CN1014549B - Liquid chromatography - Google Patents
Liquid chromatographyInfo
- Publication number
- CN1014549B CN1014549B CN 85101215 CN85101215A CN1014549B CN 1014549 B CN1014549 B CN 1014549B CN 85101215 CN85101215 CN 85101215 CN 85101215 A CN85101215 A CN 85101215A CN 1014549 B CN1014549 B CN 1014549B
- Authority
- CN
- China
- Prior art keywords
- liquid
- suction
- bubble
- piston pump
- bubble detection
- 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
Links
Images
Landscapes
- Control Of Positive-Displacement Pumps (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention relates to a liquid phase chromatograph. A flow path switching device is arranged in a liquid flow supply path of at the suction side of a fluid feeding pump; an air bubble detection device is arranged at one side of the flow path switching device corresponding to a piston pump; a component of the liquid flow supply path from the air bubble detection device to the flow path switching device is greater than the single suction volume of the piston pump; the flow path switching device is connected to a suction/ ejection device which sucks and ejects a liquid flow with gas bubbles; the flow path switching device make switching movement according to an air bubble detection signal output from the air bubble detection device so as to be connected with the suction/ ejection device. The present invention is also provided with a device which enables the suction/ ejection device to make suction movement and ejection movement.
Description
The invention relates to high speed liquid chromatograph, more particularly is to remove device about the bubble of high speed liquid chromatograph.
Generalized case in the various liquid streams that use, often is dissolved with air in the high-speed liquid chromatography instrument.Therefore, when using the high-speed liquid chromatography instrument, owing to the variation of its environment temperature, the variation (decompression) of pressure etc., the air of dissolving often forms bubble, and results from the liquid stream supply road.Particularly, the suction strainer of the suction side of the liquid-feeding pump (piston pump) of conveying liquid stream usefulness, if because of dust dirty owing to increased the suction resistance of liquid-feeding pump, so, when liquid-feeding pump sucks solvent, the exhaust end of suction passage at it is easy to generate bubble, and when exchange liquid stream, the bubble in the filtrator is difficult to take out, so just exist under the situation of long-time interruption the problem that this bubble is overflowed.In addition, for example, switch several liquid streams to analyze in the situation that will carry out that amino acid analysis, test portion concentrate etc., suction side at liquid-feeding pump, owing to be provided with flow channel switching valve door, in-line filter etc., the flow path resistance that makes liquid stream supply with the road becomes big, therefore is easy to generate bubble equally.
As the countermeasure of above problem, degasification fully before using liquid stream, and the depassing unit of in liquid chromatograph, packing into, liquid stream is supplied with the road.For example, constitute with polyfluortetraethylene pipe, and make this pipe around be in decompression state with degasification.
But,, remove troublesome poeration with above-mentioned known degasification method, in addition, aspect the package assembly of above-mentioned depassing unit, it is elongated that the liquid of liquid-feeding pump suction side stream is supplied with the road, that is to say that fixed volume becomes big, the cost of high-speed liquid chromatography instrument uprises, and this is inappropriate.
In view of above situation, one of fundamental purpose of the present invention is to absorb on the liquid stream supply road of side at liquid-feeding pump, and the bubble detection device is set.Do not increase fixed volume,, in liquid-feeding pump, just can prevent the inflow of bubble with the structure of cheapness.
The invention relates to a kind of liquid chromatograph, it has by it supplies with the road to the separating column conveying device, at the couple positioned opposite bubble detection device of this flow passage selector device and ram pump, form the big situation of volume ratio piston pump soakage once on liquid stream supply road from this bubble detection device to flow passage selector device; And suction, the device for discharging fixed of the liquid stream that has bubble of connect sucking on flow passage selector device, spue according to the bubble detection signal from the output of bubble detection device, make flow passage selector device do that change action sucks to connect, device for discharging fixed; After connecting like this, setting makes the suction device for discharging fixed do to inhale and tells the control device of action.
Embodiment according to representing in figure below is described in detail the present invention.Yet this invention is not limited by this.
The 1st figure represents the one-piece construction of high speed liquid chromatograph (1).
