JP2568312B2 - Liquid chromatograph - Google Patents
Liquid chromatographInfo
- Publication number
- JP2568312B2 JP2568312B2 JP2327665A JP32766590A JP2568312B2 JP 2568312 B2 JP2568312 B2 JP 2568312B2 JP 2327665 A JP2327665 A JP 2327665A JP 32766590 A JP32766590 A JP 32766590A JP 2568312 B2 JP2568312 B2 JP 2568312B2
- Authority
- JP
- Japan
- Prior art keywords
- column
- connector
- liquid chromatograph
- arm
- tube
- 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.)
- Expired - Fee Related
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
- G01N30/6004—Construction of the column end pieces
-
- 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
- G01N30/6047—Construction of the column with supporting means; Holders
-
- 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
- G01N30/6091—Cartridges
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明はカラムを容易に交換し得る液体クロマトグラ
フ装置をに関する。Description: TECHNICAL FIELD The present invention relates to a liquid chromatograph apparatus in which a column can be easily exchanged.
［従来の技術］ 従来の液体クロマトグラフ装置は，特許第952275号に
記載されているように、ホルダ基体に弾性体を介して導
液路を有す一対のコネクタを設け、該コネクタ間にカラ
ムを着脱自在に装填し得るものである。前記弾性体（例
えば環状のゴムシート）はカラムの上下覆蓋と上下コネ
クタの合わせ円に対し、ゴムの弾性作用による反抗力
で、カラムの軸方向に一定の圧力が作用をする。この圧
力により、カラムとコネクタの接合面で密接性が保たれ
ている。[Prior Art] As described in Japanese Patent No. 952275, a conventional liquid chromatograph apparatus has a holder base provided with a pair of connectors having a liquid passage through an elastic body, and a column between the connectors. Can be removably loaded. The elastic body (for example, an annular rubber sheet) exerts a constant pressure in the axial direction of the column on the mating circle between the upper and lower lids of the column and the upper and lower connectors by a reaction force caused by the elastic action of the rubber. Due to this pressure, closeness is maintained at the joint surface between the column and the connector.
前記の装置は工具等を使わずに容易にかつ迅速にホル
ダ部へ着脱ができ、その耐圧力は30kg/cm2程度である。The above-mentioned device can be easily and quickly attached to and detached from the holder portion without using a tool or the like, and its withstand pressure is about 30 kg / cm 2 .
一方、特開昭58−83261号公報に記載されているもの
は、液の出入口を備えたコネクタとカラムとの連結シー
リング要素によりカラムを固定し、上下のシーリング要
素の一方が化圧部材により該カラムの軸方向に移動し、
固定状態ではシーリング要素が一定の圧力でカラムと組
合ってシールを構成し、非固定状態ではシーリング要素
がカラムの軸方向に移動してカラムを迅速に交換すでき
るものである。なお、上記の該加圧部材は空気圧または
スプリングが使用され、該シーリング要素のカラムの軸
方向への移動距離は10〜20mmとされている。On the other hand, in the device described in Japanese Patent Application Laid-Open No. 58-83261, a column is fixed by a connecting sealing element for connecting a connector provided with a liquid inlet / outlet to the column, and one of the upper and lower sealing elements is formed by a pressure member. Move in the axial direction of the column,
In the fixed state, the sealing element is combined with the column at a constant pressure to form a seal, and in the non-fixed state, the sealing element moves in the axial direction of the column so that the column can be quickly replaced. The above-mentioned pressurizing member uses an air pressure or a spring, and the moving distance of the sealing element in the axial direction of the column is 10 to 20 mm.
