CN110764407A - Pressure control method and system for solid phase extraction column and electronic equipment - Google Patents
Pressure control method and system for solid phase extraction column and electronic equipment Download PDFInfo
- Publication number
- CN110764407A CN110764407A CN201911177334.5A CN201911177334A CN110764407A CN 110764407 A CN110764407 A CN 110764407A CN 201911177334 A CN201911177334 A CN 201911177334A CN 110764407 A CN110764407 A CN 110764407A
- Authority
- CN
- China
- Prior art keywords
- phase extraction
- extraction column
- solid
- pressure
- liquid level
- 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.)
- Granted
Links
- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 202
- 239000007788 liquid Substances 0.000 claims abstract description 121
- 238000002347 injection Methods 0.000 claims abstract description 64
- 239000007924 injection Substances 0.000 claims abstract description 64
- 230000001276 controlling effect Effects 0.000 claims abstract description 36
- 238000004364 calculation method Methods 0.000 claims description 8
- 238000004590 computer program Methods 0.000 claims description 7
- 230000000903 blocking Effects 0.000 abstract description 8
- 239000000523 sample Substances 0.000 description 19
- 238000000605 extraction Methods 0.000 description 14
- 238000004891 communication Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 230000001629 suppression Effects 0.000 description 4
- 230000000875 corresponding Effects 0.000 description 3
- 230000001808 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 238000004422 calculation algorithm Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000003068 static Effects 0.000 description 2
- 238000005039 chemical industry Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drugs Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000802 evaporation-induced self-assembly Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000002452 interceptive Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000001172 liquid--solid extraction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 230000003287 optical Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05B—CONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
- G05B11/00—Automatic controllers
- G05B11/01—Automatic controllers electric
- G05B11/36—Automatic controllers electric with provision for obtaining particular characteristics, e.g. proportional, integral, differential
- G05B11/42—Automatic controllers electric with provision for obtaining particular characteristics, e.g. proportional, integral, differential for obtaining a characteristic which is both proportional and time-dependent, e.g. P.I., P.I.D.
Abstract
The invention provides a pressure control method and system for a solid-phase extraction column and electronic equipment, and relates to the field of solid-phase extraction column control. The method comprises the step of controlling the liquid level height in the solid-phase extraction column in real time according to a preset first output pressure value. And when the liquid level in the solid-phase extraction column reaches the first height threshold value for the first time, controlling the liquid level in the solid-phase extraction column in real time according to a preset second output pressure value. And when the liquid level in the solid-phase extraction column reaches the first height threshold value for the second time, controlling the liquid level in the solid-phase extraction column in real time according to a preset third output pressure value. And stopping the liquid injection operation of the solid phase extraction column when the liquid level in the solid phase extraction column reaches the first height threshold for the third time. The method adopts three-level pressure closed-loop control, improves the stability of pressure control, relieves the blocking condition of various solid-phase extraction columns, detects the liquid level height of the solid-phase extraction column through a double-layer needle structure, and effectively solves the problem of blocking treatment of the solid-phase extraction column.
Description
Technical Field
The invention relates to the field of solid-phase extraction column control, in particular to a pressure control method and system for a solid-phase extraction column and electronic equipment.
Background
The extraction mode of the prior full-automatic solid phase extraction equipment comprises negative pressure extraction and positive pressure extraction, wherein the negative pressure extraction only can reach 0.1MPa, so that the speed of liquid flowing through a solid phase extraction column is very slow, and the processing capacity is very weak particularly when the solid phase extraction column is blocked; the pressure of positive pressure extraction can reach more than 5 times of that of negative pressure extraction, but the positive pressure extraction also faces the problem of blockage of a solid phase extraction column.
In the prior art, two treatment modes are provided when a solid phase extraction column is blocked: one is to keep the speed of the injection pump to increase the pressure all the time, stop the action after the pressure reaches the set limit value, and wait for artificial treatment; the other method is that the liquid is filtered in one step before passing through the solid phase extraction column, and part of impurities are filtered, but the blockage caused by the quality problem of the solid phase extraction column cannot be guaranteed.
Disclosure of Invention
In view of the above, the present invention provides a method, a system, and an electronic device for controlling pressure of a solid-phase extraction column, which satisfy various blocking conditions of various solid-phase extraction columns by using three-stage closed-loop pressure control, thereby improving the stability of pressure control, and further, a double-layer sampling needle structure is adopted, and a liquid level sensor is used to effectively position the liquid level height, thereby forming closed-loop liquid level control, and effectively solving the problem of blocking treatment of the solid-phase extraction column.
In a first aspect, an embodiment of the present invention provides a method for controlling pressure of a solid phase extraction column, where the method includes:
acquiring first pressure deviation data of the solid-phase extraction column in real time according to a preset first output pressure value;
controlling the liquid level height in the solid phase extraction column according to the first pressure deviation data;
when the liquid level height in the solid-phase extraction column reaches a first height threshold value for the first time, acquiring second pressure deviation data of the solid-phase extraction column in real time according to a preset second output pressure value; controlling the liquid level height in the solid-phase extraction column according to the second pressure deviation data; the preset second output pressure value is greater than the preset first output pressure value;
when the liquid level in the solid-phase extraction column reaches the first height threshold for the second time, acquiring third pressure deviation data of the solid-phase extraction column in real time according to a preset third output pressure value; controlling the liquid level height in the solid-phase extraction column according to the third pressure deviation data; the preset third output pressure value is greater than the preset second output pressure value and reaches the maximum pressure value of the solid-phase extraction column;
stopping the liquid injection operation of the solid phase extraction column when the liquid level in the solid phase extraction column reaches the first height threshold for the third time; and when the liquid level height in the solid phase extraction column is reduced to a second height threshold value, the liquid injection operation of the solid phase extraction column is executed again.
In some embodiments, the step of controlling the liquid level in the solid-phase extraction column according to the pressure deviation data is implemented by a pid control model, which specifically includes:
acquiring pressure deviation data, wherein the pressure deviation data comprises a pressure deviation value and a pressure deviation change rate;
inputting the pressure deviation value and the pressure deviation change rate into an initialized PID control model for calculation to obtain a control result of the PID control model;
and controlling the liquid level height in the solid-phase extraction column according to the control result of the proportional-integral-derivative control model.
In some embodiments, the step of inputting the pressure deviation value and the pressure deviation change rate into the initialized pid control model for calculation is implemented by using the following equations:
in the above formula, u (n) is the control result of the pid control model; e is the pressure deviation value; ec (n) is the rate of change of pressure deviation; kp is a proportionality coefficient; ki is an integral coefficient; kd is a differential coefficient.
In some embodiments, the pid control model is divided into a plurality of fuzzy subsets according to a positive-negative relationship among the proportional coefficient, the integral coefficient, and the differential coefficient.
In some embodiments, the membership functions of the proportional coefficient, the integral coefficient and the differential coefficient are composed of a Z-type function, a trigonometric function and an S-type function.
In some embodiments, the first output pressure value is 0-33% of the maximum pressure value; the second output pressure value is 33-66% of the maximum pressure value; the third output pressure value is 66% -100% of the maximum pressure value.
In some embodiments, the first height threshold is higher than the second height threshold.
In a second aspect, an embodiment of the present invention provides a pressure control system for a solid phase extraction column, the system including: the pressure sensor and the liquid level sensor are connected with the main control unit; one end of the liquid level sensor is connected with a sample injection needle which is arranged in the solid phase extraction column;
one end of the main control unit is connected with the injection pump driving unit, and the injection pump is controlled by the injection pump driving unit to fill liquid into the solid-phase extraction column;
the pressure sensor is arranged between the injection pump and the solid-phase extraction column and is used for measuring the pressure in the solid-phase extraction column;
a proportional integral differential control model is arranged in the main control unit; the pid control model controls the pressure of the solid phase extraction column by the pressure control method of the solid phase extraction column as mentioned in the first aspect.
In a third aspect, an embodiment of the present invention provides an electronic device, including: a processor and a storage device; the storage device has stored thereon a computer program which, when executed by the processor, performs the steps of the method of pressure control of a solid phase extraction column described above.
In a fourth aspect, the embodiments of the present invention provide a computer-readable storage medium, on which a computer program is stored, where the computer program is executed by a processor to perform the steps of the pressure control method for a solid phase extraction column.
The embodiment of the invention has the following beneficial effects: the embodiment of the invention provides a pressure control method, a system and electronic equipment of a solid-phase extraction column. And when the liquid level in the solid-phase extraction column reaches a first height threshold for the first time, acquiring second pressure deviation data of the solid-phase extraction column in real time according to a preset second output pressure value. And controlling the liquid level height in the solid-phase extraction column according to the second pressure deviation data. Wherein the preset second output pressure value is larger than the preset first output pressure value. And when the liquid level in the solid-phase extraction column reaches the first height threshold for the second time, acquiring third pressure deviation data of the solid-phase extraction column in real time according to a preset third output pressure value. And controlling the liquid level height in the solid-phase extraction column according to the third pressure deviation data. And the preset third output pressure value is greater than the preset second output pressure value and reaches the maximum pressure value of the solid-phase extraction column. And stopping the liquid injection operation of the solid phase extraction column when the liquid level in the solid phase extraction column reaches the first height threshold for the third time. And performing liquid injection operation of the solid phase extraction column again until the liquid level height in the solid phase extraction column is reduced to a second height threshold value. The method adopts three-level pressure closed-loop control, meets various blocking conditions of various solid-phase extraction columns, further improves the stability of pressure control, can adopt a double-layer sample injection needle structure, can effectively position the liquid level height by being assisted by a liquid level sensor, forms liquid level closed-loop control, and effectively solves the problem of blocking treatment of the solid-phase extraction columns.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of a method for controlling the pressure of a solid phase extraction column according to an embodiment of the present invention;
FIG. 2 is a flowchart illustrating a step of controlling a liquid level in a solid phase extraction column according to pressure deviation data in a method for controlling a pressure of a solid phase extraction column according to an embodiment of the present invention;
FIG. 3 is a diagram illustrating a PID controller in the pressure control method for a solid phase extraction column according to an embodiment of the invention;
FIG. 4 is a schematic structural diagram of a pressure control system of a solid phase extraction column according to an embodiment of the present invention;
FIG. 5 is a diagram of a double-layer sampling needle structure in a pressure control system of a solid phase extraction column according to an embodiment of the present invention;
fig. 6 is a schematic structural diagram of an electronic device according to an embodiment of the present invention.
Icon:
401-a master control unit; 402-syringe pump drive unit; 403-syringe pump; 404-injection pump piston, 405-pressure sensor, 406-liquid level sensor, 407-SPE plunger, 408-double-layer sample injection needle, 409-SPE column and 410-SPE column packing; 41-outer wall, 42-insulating substance; 43-the inner wall of the sample injection needle; 101-a processor; 102-a memory; 103-a bus; 104-communication interface.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Solid-Phase Extraction (SPE) is a sample pretreatment technology developed in recent years, is developed by combining liquid-Solid Extraction and column liquid chromatography, is mainly used for separating, purifying and concentrating samples, can improve the recovery rate of analytes compared with the traditional liquid-liquid Extraction method, more effectively separates the analytes from interfering components, reduces the sample pretreatment process, is simple to operate, saves time and labor, and is widely applied to the fields of medicines, foods, environments, commercial inspection, chemical industry and the like.
The extraction mode of the prior full-automatic solid phase extraction equipment comprises negative pressure extraction and positive pressure extraction, wherein the negative pressure extraction only can reach 0.1MPa, so that the speed of liquid flowing through a solid phase extraction column is very slow, and the processing capacity is very weak particularly when the solid phase extraction column is blocked. The pressure of positive pressure extraction can reach more than 5 times of that of negative pressure extraction, but the positive pressure extraction also faces the problem of blockage of a solid phase extraction column.
In the prior art, two treatment modes are provided when a solid phase extraction column is blocked: one is to keep the speed of the injection pump to increase the pressure all the time, stop the action after the pressure reaches the set limit value, and wait for artificial treatment; the other mode is that the liquid is filtered in one step before passing through the solid phase extraction column, and part of impurities are filtered, but the blockage caused by the quality problem of the solid phase extraction column cannot be guaranteed.
In view of the above problems in the prior solid phase extraction, the present invention provides a method, a system and an electronic device for controlling the pressure of a solid phase extraction column, which can be applied in the solid phase extraction process and can be implemented by using related software or hardware, and will be described below by way of example.
To facilitate understanding of this embodiment, a detailed description will be given of a pressure control method of a solid phase extraction column disclosed in this embodiment of the present invention, which is illustrated in fig. 1 and includes:
step S101, acquiring first pressure deviation data of the solid-phase extraction column in real time according to a preset first output pressure value.
In a solid phase extraction device, a pressure sensor and a corresponding main control unit are usually provided, wherein the main control unit obtains the pressure in a solid phase extraction column through the connected pressure sensor.
The height of the solid phase extraction column needs to be controlled according to the flow rate set by a user, and the solid phase extraction column is realized by applying pressure to the solid phase extraction column through an injection pump arranged outside the solid phase extraction column. The applied pressure is controlled by a syringe pump drive unit connected to the master control unit.
The method comprises the steps of applying pressure to the interior of a solid-phase extraction column through a preset first output pressure value, obtaining the pressure in the solid-phase extraction column through a pressure sensor, and then calculating a pressure deviation value for controlling the liquid level height of the solid-phase extraction column.
And S102, controlling the liquid level height in the solid-phase extraction column according to the first pressure deviation data.
The first pressure deviation data measure whether the pressure in the solid-phase extraction column is normal or not, the acquisition frequency of the pressure deviation data is determined according to the actual situation, the faster the data acquisition frequency is, the faster the response can be made to the pressure deviation situation, but the faster the data acquisition frequency is, more data processing pressure can be brought; conversely, the slower the data acquisition frequency, the less data processing pressure, but the slower the response speed to pressure deviation conditions.
And acquiring pressure change data through the acquired first pressure deviation data, and controlling the injection pump to perform liquid injection operation on the solid-phase extraction column by the injection pump driving unit according to the change data, so that a preset first pressure value is reached in the solid-phase extraction column, and the height of the liquid level in the solid-phase extraction column is sequentially controlled.
Step S103, when the liquid level in the solid-phase extraction column reaches a first height threshold for the first time, acquiring second pressure deviation data of the solid-phase extraction column in real time according to a preset second output pressure value; controlling the liquid level height in the solid-phase extraction column according to the second pressure deviation data; the preset second output pressure value is larger than the preset first output pressure value.
When the filler in the solid phase extraction column is not completely activated, or the solid phase extraction column is blocked due to more liquid particles, the pressure in the solid phase extraction column is increased. And if the liquid level height in the solid-phase extraction column reaches the first height threshold value for the first time, setting the output pressure of the injection pump as a preset second output pressure, wherein the preset second output pressure value is greater than the preset first output pressure value. The pressure of the injection pump is increased, so that the liquid level in the solid-phase extraction column is reduced, and the liquid level height in the solid-phase extraction column is controlled by acquiring second pressure deviation data of the solid-phase extraction column in real time.
The setting of the first height threshold can be realized by arranging a related sensor with fixed height in the solid phase extraction column, for example, a probe is arranged in the solid phase extraction column, one side of the probe is connected with a liquid level sensor, the liquid level height of the solid phase extraction column can be detected in real time, and when the liquid level reaches the probe, the liquid level height in the solid phase extraction column can be indicated to reach the first height threshold.
Step S104, when the liquid level in the solid-phase extraction column reaches the first height threshold for the second time, acquiring third pressure deviation data of the solid-phase extraction column in real time according to a preset third output pressure value; controlling the liquid level height in the solid-phase extraction column according to the third pressure deviation data; and the preset third output pressure value is greater than the preset second output pressure value and reaches the maximum pressure value of the solid-phase extraction column.
And if the congestion condition in the solid-phase extraction column continues to develop, when the liquid level in the solid-phase extraction column reaches the first height threshold value for the second time, setting the output pressure of the injection pump as a preset third output pressure, wherein the preset third output pressure value is greater than the preset second output pressure value and reaches the maximum pressure value of the solid-phase extraction column. The pressure of the injection pump is increased, so that the liquid level in the solid-phase extraction column is reduced, and the liquid level height in the solid-phase extraction column is controlled by acquiring the third pressure deviation data of the solid-phase extraction column in real time. The above-described process is implemented similarly to step S103, and when the liquid level reaches the first height threshold again, the pressure of the syringe pump is output to the maximum value, so that the liquid level falls.
