JPS60207054A - Liquid chromatography - Google Patents

Liquid chromatography

Info

Publication number
JPS60207054A
JPS60207054A JP59064137A JP6413784A JPS60207054A JP S60207054 A JPS60207054 A JP S60207054A JP 59064137 A JP59064137 A JP 59064137A JP 6413784 A JP6413784 A JP 6413784A JP S60207054 A JPS60207054 A JP S60207054A
Authority
JP
Japan
Prior art keywords
column
liquid
bellows
backflash
liquid feed
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
Application number
JP59064137A
Other languages
Japanese (ja)
Inventor
Toshibumi Kita
俊文 喜多
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Shimazu Seisakusho KK
Original Assignee
Shimadzu Corp
Shimazu Seisakusho KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp, Shimazu Seisakusho KK filed Critical Shimadzu Corp
Priority to JP59064137A priority Critical patent/JPS60207054A/en
Publication of JPS60207054A publication Critical patent/JPS60207054A/en
Pending legal-status Critical Current

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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/38—Flow patterns
    • G01N30/40—Flow patterns using back flushing
    • 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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/38—Flow patterns
    • G01N30/40—Flow patterns using back flushing
    • G01N2030/402—Flow patterns using back flushing purging a device

Abstract

PURPOSE:To simplify the backflash mechanism of a column, by providing the column to a liquid feed pipe in a rotatable manner. CONSTITUTION:In applying backflash to a column 5, a current is supplied to the heater 18 in connection mechanisms 9<-1>, 9<-2> at first by a control means 10 and bellows 12 formed of a shape memory alloy are contracted under heating to release the connection between both ends of the column 5 and liquid feed pipes A, B. Subsequently, a rotary drive mechanism 8 is operated by the control means 10 to rotate the column 5 by 180 deg. and heating to the bellows 12 is stopped at a position where each column end is reversed. Whereupon, the belows 12 extend to connect the ends of the column 5 to the liquid feed pipes A, B. When a moving phase liquid is sent in the column 5 in this state, the flow in the column 5 takes the direction opposite to the preceding one and backflash is applied to the column 5 in order to discharge an unseparated component. By the above mentioned constitution, the length of a flowline is shortened and a time required in analysis becomes short.

Description

【発明の詳細な説明】 （イ）産業上の利用分野 この発明は液体クロマトグラフに関し、特・こ試料分析
流路とカラムの構成・こ関するものである。DETAILED DESCRIPTION OF THE INVENTION (a) Field of Industrial Application This invention relates to liquid chromatographs, and particularly to the structure of sample analysis channels and columns.

（ロ）従来技術 従来液体クロマトグラフにおいて、カラムへバックフラ
ッシュをかける優こは第１図に示すように、試料注入口
（３）より注入された試料を移動相液溜（１）の移動相
液に添加し、送液ポンプ（２）で試料送液パイプ（２）
より切換バルブ（４）を介してカラム（５）に送液し７
分離した試料液は送液パイプ■を経て検出器（６）より
廃液溜（７）へ至るようＧこ構成された分析経路にあっ
て。(b) Prior Art In a conventional liquid chromatograph, Yuko backflushes the column by transferring the sample injected from the sample injection port (3) to the mobile phase in the mobile phase reservoir (1), as shown in Figure 1. Add the liquid to the sample liquid feed pipe (2) using the liquid feed pump (2).
The liquid is sent to the column (5) via the switching valve (4).
The separated sample liquid is in an analysis path configured to go from the detector (6) to the waste liquid reservoir (7) via the liquid sending pipe (2).

バイパス流路用の送液パイプ０を切換バルブ（４）とカ
ラム（５）との開側こ別途配設し、切換バルブ（４）で
流路の接続を切換えて行なっている。A liquid sending pipe 0 for the bypass channel is separately provided on the open side of the switching valve (4) and the column (5), and the switching valve (4) switches the connection of the channels.

すなわち、第１図昏こおいて、最初切換えバルブ（４）
は実線状態に各送液パイプを接続しており、この状態で
分析を行なう。カラム（５）中に残っている未分離成分
を分析する時は、切換バルブ（４）を点線のよう）こ切
換え又カラム（５）へ流れる移動相の方向を通にして行
なっている。That is, in Fig. 1, first selector valve (4)
Each liquid sending pipe is connected to the solid line state, and analysis is performed in this state. When analyzing unseparated components remaining in the column (5), the switching valve (4) is switched (as indicated by the dotted line) to allow the mobile phase to flow into the column (5).

このようにバックフラッシュをかける場合は、バイパス
流路を並設し切換バルブを介して各流路の連結を行なわ
ねばならず、流路構成が複雑となり、また、試料注入か
らカラムへの流路も長くなって分析時間が長くなるとい
う欠点があった。When backflushing is performed in this way, it is necessary to install bypass channels in parallel and connect each channel via a switching valve, which complicates the channel configuration. This has the disadvantage that the analysis time becomes longer.

（ハ）目的 この発明は上記したような流路構成によりバンクフラノ
シーをかける場合の欠点を解消するためになされたもの
であり、バイパス流路を設けるといった流路の構成を変
えることなくバンクフラッシュを行なえる液体クロマト
グラフの提供を目的とする。(C) Purpose This invention was made to eliminate the disadvantages of bank flushing using the above-mentioned flow path configuration, and it is possible to perform bank flushing without changing the flow path configuration such as providing a bypass flow path. The purpose is to provide a liquid chromatograph that can perform

に）構成 この発明に係る液体クロマトグラフは、移動相液により
試料をカラムへ送液オる送液パイプ及びカラムで分離さ
れた試料を検出器へ送液する送液パイプ醗こ対してカラ
ムを回転自在昏こ設けるとともに、このカラム両端と前
記各送液パイプとを着脱自在に連結する連結機構を設け
たことを特徴とする。B) Structure The liquid chromatograph according to the present invention has a liquid sending pipe that sends the sample to the column using a mobile phase liquid, and a liquid sending pipe that sends the sample separated by the column to the detector. The present invention is characterized in that a rotatable column is provided, and a connecting mechanism is provided to connect both ends of the column and each of the liquid feeding pipes in a detachable manner.

（ホ）実施例 以下図面に基づいてこの発明の実施例である液体クロマ
トグラフにつぃて説明する。(e) Example A liquid chromatograph which is an example of the present invention will be described below based on the drawings.

第２図は実施例である液体クロマトグラフの流路構成を
示す模式図である。試料注入口（３）より注入された試
料を移動相液溜（１）の移動相液に溶解させ、送液ポン
プ（２）ヲこよりカラム（５）へ送り込む送液パイプ囚
と、カラム（５）で分離された試料を検出器（６）へ送
液する送液パイプ０３）とをこ対してカラム（５）の両
端（５Ａ）　（５Ｂ）は連結機構（９−１）　（９−２
）　ｔこよって連結されている。この連結機構（９−１
）はたとえば第３図に示すよう・こ、送液パイプ囚端部
Ｇこ対し固定配設した断熱部材よりなる枠体α旧こ、形
状記憶合金で形成したベローズ■と、送液パイプ囚と連
結した可撓材料で形成されたベローズ＋１３１とベロー
ズ（１３１に連結した送液パイプ（＋４１が開ロシヘロ
ーズαＺＧこ連結し、カラム端が挿入される円管状室０
６）を有し、これを３０１Ｊング０９を内装した断熱部
材からなる枠体α５）とが連設されるととも昏こ、形状
記憶合金で形成したベローズ（１３１を加温するヒータ
ＱＩＤが配置され、これら枠体圓、ベローズ（１２）（
１３１，ヒ−タ（ＩＩＤ、枠体α９の周囲をさらに容器
枠（＋７１で被覆している。FIG. 2 is a schematic diagram showing the channel configuration of a liquid chromatograph according to an embodiment. The sample injected from the sample injection port (3) is dissolved in the mobile phase liquid in the mobile phase reservoir (1) and sent to the column (5) via the liquid feed pump (2), and the column (5). ) The ends (5A) (5B) of the column (5) are connected to the connection mechanism (9-1) (9-2
) are connected by t. This connection mechanism (9-1
) is, for example, as shown in Fig. 3, a frame α made of a heat insulating member fixedly disposed against the liquid sending pipe captive end G, a bellows ■ formed of a shape memory alloy, and a liquid feeding pipe captive end G. The bellows +131 formed of a flexible material connected to the liquid sending pipe (+41 connected to the bellows
6), which is connected to a frame body α5) made of a heat insulating member with 301J 09 inside, and a heater QID for heating the bellows (131) made of a shape memory alloy is arranged. These frame circles, bellows (12) (
131, heater (IID), the periphery of the frame α9 is further covered with a container frame (+71).

ただし、枠体（１５１は容器枠αりとの当接面で摺動で
きるように容器枠（＋７１には固定されない。連結機構
（９−２）も全く同様をこ構成されている。However, the frame body (151) is not fixed to the container frame (+71) so that it can slide on the contact surface with the container frame α.The connection mechanism (9-2) is also constructed in exactly the same manner.

ヒータ０８１Ｇこよってベローズ（１２１を加熱し１次
いで加熱を停止すると、その温度変化を３応じて形状記
憶合金の物性により、ベローズ（Ｉ２１が変態し伸縮動
作を行なう。すなわち、ヒータα８）をこよって加熱さ
れると、ベローズα２が縮少しく第３図（イ））、枠体
Ｑ５１が後退して、その円管状室（＋６１に収納されて
いたカラム端（５Ａ）が露見する（第３図（ロ））。送
液パイプの）側も同様に連結機構（９−２）が作動して
カラム端（５Ｂ）が露見する。またベローズα２は加温
を停止すると伸張し、カラム端が円管状室内０Ｇｌへの
収納位置にあれば、その円管状室（１６１内に密着収納
する。カラム（５）の中心部をこはカラム回転駆動機構
（８）が設けられており、カラム端（５Ａ）（５Ｂ）が
連結機構（９−１）（９−２）をこより送液パイプ（Ａ
）ＣＢ）との連結を解除され、上記のようをこ露見した
状態においてカラム（５）を１８０度回転させるもので
ある。連結機構（９−１）（９−２）の送液パイプとカ
ラム端との連結動作及びカラムの回転駆動は制御手段α
σによって、たとえばシーケンス制御され、各動作が順
次行なわれる。もちろん１本発明においては、連結動作
とカラムの回転は手動によって行なわせるようをこして
もよい。Heater 081G heats the bellows (121) and then stops the heating. Depending on the temperature change, the bellows (I21) transforms and expands and contracts due to the physical properties of the shape memory alloy. In other words, the heater α8 When heated, the bellows α2 contracts (Fig. 3 (A)), the frame Q51 retreats, and the column end (5A) housed in its circular tubular chamber (+61) is exposed (Fig. 3 (A)). (b)) On the ) side of the liquid sending pipe, the connecting mechanism (9-2) is activated in the same way, and the column end (5B) is exposed. Further, the bellows α2 expands when heating is stopped, and when the end of the column is in the storage position in the circular tubular chamber 0Gl, it is tightly stored in the circular tubular chamber (161). A rotation drive mechanism (8) is provided, and the column ends (5A) (5B) are connected to the liquid sending pipe (A) through the coupling mechanisms (9-1) (9-2).
) The column (5) is rotated 180 degrees in the state where the connection with CB) is released and the column (5) is exposed as described above. The connection operation between the liquid sending pipe and the column end of the connection mechanism (9-1) (9-2) and the rotational drive of the column are controlled by the control means α.
For example, sequence control is performed by σ, and each operation is performed sequentially. Of course, in one embodiment of the present invention, the coupling operation and the rotation of the column may be performed manually.

