CN1003396B - Liquid chromatograph - Google Patents
Liquid chromatograph Download PDFInfo
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- CN1003396B CN1003396B CN85101476.3A CN85101476A CN1003396B CN 1003396 B CN1003396 B CN 1003396B CN 85101476 A CN85101476 A CN 85101476A CN 1003396 B CN1003396 B CN 1003396B
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- discharge opeing
- pump
- signal
- plunger
- pressure
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- Control Of Positive-Displacement Pumps (AREA)
- Reciprocating Pumps (AREA)
Abstract
The present invention relates to a liquid chromatograph capable of avoiding liquid flow pulsation without a buffer, which is provided with a plunger pump and a control part of the plunger pump, wherein the plunger pump is formed by respectively connecting liquid draining ends and liquid pumping ends of a main pump and an auxiliary pump which have the same structure; the control part of the plunger pump comprises a pressure detecting device, a liquid drainage displacement detecting device of a plunger of the main pump, a storage device for storing output signals of the two devices and a speed control device, and a liquid drainage displacement signal is compared with the set value so that a compression drive signal or a control signal of liquid drainage speed are emitted to the auxiliary pump.
Description
This is the invention about chromatographic analyzer of liquid phase, in detail, is the invention about the structure that prevents liquid stream conveying pulsation in the high-speed liquid phase chromatogram analysis instrument.
Usually, the liquid stream discharge pump in the high-speed liquid phase chromatogram analysis instrument mainly adopts small-sized plunger reciprocating pump, and it is this pump most important character for a short time that its stability of flow, particularly liquid stream are carried pulsation.
Therefore, all be to dispose a plurality of above-mentioned small-sized plunger pumps simultaneously in the past, when liquid stream is carried, make its discharge opeing shift position lapping and drive each plunger, and no matter still use single plunger pump with said pump, all to monitor,, prevent to change the variation that causes pump discharge opeing pressure because of compressibility with the discharge opeing translational speed of monitored results FEEDBACK CONTROL plunger to the discharge opeing pressure of pump.Pulsation when reducing the conveying of liquid stream.
Yet, this structure is used for high sensitivity detector, for example, be used to pulse responsive differential refractometer detecting device, electrochemical detector and when analyzing, because the velocity of plunger tracing property that pulsation is revised is good inadequately, need on the liquid stream supply road of plunger discharge opeing side, to add bigger impact damper, stop fluid pulse, but still can not prevent pulsation fully.And because impact damper is bigger, the dead zone of liquid stream is also big, and practicality is bad.
In view of the foregoing, a fundamental purpose of the present invention is not adopt impact damper, and with two ram pumps, the dead zone is diminished, and reaches pulse free ground and carries out the conveying of liquid stream.
By carrying in the ram pump of mobile liquid and the chromatographic analyzer of liquid phase that this pump operation control part is formed along supplying with the road direction separating column, ram pump is by main pump and auxiliary pump with spline structure, and their two drain sides and two liquid pumping sides are formed by connecting respectively, the plunger of main pump is about to move the beginning a certain moment of back with discharge opeing before the termination except that moving in discharge opeing, all be to move do discharge opeing by predefined speed, in addition, it is also made the high speed drawing liquid and moves to be higher than this discharge opeing translational speed.The operation control part of ram pump has: the pressure-detecting device of two pump discharge opeing sides; Detect the position detecting device of main pump plunger discharge opeing shift position; When the main pump plunger moves do discharge opeing with the speed of setting, to the storage facility of storing respectively from the output signal of discharge opeing detector for movable position and pressure-detecting device; When discharge opeing shift position detection signal is consistent with the discharge opeing shift position storage signal of setting, drive signal to auxiliary pump output preparation compression usefulness, simultaneously, the discharge opeing movement pressure of pressure detecting signal and setting is stored signal to be compared, when storage signal in the discharge opeing shift position of discharge opeing shift position detection signal and setting is inconsistent, for making their consistent speed control units to auxiliary pump output discharge opeing translational speed control signal.
Elaborate with the embodiment shown in scheming, certainly, this invention is not limited only to this example.
In 1-4 figure, high speed Liquid Chromatograph (1) mainly carries the ram pump (5) of liquid stream (3), the drive division (6) and the operation control part (7) of this ram pump to constitute by supply with road (4) by liquid stream to separating column (2).(8) be thrower, (9) are detecting devices.
Ram pump (5) is made of main pump (10) and auxiliary pump (11), and the discharge opeing side of two pumps and drawing liquid side all are connected with retaining valve (12) (12) ...
Above-mentioned drive division (6) is made the step motor A and the B(17 of the distortion cam rotation of the same spline structure that moves back and forth separately by the plunger (13) that makes above-mentioned two pumps (10) (11) (14 in the drawings omit)) (18) constitute.One (15) in the distortion cam (15) (16) are shown in the 2nd figure, are approximately circular plate type.Corresponding to central angle 270(Q
1) the outer make the plunger (13) (14) of each pump do reciprocating action by given speed, and at remaining 90(Q
2) between then do high speed drawing liquid action.(10) be volute spring.Main pump plunger (13) except its discharge opeing move be about to stop before or its discharge opeing move incipient in a flash, all by predefined speed (Va moves do discharge opeing, liquid stream supply with in the road (4) make when flow setting signal by the flow setting circuit (20) of setting flow (V) (referring to the 4th figure) liquor charging and circuit output in view of the above moves plunger (13) with the motor drive circuit (21) that moves of high speed drawing liquid greater than above-mentioned setting speed (Va) all with the step motor A(17 of main pump (10)) be electrically connected.
Above-mentioned operation control part (7) has pressure transducer (22) that detects liquid stream (3) liquor charging pressure and the pick-up unit (23) (24) that detects two pump plungers (13) (14) discharge opeing shift position.This pressure transducer (22) is contained in the liquid stream of two pumps (10) (11) discharge opeing side and supplies with in the road (4), and discharge opeing detector for movable position (23) (24) is to finish by being fixed on the photoelectric sensor that respectively is out of shape cam (15) (16) outer.(the t of the 3rd figure when operation control part (7) also has the plunger (13) in main pump (10) to move with the drain age velocity of setting
1Constantly) to the storing apparatus (25) stored respectively from the output signal of photoelectric sensor (23) and pressure transducer (22) and by step motor B(18) and in the time of auxiliary pump (11) output drive signal, as the level pressure power driving circuit (26) of the speed control unit of output discharge opeing translational speed control signal.
Above-mentioned memory storage (25) is made of plunger position watch-dog (27) and pressure storage circuitry (28), and plunger position watch-dog and level pressure power driving circuit (26), motor drive circuit (21) and pressure storage circuitry (28) are electrically connected.
Action to high-speed liquid phase chromatogram analysis instrument (1) is illustrated below.
At first, according to flow setting signal from liquid stream initialization circuit (20), shown in the 3rd figure, the discharge opeing translational speed Va efflux flow (3) of main pump (10) to set.So the plunger (13) in main pump (10) arrives the t before termination is soon moved in discharge opeing
1Constantly,, drive step motor B(17 by level pressure power driving circuit (26) output drive signal), and, the stream of the liquid in the pump head of auxiliary pump (11) (3) is done the preparation compression along discharge opeing direction mobile plunger (14).To t
2-t
3Curve constantly shown in the 3rd figure, the drain age velocity of main pump (10) reduces, when the discharge opeing movement pressure of the pressure detecting signal of pressure transducer (22) and setting is stored signal when inconsistent, then to step motor B(18) export discharge opeing translational speed control signal from level pressure driving circuit (26), make pressure detecting signal at this moment consistent with setting movement pressure storage signal.Main pump (10) stops the discharge opeing action then, in case with t
3-t
4Speed V constantly
1In 0.2 second, carry out the action of high speed drawing liquid, then the discharge opeing translational speed (V of the plunger (14) of auxiliary pump (11)
2) increase gradually, with aforesaid t
2The same constantly, make pressure signal at this moment consistent with aforesaid storage signal.So at t
4-t
5Between, main pump (10) is only with the stream of the liquid in proportional its pump head of amount precompression of pressure therewith.When arriving tt
5Constantly, the retaining valve (12) of main pump (10) outlet side is open, by main pump (10) efflux flow (3).When the draining flow from main pump (10) increases gradually, send speed control signal by plunger position watch-dog (27), make the discharge opeing translational speed of auxiliary pump plunger (14) resemble reduction the curve of the 3rd figure.At this moment, because the discharge opeing of main pump (10) claims speed littler than Va, at t
6Constantly do not produce pulsation.Then, along with the raising of main pump (10) plunger (13) discharge opeing translational speed, the discharge opeing translational speed of auxiliary pump (11) plunger reduces gradually.t
7After, only carry liquid stream (3) by main pump (10).And step motor B(18) at t
7-t
8Between stop to be driven, at t
8-t
9Between then with t
1-t
7Between make inversion driving on the contrary, aspirated liquid stream (3) is (referring to the 3rd figure V
3).
The 4th figure is the lifting rate curve of two pumps (10) (11).1 stroke lifting rate of main pump (10) is 100 μ l, on the other hand, because the suction time of main pump (10) as previously mentioned, shorter, if setting draining flow is the 1ml/ timesharing, 1 stroke lifting rate of auxiliary pump (11) is (referring to the oblique line part of the 4th figure) about 4 μ l.
Like this, main pump (10) and auxiliary pump move (11), supply with at liquid stream and carry liquid stream (3) in the road (4).
High-speed liquid phase chromatogram analysis instrument (1) structure with above-mentioned can obtain following result.
(a) because the increase of the discharge opeing translational speed of auxiliary pump (11) plunger and reduce and all compare slowly, to revise the speed Tracking that is acted on better for the plunger pulsation, so the pulsation can prevent that main pump (10) and auxiliary pump (11) from replacing the time.
(b) because (a) item is arranged, promptly use the responsive detecting device of pulsation, also can be without impact damper, the dead zone is little, and not influenced by baseline noise, can detect test portion in high sensitivity.
(c),, can automatically be revised the compressibility of liquid stream with the kind and the liquor charging pressure independent thereof of liquid stream because the stream of the liquid before and after main pump (10) high speed suction action discharge pressure is revised with auxiliary pump (11).
(d) in 2 pump pressure steepness are analyzed, during the pressure gradient liquor charging of micrometeor scope, do not supply with dead zone in the road and bring influence compressibility because of liquid stream, or the fluctuations in discharge that causes because of pulsation, so can carry out the pressure gradient analysis accurately.
As other the embodiment main pump and auxiliary pump on 2 secondary above-mentioned pressure transducers are installed simultaneously, connect their pressure transducer outlets separately, supply with the Lu Zhongshe mixer at the liquid stream of its outlet side, and can constitute the pressure gradient device of 2 pumps.At this moment, adopt above-mentioned operation control part, when pressure gradient is analyzed, also can revise the automatic compressibility of liquid stream, and, irrelevant with the variation of the discharge opeing pressure of setting, can make the melting concn of liquid stream keep certain.And because not pulsation also can obtain melting concn no change, stable in the tiny flow quantity scope.
(6) effect
Ram pump among the present invention is made up of main pump and auxiliary pump, for soon lifting rate after preventing to begin to discharge opeing before main pump from be about to stopping from discharge opeing reduces, and allow auxiliary pump carry out the discharge opeing action, do not need impact damper, less dead zone can be arranged, liquid stream is carried on pulse free ground, even thereby adopt the responsive detecting devices of pulsation such as differential refractometer detecting device, electrochemical detector, also can detect test portion with sensitivity.
The 1st figure belongs to high speed liquid chromatograph example structure key diagram of the present invention, the 2nd figure is a key diagram of showing distortion cam action state, the 3rd figure is the velocity diagram of main pump and auxiliary pump discharge opeing drawing liquid length velocity relation, and the 4th figure is the discharge opeing spirogram of main pump and auxiliary pump 1 stroke.
(1) ... the high-speed liquid phase chromatogram analysis instrument,
(2) ... separating column, (3) ... liquid stream, (4) ... liquid stream is supplied with the road,
(5) ... ram pump, (7) ... motion control device, (10) ... main pump,
(11) ... auxiliary pump,
(13) (14) ... plunger, (22) ... pressure sensor,
(23) ... discharge opeing shift position detecting device,
(25) ... storing apparatus, (26) level pressure power driving circuit (speed control unit)
(Va) ... set the discharge opeing translational speed, (V
1) ... high speed drawing liquid translational speed.
Claims (1)
1, a kind of chromatographic analyzer of liquid phase of forming by pump, separating column and detecting device, it is characterized in that described ram pump is to make main pump and auxiliary pump, and their two drain sides and two liquid pumping sides are formed by connecting respectively, the plunger of main pump all is to do the discharge opeing action by predefined speed except that before the discharge opeing action will soon stop and certain moment after the discharge opeing action beginning.The operation control part of ram pump has: the pressure-detecting device of two pump discharge opeing sides; Detect the position detecting device of main pump plunger discharge opeing shift position; When the main pump plunger moves do discharge opeing with the speed of setting, to the storing apparatus that stores respectively from the output signal of discharge opeing detector for movable position and pressure-detecting device; When discharge opeing shift position detection signal is consistent with the discharge opeing shift position storage signal of setting, drive signal to auxiliary pump output preparation compression usefulness, discharge opeing movement pressure storage signal with pressure detecting signal and setting is compared simultaneously, when storage signal in the discharge opeing shift position of discharge opeing shift position detection signal and setting is inconsistent, for making their consistent speed control units to auxiliary pump output discharge opeing translational speed control signal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85101476.3A CN1003396B (en) | 1985-04-01 | 1985-04-01 | Liquid chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85101476.3A CN1003396B (en) | 1985-04-01 | 1985-04-01 | Liquid chromatograph |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85101476A CN85101476A (en) | 1987-01-24 |
| CN1003396B true CN1003396B (en) | 1989-02-22 |
Family
ID=4791859
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85101476.3A Expired CN1003396B (en) | 1985-04-01 | 1985-04-01 | Liquid chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1003396B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5624825B2 (en) * | 2010-07-29 | 2014-11-12 | 株式会社日立ハイテクノロジーズ | Liquid chromatograph pump and liquid chromatograph |
| CN110809713B (en) * | 2017-10-23 | 2022-06-21 | 株式会社岛津制作所 | Liquid feeding device and fluid chromatograph |
-
1985
- 1985-04-01 CN CN85101476.3A patent/CN1003396B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN85101476A (en) | 1987-01-24 |
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