JPH04323557A - Device for filling column for chromatography - Google Patents
Device for filling column for chromatographyInfo
- Publication number
- JPH04323557A JPH04323557A JP3119379A JP11937991A JPH04323557A JP H04323557 A JPH04323557 A JP H04323557A JP 3119379 A JP3119379 A JP 3119379A JP 11937991 A JP11937991 A JP 11937991A JP H04323557 A JPH04323557 A JP H04323557A
- Authority
- JP
- Japan
- Prior art keywords
- column
- gel
- solvent
- filling
- tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000004587 chromatography analysis Methods 0.000 title claims description 19
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 238000012856 packing Methods 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 6
- 238000004904 shortening Methods 0.000 abstract description 2
- 239000000499 gel Substances 0.000 description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 6
- 238000004062 sedimentation Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000003480 eluent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/56—Packing methods or coating methods
- G01N2030/562—Packing methods or coating methods packing
- G01N2030/565—Packing methods or coating methods packing slurry packing
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明はクロマトグラフィ用カラ
ム充填装置に係り、特にシリカ、各種ポリマ等の粉状分
離材をクロマトグラフィ用カラムに充填するクロマトグ
ラフィ用カラム充填装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a column packing apparatus for chromatography, and more particularly to a column packing apparatus for chromatography for filling a chromatography column with a powdery separation material such as silica or various polymers.
【０００２】0002
【従来の技術】従来から、クロマトグラフィ装置は、円
筒状のカラム内にシリカ、ポリマ等のゲルと呼ばれる粉
状分離材を充填することが必要である。この粉状分離材
が充填されたカラムを使用して分離、精製を行う場合、
先ずカラムの上部から対象液を注入する。注入された前
記対象液は前記粉状分離材を通過する際、対象液中の成
分毎によって移動速度に差が生じる。これによって、前
記対象液中から目的成分を分取することができる。2. Description of the Related Art Conventionally, chromatography apparatuses have required filling a cylindrical column with a powdery separation material called gel, such as silica or polymer. When performing separation and purification using a column packed with this powdery separation material,
First, the target liquid is injected from the top of the column. When the injected target liquid passes through the powder separation material, the moving speed differs depending on the component in the target liquid. Thereby, the target component can be fractionated from the target liquid.
【０００３】このように、クロマトグラフィ装置は、成
分毎の移動速度差を利用するので、カラム内に於ける前
記ゲルの充填状態がカラムの性能に大きく影響する。通
常、ゲルの充填装置は乾式法と湿式法とに大別すること
ができる。前記乾式法では、加振装置を使用してカラム
を振動させながら充填する。この乾式法は、特別の充填
設備が要らないという利点があるが、ゲルの粒子径の大
きなものやゲル形状が球状でないのは充填することがで
きず、また大型カラムになると加振が困難になるという
欠点がある。[0003] As described above, since the chromatography apparatus utilizes the difference in movement speed of each component, the filling state of the gel in the column greatly influences the performance of the column. Generally, gel filling devices can be roughly divided into dry methods and wet methods. In the dry method, a vibrating device is used to vibrate the column while filling the column. This dry method has the advantage of not requiring special packing equipment, but it is not possible to pack gels with large particle diameters or gels that are not spherical, and it is difficult to excite large columns. It has the disadvantage of becoming.
【０００４】これに対し、湿式法はカラムの上部にスラ
リを溜めるパッカを連結し、このパッカ内にスラリを入
れて高圧ポンプでカラム内に押し込んで充填する。この
湿式法では、ゲルの形状に影響されないという利点があ
るが、充填設備が大型になるので生産用として使用する
クロマトグラフィ装置には適応できないという欠点があ
る。On the other hand, in the wet method, a packer for storing slurry is connected to the upper part of the column, and the slurry is put into the packer and is forced into the column using a high-pressure pump to fill the column. This wet method has the advantage of not being affected by the shape of the gel, but has the disadvantage that it requires large filling equipment and cannot be applied to chromatography equipment used for production.
【０００５】このような不具合を解消する手段として、
図２に示す充填装置（特開昭６３−３２６０ 号公報に
開示された）がある。この充填装置によれば、高圧スラ
リポンプ１を用いてスラリ状のゲルをカラム２に直接圧
入するようにしたので、湿式法の特徴を生かして生産用
として使用することができる。しかし、ゲルの粒子径が
大きく（２０μｍ以上）なると、前記高圧スラリポンプ
１を用いた場合、圧入時にゲルが摩耗するという欠点が
ある。
また、ゲルの粒子径が大きいと、ゲルの自然沈降作用で
充填することができるので、この場合においては自然沈
降させて充填するようにしている。[0005] As a means to eliminate such problems,
There is a filling device shown in FIG. 2 (disclosed in Japanese Patent Laid-Open No. 63-3260). According to this filling device, the gel slurry is directly pressurized into the column 2 using the high-pressure slurry pump 1, so it can be used for production by taking advantage of the characteristics of the wet method. However, when the particle size of the gel is large (20 μm or more), there is a drawback that when the high-pressure slurry pump 1 is used, the gel is worn out during press-fitting. Furthermore, if the particle size of the gel is large, the gel can be filled by natural sedimentation, so in this case, the gel is filled by natural sedimentation.
【０００６】[0006]
【発明が解決しようとする課題】しかしながら、ゲルを
自然沈降させて充填した場合、充填に長時間かかるとい
う欠点がある。本発明は、このような事情に鑑みてなさ
れたもので、生産設備用として簡単な設備で、且つ充填
時間を短縮することができるクロマトグラフィ用カラム
充填装置を提供することを目的とする。[Problems to be Solved by the Invention] However, when the gel is filled by allowing it to settle naturally, there is a drawback that it takes a long time to fill the gel. The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a column packing device for chromatography that is a simple facility for production equipment and can shorten the filling time.
【０００７】[0007]
【課題を解決する為の手段】本発明は、前記目的を達成
する為に、物質の分離、精製用の粉状分離材を溶媒と混
合してスラリ状にし、円筒状のカラム内に自然沈降させ
て充填するクロマトグラフィ用カラム充填装置に於いて
、前記カラムの下部に前記溶媒のみが通過可能なフイル
タを取付けると共に、該フイルタを介して溶媒吸引装置
を取付けたことを特徴とする。[Means for Solving the Problems] In order to achieve the above-mentioned object, the present invention mixes a powdery separation material for separation and purification of substances with a solvent to form a slurry, and naturally settles the slurry in a cylindrical column. The column packing apparatus for chromatography is characterized in that a filter through which only the solvent can pass is attached to the lower part of the column, and a solvent suction device is attached through the filter.
【０００８】[0008]
【作用】本発明によれば、ゲルの粒子径が大きくなると
、高圧スラリポンプを用いなくても通液抵抗が小さい為
、ゲルを圧入するには至らず、自然沈降で常に一定のカ
ラム性能になることを実験により確認し、この自然沈降
による充填時間を短縮する手段として、カラムの下部に
溶媒のみが通過可能なフイルタを取付けると共に、該フ
イルタを介して溶媒吸引装置を取付ける。これにより、
スラリ状のゲルは、溶媒吸引装置の溶媒吸引作用によっ
て充填が促進される。従って、ゲルの充填時間を短縮す
ることができる。[Function] According to the present invention, when the particle size of the gel becomes large, the liquid flow resistance is small even without using a high-pressure slurry pump, so it is not possible to force-inject the gel, and natural sedimentation always maintains a constant column performance. As a means of shortening the filling time due to natural sedimentation, we have confirmed through experiments that a filter through which only the solvent can pass is attached to the bottom of the column, and a solvent suction device is attached through the filter. This results in
Filling of the slurry-like gel is facilitated by the solvent suction action of the solvent suction device. Therefore, the gel filling time can be shortened.
【０００９】[0009]
【実施例】以下添付図面に従って本発明に係るクロマト
グラフィ用カラム充填装置の好ましい実施例について詳
説する。図１は本発明に係るクロマトグラフィ用カラム
充填装置の実施例が示され、筒状に形成されたカラム１
０の上方にはスラリタンク１２が配設される。このスラ
リタンク１２にはゲル１４と溶媒２０とを混合する為の
攪拌装置１６が設けられると共に、その下部にスラリ状
ゲルをカラム１０に投入する為の供給バルブ１８が連結
されている。DESCRIPTION OF THE PREFERRED EMBODIMENTS Preferred embodiments of the chromatography column packing apparatus according to the present invention will be described in detail below with reference to the accompanying drawings. FIG. 1 shows an embodiment of a column packing device for chromatography according to the present invention, in which a column 1 formed in a cylindrical shape is shown.
A slurry tank 12 is disposed above 0. This slurry tank 12 is provided with a stirring device 16 for mixing the gel 14 and the solvent 20, and a supply valve 18 for introducing the slurry gel into the column 10 is connected to the lower part of the stirring device 16.
【００１０】前記カラム１０の底部にはフイルタ２２が
取付けらる。このフイルタ２２は前記シリカ１４を通過
させず、溶媒２０のみを通過させることができる性能を
有してしる。前記フイルタ２２の下部にはバルブ２４を
介してリザーバタンク２６が連通される。また、このリ
ザーバタンク２６には真空ポンプ２８が連通されている
。A filter 22 is attached to the bottom of the column 10. This filter 22 has the ability to not allow the silica 14 to pass through, but only the solvent 20 to pass through. A reservoir tank 26 is communicated with the lower part of the filter 22 via a valve 24 . Further, a vacuum pump 28 is connected to the reservoir tank 26 .
【００１１】次に、前記の如く構成されたクロマトグラ
フィ用カラム充填装置の作用について説明する。先ず、
攪拌装置１６を作動して、スラリタンク１２内でゲル１
４と溶媒２０を充分に攪拌し、スラリ状にする。ここで
、スラリ濃度は、ゲル１４が溶媒２０中で完全に分散す
る為に低い方が好ましいので、５％から２０％に設定す
る。また、ゲル１４の攪拌中にバルブ２４を閉めると共
に、真空ポンプ２８を作動してリザーバタンク２６を減
圧し所定の真空度にする。Next, the operation of the chromatography column packing apparatus constructed as described above will be explained. First of all,
The stirring device 16 is operated to stir the gel 1 in the slurry tank 12.
4 and solvent 20 are sufficiently stirred to form a slurry. Here, since it is preferable that the slurry concentration be low in order for the gel 14 to be completely dispersed in the solvent 20, it is set to 5% to 20%. Further, while stirring the gel 14, the valve 24 is closed, and the vacuum pump 28 is operated to reduce the pressure in the reservoir tank 26 to a predetermined degree of vacuum.
【００１２】次に、スラリタンク１２のバルブ１８を開
放し、スラリタンク１２からスラリ状ゲル１４を溶媒２
０と共にカラム１０に投入する。そして、カラム１０内
に於ける溶媒２０の液面３０が、カラム１０の底部から
１０センチから２０センチに上昇した時点でバルブ２４
を開放する。これによって、カラム１０内の溶媒２０は
、前記リザーバタンク２６が減圧されていることにより
、フイルタ２２を介してリザーバタンク２６に吸引され
る。この時、カラム１０内に於ける前記液面３０が、充
填されたゲル面よりも常に上になるように、バルブ２４
と真空ポンプ２８を予め調整しておくことが重要である
。Next, the valve 18 of the slurry tank 12 is opened, and the slurry gel 14 is transferred from the slurry tank 12 to the solvent 2.
0 into the column 10. Then, when the liquid level 30 of the solvent 20 in the column 10 rises from 10 cm to 20 cm from the bottom of the column 10, the valve 24
to open. As a result, the solvent 20 in the column 10 is sucked into the reservoir tank 26 via the filter 22 because the pressure in the reservoir tank 26 is reduced. At this time, the valve 24 is set so that the liquid level 30 in the column 10 is always above the filled gel surface.
It is important to adjust the vacuum pump 28 in advance.
【００１３】従って、カラム１０内で自然沈降中のゲル
１４は、溶媒２０がフイルタ２２を介して吸引されるの
で、この吸引作用に伴って充填が促進する。これにより
、本実施例によれば、自然沈降のみで充填していた従来
のクロマトグラフィ用カラム充填装置と比較して、ゲル
１４の充填時間を大幅に短縮することができる。次いで
、前述したゲル面がカラム１０の上面まで上昇した時点
でバルブ１８、バルブ２４を閉めると共に、真空ポンプ
２８を停止する。その後、ゲル１４をカラム１０の最上
部まで、即ち図示しないカラム上部フランジとゲル面と
の隙間がなくなるまで補充した後、カラム上部フランジ
を閉めることにより、ゲル１４の充填が終了する。[0013] Therefore, since the solvent 20 is suctioned through the filter 22 in the gel 14 that is spontaneously settling in the column 10, the filling of the gel 14 is promoted by this suction action. As a result, according to this embodiment, the time for filling the gel 14 can be significantly shortened compared to the conventional chromatography column packing apparatus in which packing is performed only by natural sedimentation. Next, when the gel surface mentioned above rises to the upper surface of the column 10, the valves 18 and 24 are closed, and the vacuum pump 28 is stopped. Thereafter, the gel 14 is replenished to the top of the column 10, that is, until there is no gap between the column upper flange (not shown) and the gel surface, and then the column upper flange is closed, thereby completing the filling of the gel 14.
【００１４】次に、本実施例のクロマトグラフィ用カラ
ム充填装置を使用した実験例を示す。
〈条件〉
■ゲル１４として、２０μｍから４０μｍのシリカを使
用する。■前記シリカをヘキサン（溶媒２０）で１０％
程度のスラリ状にする。Next, an experimental example using the chromatography column packing apparatus of this embodiment will be shown. <Conditions> (2) As the gel 14, silica with a thickness of 20 μm to 40 μm is used. ■ 10% of the silica with hexane (solvent 20)
Make it into a slurry.
【００１５】■前記スラリ状のシリカをカラム１０（直
径１０６ｍｍ×高さ５００ｍｍ）に投入する。
■リザーバタンク２６の吸引力を４５０ｍｍＨｇから５
００ｍｍＨｇ（ヘキサンの吸引量０．５ｌ／ｍｉｎから
１．０ｌ／ｍｉｎ）に設定する。
このような条件で充填した後、ヘキサン／酢酢エチル＝
８５／１５の溶離液でフタル酸ジ−ｎ−ブチルを用いて
カラム１０の性能を測定したところ、理論段数で７００
０段／ｍ以上であり、その充填時間も短縮できたことが
判明した。(2) The slurry-like silica is charged into a column 10 (diameter 106 mm x height 500 mm). ■ Increase the suction power of the reservoir tank 26 from 450mmHg to 5
00 mmHg (hexane suction amount from 0.5 l/min to 1.0 l/min). After filling under these conditions, hexane/ethyl acetate=
When the performance of column 10 was measured using di-n-butyl phthalate with an eluent of 85/15, the number of theoretical plates was 700.
It was found that the filling time was 0 stages/m or more, and that the filling time could also be shortened.
【００１６】尚、本実施例ではカラム上部のデッドスペ
ースを無くす為にゲル１４を単に補充する方法について
説明したが、これに限られるものではなく、カラム１０
の上部に延長カラムを取付けて、この延長カラムまでゲ
ル１４を充填した後、延長カラムを取り外してカラム１
０の上部をフランジで固定するようにしても良い。また
、フランジを可動栓構造とし、ゲル充填後、この可動栓
によってカラム１０の上部のデッドスペースを無くすよ
うにしても良い。In this embodiment, the method of simply replenishing the gel 14 in order to eliminate the dead space at the top of the column has been described, but the method is not limited to this.
Attach an extension column to the top of column 1 and fill it with gel 14, then remove the extension column and fill column 1.
The upper part of 0 may be fixed with a flange. Alternatively, the flange may have a movable plug structure, and the dead space at the top of the column 10 may be eliminated by the movable plug after gel filling.
【００１７】[0017]
【発明の効果】以上説明したように、本発明に係るクロ
マトグラフィ用カラム充填装置によれば、カラムの下部
に溶媒のみが通過可能なフイルタを取付けると共に、該
フイルタを介して溶媒吸引装置を取付けて、溶媒吸引装
置の溶媒吸引作用によってゲルの充填を促進させたので
、生産設備用として簡単な設備で、且つ充填時間を短縮
することができる。As explained above, according to the chromatography column packing device of the present invention, a filter through which only the solvent can pass is attached to the lower part of the column, and a solvent suction device is attached through the filter. Since gel filling is promoted by the solvent suction action of the solvent suction device, it is possible to use simple equipment for production equipment and shorten the filling time.
【図１】本発明に係るクロマトグラフィ用カラム充填装
置の実施例を示す説明図FIG. 1 is an explanatory diagram showing an example of a column packing device for chromatography according to the present invention.
【図２】従来のクロマトグラフィ用カラム充填装置の実
施例を示す説明図[Fig. 2] An explanatory diagram showing an example of a conventional column packing device for chromatography.
１０…カラム １２…スラリタンク １４…ゲル １８、２４…バルブ ２２…フイルタ ２６…リザーバタンク ２８…真空ポンプ 10...Column 12...Slurry tank 14...Gel 18, 24...Valve 22...Filter 26...Reservoir tank 28...Vacuum pump
Claims (1)
媒と混合してスラリ状にし、円筒状のカラム内に自然沈
降させて充填するクロマトグラフィ用カラム充填装置に
於いて、前記カラムの下部に前記溶媒のみが通過可能な
フイルタを取付けると共に、該フイルタを介して溶媒吸
引装置を取付けたことを特徴とするクロマトグラフィ用
カラム充填装置。Claim 1: A chromatography column packing device in which a powdery separation material for separation and purification of substances is mixed with a solvent to form a slurry, and the slurry is allowed to naturally settle and packed into a cylindrical column. A column packing device for chromatography, characterized in that a filter through which only the solvent can pass is attached to the lower part, and a solvent suction device is attached through the filter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3119379A JPH04323557A (en) | 1991-04-23 | 1991-04-23 | Device for filling column for chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3119379A JPH04323557A (en) | 1991-04-23 | 1991-04-23 | Device for filling column for chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04323557A true JPH04323557A (en) | 1992-11-12 |
Family
ID=14760057
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3119379A Pending JPH04323557A (en) | 1991-04-23 | 1991-04-23 | Device for filling column for chromatography |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04323557A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008082339A1 (en) * | 2007-01-02 | 2008-07-10 | Ge Healthcare Bio-Sciences Ab | Separation media slurry tank |
| WO2009157853A1 (en) * | 2008-06-27 | 2009-12-30 | Ge Healthcare Bio-Sciences Ab | Separation media slurry tank |
| CN103091432A (en) * | 2011-10-31 | 2013-05-08 | 天津市科密欧化学试剂有限公司 | Method for coating stationary phase in capillary column |
| CN103091431A (en) * | 2011-10-31 | 2013-05-08 | 天津市科密欧化学试剂有限公司 | Coating apparatus for immobile phase in capillary column |
| CN103675169A (en) * | 2012-08-31 | 2014-03-26 | 月旭材料科技(上海)有限公司 | Method for filling gel chromatographic columns |
-
1991
- 1991-04-23 JP JP3119379A patent/JPH04323557A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008082339A1 (en) * | 2007-01-02 | 2008-07-10 | Ge Healthcare Bio-Sciences Ab | Separation media slurry tank |
| US8092073B2 (en) | 2007-01-02 | 2012-01-10 | Ge Healthcare Bio-Sciences Ab | Separation media slurry tank |
| WO2009157853A1 (en) * | 2008-06-27 | 2009-12-30 | Ge Healthcare Bio-Sciences Ab | Separation media slurry tank |
| JP2011525988A (en) * | 2008-06-27 | 2011-09-29 | ジーイー・ヘルスケア・バイオサイエンス・アクチボラグ | Separation medium slurry tank |
| CN103091432A (en) * | 2011-10-31 | 2013-05-08 | 天津市科密欧化学试剂有限公司 | Method for coating stationary phase in capillary column |
| CN103091431A (en) * | 2011-10-31 | 2013-05-08 | 天津市科密欧化学试剂有限公司 | Coating apparatus for immobile phase in capillary column |
| CN103675169A (en) * | 2012-08-31 | 2014-03-26 | 月旭材料科技(上海)有限公司 | Method for filling gel chromatographic columns |
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