JP2833130B2 - High-performance liquid chromatograph - Google Patents
High-performance liquid chromatographInfo
- Publication number
- JP2833130B2 JP2833130B2 JP8576490A JP8576490A JP2833130B2 JP 2833130 B2 JP2833130 B2 JP 2833130B2 JP 8576490 A JP8576490 A JP 8576490A JP 8576490 A JP8576490 A JP 8576490A JP 2833130 B2 JP2833130 B2 JP 2833130B2
- Authority
- JP
- Japan
- Prior art keywords
- liquid
- pump
- performance liquid
- liquid chromatograph
- mobile phase
- 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
Description
【発明の詳細な説明】 （イ）産業上の利用分野 この発明は高速液体クロマトグラフに関する。さらに
詳しくは、その改良に関する。The present invention relates to a high-performance liquid chromatograph. More specifically, it relates to the improvement.
（ロ）従来の技術 従来、例えば高速液体クロマトグラフ（以下HPLC）等
におけるように定流量送液を行う場合は、基本的にはポ
ンプの回転数と送液量は比例するという考えに基づい
て、意図する流量に対応して当初に設定された一定の回
転数により駆動される送液ポンプと、圧力センサと、ダ
ンパからなる送液システムが用いられている。(B) Conventional technology Conventionally, when a constant flow rate liquid supply is performed as in, for example, a high performance liquid chromatograph (hereinafter referred to as HPLC), based on the idea that the pump rotation speed and the liquid supply amount are basically proportional. In addition, a liquid supply system including a liquid supply pump driven at a fixed number of rotations initially set corresponding to an intended flow rate, a pressure sensor, and a damper is used.
上記送液ポンプは通常第２図に示すようなプランジャ
型ポンプであり、モータの回転をカムにより往復運動に
変換し、これによるプランジャの動作と逆止弁の働きに
より送液するものである。The liquid feed pump is usually a plunger type pump as shown in FIG. 2, in which the rotation of the motor is converted into a reciprocating motion by a cam, and the liquid is fed by the operation of the plunger and the function of the check valve.
（ハ）発明が解決しようとする課題 上記プランジャ型の送液ポンプでは、該ポンプの入口
側に気泡が入った場合等には必ず流量が低下してしま
う。このようなポンプ不調は分析精度や再現性等の不良
の原因となるので、ポンプの脱気を行うなど多大な注意
を要する。(C) Problems to be Solved by the Invention In the above-mentioned plunger type liquid feed pump, the flow rate always decreases when air bubbles enter the inlet side of the pump. Since such a pump malfunction causes a failure such as analysis accuracy and reproducibility, great care must be taken such as degassing the pump.
この発明はかかる状況に鑑み為されたものであり、常
に一定量の送液が可能に構成された送液システムを有す
る高速液体クロマトグラフを提供しようとするものであ
る。The present invention has been made in view of such a situation, and an object of the present invention is to provide a high-performance liquid chromatograph having a liquid sending system configured to always send a fixed amount of liquid.
（ニ）課題を解決するための手段 かくしてこの発明によれば、移動相貯留部、送液手
段、試料注入部、分離カラム、検出器をこの順に有する
分析流路を備えてなる高速液体クロマトグラフであっ
て、上記分析流路の前記送液手段と試料注入部との間に
挿入接続される抵抗管路と、この抵抗管路の前段及び後
段にそれぞれ設けられる圧力センサと、これらのセンサ
の出力差を一定に保持しうるよう送液手段に送液量を変
更する作動を指令する送液手段制御部とから構成される
送液制御機構を設けたことを特徴とする高速液体クロマ
トグラフが提供される。(D) Means for Solving the Problems According to the present invention, a high-performance liquid chromatograph comprising an analytical flow path having a mobile phase storage unit, a liquid sending unit, a sample injection unit, a separation column, and a detector in this order. And a resistance pipe inserted and connected between the liquid sending means and the sample injection section of the analysis flow path, pressure sensors provided at a front stage and a rear stage of the resistance pipe, respectively, A high-performance liquid chromatograph characterized by having a liquid supply control mechanism comprising a liquid supply means control unit for instructing the liquid supply means to change the liquid supply amount so that the output difference can be kept constant. Provided.
この発明の高速液体クロマトグラフ（以下この発明の
装置という）は、後述する送液制御機構を設ける以外
は、当該分野で公知の高速液体クロマトグラフ（以下HP
LCという）を基本構成として用いることができる。The high-performance liquid chromatograph of the present invention (hereinafter referred to as the apparatus of the present invention) is a high-performance liquid chromatograph (hereinafter referred to as HP
LC) can be used as a basic configuration.
この発明の装置において、上記送液制御機構は、送液
中にフィードバックして送液量が調節できるよう構成さ
れる。すなわち、分析流路の送液手段と試料注入部との
間に抵抗管路を設け、この抵抗管路の前段及び後段にそ
れぞれ圧力センサを設け、これらのセンサの出力に基づ
いて圧力差を算出し、この圧力差が常に一定となるよう
に送液手段に送液量を変更する作動を指令する制御部を
具備して構成される。In the apparatus according to the present invention, the liquid feeding control mechanism is configured so that the liquid feeding amount can be adjusted by feeding back during the liquid feeding. That is, a resistance pipe is provided between the liquid sending means of the analysis flow path and the sample injection section, pressure sensors are provided at the front and rear stages of the resistance pipe, respectively, and the pressure difference is calculated based on the outputs of these sensors. A control unit is provided for instructing the liquid sending means to change the liquid sending amount so that the pressure difference is always constant.
上記抵抗管路は、その前後で圧力差を生じうるもので
ありかつ分析上支障をきたさないものである限り、いず
れの形状であってもよい。The resistance conduit may have any shape as long as it can generate a pressure difference before and after the resistance conduit and does not hinder the analysis.
上記抵抗管路の前段及び後段にそれぞれ設けられる圧
力センサは、当該分野で公知のもの例えばストレインゲ
ージ等がそのまま使用できる。上記前段とは抵抗管路と
送液手段との間のいずれかの部位をいい、後段とは抵抗
管路と試料注入部との間のいずれかの部位をいう。As the pressure sensors provided at the front and rear stages of the resistance pipe, those known in the art, such as strain gauges, can be used as they are. The former stage means any part between the resistance conduit and the liquid sending means, and the latter part means any part between the resistance conduit and the sample injection part.
上記送液手段制御部は、上記２つの圧力センサの出力
を比較する比較部と、この比較部から出力される差出力
に基づいて送液手段の駆動を調節しうる駆動調節部とか
ら主として構成される。この駆動調節部には、PID制御
可能な演算機能が備えられる。The liquid feeding unit control unit mainly includes a comparison unit that compares the outputs of the two pressure sensors, and a drive adjustment unit that can adjust the driving of the liquid feeding unit based on the difference output output from the comparison unit. Is done. This drive adjustment unit is provided with an arithmetic function capable of PID control.
この発明の装置は、単一の移動相供給部からなる通常
のHPLCにも、また移動相及び送液手段を有する移動相供
給路を複数備えてこれらを合流し、この合流路を、分析
流路の試料注入部に前段に接続するいわゆるグラジェン
ド溶出が可能な方式のHPLCにも適用することができる。
後者に適用する場合、各移動相供給路にそれぞれ上記送
液制御機構を設けるものであってもよいが、後段側の圧
力センサを、合流部後段でかつ試料注入部前段の分析流
路に設定される１つの圧力センサで共用することも可能
である。The apparatus of the present invention is also used for ordinary HPLC comprising a single mobile phase supply unit, and also includes a plurality of mobile phase supply paths having a mobile phase and a liquid sending means, which are joined together. The present invention can also be applied to an HPLC of a type capable of so-called gradient elution, which is connected to a sample injection portion of a channel at a preceding stage.
When applied to the latter, the above-mentioned liquid sending control mechanism may be provided for each mobile phase supply path, but the pressure sensor on the subsequent stage is set in the analysis flow path after the confluence part and before the sample injection part. It is also possible to share a single pressure sensor.
なお、この発明の装置の分析流路にダンパが設けられ
る場合は、送液手段と抵抗管路の前段に設定される圧力
センサとの間であってもよく、またこの圧力センサと抵
抗管路の間であってもよい。When a damper is provided in the analysis flow path of the apparatus of the present invention, the damper may be provided between the liquid sending means and a pressure sensor set at a preceding stage of the resistance pipe. May be between.
（ホ）作用 この発明によれば、移動相貯留槽から送液手段により
分析流路を移送される移動相について、抵抗管路の前後
においてその流体圧力が検知される。この結果得られる
圧力差の変動に基づいて、送液手段の送液量がフィード
バック制御され、分析流路には定流量で送液されること
となる。(E) Function According to the present invention, the fluid pressure of the mobile phase transferred from the mobile phase storage tank to the analysis channel by the liquid sending means is detected before and after the resistance pipe. Based on the fluctuation of the pressure difference obtained as a result, the amount of liquid sent by the liquid sending means is feedback-controlled, and the liquid is sent to the analysis flow path at a constant flow rate.
以下実施例によりこの発明を詳細に説明するが、これ
によりこの発明は限定されるものではない。Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
（ヘ）実施例 第１図はこの発明の高速液体クロマトグラフ（以下HP
LC）の一例の構成説明図である。同図においてHPLC
（１）、移動相貯留槽（２）、送液ポンプ（３）、ダン
パ（４）、抵抗管路（５）、試料インジェクタ（６）、
分離カラム（７）、検出器（８）をこの順に接続しドレ
ンに延設される分析流路（ａ）と、上記抵抗管路（５）
の前段及び後段の分析流路（ａ）に設けられた圧力セン
サＡ（51）、Ｂ（52）と、これらの圧力センサからの出
力に基づいて送液ポンプ（３）の送液量を調節するポン
プ制御部（９）とから主として構成されている。(F) Example FIG. 1 shows a high performance liquid chromatograph (hereinafter referred to as HP) of the present invention.
FIG. 3 is an explanatory diagram of an example of a configuration (LC). In the figure, HPLC
(1), mobile phase storage tank (2), liquid sending pump (3), damper (4), resistance line (5), sample injector (6),
An analysis flow path (a) connected to a separation column (7) and a detector (8) in this order and extending to a drain, and the resistance pipe (5)
The pressure sensors A (51) and B (52) provided in the upstream and downstream analysis flow paths (a), and the flow rate of the liquid feed pump (3) is adjusted based on the outputs from these pressure sensors. And a pump controller (9).
上記送液ポンプ（３）は第２図に示すようなプランジ
ャ型ポンプが用いられている。該ポンプは、モータ（3
1）の回転をカム（32）により往復運動に変換し、これ
によるプランジャ（33）の動作と逆止弁（34）（35）の
働きにより送液するものである。A plunger type pump as shown in FIG. 2 is used as the liquid sending pump (3). The pump has a motor (3
The rotation of 1) is converted into a reciprocating motion by the cam (32), and the liquid is fed by the operation of the plunger (33) and the action of the check valves (34) (35).
上記抵抗管路（５）は、内径0.1mmφ、長さ2mのSUS31
6製で構成されたパイプである。The resistance pipe (5) is made of SUS31 with an inner diameter of 0.1 mm and a length of 2 m.
This is a pipe made of six.
圧力センサA,Bはいずれもストレインゲージが用いら
れている。Each of the pressure sensors A and B uses a strain gauge.
ポンプ制御部（９）は、図示しない記憶部及びPID制
御可能な比較演算機能を有する駆動調節部を備えてい
る。記憶部には設定流量（Ｆ）が記憶される。また駆動
調節部は送液ポンプに電気接続され、このポンプの駆動
を調節して送液量を変更できるように構成されている。The pump control unit (9) includes a storage unit (not shown) and a drive adjustment unit having a PID-controllable comparison operation function. The set flow rate (F) is stored in the storage unit. The drive adjusting section is electrically connected to the liquid feed pump, and is configured to adjust the drive of the pump to change the liquid feed amount.
上記駆動調節部では、送液ポンプ（３）の駆動スピー
ドＳ（ｔ）、圧力センサA,Bのそれぞれの出力Ａ（ｔ）,
B（ｔ）、記憶部に設定されるＦとから、設定値と測定
値の偏差の時間関数ｅ（ｔ）が、ｅ（ｔ）＝Ｆ−〔Ａ
（ｔ）−Ｂ（ｔ）〕で設定されており、これらに基づい
て下記式： Ｓ（ｔ）＝K1・ｅ（ｔ）＋K2・〔de（ｔ）
/dt〕＋K3∫ｅ（ｔ）dt によるPID制御が行われるよう設定されている。In the drive adjusting section, the drive speed S (t) of the liquid feed pump (3), the respective outputs A (t),
From B (t) and F set in the storage unit, the time function e (t) of the deviation between the set value and the measured value is e (t) = F− [A
(T) −B (t)], and based on these, the following equation is obtained: S (t) = K 1 · e (t) + K 2 · [de (t)
/ dt] + K 3 ∫e (t) dt so that PID control is performed.
従って上記HPLC（１）の送液作動において、ｅ（ｔ）
＝０となるようにPID制御がなされれば、 ｅ（ｔ）＝Ｆ−〔Ａ（ｔ）−Ｂ（ｔ）〕＝０より Ａ（ｔ）−Ｂ（ｔ）＝Ｆとなり、 定流量制御されることとなる。Therefore, in the liquid feeding operation of the HPLC (1), e (t)
If PID control is performed so that = 0, then e (t) = F− [A (t) −B (t)] = 0, so that A (t) −B (t) = F, and constant flow rate control Will be done.
また、他の実施例として移動相供給路が２流路（ｂ）
（ｃ）タイプのグラジェント送液時の構成を第３図に示
す。この構成では、圧力センサＡに相当するもの（図中
A1,A2）及び抵抗管路はそれぞれ個々の移動相供給路に
設けられるが、圧力センサＢに相当するもの（図中
Ｂ′）は共用するように構成されている。そして圧力セ
ンサA1−Ｂ′の出力差及び圧力センサA2−Ｂ′の出力差
は１つのポンプ制御部に出力され、ここで上記と同様に
PID制御がなされ、これにより各移動相供給路の各送液
ポンプが制御されて、それぞれ定流量制御されることと
なる。Further, as another embodiment, the mobile phase supply path has two flow paths (b).
FIG. 3 shows the configuration of the (c) type when a gradient liquid is supplied. In this configuration, one equivalent to the pressure sensor A (in the figure,
A 1 , A 2 ) and the resistance pipeline are provided in the respective mobile phase supply channels, but the one corresponding to the pressure sensor B (B ′ in the figure) is configured to be shared. Then, the output difference between the pressure sensors A 1 -B ′ and the output difference between the pressure sensors A 2 -B ′ are output to one pump control unit, and here, as described above,
PID control is performed, whereby each liquid feed pump in each mobile phase supply path is controlled, and constant flow rate control is performed.
（ト）発明の効果 この発明によれば、フィードバック制御により送液手
段の流量をコントロールするため、送液手段が不調にな
っても定流量を維持でき、HPLCシステムとして信頼性を
大幅に向上することができる。(G) Effects of the Invention According to the present invention, since the flow rate of the liquid sending means is controlled by feedback control, a constant flow rate can be maintained even if the liquid sending means becomes malfunctioning, and the reliability of the HPLC system is greatly improved. be able to.
第１図はこの発明の高速液体クロマトグラフの一例の構
成説明図、第２図はプランジャ型ポンプの要部構成説明
図、第３図はこの発明の他の例の第１図相当図である。 ２……移動相貯留槽、３……送液ポンプ、４……ダン
パ、５……抵抗管路、６……試料インジェクタ、７……
分離カラム、８……検出器、９……ポンプ制御部、51,5
2……圧力センサ。FIG. 1 is an explanatory diagram of an example of a high-performance liquid chromatograph of the present invention, FIG. 2 is an explanatory diagram of a main portion of a plunger pump, and FIG. 3 is a diagram corresponding to FIG. 1 of another example of the present invention. . 2 ... mobile phase storage tank, 3 ... liquid sending pump, 4 ... damper, 5 ... resistance line, 6 ... sample injector, 7 ...
Separation column, 8 Detector, 9 Pump control unit, 51,5
2 ... Pressure sensor.
Claims (1)
離カラム、検出器をこの順に有する分析流路を備えてな
る高速液体クロマトグラフであって、 上記分析流路の前記送液手段と試料注入部との間に挿入
接続される抵抗管路と、この抵抗管路の前段及び後段に
それぞれ設けられる圧力センサと、これらのセンサの出
力差を一定に保持しうるよう送液手段に送液量を変更す
る作動を指令する送液手段制御部とから構成される送液
制御機構を設けたことを特徴とする高速液体クロマトグ
ラフ。1. A high-performance liquid chromatograph comprising an analysis flow path having a mobile phase storage section, a liquid sending means, a sample injection section, a separation column, and a detector in this order. Resistance line inserted and connected between the means and the sample injecting section, pressure sensors provided at the front and rear stages of the resistance line, respectively, and liquid sending means so that the output difference between these sensors can be kept constant. A high-performance liquid chromatograph, characterized by further comprising a liquid-feeding control mechanism comprising a liquid-feeding means control unit for instructing an operation to change the liquid-feeding amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8576490A JP2833130B2 (en) | 1990-03-30 | 1990-03-30 | High-performance liquid chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8576490A JP2833130B2 (en) | 1990-03-30 | 1990-03-30 | High-performance liquid chromatograph |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03282362A JPH03282362A (en) | 1991-12-12 |
| JP2833130B2 true JP2833130B2 (en) | 1998-12-09 |
Family
ID=13867938
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8576490A Expired - Fee Related JP2833130B2 (en) | 1990-03-30 | 1990-03-30 | High-performance liquid chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2833130B2 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2824443B2 (en) * | 1994-05-12 | 1998-11-11 | ティ・エフ・シィ株式会社 | Preparative liquid chromatography equipment |
| JP3534944B2 (en) * | 1996-06-05 | 2004-06-07 | ジーエルサイエンス株式会社 | Liquid chromatograph mixer |
| US6780315B2 (en) * | 2002-12-09 | 2004-08-24 | Waters Investments Limited | Backflow prevention for high pressure gradient systems |
| JP4645437B2 (en) * | 2005-12-22 | 2011-03-09 | 株式会社島津製作所 | Gradient liquid feeder |
| JP6040726B2 (en) * | 2012-11-20 | 2016-12-07 | 東ソー株式会社 | Liquid chromatograph apparatus provided with a flow meter and flow rate correction method in the apparatus |
| CN113544503B (en) * | 2019-03-13 | 2024-02-06 | 株式会社岛津制作所 | Liquid chromatograph |
-
1990
- 1990-03-30 JP JP8576490A patent/JP2833130B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03282362A (en) | 1991-12-12 |
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