JP2516332B2 - Fluid pump with temperature controller to keep mass flow rate constant - Google Patents
Fluid pump with temperature controller to keep mass flow rate constantInfo
- Publication number
- JP2516332B2 JP2516332B2 JP60186814A JP18681485A JP2516332B2 JP 2516332 B2 JP2516332 B2 JP 2516332B2 JP 60186814 A JP60186814 A JP 60186814A JP 18681485 A JP18681485 A JP 18681485A JP 2516332 B2 JP2516332 B2 JP 2516332B2
- Authority
- JP
- Japan
- Prior art keywords
- fluid
- fluid pump
- temperature
- flow rate
- constant
- 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
- Reciprocating Pumps (AREA)
Description
【発明の詳細な説明】 発明の目的 産業上の利用分野 本発明はクロマトグラフィ用送液ポンプとして主に使
われる流体ポンプに関し、特に流入する流体及びポンプ
チェンバを一定温度に保持して流体の質量流量を一定に
保つ温調装置付流体ポンプに関するものである。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fluid pump mainly used as a liquid-sending pump for chromatography, and more particularly to a fluid flow rate and a mass flow rate of the fluid which are maintained at a constant temperature of the inflowing fluid and the pump chamber. The present invention relates to a fluid pump with a temperature control device that keeps the temperature constant.
従来技術 HPLC,SFC(超臨界流体クロマトグラフィ)等のクロマ
トグラフィ用送液ポンプとしては、従来往復動ピストン
型が一般に使われている。この種の流体ポンプは、流体
の流入のみを許容する逆止弁を備えた流入路と流体の流
出のみを許容する逆止弁を備えた流出路と連通したチェ
ンバを有し、チェンバ内でピストンを往復動させること
で流体を吸引・吐出するものである。この型式のポンプ
の単位時間当りの吐出量は次のように表わされる: Q=K・Vc・N 但しKは効率、Vcはピストンの移動による容積変化を
体積で表わした値、Nは単位時間当りのピストンのスト
ローク数。2. Description of the Related Art Conventionally, a reciprocating piston type pump is generally used as a liquid delivery pump for chromatography such as HPLC and SFC (supercritical fluid chromatography). This type of fluid pump has a chamber communicating with an inflow passage having a check valve that allows only the inflow of fluid and an outflow passage having a check valve that allows only the outflow of fluid, and a piston in the chamber. The fluid is sucked and discharged by reciprocating. The discharge rate per unit time of this type of pump is expressed as follows: Q = K · Vc · N where K is efficiency, Vc is the volume change due to piston movement in volume, and N is the unit time. Number of strokes of piston per hit.
上記の吐出量はポンプの構造、逆止弁の効率、流体の
圧縮率、背圧の大きさによって変化するが、要するに従
来のこの種流体ポンプは単位時間当り一定体積の流体を
送出する。時間的変動を生ずる効率の変化については、
背圧等をモニタし予め定められた分だけ単位時間当りの
ストローク数を増減することによってかなり良く補正可
能である。The above-mentioned discharge amount varies depending on the structure of the pump, the efficiency of the check valve, the compressibility of the fluid, and the magnitude of the back pressure. In short, the conventional fluid pump of this type delivers a constant volume of fluid per unit time. For changes in efficiency that cause temporal fluctuations,
It can be corrected quite well by monitoring back pressure and increasing / decreasing the number of strokes per unit time by a predetermined amount.
発明が解決しようとする問題点 しかしながら、液体クロマトグラフィ等で用いられる
有機溶媒は、例えばメチルアルコールの場合、温度1℃
当りの体積膨張は0.12%にも及び、ポンプの体積流量は
一定であっても、質量流量は温度によって大きく左右さ
れる。この温度が質量流量に及ぼす影響を第1図のグラ
フに示す。図中横軸は温度(℃),点線縦軸は体積流量
(ml/min),実線縦軸は質量流量(g/min)で、体積流
量を0.4ml/min(菱形),1.0ml/min(3角),5.0ml/min
(4角)及び9.9ml/min(丸)とした場合(破線)の質
量流量(実線)を示している。Problems to be Solved by the Invention However, when the organic solvent used in liquid chromatography or the like is, for example, methyl alcohol, the temperature is 1 ° C.
The volume expansion per unit reaches 0.12%, and even if the volumetric flow rate of the pump is constant, the mass flow rate greatly depends on the temperature. The effect of this temperature on the mass flow rate is shown in the graph of FIG. In the figure, the horizontal axis is temperature (° C), the dotted vertical axis is the volume flow rate (ml / min), the solid vertical axis is the mass flow rate (g / min), and the volume flow rate is 0.4 ml / min (diamond), 1.0 ml / min (Triangle), 5.0 ml / min
The mass flow rate (solid line) is shown for (square) and 9.9 ml / min (circle) (broken line).
現在HPLCにおいて要求される流量精密度は1%以上で
あり、特に分子量分布の測定に用いられるGPC(ゲル・
パーミエーション・クロマトグラフィ)では0.1%とい
う値が要求されている。従来、保持時間の良好な再現性
を得るため、カラム部を一定温度に保つことが行なわれ
ており、ある程度の効果を得ている。しかし上述のごと
く、従来ポンプの送出流量は体積流量でのみ制御されて
いるため、室温変化による溶媒温度の変化、機械的摩擦
等によるチェンバ内の温度上昇等によって体積流量は一
定であっても、質量流量は大きく変化する。この結果、
カラム部の温度を一定に保っていても、カラムを流通す
る溶媒の質量流量が変化し、試料成分の保持時間を一定
に保つのが不可能となる。At present, the flow rate accuracy required for HPLC is 1% or more, and especially GPC (gel
A value of 0.1% is required for permeation chromatography). Conventionally, in order to obtain a good reproducibility of the holding time, the column part has been kept at a constant temperature, and some effects have been obtained. However, as described above, since the delivery flow rate of the conventional pump is controlled only by the volumetric flow rate, even if the volumetric flow rate is constant due to changes in the solvent temperature due to room temperature changes, temperature rise in the chamber due to mechanical friction, etc., Mass flow rates vary greatly. As a result,
Even if the temperature of the column section is kept constant, the mass flow rate of the solvent flowing through the column changes, and it becomes impossible to keep the retention time of the sample components constant.
従って本発明の目的は、上記の点を改良し、流体(溶
媒)温度とチェッバ温度を一定に保持することによって
質量流量を一定に保つ流体ポンプを提供するものであ
る。Therefore, an object of the present invention is to improve the above points and provide a fluid pump which keeps a mass flow rate constant by keeping a fluid (solvent) temperature and a Cheber temperature constant.
発明の構成 問題点を解決するための手段 上記の目的を達成するため、本発明による流体ポンプ
は、流入のみを許容する流入路と流出のみを許容する流
出路と連通したチェンバをヘッドに備え、該チェンバ内
でピストンを往復動させることによって流体を吸引吐出
する流体ポンプにおいて、ポンプに流入する流体及びポ
ンプチェンバを一定温度に保持する手段を備えたことを
特徴とするものである。Means for Solving the Problems In order to achieve the above-mentioned object, a fluid pump according to the present invention comprises, in a head, a chamber that communicates with an inflow passage that allows only inflow and an outflow passage that allows only outflow. A fluid pump for sucking and discharging a fluid by reciprocating a piston in the chamber is provided with means for holding the fluid flowing into the pump and the pump chamber at a constant temperature.
前記一定温度に保持する手段は、流体を通す熱平衡コ
イルと、ヘッドに接続されたアルミブロックと、該アル
ミブロックの温度を一定に保持する循環恒温槽等の手段
とを備えて成るのが好ましい。The means for maintaining the constant temperature preferably comprises a heat balancing coil for passing a fluid, an aluminum block connected to the head, and a means such as a circulation constant temperature bath for keeping the temperature of the aluminum block constant.
実施例 以下本発明の一実施例を第2図を参照して詳しく説明
する。Embodiment An embodiment of the present invention will be described in detail below with reference to FIG.
第2図は本発明による流体ポンプの構成を概略的に示
した図で、図中3がポンプのヘッドであり、ヘッド3に
は吸引管6をヘッドに取付ける入口部材7と吐出管8を
ヘッドに取付ける出口部材9が設けられている。FIG. 2 is a diagram schematically showing the structure of a fluid pump according to the present invention. In the figure, 3 is a head of a pump, and an inlet member 7 for attaching a suction pipe 6 to the head and a discharge pipe 8 are provided in the head 3. An outlet member 9 to be attached to is provided.
ヘッド3の内部構成は良く知られているので特に図示
しないが、簡単に説明すると、ヘッド3にはチェンバと
入口部材7、出口部材9を介して吸引管6、吐出管8と
連通する流入路、流出路がそれぞれ設けられ、チェンバ
は一側面(図中右側)で開口している。流入路には流入
のみを許容する逆止弁、流出路には流出のみを許容する
逆止弁が設けられているため、流体は一方向にのみ流れ
る。チェンバ内には液密シールを介してピストンが挿通
され、ピストンがピストン駆動装置10によって図中左右
方向に往復動されるにつれ、流体がチェンバ内に順次吸
引されそこから吐出される。Although the internal structure of the head 3 is well known, it is not shown in the figure, but in brief, the head 3 has an inflow passage communicating with the suction pipe 6 and the discharge pipe 8 through the chamber and the inlet member 7 and the outlet member 9. , Outflow channels are provided respectively, and the chamber is open on one side (right side in the figure). Since the inflow passage is provided with a check valve that allows only inflow and the outflow passage has a check valve that allows only outflow, the fluid flows only in one direction. A piston is inserted through a liquid-tight seal in the chamber, and as the piston is reciprocated in the left-right direction in the figure by the piston drive device 10, fluid is sequentially sucked into the chamber and discharged therefrom.
上記のごとき流体ポンプによって単位時間当り一定の
体積流量を吐出できるが、前述のごとく流体及びチェン
バの温度変化に伴い質量流量が変化するため、本発明で
はポンプへの流入流体及びチェンバの温度を一定に保持
する手段を設けることによって質量流量を一定に保つ。Although a constant volumetric flow rate can be discharged per unit time by the fluid pump as described above, the mass flow rate changes with the temperature change of the fluid and the chamber as described above, so in the present invention, the temperature of the fluid flowing into the pump and the temperature of the chamber are constant. The mass flow rate is kept constant by providing a means for holding it.
温度を一定に保持する上記手段の好ましい実施例を次
に説明する。第2図中1は流体の入ったボトルで、クロ
マトグラフィに適用されるときはメチルアルコール等の
有機溶媒が流体として使われる。溶媒はボトル1から吸
引管6を通ってヘッド3へ導かれるが、図示のごとく吸
引管6はその中間部が熱平衡コイル2に構成されてい
る。後述のアルミブロック4により熱平衡コイル2を取
巻く周囲温度は一定に保持されているので、溶媒は熱平
衡コイル2を通る間に一定温度とされ、周囲温度の変化
による影響を受けない。A preferred embodiment of the above means for keeping the temperature constant will now be described. In FIG. 2, reference numeral 1 is a bottle containing a fluid, and an organic solvent such as methyl alcohol is used as the fluid when applied to chromatography. The solvent is guided from the bottle 1 through the suction pipe 6 to the head 3, and as shown in the drawing, the suction pipe 6 has a heat balance coil 2 in the middle thereof. Since the ambient temperature surrounding the thermal equilibrium coil 2 is kept constant by the aluminum block 4 described later, the solvent is kept at a constant temperature while passing through the thermal equilibrium coil 2 and is not affected by the change in ambient temperature.
又本発明では、流体ポンプのヘッド3がアルミブロッ
ク4へ熱伝導可能に接続され、アルミブロック4は循環
恒温槽5から送られてくる熱媒体によって温度調節され
る。従って、ヘッド3内のチェンバは一定温度に保持さ
れ、機械的摩擦等による温度変化の影響を受けない。又
上述のごとく、アルミブロック4は熱平衡コイル2を含
む周囲の温度を一定に値持つ役割も果す。Further, in the present invention, the head 3 of the fluid pump is connected to the aluminum block 4 so as to be able to conduct heat, and the temperature of the aluminum block 4 is adjusted by the heat medium sent from the circulation constant temperature bath 5. Therefore, the chamber in the head 3 is maintained at a constant temperature and is not affected by temperature changes due to mechanical friction or the like. Further, as described above, the aluminum block 4 also plays a role of keeping the ambient temperature including the heat balance coil 2 at a constant value.
尚、図示の実施例では、循環恒温槽を使って温度調節
を行なっているが、温度調節の方法はこれに限られず、
ペルチェ素子を用いる等その他の方法によっても同様な
効果が得られる。In the illustrated embodiment, the temperature is controlled by using the circulation constant temperature bath, but the method of temperature control is not limited to this.
Similar effects can be obtained by other methods such as using a Peltier element.
発明の効果 以上述べたように本発明によれば、流入流体(溶媒)
とチェンバの温度を一定に保持することによって質量流
量を常時一定に保つ流体ポンプが得られるため、これを
クロマトグラフィに適用すれば試料成分の保持時間が周
囲温度やチェンバ温度の変化によって変動するのを防止
でき、特に高い流量精密が要求されるGPC等において大
きな効果を発揮する。As described above, according to the present invention, the inflow fluid (solvent)
Since the fluid pump that keeps the mass flow rate constant at all times can be obtained by keeping the chamber temperature and chamber temperature constant, the retention time of the sample components can be changed by the change of ambient temperature and chamber temperature if this is applied to chromatography. It can be prevented and exerts a great effect especially in GPC, etc., where high flow rate precision is required.
【図面の簡単な説明】 第1図は温度変化が質量流量に及ぼす影響を示すグラ
フ、第2図は本発明による流体ポンプの概略構成図であ
る。 1……流体(溶媒)ボトル、2……熱平衡コイル、3…
…ヘッド、4……アルミブロック、5……循環恒温槽、
6……吸引管、8……吐出管、10……ピストン駆動装
置。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a graph showing the effect of temperature change on mass flow rate, and FIG. 2 is a schematic configuration diagram of a fluid pump according to the present invention. 1 ... Fluid (solvent) bottle, 2 ... Thermal equilibrium coil, 3 ...
… Head, 4… Aluminum block, 5… Circulating constant temperature bath,
6 ... Suction pipe, 8 ... Discharge pipe, 10 ... Piston drive device.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 黒須 泰行 八王子市石川町2967番地の5 日本分光 工業株式会社内 (56)参考文献 実開 昭47−703(JP,U) 特公 昭36−8988(JP,B1) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Yasuyuki Kurosu 529-2967 Ishikawa-cho, Hachioji City, JASCO Corp. (56) References (JP, B1)
Claims (1)
容する流出路と連通したチェンバをヘッドに備え、該チ
ェンバ内でピストンを往復運動させることによって流体
を吸引吐出する流体ポンプにおいて、 前記流体ポンプに吸引される流体が貯留される溶媒ボト
ルと、 前記溶媒ボトルと流体ポンプの流入路を連通し、溶媒ボ
トル内の流体を流体ポンプの流入路に供給可能な略螺旋
状の管である熱平衡コイルと、 前記流体ポンプのヘッドと熱伝導可能に接続される金属
製のブロックと、 前記熱平衡コイル及び金属製ブロックの温度を一定に保
持可能な恒温手段と、 を備えたことを特徴とする質量流量を一定に保つ温調装
置付流体ポンプ。1. A fluid pump for sucking and discharging a fluid by providing a head with a chamber communicating with an inflow passage for allowing only an inflow and an outflow passage for allowing only an outflow, and reciprocally moving a piston in the chamber. A solvent bottle in which the fluid sucked by the fluid pump is stored, and a substantially spiral pipe that connects the solvent bottle and the inflow passage of the fluid pump and can supply the fluid in the solvent bottle to the inflow passage of the fluid pump. A heat balance coil; a metal block connected to the head of the fluid pump so as to be able to conduct heat; and a constant temperature unit capable of keeping the temperature of the heat balance coil and the metal block constant. Fluid pump with temperature controller that keeps the mass flow rate constant.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP60186814A JP2516332B2 (en) | 1985-08-26 | 1985-08-26 | Fluid pump with temperature controller to keep mass flow rate constant |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP60186814A JP2516332B2 (en) | 1985-08-26 | 1985-08-26 | Fluid pump with temperature controller to keep mass flow rate constant |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS6245982A JPS6245982A (en) | 1987-02-27 |
JP2516332B2 true JP2516332B2 (en) | 1996-07-24 |
Family
ID=16195057
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP60186814A Expired - Fee Related JP2516332B2 (en) | 1985-08-26 | 1985-08-26 | Fluid pump with temperature controller to keep mass flow rate constant |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2516332B2 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110494747A (en) * | 2017-04-26 | 2019-11-22 | 株式会社岛津制作所 | Liquid feeding device and fluid chromatograph |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5690828A (en) * | 1990-07-13 | 1997-11-25 | Isco, Inc. | Apparatus and method for supercritical fluid extraction |
JP5035959B2 (en) * | 2006-11-30 | 2012-09-26 | 独立行政法人産業技術総合研究所 | Method and apparatus for supplying fluid under high pressure |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS47703U (en) * | 1971-01-18 | 1972-08-05 |
-
1985
- 1985-08-26 JP JP60186814A patent/JP2516332B2/en not_active Expired - Fee Related
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110494747A (en) * | 2017-04-26 | 2019-11-22 | 株式会社岛津制作所 | Liquid feeding device and fluid chromatograph |
CN110494747B (en) * | 2017-04-26 | 2021-12-28 | 株式会社岛津制作所 | Liquid feeding device and fluid chromatograph |
Also Published As
Publication number | Publication date |
---|---|
JPS6245982A (en) | 1987-02-27 |
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