(2) (2) etc. are liquid stream A～F, these liquid streams, by supplying with road (3), with piston pump (4) to pressure transducer (5), tamping (6), nozzle (7), column jecket (8) and detector (9) force feed.In addition, aforementioned various liquid flows (2) (2).Remove their dirt with inhaling filtrator (10), simultaneously, the liquid transition that is fit to is arrived the supply road with 7 hole liquid flowing conversion valve doors (27).On the other hand, do to suck, disgorging motion by discoideus cam (11) and piston pump motor (12) by being roughly for piston pump (4).Its suction, disgorging motion are installed in the optical sensor (13) on the cam (11) and the control of the piston position watch-dog (14) that moves according to the signal of this sensor output.
Supply with on the road (3) at the stream of the liquid between piston pump (4) and the liquid flowing conversion valve door (27), be provided with 3 three-way electromagnetic valve A(15 as flow path converter), simultaneously, bubble is set and detects part (16) between this 3 three-way electromagnetic valve A and liquid flowing conversion valve door (27).From 3 three-way electromagnetic valve door A(15) 1 exhausr port (d), to suck, be connected with absorption between the syringe (17) of device for discharging fixed, the road that spues (18).In the middle of this absorption, the road that spues, also be provided with 3 three-way electromagnetic valve B(19), its exhausr port (9) connects discharge opeing road (20).(21) be to make syringe make the injector motor of suction, disgorging motion.
The 2nd figure is the enlarged drawing that aforementioned bubble detects part (16).Bubble detects part (16) and 3 three-way electromagnetic valve A(15) between the capacity on liquid stream supply road (3), soakage than a stroke of piston pump (4) is big a little, and the light signal that is provided with light emitting diode (22) on its outer wall next door and accepts this light emitting diode is as the phototriode of exporting.
(24) be the control section that sends control signal according to the signal of this phototriode output.This control section (24) makes piston pump motor (12) and injector motor (21) stop and starting respectively by its control signal, along with above-mentioned action, makes 3 three-way electromagnetic valve B(19) make switching motion.In addition, 3 three-way electromagnetic valve A(15) switching motion is that the signal according to piston position control device (14) output carries out, and when piston pump (4) when sucking, liquid stream is supplied with road (3) and is connected to 3 three-way electromagnetic valve A(15) b and c hole.
Below, the course of work of above-mentioned liquid chromatograph (1) is done an explanation.
The 3rd figure is that dotted line is represented critical value from the electric current coordinate figure of phototriode output.The 4th figure be piston pump (4) suction, oscillogram spues.Below to bubble detect the part (16) outlet a, the entrance side retaining valve e of piston pump (4) and 3 three-way electromagnetic valve B(19) all the other 2 hole f, h explain.
Liquid stream between a～b～c～e is supplied with on the road (3) not to be had in the bubble (25), if piston pump (4) is made suction action, then a～b alternately flows into from the liquid stream (2) that bubble detects part (16) outflow.Secondly, in this liquid stream, if there is a bubble to enter, when detecting part (16) by bubble, the output current of the phototriode on the 3rd figure (23), just the output current i when bubble detects
1Become i
2If t to the 4th figure
1, 3 three-way electromagnetic valve A(15) just be transformed into b～d.Simultaneously, 3 three-way electromagnetic valve B(19) also make conducting between f～h according to the control signal of coming by control section (24), simultaneously, and injector motor (21) action, syringe (17) is made suction action, once sucks the whole liquid streams that have bubble between a～b～d.And, if detected bubble, then keep above-mentioned state, make syringe (17) make suction action, the bubble between a～b (25) is removed.Therefore, if syringe (17) is in the suction process, bubble is not detected, 3 three-way electromagnetic valve B(19) also conducting g and h exhausr port, simultaneously, injector motor (21) is made disgorging motion, the liquid stream (2) in the exhaustjet device (17).In addition, be the occasion of a kind at liquid stream (2), make 3 three-way electromagnetic valve B(19) outlet (g) return, liquid (2) flow liquid body container (26) then, thus save liquid (2).During the above bubble removal, be the t of the 4th figure
1～t
2Time (△ t).Also have, as piston pump will with quantitatively spue, high speed induction type piston pump, for example, if its discharge flow is decided to be daily use traffic about 1ml/min, so aforementioned △ t just became about 6 seconds, the capacity V of syringe (17)
cIf the capacity V of piston pump (4)
e100 times just enough.Here, if V
eBe 100 μ l, V so
cJust become 10ml.
As, more than the high speed liquid chromatograph of Gou Chenging (1) can increase following effect:
(a) supply with bubble among a～b on road (3) owing to remove liquid stream with syringe (17), fixed volume needn't be very big, then with cheap construction, just can prevent from that liquid at the exhaust end of piston pump from flowing in the supply road (3) to enter bubble.
(b) peripheral hardware not in liquid stream is supplied with road (3), three-way solenoid valve A(15), and as preceding paragraph (a), owing to fixed volume is little, the conversion of liquid (2) is simple.
(c), in the step method as amino acid analysis etc., there is not bubble to enter piston pump (4), just exchanging liquid promptly for preceding paragraph (b).
For other embodiment, above bubble removal structure, when the preparation water of piston pump in the occasion of carrying out automatically, also can utilize.For example, at the 1st figure, from each liquid container (26) (26) ... have only under the situation of air in the liquid stream supply road (3) of retaining valve (e), piston pump (4) can not suck liquid to rely on oneself.Therefore b, 3 three-way electromagnetic valve A(15) and d exhausr port are connected, and make liquid flowing conversion valve (27) work order change action.When its change action passes through a week, each liquid is flowed (2) (2) with syringe (17) ... be drawn into the b position, because its capacity is little, piston pump (4) can attract to come the liquid (2) of b position between c～e.In addition, this method also can be used in the occasion that each liquid exchanges rapidly.
According to the present invention, in the stream of the liquid between flow passage selector device that is in the piston pump suction side and the bubble detection device, when entering bubble, owing to this liquid stream is drawn into outside the liquor charging road with suction, device for discharging fixed, can not increase the liquid supply road length that piston pump absorbs side, thereby, can prevent from the liquid stream supply road of piston pump exhaust end, to enter bubble with cheap and simple structure.And even in the occasion of using multiple liquid, the exchange of these liquid also can promptly be carried out.
What the 1st figure represented is the structure key diagram of an embodiment of high speed liquid chromatograph of the present invention, and the 2nd figure is the summary pie graph of this bubble detection device, and the 3rd figure is the output current mode chart of this phototriode.The 4th figure be this piston pump suction, the waveform key diagram spues.
(1) ... liquid chromatograph,
(2) ... liquid,
(3) liquid stream is supplied with the road,
(4) ... piston pump,
(15) ... 3 three-way electromagnetic valve A flow passage selector devices,
(16) ... the bubble detection device,
(17) ... syringe input, device for discharging fixed,
(22) ... light emitting diode,
(23) ... phototriode.
Claims (3)
1, a kind of liquid chromatograph comprises liquid supply road, separating column, detecting device and passes through to supply with the piston pump of road to separating column conveying liquid, and it also comprises:
Liquid stream in the suction side of liquid-feeding pump is supplied with on the road, and flow passage selector device is set,
Relative side at this flow passage selector device and piston pump is provided with photoelectricity bubble detection device, forms the big situation of single intake of the volume ratio piston pump on the liquid stream supply road from this photoelectricity bubble detection device to flow passage selector device,
On flow passage selector device, connect to suck, spue suction, the device for discharging fixed of the liquid stream that has bubble,
Bubble detection signal according to from the output of photoelectricity bubble detection device makes flow passage selector device do change action, with connection suction, device for discharging fixed,
After connecting like this, be provided with again and make suction, the suction of device for discharging fixed do, tell the device of action.
2, liquid chromatograph according to claim 1, its liquid stream is supplied with the route polyfluortetraethylene pipe and is constituted.
3, liquid chromatograph according to claim 1 and 2, its photoelectricity bubble detection device is made of light emitting diode that is provided with by polyfluortetraethylene pipe and phototriode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85101215 CN1014549B (en) | 1985-04-01 | 1985-04-01 | Liquid chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85101215 CN1014549B (en) | 1985-04-01 | 1985-04-01 | Liquid chromatography |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85101215A CN85101215A (en) | 1987-01-24 |
| CN1014549B true CN1014549B (en) | 1991-10-30 |
Family
ID=4791693
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85101215 Expired CN1014549B (en) | 1985-04-01 | 1985-04-01 | Liquid chromatography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1014549B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100399021C (en) * | 2004-01-30 | 2008-07-02 | 株式会社岛津制作所 | Liquid chromatograph |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10107273B2 (en) * | 2008-08-07 | 2018-10-23 | Agilent Technologies, Inc. | Synchronization of supply flow paths |
| WO2010124741A1 (en) * | 2009-04-30 | 2010-11-04 | Agilent Technologies, Inc. | Determining fluid compressibility while delivering fluid |
| CN105606720B (en) * | 2015-11-20 | 2018-06-26 | 国网山东青州市供电公司 | The sample preparation of electric power gas-chromatography is vented instrument |
| JP7040392B2 (en) * | 2018-10-03 | 2022-03-23 | 株式会社島津製作所 | How to adjust the sample injection device and sample injection device |
| EP3748354B1 (en) * | 2019-06-04 | 2022-04-06 | F. Hoffmann-La Roche AG | Quick liquid exchange in liquid chromatography |
| KR102410793B1 (en) * | 2021-11-10 | 2022-06-22 | 주식회사 위드텍 | Apparatus and method for sampling luquid |
-
1985
- 1985-04-01 CN CN 85101215 patent/CN1014549B/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100399021C (en) * | 2004-01-30 | 2008-07-02 | 株式会社岛津制作所 | Liquid chromatograph |
Also Published As
| Publication number | Publication date |
|---|---|
| CN85101215A (en) | 1987-01-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104690047B (en) | A kind of liquid chromatograph sample intake passage cleans device | |
| US7862716B2 (en) | HPLC schematic with integrated sample cleaning system | |
| JP5111476B2 (en) | Liquid sample analyzer and liquid sample introduction device | |
| CN1014549B (en) | Liquid chromatography | |
| CN200989905Y (en) | Liquid path system for full automatic biochemical analyzer | |
| US4310420A (en) | Mobile phase supplying method in the liquid chromatography and apparatus therefor | |
| DE69914604T2 (en) | METHOD FOR MONITORING A RECORDING AND DELIVERY SYSTEM | |
| CA1326696C (en) | Apparatus and method for the separation and/or formation of immiscible liquid streams | |
| US20080229809A1 (en) | Sample Injection Device, Sample Injection Method, and Liquid Chromatograph | |
| GB2338433A (en) | Liquid Chromatograph | |
| CN1648657A (en) | Liquid chromatograph | |
| EP1843153B1 (en) | Sample injector, sample injecting method and liquid chromatography device | |
| CN104914031A (en) | Flow cytometry fluid path system and flow cytometry method | |
| EP2990791B1 (en) | Switching valve for a flow-type analysis device | |
| KR101686455B1 (en) | Sample injection device, sample injection method, and liquid chromatography device | |
| CN1898617A (en) | Liquid dispensing and recirculating system with sensor | |
| CN205209962U (en) | STREAMING fluorescence detector's liquid way system | |
| CN106701556A (en) | Digital PCR (Polymerase Chain Reaction) detection device and liquid path system thereof | |
| JP2006317331A (en) | Determination device and method of clogging state in tube | |
| CN201965136U (en) | Flow path system for automation biochemical reaction flow | |
| CN2511399Y (en) | Cleaning device for spray | |
| EP1154270B1 (en) | Glycated hemoglobin analyzer | |
| JPS62113066A (en) | Sample introducing device for non-segment type continuous flow analysis | |
| CN208450119U (en) | A kind of cleaning device safely and fast cleaning rubber tube inner wall | |
| KR101863697B1 (en) | The flow regulator valve for collecting tubes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C13 | Decision | ||
| GR02 | Examined patent application | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |