JPH062518B2 - Quantitative liquid transfer device for fluid chromatograph - Google Patents
Quantitative liquid transfer device for fluid chromatographInfo
- Publication number
- JPH062518B2 JPH062518B2 JP59085600A JP8560084A JPH062518B2 JP H062518 B2 JPH062518 B2 JP H062518B2 JP 59085600 A JP59085600 A JP 59085600A JP 8560084 A JP8560084 A JP 8560084A JP H062518 B2 JPH062518 B2 JP H062518B2
- Authority
- JP
- Japan
- Prior art keywords
- liquid
- pipe line
- suction
- discharge
- return
- 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
Landscapes
- Loading And Unloading Of Fuel Tanks Or Ships (AREA)
- Reciprocating Pumps (AREA)
- Control Of Positive-Displacement Pumps (AREA)
- Pipeline Systems (AREA)
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用定量送液装置に関し、
特に微量液体の吸引−吐出を繰返すポンプによる液体ク
ロマトグラフ用定量送液装置に関する。DETAILED DESCRIPTION OF THE INVENTION (a) Field of Industrial Application The present invention relates to a fixed-quantity liquid sending device for a liquid chromatograph,
In particular, the present invention relates to a constant-quantity liquid-feeding device for a liquid chromatograph, which uses a pump that repeats suction-discharge of a trace amount of liquid.
（ロ）従来技術 従来、例えば液体クロマトグラフに吸引−吐出を繰返す
ポンプによってそのポンプの吐出容量以下の範囲で移動
相を送液する場合には、必要量以上の余剰移動相はいわ
ゆるスプリット法により系外に取り出して捨てるとか、
または第２図に構成説明図を示すような送液装置で余剰
移動相を移動相容器に戻すことが行われている。前者の
方法では大量の移動相が失なわれ不経済であり、後者の
場合は前者のような問題はないが次のような問題点があ
る。(B) Conventional technology Conventionally, for example, when a mobile phase is pumped by a pump that repeats suction-discharge to a liquid chromatograph in a range not more than the discharge capacity of the pump, excess mobile phase of a necessary amount or more is obtained by a so-called split method. Like taking it out of the system and throwing it away,
Alternatively, the surplus mobile phase is returned to the mobile phase container by a liquid delivery device as shown in the configuration diagram of FIG. The former method loses a large amount of mobile phase and is uneconomical. In the latter case, there is no problem like the former, but there are the following problems.
第２図において移動相容器(11)中の移動相(12)は吸引管
路(13)を通じてプランジャーポンプ(14)によって吸引−
吐出され、吐出管路(15)を通じて液体クロマトグラフ部
(16)に送られる。そのときに吸引−吐出される移動相の
一部が、カラム(17)を具備する戻り管路(18)を通じて移
動相容器(11)に戻される。In FIG. 2, the mobile phase (12) in the mobile phase container (11) is sucked by the plunger pump (14) through the suction conduit (13).
Discharged, liquid chromatograph section through discharge line (15)
Sent to (16). At that time, a part of the mobile phase sucked and discharged is returned to the mobile phase container (11) through the return conduit (18) provided with the column (17).
この場合戻される移動相容はカラムを有する戻り管路を
通過する際にジュール熱が発生する。その結果移動相(1
2)の温度が時間の経過とともに上昇するので、移動相の
送液量が変化するとともに液体クロマトグラフ部のカラ
ム温度も変化しその化学平衡がずれることから、クロマ
トグラフのリテンションタイムが変動し、分析値の再現
性が低下する。In this case, the returned mobile phase generates Joule heat when passing through the return line having the column. As a result, the mobile phase (1
Since the temperature of 2) rises with the passage of time, the liquid phase flow rate of the mobile phase changes and the column temperature of the liquid chromatograph part also changes, which shifts the chemical equilibrium, thus changing the retention time of the chromatograph, The reproducibility of the analytical value decreases.
したがって第２図に示すような送液装置では再現性良好
で高い精度の液体クロマトグラフ分析は困難である。Therefore, it is difficult to perform liquid chromatographic analysis with good reproducibility and high accuracy using the liquid delivery device as shown in FIG.
この発明は上記のような問題点を改善するためになされ
たものである。The present invention has been made to solve the above problems.
（ハ）目的 この発明の目的は、微量の液体を、温度変動を防止し高
精度の送液量で送液する液体クロマトグラフ用定量送液
装置を提供するにある。(C) Object An object of the present invention is to provide a quantitative liquid sending device for a liquid chromatograph that sends a small amount of liquid with a highly accurate liquid sending amount while preventing temperature fluctuation.
（ニ）構成 この発明は液体容器、吸引−吐出を繰返す定量送液ポン
プ、送液ポンプの吸引側と液体容器を連結する吸引管
路、送液ポンプの吐出側と液体クロマトグラフ部とを連
結する吐出管路、及び吸引管路と吐出管路とを連結しか
つカラムを有する戻り管路とからなり、吸引管路と戻り
管路との連結部から液体容器に至るまでの吸引管路の内
容積が、戻り液が液体容器に戻らず吸引管路内に貯留さ
れるのを保障し、微量液体の温度変動を防ぐのに足る内
容積であることを特徴とする液体クロマトグラフ用定量
送液装置を提供するものである。(D) Structure The present invention relates to a liquid container, a fixed-quantity liquid supply pump that repeats suction-discharge, a suction pipe line that connects the suction side of the liquid supply pump and the liquid container, and a discharge side of the liquid supply pump and the liquid chromatograph section. Of the suction pipeline from the connecting portion between the suction pipeline and the return pipeline to the liquid container. Quantitative delivery for a liquid chromatograph characterized in that the internal volume is sufficient to ensure that the return liquid is not returned to the liquid container and is stored in the suction pipe line and to prevent temperature fluctuations of a trace amount of liquid. A liquid device is provided.
この発明の装置は、液体容器中の液体を該ポンプによっ
て吸引管路を通じて吸引し吐出管路を通じて吐出して吐
出管路に連結された液体クロマトグラフ部に送り、吐出
液の一部が戻り管路に戻される。戻り管路にはカラムが
具備され、例えば戻り液量を吐出液量の１／10にしたい
ときは液体クロマトグラフ部の送液抵抗と戻り管路＋吸
引管路の送液抵抗を９：１に調整される。The apparatus of the present invention is such that the liquid in the liquid container is sucked by the pump through the suction pipeline, discharged through the discharge pipeline and sent to the liquid chromatograph unit connected to the discharge pipeline, and a part of the discharge fluid is returned to the return pipe. Returned to the road. A column is provided in the return pipe line. For example, when it is desired to make the return liquid volume 1/10 of the discharge liquid volume, the liquid transfer resistance of the liquid chromatograph section and the liquid transfer resistance of the return pipe line + the suction pipe line are set to 9: 1. Adjusted to.
そして吸引管路と戻り管路との連結部から液体容器に至
るまでの吸引管路の内容積が、戻り液が液体容器に戻ら
ず吸引管路内に貯留されるのを保障するに足る内容積で
あり、具体的には少なくも一回の戻り液容積より大きい
ので、戻り液は液体容器内の液体中にまで戻ることはな
い。そして液体クロマトグラフ部に送られる液体の温度
は吸引管路、送液ポンプ及び戻り管路の循環系で短時間
のうちに平衡に達するので、高精度で定量送液ができ、
かつ液体クロマトグラフ部の温度も短時間で平衡に達し
温度変動がほとんどない。The content of the suction pipe line from the connection between the suction pipe line and the return pipe line to the liquid container is sufficient to ensure that the return liquid is stored in the suction pipe line without returning to the liquid container. The return liquid does not return to the liquid in the liquid container because it is a product, and is larger than at least one return liquid volume. And since the temperature of the liquid sent to the liquid chromatograph reaches equilibrium in a short time in the circulation system of the suction pipe line, the liquid feed pump and the return pipe line, it is possible to quantitatively deliver liquid with high accuracy,
Moreover, the temperature of the liquid chromatograph reaches equilibrium in a short time, and the temperature hardly changes.
この発明の装置に用いられる送液ポンプとしてはプラン
ジャーポンプ（逆止弁付）、ギヤポンプ、ダイヤフラム
ポンプなどが挙げられ、とくに100μl/min程度の微量吐
出量の吸引−吐出を繰返す送液ポンプが用いられる。Examples of the liquid-sending pump used in the device of the present invention include a plunger pump (with a check valve), a gear pump, a diaphragm pump, and the like, and particularly a liquid-sending pump that repeats suction-discharge of a minute discharge amount of about 100 μl / min. Used.
吸引管路、吐出管路及び戻り管路としては従来用いられ
ている、例えばテフロンチューブ、ステンレスチューブ
などが用いられる。As the suction pipe line, the discharge pipe line and the return pipe line, for example, a Teflon tube, a stainless tube or the like which is conventionally used is used.
（ホ）実施例 第１図にこの発明の装置の一実施例である液体クロマト
グラフ用の移動相送液装置の構成説明図を示した。(E) Example FIG. 1 shows an explanatory diagram of the configuration of a mobile phase liquid sending apparatus for a liquid chromatograph, which is an example of the apparatus of the present invention.
すなわち、(1)は移動相(2)の入った移動相容器である。
吸引管路(3)は、その一端が吸引側と吐出側に逆止弁
(C1)(C2)を有するプランジャーポンプ(4)の吸引側に連
結され、他方端には吸引フィルター(F)が取付けられ、
移動相(2)内に入れられている。一方プランジャーポン
プ(4)の吐出側には吐出管路(5)と液体クロマトグラフ
(6)とが順に連結されている。そしてカラム(7)を具備す
る戻り管路(8)がＴ字管(T1)と(T2)によって吸引管路(3)
と吐出管路(5)に連結されている。That is, (1) is a mobile phase container containing the mobile phase (2).
The suction pipe line (3) has a check valve at one end on the suction side and the discharge side.
(C 1 ) (C 2 ) is connected to the suction side of the plunger pump (4), the suction filter (F) is attached to the other end,
It is contained in the mobile phase (2). On the other hand, on the discharge side of the plunger pump (4), the discharge line (5) and the liquid chromatograph
(6) and are connected in order. And the return line (8) equipped with the column (7) is connected by the T-tubes (T 1 ) and (T 2 ) to the suction line (3).
And the discharge line (5).
移動相(2)はプランジャーポンプ(4)によって吸引フィル
ター(F)と吸引管路(3)を通じて吸引され吐出管路(5)を
通じて液体クロマトグラフ部(6)に送られる。そして吐
出液の一部は戻り管路(8)を通じて戻される。例えば液
体クロマトグラフ部(6)の送液抵抗と戻り管路(8)＋吸引
管路(3)の送液抵抗との比率を９：１調整しておけば吐
出液の９／10が戻される。しかし吸引管路(3)における
戻り管路(8)が連結されている部位から移動相までの内
容積の合計が一回の戻り液容積より大きいので戻り液が
移動相(2)には入らない。そして吐出液の温度は短時間
で平衡に達するので、高精度で定量送液することがで
き、液体クロマトグラフのカラムの温度も変動が小さく
再現性の良好な分析を行うことができる。The mobile phase (2) is sucked by the plunger pump (4) through the suction filter (F) and the suction conduit (3) and sent to the liquid chromatograph section (6) through the discharge conduit (5). Then, a part of the discharged liquid is returned through the return line (8). For example, if you adjust the ratio of the liquid sending resistance of the liquid chromatograph section (6) to the liquid sending resistance of the return line (8) + the suction line (3) to 9: 1, 9/10 of the discharged liquid will be returned. Be done. However, since the total internal volume from the part where the return line (8) is connected in the suction line (3) to the mobile phase is larger than the volume of return liquid once, the return liquid does not enter the mobile phase (2). Absent. Further, since the temperature of the discharged liquid reaches equilibrium in a short time, it is possible to carry out quantitative liquid feeding with high accuracy, and the temperature of the column of the liquid chromatograph has little fluctuation and can be analyzed with good reproducibility.
（ヘ）効果 この発明の装置によれば、微量液体を、温度の変動を防
止し高精度の吐出量で送液することができる。(F) Effect According to the device of the present invention, it is possible to prevent the temperature from fluctuating and send the liquid in a highly accurate discharge amount.
第１図はこの発明の一実施例の液体クロマトグラフ用定
量送液装置の構成説明図、第２図は従来の液体クロマト
グラフ用定量送液装置の一例の構成説明図である。 (1,11)…移動相容器、(2,12)…移動相、 (C1.C2.C′1.C′2)…逆止弁、 (4,14)…プランジャーポンプ、 （Ca,Ca′）…カム、（Ph,Ph′）…ポンプヘッド、 (5,15)…吐出管路、 （6,6′）…液体クロマトグラフ部、 (7,17)…カラム、(8,18)…戻り管路、 （F,F′）…吸引フィルター、 (T1.T2.T′2)…Ｔ字管。FIG. 1 is a structural explanatory view of a quantitative liquid sending device for a liquid chromatograph according to an embodiment of the present invention, and FIG. 2 is a structural explanatory view of an example of a conventional quantitative liquid sending device for a liquid chromatograph. (1,11)… Mobile phase container, (2,12)… Mobile phase, (C 1 .C 2 .C ′ 1 .C ′ 2 )… Check valve, (4,14)… Plunger pump, ( Ca, Ca ′)… Cam, (Ph, Ph ′)… Pump head, (5,15)… Discharge line, (6,6 ′)… Liquid chromatograph, (7,17)… Column, (8 , 18)… Return line, (F, F ′)… Suction filter, (T 1 .T 2 .T ′ 2 ) ... T tube.
Claims (1)
定量送液ポンプ、送液ポンプの吸引側と液体容器を連結
する吸引管路、送液ポンプの吐出側と液体クロマトグラ
フ部とを連結する吐出管路、及び吸引管路と吐出管路と
を連結しかつカラムを有する戻り管路とからなり、吸引
管路と戻り管路との連結部から液体容器に至るまでの吸
引管路の内容積が、戻り液が液体容器に戻らず吸引管路
内に貯留されるのを保障し、微量液体の温度変動を防ぐ
のに足る内容積であることを特徴とする液体クロマトグ
ラフ用定量送液装置。1. A liquid container, a fixed amount liquid feed pump for repeating suction-discharge of a trace amount of liquid, a suction pipe line connecting the suction side of the liquid feed pump and the liquid container, a discharge side of the liquid feed pump and a liquid chromatograph section. A suction pipe line that is composed of a discharge pipe line to be connected and a return pipe line that connects the suction pipe line and the discharge pipe line and has a column, and from the connecting portion of the suction pipe line and the return pipe line to the liquid container. Quantitative determination for liquid chromatograph characterized by ensuring that the return liquid is stored in the suction pipe line without returning to the liquid container and prevents the temperature fluctuation of a trace amount of liquid. Liquid transfer device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59085600A JPH062518B2 (en) | 1984-04-26 | 1984-04-26 | Quantitative liquid transfer device for fluid chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59085600A JPH062518B2 (en) | 1984-04-26 | 1984-04-26 | Quantitative liquid transfer device for fluid chromatograph |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60228300A JPS60228300A (en) | 1985-11-13 |
| JPH062518B2 true JPH062518B2 (en) | 1994-01-12 |
Family
ID=13863315
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59085600A Expired - Fee Related JPH062518B2 (en) | 1984-04-26 | 1984-04-26 | Quantitative liquid transfer device for fluid chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH062518B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7001457B2 (en) | 2001-05-01 | 2006-02-21 | Ricoh Company, Ltd. | Crystal growth method, crystal growth apparatus, group-III nitride crystal and group-III nitride semiconductor device |
| JP4640899B2 (en) * | 2001-06-28 | 2011-03-02 | 株式会社リコー | Group III nitride crystal growth equipment |
| JP2005145479A (en) * | 2003-11-12 | 2005-06-09 | Norichika Azuma | Collection device of liquid from automobile to be dismantled |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6026921B2 (en) * | 1979-09-05 | 1985-06-26 | 株式会社東芝 | Boiler feed pump control device |
-
1984
- 1984-04-26 JP JP59085600A patent/JPH062518B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60228300A (en) | 1985-11-13 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |