CN114910215A - Liquid transfer device and calibration method for liquid chromatograph - Google Patents
Liquid transfer device and calibration method for liquid chromatograph Download PDFInfo
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- CN114910215A CN114910215A CN202210551677.9A CN202210551677A CN114910215A CN 114910215 A CN114910215 A CN 114910215A CN 202210551677 A CN202210551677 A CN 202210551677A CN 114910215 A CN114910215 A CN 114910215A
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- plunger pump
- liquid
- pressure sensor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L27/00—Testing or calibrating of apparatus for measuring fluid pressure
- G01L27/002—Calibrating, i.e. establishing true relation between transducer output value and value to be measured, zeroing, linearising or span error determination
- G01L27/005—Apparatus for calibrating pressure sensors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
Abstract
The invention provides a liquid conveying device and a correction method of a liquid chromatograph, wherein the correction method of the liquid conveying device comprises the following steps: when the second plunger pump conveys liquid outwards, the first plunger pump sucks the liquid, and a first one-way valve between the first plunger pump and the second plunger pump is in a closed state; the first plunger pump pre-compresses the sucked liquid, when the variation of the first parameter of the second pressure sensor at the downstream of the output end of the second plunger pump or the variation of the second parameter exceeds a first threshold value, the first one-way valve is in a communication state, the first plunger pump stops pre-compression, and the first parameter of the second pressure sensor at the moment is recorded V1 And a first parameter of a first pressure sensor between the first plunger pump and the second plunger pump V2 ′ (ii) a Using a first parameter V1 And V2 ′ slope of response to the first pressure sensor K1 And/or the slope of the response of the second pressure sensor K2 And carrying out normalization correction. The invention has the advantages of automation, stable liquid delivery and the like.
Description
Technical Field
The present invention relates to calibration of a pressure sensor, and more particularly to a liquid transfer device and a calibration method for a liquid chromatograph.
Background
In a liquid chromatograph system, a pump assembly is matched with an inlet one-way valve and an outlet one-way valve to suck normal-pressure liquid, then the normal-pressure liquid is compressed and boosted, and then the normal-pressure liquid is conveyed to the downstream direction according to a certain flow rate and pressure. In order to solve the 'suction-discharge' periodic limitation of a single-group reciprocating plunger pump applied to a liquid chromatography pump, two groups of pumps are generally adopted in series or parallel connection in practical application, and the limitation is overcome by cooperatively controlling, alternately and complementarily between the two groups of pumps, so that constant-current output is realized.
In order to ensure that the switching coordination between two groups of pumps adopting a serial or parallel mode is smoother, a pressure sensor is often arranged in each group of pump flow paths, the sucked normal-pressure liquid is pre-compressed in advance through the feedback of the pressure sensor, and the pressure is increased to the same pressure of the other group of pumps conveying the liquid downstream. The uniformity of the performance of the pressure sensors distributed in the flow paths of the two sets of pumps directly affects the synergistic cooperation effect of the two sets of pumps.
The existing technical scheme is that in the production stage of products, the zero point and the slope of the response of two pressure sensors are adjusted to be consistent in advance on a tool, then the two pressure sensors are installed in a liquid chromatograph system for use, and in the continuous work of the liquid chromatograph, the time of communicating the atmospheric pressure in the liquid pumping stage is utilized to correct the zero point drift of the pressure sensors, but the slope drift of the pressure sensors cannot be effectively corrected. Therefore, the pressure sensor is required to have a very high slope anti-drift characteristic. However, there is a problem that the slope drift of the pressure sensor cannot be corrected automatically, and the performance of the liquid chromatography pump is degraded.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a correction method of a liquid conveying device.
The purpose of the invention is realized by the following technical scheme:
the correction method of the liquid conveying device comprises the following steps:
when the second plunger pump conveys liquid outwards, the first plunger pump sucks the liquid, and a first one-way valve between the first plunger pump and the second plunger pump is in a closed state;
the first plunger pump pre-compresses the sucked liquid, when the variation of the first parameter of the second pressure sensor at the downstream of the output end of the second plunger pump or the variation of the second parameter exceeds a first threshold value, the first one-way valve is in a communication state, the first plunger pump stops pre-compression, and the first parameter V of the second pressure sensor at the moment is recorded 1 And a first parameter V 'of a first pressure sensor between the first and second plunger pumps' 2 ;
Using a first parameter V 1 And V' 2 Slope K of response to the first pressure sensor 1 And the response slope K of the second pressure sensor 2 And carrying out normalization correction.
The invention also aims to provide a correction method of the liquid chromatograph, and the invention aims to be realized by the following technical scheme:
a calibration method for a liquid chromatograph including the calibration method for a liquid transport apparatus of the present invention, the liquid chromatograph including the liquid transport apparatus.
Compared with the prior art, the invention has the beneficial effects that:
1. automatic correction;
the slope drift of the pressure sensor is corrected automatically and in real time, the slope drift resistance of the pressure sensor of a liquid conveying device (a liquid chromatography system) is effectively improved, and the stability of liquid conveying is further ensured;
2. the requirements on the device are reduced;
by utilizing the automatic correction of the invention, the requirements of the liquid conveying device (liquid chromatography system) on the stability and consistency of the pressure sensor are reduced, and the production and manufacturing cost is greatly reduced.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solution of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic illustration of a calibration method for a liquid delivery device according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a liquid delivery device according to an embodiment of the present invention.
Detailed Description
Fig. 1-2 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 schematically shows a calibration method of a liquid transport apparatus according to an embodiment of the present invention, and as shown in fig. 1, the calibration method of the liquid transport apparatus includes:
when the second plunger pump conveys liquid outwards, the first plunger pump sucks in the liquid, and a first one-way valve between the first plunger pump and the second plunger pump is in a closed state, as shown in fig. 2;
the first plunger pump pre-compresses the sucked liquid, when the variation of the first parameter of the second pressure sensor at the downstream of the output end of the second plunger pump or the variation of the second parameter exceeds a first threshold value, the first one-way valve is in a communication state, the first plunger pump stops pre-compression, and the first parameter V of the second pressure sensor at the moment is recorded 1 And a first parameter V 'of a first pressure sensor between the first and second plunger pumps' 2 ;
Using a first parameter V 1 And V' 2 Slope K of response to the first pressure sensor 1 And/or the response slope K of the second pressure sensor 2 And carrying out normalization correction.
In order to accurately correct the pressure sensor, further, the first parameter V is judged 1 And V' 2 Whether the difference is greater than a second threshold;
if the difference is greater than a second threshold, the response slope K is adjusted 1 And the response slope K 2 And carrying out normalization correction.
If the difference P is greater than the second threshold value, so as toSlope K of response to the first pressure sensor 1 And the response slope K of the second pressure sensor 2 And carrying out normalization correction.
Example 2:
an application example of the correction method of the liquid transport apparatus according to embodiment 1 of the present invention to the correction of a liquid chromatograph.
In this application example, the calibration method of the liquid chromatograph includes a calibration method of a liquid transport apparatus, the liquid chromatograph includes the liquid transport apparatus, and the calibration method of the liquid transport apparatus is:
in the stage of stable constant-current downstream infusion of the second reciprocating plunger pump, the first reciprocating plunger pump quickly sucks liquid at atmospheric pressure from the input end of the first one-way valve, and the second one-way valve between the first reciprocating plunger pump and the second reciprocating plunger pump is in a closed state at the moment;
the first reciprocating plunger pump pre-compresses the sucked liquid until the response value (namely the first parameter) of a second pressure sensor arranged at the downstream of the second reciprocating plunger pump deviates from a stable value and exceeds a set first threshold value by 50psi, namely the variation of the first parameter is more than 50psi, at the moment, the second one-way valve is in a communication state, the pre-compression of the first reciprocating plunger pump is stopped, and the response value V of the first pressure sensor between the first plunger pump and the second plunger pump is synchronously recorded 1 And a second pressure sensor response value V' 2 (ii) a The first reciprocating plunger pump, the first pressure sensor, the second one-way valve and the second reciprocating plunger pump are arranged in sequence;
judging a first parameter V 1 And V' 2 Difference of (2)Whether greater than a second threshold, such as 0.001;
if the difference is greater than a second threshold value, so as toSlope K of response to the first pressure sensor 1 And the response slope K of the second pressure sensor 2 And carrying out normalization correction.
After the correction is completed, the first reciprocating plunger pump directly performs pre-compression closed-loop control according to the response of the first pressure sensor in subsequent continuous work until the correction method is started again when the response fluctuation of the second pressure sensor exceeds 40psi during normal cooperative alternating operation of the first reciprocating plunger pump and the second reciprocating plunger pump.
Example 3:
an application example of the correction method of the liquid transport apparatus according to embodiment 1 of the present invention to the correction of a liquid chromatograph.
In this application example, the calibration method of the liquid chromatograph includes a calibration method of a liquid transport apparatus, the liquid chromatograph includes the liquid transport apparatus, and the calibration method of the liquid transport apparatus is:
in the stage of the downstream infusion of the second reciprocating plunger pump in a uniform acceleration and stabilization mode, the first reciprocating plunger pump quickly sucks liquid at the atmospheric pressure from the input end of the first one-way valve, and the second one-way valve between the first reciprocating plunger pump and the second reciprocating plunger pump is in a closed state;
the first reciprocating plunger pump precompresses the liquid drawn in until the response slope of a second pressure sensor (i.e., a second parameter) disposed downstream of the second reciprocating plunger pumpNumber) deviates from a stable value by an amount exceeding a set first threshold value of 0.02K 2 And the second check valve is in a communication state at this time, the pre-compression of the first reciprocating plunger pump is stopped, and the response value V of the first pressure sensor between the first plunger pump and the second plunger pump is synchronously recorded 1 And a second pressure sensor response value V' 2 (ii) a The first reciprocating plunger pump, the first pressure sensor, the second one-way valve and the second reciprocating plunger pump are arranged in sequence;
judgment response value V 1 And V' 2 Difference of (2)Whether greater than a second threshold, such as 0.002;
if the difference is larger than a second threshold value, the response slope K of the second pressure sensor is used 2 Slope K of response to first pressure sensor 1 And carrying out normalization correction.
After the correction is completed, the first reciprocating plunger pump directly performs pre-compression closed-loop control according to the response of the first pressure sensor in subsequent continuous work until the correction method is started again when the response fluctuation of the second pressure sensor exceeds 40psi during normal cooperative alternating operation of the first reciprocating plunger pump and the second reciprocating plunger pump.
In the present invention, as seen from the embodiment, the first threshold and the second threshold have no absolute uniform value, and the size is related to specific requirements, such as the requirement of accuracy of correction, the requirement of efficiency of correction, etc., and for those skilled in the art, a specific way to determine the size of the threshold based on different requirements is the prior art.
Claims (6)
1. The correction method of the liquid conveying device comprises the following steps:
when the second plunger pump conveys liquid outwards, the first plunger pump sucks the liquid, and a first one-way valve between the first plunger pump and the second plunger pump is in a closed state;
the first plunger pump pre-pumps the sucked liquidCompressing, when the variation of the first parameter of the second pressure sensor or the variation of the second parameter at the downstream of the output end of the second plunger pump exceeds a first threshold value, the first one-way valve is in a communication state, the first plunger pump stops pre-compression, and the first parameter of the second pressure sensor at the moment is recorded V1 And a first parameter of a first pressure sensor between the first plunger pump and the second plunger pump V2 ′ ;
Using the first parameter V1 And V2 ′ slope of response to the first pressure sensor K1 And/or the slope of the response of the second pressure sensor K2 And carrying out normalization correction.
2. The calibration method for a liquid delivery device according to claim 1, wherein the first parameter is determined V1 And V2 ′ whether the difference is greater than a second threshold;
if the difference is greater than a second threshold, the response slope K1 And the slope of the response K2 And carrying out normalization correction.
4. The calibration method for a liquid delivery device according to claim 1, wherein when the second plunger pump delivers the liquid at a constant flow to the outside, whether the pre-compression is stopped is determined by comparing the first parameter with a first threshold value, and the first parameter is a pressure value.
5. The correction method for a liquid transport apparatus according to claim 1, wherein when the second plunger pump transports the liquid with uniform acceleration outward, whether or not to stop the pre-compression is determined by comparing a variation amount of the second parameter, which is a response slope, with the first threshold value.
6. A calibration method for a liquid chromatograph including the calibration method for a liquid transport apparatus according to any one of claims 1 to 5, the liquid chromatograph including the liquid transport apparatus.
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CN202210551677.9A CN114910215A (en) | 2022-05-18 | 2022-05-18 | Liquid transfer device and calibration method for liquid chromatograph |
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CN202210551677.9A CN114910215A (en) | 2022-05-18 | 2022-05-18 | Liquid transfer device and calibration method for liquid chromatograph |
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Citations (7)
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US5637208A (en) * | 1993-03-05 | 1997-06-10 | Dourdeville; Theodore A. | Solvent pumping system for chromatography with switching-valve |
CN1490522A (en) * | 2002-10-18 | 2004-04-21 | ��ʽ�����������¼��� | Pump for liquid chromatograph and running method thereof |
JP2007327845A (en) * | 2006-06-07 | 2007-12-20 | Gl Sciences Inc | Liquid supplying method and device |
US20080245136A1 (en) * | 2004-05-21 | 2008-10-09 | Waters Investments Limited | Closed Loop Flow Control of a Hplc Constant Flow Pump To Enable Low-Flow Operation |
US20090193879A1 (en) * | 2008-01-31 | 2009-08-06 | Hitaci High-Technologies Corporation | Solvent delivery device and analytical system |
CN110621878A (en) * | 2017-07-03 | 2019-12-27 | 株式会社岛津制作所 | Liquid feeding device |
CN110809713A (en) * | 2017-10-23 | 2020-02-18 | 株式会社岛津制作所 | Liquid feeding device and fluid chromatograph |
-
2022
- 2022-05-18 CN CN202210551677.9A patent/CN114910215A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5637208A (en) * | 1993-03-05 | 1997-06-10 | Dourdeville; Theodore A. | Solvent pumping system for chromatography with switching-valve |
CN1490522A (en) * | 2002-10-18 | 2004-04-21 | ��ʽ�����������¼��� | Pump for liquid chromatograph and running method thereof |
US20080245136A1 (en) * | 2004-05-21 | 2008-10-09 | Waters Investments Limited | Closed Loop Flow Control of a Hplc Constant Flow Pump To Enable Low-Flow Operation |
JP2007327845A (en) * | 2006-06-07 | 2007-12-20 | Gl Sciences Inc | Liquid supplying method and device |
US20090193879A1 (en) * | 2008-01-31 | 2009-08-06 | Hitaci High-Technologies Corporation | Solvent delivery device and analytical system |
CN110621878A (en) * | 2017-07-03 | 2019-12-27 | 株式会社岛津制作所 | Liquid feeding device |
CN110809713A (en) * | 2017-10-23 | 2020-02-18 | 株式会社岛津制作所 | Liquid feeding device and fluid chromatograph |
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