, two caps 34, and two end caps 35. The deformation tube 21 is inserted into the spacer 31, and the spacer 31 is inserted into the holder 32. The O-ring 33 is fitted into the recess on the end surface of the cap 34. The O-ring 33 is in close contact with the end surface of the deformation tube 21 and / or the end surface of the separating material 10. A disk-shaped thin packing may be disposed between the O-ring 33 and the separating material 10.

  The cap 34 includes a columnar insertion portion 34 b that is inserted into the holder 32. An annular groove is formed on the end face of the insertion portion 34b, and the O-ring 33 is disposed in this groove.

  A screw thread is formed on the outer peripheral surface of the holder 32. The end cap 35 is formed with a cylindrical recess 35a in which the cap 34 is disposed. A thread groove is formed on the inner peripheral surface of the recess 35 a, and the end cap 35 is screwed to the end of the holder 32. The cap 34 is fitted into the end portion of the holder 32 by tightening the thread groove of the end cap 35 into the thread of the holder 32. In this way, the O-ring 33 and the cap 34 press the end surface of the deformation tube 21. That is, the O-ring 33 and the cap 34 function as pressing members.

  The cap 34 has a notch 34a. Further, the end surface of the holder 32 is formed with a convex portion 32a that fits into the notch portion 34a. The notch 34a and the protrusion 32a prevent the O-ring 33 and the cap 34 from rotating with respect to the deformable tube 21 when the O-ring 33 and the cap 34 move. In this way, when the O-ring 33 and the cap 34 press the end surface of the deformable tube 21, the deformable tube 21 is suppressed from being twisted. As a result, it is possible to prevent leakage due to twisting of the deformable tube 21 and damage to the separating material 10 (porous body 11).

  The cap 34 is formed with an introduction port 34c through which a separation object is introduced. Further, the end cap 35 is formed with a through hole 35b for introducing the separation object into the introduction port 34c. The separation object passes through the through hole 35b and the introduction port 34c and is guided to the vitreous porous body 11 of the separation material 10. The separation object that has passed through the porous body 11 passes through the other inlet 34c and the through hole 35b and comes out of the cartridge column 20.

  The inner diameter of the holder 32 is preferably substantially the same as or slightly larger than the outer diameter of the spacer 31. It is preferable that the inner diameter of the spacer 31 is substantially the same as or smaller than the outer diameter of the deformable tube 21 when no external pressure is applied. When the inner diameter of the spacer 31 is smaller than the outer diameter of the deformable tube 21, the outer peripheral surface of the deformable tube 21 is pressed by the spacer 31 by inserting the separating material 10 and the deformable tube 21 into the spacer 31.

  Usually, members other than the O-ring 33 among the constituent members of the housing 30 are made of a non-elastic substance (plastomer) as described above.

  The spacer 31 may be divisible along the long axis. For example, the spacer 31 may be divisible into two semi-cylindrical parts. When the splittable spacer 31 is used, the deformable tube 21 having an outer diameter larger than the inner diameter of the spacer 31 can be accommodated in the spacer 31 relatively easily.

  As long as the effect of the present invention is obtained, the number of other members arranged in one member may be one or plural. For example, the outer peripheral surface of one separation member 10 may be covered with a plurality of deformation tubes 21. Further, the outer peripheral surfaces of the plurality of separation members 10 may be covered with one deformation tube 21. In addition, a plurality of separation members 10 may be arranged in the spacer 31 or a plurality of deformation tubes 21 may be arranged. A plurality of spacers 31 may be arranged in one holder 32.

  Further, the spacer 31 can be omitted. In this case, the inner diameter of the holder 32 is preferably substantially the same as or smaller than the outer diameter of the deformable tube 21. In this case, the relationship between the inner diameter of the holder 32 and the outer diameter of the deformable tube 21 is the same as that described above for the inner diameter of the spacer and the outer diameter of the deformable tube.

  The holder 32 may be divisible along the long axis. Examples of such holders are shown in FIGS. 4 (a) and (b). The holder 41 in FIG. 4A includes a semi-cylindrical holder 42 and a semi-cylindrical holder 43. The holder 42 includes a protrusion 42a having a hook-shaped portion as a fixing means. The holder 43 is formed with a hole 43a as a fixing means, and the hole 43a holds the protrusion 42a. By holding the protrusion 42 a in the hole 43 a, the holder 42 and the holder 43 are fixed to each other to form a cylindrical holder 41. A screw thread is formed on the outer peripheral surface of the holder 41.

  The holder 45 in FIG. 4B includes a semi-cylindrical holder 46 and a semi-cylindrical holder 47. The holder 46 includes a protrusion 46a as a fixing means. The holder 47 is formed with a hole 47a corresponding to the protrusion 46a as a fixing means. The protrusion 46a is inserted into the hole 47a, and the holder 46 and the holder 47 are fixed. In the holder 46 of FIG. 4B, the plurality of protrusions 46a are formed asymmetrically with respect to the central axis. According to such a structure, it can prevent assembling in a wrong direction. As shown in FIG. 4C, a flat cutout portion 47 a is formed in a part of the outer peripheral portion of the holder 47. Although not shown, the holder 46 is also formed with a similar notch. When the cap is tightened or loosened, the holder can be fixed by holding the notch with a spanner.

[Example of column module]
Hereinafter, an example of the column module of the present invention will be described. A perspective view of the column module of the present invention is shown in FIG. The column module 50 in FIG. 5 includes a container 51 and two caps 52. The cap 52 is formed with a screw thread, and the container 51 is formed with a screw groove that fits into the screw thread. The cap 52 is fixed to the container 51 by screwing the cap 52.

  The container 51 is formed with an inlet 51a for injecting liquid and an outlet (not shown) for discharging the liquid. The inside of the container 51 is hollow, and the inside of the container 51 can be pressurized to a predetermined pressure by injecting liquid from the injection port 51a. The container 51 may be provided with a pressure gauge that indicates the pressure of the liquid in the container 51.

  In the container 51, the cartridge column of the present invention is arranged. An exploded perspective view of an example of the cartridge column arranged in the container 51 is shown in FIG.

  The cartridge column 60 in FIG. 6 includes the separating material 10, the deformable tube 21, and the housing 61. The housing 61 includes a spacer 62, two O-rings 33, and two end caps 63. All the outer peripheral surfaces of the separating material 10 are covered with three deformation tubes 21. Three spacers 62 are arranged on the outer periphery of the three deformable tubes 21. FIG. 6 shows an example in which the three deformable tubes 21 and the three spacers 62 are used, but the number thereof is not limited and may be one or two or more. Also good.

  In the container 51, the two end caps 63 of the cartridge column 60 are fixed by the cap 52. By screwing the cap 52 into the thread groove of the container 51, the end cap 63 and the O-ring 33 press the separating material 10, and the separating material 10 is fixed. As a result, the separation object introduced from the through hole of the cap 52 reaches the separation material 10 without leaking.

  The spacer 62 has a cylindrical shape in which a notch 62a that reaches the inner peripheral surface from the outer peripheral surface is formed. A notch 62 b is formed on the outer periphery of one end of the spacer 62. Further, a notch 62c corresponding to the notch 62b is formed in the inner peripheral portion of the other end of the spacer 62. Adjacent spacers 62 are fixed by these notches.

  The container 51 is filled with a pressurized liquid. Since the notch 62 a is formed in the spacer 62, the liquid pressure is applied to the outer peripheral surface of the deformable tube 21. As a result, the inner peripheral surface of the deformation tube 21 presses the outer peripheral surface of the separating material 10. Therefore, the separation target is prevented from leaking between the vitreous porous body 11 and the heat shrinkable tube 12. By suppressing leakage, separation with high accuracy and reproducibility is realized.

  In the example of FIG. 6, the case where the spacer in which the notch 62 a is formed is used, but a cylindrical spacer in which a plurality of through holes are formed may be used.

  There is no limitation on the size of the vitreous porous body 11 used in the cartridge column and the column module of the present invention. However, in the present invention, it is possible to use a relatively large glassy porous body 11.

  When the vitreous porous body 11 having a relatively large diameter is used, the separation target introduced from one inlet may not be uniformly dispersed in the vitreous porous body 11. In such a case, you may arrange | position the distributor for disperse | distributing a separation target object to the end surface by the side of an inlet port among the end surfaces of the porous body 11. FIG. FIG. 7A shows a top view of an example of such a distributor, and FIG. 7B shows an end view taken along line VIIb-VIIb in FIG. 7A. The distributor 70 in FIG. 7 has a disk shape. On one side of the distributor 70, grooves 70a having different lengths are formed radially. A through hole 70b is formed at the end of the groove 70a. The separation object is introduced into the central portion of the groove 70a, dispersed, and introduced into the porous body 11 from the through hole 70b. Therefore, by using the distributor 70, the separation target can be introduced into the porous body 11 more uniformly. The distributor is not limited to the column module, and may be applied to other cartridge columns of the present invention.

  Moreover, although the case where the external shape of the housing was a columnar shape was shown in the above example, the external shape of the housing may be another shape, for example, a prism shape.

  Moreover, although the case where the spacer 31 cannot be divided was shown in the above example, the spacer 31 may be divided. The spacer 31 can also be divided in the same manner as the holders 41 and 45. Examples of spacers that can be divided are shown in FIGS.

  The spacer 81 shown in FIG. 8A includes semicylindrical members 82 and 83. The member 82 includes a protrusion 82a. The member 83 is formed with a hole 83a for holding the protrusion 82a. By holding the protrusion 82a in the hole 83a, a cylindrical spacer is formed.

  The spacer 85 shown in FIG. 8B includes semi-cylindrical members 86 and 87. The member 86 includes a protrusion 86a. The member 87 has a hole 87a into which the protrusion 86a is inserted. A cylindrical spacer is formed by inserting the projection 86a into the hole 87a. In the case of the spacer 85, unlike the holder 45, no thread is formed. Therefore, the protrusion 86 a and the hole 87 a may be formed symmetrically or asymmetrically.

[Example]
Separation was evaluated using a column having a structure similar to that of the cartridge column 20 shown in FIG. The size of the vitreous porous body 11 used was 2.2 mm in diameter and 50 mm in length. As the heat shrinkable tube 12, a fluorine tube (thickness: about 0.4 mm) manufactured by Pennitto Co., Ltd. was used. For the deformed tube 21, ten tubes made of soft Teflon (soft PTFE) having an inner diameter of about 2.6 mm, an outer diameter of about 6.7 mm, and a length of about 5 mm were used.

  Liquid chromatography of a sample containing benzene, toluene, ethylbenzene, propylbenzene, butylbenzene, amylbenzene and hexylbenzene was performed using the cartridge column. The measurement results are shown in FIG. As shown in FIG. 9, the peak of each component was sharp and separation was possible with high accuracy.

  The embodiments of the present invention have been described above by way of examples, but the present invention is not limited to the above-described embodiments, and can be applied to other embodiments based on the technical idea of the present invention.

  In another aspect, the present invention is also applicable to a column using a columnar separation material other than a vitreous porous body.

  The present invention can be applied to chromatography. The cartridge column and the column module of the present invention can be used for, for example, liquid chromatography, gas chromatography, separation analysis, and apparatuses thereof. According to the cartridge column and the column module of the present invention, it is possible to separate various substances such as organic compounds such as proteins and peptides.

(A) And (b) is sectional drawing which shows an example of the separating material used by this invention, respectively. (A) And (b) is sectional drawing which shows an example of the separating material respectively arrange | positioned in a deformation | transformation tube. It is a disassembled perspective view which shows an example of the cartridge column of this invention. It is a perspective view which shows the example of the holder used by this invention. It is a perspective view which shows an example of the column module of this invention. It is a disassembled perspective view which shows an example of the cartridge column used with the column module of this invention. It is (a) top view and (b) end elevation which show an example of the distributor used by this invention. It is a disassembled perspective view which shows the example of the spacer used by this invention. It is a graph which shows the result of the liquid chromatography performed using the cartridge column of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Separation material 11 Porous body 12 Heat-shrinkable tube 21 Deformation tube 20, 60 Cartridge column 30, 61 Housing 31, 62, 81, 85 Spacer 32, 41, 45 Holder 33 O-ring 34, 52 Cap 35, 63 End cap 50 Column module 51 Container 51a Inlet

Claims (12)

A columnar separator,
A tube arranged to cover the outer peripheral surface of the separating material;
A housing for holding the separating member and the tube,
The compression rate of the tube at 25 ° C. is in the range of 5% to 90%;
The cartridge column in which the separation material includes a columnar vitreous porous body and a heat shrinkable tube covering an outer peripheral surface of the vitreous porous body.   The cartridge column according to claim 1, wherein the tube is made of soft polytetrafluoroethylene. A columnar separator,
A tube arranged to cover the outer peripheral surface of the separating material;
A housing for holding the separating member and the tube,
The tube is an elastomer tube;
The cartridge column in which the separation material includes a columnar vitreous porous body and a heat shrinkable tube covering an outer peripheral surface of the vitreous porous body.   The cartridge column according to claim 1, wherein the housing includes a holder into which the separation material and the tube are inserted.   The cartridge column according to claim 4, wherein the housing further includes a cylindrical spacer disposed between the tube and the holder.   The cartridge column according to claim 5, wherein the spacer is separable into two semicylindrical members.   The cartridge column according to any one of claims 1 to 6, wherein the housing further includes two pressing members movable so as to press each of the two end faces of the tube.   The cartridge column according to claim 7, wherein the pressing member is movable without rotating with respect to an end surface of the tube.   The cartridge column according to any one of claims 1 to 8, wherein the housing holds the separation member and the tube while pressing two end surfaces and an outer peripheral surface of the tube. A column module comprising a container capable of filling a pressurized fluid therein, and a cartridge column disposed in the container,
The cartridge column according to claim 1, wherein the cartridge column is
A column module, wherein the housing of the cartridge column is configured to transmit the fluid pressure to the tube. A column module comprising a container capable of filling a fluid therein and a cartridge column disposed in the container,
The cartridge column according to claim 3, wherein the cartridge column is
A column module, wherein the housing of the cartridge column is configured to transmit the fluid pressure to the tube. The housing includes a cylindrical holder;
The column module according to claim 10 or 11, wherein an opening through which the fluid can pass is formed in a side wall of the holder.

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