しかし、前記のものが実施された例は極く一部で、一
般に広く使用されているカラムは、ガスクロマトグラフ
ィと同様に、第11図に示す様に，カラム１の両端に取付
けたエンドフィッティング２の出入口へ、流路用配管３
にフェラル等のシール材を介して中空ボルト４取付け、
スパナ５等で締付けて液圧力をシールしている。該カラ
ム１は、中空のクロマト管に充填剤を詰め、その両端に
フィルタ材とシール材を取付け、エンドフィッティング
２とクロマト管１がネジ止めされている。これによっ
て、カラムの軸方向の移動させたエンドフィッティング
により、クロマト管とシール材が押圧されシールを形成
している。また、前記配管を中空ボルト４でカラムのエ
ンドフィッティングへ取付ける時も、同様にカラムの軸
方向の中空ボルトを移動させてシール形成している。However, only a small number of the cases where the above-mentioned ones have been implemented. In general, widely used columns include end fittings 2 attached to both ends of a column 1 as shown in FIG. Pipe 3
Attach the hollow bolt 4 via a sealing material such as ferrule
The liquid pressure is sealed by tightening with a wrench 5 or the like. In the column 1, a hollow chromatographic tube is filled with a filler, and a filter material and a sealing material are attached to both ends thereof. The end fitting 2 and the chromatographic tube 1 are screwed. Thus, the chromatographic tube and the sealing material are pressed by the end fitting moved in the axial direction of the column to form a seal. Also, when the pipe is attached to the end fitting of the column with the hollow bolt 4, the seal is formed by moving the hollow bolt in the axial direction of the column in the same manner.
これらのカラムは、いずれも死容積を最小となるよう
に設計されている。また、クロマトグラムの再現性、ピ
ークの分離およびベースラインの安定性を図るためのカ
ラム温度の保持方法としては、第11図の様にカラムを蓋
71付きの空気恒温槽６に収容する方法、恒温水槽のカラ
ムを浸漬する方法、あるいは恒温のアルミニウムなどの
金属ブロック性の套管をカラムに被せる方法などが知ら
れている。Each of these columns is designed to minimize dead volume. As a method for maintaining the column temperature for chromatogram reproducibility, peak separation, and baseline stability, cover the column as shown in Fig. 11.
A method of accommodating the column in the air thermostat 6 provided with 71, a method of immersing a column in a thermostat water bath, and a method of covering a column with a metal-blocking sheath of aluminum or the like having a constant temperature are known.
［発明が解決しようとする課題］ 近年、カラムが長く、液の流速が速い、高速液体クロ
マトグラフィ等においては、カラムの充填剤の粒径が３
μｍ以下と細かいために、カラム壁へ液圧が100kg/cm2
以上となり、前記従来のシール方法ではカラムとコネク
タの接続部から液が洩れてしまうと云う問題があった。[Problems to be Solved by the Invention] In recent years, in high-performance liquid chromatography or the like in which the column is long and the liquid flow rate is high, the particle size of the column packing material is 3
Liquid pressure of 100 kg / cm 2 on column wall
As described above, the conventional sealing method has a problem that the liquid leaks from the connection between the column and the connector.
また、カラムのエンドフィッティングと中空ボルトの
ネジ部をスパナ等を用いて締付け、または、取りはずす
作業は、操作に熟練していることが必要であり、また、
煩雑でもある。特に、カラム温度を保持するめの前記恒
温槽が取付けられている場合は、該カラムの交換は容易
ではない。In addition, the operation of tightening or removing the end fitting of the column and the threaded portion of the hollow bolt using a spanner or the like requires skill in the operation.
It is also complicated. In particular, when the constant temperature bath for maintaining the column temperature is attached, it is not easy to replace the column.
本発明の目的は、前記課題を解決するためになされた
もので、カラムの交換が容易で、かつ、高い液圧力（例
えば、100kg/cm2）でも液洩れが生じない液体クロマト
グラフ装置を提供することにある。An object of the present invention is to solve the above-mentioned problems, and to provide a liquid chromatograph device in which a column can be easily replaced and liquid leakage does not occur even at a high liquid pressure (for example, 100 kg / cm 2 ). Is to do.
本発明の他の目的は、カラムの交換が容易な恒温槽を
備えた液体クロマトグラム装置を提供することにある。Another object of the present invention is to provide a liquid chromatogram apparatus provided with a thermostat in which a column can be easily replaced.
