CN113663364B - Chromatography device - Google Patents
Chromatography device Download PDFInfo
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- CN113663364B CN113663364B CN202010406963.7A CN202010406963A CN113663364B CN 113663364 B CN113663364 B CN 113663364B CN 202010406963 A CN202010406963 A CN 202010406963A CN 113663364 B CN113663364 B CN 113663364B
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- 238000004587 chromatography analysis Methods 0.000 title claims abstract description 62
- 239000007788 liquid Substances 0.000 claims abstract description 149
- 239000002253 acid Substances 0.000 claims abstract description 48
- 239000003513 alkali Substances 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000000872 buffer Substances 0.000 claims abstract description 18
- 230000001105 regulatory effect Effects 0.000 claims description 38
- 230000003750 conditioning effect Effects 0.000 claims description 14
- 238000011068 loading method Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 5
- 230000006378 damage Effects 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000011097 chromatography purification Methods 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/14—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the introduction of the feed to the apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/12—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the preparation of the feed
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
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- Molecular Biology (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
本发明公开了一种层析装置。该层析装置包括样品在线调节机构、样品储存机构、气泡陷阱机构以及层析机构，样品在线调节机构包括样品调节罐、搅拌组件、酸液进管、碱液进管、电导调节液进管、pH感应器以及电导感应器，样品调节罐上设置有样品进样口，酸液进管、碱液进管以及电导调节液进管均与样品调节罐连通，pH感应器以及电导感应器均与所述样品调节罐连接，搅拌组件与所述样品调节罐连接以实现对所述样品调节罐内的液体搅拌，所述样品储存机构、所述气泡陷阱机构以及所述层析机构依次顺序与所述样品调节罐连通，所述样品储存机构与所述气泡陷阱机构之间设置有层析缓冲液接口。该层析装置能够节时节力、提高层析效率、稳定性高。
The invention discloses a chromatography device. The chromatography device comprises a sample online adjustment mechanism, a sample storage mechanism, a bubble trap mechanism and a chromatography mechanism. The sample online adjustment mechanism comprises a sample adjustment tank, a stirring assembly, an acid inlet pipe, an alkali inlet pipe, a conductivity adjustment liquid inlet pipe, a pH sensor and a conductivity sensor. The sample adjustment tank is provided with a sample inlet port. The acid inlet pipe, the alkali inlet pipe and the conductivity adjustment liquid inlet pipe are all connected to the sample adjustment tank. The pH sensor and the conductivity sensor are both connected to the sample adjustment tank. The stirring assembly is connected to the sample adjustment tank to achieve stirring of the liquid in the sample adjustment tank. The sample storage mechanism, the bubble trap mechanism and the chromatography mechanism are connected to the sample adjustment tank in sequence. A chromatography buffer interface is provided between the sample storage mechanism and the bubble trap mechanism. The chromatography device can save time and labor, improve chromatography efficiency and has high stability.
Description
Technical Field
The invention relates to the technical field of biology, in particular to a chromatographic device.
Background
Many samples require conditioning of pH and conductivity prior to chromatographic purification, and in the prior art this conditioning is typically performed manually. For example, a certain amount of acidic or alkaline solution is added into the sample to reduce or increase the pH, the sample is diluted by a low-salt solution to reduce the conductivity of the sample, or a high-salt solution is added into the sample to increase the conductivity of the sample, the pH and the conductivity are sampled and detected after a certain amount of adjusting solution is added each time so as to prevent the pH and the conductivity from exceeding the target range, and chromatographic loading can be started after the sample is adjusted. The manual adjustment process is time consuming and laborious and increases the risk of sample contamination as well as the handling due to the inability to detect the pH and conductance of the sample in real time. Such manual adjustment is typically performed by adjusting the sample in tens of liters or hundreds of liters at a time, and the loading process typically takes several hours, which increases the risk of sample destruction if the sample is not stable under the pH and conductivity conditions required for loading. If a batch of samples is to be conditioned in batches, reducing the exposure time of the samples reduces the risk of sample damage, but this increases the number of manual operations and the amount of labor.
Disclosure of Invention
Accordingly, there is a need for a chromatography device that can save time and effort, improve the chromatography efficiency, and has high stability.
The utility model provides a chromatographic device, includes sample on-line adjustment mechanism, sample storage mechanism, bubble trap mechanism and chromatographic mechanism, sample on-line adjustment mechanism includes sample adjustment jar, stirring subassembly, acidizing fluid advance the pipe, alkali lye advances pipe, electric conductance adjustment liquid advances pipe, pH inductor and electric conductance inductor, be provided with the sample inlet on the sample adjustment jar, the acidizing fluid advance the pipe alkali lye advance the pipe and electric conductance adjustment liquid advances the pipe all with sample adjustment jar intercommunication, pH inductor and electric conductance inductor all with sample adjustment jar is connected, stirring subassembly with sample adjustment jar is connected in order to realize right liquid stirring in the sample adjustment jar, sample storage mechanism bubble trap mechanism with chromatographic mechanism in proper order with sample adjustment jar intercommunication, sample storage mechanism with still be provided with the chromatography buffer interface between the bubble trap mechanism.
In one embodiment, the sample on-line adjusting mechanism further comprises a sample inlet tube, and the sample inlet tube is communicated with the sample inlet.
In one embodiment, the sample on-line adjusting mechanism further comprises a pneumatic valve, and the acid liquid inlet pipe and/or the alkali liquid inlet pipe and/or the conductance adjusting liquid inlet pipe and/or the sample inlet pipe is provided with the pneumatic valve.
In one embodiment, the sample on-line adjusting mechanism further comprises a metering pump, and the metering pump is arranged on the acid liquid inlet pipe and/or the alkali liquid inlet pipe.
In one embodiment, the sample on-line adjusting mechanism further comprises a diaphragm pump, and the conductance adjusting liquid inlet pipe and/or the sample inlet pipe are/is provided with the diaphragm pump.
In one embodiment, an acid liquid drain port is arranged at one end of the acid liquid inlet pipe, which is close to the sample adjusting tank;
And/or an alkali liquor liquid outlet is arranged at one end of the alkali liquor inlet pipe, which is close to the sample regulating tank;
and/or one end of the conductance regulating liquid inlet pipe, which is close to the sample regulating tank, is provided with a conductance regulating liquid drain port;
and/or one end of the sample inlet pipe, which is close to the sample regulating tank, is provided with a sample liquid outlet.
In one embodiment, the sample conditioning tank is provided with a conditioning tank vent, and a pneumatic valve for opening or closing the conditioning tank vent is arranged at the conditioning tank vent.
In one embodiment, one or more of a bubble sensor, a pH sensor, a conductivity sensor, a pressure sensor and a diaphragm pump are arranged on the pipeline between the sample storage mechanism and the bubble trap mechanism.
In one embodiment, the bubble trap mechanism is communicated with the sample storage mechanism and the chromatography mechanism through a pneumatic valve group with a bypass function, and a plurality of liquid level sensors are arranged on the bubble trap mechanism.
In one embodiment, the chromatographic mechanism communicates with the bubble trap mechanism through a pneumatic valve block with bypass function.
In one embodiment, a flow meter and/or a pressure sensor is provided on the conduit between the bubble trap mechanism and the chromatographic mechanism.
In one embodiment, the liquid outlet end of the chromatographic mechanism is further provided with one or more of a UV detector, a pH sensor, a conductivity sensor and a multi-channel pneumatic valve group.
When the chromatographic device is used for chromatographic work, the time and the force are saved, the chromatographic efficiency is improved, and the stability is high. The invention solves the problems that the manual adjustment process in the traditional technology is time-consuming and labor-consuming, and the pH and the conductivity of the sample cannot be detected in real time, reduces the risk of sample pollution, avoids the condition that the sample is adjusted for tens of liters or more than tens of hundred liters at one time during the manual adjustment, saves a great amount of time, has high stability of the pH and the conductivity conditions required by sample loading, and reduces the risk of sample damage. The invention can realize continuous operation of a batch of samples, and can achieve the purposes of reducing the exposure time of the samples and reducing the risk of damaging the samples on the premise of not increasing the operation times and the labor capacity of the human beings.
When the chromatographic device is used, the corresponding pipelines are filled with the sample, the electric conduction regulating liquid, the acid liquid and/or the alkali liquid, then the sample, the electric conduction regulating liquid, the acid liquid and/or the alkali liquid enter the sample regulating tank according to the ratio tested in advance, the sample, the electric conduction regulating liquid, the acid liquid and/or the alkali liquid are stirred and mixed uniformly at a low speed, meanwhile, the pH sensor and the electric conduction sensor in the sample regulating tank detect in real time, the system program controls the adding amount of the sample, the adding amount of the electric conduction regulating liquid, the adding amount of the acid liquid and/or the adding amount of the alkali liquid to be finely adjusted according to the feedback data, and when the pH and the electric conduction reach the preset control range, the sample regulation is stopped. The sample adjustment tank is communicated with the sample storage mechanism, all adjusted samples enter the sample storage mechanism, the sample adjustment tank is disconnected with the sample storage mechanism, chromatography is started, loading starts, in the loading process, the sample adjustment tank starts to repeat the sample adjustment work, the adjusted samples enter the sample storage mechanism, the adjusted samples are always kept in the sample storage mechanism for loading, and meanwhile, the samples are adjusted in batches in the sample adjustment tank, so that the online adjustment and loading of the samples are realized until all the samples are adjusted, the adjustment and loading cycles are realized, and the online continuous chromatography work is realized.
Drawings
FIG. 1 is a schematic diagram of a chromatographic apparatus according to an embodiment of the invention.
Description of the reference numerals
10. The chromatography device comprises a chromatography device 100, a sample online regulating mechanism 101, a sample regulating tank 1011, a regulating tank vent, a 102, a stirring assembly, 103, a sample inlet pipe 1031, a sample liquid outlet port 104, a conductivity regulating liquid inlet pipe 1041, a conductivity regulating liquid outlet port 1041, a 105, an acid liquid inlet pipe 1051, an acid liquid outlet port 106a, 106b, 106c, a pH sensor 107a, 107b, 107c, a conductivity sensor 108, an alkali liquid inlet pipe 1081, an alkali liquid outlet port 109a, 109b, 109c, 109d, 109e, 109f, a pneumatic valve 110a, 110b, 110c, a diaphragm pump 111a, 111b, 111c, 111d, 111e, a flowmeter, 112a, 112b, a metering pump, 200, a sample storage mechanism 201, a storage vent 300, a bubble mechanism 301, a trap mechanism vent 302, a trap mechanism vent port 400, a chromatography mechanism 500a, 500b, a multi-channel valve set, 600a, 600b, a pressure sensor 700, a UV detector, 800b, a bypass function liquid level sensor interface 1100, a, 900, a buffer interface sensor, and a buffer.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
In the description of the present invention, it should be understood that terms such as "center," "upper," "lower," "bottom," "inner," "outer," and the like are used in the description of the present invention to indicate orientations or positional relationships based on the orientations or relationships shown in the drawings, and are merely used for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
It should be understood that the terms "first," "second," and the like are used herein to describe various information, but such information should not be limited to these terms, which are used merely to distinguish one type of information from another. For example, a "first" message may also be referred to as a "second" message, and similarly, a "second" message may also be referred to as a "first" message, without departing from the scope of the invention.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "connected," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, integrally connected, mechanically connected, electrically connected, directly connected, indirectly connected through intermediaries, and may be in communication with each other between two elements, i.e., when an element is referred to as being "fixed" to another element, it may be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to FIG. 1, a chromatography apparatus 10 is provided according to an embodiment of the present invention.
The chromatography apparatus 10 includes a sample in-line adjustment mechanism 100, a sample storage mechanism 200, a bubble trap mechanism 300, a chromatography mechanism 400, and a control mechanism. The control mechanism is electrically connected to the sample on-line conditioning mechanism 100, the bubble trap mechanism 300, and the chromatographic mechanism 400, and may be a PLC, PID, etc., which is not shown in fig. 1.
The sample online adjustment mechanism 100 comprises a sample adjustment tank 101, a stirring assembly 102, an acid liquid inlet pipe 105, an alkali liquid inlet pipe 108, a conductivity adjustment liquid inlet pipe 104, a pH sensor 106a and a conductivity sensor 107a. The sample adjustment tank 101 is provided with a sample inlet. The acid liquid inlet pipe 105, the alkali liquid inlet pipe 108 and the electric conduction adjusting liquid inlet pipe 104 are all communicated with the sample adjusting tank 101. The pH sensor 106a and the conductivity sensor 107a are connected to the sample adjustment tank 101. The stirring assembly 102, the pH sensor 106a and the conductivity sensor 107a are electrically connected with a control mechanism, and the control mechanism controls the addition amount of the sample, the addition amount of the conductivity regulating liquid, the addition amount of the acid liquid and/or the addition amount of the alkali liquid according to the data fed back by the pH sensor 106a and the conductivity sensor 107a for fine adjustment.
Further, a sample inlet 103 is connected to the sample inlet.
The acid liquid inlet pipe 105 is provided with a pneumatic valve 109c, the alkali liquid inlet pipe 108 is provided with a pneumatic valve 109f, and/or the conductance regulating liquid inlet pipe 104 is provided with a pneumatic valve 109b, and/or the sample inlet pipe 103 is provided with a pneumatic valve 109a. The pneumatic valves 109a, 109b, 109c, 109f may be electrically connected to a control mechanism.
In one embodiment, the chromatographic apparatus 10 further comprises a flow meter, wherein the flow meter 111a is disposed on the sample inlet tube 103, and the flow rate of the sample inlet tube 103 is monitored and controlled by the flow meter 111 a. And/or the flow meter 111b is provided on the conductance-adjusting liquid inlet pipe 104, and the flow rate of the conductance-adjusting liquid inlet pipe 104 is monitored and controlled by the flow meter 111 b. And/or the acid inlet pipe 105 is also provided with a flowmeter 111c, and the flow rate of the acid inlet pipe 105 is monitored and controlled by the flowmeter 111 c. And/or the alkali liquor inlet pipe 108 is provided with a flowmeter 111e, and the flow rate of the alkali liquor inlet pipe 108 is monitored and controlled by the flowmeter 111 e. The flow meters 111a, 111b, 111c, 111e may all be electrically connected to the control mechanism.
The agitation assembly 102 is connected to the sample conditioning tank 101 to effect agitation of the liquid within the sample conditioning tank 101. Further, the stirring assembly 102 includes a stirring paddle and a stirring motor electrically connected to the control mechanism. The stirring rake sets up in sample adjustment jar 101, and agitator motor installs the top of sample adjustment jar 101 and is connected with the stirring rake, and agitator motor is used for driving the stirring rake and rotates, and agitator motor's rotational speed is adjustable, controllable to make the rotational speed that can the stirring rake adjustable, controllable. The paddles and the stirring motor are not shown in fig. 1.
The sample storage mechanism 200, the bubble trap mechanism 300, and the chromatographic mechanism 400 are sequentially connected to the sample adjustment tank 101. Specifically, the sample storage mechanism 200 communicates with the sample adjustment tank 101, and the sample storage mechanism 200 communicates with the bubble trap mechanism 300 and the chromatographic mechanism 400 in this order through pipes.
Sample storage mechanism 200 may be a sample storage tank. When the device is arranged, the position of the sample storage mechanism 200 is arranged below the sample adjusting tank 101, so that the adjusted sample can enter the sample storage mechanism 200 under the action of gravity, a mechanical pump is not needed, and electric energy resources are saved. A pneumatic valve 109d is provided in the pipe between the sample adjustment tank 101 and the sample storage mechanism 200.
A chromatography buffer interface 1001 is provided between the sample storage mechanism 200 and the bubble trap mechanism 300, and the chromatography buffer interface 1001 is used for feeding a chromatography buffer. In one embodiment, there are a plurality of chromatography buffer interfaces 1001, and the plurality of chromatography buffer interfaces 1001 are in communication with the tubing between the sample storage mechanism 200 and the bubble trap mechanism 300 through the multi-channel pneumatic valve block 500 a.
Furthermore, an external liquid inlet mechanism can be arranged at the interface of the chromatographic buffer solution. Specifically, the liquid feeding mechanism is communicated with the pipeline between the sample storage mechanism 200 and the bubble trap mechanism 300 through the multi-channel pneumatic valve group 500 a. The multi-channel pneumatic valve block 500a communicates with the feed mechanism through a plurality of chromatography buffer interfaces 1001. The liquid inlet mechanism is used for pumping chromatographic buffer into the chromatographic buffer interface 1001 and the chromatographic mechanism 400, and the liquid inlet mechanism can be a syringe, a sample bottle, a sample pump communicated with the chromatographic buffer, and the like. In fig. 1, the liquid feeding mechanism is not shown. The liquid inlet mechanism may be a third-party environmental element, or may be a part of the chromatographic apparatus 10 of the present invention.
The bubble trap mechanism 300 has a trap mechanism exhaust port 301 and a trap mechanism drain port 302.
When the chromatographic device 10 is used for chromatographic work, the time and the force are saved, the chromatographic efficiency is improved, and the stability is high. The invention solves the problems that the manual adjustment process in the traditional technology is time-consuming and labor-consuming, and the pH and the conductivity of the sample cannot be detected in real time, reduces the risk of sample pollution, avoids the condition that the sample is adjusted for tens of liters or more than tens of hundred liters at one time during the manual adjustment, saves a great amount of time, has high stability of the pH and the conductivity conditions required by sample loading, and reduces the risk of sample damage. The invention can realize continuous operation of a batch of samples, and can achieve the purposes of reducing the exposure time of the samples and reducing the risk of damaging the samples on the premise of not increasing the number of manual operation and labor capacity.
In a specific example, the sample in-line conditioning mechanism 100 further includes a diaphragm pump. Wherein, the sample inlet pipe 103 is provided with a diaphragm pump 110a, and/or the conductance regulating liquid inlet pipe 104 is provided with a diaphragm pump 110b. The diaphragm pumps 110a, 110b may each be electrically connected to a control mechanism.
In a specific example, the acid liquid inlet pipe 105 is provided with an acid liquid outlet 1051 near the end of the sample adjustment tank 101. The purpose of the arrangement of the acid liquid discharge port 1051 is that the acid liquid inlet pipe 105 needs to be filled with acid liquid before the start of chromatography, and a small part of the acid liquid is discharged through the acid liquid discharge port 1051, so that the acid liquid inlet pipe 105 can be quickly confirmed to be filled with acid liquid. After the acid liquid inlet pipe 105 is filled with the acid liquid, the accuracy of adjustment can be improved, and the adjustment efficiency can be improved.
And/or, the alkali liquor inlet pipe 108 is provided with an alkali liquor drain 1081 near one end of the sample adjustment tank 101. The purpose of the arrangement of the lye drain 1081 is as follows, before the beginning of chromatography, the lye inlet tube 108 needs to be filled with lye, and the lye inlet tube 108 can be quickly confirmed by draining a small part through the lye drain 1081. After the alkali liquor inlet pipe 108 is filled with alkali liquor, the accuracy of adjustment can be improved, and the adjustment efficiency is improved.
And/or, the conductance-adjusting liquid inlet pipe 104 is provided with a conductance-adjusting liquid outlet 1041 near one end of the sample-adjusting tank 101. The purpose of the arrangement of the conductivity-adjusting liquid drain 1041 is that before the start of chromatography, the conductivity-adjusting liquid inlet pipe 104 needs to be filled with the conductivity-adjusting liquid, and a small portion is drained through the conductivity-adjusting liquid drain 1041, so that the filling of the conductivity-adjusting liquid inlet pipe 104 with the conductivity-adjusting liquid can be confirmed quickly. After the conductivity regulating liquid inlet pipe 104 is filled with the conductivity regulating liquid, the regulating precision can be improved, and the regulating efficiency can be improved.
And/or, the sample liquid outlet 1031 is arranged at one end of the sample inlet pipe 103 close to the sample regulating tank 101. The purpose of the arrangement of the sample liquid outlet 1031 is that the sample inlet tube 103 needs to be filled with the conductivity adjusting liquid before the start of chromatography, and a small portion is discharged through the sample liquid outlet 1031, so that the filling of the sample inlet tube 103 with the sample can be confirmed quickly. After the sample inlet pipe 103 is filled with the sample, the accuracy of adjustment can be improved, and the adjustment efficiency is improved.
In a specific example, the sample conditioning tank 101 is provided with a conditioning tank vent 1011. At the adjustment tank exhaust port 1011, a pneumatic valve 109e for opening or closing the adjustment tank exhaust port 1011 is provided. The sample storage mechanism 200 is provided with a storage vent 201.
In a specific example, the sample online adjustment mechanism 100 further includes a metering pump, which may be a high-precision metering pump. A metering pump 112a is provided on the acid inlet pipe 105. And/or the lye inlet pipe 108 is provided with a metering pump 112b. Metering pumps 112a, 112b may each be electrically connected to a control mechanism. The metering pumps 112a, 112b can accurately control the amount of acid or alkali liquor added, and can improve the accuracy and efficiency of adjustment.
In a specific example, one or more of the bubble sensor 1100, the pressure sensor 600a, and the diaphragm pump 110c are provided on a pipe between the sample storage mechanism 200 and the bubble trap mechanism 300. The bubble sensor 1100, the pressure sensor 600a, and the diaphragm pump 110c may be electrically connected to a control mechanism. Preferably, a bubble sensor 1100, a pressure sensor 600a, and a diaphragm pump 110c are provided on the pipe between the sample storage mechanism 200 and the bubble trap mechanism 300. The positions of the bubble sensor 1100, the pressure sensor 600a, and the diaphragm pump 110c may be adjusted as needed. Further, one or more of a pH sensor 106b and a conductivity sensor 107b are further disposed on the pipe between the sample storage mechanism 200 and the bubble trap mechanism 300, and the pH sensor 106b and the conductivity sensor 107b can be electrically connected to the control mechanism. Preferably, a pH sensor 106b and a conductivity sensor 107b are provided on the conduit between the sample storage mechanism 200 and the bubble trap mechanism 300.
A flow meter 111c is further provided on the pipe between the sample storage mechanism 200 and the bubble trap mechanism 300, and the flow rate on the pipe is monitored and controlled by the flow meter 111 c. The flow meter 111c may be electrically connected to the control mechanism.
In a specific example, bubble trap mechanism 300 communicates with sample storage mechanism 200 and chromatographic mechanism 400 through a bypass-enabled pneumatic valve block 800 a. The bubble trap mechanism 300 is provided with a plurality of liquid level sensors, at least one liquid level sensor is provided at the top of the bubble trap mechanism 300, and at least one liquid level sensor is provided at the bottom of the bubble trap mechanism 300. Preferably, referring to FIG. 1, an embodiment of the present invention shows two liquid level sensors 900a and 900b, wherein one liquid level sensor 900a is disposed at the top of the bubble trap mechanism 300 and one liquid level sensor 900b is disposed at the bottom of the bubble trap mechanism 300. The pneumatic valve set 800a with bypass function and the liquid level sensors 900a, 900a can be electrically connected with the control mechanism.
A pressure sensor 600b may be provided on the conduit between the bubble trap mechanism 300 and the chromatographic mechanism 400. The flow meter 111d may also be provided on the conduit between the bubble trap mechanism 300 and the chromatographic mechanism 400, the flow rate on the conduit being monitored and controlled by the flow meter 111 d. The pressure sensor 600b and the flow meter 111d may be electrically connected to the control mechanism.
In a specific example, the chromatographic mechanism 400 communicates with the bubble trap mechanism 300 through a bypass-enabled pneumatic valve block 800 b. The bypass function pneumatic valve block 800b may be electrically connected to a control mechanism.
In a specific example, the liquid outlet end of the chromatographic mechanism 400 is further connected to a UV detector 700, and the UV detector 700 is used for detecting the protein concentration in the liquid. The UV detector 700 may be electrically connected to a control mechanism.
In a specific example, the liquid outlet end of the chromatographic mechanism 400 is further provided with a liquid outlet 1002. The number of liquid outlets 1002 may be plural. When the number of the liquid outlets 1002 is plural, the liquid outlet end is communicated with the plurality of liquid outlets 1002 through the multi-channel pneumatic valve group 500 b. The chromatographic liquid after chromatography can flow out through any one of the liquid outlets 1002 through the multi-channel pneumatic valve group 500 b.
The conduit at the outlet end of the chromatographic mechanism 400 may also be provided with a conductivity sensor 107c and/or a pH sensor 106c. The conductivity sensor 107c and the pH sensor 106c may be electrically connected to the control mechanism.
The chromatographic apparatus 10 of the present invention, when operated by chromatography, comprises the steps of:
The sample inlet pipe 103, the electric conduction adjusting liquid inlet pipe 104, the acid inlet pipe 105 and the pneumatic valves 109a, 109b, 109c and 109f on the alkali liquid inlet pipe 108 are opened, the acid inlet pipe 105 is filled with acid liquid, a small part is discharged through the acid liquid outlet 1051, and the acid liquid inlet pipe 105 is quickly confirmed to be filled with acid liquid. The alkali liquor inlet pipe 108 is filled with alkali liquor, and a small part is discharged through the alkali liquor outlet 1081, so that the alkali liquor inlet pipe 108 is quickly confirmed to be filled with alkali liquor. The conductivity adjusting liquid inlet pipe 104 is filled with the conductivity adjusting liquid, and a small part is discharged through the conductivity adjusting liquid outlet 1041, so that the conductivity adjusting liquid inlet pipe 104 is quickly confirmed to be filled with the conductivity adjusting liquid. The sample inlet tube 103 is filled with the sample, and a small part is discharged through the sample liquid outlet 1031, so that the sample inlet tube 103 is quickly confirmed to be filled with the sample.
The conductivity regulating liquid, acid liquid and/or alkali liquid enter the sample regulating tank 101 according to the pre-tested proportion, and the stirring motor drives the stirring paddle to rotate at a low speed according to the preset rotating speed. The pH value and the electric conductivity of the sample in the sample regulating tank 101 are detected by the pH sensor 106a and the electric conductivity sensor 107a, the pH value and the electric conductivity data are fed back to the control mechanism in real time, the control mechanism compares the preset data, and when the pH value and the electric conductivity data exceed the preset control range, the adding amount of the sample, the adding amount of the electric conductivity regulating liquid, the adding amount of the acid liquid and/or the adding amount of the alkali liquid are finely adjusted, and the stirring motor keeps driving the stirring paddle to rotate at a low speed according to a preset rotating speed. The pH sensor 106a and the conductivity sensor 107a in the sample adjustment tank 101 detect in real time, and when the pH and the conductivity reach a preset control range, the sample adjustment is stopped.
The pneumatic valve 109d between the sample adjustment tank 101 and the sample storage mechanism 200 is opened, the sample in the sample adjustment tank 101 enters the sample storage mechanism 200 under the action of gravity, all the adjusted sample enters the sample storage mechanism 200, and the pneumatic valve 109d between the sample adjustment tank 101 and the sample storage mechanism 200 is disconnected.
The chromatography is started, and the liquid inlet mechanism starts to input the chromatography buffer liquid to the pipeline between the sample storage mechanism 200 and the bubble trap mechanism 300 through the chromatography buffer liquid interface 1001 and the multi-channel pneumatic valve group 500a, so that the mixing of the chromatography buffer liquid and the sample is realized. The chromatographic buffer solution is mixed with the sample to form a mixed solution, the mixed solution is detected by the bubble sensor 1100, the pH sensor 106b, the conductivity sensor 107b and the pressure sensor 600a, the mixed solution after detection reaches the bubble trap mechanism 300, the bubble trap mechanism 300 removes bubbles from the mixed solution, and the mixed solution after the bubbles are removed is detected by the pressure sensor 600b again. In the process of loading, the sample adjustment tank 101 starts to repeat the sample adjustment work again, and the adjusted sample enters the sample storage mechanism 200 for storage, so that the adjusted sample is always kept in the sample storage mechanism 200 for loading, and meanwhile, the sample adjustment tank 101 internally adjusts the sample in batches.
The mixed liquid processed by the bubble trap mechanism 300 and pressure-detected by the pressure sensor 600b enters the chromatography mechanism 400 to perform a chromatography process, and the flow rate of the mixed liquid entering the chromatography mechanism 400 can be monitored and controlled by the flow meter 111 d. After the chromatographic liquid is detected by the UV detector 700, the liquid is discharged through the multi-channel pneumatic valve group 500b, and the chromatographic liquid after chromatography can flow out through any one or a plurality of liquid outlets 1002 through the multi-channel pneumatic valve group 500 b.
In summary, when the chromatographic apparatus 10 of the present invention is used, the corresponding pipeline is filled with the sample, the conductivity-adjusting liquid, the acid solution and/or the alkali solution, then the sample, the conductivity-adjusting liquid, the acid solution and/or the alkali solution enter the sample-adjusting tank 101 according to the pre-tested proportion, and are stirred and mixed uniformly at a low speed, meanwhile, the pH sensor 106a and the conductivity sensor 107a in the sample-adjusting tank 101 detect in real time, the control mechanism controls the adding amount of the sample, the adding amount of the conductivity-adjusting liquid, the adding amount of the acid solution and/or the adding amount of the alkali solution according to the feedback data, and fine adjustment is performed, when the pH and the conductivity data fed back by the pH sensor 106a and the conductivity sensor 107a reach the preset range of the control mechanism, the sample adjustment is stopped. The sample adjustment tank 101 is in communication with the sample storage mechanism 200, and all of the adjusted sample enters the sample storage mechanism 200, and the sample adjustment tank 101 is disconnected from the sample storage mechanism 200. The chromatography starts, the liquid inlet mechanism and the chromatography mechanism 400 work, the liquid inlet mechanism starts to pump chromatography buffer liquid and mix with the sample and then enters the chromatography mechanism 400, in the working process of the chromatography mechanism, the sample adjusting tank 101 starts to repeat the sample adjusting work, the adjusted sample enters the sample storage mechanism 200, the sample storage mechanism 200 always keeps the adjusted sample for loading, and meanwhile, the sample adjusting tank 101 adjusts the sample in batches and at intervals, so as to realize the on-line adjustment and loading of the sample until all the samples are adjusted, so as to realize the cycle of adjustment and loading, and realize the on-line continuous chromatography work.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
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| CN118818961B (en) * | 2024-09-19 | 2025-02-11 | 杭州励贝电液科技有限公司 | A PID control method and system for proportional servo valve |
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