CN104101658B - It is a kind of can be with the high performance liquid chromatograph of coutroi velocity - Google Patents
It is a kind of can be with the high performance liquid chromatograph of coutroi velocity Download PDFInfo
- Publication number
- CN104101658B CN104101658B CN201310122106.4A CN201310122106A CN104101658B CN 104101658 B CN104101658 B CN 104101658B CN 201310122106 A CN201310122106 A CN 201310122106A CN 104101658 B CN104101658 B CN 104101658B
- Authority
- CN
- China
- Prior art keywords
- outlet check
- volume
- liquid chromatograph
- check valves
- high performance
- 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.)
- Active
Links
Landscapes
- Control Of Positive-Displacement Pumps (AREA)
Abstract
The present invention provides it is a kind of can be with the high performance liquid chromatograph of coutroi velocity, including the double pump head plunger pump in series one by actuated by cams, one control system, plunger pump in series includes a main pump chamber, a main pump headpin plug, an auxiliary pump chamber, one auxiliary pump headpin plug, and the Outlet check valves for being used to connect main pump chamber and auxiliary pump chamber, control system are used for the movement for controlling main pump headpin plug and auxiliary pump headpin plug, control system is additionally operable to circulation and performs following steps：According to the configuration parameter of system pressure and liquid chromatograph, the calculated value of one outlet check valve opening point is obtained；Further according to system pressure, the calibration value of one outlet check valve opening point is obtained；Calculated value is added into the calibration value, obtains the actual value of Outlet check valves opening point；According to actual value, a compression volume is obtained；According to compression volume, the rotating speed of cam is controlled.The liquid chromatograph of the present invention, ensure that the mixed proportion of mobile phase, improves the accuracy of measurement result.
Description
Technical field
The present invention relates to liquid chromatograph field.
Background technology
High performance liquid chromatography is a chromatographic important branch, it is using liquid as mobile phase, using high pressure infuser system
System, the mobile phases such as the single solvent with opposed polarity or the mixed solvent of different proportion, buffer solution are pumped together with sample
Enter the chromatographic column of stationary phase is housed, after each component of sample is separated in column, be detected into detector, so that real
Now to the qualitative and quantitative analysis of sample.This method has become in the ambits such as chemistry, medicine, industry, agronomy, commodity inspection and method inspection
Important separate analytical technique.High performance liquid chromatograph（HPLC）It is the instrument for this analysis method.
As shown in Figure 1, high performance liquid chromatograph 1 is usually by solution organizer 101, infusion pump 102, injector 103, chromatography
The part such as column 104, detector 105, information processing system 106 and control system 107 forms, wherein in solution organizer 101
Solution is injected into the system of liquid chromatograph 1 after degassing, as mobile phase by infusion pump 102, sample solution pass through into
Sample device 103 injects mobile phase, and is loaded into chromatographic column 104 by mobile phase（Stationary phase）It is interior, due to each component in sample solution
There is different polarity from chromatographic column, when sample solution makees relative motion in chromatographic column 104, by repeated multiple times absorption-
The assigning process of desorption, each component produce larger difference in translational speed, are finally separated into single component successively from color
To compose in column 104 and separate out, the component of precipitation passes through monochromatic projection, and detector 105 detects the change of luminous intensity, and these
Optical signal is converted into electric signal and is transmitted to information processing system 106, and information processing system 106 is mainly used for the number that analysis receives
According to, and finally show them in the form of collection of illustrative plates.Control system 107 be used for realization to the control of each component in chromatograph and
Data processing etc. operates.
Wherein, infusion pump 102 is the power source of high performance liquid chromatograph 1, for by one or more kinds of mobile phases according to
Certain ratio is mixed, and is then delivered in the system of liquid chromatograph 1, its instrument index influenced includes pressure arteries and veins
Dynamic and mobile phase mixed proportion accuracy, if pressure fluctuation is big, just illustrates that the flow that infusion pump is exported is unstable, then flows
Fast precision will be poor, so that cause the fluctuation of detector baseline, the final testing result for influencing chromatograph 1；If mobile phase
Mixed proportion is inaccurate, then the result tested every time may will differ larger, cause no comparativity, and same method
Tested on different instruments and also have larger difference, be unfavorable for establishing the test method of unified standard.
At present, widely used high pressure pump is the double pump head plunger pump in series by actuated by cams.It is as shown in Fig. 2, double
Pump head connects reciprocating pump 2 mainly by main pump headpin plug 201, auxiliary pump headpin plug 202, main pump chamber 203, auxiliary pump chamber 204, entrance
The components such as check valve 205, Outlet check valves 206 and pressure sensor 207 form, and wherein plunger 201,202 is used for realization liquid
Compression, main pump chamber 203 and auxiliary pump chamber 204 be used to store liquid, and inlet one-way valve 205 is located at the arrival end of main pump chamber 203, goes out
Mouth check valve 206 is between main pump chamber 203 and auxiliary pump chamber 204, for isolating main pump chamber 203 and auxiliary pump chamber 204, pressure sensing
Device 207 is located at the exit of auxiliary pump chamber 204, for detecting system pressure.When liquid chromatograph 1 is run, control system 107 controls
Stepper motor operates, and motor drives cam rotation, then actuated by cams piston rod movement, and circular motion is converted the fortune that is in line
Dynamic, piston rod drives main pump headpin plug 201 and the 202 reciprocating and staggered movement of auxiliary pump headpin plug, realizes shuttle liquid conveying, and
And control system 107 controls the movement of major-minor pump head plunger according to cam curve so that output pressure is steady, with reference to Fig. 3, is
Cam curve figure, wherein abscissa are the step numbers of stepper motor, and ordinate is the movement velocity of cam, 3 curves point in figure
Do not represent main cam speed change curves, auxiliary cam speed change curves and two cams and speed change curves, wherein main
Cam and auxiliary cam are respectively used to the operation of driving main pump headpin plug and auxiliary pump headpin plug, and control system 107 is by controlling motor
Operating, be indirectly controlled the movement of major and minor pump head plunger.
But since liquid has compressibility, and the influence of the factor such as pump chamber volume and check valve leakage so that outlet
For the opening point of check valve 206 actually not at the switching point of main pump chamber liquid sucking-discharging, concrete reason is as follows：
With reference to reference to figure 3 and Fig. 4, at the T1 moment, main pump headpin plug 201 is in the low order end of main pump chamber 203, auxiliary pump headpin plug
202 auxiliary pump chamber 204 high order end, main pump chamber 203 begins preparing for imbibition, and auxiliary pump chamber 204 starts discharge opeing, at this time inlet one-way valve
205 and Outlet check valves 206 be turned off；T2 moment, main pump headpin plug 201 are run to the left, and auxiliary pump headpin plug 202 is run to the right,
203 imbibition of main pump chamber, inlet one-way valve 205 are opened, and Outlet check valves 206 are closed；T3 moment, main pump headpin plug 201 are run to
High order end, is filled with liquid in main pump chamber 203, main pump chamber 203 begins preparing for discharge opeing；T4 moment, main pump headpin plug 201 start to arrange
Liquid, auxiliary pump headpin plug 202 have run to low order end.Outlet check valves 206 have already turned on.Based on the total flow output entirely pumped becomes
The lifting rate of pump chamber 203 subtracts the liquid absorption amount of auxiliary pump chamber 204.T5 moment, auxiliary pump headpin plug 202 have run to high order end, main pump
Headpin plug 201 is still run to the right ... ..., and the operation so to move in circles, realizes the transmission of liquid.
Because Outlet check valves are by extraneous pressure-actuated passive valve, the pressure only worked as in main pump chamber 203 is big
In auxiliary pump chamber 204 during pressure, Outlet check valves 206 can just be opened, since liquid has different bodies at various pressures
Product（That is compressibility）And check valve has the reasons such as leakage and causes the opening points of Outlet check valves 206 not at the T3 moment, often
It can delay, it can be seen that in order to open Outlet check valves 206, main pump headpin plug 201 needs to run a distance to the right,
Liquid is compressed, Outlet check valves 206 could start discharge opeing after opening, but this partially liq compressed does not export
Into system, it is inaccurate for so will result in actual output liquid volume, therefore it is also not to cause the flow velocity of mobile phase
Accurately, and mobile phase mixed proportion it is inaccurate；And as system pressure changes, the liquid of the compression of main pump headpin plug 201
Body volume can also change, and so transplanting for measuring method and versatility can all have an impact.
Such as：One overall flow rate 1ml/min ratio of binary high pressure pump operation is the test condition of 30% methanol aqueous solution.
If system pressure is normal pressure at this time, the flow velocity operating that a pump is leaked water according to 0.7ml/min can be set, another pump walks first
Alcohol is operated according to the flow velocity of 0.3ml/min, is so exactly 30% methanol water mixed solution after their mixing.If at this time
System pressure is 30Mpa, is configured according further to flow velocity above, then the output volume flow rate for the pump actually leaked water is
0.296ml/min, the output volume flow rate for walking the pump of methanol is 0.675ml/min, and the ratio of reality output is 30.5%, real
The overall flow rate of border output is 0.971ml/min, and when system pressure changes, export ratio and volume flow rate can also change.
It is described on end, lack a kind of change for being enable to respond quickly system pressure in the prior art, accurately control mobile phase
Flow velocity high performance liquid chromatograph.
The content of the invention
In order to solve the problems in the existing technology, the present invention provides a kind of change for being enable to respond quickly system pressure
Change, the high performance liquid chromatograph of the flow velocity of accurate control mobile phase.
The present invention provides it is a kind of can be with the high performance liquid chromatograph of coutroi velocity, including one the double pump by actuated by cams
Head plunger pump in series, a control system, the plunger pump in series include a main pump chamber, a main pump headpin plug, one
Auxiliary pump chamber, an auxiliary pump headpin plug, and the Outlet check valves for being used to connect the main pump chamber and auxiliary pump chamber, it is described
Control system is used for the movement for controlling main pump headpin plug and auxiliary pump headpin plug, and it is following that the control system is additionally operable to circulation execution
Step：
1）According to the configuration parameter of the system pressure and the liquid chromatograph, obtain one outlet check valve and open
Open calculated value a little；
2）Further according to the system pressure, the calibration value of one outlet check valve opening point is obtained；
3）According to the actual value and the sum of the calibration value, the actual value of Outlet check valves opening point is obtained；
4）According to the actual value, a compression volume is obtained；
5）According to the compression volume, the rotating speed of the cam is controlled.
In liquid chromatograph of the present invention, described 1）According to the system pressure and the liquid chromatogram
The configuration parameter of instrument, obtains the calculated value of one outlet check valve opening point, can refer to, according to the system pressure and institute
The configuration parameter for the liquid chromatograph stated, obtains the initial compression liquid volume of the main pump headpin plug, and the outlet
The leakage volume of check valve, then according to the initial compression liquid volume and the leakage volume, obtains described going out
The calculated value of mouth check valve opening point.
In liquid chromatograph of the present invention, system pressure and the liquid chromatograph described in the basis
Configuration parameter, obtain the initial compression liquid volume of main pump headpin plug and the leakage body of the Outlet check valves
Product, can refer to, the compressed coefficient of liquid in main pump chamber is multiplied by with the system pressure, multiplied by with main pump cavity volume, obtain
The initial compression liquid volume of the main pump headpin plug, and letting out for the Outlet check valves is multiplied by with the system pressure
Constant is leaked, obtains the leakage volume of the Outlet check valves.
In liquid chromatograph of the present invention, according to the initial compression liquid volume and the leakage body
Product, obtains the calculated value of the Outlet check valves opening point, can refer to, the initial compression liquid volume is added institute
The leakage volume stated, and according to above-mentioned volume and and the cam curve functional equation, obtain the outlet list
To the calculated value of valve opening point.
In liquid chromatograph of the present invention, described 2）Further according to the system pressure, one outlet is obtained
The calibration value of check valve opening point, can refer to, according to rising or falling for the system pressure near Outlet check valves opening point
Amplitude, obtain the calibration value of the Outlet check valves opening point.
In liquid chromatograph of the present invention, the system pressure according near Outlet check valves opening point
Amplitude is risen or fallen, the calibration value of the Outlet check valves opening point is obtained, can refer to, with the system pressure
Rising amplitude is multiplied by calibration factor -2, the calibration value of the Outlet check valves opening point is obtained, with the system pressure
The descent amplitude of power is multiplied by a calibration factor 2, obtains the calibration value of the opening point of the Outlet check valves.
In liquid chromatograph of the present invention, 4）According to the actual value, a compression volume, Ke Yishi are obtained
Refer to, according to the actual value and the functional equation of the curve of the cam, obtain the compression volume.
In liquid chromatograph of the present invention, 5）According to the compression volume, the rotating speed of the cam is controlled,
It can refer to, according to the proportionate relationship of the compression volume and the stroke volume of the main pump headpin plug, control described
The rotating speed of cam.
Liquid chromatograph of the present invention, can with influence of the quick response system pressure to Outlet check valves opening point,
Constantly calibrated to opening point, according to the opening point after calibration, adjust the rotating speed of cam, so that the flow velocity of mobile phase is adjusted,
It ensure that the mixed proportion of mobile phase, improve the accuracy of measurement result, and the result difference measured every time is smaller, is beneficial to
Establish unified test method.
And liquid chromatograph of the present invention, by constantly calibrating the opening point of Outlet check valves, alleviates system
Pressure fluctuation, improves the measurement accuracy of instrument.
Brief description of the drawings
Fig. 1 is the structure diagram of high performance liquid chromatograph 1.
Fig. 2 is the structure diagram of double pump head plunger pump in series 2.
Fig. 3 is the cam curve figure for driving double pump head plunger pump in series 2.
Fig. 4 is double pump head plunger pump in series 2 in working state schematic representation at different moments.
Fig. 5 is the work flow diagram of the control method described in present pre-ferred embodiments.
Fig. 6 is the curve map for the main cam for driving main pump headpin plug 201.
Fig. 7 is that the amplitude of the system pressure in liquid chromatograph 1 produces pressue-graph when rising.
Fig. 8 is that the amplitude of the system pressure in liquid chromatograph 1 produces pressue-graph when declining.
Fig. 9 is the stable pressue-graph of system pressure after calibration.
Embodiment
The preferred embodiment of the present invention is introduced below in conjunction with the accompanying drawings.
With reference to figure 1, the high performance liquid chromatograph 1 in the present embodiment includes solution organizer 101, infusion pump 102, injector
103rd, in chromatographic column 104, detector 105, information processing system 106 and control system 107 etc., wherein solution organizer 101
Solution is injected into the system of liquid chromatograph 1 after degassing, as mobile phase by infusion pump 102, sample solution pass through into
Sample device 103 injects mobile phase, and is loaded into chromatographic column 104 by mobile phase（Stationary phase）It is interior, due to each component in sample solution
There is different polarity from chromatographic column, when sample solution makees relative motion in chromatographic column 104, by repeated multiple times absorption-
The assigning process of desorption, each component produce larger difference in translational speed, are finally separated into single component successively from color
To compose in column 104 and separate out, the component of precipitation passes through monochromatic projection, and detector 105 detects the change of luminous intensity, and these
Optical signal is converted into electric signal and is transmitted to information processing system 106, and the data received are carried out numeral by information processing system 106
Analysis, and finally show them in the form of collection of illustrative plates, control system 107 is used for realization the control to each component in chromatograph
Operated with data processing etc..
As an example, information processing system 106 can have the equipment reality of information processing capability by computer etc.
It is existing.
As an example, control system 107 can be realized by digital processing units such as DSP, FPGA, and controlled and be
System 107 can be embedded in the system of detector 105.
As an example, infusion pump 102 can be single pump, binary pump or quaternary pump.
With reference to figure 2, in the present embodiment, infusion pump 102 of the invention is by the double pump head plunger pump in series 2 shown in Fig. 2
Form, plunger pump in series 2 mainly includes main pump headpin plug 201, auxiliary pump headpin plug 202, main pump chamber 203, auxiliary pump chamber 204, entrance
The components such as check valve 205, Outlet check valves 206 and pressure sensor 207 form, and wherein plunger 201,202 is used for realization liquid
Compression, main pump chamber 203 and auxiliary pump chamber 204 be used to store liquid, and inlet one-way valve 205 is located at the arrival end of main pump chamber 203, goes out
Mouth check valve 206 is between main pump chamber 203 and auxiliary pump chamber 204, for isolating main pump chamber 203 and auxiliary pump chamber 204, pressure sensing
Device 207 is located at the exit of auxiliary pump chamber 204, for detecting system pressure V.When liquid chromatograph 1 is run, control system 107 is controlled
Stepper motor operating processed, motor drive cam rotation, then actuated by cams piston rod movement, and circular motion is converted the fortune that is in line
Dynamic, piston rod drives main pump headpin plug 201 and the 202 reciprocating and staggered movement of auxiliary pump headpin plug, realizes shuttle liquid conveying, and
And control system 107 controls the movement of major-minor pump head plunger according to cam curve so that output pressure is steady, with reference to Fig. 3, is
Cam curve figure, wherein abscissa are the step numbers of stepper motor, and ordinate is the movement velocity of cam, 3 curves point in figure
Do not represent main cam speed change curves, auxiliary cam speed change curves and two cams and speed change curves, control system
System 107 is indirectly controlled the movement of major and minor pump head plunger by controlling the operating of motor.
From the description of background technology as can be seen that the change of flow rate of mobile phase, is due to system pressure V changes, causes liquid
The change of the compressed coefficient of body and the leakage rate of Outlet check valves 206, and then cause the opening point of Outlet check valves 206 to lag institute
Caused by, therefore, in order to solve the problems, such as that flow rate of mobile phase is uncertain in the prior art, the present invention obtains main plunger pump head first
201, in order to make Outlet check valves 206 open the volume of compressed liquid, then by the liquid volume, obtain cam rotating speed
Variable quantity, so as to control the speed of cam in turn, cam is improved corresponding speed to compensate the liquid bulk of above-mentioned compression
Product.
With reference to figure 5, control method of the present invention is：
The control system circulation performs following steps：
501：According to the configuration parameter of system pressure V and liquid chromatograph 1, the meter of 206 opening point of Outlet check valves is obtained
Calculation value；
502：Further according to system pressure V, the calibration value of 206 opening point of Outlet check valves is obtained；
503：According to the sum of calculated value and calibration value, the actual value of 206 opening point of Outlet check valves is obtained；
504：According to actual value, compression volume Vb is obtained；
505：According to compression volume Vb, the rotating speed of cam is controlled.
It is the opening point that requirement obtains Outlet check valves 206 first, and then main plunger pump head 201 is obtained according to opening point and is compressed
Liquid volume.Specific method is as follows：
501：According to the configuration parameter of system pressure V and liquid chromatograph 1, the meter of 206 opening point of Outlet check valves is obtained
Calculation value；
502：Further according to system pressure V, the calibration value of 206 opening point of Outlet check valves is obtained；
503：According to the sum of calculated value and calibration value, the actual value of 206 opening point of Outlet check valves is obtained；
For the present invention by the Factor Decomposition of influence 206 opening point of Outlet check valves into two classes, the first kind is according to system configuration
Obtained calculated value, calculated value refer to the theoretical value in the case where instrument configuration is fixed, obtained according to theoretical formula method；Separately
One kind is the calibration value obtained according to the change of instrument processing error and measuring condition, and calibration value refers to due in measurement process
The processing differences of instrument, and the slight change value caused by the change of internal and external environment.Finally by calculated value and calibration value phase
Add, obtain the actual value of 206 opening point of Outlet check valves.The control method opens Outlet check valves 206 because having taken into full account
Open influence factor a little, so as to the actual value of the opening point for the check valve 206 that more fast and accurately finds an exit.
The opening point for the check valve 206 that finds an exit is described in detail below realizes process：
501：According to the configuration parameter of system pressure V and liquid chromatograph 1, the calculating of one outlet check valve 206 is obtained
Value；
The wherein described system pressure V refers to the pressure in chromatograph system, is that finger pressure passes in the present embodiment
The pressure that sensor 207 detects；The configuration parameter refers to meet apparatus measures needs, is configured for chromatograph 1 each
The physical size of kind component or characteristic index parameter etc..
Further, according to the configuration parameter of the system pressure V and the liquid chromatograph, one outlet is obtained
The calculated value of check valve opening point, refers to,
According to the configuration parameter of the system pressure V of liquid chromatograph 1 and liquid chromatograph 1, main pump headpin plug 201 is obtained
Initial compression liquid volume Vs, and the leakage volume Vx of Outlet check valves 206, then according to initial compression liquid volume Vs and letting out
Volume Vx is leaked, obtains the calculated value of Outlet check valves opening point 206.
According to the introduction of background technology, the condition that Outlet check valves 206 are opened is that fluid pressure in main pump chamber 203 is more than
Opened during fluid pressure in auxiliary pump chamber 204, if it is assumed that the liquid in pump chamber is ideally incompressible, and
The leakage rate of Outlet check valves 206 is zero, then the opening point of Outlet check valves 206 is exactly on cam curve as shown in Figure 3
Main pump headpin plug 201 starts the position T3 of discharge opeing, but in actually measuring, opening point is often deferred to T4 positions, also
It is that main pump headpin plug 201 needs to compress a certain amount of liquid volume and just can open Outlet check valves 206.The reason is that, liquid
All it is that there is certain compressed coefficient, i.e., volume is different to the liquid of identical molecular weight at various pressures, so being
Opening Outlet check valves 206, main pump headpin plug 201 need to compress a certain amount of volume, initial compression liquid volume Vs, and by
Can all there is certain leakage in the Outlet check valves 206 actually used, and certain volume can be leaked away, i.e. leakage volume Vx,
Therefore, it is necessary to consider the initial compression of main pump headpin plug 201 when the calculated value of opening point of Outlet check valves 206 is calculated
The sum of the leakage volume Vx of liquid volume Vs and Outlet check valves 206.
Further, according to the configuration parameter of the system pressure V of liquid chromatograph 1 and liquid chromatograph 1, main pump is obtained
The initial compression liquid volume Vs of headpin plug 201, and the leakage volume Vx of Outlet check valves 206, refer to
The compressed coefficient C1 of liquid in main pump chamber 203 is multiplied by with system pressure V, multiplied by with main pump cavity volume Vz, is led
The initial compression liquid volume Vs of pump head plunger 201, and
The leakage constant C2 of Outlet check valves 206 is multiplied by with system pressure V, obtains the leakage volume of Outlet check valves 206
Vx。
When main pump chamber 203 there is not discharge opeing, pressure therein is normal pressure, and pressure in auxiliary pump chamber 204 at this time（That is system
Pressure）It is high pressure at this time, in order to open Outlet check valves 206, it is necessary to the pressure in main pump chamber 203 is more than system pressure V,
Since the liquid volume under normal pressure is bigger than the liquid volume under high pressure（It is related with liquid compressibility factor）, so main pump headpin plug
201 need to move a distance, compress the liquid in main pump chamber 203 to produce high pressure, and inventor have passed through analysis and anti-for this
Multiple test, obtains the liquid volume that main pump headpin plug 201 moves the compression of this segment distance（That is initial compression liquid volume Vs）With
System pressure V, the compressed coefficient C1 of liquid are related with the volume Vz of main pump chamber 203, i.e. Vs=V × C1 × Vz.
Also, also as Outlet check valves 206 have certain leakage, so main pump headpin plug 201 needs the liquid compressed
Body volume also needs to the leakage rate plus Outlet check valves 206, and inventor with after test, obtains Outlet check valves by analysis
206 leakage volume Vx and system pressure V and leakage constant C2 is related, i.e. Vx=V × C2.
Finally, according to obtained initial compression liquid volume Vs and the leakage volume of Outlet check valves 206, it is single to obtain outlet
To the calculated value of 206 opening point of valve, refer to,
By initial compression liquid volume Vs add Outlet check valves 206 leakage volume, and according to their volumes and Vh
With the functional equation of the cam curve, the calculated value of the opening point of Outlet check valves is obtained.
It can be seen that according to analysis above by the leakage volume of initial compression liquid volume Vs and Outlet check valves 206
Vx can obtain a volume after being added, which is exactly to reach the condition of the opening of Outlet check valves 206, main pump headpin plug
Liquid volume Vh=Vs+Vx=V × C1 × Vz+V × C2 that 201 needs compress, but because the opening point of Outlet check valves 206
Calculated value actually refers to the operating step number of stepper motor, so we also need to be converted to stepper motor according to volume Vh
Operate step number.
It is the speed of main cam with reference to figure 6（Ordinate）- stepper motor steps（Abscissa）Graph of relation, in figure
A points be point that main pump headpin plug 201 starts discharge opeing, this point is fixed, and Sp points are the actual unlatchings of Outlet check valves 206
Point, according to analysis above, Sp points and system pressure V, liquid compressibility factor C1, the volume Vz and Outlet check valves of main pump chamber
206 leadage coefficient is relevant, and the area of dash area is liquid volume Vh, further according to the functional equation of cam curve（It is convex
The functional equation for taking turns curve represents the functional relation of cam speed and stepper motor steps）, a two element equations can be obtained,
The value of Sp points can be obtained by solving equation group.
It is assumed that volume Vh=10000ul is calculated by above, the functional equation of cam curve is y=2x, and y is represented
The speed of cam, x represent stepper motor steps, and 2 be the slope to that section of cam curve between Sp points in A points, then can be with
Obtain following two element equations：
y=2x
xy/2=2
Finally try to achieve x=100, y=200
That is the abscissa that the abscissa of Sp points subtracts A points is equal to 100, it is assumed that the abscissa of A points is 100, therefore can be obtained
To the abscissa of Sp points, i.e. the calculated value of 201 opening point of Outlet check valves is the step of 100+100=200.
In the present embodiment, the curve of cam is the memory that control system 107 is stored in by way of data list
In, when calculating the calculated value of 206 opening point of Outlet check valves, the step of corresponding stepper motor is found by way of tabling look-up
Number, that is, the calculated value of 206 opening point of Outlet check valves.
502：According to system pressure V, the calibration value of 206 opening point of Outlet check valves is obtained；
Since different instruments can all have differences in processing, and due to measuring condition, such as the change of temperature etc.,
In instrument operational process, it can also cause the change of the compressed coefficient C1 of such as liquid or the leakage constant C2 of Outlet check valves 206,
So the present invention can obtain within each service cycle of cam according to the change for the amplitude that system pressure P rises or falls
The calibration value of 206 opening point of one outlet check valve, the value can more accurately reflect single due to being exported caused by above-mentioned factor
Change to the opening point of valve 206.
After liquid chromatograph 1 is started shooting, control system 107 can be carried out first according to the calculated value of 206 opening point of Outlet check valves
Control, then according to the change for detecting system pressure 107, judges the change of system pressure amplitude, if pressure magnitude is with putting down
Equal amplitude is compared to rising or declines, then and just there is deviation in the opening point of explanation Outlet check valves 206, in the present invention,
After inventor is by long-term test, a calibration factor is drawn, when pressure changes, be just multiplied by with the changing value of pressure
The calibration factor, has just obtained the calibration value of 206 opening point of Outlet check valves.
For example, with reference to figure 7, the amplitude of system pressure P rises 20psi in figure, illustrates the change due to measuring condition, leads
The calculated value of 206 opening point of Outlet check valves is caused to move forward than actual value, so the actual value of opening point in order to obtain, it is necessary to
Calibration factor -2 are multiplied by with the system pressure P amplitude 20psi risen, obtain the calibration value -40 of 206 opening point of Outlet check valves
Step；Referring again to Fig. 8, the amplitude of system pressure P have dropped 20psi in figure, illustrate the change due to measuring condition, cause outlet single
Retreated to the calculated value of 206 opening point of valve than actual value, so the actual value of opening point in order to obtain, it is necessary to system pressure
The amplitude 20 that power P declines is multiplied by calibration factor 2, obtains 40 step of calibration value of opening point.
503：Above-mentioned calculated value is added into above-mentioned calibration value, obtains the actual value of 206 opening point of Outlet check valves；
Finally, calculated value obtained above is added into calibration value, just obtains the reality of 206 opening point of Outlet check valves
Value.
For example, 200 steps are equal to by the calculated value that 206 opening point of Outlet check valves is calculated above, then be
In the case that pressure of uniting rises, final actual value adds the step of calibration value -40, i.e. Outlet check valves 206 equal to 200 step of calculated value
The actual value of opening point be 160 steps；And in the case where system pressure declines, final actual value is equal to 200 step of calculated value
Plus 40 step of calibration value, i.e. the actual value of the opening point of Outlet check valves 206 is 240 steps.
504：According to actual value, compression volume Vb is obtained；
It is the stable design sketch of system pressure P after Outlet check valves 206 are calibrated with reference to figure 9.As can be seen that by upper
After the method stated is calibrated, system pressure becomes steadily, also the value of the opening point of the Outlet check valves 206 with regard to explanation at this time
Should be accurately, so the value according to opening point at this time, it becomes possible to obtain main pump headpin plug 201 to make outlet unidirectional
Valve 206 is opened, the liquid volume compressed, i.e. compression volume Vb.
Specifically, according to the actual value and the functional equation of the curve of the cam, the compression body is obtained
Product.
Pass through the actual value of the opening point that Outlet check valves 206 are calculated above, it is assumed that be 160 steps, then by this
Value is taken in the functional equation of cam curve, is, for example, y=2x, with regard to that can obtain compression volume Vb.Specific method is, it is assumed that x=
160, so the abscissa of y=320, A point is 100, then Vb=320*（160-100）/2=9600ul
505:According to compression volume Vb, the rotating speed of cam is controlled
Specifically refer to, according to the proportionate relationship of compression volume Vb and the stroke volume Vc of main pump headpin plug 201, described in control
Cam rotating speed.
When stroke volume Vc refers to perfect condition, the discharge opeing volume of main pump headpin plug 201, it is known quantity.
It is assumed that stroke volume Vc=192000ul, the flow velocity of mobile phase is T=1ml/min, then cam is in the ideal situation
Rotating speed is R=T/Vc=1/192, but in an actual situation, since main plunger pump head 201 have compressed liquid volume Vb, so such as
Fruit cam is operated according further to R, is the flow velocity 1ml/min that cannot reach mobile phase, in order to compensate for compression volume Vb, the reality of cam
Rotating speed should be：
R*Vc/(Vc-Vb)=1/(192-9.6)=1/182.4
As it can be seen that the rotating speed of cam reduces, so as to compensate for the liquid of compression volume Vb part.
It is described on end, after liquid chromatograph 1 brings into operation, detecting system pressure P first, then 107 basis of control system
The relevant configured parameter of system pressure P and above-mentioned liquid chromatograph, obtain the calculated value of 206 opening point of Outlet check valves,
After chromatograph 1 runs a period of time, pressure sensor 207 can detect the change of system pressure P, and control system 107 is according to being
Unite the change of pressure P, obtain the calibration value of Outlet check valves 206, above-mentioned calculated value is added with calibration value to obtain opening point
Actual value, that is, stepper motor operating step number, the curve of actual value and cam further according to opening point, obtains main pump head
The compression volume Vb of plunger 201, finally obtains the rotating speed of cam reality according to Vb and stroke volume Vc, is previously mentioned that column
Plug pump is to drive cam rotation by stepper motor, then actuated by cams piston rod movement, and circular motion is converted the fortune that is in line
Dynamic, piston rod drives main pump headpin plug 201 and the 202 reciprocating and staggered movement of auxiliary pump headpin plug, so by adjusting the rotating speed of cam,
The final adjusting realized to velocity of plunger, also just have adjusted the flow velocity of mobile phase so that the flow velocity of reality output mobile phase reaches
To predetermined flow velocity, the accuracy of apparatus measures ensure that, and mobile phase mixed proportion is accurate.
In the present embodiment, it is the just adjustment of progress flow rate of mobile phase, when this adjustment is after system pressure P is steady
Shi Yunhang's.
In the present embodiment, the calculated value is computing, and is added with calibration value at this time, obtains opening point
Actual value, the actual value so obtained can more accurately reflect actual 206 opening point of Outlet check valves.
As other for example, according to the demand of the measurement accuracy of different system, calculated value can also be according to certain
Time interval is calculated, and is then added with calibration value at this time, obtains the actual value of opening point.
In the present embodiment, calibration value be cam operation a cycle calculate once, then with corresponding calculating at this time
Value is added, and obtains the actual value of opening point.The actual value so obtained can more accurately reflect actual Outlet check valves
206 opening point.
As other for example, according to the demand of the measurement accuracy of different system, calibration value can also be transported in cam
2 or 3 computation of Period of row once, are then added with corresponding calculated value at this time, obtain the actual value of opening point.
In the present embodiment, it is that no system pressure changes because when chromatograph 1 is just started shooting, so opening
The initial value of point calibration value is 0.
Liquid chromatograph of the present invention, there is provided a kind of liquid chromatograph that can control flow rate of mobile phase, this method
The actual opening point of Outlet check valves 206 is obtained according to the configuration parameter of system pressure and instrument, and is obtained according to the opening point
The liquid volume Vb compressed to main pump headpin plug 201, so as to obtain the rotating speed of cam reality, finally obtains accurate mobile phase stream
Speed so that the mixed proportion of mobile phase is more accurate, and the measurement of instrument is more accurate, and measuring method versatility is more preferable.
Above-described is only the specific embodiment of the present invention, and the protection domain being not intended to limit the present invention is all at this
The spirit of invention and any modification, equivalent substitution, improvement and etc. within principle, done, should be included in the protection model of the present invention
Within enclosing.
Claims (8)
1. a kind of can be with the high performance liquid chromatograph of coutroi velocity, including one the double pump head plunger pump in series by actuated by cams,
One control system,
The plunger pump in series includes a main pump chamber, a main pump headpin plug, an auxiliary pump chamber, an auxiliary pump headpin plug,
And the Outlet check valves for being used to connect the main pump chamber and auxiliary pump chamber,
The control system is used for the movement for controlling main pump headpin plug and auxiliary pump headpin plug,
It is characterized in that,
The control system is additionally operable to circulation and performs following steps：
1) according to the configuration parameter of the system pressure of the high performance liquid chromatograph and the high performance liquid chromatograph, obtain
The calculated value of one outlet check valve opening point；
2) further according to the system pressure of the high performance liquid chromatograph, the calibration value of one outlet check valve opening point is obtained；
3) according to the sum of the calculated value and calibration value, the actual value of Outlet check valves opening point is obtained；
4) according to the actual value, a compression volume is obtained；
5) according to the compression volume, the rotating speed of the cam is controlled；
Wherein,
1) described joins according to the configuration of the system pressure of the high performance liquid chromatograph and the high performance liquid chromatograph
Number, obtains the calculated value of one outlet check valve opening point, refers to,
According to the configuration parameter of the system pressure of the high performance liquid chromatograph and the high performance liquid chromatograph, institute is obtained
The initial compression liquid volume for the main pump headpin plug stated, and the leakage volume of the Outlet check valves, then according to described
Initial compression liquid volume and the leakage volume, obtain the calculated value of the Outlet check valves opening point.
2. high performance liquid chromatograph according to claim 1, it is characterised in that
The configuration parameter of the system pressure of high performance liquid chromatograph described in the basis and the high performance liquid chromatograph,
The initial compression liquid volume of main pump headpin plug and the leakage volume of the Outlet check valves is obtained, is referred to,
The compressed coefficient of liquid in main pump chamber is multiplied by with the system pressure of the high performance liquid chromatograph, multiplied by with main pump cavity
Product, obtains the initial compression liquid volume of the main pump headpin plug, and
The leakage constant of the Outlet check valves is multiplied by with the system pressure of the high performance liquid chromatograph, is obtained described
The leakage volume of Outlet check valves.
3. high performance liquid chromatograph according to claim 2, it is characterised in that
According to the initial compression liquid volume and the leakage volume, the meter of the Outlet check valves opening point is obtained
Calculation value, refers to,
The initial compression liquid volume is added into the leakage volume, and according to above-mentioned volume and and the cam
Curve functional equation, obtain the calculated value of the Outlet check valves opening point.
4. according to the high performance liquid chromatograph described in claim 1,2 or 3, it is characterised in that
It is described 2) further according to the system pressure of the high performance liquid chromatograph, obtain the school of one outlet check valve opening point
Quasi- value,
Refer to,
According to the amplitude risen or fallen of the system pressure near Outlet check valves opening point, the Outlet check valves are obtained
The calibration value of opening point.
5. high performance liquid chromatograph according to claim 4, it is characterised in that described according to Outlet check valves opening point
Neighbouring system pressure rises or falls amplitude, obtains the calibration value of the Outlet check valves opening point, refers to,
Calibration factor -2 are multiplied by with the rising amplitude of the system pressure, obtain the Outlet check valves opening point
Calibration value,
A calibration factor 2 is multiplied by with the descent amplitude of the system pressure of the high performance liquid chromatograph, obtains described going out
The calibration value of the opening point of mouth check valve.
6. according to the high performance liquid chromatograph described in claim 1,2 or 3, it is characterised in that
4) according to the actual value, a compression volume is obtained, is referred to,
According to the actual value and the functional equation of the curve of the cam, the compression volume is obtained.
7. high performance liquid chromatograph according to claim 1, it is characterised in that
5) according to the compression volume, the rotating speed of the cam is controlled, is referred to,
According to the proportionate relationship of the compression volume and the stroke volume of the main pump headpin plug, the cam is controlled
Rotating speed.
8. high performance liquid chromatograph according to claim 6, it is characterised in that
5) according to the compression volume, the rotating speed of the cam is controlled, is referred to,
According to the proportionate relationship of the compression volume and the stroke volume of the main pump headpin plug, the cam is controlled
Rotating speed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310122106.4A CN104101658B (en) | 2013-04-10 | 2013-04-10 | It is a kind of can be with the high performance liquid chromatograph of coutroi velocity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310122106.4A CN104101658B (en) | 2013-04-10 | 2013-04-10 | It is a kind of can be with the high performance liquid chromatograph of coutroi velocity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104101658A CN104101658A (en) | 2014-10-15 |
| CN104101658B true CN104101658B (en) | 2018-04-24 |
Family
ID=51669981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310122106.4A Active CN104101658B (en) | 2013-04-10 | 2013-04-10 | It is a kind of can be with the high performance liquid chromatograph of coutroi velocity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104101658B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107781153B (en) * | 2016-08-31 | 2020-06-30 | 北京普源精电科技有限公司 | Method and device for controlling system pressure pulsation and high-pressure infusion pump |
| CN107784147B (en) * | 2016-08-31 | 2023-04-18 | 北京普源精电科技有限公司 | Method and device for controlling flow rate of main pump and auxiliary pump of high-pressure infusion pump |
| DE102017115242A1 (en) | 2017-07-07 | 2019-01-10 | Dionex Softron Gmbh | Pump operation method, use of the method in HPLC, pump, pump system and HPLC system |
| JP6866835B2 (en) * | 2017-12-01 | 2021-04-28 | 株式会社島津製作所 | Liquid delivery pump for fluid chromatograph |
| CN108169394B (en) * | 2017-12-26 | 2019-11-29 | 迈克医疗电子有限公司 | Flow control methods and device, analysis instrument and computer readable storage medium |
| CN110794069A (en) * | 2019-10-08 | 2020-02-14 | 北京卫星制造厂有限公司 | Micro-upgrade volume-based organic solvent liquid compressibility online test method and system |
| CN111812262B (en) * | 2020-07-17 | 2023-06-30 | 依利特(苏州)分析仪器有限公司 | Liquid chromatography multielement low-pressure low-proportion control method and device |
| CN112903853B (en) * | 2021-01-22 | 2022-11-29 | 海易（大连）实业有限公司 | Control system and control method of high performance liquid chromatograph |
| US11828175B2 (en) | 2021-07-08 | 2023-11-28 | Saudi Arabian Oil Company | Systems and methods for measuring phase flow rates of a multiphase production fluid |
| CN114941621B (en) * | 2022-04-29 | 2023-03-14 | 鲲鹏仪器(大连)有限公司 | Control method for realizing stable liquid delivery of high performance liquid chromatograph |
| CN115166119A (en) * | 2022-06-30 | 2022-10-11 | 鲲鹏仪器(大连)有限公司 | High-precision low-pressure gradient method of high performance liquid chromatograph |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201696242U (en) * | 2010-04-22 | 2011-01-05 | 杭州奥希科技有限公司 | Double-plunger high-pressure infusion pump for liquid chromatograph |
| DE102010030325A1 (en) * | 2010-06-22 | 2011-12-22 | Agilent Technologies Inc. | Fluid pump e.g. piston pump, for use in e.g. high-performance liquid chromatography apparatus, has control unit configured such that actual volume of pumped fluid is adjusted to predetermined nominal volume of transported fluid |
| CN202693596U (en) * | 2011-02-09 | 2013-01-23 | 安捷伦科技有限公司 | Liquid supply system with optimized switching between different solvents |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004150402A (en) * | 2002-11-01 | 2004-05-27 | Hitachi High-Technologies Corp | Pump for liquid chromatography |
| JP5049808B2 (en) * | 2008-01-31 | 2012-10-17 | 株式会社日立ハイテクノロジーズ | Liquid feeding device and analyzer having the same |
| 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 |
-
2013
- 2013-04-10 CN CN201310122106.4A patent/CN104101658B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201696242U (en) * | 2010-04-22 | 2011-01-05 | 杭州奥希科技有限公司 | Double-plunger high-pressure infusion pump for liquid chromatograph |
| DE102010030325A1 (en) * | 2010-06-22 | 2011-12-22 | Agilent Technologies Inc. | Fluid pump e.g. piston pump, for use in e.g. high-performance liquid chromatography apparatus, has control unit configured such that actual volume of pumped fluid is adjusted to predetermined nominal volume of transported fluid |
| CN202693596U (en) * | 2011-02-09 | 2013-01-23 | 安捷伦科技有限公司 | Liquid supply system with optimized switching between different solvents |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104101658A (en) | 2014-10-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104101658B (en) | It is a kind of can be with the high performance liquid chromatograph of coutroi velocity | |
| US7578173B2 (en) | Chromatography system with flow sensing | |
| CN104101669B (en) | A kind of high performance liquid chromatograph for control system pressure fluctuation | |
| US7674375B2 (en) | Closed loop flow control of a HPLC constant flow pump to enable low-flow operation | |
| US8685218B2 (en) | Precision flow control system | |
| Li et al. | Miniaturised medium pressure capillary liquid chromatography system with flexible open platform design using off-the-shelf microfluidic components | |
| US8191405B2 (en) | Solvent delivery device and analytical system | |
| US20030052007A1 (en) | Precision flow control system | |
| CN102866218B (en) | Intake monitoring for accurate proportioning | |
| JPS5879683A (en) | Fixed volume type high pressure pump | |
| CN104931625A (en) | Method for adjusting a gradient delay volume | |
| US20080047611A1 (en) | Fluid pump having low pressure metering and high pressure delivering | |
| WO2010137554A1 (en) | Liquid delivery device and liquid chromatography device | |
| JP5887412B2 (en) | Liquid chromatograph device and liquid feeding device | |
| CN107345890A (en) | A kind of shale gas adsorption-desorption/exploitation simulated experiment apparatus and method | |
| CN107781153A (en) | The method and apparatus and high pressure pump of control system pressure fluctuation | |
| CN104111342A (en) | Precise loading system, precise loading method, and biochemistry analyzer | |
| CN104730180B (en) | A kind of liquid chromatograph with mixed proportion debugging functions | |
| CN108167171A (en) | A kind of control method that pump pressure fluctuation automatically corrects of infusing | |
| US10976289B2 (en) | Corrected flow reporting under dynamic conditions by system modeling | |
| GB2454783A (en) | HPLC constant flow pump to enable low-flow operation, wherein thermal-based sensors are contained within an isothermal block | |
| CN111289681A (en) | Injection method suitable for marine instrument | |
| JPS63313032A (en) | Measuring instrument for viscosity of liquid | |
| WO2013083187A1 (en) | Calibration procedure for fluidic sensors |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20160510 Address after: 102206 Beijing City, Shahe Town, step on the river village, No. 156 Applicant after: Beijing RIGOL Science and Technology Co., Ltd. Address before: 102206 Beijing City, Shahe Town, step on the river village, No. 156 Applicant before: Beijing Rigol Technologies, Inc. |
|
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180111 Address after: Kolding road high tech Zone of Suzhou City, Jiangsu Province, No. 8 215000 Applicant after: SUZHOU RIGOL PRECISION ELECTRIC TECHNOLOGIES CO., LTD. Address before: 102206 Beijing City, Shahe Town, step on the river village, No. 156 Applicant before: Beijing RIGOL Science and Technology Co., Ltd. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200121 Address after: 215000 Room 408, building 1, No. 8, Jinfeng Road, hi tech city, Suzhou City, Jiangsu Province Patentee after: Suzhou Litong Precision Measurement System Co., Ltd Address before: Kolding road high tech Zone of Suzhou City, Jiangsu Province, No. 8 215000 Patentee before: SUZHOU RIGOL PRECISION ELECTRIC TECHNOLOGIES CO., LTD. |