［課題を解決するための手段］ 前記課題を解決する本発明の要旨は、液移送ポンプ、
試料注入弁，分離カラムおよび検出器を備えた液体クロ
マトグラフ装置において、 前記カラムをクロマト管とその収容体に分割し、該ク
ロマト管は端部にフィルタとシール部材が装着され、前
記収容体はクロマト管を収める前後にコネクタを配置
し、該コネクタの少なくとも一方にはカム機構，リンク
機構またはクランク機構により駆動する駆動機構部と、
これと連動する梃子機構部を有し、該梃子機構部はアー
ムに連結され、前記梃子機構部は前記アームの開閉操作
により連動する駆動機構部を介して前記コネクタをクロ
マト管の軸方向に駆動し、押圧力を増倍できるよう構成
されていることを特徴とする液体クロマトグラフ装置に
ある。Means for Solving the Problems The gist of the present invention for solving the problems is a liquid transfer pump,
In a liquid chromatograph apparatus provided with a sample injection valve, a separation column and a detector, the column is divided into a chromatographic tube and a container thereof, and the chromatographic tube is provided with a filter and a seal member at an end, and the container is A connector is disposed before and after housing the chromatographic tube, and at least one of the connectors has a driving mechanism driven by a cam mechanism, a link mechanism, or a crank mechanism;
The lever mechanism is connected to an arm, and the lever mechanism drives the connector in the axial direction of the chromatographic tube via a drive mechanism that operates in conjunction with the opening and closing operation of the arm. And a liquid chromatograph device configured to be able to multiply the pressing force.
前記本発明をより具体的に説明すると、液体クロマト
グラフの装置のカラムが、コネクタとクロマト管に分割
されており、該クロマト管の両端はフィルタとシール材
を固着し、上記コネクタとクロマト管の結合部の耐圧力
の向上を図るために、該クロマト管の軸と平行にコネク
タを押圧する押圧機構部を設け、これとアームの梃子機
構部とを組合せることにより大きな押圧力を加えるよう
にしたものである。More specifically describing the present invention, a column of a liquid chromatograph apparatus is divided into a connector and a chromatographic tube, and both ends of the chromatographic tube are fixed with a filter and a sealing material. In order to improve the pressure resistance of the connecting portion, a pressing mechanism for pressing the connector in parallel with the axis of the chromatograph tube is provided, and a large pressing force is applied by combining this with the lever mechanism of the arm. It was done.
また、当該クロマト管の交換の作業性を向上させるた
めに、特に工具等を用いなくとも前記アームを開閉する
だけでクロマト管を装着または脱着させることができる
様にしたものである。Further, in order to improve the workability of replacing the chromatographic tube, the chromatographic tube can be attached or detached only by opening and closing the arm without using a tool or the like.
［作用］ 本発明は、アームの梃子機構の作用によりコネクタと
クロマト管の結合部の耐圧力を向上することができる。
また、アームの押圧機構部の設けたカム機構、リンク機
構またはクランク機構と組合せることによって、更に、
押圧力を増すことができ、これによってシール部は更に
高い液圧力を保持することができる。[Operation] The present invention can improve the pressure resistance of the joint between the connector and the chromatographic tube by the operation of the lever mechanism of the arm.
Further, by combining with a cam mechanism, a link mechanism, or a crank mechanism provided with a pressing mechanism of the arm,
The pressing force can be increased, so that the seal can maintain a higher hydraulic pressure.
上記のコネクタとクロマト管の接続は、クロマト管の
端部またはシール部のコネクタの合せ面の形状を相互に
嵌合される形状とすることで容易に連結することができ
る。特に、テーパー状に形成したものがシール効果が大
きい。また、接続部を球面状にすることによってコネク
タとクロマト管の接続が易い。The connection between the connector and the chromatographic tube can be easily performed by making the shape of the mating surface of the connector of the end portion of the chromatographic tube or the connector of the seal portion mutually fit. In particular, those formed in a tapered shape have a large sealing effect. Further, the connection between the connector and the chromatographic tube is facilitated by making the connection portion spherical.
また、本発明のカラムは、クロマト管の周囲を温度制
御可能なアルミニウム等の金属ブロックで密着する構造
にすることで、該カラムの交換作業を容易に行なうこと
ができる。Further, the column of the present invention has a structure in which the periphery of the chromatographic tube is in close contact with a metal block of aluminum or the like whose temperature can be controlled, so that the column can be easily replaced.
［実施例］ 以下、本発明を第１図および第２図の実施例により、
具体的に説明する。[Example] Hereinafter, the present invention will be described with reference to the examples shown in FIGS. 1 and 2.
This will be specifically described.
クロマト管１とプルカラム２のそれぞれの両端部には
フィルタ13とシール部材14が取付けてあり、該端部とコ
ネクタ４との組合わせ面にはテーパー状の段差部15が設
けられている。該コネクタ４にはフェラル16、中空ボル
ト17、配管18が設けられ、カム10側のコネクタ４には戻
しバネ19とローラーピン20が取付てある。A filter 13 and a seal member 14 are attached to both ends of the chromatographic tube 1 and the pull column 2, respectively, and a tapered step 15 is provided on a surface where the end and the connector 4 are combined. The connector 4 is provided with a ferrule 16, a hollow bolt 17, and a pipe 18, and the connector 4 on the cam 10 side is provided with a return spring 19 and a roller pin 20.
他方のコネクタ４′は圧力調整用のバネ21を有し、該
コネクタ４′の保持体７を収容体３の取付溝22に固定さ
れている。The other connector 4 ′ has a pressure adjusting spring 21, and the holder 7 of the connector 4 ′ is fixed to the mounting groove 22 of the housing 3.
クロマト管１を収容体３にある二つのコネクタ4,4′
間に収め、押圧部のカム10がアーム12の梃子機構で回動
し、ローラーピン20を介してコネクタ４を押圧し、更
に、プレカラム２とクロマト管１を押圧することにより
コネクタ４′で受け止める。このとき圧力調整用のバネ
21が押圧力の過乗分を緩衝する作用を有する。該コネク
タ４とプレカラム２およびクロマト管１の組合せ面の形
状が相互に同心同状に形成されているのでテーパー状の
段差部15によって合わせ面が相互に案内し合って組合わ
されシールされる。Connect the chromatographic tube 1 to the two connectors 4, 4 'in the container 3.
The cam 10 of the pressing portion is rotated by the lever mechanism of the arm 12, presses the connector 4 via the roller pin 20, and further presses the precolumn 2 and the chromatographic tube 1 to be received by the connector 4 '. . At this time, the spring for pressure adjustment
Reference numeral 21 has an effect of buffering the excess of the pressing force. Since the combined surfaces of the connector 4 and the precolumn 2 and the chromatographic tube 1 are formed concentrically and concentrically, the mating surfaces are mutually guided and combined by the tapered step portion 15 to be sealed.
前記装置において、シール部材は四フッ化エチレン樹
脂、カム材は鋼材、他の大部分の部材はステンレス鋼材
を使用した。In the above apparatus, the seal member was made of tetrafluoroethylene resin, the cam member was made of steel, and most of the other members were made of stainless steel.
一方、収容体３およびアーム12に取付けたヒータ５、
測温体６は外部の温度制御装置（図示せず）に接続さ
れ、所定の温度に制御される。On the other hand, the heater 5 attached to the container 3 and the arm 12,
The temperature measuring element 6 is connected to an external temperature control device (not shown) and is controlled to a predetermined temperature.
前記第１図において、クロマト管１やプレカラム２を
交換する際には、第２図に示す様に前記アーム12を上方
に開くことによりカム10が回動し、カムの送り戻し量だ
けコネクタ４が戻され、クロマト管1,プレカラム２を容
易に脱着することができる。また、長さが異なるクロマ
ト管の場合には、保持体７を所定の長さに見合った取付
溝22に移動し配管18を取出溝23に合わせることで調節す
ることができる。In FIG. 1, when the chromatographic tube 1 and the pre-column 2 are exchanged, the cam 10 rotates by opening the arm 12 upward as shown in FIG. Is returned, and the chromatographic tube 1 and the precolumn 2 can be easily detached. In the case of chromatographic tubes having different lengths, the adjustment can be performed by moving the holder 7 to the mounting groove 22 corresponding to the predetermined length, and aligning the pipe 18 with the extracting groove 23.
次に、本発明の他の実施例を第３図、第４図、第５図
により説明する。Next, another embodiment of the present invention will be described with reference to FIGS. 3, 4, and 5. FIG.
クロマト管１を筒状のブロック24に収容し、その両端
に配置したコネクタ４と板状のワッシャ形バネ21と保持
体７が収容体３に設けてある。The chromatographic tube 1 is housed in a tubular block 24, and connectors 4 arranged at both ends thereof, a plate-like washer-shaped spring 21 and a holder 7 are provided in the housing 3.
左方の保持体７と収容体３の接続部にはネジ部41を設
け、アーム12を支える軸25が取付けられている。一方の
アーム12の右方にはリンク26を支える軸27と開閉リンク
28とを支える軸29、可動の保持体７′を支える軸30、31
が連結されている。また、アルミニウム材のブロック24
にはヒータ５と測温体６が設けられている。さらに、ア
ーム12の右方にはフック32を設け、可動の保持体７の上
部を引掛けることができる。A screw portion 41 is provided at a connection portion between the holding member 7 and the container 3 on the left side, and a shaft 25 for supporting the arm 12 is attached. On the right side of one arm 12, a shaft 27 supporting a link 26 and an opening / closing link
A shaft 29 for supporting the movable holding member 7 ';
Are connected. Also, the aluminum block 24
Is provided with a heater 5 and a temperature measuring element 6. Further, a hook 32 is provided on the right side of the arm 12 so that the upper part of the movable holder 7 can be hooked.
次に、本実施の動作を第４図、第５図で説明する。フ
ック32を可動の保持体７′から外すと、アーム12が上方
の開き、同時に連動してリンク26、開閉リンク28、可動
の保持体７′が開くのである。またそのとき、同時に軸
29に連結した連動棒33がクロマト管１を取り出す動作を
する。アームの開く角度が約30℃である。アーム12の長
さｌに対し、リンク26の長さは約1/2であり、また、可
動の保持対７′の長さは約1/4である。動作は、固定状
態のときには０゜で開くときはアーム12がａ、ｂ、ｃ、
ｄ、ｅの順で開くと、可動の保持体７′もａ′、ｂ′、
ｃ′、ｄ′、ｅ′の順に90℃まで開く。この可動の保持
体７′はクランク機構と同様に動く。Next, the operation of this embodiment will be described with reference to FIGS. When the hook 32 is removed from the movable holder 7 ', the arm 12 is opened upward, and at the same time, the link 26, the opening / closing link 28 and the movable holder 7' are opened in conjunction with each other. At that time, the axis
An interlocking rod 33 connected to 29 operates to take out the chromatographic tube 1. The opening angle of the arm is about 30 ° C. For the length 1 of the arm 12, the length of the link 26 is about 1/2 and the length of the movable holding pair 7 'is about 1/4. The operation is such that the arm 12 is a, b, c,
When opened in the order of d and e, the movable holder 7 'is also a', b ',
Open to 90 ° C. in the order of c ′, d ′, e ′. This movable holder 7 'moves similarly to the crank mechanism.
クロマト管１を交換して、可動の保持体７′を閉じる
ときにはアーム12を押すだけで可動の保持体７′が閉
じ、クロマト管１をコネクタ４で強力に押し付けシール
され、液圧力を保持する。そのとき、他方のネジ部41を
設けた保持体７は該コネクタ４の過剰な押し付け圧力を
バネ21が緩衝する。また、左方のネジ部41の保持体７を
前後に移動させてバネ21の位置を移動させることで耐圧
力の調整を行なうことができる。When the chromatographic tube 1 is replaced and the movable holding member 7 'is closed, the movable holding member 7' is closed simply by pressing the arm 12, and the chromatographic tube 1 is strongly pressed by the connector 4 to be sealed to maintain the liquid pressure. . At this time, the spring 21 buffers the excessive pressing pressure of the connector 4 in the holder 7 provided with the other screw portion 41. In addition, by moving the position of the spring 21 by moving the holder 7 of the left screw portion 41 back and forth, the pressure resistance can be adjusted.
本発明のカラムを液体クロマトグラフに装着した流路
図を第６図に示す。FIG. 6 shows a flow chart in which the column of the present invention is mounted on a liquid chromatograph.
クロマト管１を収容した収容体３に取り付けたヒータ
５の測温体６は外部の温度制御装置34に接続されてい
る。該収容体３の入口側にはオートサンプラー35の試料
導入弁36、ポンプ37、溶離液38が接続され、該収溶体３
の出口側には検出器39とデーター処理装置40が接続され
ている。The temperature measuring element 6 of the heater 5 attached to the container 3 accommodating the chromatographic tube 1 is connected to an external temperature controller 34. A sample introduction valve 36, a pump 37, and an eluent 38 of an autosampler 35 are connected to the inlet side of the container 3,
A detector 39 and a data processing device 40 are connected to the outlet side of the device.
ポンプ37で送液された溶離液38は、試料導入弁36を経
由して収容体３のクロマト管１中を流れ検出器39に到達
し、クロマト管１で分離した成分を検出する。なお、液
圧の変化はポンプ37の圧力計で検出したクロマトグラム
は検出器39で測定される。The eluent 38 sent by the pump 37 flows through the chromatographic tube 1 of the container 3 via the sample introduction valve 36, reaches the detector 39, and detects components separated by the chromatographic tube 1. The change in the fluid pressure is detected by the pressure gauge of the pump 37 and the chromatogram is measured by the detector 39.
本発明の実施例による耐圧力の効果を第７図による説
明する。The effect of the withstand pressure according to the embodiment of the present invention will be described with reference to FIG.
溶離液にメタノールを用い、カラムは内径4mm×長さ5
0mm、カラム充填材としては平均粒径２μｍのシリカODS
を用いた。Use methanol as the eluent, and the column has an inner diameter of 4 mm x length 5
0 mm, silica ODS with an average particle size of 2 μm as a column packing material
Was used.
流速1ml/分で加圧後に止め、各加圧での耐圧減少量が
１分間に5kg/cm2以下の点を測定点とした。この測定に
はポンプ37と収容体３を直結し、収容体の出口、または
カラムの出口を止めて測定した。横軸にカラムのコネク
タの押圧力、たて軸に耐圧力を示す。It was stopped after pressurization at a flow rate of 1 ml / min, and the point at which the decrease in pressure resistance at each pressurization was 5 kg / cm 2 or less per minute was taken as a measurement point. For this measurement, the pump 37 and the container 3 were directly connected, and the measurement was performed with the outlet of the container or the outlet of the column stopped. The horizontal axis shows the pressing force of the column connector, and the vertical axis shows the withstand pressure.
Ａは本発明のカラム、Ｂは第11図に示す従来のカラム
による耐圧力と押圧力との関係を示す。A shows the relationship between the pressure resistance and the pressing force of the column of the present invention and B shows the conventional column shown in FIG.
図から本発明のカラムは従来のカラムに比べて1/4の
押圧力で良いことが分かる。From the figure, it can be seen that the column of the present invention requires only 1/4 the pressing force as compared with the conventional column.
また、本実施例のカラムによるクロマトグラム上のベ
ースラインの安定性を従来のカラムと比較測定した。測
定条件は、流速1ml/分、カラム温度40℃、検出器:UV254
nmである。測定結果を第８図に示す。横軸に時間、たて
軸に出力電力の変化を示す。In addition, the stability of the baseline on the chromatogram of the column of this example was measured in comparison with a conventional column. Measurement conditions were as follows: flow rate 1 ml / min, column temperature 40 ° C, detector: UV254
nm. FIG. 8 shows the measurement results. The horizontal axis shows time, and the vertical axis shows changes in output power.
Ａは本発明のカラムによるベースラインであり、Ｂは
第11図に示す従来カラムによるベースラインである。ベ
ースラインノイズは従来の1/3であり、ドリフトもほと
んど認められない。A is the baseline using the column of the present invention, and B is the baseline using the conventional column shown in FIG. Baseline noise is 1/3 of conventional, and drift is hardly recognized.
次に、本実施例によるクロマトグラムを第９図に示
す。Next, a chromatogram according to this example is shown in FIG.
測定条件は前記実施例と同様であり、試料としては
ベンゼン、ナフタレン、ジフェニル、フュナント
レン、フルオレン、ピレン、クリセン、3,4−
ベンゾピレンのそれぞれを１μ注入し測定した。横軸
に溶出時間、たて軸に吸光度を示す。The measurement conditions are the same as those in the above-mentioned Example, and benzene, naphthalene, diphenyl, funanthrene, fluorene, pyrene, chrysene, 3,4-
1 μ of each of benzopyrene was injected and measured. The horizontal axis shows elution time, and the vertical axis shows absorbance.
本実施例によれば極めて良い分離特性を示している。 According to the present embodiment, extremely good separation characteristics are shown.
また、試料としてベンゼンを用いた場合のカラムの分
離性能を表すカラム効率（HETP）を第10図に示す。横軸
に溶離液がカラム内を通る線速度（ｕ）、たて軸にカラ
ム効率（HETP）を示す。FIG. 10 shows the column efficiency (HETP) showing the column separation performance when benzene was used as the sample. The horizontal axis shows the linear velocity (u) of the eluent passing through the column, and the vertical axis shows the column efficiency (HETP).
本発明の実施例のHETPは５μｍであり、極めて高いカ
ラム効率を示した。The HETP of the example of the present invention was 5 μm, and showed extremely high column efficiency.
［発明の効果］ 本発明によれば、高い耐圧力が得られ、ベースライン
の安定性並びに極めて良い分離特性と、カラム効率の優
れた液体クロマトグラフ装置が得られる。[Effects of the Invention] According to the present invention, a liquid chromatograph apparatus having high pressure resistance, excellent baseline stability, extremely good separation characteristics, and excellent column efficiency can be obtained.
また、クロマト管の交換をアームの開閉操作により容
易に行なうことができる。Further, the exchange of the chromatographic tube can be easily performed by opening and closing the arm.
第１図は本発明の一実施例である液体クロマトグラフ装
置のカラムの縦断面図、第２図は第１図の動作を説明す
る断面斜視図、第３図は本発明の他の実施例であるカラ
ムの縦断面図、第４図は第３図の動作を説明する断面斜
視図、第５図は第４図の動作の説明図、第６図は本発明
の液体クロマトグラフ装置の流路図、第７図は液体クロ
マトグラフ装置のカラムの耐圧力を示す曲線図、第８図
はクロマトグラムのノイズとドリフトを示す曲線図、第
９図は本発明の実施例によるクロマトグラム、第10図は
本発明の液体クロマトグラフ装置のカラム流速（ｕ）と
カラム効率（HETP）の関係を示す曲線図、第11図は従来
の液体クロマトグラフ装置のカラム恒温槽へのカラム取
付け状況を示す斜視図である。 １……クロマト管、３……収容体、４……コネクタ、５
……ヒータ、６……測温体、７……コネクタ保持体、９
……カム軸、10……カム、12……アーム、13……フィル
タ、14……シール部材、15……テーパー状段差、16……
フェラル、17……中空ボルト、18……配管、21……圧力
調整バネ、25,27,29,30,31……軸、26,28……リンク、2
4……ブロック、32……フック、33……連動棒、41……
ネジ部。FIG. 1 is a longitudinal sectional view of a column of a liquid chromatograph apparatus according to one embodiment of the present invention, FIG. 2 is a perspective sectional view illustrating the operation of FIG. 1, and FIG. 3 is another embodiment of the present invention. FIG. 4 is a sectional perspective view for explaining the operation of FIG. 3, FIG. 5 is an explanatory view of the operation of FIG. 4, and FIG. 6 is a flow chart of the liquid chromatograph of the present invention. FIG. 7 is a curve diagram showing the pressure resistance of the column of the liquid chromatograph device, FIG. 8 is a curve diagram showing the noise and drift of the chromatogram, FIG. 9 is a chromatogram according to the embodiment of the present invention. FIG. 10 is a curve diagram showing the relationship between the column flow rate (u) and the column efficiency (HETP) of the liquid chromatograph of the present invention, and FIG. It is a perspective view. 1. Chromatographic tube, 3 .... container, 4 .... connector, 5
... heater, 6 ... temperature detector, 7 ... connector holder, 9
... Cam shaft, 10 ... Cam, 12 ... Arm, 13 ... Filter, 14 ... Seal member, 15 ... Tapered step, 16 ...
Ferrule, 17 Hollow bolt, 18 Piping, 21 Pressure adjusting spring, 25, 27, 29, 30, 31… Shaft, 26, 28… Link, 2
4 …… Block, 32 …… Hook, 33 …… Interlocking rod, 41 ……
Screw part.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平２−238362（ＪＰ，Ａ) 実開 昭62−143260（ＪＰ，Ｕ) 実開 昭64−44463（ＪＰ，Ｕ) ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-2-238362 (JP, A) JP-A 62-143260 (JP, U) JP-A 64-44463 (JP, U)
Claims (4)
よび検出器を備えた液体クロマトグラフ装置において、 前記カラムをクロマト管とその収容体に分割し、該クロ
マト管は端部にフィルタとシール部材が装着され、前記
収容体はクロマト管を収める前後にコネクタを配置し、
該コネクタの少なくとも一方にはカム機構，リンク機構
またはクランク機構により駆動する駆動機構部と、これ
と連動する梃子機構部を有し、該梃子機構部はアームに
連結され、前記梃子機構部は前記アームの開閉操作によ
り連動する駆動機構部を介して前記コネクタをクロマト
管の軸方向に駆動し、押圧力を増倍できるよう構成され
ていることを特徴とする液体クロマトグラフ装置。1. A liquid chromatograph apparatus comprising a liquid transfer pump, a sample injection valve, a separation column, and a detector, wherein the column is divided into a chromatographic tube and a container thereof, and the chromatographic tube has a filter and a seal at an end. A member is mounted, the container arranges a connector before and after accommodating the chromatographic tube,
At least one of the connectors has a driving mechanism driven by a cam mechanism, a link mechanism, or a crank mechanism, and a lever mechanism that operates in conjunction with the driving mechanism. The lever mechanism is connected to an arm, and the lever mechanism is connected to the arm. A liquid chromatograph apparatus characterized in that the connector is configured to be driven in the axial direction of a chromatograph tube via a driving mechanism section that is interlocked with opening and closing operations of an arm so that the pressing force can be increased.
請求項１に記載の液体クロマトグラフ装置。2. The liquid chromatograph apparatus according to claim 1, wherein said container has temperature control means.
請求項１または２に記載の液体クロマトグラフ装置。3. The liquid chromatograph apparatus according to claim 1, wherein one of said connectors includes a buffer.
形状が、相互に同心円状のテーパー構造に形成されてい
る請求項１〜３のいずれかに記載の液体クロマトグラフ
装置。4. The liquid chromatograph apparatus according to claim 1, wherein a shape of a connecting surface between said chromatograph tube and said connector is formed in a mutually concentric tapered structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2327665A JP2568312B2 (en) | 1990-11-28 | 1990-11-28 | Liquid chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2327665A JP2568312B2 (en) | 1990-11-28 | 1990-11-28 | Liquid chromatograph |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04194749A JPH04194749A (en) | 1992-07-14 |
| JP2568312B2 true JP2568312B2 (en) | 1997-01-08 |
Family
ID=18201602
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2327665A Expired - Fee Related JP2568312B2 (en) | 1990-11-28 | 1990-11-28 | Liquid chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2568312B2 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5048477B2 (en) * | 2004-03-05 | 2012-10-17 | ウオーターズ・テクノロジーズ・コーポレイシヨン | Apparatus for holding a column or cartridge in the vicinity of a detector and method of using the apparatus |
| US8794676B2 (en) | 2008-05-30 | 2014-08-05 | Waters Technologies Corporation | Device and method for connecting fluid conduits |
| JP5879592B2 (en) * | 2011-12-26 | 2016-03-08 | 東京理化器械株式会社 | column |
| JP7481320B2 (en) * | 2019-02-27 | 2024-05-10 | 株式会社日立ハイテク | Analytical equipment column oven |
| GB2603139B (en) * | 2021-01-27 | 2024-01-10 | Agilent Technologies Inc | Mounting a sample separation unit by a swivel mechanism |
| CN115754105A (en) * | 2022-11-25 | 2023-03-07 | 探普(南京)工业科技有限公司 | Detachable chromatographic column used at low temperature |
| JP2024108928A (en) | 2023-01-31 | 2024-08-13 | アークレイ株式会社 | Flow path member joint structure and column |
| JP2024108927A (en) | 2023-01-31 | 2024-08-13 | アークレイ株式会社 | Flow path member joint structure and column attachment/detachment unit |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62143260U (en) * | 1986-03-05 | 1987-09-09 | ||
| JPS6444463U (en) * | 1987-09-14 | 1989-03-16 | ||
| JPH02238362A (en) * | 1989-03-13 | 1990-09-20 | Meidensha Corp | Column and mounting device of biochemical analyzer |
-
1990
- 1990-11-28 JP JP2327665A patent/JP2568312B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04194749A (en) | 1992-07-14 |
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