JPH0424540A - Parallax-refractive-index detector for liquid chromatograph - Google Patents
Parallax-refractive-index detector for liquid chromatographInfo
- Publication number
- JPH0424540A JPH0424540A JP12900590A JP12900590A JPH0424540A JP H0424540 A JPH0424540 A JP H0424540A JP 12900590 A JP12900590 A JP 12900590A JP 12900590 A JP12900590 A JP 12900590A JP H0424540 A JPH0424540 A JP H0424540A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- cell
- solvent
- flow path
- flow
- 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.)
- Granted
Links
- 239000007788 liquid Substances 0.000 title abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 46
- 238000000926 separation method Methods 0.000 claims description 10
- 238000004811 liquid chromatography Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract description 20
- 238000002347 injection Methods 0.000 abstract description 4
- 239000007924 injection Substances 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- YMHOBZXQZVXHBM-UHFFFAOYSA-N 2,5-dimethoxy-4-bromophenethylamine Chemical compound COC1=CC(CCN)=C(OC)C=C1Br YMHOBZXQZVXHBM-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 241000545067 Venus Species 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は液体クロマトグラフ用として汎用であり広範囲
な試料を測定できる示差屈折率検出器に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a differential refractive index detector that is versatile for use in liquid chromatographs and can measure a wide range of samples.
（従来の技術）
従来、サンプルセル及びリファレンスセルを備え、両セ
ルに溶媒を送液する液体クロマトグラフ用示差屈折率検
出器（以下ダブルフロー型Ｒ１検出器と表現）は、送液
溶媒の状態変化による出力信号の変動を取り除くため、
検出器外部から各セルへの送液を必要とする。(Prior art) Conventionally, a differential refractive index detector for liquid chromatography (hereinafter referred to as a double flow type R1 detector), which is equipped with a sample cell and a reference cell and which sends a solvent to both cells, detects the state of the sending solvent. In order to remove fluctuations in the output signal due to changes,
Requires liquid to be delivered to each cell from outside the detector.
サンプルセル及びリファレンスセルへの送液は、ポンプ
２台による送液又は、サンプルセルへの溶媒の一部を分
離カラムの前で分岐してリファレンスセルに送液する方
法がとられ、送液の条件を同一とするため、サンプルセ
ル及びリファレンスセル入口に同一の分離カラムを接続
する必要がある。The liquid is sent to the sample cell and the reference cell by using two pumps, or by branching a part of the solvent to the sample cell in front of the separation column and sending it to the reference cell. In order to make the conditions the same, it is necessary to connect the same separation column to the sample cell and reference cell inlets.
また、サンプルセルへ送液する溶媒の一部をリファレン
スセルへ封入する方法（リファレンス・ストップ型）に
おいては、送液溶媒及び封入溶媒の状態変化が影響し、
出力信号の安定性を欠いている。In addition, in the method (reference stop type) in which a part of the solvent to be sent to the sample cell is sealed in the reference cell, changes in the state of the sending solvent and the filling solvent are affected.
Output signal lacks stability.
（発明が解決しようとする問題点）
本発明の目的は、ダブルフロー型Ｒ１検出器において、
リファレンスセルへの検出器外部からの別の送液を不要
とした上で、検出器出力信号の安定性をリファレンス・
ストップ型Ｒ１検出器より向上させ、ダブルフロー型Ｒ
１検出器に近づけるものである。(Problems to be Solved by the Invention) The purpose of the present invention is to solve the following problems in a double flow type R1 detector:
In addition to eliminating the need for a separate liquid supply from outside the detector to the reference cell, the stability of the detector output signal can be checked using the reference cell.
Improved from stop type R1 detector, double flow type R
1 detector.
（問題点を解決するための手段および作用）本発明は、
サンプルセルへ送液される溶媒をサンプルセル入口又は
出口で分岐し、バッファタンクを介してリファレンスセ
ルへ導くことにより、試料注入後試料を含む溶媒をバッ
ファタンクにトラップさせるとともに、試料注入前にバ
ッファタンクに送液された試料を含まない溶媒がリファ
レンスセルに流入し、両セル内の溶媒の状態変化を一定
時間補償する方法と、トラップ時間が終了した場合、バ
ッファタンク及びリファレンスセルを試料を含まない溶
媒により洗浄するための流路を構成し、連続的な使用を
可能とする機構を具備することにある。(Means and effects for solving the problems) The present invention has the following features:
By branching the solvent sent to the sample cell at the sample cell inlet or outlet and guiding it to the reference cell via the buffer tank, the solvent containing the sample is trapped in the buffer tank after sample injection, and the buffer is removed before sample injection. A method in which the solvent that does not contain the sample sent to the tank flows into the reference cell to compensate for changes in the state of the solvent in both cells for a certain period of time, and when the trap time ends, the buffer tank and the reference cell are transferred to the buffer tank and the reference cell that do not contain the sample. The purpose of the present invention is to provide a mechanism that configures a flow path for cleaning with a free solvent and enables continuous use.
すなわち、本発明は、分離カラムで試料成分を分離した
後の示差屈折率検出器のサンプルセルに流入する溶媒又
はサンプルセルから流出した溶媒の一部をリファレンス
セルに送液することを特徴とする液体クロマトグラフ用
示差屈折率検出器を提供するものである。That is, the present invention is characterized in that a part of the solvent flowing into the sample cell of the differential refractive index detector after separating sample components in the separation column or the solvent flowing out from the sample cell is sent to the reference cell. A differential refractive index detector for liquid chromatography is provided.
（作用） 以下、本発明を図面により説明する。(effect) Hereinafter, the present invention will be explained with reference to the drawings.
第１図はサンプルセルへ流入する送液溶媒の一部をサン
プルセル入口で分岐し、リファレンスセルへの送液溶媒
とする例である。FIG. 1 shows an example in which a part of the liquid feeding solvent flowing into the sample cell is branched off at the sample cell inlet and used as the liquid feeding solvent to the reference cell.
１ＴＰｌ定手順としては、まず洗浄バブル（Ｖ）を開い
た状態でポンプ（Ｐ）により送液し、サンプルセル側、
リファレンス側の各流路の洗浄を行う。As for the 1TPl determination procedure, first, the cleaning bubble (V) is opened and the pump (P) is used to send the liquid, and the sample cell side,
Clean each channel on the reference side.
洗浄バルブが開いた状態では、サンプルセル入口で分岐
された各流量はほぼ均等であり、検出器内の流路は測定
溶媒で満たされる。When the cleaning valve is open, the flow rates branched off at the sample cell inlet are approximately equal, and the flow path within the detector is filled with the measurement solvent.
流路の洗浄が終了した後、洗浄バルブを閉じ、リファレ
ンスセルへの流量を制限する。リファレンスセルへの流
量は、細管、フィルター、制限オリフィス、弁などから
成る抵抗（ｒ）により、サンプル側流量の約１／１００
以下、好ましくは１１５００以下とする。。After cleaning the flow path, close the cleaning valve to limit the flow rate to the reference cell. The flow rate to the reference cell is approximately 1/100 of the flow rate on the sample side due to resistance (r) consisting of capillary tubes, filters, restrictive orifices, valves, etc.
Hereinafter, preferably 11,500 or less. .
試料の注入は、この洗浄バルブを閉じた状態で行う。試
料注入器（Ｉ）から注入された試料は、分離カラム（Ｃ
）を経てサンプルセルへ流入するが、この際リファレン
ス側流路へも試料の約１／１０００が流入する。このリ
ファレンス側流路内の試料は、リファレンス側の流れに
より送液されるが、バッファタンク（Ｔ）を含むリファ
レンス側流路の容積とリファレンス側流路の比により定
まる一定時間、リファレンス側流路内に留まり、リファ
レンスセルへは流入しない。このバッファタン（Ｔ）は
、配管の径を太くしたり、配管の長さを長くすることに
より、上記の目的が達成されるものである。したがって
、測定の間リファレンスセルへは、試料を含まないバッ
フ７タンク中の溶媒が微量ながら常時送酸され、リファ
レンスセル内の溶媒の状態変化を防ぐとともにサンプル
側の送液溶媒の状態変化を補償し、ダブルフロー型と同
程度の安定性を得ることが可能である。Injection of the sample is performed with this cleaning valve closed. The sample injected from the sample injector (I) is transferred to the separation column (C
), but at this time, about 1/1000 of the sample also flows into the reference side flow path. The sample in this reference side flow path is fed by the flow on the reference side, but for a certain period of time determined by the volume of the reference side flow path including the buffer tank (T) and the ratio of the reference side flow path, the sample is transferred to the reference side flow path. remains within the cell and does not flow into the reference cell. This buffer tongue (T) achieves the above purpose by increasing the diameter of the pipe or increasing the length of the pipe. Therefore, during measurement, a small amount of the solvent in the buffer 7 tank that does not contain the sample is constantly fed to the reference cell, preventing changes in the state of the solvent in the reference cell and compensating for changes in the state of the sending solvent on the sample side. However, it is possible to obtain stability comparable to that of the double flow type.
第２図は、サンプルセルへ流入する送液溶媒の一部をサ
ンプルセル出口で分岐し、リファレンスセルへの送液溶
媒とする例である。FIG. 2 shows an example in which a part of the liquid-feeding solvent flowing into the sample cell is branched off at the sample cell outlet and is used as the liquid-feeding solvent to the reference cell.
測定の方法としては、洗浄バルブ（Ｖ）により、リファ
レンスセル出口と検出器出口を接続、サンプルセル出口
と検出器出口とを遮断する。この状態でポンプ（Ｐ）に
より送液すると、サンプルセルへの流入した溶媒の金星
がバッファタンク、リファレンスセルを経て検出器出口
へ流れ、流路は洗浄される。As for the measurement method, the reference cell outlet and the detector outlet are connected by a cleaning valve (V), and the sample cell outlet and the detector outlet are shut off. When the pump (P) is used to send the liquid in this state, the solvent Venus that has flowed into the sample cell flows to the detector outlet via the buffer tank and the reference cell, thereby cleaning the flow path.
流路の洗浄が終了した後、洗浄バルブを切り換え、サン
プルセルと検出器出口を接続し、リファレンスセルと検
出器出口を遮断する。この状態では、リファレンスセル
への流；は抵抗（ｒ）によりサンプルセルへの流量の約
１／１０００に制限される。試料の注入は、リファレン
スセルへの流量が制限された状態で行う。試料注入器（
１）から注入された試料は、分離カラム（Ｃ）、サンプ
ルセルを経て検出器出口へ送液されるが、試料の約１／
１０００は分岐点よりリファレンス側流路へ流入する。After cleaning the flow path, switch the cleaning valve, connect the sample cell and the detector outlet, and shut off the reference cell and the detector outlet. In this state, the flow to the reference cell is limited by resistance (r) to about 1/1000 of the flow to the sample cell. The sample is injected while the flow rate to the reference cell is restricted. Sample injector (
The sample injected from 1) is sent to the detector outlet via the separation column (C) and the sample cell, but about 1/2 of the sample is
1000 flows into the reference side flow path from the branch point.
このリファレンス側流路内の試料は、リファレンス側の
流れにより送液されるが、バッファタンク（Ｔ）の容積
とリファレンス側流量の比により定まる一定時間、バッ
ファタンク内にょリ、リファレンスセルへの流入は起こ
らな％％０前記一定時間、リファレンスセルへ番よ試料
を含まないバッファタンク中の溶媒が微量な力（ら常■
寺送液され、リファレンスセル内の溶媒の状態変イヒを
防ぐとともに、サンプル側の送液溶媒の状態変イヒを補
償し、ダブルフロー型と同程度の安定性を得ることが可
能となる。The sample in this reference side channel is transported by the flow on the reference side, but for a certain period of time determined by the ratio of the volume of the buffer tank (T) and the flow rate on the reference side, the sample flows into the buffer tank and flows into the reference cell. %%0 During the specified period of time, the solvent in the buffer tank that does not contain the sample is transferred to the reference cell under a small amount of force (normally
In addition to preventing changes in the state of the solvent in the reference cell when the liquid is sent to the sample side, it also compensates for changes in the state of the sending solvent on the sample side, making it possible to obtain stability comparable to that of the double flow type.
第３図は、サンプルセルへの送液される溶媒の一部をサ
ンプルセル入口及びサンプルセル分岐し、リファレンス
セルへの送液溶媒とする例である。FIG. 3 is an example in which a part of the solvent sent to the sample cell is branched off to the sample cell inlet and used as the solvent sent to the reference cell.
測定手順としては、まず洗浄）くルブ（Ｖ）によりサン
プルセル入口の分岐点１とノく・ソファタンク（Ｔ）を
接続する。この状態でポンプ（Ｐ） ｊこより送液する
と、溶媒は分岐点１よりほぼ均等１こ分流し、サンプル
セル側、リファレンスセル側番流路は洗浄される。As for the measurement procedure, first connect the branch point 1 of the sample cell inlet and the sofa tank (T) using the cleaning tube (V). In this state, when the pump (P) pumps the liquid, the solvent flows almost evenly from the branch point 1, and the flow paths on the sample cell side and the reference cell side are cleaned.
流路の洗浄が終了した後、洗浄ノくルブ（Ｖ）を切り換
え、分岐点１とバ・ソファタンクを遮断すると、リファ
レンスセルへの流量は抵抗（ｒ）によリサンプルセルへ
の流量の約１／１０００に制限される。After cleaning the flow path, switch the cleaning knob (V) to shut off branch point 1 and the bath tank, and the flow rate to the reference cell will be the same as the flow rate to the resample cell due to the resistance (r). It is limited to about 1/1000.
試料の注入はリファレンスセルへの流量が制限された状
態で行う。試料注入器（１）より注入された試料は分離
カラム（Ｃ）、サンプルセルを経て検出器出口へ送液さ
れるが、試料の約１／１０００はサンプルセル出口の分
岐点よりリファレンス側流路へ流入する。このリファレ
ンス側流路内の試料は、リファレンス側の流れにより送
液されるが、バッファタンクの容積とリファレンス側流
量の比により定まる一定時間、バッファタンク内に留ま
り、サンプルセルへの流入は起こらない。The sample is injected while the flow rate to the reference cell is restricted. The sample injected from the sample injector (1) is sent to the detector outlet via the separation column (C) and the sample cell, but about 1/1000 of the sample is sent to the reference side flow path from the branch point at the sample cell outlet. flows into. The sample in this reference side channel is transported by the flow on the reference side, but remains in the buffer tank for a certain period of time determined by the ratio of the volume of the buffer tank and the flow rate on the reference side, and does not flow into the sample cell. .
前記一定時間、リファレンスセルへは試料を含まないバ
ッファタンク内の溶媒が微量ながら常時送液され、リフ
ァレンスセル内の溶媒の状態変化を防ぐとともに、サン
プル側の送液溶媒の状態変化を補償し、ダブルフロー型
と同程度の安定性を得ることが可能となる。During the certain period of time, a small amount of the solvent in the buffer tank that does not contain the sample is constantly sent to the reference cell to prevent changes in the state of the solvent in the reference cell and to compensate for changes in the state of the sending solvent on the sample side. It becomes possible to obtain the same level of stability as the double flow type.
第４図は、送液溶媒の一部をサンプルセル出口で分岐し
、リファレンスセルへの送液溶媒とする実施例であり、
分岐タンク（Ｊ）の内部にテフロン製バッファタンク（
Ｔ）を設け、ノ＜・ソファタンク内の溶媒の溶存ガスの
変化を補償する構造である。FIG. 4 shows an example in which a part of the liquid feeding solvent is branched at the sample cell outlet and is used as the liquid feeding solvent to the reference cell.
There is a Teflon buffer tank (
T) is provided to compensate for changes in dissolved gas in the solvent in the tank.
ｉ’ｌＦＩ定方法と定石法、まず洗浄バルブ（Ｖ）によ
り分岐タンク（Ｊ）と検出器出口を遮断し、リフアレン
セル出口と検出器出口とを接続する。この状態でポンプ
（Ｐ）により送液を行うと、送液溶媒は、サンプルセル
（Ｓ）、分岐タンク（Ｊ）、バッファタンク（Ｔ）、リ
ファレンスセル（Ｒ）を流れ、各セルの洗浄が行われる
。i'lFI determination method and established method: First, the branch tank (J) and the detector outlet are shut off using the cleaning valve (V), and the reference cell outlet and the detector outlet are connected. When the pump (P) is used to send liquid in this state, the sending solvent flows through the sample cell (S), branch tank (J), buffer tank (T), and reference cell (R), and each cell is washed. It will be done.
流路の洗浄が終了した後、洗浄バルブ（Ｖ）を切り変え
、分岐タンク（Ｊ）と検出器出口を接続し、リファレン
スセルと検出器出口遮断すると、リファレンスセルへの
流量は抵抗（「）によりサンプルセルへの流量の約１／
１０００に制限される。After cleaning the flow path, switch the cleaning valve (V), connect the branch tank (J) and the detector outlet, and shut off the reference cell and detector outlet. Approximately 1/1/2 of the flow rate to the sample cell
Limited to 1000.
試料の注入は、リファレンスセルへの流量が制限された
状態で行う。試料注入器（１）より注入された試料は分
離カラム（Ｃ）、サンプルセル、分岐タンクを経て検出
器出口へ送液されるが、試料の約１／１０００は、分岐
タンク内においてバッファタンクよりリファレンス側流
路へ流入する。The sample is injected while the flow rate to the reference cell is restricted. The sample injected from the sample injector (1) is sent to the detector outlet via the separation column (C), sample cell, and branch tank, but about 1/1000 of the sample is transferred from the buffer tank in the branch tank. Flows into the reference side flow path.
このリファレス側流路内の試料は、リファレンス側の流
れにより送液されるが、バッファタンクの容積とリファ
レンス側流量の比により定まる一定時間、バッファタン
ク内にに留まり、サンプルセルへは流入しない。前記一
定時間、リファレンスセルへは試料を含まないバッファ
タンク内の溶媒が微量ながら常時送液され、リファレン
スセル内の溶媒の状態変化を防ぐとともに、サンプル側
の送液溶媒の状態変化を補償し、ダブルフロー型と同程
度の安定性を得ることが可能となる。The sample in this reference side flow path is sent by the flow on the reference side, but remains in the buffer tank for a certain period of time determined by the ratio of the volume of the buffer tank and the flow rate on the reference side, and does not flow into the sample cell. During the certain period of time, a small amount of the solvent in the buffer tank that does not contain the sample is constantly sent to the reference cell to prevent changes in the state of the solvent in the reference cell and to compensate for changes in the state of the sending solvent on the sample side. It becomes possible to obtain the same level of stability as the double flow type.
（発明の効果）
以上、本発明によれば、次の様な効果を得ることができ
る。(Effects of the Invention) As described above, according to the present invention, the following effects can be obtained.
（１）検出器外部よりサンプルセルへの単一流路でよい
。(1) A single flow path from outside the detector to the sample cell is sufficient.
（２）別途リファレンスセルへの送液が不要なため、溶
媒の消費量がダブルフロー型Ｒ１検出器の約半分となる
。(2) Since there is no need to separately send liquid to the reference cell, the amount of solvent consumed is approximately half that of the double flow type R1 detector.
（３）流量及び外的影響を補償するためのリファレンス
セル用分離カラムが不要である。(3) No reference cell separation column is required to compensate for flow rates and external influences.
（４）単一流路でダブルフロー型Ｒ１検出器と同程度の
安定性が得られる。(4) A single flow path provides the same level of stability as a double flow type R1 detector.
（５）洗浄操作により、連続的な使用が可能である。(5) Continuous use is possible through cleaning operations.
第１〜４図は本発明の実施の態様をそれぞれ示す流路図
である。
Ｐ・・・試料注入器 Ｉ・・・試料注入器Ｃ・・
・分離カラム ｒ・・・抵抗■・・・洗浄バルブ
Ｔ・・・バッファタンクＪ・・・分岐タンク
Ｓ・・・サンプルセルＲ・・・リファレンスセル
Ｄ・・・検出器特許出願人 東ソー株式会社1 to 4 are flow path diagrams showing embodiments of the present invention, respectively. P...Sample injector I...Sample injector C...
・Separation column r...Resistance ■...Washing valve T...Buffer tank J...Branch tank
S...Sample cell R...Reference cell D...Detector patent applicant Tosoh Corporation
Claims (1)
のサンプルセルに流入する溶媒又はサンプルセルから流
出した溶媒の一部をリファレンスセルに送液することを
特徴とする液体クロマトグラフ用示差屈折率検出器。Differential refraction for liquid chromatography, characterized in that a part of the solvent flowing into the sample cell of a differential refractive index detector after separating sample components in a separation column or the solvent flowing out from the sample cell is sent to a reference cell. rate detector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12900590A JP3146485B2 (en) | 1990-05-21 | 1990-05-21 | Differential refractive index detector for liquid chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12900590A JP3146485B2 (en) | 1990-05-21 | 1990-05-21 | Differential refractive index detector for liquid chromatography |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0424540A true JPH0424540A (en) | 1992-01-28 |
| JP3146485B2 JP3146485B2 (en) | 2001-03-19 |
Family
ID=14998800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12900590A Expired - Lifetime JP3146485B2 (en) | 1990-05-21 | 1990-05-21 | Differential refractive index detector for liquid chromatography |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3146485B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6295125B1 (en) * | 1999-07-23 | 2001-09-25 | Showa Denko K.K. | Differential refractive index detector and liquid chromatograph equipped with the same |
| US7551270B2 (en) | 2006-07-28 | 2009-06-23 | Shimadzu Corporation | Differential refractive index detector |
-
1990
- 1990-05-21 JP JP12900590A patent/JP3146485B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6295125B1 (en) * | 1999-07-23 | 2001-09-25 | Showa Denko K.K. | Differential refractive index detector and liquid chromatograph equipped with the same |
| US7551270B2 (en) | 2006-07-28 | 2009-06-23 | Shimadzu Corporation | Differential refractive index detector |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3146485B2 (en) | 2001-03-19 |
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