上記のように構成された液体クロマトグラフにおいて、
カラムへバックフラッシュをかける蚤こは、連結機構（
９−１）（９−２）により。In the liquid chromatograph configured as above,
The flea that backflushes the column is connected to the coupling mechanism (
9-1) (9-2).

各形状記憶合金で形成されたベローズを加温し、縮少さ
せてカラム両端の送液パイプとの連結を解き７回転駆動
機構にまりカラムを１８０度回転し、各カラム端が反転
した位置で。The bellows formed from each shape memory alloy are heated, contracted, and disconnected from the liquid supply pipes at both ends of the column.Then, the column is rotated 180 degrees by a 7-rotation drive mechanism, and each column end is in an inverted position. .

ベローズへの加熱を停止すれば、ベローズが伸長し、カ
ラム端を各送液パイプと連結する。When heating to the bellows is stopped, the bellows expands and connects the ends of the column to each liquid feeding pipe.

この状態で移動相液を送り込めば、カラム内での流れは
今までの逆方同になり、未分離成分が排出され、バック
フラッシュをかけたことになる。If the mobile phase liquid is sent in this state, the flow within the column will be the same as before, and unseparated components will be discharged, resulting in backflushing.

カラムの回転中蛋こカラム内の溶液が飛び散ることは、
カラムの内容積からして起こり得す７回転を適当な速度
で行なえばよい。またカラムの同転中に連続流出してい
る移動相液は系外へ排出してもよく、排出用のバイパス
流路を設けて排出するようにしてもよい。The solution in the protein column may scatter while the column is rotating.
Seven rotations, which can occur depending on the internal volume of the column, may be performed at an appropriate speed. Further, the mobile phase liquid that is continuously flowing out during the same rotation of the column may be discharged to the outside of the system, or a bypass passage for discharge may be provided to discharge it.

（へ）効果 この発明に係る液体クロマトグラフは上記のよう・こ構
成され、動作するので、従来のようをこバイパス流路を
設けて試料注入口からカラムへの流路の距龍が長くなる
といった流路構成を不要とし、流路長を短かくできて、
しかもカラムを回転させることをこより容易昏こバック
フラッシュをかけることができ９分析時間の短縮を図る
ことができるものである。(f) Effects Since the liquid chromatograph according to the present invention is constructed and operates as described above, a bypass flow path is provided as in the conventional case, and the distance of the flow path from the sample injection port to the column is lengthened. This eliminates the need for such a flow path configuration and shortens the flow path length.
Furthermore, backflushing can be easily performed by rotating the column, and the analysis time can be shortened.

【図面の簡単な説明】[Brief explanation of the drawing]

第１図は従来装置の流路構成を示す模式図であり、第２
図は本発明の実施例である液体クロマトグラフの流路構
成を示す模式図である。第３図は本発明に使用される連
結機構の１実施例を示す断面図である。 １１１・・・移動相液溜　（３）・・・試料注入口（５
）・・・カラム　（６）・・・検出器（８）・・・回転
駆動機構　（９−１）　（９−２）・・・連結機構囚■
・・・送液パイプ 第１図 り 第２図 ＬＩ 第３図 −１ 手続補正帯 ］　事件の表示 昭和５９年特許願第０６４１３７号 ２　発明の名称 液体クロマトグラフ ３　補正をする者 事件との関係　特許出願人 住　所　京都市中京区河原町通二条下ルーツ船人町３７
８番地 名　称　（１９９）　株式会社　島津製作所代表者　取
締役社長　横地節男 ４代理人 住　所　〒６１５京都市右京区画大路通五条下ル東中水
町５番地　ユタ力第−ビル８階 ５　補正命令の日付　自　発 ７　補正の対象 移動相液により試料をカラムへ透１１空送液パイプ及び
カラムで分離された試料を検出器へ送液する送液パイプ
に対してカラムを回転自在に設けるとともに、このカラ
ム両端と前記各送液パイプとを着脱自在に連結する連結
機構を設けたことを特徴とする液体クロマトグラフ。FIG. 1 is a schematic diagram showing the flow path configuration of a conventional device.
The figure is a schematic diagram showing the flow path configuration of a liquid chromatograph that is an example of the present invention. FIG. 3 is a sectional view showing one embodiment of the coupling mechanism used in the present invention. 111... Mobile phase reservoir (3)... Sample injection port (5
)... Column (6)... Detector (8)... Rotation drive mechanism (9-1) (9-2)... Connection mechanism prisoner ■
・・・Liquid Pipe 1 Diagram 2 LI Figure 3-1 Procedural Amendment Band] Indication of the case 1982 Patent Application No. 064137 2 Name of the invention Liquid chromatograph 3 Person making the amendment Relationship with the case Patent Applicant Address: 37 Roots Funatocho, Kawaramachi-dori Nijo-shita, Nakagyo-ku, Kyoto City
No. 8 Name Name (199) Shimadzu Corporation Representative President Setsuo Yokochi 4 Agent address 5, Higashinakasui-cho, Gojo-shita-ru, Oji-dori, Ukyo-ku, Kyoto-shi 615 8th floor, 5th floor, Yuta Chikara Dai Building Date of amendment order Spontaneous 7 The sample is sent to the column using the mobile phase liquid to be corrected.The column is rotatably installed in relation to the empty liquid sending pipe and the liquid sending pipe that sends the sample separated by the column to the detector. A liquid chromatograph characterized in that a connecting mechanism is provided to detachably connect both ends to each of the liquid sending pipes.

Claims (1)

【特許請求の範囲】[Claims] 移動相液により試料をカラムへ送液パイプ及びカラムで
分離された試料を検出器へ送液する送液パイプをこ対し
てカラムを回転自在をこ設けるととも昏こ、このカラム
両端と前記各送液パイプとを着脱自在をこ連結する連結
機構を設けたことを特徴とする液体クロマトグラフ。It is also possible to install a rotatable column with a pipe for transporting the sample to the column using the mobile phase liquid and a pipe for transporting the sample separated by the column to the detector. A liquid chromatograph characterized by being provided with a connection mechanism that detachably connects it to a liquid sending pipe.
JP59064137A 1984-03-31 1984-03-31 Liquid chromatography Pending JPS60207054A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59064137A JPS60207054A (en) 1984-03-31 1984-03-31 Liquid chromatography

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59064137A JPS60207054A (en) 1984-03-31 1984-03-31 Liquid chromatography

Publications (1)

Publication Number Publication Date
JPS60207054A true JPS60207054A (en) 1985-10-18

Family

ID=13249384

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59064137A Pending JPS60207054A (en) 1984-03-31 1984-03-31 Liquid chromatography

Country Status (1)

Country Link
JP (1) JPS60207054A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6279355A (en) * 1985-10-03 1987-04-11 Kurita Water Ind Ltd Chromatography method and apparatus
EP0868932A2 (en) * 1997-04-01 1998-10-07 Wako Pure Chemical Industries Ltd Method for separating components in liquid specimen and apparatus used in said method
US6585937B1 (en) * 1997-11-20 2003-07-01 Esa, Inc. Electrochemical analysis system

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6279355A (en) * 1985-10-03 1987-04-11 Kurita Water Ind Ltd Chromatography method and apparatus
EP0868932A2 (en) * 1997-04-01 1998-10-07 Wako Pure Chemical Industries Ltd Method for separating components in liquid specimen and apparatus used in said method
EP0868932A3 (en) * 1997-04-01 2000-12-06 Wako Pure Chemical Industries Ltd Method for separating components in liquid specimen and apparatus used in said method
US6585937B1 (en) * 1997-11-20 2003-07-01 Esa, Inc. Electrochemical analysis system

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