JPH0972890A - Laminated column for liquid chromatography - Google Patents
Laminated column for liquid chromatographyInfo
- Publication number
- JPH0972890A JPH0972890A JP22648695A JP22648695A JPH0972890A JP H0972890 A JPH0972890 A JP H0972890A JP 22648695 A JP22648695 A JP 22648695A JP 22648695 A JP22648695 A JP 22648695A JP H0972890 A JPH0972890 A JP H0972890A
- Authority
- JP
- Japan
- Prior art keywords
- filter
- column
- units
- pressure
- unit
- 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
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
- G01N30/60—Construction of the column
- G01N30/6034—Construction of the column joining multiple columns
- G01N30/6039—Construction of the column joining multiple columns in series
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8881—Modular construction, specially adapted therefor
-
- 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
- G01N30/60—Construction of the column
- G01N30/6004—Construction of the column end pieces
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、液体クロマトグラ
フにおいて、試料溶液中の溶質を充填剤により吸着、分
離させるためのカラムに関する。TECHNICAL FIELD The present invention relates to a column for adsorbing and separating a solute contained in a sample solution by a packing material in a liquid chromatograph.
【0002】[0002]
【従来の技術】液体クロマトグラフ用カラムは、試料溶
液の出入口を焼結ステンレス等からなるフィルタで仕切
ったクロマト管(円柱管)に粒子径が数10μm〜数μ
mの充填剤を充填したものが使用される。充填剤として
は、無機系(例えばシリカゲル)や有機ポリマー系(例
えばポリスチレン)等種々のものがある。2. Description of the Related Art A column for a liquid chromatograph has a chromatographic tube (cylindrical tube) whose inlet and outlet for a sample solution are partitioned by a filter made of sintered stainless steel or the like and has a particle size of several tens of μm to several μm.
m filled with filler is used. There are various fillers such as an inorganic type (eg silica gel) and an organic polymer type (eg polystyrene).
【0003】[0003]
【発明が解決しようとする課題】液体クロマトグラフで
高速分析を行うためには、カラムに流す試料溶液の流速
を上げる必要がある。しかしながら、耐圧性の低い有機
ポリマー系の充填剤の場合には、流速による圧力上昇に
より充填剤粒子が潰されてしまい、この粒子によりカラ
ムの出口フィルタが目詰まりを起こすため、さらに圧力
が上昇してしまい、圧力を下げても完全には元の状態に
戻らなくなり、ピーク分離能の低下やカラム圧力上昇に
より安定した分析が不可能になる。In order to perform high-speed analysis with a liquid chromatograph, it is necessary to increase the flow rate of the sample solution flowing through the column. However, in the case of an organic polymer-based packing material having low pressure resistance, the packing material particles are crushed due to the pressure increase due to the flow rate, and the particles cause clogging of the outlet filter of the column, further increasing the pressure. Even if the pressure is lowered, it will not completely return to the original state, and stable analysis will become impossible due to a decrease in peak resolution and an increase in column pressure.
【0004】従って、高速分析を行うためには、カラム
を短くして圧力を下げる必要があるが、カラムを短くす
るとピーク分離能が低下してしまう。また、高分離の分
析を行うためには、カラムを長くするか、より微細な粒
子径の充填剤を使用する必要があるが、この場合にはカ
ラム圧の上昇を招くため、流速を下げる必要があり、よ
り分析時間が長くなってしまう。Therefore, in order to perform high-speed analysis, it is necessary to shorten the column to lower the pressure, but shortening the column lowers the peak resolution. In addition, in order to perform high resolution analysis, it is necessary to lengthen the column or use a packing material with a finer particle size, but in this case, the column pressure will rise, so it is necessary to reduce the flow rate. Therefore, the analysis time becomes longer.
【0005】本発明は、上記課題を解決するものであっ
て、流速を上げても或いはカラムの長さを長くしても、
圧力を分散させることにより充填剤粒子の潰れをなくし
てフィルタの目詰まりを防止し、高速分析或いは高分離
分析を可能にする液体クロマトグラフ用積層カラムを提
供することを目的とする。The present invention is intended to solve the above-mentioned problems, and even if the flow rate is increased or the length of the column is increased,
An object of the present invention is to provide a laminated column for a liquid chromatograph capable of performing high-speed analysis or high-separation analysis by preventing the filler particles from being crushed by dispersing the pressure to prevent the filter from being clogged.
【0006】[0006]
【課題を解決するための手段】上記目的を達成するため
に、本発明の液体クロマトグラフ用積層カラムは、一端
にフィルタ押さえ部及びねじ部が形成され、他端にフィ
ルタ支持部及びねじ部が形成され、内部に充填部が形成
されたカラムユニットを備え、該カラムユニットの複数
をフィルタを介して多段に接続すると共に、該接続部を
シール部材でシールしたことを特徴とする。In order to achieve the above object, a laminated column for a liquid chromatograph of the present invention is provided with a filter pressing portion and a screw portion at one end and a filter supporting portion and a screw portion at the other end. The present invention is characterized in that it is provided with a column unit having a filling portion formed therein, a plurality of the column units are connected in multiple stages via a filter, and the connecting portion is sealed by a sealing member.
【0007】[0007]
【発明の実施の形態】以下、本発明の実施の形態を図面
を参照しつつ説明する。図1は、本発明の液体クロマト
グラフ用積層カラムの1例を示し、図(A)は軸方向断
面図、図(B)は図(A)における接続部Bの拡大断面
図である。BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described below with reference to the drawings. 1A and 1B show an example of a laminated column for a liquid chromatograph of the present invention. FIG. 1A is an axial sectional view, and FIG. 1B is an enlarged sectional view of a connecting portion B in FIG. 1A.
【0008】本発明に係わる積層カラム1は、3本のカ
ラムユニット2a、2b、2cを多段に接続し、両端に
カラム栓3a、3bを接続している。各カラムユニット
2a〜2cは、内部にパイプ状の充填部13を有し、カ
ラムユニット2b、2cの一端外側にフィルタ押さえ部
4、段部5及び雄ねじ部6が形成され、カラムユニット
2b、2cの他端内側にフィルタ支持部7、段部8及び
雌ねじ部9が形成されている。カラムユニット2aに
は、両端外側にフィルタ押さえ部4、段部5及び雄ねじ
部6が形成されている。In the laminated column 1 according to the present invention, three column units 2a, 2b and 2c are connected in multiple stages and column stoppers 3a and 3b are connected to both ends. Each of the column units 2a to 2c has a pipe-shaped filling portion 13 inside, and a filter pressing portion 4, a step portion 5 and a male screw portion 6 are formed outside one end of the column units 2b and 2c. A filter supporting portion 7, a step portion 8 and a female screw portion 9 are formed inside the other end of the. The column unit 2a is formed with a filter pressing portion 4, a step portion 5, and a male screw portion 6 on the outer sides of both ends.
【0009】また、カラム栓3a、3bには、図示しな
い送液管に接続される接続部10が形成され、一端内側
にフィルタ支持部7、段部8及び雌ねじ部9が形成され
ている。なお、カラムユニット2aの他端をカラムユニ
ット2b、2cと同様に雌ねじ構造とし、カラム栓3a
を雄ねじ構造にするようにしてもよい。Further, the column stoppers 3a, 3b are provided with a connecting portion 10 connected to a liquid feeding pipe (not shown), and a filter supporting portion 7, a step portion 8 and an internal thread portion 9 are formed inside one end thereof. The other end of the column unit 2a has a female screw structure like the column units 2b and 2c, and the column stopper 3a
May have a male screw structure.
【0010】各カラムユニット2a〜2c及びカラム栓
3a、3bの接続部には、フィルタ押さえ部4とフィル
タ支持部7間にフィルタ11が挟着され、段部5、8間
にOリングからなるシール部材12が装着されている。
このシール部材12は、フィルタ11を押さえる圧力を
細かく調整でき、何度でも分解、再使用できる構造にな
っている。A filter 11 is sandwiched between the filter pressing portion 4 and the filter supporting portion 7 at the connecting portion of each of the column units 2a to 2c and the column stoppers 3a and 3b, and an O-ring is formed between the step portions 5 and 8. The seal member 12 is attached.
The sealing member 12 has a structure in which the pressure for pressing the filter 11 can be finely adjusted, and can be disassembled and reused any number of times.
【0011】上記構成からなる積層カラムの組立につい
て説明すると、最下段のカラムユニット2aにカラム栓
3aを接続した状態で、充填部13内に充填剤を山盛り
に充填した後、山をすり切りしてフィルタ11を載置
し、2段目のカラムユニット2bを重ねて両カラムユニ
ット2a、2bの雄ねじ部6及び雌ねじ部9を螺合して
いき、カラムユニット2aのフィルタ押さえ部4でフィ
ルタ11をカラムユニット2bのフィルタ支持部7に押
圧固定する。以上の操作を繰り返してカラムユニット2
c、カラム栓3bを多段に組み立てていく。The assembly of the laminated column having the above-mentioned structure will be described. With the column plug 3a connected to the lowest column unit 2a, the filler is filled in the filling portion 13 in a heap and then the mountain is cut off. The filter 11 is placed, the second column unit 2b is overlaid, and the male screw portion 6 and the female screw portion 9 of both column units 2a and 2b are screwed together, and the filter 11 is fixed by the filter holding portion 4 of the column unit 2a. The column unit 2b is pressed and fixed to the filter supporting portion 7. Repeat the above operation for column unit 2
c, assembling the column stopper 3b in multiple stages.
【0012】なお、上記の例においては、3本のカラム
ユニットを多段に接続したものについて説明している
が、これに限定されるものでなく、カラムユニットの数
は、高速分析或いは高分離分析に合わせて設定するもの
である。In the above example, three column units are connected in multiple stages, but the number of column units is not limited to this, and the number of column units can be high-speed analysis or high-resolution analysis. It is set according to.
【0013】カラムユニットの長さは、有機ポリマー系
充填剤の耐圧性とカラムに流す溶液の流速による圧力上
昇との関係、すなわち充填剤粒子が潰れフィルタの目詰
まりを起こす圧力以下の長さに設定する。フィルタ11
は、使用する充填剤の粒子径以下のものを用い、フィル
タが厚いと拡散の原因となり分離能が低下するので薄く
て耐圧性があるものがよい。The length of the column unit has a relationship between the pressure resistance of the organic polymer-based packing material and the pressure increase due to the flow rate of the solution flowing through the column, that is, a length equal to or less than the pressure at which the packing material particles are crushed and the filter is clogged. Set. Filter 11
Is a filler having a particle size equal to or smaller than that of the filler to be used. If the filter is thick, it causes diffusion and lowers the separability.
【0014】本発明においては、高速分析のために溶液
の流速を上げた場合、各カラムユニットに圧力を分散
(ユニットが3本であれば1/3の圧力)させることが
できるので、充填剤粒子が潰れることがなくフィルタの
目詰まりを防止することができる。また、カラム全体の
長さを長くしても、圧力上昇を招くことがないのでフィ
ルタの目詰まりを防止し、高分離分析を可能にする。さ
らに、積層カラム表面に凹凸がないような接続構造にし
たため、積層カラムをヒートブロックに挿入して加熱す
るに当たり、ヒートブロックからの熱伝導を容易且つ均
一に行うことができる。In the present invention, when the flow rate of the solution is increased for high-speed analysis, it is possible to disperse the pressure in each column unit (if there are three units, the pressure is 1/3). It is possible to prevent clogging of the filter without particles being crushed. Further, even if the length of the entire column is lengthened, the pressure does not rise, so that the filter is prevented from being clogged and high resolution analysis is enabled. Furthermore, since the connection structure has no unevenness on the surface of the laminated column, when the laminated column is inserted into the heat block and heated, heat conduction from the heat block can be performed easily and uniformly.
【図1】本発明の液体クロマトグラフ用積層カラムの1
例を示し、図(A)は軸方向断面図、図(B)は図
(A)における接続部Bの拡大断面図である。FIG. 1 is a laminated column 1 for a liquid chromatograph according to the present invention.
An example is shown, Fig. (A) is a sectional view in the axial direction, and Fig. (B) is an enlarged sectional view of a connecting portion B in Fig. (A).
1…積層カラム、2a〜2b…カラムユニット、3a、
3b…カラム栓 4…フィルタ押さえ部、5…段部、6…雄ねじ部、7…
フィルタ支持部 8…段部、9…雌ねじ部、11…フィルタ、12…シー
ル部材、13…充填部1 ... laminated column, 2a-2b ... column unit, 3a,
3b ... Column stopper 4 ... Filter holding portion, 5 ... Step portion, 6 ... Male thread portion, 7 ...
Filter support portion 8 ... Step portion, 9 ... Female thread portion, 11 ... Filter, 12 ... Seal member, 13 ... Filling portion
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成7年9月5日[Submission date] September 5, 1995
【手続補正1】[Procedure amendment 1]
【補正対象書類名】図面[Document name to be amended] Drawing
【補正対象項目名】図1[Correction target item name] Fig. 1
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【図1】 FIG.
Claims (1)
され、他端にフィルタ支持部及びねじ部が形成され、内
部に充填部が形成されたカラムユニットを備え、該カラ
ムユニットの複数をフィルタを介して多段に接続すると
共に、該接続部をシール部材でシールしたことを特徴と
する液体クロマトグラフ用積層カラム。1. A column unit having a filter holding part and a screw part formed at one end, a filter support part and a screw part formed at the other end, and a filling part formed inside, and a plurality of the column units are filtered. A multi-layer column for liquid chromatograph, characterized in that it is connected in a multi-stage manner via and the connection part is sealed by a seal member.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP22648695A JPH0972890A (en) | 1995-09-04 | 1995-09-04 | Laminated column for liquid chromatography |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP22648695A JPH0972890A (en) | 1995-09-04 | 1995-09-04 | Laminated column for liquid chromatography |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH0972890A true JPH0972890A (en) | 1997-03-18 |
Family
ID=16845861
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP22648695A Pending JPH0972890A (en) | 1995-09-04 | 1995-09-04 | Laminated column for liquid chromatography |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0972890A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2006125564A3 (en) * | 2005-05-23 | 2008-01-03 | Bischoff Analysentechnik Und G | Elements for separating substances by distributing between a stationary and a mobile phase, and method for the production of a separating device |
JP2008510172A (en) * | 2004-08-19 | 2008-04-03 | ウオーターズ・インベストメンツ・リミテツド | Device, method and apparatus for performing separation |
JP2008519277A (en) * | 2004-11-04 | 2008-06-05 | バイオ−ラッド・パスツール | Stackable chromatography module and chromatography column comprising a stack of such modules |
-
1995
- 1995-09-04 JP JP22648695A patent/JPH0972890A/en active Pending
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2008510172A (en) * | 2004-08-19 | 2008-04-03 | ウオーターズ・インベストメンツ・リミテツド | Device, method and apparatus for performing separation |
JP4909897B2 (en) * | 2004-08-19 | 2012-04-04 | ウオーターズ・テクノロジーズ・コーポレイシヨン | Device, method and apparatus for performing separation |
US8845892B2 (en) | 2004-08-19 | 2014-09-30 | Waters Technologies Corporation | Device, method and apparatus for performing separations |
JP2008519277A (en) * | 2004-11-04 | 2008-06-05 | バイオ−ラッド・パスツール | Stackable chromatography module and chromatography column comprising a stack of such modules |
WO2006125564A3 (en) * | 2005-05-23 | 2008-01-03 | Bischoff Analysentechnik Und G | Elements for separating substances by distributing between a stationary and a mobile phase, and method for the production of a separating device |
JP2008542695A (en) * | 2005-05-23 | 2008-11-27 | ビショフ・アナリューゼンテクニク・ウント−ゲレーテ・ゲーエムベーハー | Element for separating substances by dispersing between stationary phase and mobile phase and method for producing separation device |
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Legal Events
Date | Code | Title | Description |
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A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20030226 |