Step S105, stopping liquid injection operation of the solid phase extraction column when the liquid level in the solid phase extraction column reaches the first height threshold for the third time; and when the liquid level height in the solid phase extraction column is reduced to a second height threshold value, the liquid injection operation of the solid phase extraction column is executed again.
If the congestion condition in the solid-phase extraction column continues to develop, when the liquid level in the solid-phase extraction column reaches the first height threshold for the third time, the output pressure of the injection pump is the maximum output, so that the liquid injection operation of the solid-phase extraction column needs to be stopped, and the liquid level of the solid-phase extraction column continuously drops. And when the liquid level height in the solid phase extraction column is reduced to a second height threshold value, the liquid injection operation of the solid phase extraction column is executed again.
The second height threshold value can be set to be equal to the first height threshold value or be a value smaller than the first height threshold value, and the smaller the value of the threshold value is, the longer the liquid injection stopping time is; conversely, a larger value of the threshold value indicates a shorter time for stopping the injection.
In the method for controlling the pressure of the solid-phase extraction column according to the embodiment of the present invention, first pressure deviation data of the solid-phase extraction column is obtained in real time according to a preset first output pressure value, and then the liquid level in the solid-phase extraction column is controlled according to the first pressure deviation data. And when the liquid level in the solid-phase extraction column reaches a first height threshold for the first time, acquiring second pressure deviation data of the solid-phase extraction column in real time according to a preset second output pressure value. And controlling the liquid level height in the solid-phase extraction column according to the second pressure deviation data. Wherein the preset second output pressure value is larger than the preset first output pressure value. And when the liquid level in the solid-phase extraction column reaches the first height threshold for the second time, acquiring third pressure deviation data of the solid-phase extraction column in real time according to a preset third output pressure value. And controlling the liquid level height in the solid-phase extraction column according to the third pressure deviation data. And the preset third output pressure value is greater than the preset second output pressure value and reaches the maximum pressure value of the solid-phase extraction column. And stopping the liquid injection operation of the solid phase extraction column when the liquid level in the solid phase extraction column reaches the first height threshold for the third time. And performing liquid injection operation of the solid phase extraction column again until the liquid level height in the solid phase extraction column is reduced to a second height threshold value. The method adopts three-stage pressure closed-loop control, meets various blocking conditions of various solid-phase extraction columns, further improves the stability of pressure control, and effectively solves the problem of blocking treatment of the solid-phase extraction columns.
In some embodiments, the step of controlling the liquid level in the solid-phase extraction column according to the pressure deviation data is implemented by a pid control model, as shown in fig. 2, which specifically includes:
in step S201, pressure deviation data is acquired, and the pressure deviation data includes a pressure deviation value and a pressure deviation change rate.
By acquiring pressure deviation data at different times, a pressure deviation value and a pressure deviation change rate are calculated, specifically, as follows:
e＝p1-p2
wherein e is a pressure deviation value; ec is the pressure deviation change rate; p is a radical of1The pressure value at the first moment is taken as the pressure value; p is a radical of2The pressure value at the second moment; t is the interval between the first time and the second time.
Step S202, inputting the pressure deviation value and the pressure deviation change rate into the initialized PID control model for calculation, and obtaining a control result of the PID control model.
A proportional-integral-derivative control (proportional-integral-derivative control) model is a typical unit negative feedback control model, and the model is composed of a PID controller and a controlled object.
P in the PID model is proportional (proportionality) control. Proportional control is one of the simplest control methods. The output of the controller is proportional to the input error signal. There is a Steady-state error in the system output when there is only proportional control.
I in the PID model refers to integral (integral) control. In integral control, the output of the controller is proportional to the integral of the input error signal. For an automatic control System, if there is a Steady-state Error after entering a Steady state, the control System is called as a System with a Steady-state Error or a System with a difference Error for short. To eliminate steady state errors, an "integral term" must be introduced into the controller. The integral term integrates the error over time, increasing with time. Thus, even if the error is small, the integral term increases with time, which drives the output of the controller to increase further reducing the steady state error until it approaches zero. Therefore, the proportional Plus Integral (PI) controller can enable the system to have almost no steady-state error after the system enters the steady state.
D in the PID model is referred to as derivative (derivative) control. In the differential control, the output of the controller is in a proportional relationship with the differential of the input error signal (i.e., the rate of change of the error). The automatic control system may oscillate or even destabilize during the adjustment process to overcome the error. The reason for this is that the presence of a large inertia component (link) or a hysteresis (delay) component has the effect of suppressing the error, the variation of which always lags behind the variation of the error. The solution is to "lead" the change in the effect of the suppression error, i.e. when the error is close to zero, the effect of the suppression error should be zero. That is, it is often not sufficient to introduce a "proportional" term into the controller, which acts to amplify only the magnitude of the error, but to add a "derivative term" which predicts the tendency of the error to change, so that a controller with proportional + derivative can bring the control action of the suppressed error to zero or even negative in advance, thus avoiding severe overshoot of the controlled quantity. Therefore, for controlled objects with greater inertia or hysteresis, the proportional Plus Derivative (PD) controller can improve the dynamic characteristics of the system during adjustment.
Specifically, in some embodiments, the step of inputting the pressure deviation value and the pressure deviation change rate into the initialized pid control model for calculation is implemented by using the following equations:
in the above formula, u (n) is the control result of the pid control model; e is the pressure deviation value; ec (n) is the rate of change of pressure deviation; kp is a proportionality coefficient; ki is an integral coefficient; kd is a differential coefficient.
In the pid control model, the plurality of fuzzy subsets are divided according to the positive-negative relationship among the proportional coefficient, the integral coefficient and the differential coefficient.
For example, the fuzzy subset may be set to { negative large, negative medium, negative small, zero, positive small, positive medium, positive large }, and abbreviated as { NB, NM, NS, Z, PS, PM, PB }.
And step S203, controlling the liquid level height in the solid-phase extraction column according to the control result of the PID control model.
In the specific control process, the main control unit controls the action of the injection pump by controlling the injection pump driving unit according to the change of the U (n) value, and further controls the SPE column pressure to reach a preset pressure value.
The idea of PID parameter self-tuning is to find out the fuzzy relation between 3 parameters kp, ki, kd of the PID controller and the pressure deviation e and the pressure deviation change rate ec, detect e and ec continuously during operation, and modify 3 parameters on line according to the fuzzy control rule to meet different requirements of different e and ec on the controller parameters, so that the controlled object has good dynamic and static performances, and the structure diagram of the controller is as shown in FIG. 3.
The logic relationship of the control rule is as follows:
If(e is NB)then(kp is PB)(ki is Z)(kd is PS)；
If(e is NM)and(ec is NM)then(kp is PM)(ki is PS)(kd is PM)；
If(e is NM)and(ec is PM)then(kp is PM)(ki is PS)(kd is PM)；
If(e is NS)and(ec is NS)then(kp is PB)(ki is PB)(kd is PM)；
If(e is NS)and(ec is PS)then(kp is PB)(ki is PB)(kd is PM)；
If(e is PS)and(ec is NS)then(kp is PB)(ki is PB)(kd is PM)；
If(e is PS)and(ec is PS)then(kp is PB)(ki is PB)(kd is PM)；
If(e is PM)and(ec is NM)then(kp is PB)(ki is Z)(kd is PS)；
If(e is PM)and(ec is PM)then(kp is PB)(ki is Z)(kd is PS)；
If(e is PB)then(kp is PB)(ki is Z)(kd is PS)；
in some embodiments, the membership functions of the proportional coefficient, the integral coefficient and the differential coefficient are composed of a Z-type function, a trigonometric function and an S-type function.
Specifically, the membership functions of e, ec, kp, ki and kd are all composed of a Z-type function, a triangular function and an S-type function, and the membership functions of the variables are shown in the following table:
the resulting kp, ki and kd values were calculated by the following equations:
then the main control unit controls the action of the injection pump through the injection pump driving unit according to the change of the U (n) value, thereby controlling the pressure of the solid phase extraction column and further controlling the liquid level height in the solid phase extraction column.
In some embodiments, the first output pressure value is 0-33% of the maximum pressure value; the second output pressure value is 33-66% of the maximum pressure value; the third output pressure value is 66% -100% of the maximum pressure value.
Because three-level pressure control is adopted, the third pressure output value is greater than the second output pressure value, and the second output pressure value is greater than the first output pressure value, so that the third pressure value is taken as a pressure range according to one third of the maximum pressure value, and the three pressure values are set. Through adopting tertiary pressure closed-loop control, satisfy various jam situations of all kinds of solid phase extraction columns, and then improved pressure control's stability, the effectual problem of solving solid phase extraction column jam and handling.
According to the embodiment, the three parameters of kp, ki and kd in the PID algorithm can be corrected on line by controlling the fuzzy subset according to the PID model, the problem that the three parameters in the PID algorithm are required to be different due to different resistances of the SPE column is effectively solved, and the stability of pressure control is further improved.
Corresponding to the embodiment of the pressure control method for the solid phase extraction column, this embodiment further provides a pressure control system for the solid phase extraction column, as shown in fig. 4, the system includes:
a pressure sensor 405 and a liquid level sensor 406 connected to the main control unit 401; one end of the liquid level sensor 406 is connected to a double-layer sample injection needle 408, and the sample injection needle is arranged in an SPE column 409.
One end of the main control unit 401 is connected to a syringe pump driving unit 402, and a syringe pump 403 is controlled by the syringe pump driving unit 402 to fill the SPE column 409 with liquid.
A pressure sensor 405 is disposed between the syringe pump 403 and the SPE column 409 for measuring the pressure in the SPE column 409;
a proportional-integral-derivative control model is arranged in the main control unit 401; the pid control model controls the pressure of the solid phase extraction column by the pressure control method of the solid phase extraction column as mentioned in the first aspect, and the control principle and the technical effects are the same as those of the foregoing embodiments of the pressure control method of the solid phase extraction column.
Specifically, the pressure control system of the solid phase extraction column comprises: the system comprises a main control unit 401, a syringe pump driving unit 402, a syringe pump 403, a syringe pump piston 404, a pressure sensor 405, a liquid level sensor 406, an SPE plunger 407, a double-layer sample injection needle 408, an SPE column 409 and SPE column packing 410. The double-layer injection needle 408 is composed of an injection needle outer wall 41, an insulating material 42 and an injection needle inner wall 43, as shown in fig. 5. In order to calculate the position from the double-layer needle 408 to the liquid level, a conducting wire is respectively led to the liquid level sensor 406 on the outer wall 41 of the needle and the inner wall 43 of the needle, and the main control unit 401 detects the volume value between the inner wall and the outer wall of the needle through the liquid level sensor 406 and calculates the volume value.
The main control unit 401 is according to the flow rate that the user set up, the action of syringe pump piston 404 through syringe pump drive unit 402 control syringe pump 403, liquid in the syringe pump 403 can not touch double-deck injection needle 408 under normal circumstances, namely liquid can pass through SPE post 409 smoothly, SPE post filler 410 in SPE post 409 does not activate completely or cause the jam because liquid particle is more, pressure in SPE post 409 will grow, liquid just can touch double-deck injection needle 408 because can not flow out in time, and then trigger the change of level sensor 406 value, main control unit 401 can call fuzzy PID model, wherein SPE plunger 407 and double-deck injection needle 408 in close contact, guarantee that the pressure in SPE post 409 can bear the maximum default.
The specific implementation process is as follows:
the system automatically sets the output pressure to be 33% of the maximum preset value, detects the value of the pressure sensor 405 from time to time, obtains pressure values p1 and p2 twice before and after calculation of the fuzzy PID model, and calculates the pressure deviation e and the pressure deviation change rate ec, wherein e is p1-p2, and ec is de/dt.
The pressure deviation e and the pressure deviation change rate ec are brought into a fuzzy PID controller to obtain values of kp, ki and kd, fuzzy subsets of the fuzzy subsets are { negative large, negative middle, negative small, zero, positive small, positive middle and positive large }, and are abbreviated as { NB, NM, NS, Z, PS, PM and PB }, the idea of PID parameter self-tuning is to find out fuzzy relations among 3 parameters of the PID controller kp, ki and kd, the pressure deviation e and the pressure deviation change rate ec, continuously detect e and ec in operation, and modify the 3 parameters on line according to fuzzy control rules to meet different requirements of different e and ec on the controller parameters, so that a controlled object has good dynamic and static performances.
The resulting kp, ki and kd values are substituted into a digital PID function, which is as follows:
in the above formula, u (n) is the control result of the pid control model; e is the pressure deviation value; ec (n) is the rate of change of pressure deviation; kp is a proportionality coefficient; ki is an integral coefficient; kd is a differential coefficient.
The main control unit 401 controls the action of the injection pump piston 404 of the injection pump 403 through the injection pump driving unit 402 according to the change of the U (n) value, and further controls the pressure of the SPE column 409 to reach a preset pressure value;
detecting the value of the liquid level sensor 406, and if the liquid can not touch the double-layer sample injection needle 408, keeping the pressure value; if the liquid still can touch the double-layer sample injection needle 408, the system automatically sets the output pressure to be 66% of the maximum preset value, detects the value of the pressure sensor 405 from time to time, obtains pressure values p1 and p2 twice before and after calculation of the fuzzy PID model, and calculates the pressure deviation e and the pressure deviation change rate ec, wherein e is p1-p2, and ec is de/dt.
Detecting the value of the liquid level sensor 406 again, and if the liquid can not touch the double-layer sample injection needle 408, keeping the pressure value; if the liquid still can touch the double-layer sample injection needle 408, the system automatically sets the output pressure to be 100% of the maximum preset value, detects the value of the pressure sensor 405 from time to time, obtains pressure values p1 and p2 twice before and after calculation of the fuzzy PID model, and calculates the pressure deviation e and the pressure deviation change rate ec, wherein e is p1-p2, and ec is de/dt.
Detecting the value of the liquid level sensor 406 again, and if the liquid can not touch the double-layer sample injection needle 408, keeping the pressure value; if the liquid still can touch the double-layer sample injection needle 408, the action of the injection pump is stopped, and the value of the liquid level sensor 406 is detected from time to time until the liquid can not touch the double-layer sample injection needle 408.
The implementation principle and the technical effects of the pressure control system of the solid phase extraction column provided by the embodiment of the invention are the same as those of the embodiment of the pressure control method of the solid phase extraction column, and for the sake of brief description, corresponding contents in the embodiment of the method can be referred to where the embodiment is not mentioned.
The embodiment also provides an electronic device, a schematic structural diagram of which is shown in fig. 6, and the electronic device includes a processor 101 and a memory 102; the memory 102 is used for storing one or more computer instructions, and the one or more computer instructions are executed by the processor to implement the pressure control method of the solid phase extraction column.
The server shown in fig. 6 further includes a bus 103 and a communication interface 104, and the processor 101, the communication interface 104, and the memory 102 are connected through the bus 103.
The Memory 102 may include a high-speed Random Access Memory (RAM) and may also include a non-volatile Memory (non-volatile Memory), such as at least one disk Memory. Bus 103 may be an ISA bus, PCI bus, EISA bus, or the like. The bus may be divided into an address bus, a data bus, a control bus, etc. For ease of illustration, only one double-headed arrow is shown in FIG. 6, but that does not indicate only one bus or one type of bus.
The communication interface 104 is configured to connect with at least one user terminal and other network units through a network interface, and send the packaged IPv4 message or IPv4 message to the user terminal through the network interface.
The processor 101 may be an integrated circuit chip having signal processing capabilities. In implementation, the steps of the above method may be performed by integrated logic circuits of hardware or instructions in the form of software in the processor 101. The Processor 101 may be a general-purpose Processor, and includes a Central Processing Unit (CPU), a Network Processor (NP), and the like; the device can also be a Digital Signal Processor (DSP), an Application Specific Integrated Circuit (ASIC), a Field Programmable Gate Array (FPGA) or other Programmable logic device, a discrete Gate or transistor logic device, or a discrete hardware component. The various methods, steps, and logic blocks disclosed in the embodiments of the present disclosure may be implemented or performed. A general purpose processor may be a microprocessor or the processor may be any conventional processor or the like. The steps of the method disclosed in connection with the embodiments of the present disclosure may be directly implemented by a hardware decoding processor, or implemented by a combination of hardware and software modules in the decoding processor. The software module may be located in ram, flash memory, rom, prom, or eprom, registers, etc. storage media as is well known in the art. The storage medium is located in the memory 102, and the processor 101 reads the information in the memory 102 and completes the steps of the method of the foregoing embodiment in combination with the hardware thereof.
Embodiments of the present invention further provide a computer-readable storage medium, on which a computer program is stored, where the computer program, when executed by a processor, performs the steps of the method of the foregoing embodiments.
In the several embodiments provided in the present application, it should be understood that the disclosed system, apparatus, and method may be implemented in other ways. The above-described embodiments of the apparatus are merely illustrative, and for example, a division of a unit is merely a division of one logic function, and there may be other divisions when actually implemented, and for example, a plurality of units or components may be combined or integrated into another system, or some features may be omitted, or not executed. In addition, the shown or discussed mutual coupling or direct coupling or communication connection may be an indirect coupling or communication connection of devices or units through some communication interfaces, and may be in an electrical, mechanical or other form.
Units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units can be selected according to actual needs to achieve the purpose of the solution of the embodiment.
In addition, functional units in the embodiments of the present invention may be integrated into one processing unit, or each unit may exist alone physically, or two or more units are integrated into one unit.
The functions, if implemented in the form of software functional units and sold or used as a stand-alone product, may be stored in a non-volatile computer-readable storage medium executable by a processor. Based on such understanding, the technical solution of the present invention may be embodied in the form of a software product, which is stored in a storage medium and includes instructions for causing a computer device (which may be a personal computer, a server, or a network device) to execute all or part of the steps of the method according to the embodiments of the present invention. And the aforementioned storage medium includes: a U-disk, a removable hard disk, a Read-only Memory (ROM), a Random Access Memory (RAM), a magnetic disk or an optical disk, and other various media capable of storing program codes.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for controlling pressure in a solid phase extraction column, the method comprising:
acquiring first pressure deviation data of the solid-phase extraction column in real time according to a preset first output pressure value;
controlling the liquid level in the solid phase extraction column according to the first pressure deviation data;
when the liquid level height in the solid-phase extraction column reaches a first height threshold value for the first time, acquiring second pressure deviation data of the solid-phase extraction column in real time according to a preset second output pressure value; controlling the liquid level in the solid phase extraction column according to the second pressure deviation data; the preset second output pressure value is greater than the preset first output pressure value;
when the liquid level in the solid-phase extraction column reaches the first height threshold for the second time, acquiring third pressure deviation data of the solid-phase extraction column in real time according to a preset third output pressure value; controlling the liquid level in the solid phase extraction column according to the third pressure deviation data; the preset third output pressure value is greater than the preset second output pressure value and reaches the maximum pressure value of the solid-phase extraction column;
stopping liquid injection operation of the solid phase extraction column when the liquid level in the solid phase extraction column reaches a first height threshold for the third time; and when the liquid level height in the solid phase extraction column is reduced to a second height threshold value, the liquid injection operation of the solid phase extraction column is executed again.
2. The method of claim 1, wherein the step of controlling the liquid level in the solid phase extraction column based on the pressure deviation data is performed by a pid control model, comprising:
acquiring the pressure deviation data, wherein the pressure deviation data comprises a pressure deviation value and a pressure deviation change rate;
inputting the pressure deviation value and the pressure deviation change rate to the initialized PID control model for calculation to obtain a control result of the PID control model;
and controlling the liquid level height in the solid-phase extraction column according to the control result of the PID control model.
3. The method of claim 2, wherein the step of inputting the pressure deviation value and the pressure deviation change rate into the initialized pid control model is performed by the following equations:
in the above formula, u (n) is a control result of the pid control model; e is the pressure deviation value; e (n) is the rate of change of pressure deviation; kp is a proportionality coefficient; ki is an integral coefficient; kd is a differential coefficient.
4. The method according to claim 3, wherein the PID control model is divided into fuzzy subsets according to the positive and negative relations of the proportional coefficient, the integral coefficient and the differential coefficient.
5. The method of claim 3, wherein the membership functions of the proportionality coefficient, the integral coefficient and the differential coefficient are comprised of a Z-type function, a trigonometric function and an S-type function.
6. The method of claim 1, wherein said first output pressure value is 0-33% of a maximum pressure value; the second output pressure value is 33-66% of the maximum pressure value; the third output pressure value is 66% -100% of the maximum pressure value.
7. The method of claim 1, wherein the first height threshold is higher than the second height threshold.
8. A pressure control system for a solid phase extraction column, the system comprising: the pressure sensor and the liquid level sensor are connected with the main control unit; one end of the liquid level sensor is connected with a sample injection needle which is arranged in the solid phase extraction column;
one end of the main control unit is connected with an injection pump driving unit, and the injection pump is controlled by the injection pump driving unit to inject liquid into the solid-phase extraction column;
the pressure sensor is arranged between the injection pump and the solid phase extraction column and is used for measuring the pressure in the solid phase extraction column;
a proportional integral differential control model is arranged in the main control unit; the pid control model controls the pressure of the solid phase extraction column by a method as claimed in any one of claims 1 to 7.
9. An electronic device, comprising: a processor and a storage device; the storage device has stored thereon a computer program which, when executed by the processor, performs the method of any one of claims 1 to 7.
10. A computer-readable storage medium, on which a computer program is stored, which, when being executed by a processor, carries out the steps of the method according to any one of the claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911177334.5A CN110764407B (en) | 2019-11-26 | 2019-11-26 | Pressure control method and system of solid phase extraction column and electronic equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911177334.5A CN110764407B (en) | 2019-11-26 | 2019-11-26 | Pressure control method and system of solid phase extraction column and electronic equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110764407A true CN110764407A (en) | 2020-02-07 |
| CN110764407B CN110764407B (en) | 2022-12-23 |
Family
ID=69339583
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911177334.5A Active CN110764407B (en) | 2019-11-26 | 2019-11-26 | Pressure control method and system of solid phase extraction column and electronic equipment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110764407B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07275601A (en) * | 1994-04-08 | 1995-10-24 | Hitachi Ltd | Automatic solid-phase extracting apparatus with solid-phase extraction column reproducing function |
| CN102301219A (en) * | 2009-01-29 | 2011-12-28 | 株式会社日立高新技术 | Device for pretreating biological sample and mass spectrometer equipped with same |
| CN103105194A (en) * | 2011-11-11 | 2013-05-15 | 中核四〇四有限公司 | Pulsed extraction column parameter blowing measurement and interface control method |
| CN103649712A (en) * | 2011-07-08 | 2014-03-19 | 株式会社日立高新技术 | Solid phase extraction device and viscosity measurement device |
| CN106390517A (en) * | 2016-09-14 | 2017-02-15 | 济南海能仪器股份有限公司 | Control method of mechanical arm type solid phase extraction instrument |
| CN207317893U (en) * | 2017-09-04 | 2018-05-04 | 中国核电工程有限公司 | A kind of gas blow pipe structure for pulse extraction column level gauging |
| CN108279568A (en) * | 2017-12-29 | 2018-07-13 | 浙江中控软件技术有限公司 | Boundary position control method for Variable Composition slot |
| CN109018752A (en) * | 2018-07-05 | 2018-12-18 | 燕山大学 | A kind of gas shield device of serials control |
| CN109132000A (en) * | 2018-06-27 | 2019-01-04 | 燕山大学 | Pressure vessel nitrogen-filled packaging system with Staged cotrol |
-
2019
- 2019-11-26 CN CN201911177334.5A patent/CN110764407B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07275601A (en) * | 1994-04-08 | 1995-10-24 | Hitachi Ltd | Automatic solid-phase extracting apparatus with solid-phase extraction column reproducing function |
| CN102301219A (en) * | 2009-01-29 | 2011-12-28 | 株式会社日立高新技术 | Device for pretreating biological sample and mass spectrometer equipped with same |
| CN103649712A (en) * | 2011-07-08 | 2014-03-19 | 株式会社日立高新技术 | Solid phase extraction device and viscosity measurement device |
| CN103105194A (en) * | 2011-11-11 | 2013-05-15 | 中核四〇四有限公司 | Pulsed extraction column parameter blowing measurement and interface control method |
| CN106390517A (en) * | 2016-09-14 | 2017-02-15 | 济南海能仪器股份有限公司 | Control method of mechanical arm type solid phase extraction instrument |
| CN207317893U (en) * | 2017-09-04 | 2018-05-04 | 中国核电工程有限公司 | A kind of gas blow pipe structure for pulse extraction column level gauging |
| CN108279568A (en) * | 2017-12-29 | 2018-07-13 | 浙江中控软件技术有限公司 | Boundary position control method for Variable Composition slot |
| CN109132000A (en) * | 2018-06-27 | 2019-01-04 | 燕山大学 | Pressure vessel nitrogen-filled packaging system with Staged cotrol |
| CN109018752A (en) * | 2018-07-05 | 2018-12-18 | 燕山大学 | A kind of gas shield device of serials control |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110764407B (en) | 2022-12-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104271172B (en) | Choke detecting method | |
| CN104487117A (en) | Method and apparatus for detection and management of air-in-line | |
| WO2009085711A2 (en) | Dispense verification meters | |
| CN107592059A (en) | A kind of temperature protective device, method, storage medium and equipment | |
| CN110764407B (en) | Pressure control method and system of solid phase extraction column and electronic equipment | |
| CN103520786B (en) | A kind of control method of flow of blood purification peristaltic pump | |
| CN104076830A (en) | Mass flow control device, system and method used for integrated gas delivery system | |
| EP2876418A1 (en) | Optical flow measuring device and method of operation | |
| CN107569739B (en) | Detection method and device of capacitive sensor for detecting liquid in infusion tube | |
| CN103675025A (en) | Control circuit for use with four terminal sensors, and measurement system including such control circuit | |
| CN108981561B (en) | Air leakage hole determining method, vacuum motor and adsorbed article detection method thereof | |
| US10669911B2 (en) | Diesel exhaust fluid delivery system with pressure control | |
| JP4584849B2 (en) | Flocculant injection amount control method and control controller | |
| US11095270B2 (en) | Method for averaging pulsating measurement quantities | |
| WO2022179235A1 (en) | Cleaning robot control method and apparatus, cleaning robot, and storage medium | |
| US11033681B2 (en) | Automatic catheter recognition and associated methods, systems and circuits | |
| EP2990777B1 (en) | Device and method for detecting properties or the filling level of a medium in a vessel | |
| AU2015359241A1 (en) | A dispenser device and a method for rinsing the dispenser device | |
| CN102288835B (en) | Signal detection circuit and method | |
| JP4719622B2 (en) | Automatic analyzer | |
| US20220243714A1 (en) | Pump control based on bubble detection | |
| CN103480179B (en) | The liquid discharge control method of extraction tower light liquid phase, device, system and extraction equipment | |
| EP4036409A1 (en) | Flow rate control for pump with flow sensor | |
| JP7120438B2 (en) | Liquid chromatograph | |
| EP2980568A1 (en) | Device and method for detecting bubbles of vacuum container for manufacturing cosmetic contents, and recording medium for storing program code for executing method thereof by computer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |