CN209784117U - System for measuring solubility of liquid sample in supercritical carbon dioxide - Google Patents
System for measuring solubility of liquid sample in supercritical carbon dioxide Download PDFInfo
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- CN209784117U CN209784117U CN201920563208.2U CN201920563208U CN209784117U CN 209784117 U CN209784117 U CN 209784117U CN 201920563208 U CN201920563208 U CN 201920563208U CN 209784117 U CN209784117 U CN 209784117U
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Abstract
The utility model relates to a measurement system of liquid sample solubility in supercritical carbon dioxide belongs to chemical industry check out test set technical field. Including the air supply, cooling system and autoclave, admission valve and discharge valve are installed to the autoclave, this measurement system is still including sweeping the gas circuit, the sample pipeline, liquid sample storage device, temperature regulation apparatus, plunger pump and vacuum pump, the air supply passes through cooling system, the plunger pump is connected to the admission valve of autoclave, temperature regulation apparatus is used for adjusting the temperature in the autoclave, sweep the gas circuit, the sample pipeline all is equipped with the on-off valve, the air supply is through sweeping the gas circuit, the on-off valve intercommunication autoclave of sweeping the gas circuit, liquid sample storage device passes through the sample pipeline, the on-off valve intercommunication autoclave of sample pipeline, vacuum pump connection the discharge valve of autoclave. The utility model discloses realized earlier row's air and then the sample in the measurement, avoided the loss of sample in row's air operation, improved measuring result's accuracy.
Description
Technical Field
the utility model relates to a measurement system of liquid sample solubility in supercritical carbon dioxide belongs to chemical industry check out test set technical field.
background
Supercritical fluid refers to a fluid having a temperature and pressure above the critical point. At present, most researches are carried out on carbon dioxide, and the supercritical carbon dioxide fluid has the advantages of no toxicity, incombustibility, relative cheapness, high dissolving capacity, recyclability, low critical point and the like. Because of the excellent characteristics of the supercritical carbon dioxide fluid, the supercritical carbon dioxide fluid is widely researched and applied in the fields of polymer science, pharmacy, preparation of ultrafine particles and the like, and the solubility of a substance in the supercritical carbon dioxide is basic data of the research fields, so that the test of the solubility of the substance in the supercritical carbon dioxide is particularly important.
in the prior art, for example, the schemes disclosed in the patent application of the invention in china (application publication No. CN 108112876 a) and the paper "photosensitive measurement of cloud point pressure of supercritical carbon dioxide-polymer system" (chinese scientific and technical paper, 2016, 11 months, juteng, etc.) entitled "a method for adding fat-soluble nutrient components to rice" all utilize the characteristic that the dissolving capacity of supercritical carbon dioxide fluid changes with pressure to test the solubility of sample substances in supercritical carbon dioxide. The testing principle is that a quantitative test sample is dissolved in high-pressure supercritical carbon dioxide, then the pressure of the carbon dioxide is gradually reduced, the dissolving capacity of the carbon dioxide is reduced, when the carbon dioxide solution is supersaturated, the test sample in the carbon dioxide is separated out, the solution system is in a turbid state, the pressure of the carbon dioxide is the cloud point pressure, and finally the solubility of the test sample in the supercritical carbon dioxide under the current pressure and temperature can be calculated according to the information of the mass of the added test sample, the volume of the autoclave, the cloud point pressure, the current temperature and the like.
the existing supercritical carbon dioxide solubility test method generally utilizes an autoclave with a window, and in the test process, the autoclave is opened firstly, a sample substance is added, then the autoclave is closed, an exhaust valve is opened, and excessive carbon dioxide is introduced to carry out system air exhaust operation. In the process, some test samples belong to volatile substances, and the particle size of some test samples is small and easy to diffuse, so that a part of the test samples are discharged from an exhaust valve along with the flow of air flow, so that the loss of the test samples is caused, meanwhile, carbon dioxide is discharged outwards in the process of reducing the pressure in the autoclave, so that the loss of the samples is caused, but the loss is not considered in the last calculation of the solubility, so that the actually calculated solubility of the supercritical carbon dioxide is higher than the true value, and the unreal and inaccurate test result is caused.
Therefore, how to improve the accuracy of the measurement result of the solubility of the liquid sample in the supercritical carbon dioxide is a technical problem to be solved urgently.
SUMMERY OF THE UTILITY MODEL
the utility model aims at providing a measurement system of liquid sample solubility among supercritical carbon dioxide to solve present supercritical carbon dioxide solubility and measure unsafe problem.
The utility model provides a measuring system for the solubility of liquid sample in supercritical carbon dioxide for solving the technical problems, which comprises an air source, a cooling system and a high-pressure autoclave, wherein the high-pressure autoclave is provided with an air inlet valve and an air outlet valve, the measuring system also comprises a purging gas circuit, a sample pipeline, a liquid sample storage device, a temperature regulating device, a plunger pump and a vacuum pump, the air source is connected to an air inlet valve of the autoclave through a cooling system and a plunger pump, the temperature adjusting device is used for adjusting the temperature in the autoclave, the purging gas circuit and the sample pipeline are both provided with an open-close valve, the gas source is communicated with the high-pressure kettle through the purging gas circuit and the open-close valve of the purging gas circuit, the liquid sample storage device is communicated with the high-pressure kettle through the sample pipeline and an opening and closing valve of the sample pipeline, and the vacuum pump is connected with an exhaust valve of the high-pressure kettle.
Preferably, one end of the sample pipeline is communicated with the inside of the high-pressure kettle through a sample pipeline opening and closing valve, and the other end of the sample pipeline is detachably connected with the liquid sample storage device in a sealing manner.
In the scheme, when in test, a quantitative liquid sample is firstly loaded into the liquid sample storage device, then the purging gas circuit is opened, the air source is used for directly purging and exhausting air in the high-pressure kettle, then the vacuum pump is used for pumping so as to reduce the pressure intensity in the high-pressure kettle, finally, the sample pipeline is opened, and the liquid sample in the liquid sample storage device is injected into the high-pressure kettle by utilizing the suction force generated by the air pressure difference. The whole process of this scheme has realized the operation of air exhaust earlier back appearance of advance, has avoided the loss of liquid sample in the air exhaust operation to the degree of accuracy of test result has been improved. Meanwhile, the content of air impurities in the autoclave can be further reduced by the negative pressure environment in the autoclave, the purity of carbon dioxide in the system is improved, and the accuracy of a test result is further improved. In addition, the negative pressure environment within the autoclave can also help to efficiently load the sample into the autoclave.
Further, the liquid sample storage device is vertically higher than the autoclave top position.
according to the scheme, the liquid sample storage device is arranged above the top of the high-pressure kettle, the speed of the liquid sample entering the high-pressure kettle is increased by utilizing gravity, and the working efficiency of the measuring system is improved.
Further, the liquid sample storage device is a sample injection syringe or an adjustable quantitative liquid feeder or a soft packaging bag, and is used for injecting or sucking the liquid sample into the autoclave.
The scheme provides a specific liquid sample feeding device scheme, wherein the soft packaging bag can be a silicone tube, a soft plastic tube and the like.
furthermore, the on-off valve of the purging gas circuit and the on-off valve of the sample pipeline are the same, the measuring system further comprises a three-way electromagnetic valve, the gas inlet of the three-way electromagnetic valve is respectively connected with the sample pipeline or the purging pipeline, and the gas outlet of the three-way electromagnetic valve is connected with the on-off valve and used for conducting the sample pipeline or the purging pipeline.
Specifically, the three-way electromagnetic valve is provided with a first air inlet, a second air inlet and an air outlet and is used for communicating a passage between the first air inlet and the air outlet or a passage between the second air inlet and the air outlet; the air source is connected with a second air inlet of the three-way electromagnetic valve; the liquid sample storage device is detachably connected with a second air inlet of the three-way electromagnetic valve; one end of the opening and closing valve is connected with the air outlet of the three-way electromagnetic valve, and the other end of the opening and closing valve is communicated with the high-pressure kettle.
the scheme provides a more excellent pipeline connection scheme, so that the gas circuit connection is more concise and efficient, and the working efficiency of the measuring system is improved while the system cost is reduced.
The autoclave comprises two observation windows, the photoelectric detector is connected with the processing unit through the signal amplification circuit and used for receiving detection light emitted by the light source and penetrating through the two observation windows of the autoclave, and the processing unit is used for judging whether the liquid sample is separated out or not according to the intensity change of the detection light.
The scheme judges whether the liquid sample is separated out according to the light intensity change of the detection light of the supercritical carbon dioxide, replaces the conventional mode of directly watching by human eyes, and improves the reliability and the authenticity of cloud point pressure judgment.
Furthermore, the measuring system also comprises a piston and a motor, wherein the piston is arranged in the autoclave body in a sliding and sealing manner along the central axis of the autoclave body and is used for changing the volume of the autoclave, and the motor is used for driving the piston to move up and down.
The autoclave in this scheme can come reciprocating of control piston through the motor, changes the cauldron internal pressure intensity size through the volumetric change of autoclave, has avoided the operation of using discharge valve pressure release, and then has avoided the loss of liquid sample.
further, the motor drives the piston to move up and down through a crank sliding block or an eccentric wheel.
Furthermore, the photoelectric detector is a photodiode, and the processing unit is a single chip microcomputer.
Furthermore, the signal amplification circuit comprises an operational amplifier, a first resistor, a second resistor, a first capacitor, a second capacitor and a third capacitor;
The positive pole of the photodiode is grounded, the negative pole of the photodiode is connected with the reverse input end of the operational amplifier, the forward input end of the operational amplifier is grounded, the output end of the operational amplifier is grounded sequentially through a first resistor, a point A and a third capacitor, the first capacitor is connected between the reverse input end and the output end of the operational amplifier, the second resistor and the second capacitor are connected between the reverse input end of the operational amplifier and the point A after being connected in parallel, and the point A is connected with the signal input pin of the single chip microcomputer.
The scheme provides a circuit connection scheme for detecting turbidity by using a photodiode.
The utility model has the advantages that:
the utility model is specially provided with a path of purging gas circuit and a path of sample pipeline, and utilizes the vacuum pump to form a negative pressure environment in the high-pressure kettle, so as to force the liquid sample in the liquid sample storage device to enter the high-pressure kettle, the proposal of the utility model can realize the operation of air exhaust and sample injection, finally avoid the loss of the sample in the test due to the air exhaust operation, improve the accuracy of the final measurement result, and simultaneously, in the process of manufacturing the negative pressure environment in the high-pressure kettle, the content of residual air in the high-pressure kettle is further reduced, the purity of carbon dioxide in the high-pressure kettle is improved, the accuracy of a final measurement result is further improved, and the technical problem that in the prior art, a volatile and easily-diffused sample is easily discharged from an exhaust valve along with the flow of air flow to cause inaccurate final measurement result is solved.
Drawings
Fig. 1 is a schematic structural diagram of embodiment 1 of the system for measuring the solubility of a liquid sample in supercritical carbon dioxide of the present invention:
Fig. 2 is a schematic structural diagram of embodiment 2 of the system for measuring the solubility of a liquid sample in supercritical carbon dioxide of the present invention:
Fig. 3 is a schematic structural diagram of embodiment 3 of the system for measuring the solubility of a liquid sample in supercritical carbon dioxide of the present invention:
Fig. 4 is a schematic structural diagram of embodiment 4 of the system for measuring the solubility of a liquid sample in supercritical carbon dioxide of the present invention:
Fig. 5 is a schematic diagram of the circuit connection of the photoelectric sensor in embodiment 4 of the system for measuring the solubility of the liquid sample in supercritical carbon dioxide.
Detailed Description
example 1
Fig. 1 shows an embodiment of a system for measuring solubility of a liquid sample in supercritical carbon dioxide, which specifically includes a carbon dioxide steel cylinder 1, a cooling system 2, a plunger pump 3, an air inlet valve 4, an autoclave 5, a front observation window 5-1, a rear observation window 5-2, a magnetic stirrer 5-3, an exhaust valve 6, a sample injector 7, a purge valve 8-1, a sample valve 9, and a vacuum pump 10.
One end of an air inlet valve 4, an air outlet valve 6, a purge valve 8-1 and one end of a sample injection valve 9 are all communicated with the inside of the autoclave body, and electromagnetic valves with controllable switches are adopted; the front observation window 5-1 and the rear observation window 5-2 are symmetrically arranged on the outer wall of the autoclave body at two sides of the central axis of the autoclave body 5, the material of the outer wall is sapphire glass, and the inner wall of the autoclave body 5 is also provided with a temperature sensor, a pressure sensor and a heating sheet which are respectively used for detecting the temperature and the pressure inside the autoclave body and adjusting the temperature inside the autoclave body.
The carbon dioxide steel cylinder 1 is respectively connected with one end of a cooling system 2 and one end of a purge valve 8-1, the other end of the cooling system 2 is connected with an air inlet valve 4 through a plunger pump, a sample injection injector 7 is in separable and sealed connection with a sample injection valve 9 through a sealing hose, and the air outlet end of an exhaust valve 6 is connected with the air inlet end of a vacuum pump 10. Wherein the cooling system in particular uses a refrigeration compressor for cooling the carbon dioxide flowing through.
Specifically, this embodiment includes three passages into the autoclave, which are respectively:
1. The carbon dioxide injection main channel consists of a carbon dioxide steel cylinder 1, a cooling system 2, a plunger pump 3 and an air inlet valve 4 and is used for injecting liquid carbon dioxide;
2. A purging air discharge passage consisting of a carbon dioxide steel cylinder 1 and a purging valve 8-1 is used for discharging air in the high-pressure kettle 5;
3. a sample channel consisting of a sample injector 7-a sample valve 9 for feeding a liquid sample into the autoclave 5 with the aid of a vacuum pump.
The following describes the working procedure of this example with benzene (liquid) as an example:
firstly, a sample injector 7 is detached, 10mL of carbon dioxide gas is collected, 13.13g (0.1 mol) of benzene is sucked, and then a sealing hose is connected with a purge valve 8-1;
Then, the purge air exhaust passage is opened, the carbon dioxide cylinder 1 blows carbon dioxide into the autoclave 5 and blows out the carbon dioxide from the exhaust valve 6, and the air in the autoclave is squeezed out, and generally, when the volume of the added carbon dioxide reaches more than 2 times of the volume of the autoclave, the air in the autoclave is considered to be exhausted;
Then, closing the air inlet valve 4 and the sample injection valve 9, opening the exhaust valve 6 and the vacuum pump 10, pumping the autoclave 5 into a low-pressure state, closing the exhaust valve 6, then opening a sample injection channel, extruding the sample injection syringe 7, completely sending liquid samples into the autoclave by using air pressure difference, and closing the sample injection valve 9; the low pressure state is relative to the atmospheric pressure outside the autoclave, and the most ideal condition is to be vacuumized;
Then, opening a carbon dioxide injection main channel, cooling the flowing carbon dioxide to below 5 ℃ by using a cooling system 2 to convert the carbon dioxide into liquid, pumping the liquid carbon dioxide into the autoclave by using a plunger pump, controlling the injection amount of the carbon dioxide to adjust the pressure in the autoclave to 12MPa, and adjusting the temperature in the autoclave to 60 ℃ by using a heating sheet on the outer side of the autoclave body to convert the carbon dioxide into a supercritical state;
Finally, a magnetic stirrer 5-3 is used to accelerate the dissolution of benzene in carbon dioxide, then the pressure in the kettle is reduced by exhausting the gas through an exhaust valve 6, when the carbon dioxide becomes turbid due to solute precipitation observed from a front observation window 5-1, the exhaust valve 6 is closed, the cloud point pressure at this time is recorded as 10.183MPa, the temperature in the kettle is recorded as 45 ℃, the current carbon dioxide density is 302.30g/L according to literature search, and the solubility of the liquid sample in the supercritical carbon dioxide at the current cloud point pressure and temperature is 0.3027 (mass) by combining the volume of the autoclave with 100mL, namely, the fact that 0.3027 g of benzene can be dissolved in each gram of carbon dioxide at the current temperature and pressure is shown.
Example 2
Fig. 2 shows an embodiment of a system for measuring solubility of a liquid sample in supercritical carbon dioxide according to the present invention, which is different from embodiment 1 in that a three-way solenoid valve 8-2 is used as a purge valve in this embodiment, and the three-way solenoid valve 8-2 has two air inlets and one air outlet for connecting a passage between a first air inlet and the air outlet or a passage between a second air inlet and the air outlet.
The carbon dioxide steel cylinder 1 is respectively connected with one end of a cooling system 2 and a second air inlet of a three-way electromagnetic valve 8-2, the other end of the cooling system 2 is connected with an air inlet valve 4 through a plunger pump, a sample injection injector 7 is in separable and sealed connection with a first air inlet of the three-way electromagnetic valve 8-2 through a sealing hose, an air outlet of the three-way electromagnetic valve 8-2 is connected with a sample injection valve 9, and an air outlet end of an exhaust valve 6 is connected with an air inlet end of a. Wherein the cooling system in particular uses a refrigeration compressor for cooling the carbon dioxide flowing through.
Specifically, this embodiment includes three passages into the autoclave, which are respectively:
1. the carbon dioxide injection main channel consists of a carbon dioxide steel cylinder 1, a cooling system 2, a plunger pump and an air inlet valve 4 and is used for injecting liquid carbon dioxide;
2. a purging air exhaust channel consisting of a carbon dioxide steel cylinder 1, a three-way electromagnetic valve 8-2 and a sample injection valve 9 is used for exhausting air in the high-pressure kettle 5;
3. the sample injection channel consists of a sample injection syringe 7, a three-way electromagnetic valve 8-2 and a sample injection valve 9 and is used for adding a liquid sample into the autoclave 5 with the help of a vacuum pump.
The following describes the working procedure of this example with benzene (liquid) as an example:
Firstly, a sample injector 7 is detached, 10mL of carbon dioxide gas is collected, 13.13g (0.1 mol) of benzene is sucked, and then a sealing hose is connected with a purge valve 8-1;
Then, the purge air exhaust passage is opened, the carbon dioxide cylinder 1 blows carbon dioxide into the autoclave 5 and blows out the carbon dioxide from the exhaust valve 6, and the air in the autoclave is squeezed out, and generally, when the volume of the added carbon dioxide reaches more than 2 times of the volume of the autoclave, the air in the autoclave is considered to be exhausted;
Then, closing the air inlet valve 4 and the sample injection valve 9, opening the exhaust valve 6 and the vacuum pump 10, pumping the autoclave 5 into a low-pressure state, closing the exhaust valve 6, then opening a sample injection channel, extruding the sample injection syringe 7, completely sending liquid samples into the autoclave by using air pressure difference, and closing the sample injection valve 9; the low pressure state is relative to the atmospheric pressure outside the autoclave, and the most ideal condition is to be vacuumized;
Then, opening a carbon dioxide injection main channel, cooling the flowing carbon dioxide to below 5 ℃ by using a cooling system 2 to convert the carbon dioxide into liquid, pumping the liquid carbon dioxide into the autoclave by using a plunger pump, controlling the injection amount of the carbon dioxide to adjust the pressure in the autoclave to 12MPa, and adjusting the temperature in the autoclave to 60 ℃ by using a heating sheet on the outer side of the autoclave body to convert the carbon dioxide into a supercritical state;
finally, a magnetic stirrer 5-3 is used to accelerate the dissolution of benzene in carbon dioxide, then the pressure in the kettle is reduced by exhausting the gas through an exhaust valve 6, when the carbon dioxide becomes turbid due to solute precipitation observed from a front observation window 5-1, the exhaust valve 6 is closed, the cloud point pressure at this time is recorded as 10.183MPa, the temperature in the kettle is recorded as 45 ℃, the current carbon dioxide density is 302.30g/L according to literature search, and the solubility of the liquid sample in the supercritical carbon dioxide at the current cloud point pressure and temperature is 0.3027 (mass) by combining the volume of the autoclave with 100mL, namely, the fact that 0.3027 g of benzene can be dissolved in each gram of carbon dioxide at the current temperature and pressure is shown.
Example 3
Fig. 3 shows an embodiment of the measuring system for the solubility of the liquid sample in the supercritical carbon dioxide according to the present invention, the difference between the embodiment and the embodiment 2 is that the embodiment also comprises an autoclave piston 5-4, a piston connecting rod 5-5, a motor 5-6 and a crank block structure 5-7, wherein, a high-pressure kettle piston 5-4 is connected with the inner wall of the high-pressure kettle in a sliding and sealing way, one end of a piston connecting rod 5-5 is connected with the high-pressure kettle piston 5-4, the other end is connected with a motor 5-6 through a crank sliding block structure 5-7, so as to convert the rotating torque of the motor 5-6 into a pulling force for driving the piston rod 5-5 to move up and down, the crank-slider structure 5-7 may also be an eccentric wheel structure or other structures capable of converting the rotational displacement of the motor into the up-and-down displacement of the piston rod.
in the embodiment, the motor 5-6 can directly control the autoclave piston 5-4 to move up and down so as to change the pressure in the autoclave, so that the air leakage and pressure reduction are not required to be carried out through the exhaust valve 6 in the test, and the loss of a sample is avoided.
Example 4
Fig. 4 shows an embodiment of the system for measuring the solubility of a liquid sample in supercritical carbon dioxide according to the present invention, which is different from embodiment 3 in that the embodiment further includes an LED light source 11, a photodiode 12, a signal amplification circuit, an MCU and an upper computer, wherein the LED light source 11 is located on one side of the front observation window 5-1, and the photodiode 12 is located on one side of the rear observation window 5-2. The LED light source 13 is connected with the MCU through a signal amplifying circuit, and the MCU is used for judging whether the liquid sample is separated out or not according to the strength change of the received electric signal. The MCU is also connected with each electromagnetic valve, the three-way electromagnetic valve, the motor, the temperature and pressure sensor, the heating sheet and the cooling system and used for controlling the working states of the electromagnetic valves, the three-way electromagnetic valve, the motor, the temperature and pressure sensor, the heating sheet and the cooling system, and meanwhile, the MCU is also communicated with the upper computer through the RS-485 communication module, receives a control command of the upper computer and sends result data to the upper computer. The specific connections are well known in the art and will not be described further herein.
Fig. 5 is a schematic diagram of a circuit connection of the photoelectric sensor of this embodiment, where a1 is an operational amplifier, D1 is a photodiode, R1 and R2 are resistors, C1, C2 and C3 are electrolytic capacitors, the MCU is an S32K144 chip of NXP, an anode of the photodiode is grounded, a cathode of the photodiode is connected to a reverse input terminal of the operational amplifier, a forward input terminal of the operational amplifier is grounded, an output terminal of the operational amplifier is grounded sequentially through a first resistor, a point a and a third capacitor, the first capacitor is connected between the reverse input terminal and the output terminal of the operational amplifier, the second resistor is connected in parallel with the second capacitor and then connected between the reverse input terminal of the operational amplifier and the point a, and the point a is connected to a signal input pin of the single chip microcomputer. Specific component parameters need to be selected according to the signal amplification factor, and a specific selection rule is common knowledge in the art and is not described herein.
In the above embodiments, the electromagnetic valve is specifically used as the valve controller, and of course, a mechanical valve may be used instead of the same function, and such a modification should fall within the scope of the present invention.
In the above-mentioned embodiment, specifically used advance the kind syringe as liquid sample injection device, can also use adjustable quantitative liquid feeder etc. can replace the use with the device that quantitative liquid sample pours into the autoclave into, this kind of deformation should fall into the utility model discloses an within the scope of protection.
In the above embodiment, the liquid sample injection device is used as the liquid sample storage device, and certainly, a simple storage container may be used to be hermetically connected to the sample pipeline, and the negative pressure environment in the autoclave is utilized to make the liquid sample in the storage container enter the autoclave, and certainly, in order to increase the entry rate of the sample, the height of the storage container may be set at a position above the top of the autoclave, in order to make the sample more easily enter the autoclave, a soft packing box may be used as the liquid sample storage device, and the soft packing box may deform under the action of atmospheric pressure to squeeze the sample into the autoclave, and specifically, a silicone tube, a soft plastic tube, and the like may be used.
in the above embodiments, the LED light source is used as the detection light source, and other light sources such as a laser can be used as well, and such a modification should fall within the scope of the present invention.
In the above embodiments, the photodiode is used as the photodetector, and other devices such as a photoelectric probe, a phototriode, etc. can be used as the photosensor, and such a modification should fall within the scope of the present invention.
In the above embodiments, a specific amplifying circuit is provided, and specifically, different amplifying circuits can be adopted according to different photodetectors, and this kind of deformation should fall within the protection scope of the present invention.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, it should be understood by those skilled in the art that: the invention can be modified or equivalent substituted for some technical features; without departing from the spirit of the present invention, it should be understood that the scope of the claims is intended to cover all such modifications and variations.
Claims (9)
1. A system for measuring the solubility of a liquid sample in supercritical carbon dioxide comprises a gas source, a cooling system and an autoclave, wherein the autoclave is provided with an air inlet valve and an air outlet valve,
This measurement system is still including sweeping gas circuit, sample pipeline, liquid sample storage device, temperature regulation apparatus, plunger pump and vacuum pump, the air supply passes through cooling system, plunger pump connection to the admission valve of autoclave, temperature regulation apparatus is used for adjusting the temperature in the autoclave, sweep the gas circuit the sample pipeline all is equipped with the on-off valve, the air supply passes through sweep the gas circuit the on-off valve intercommunication autoclave of sweeping the gas circuit, liquid sample storage device passes through the sample pipeline the on-off valve intercommunication autoclave of sample pipeline, vacuum pump connection the discharge valve of autoclave.
2. The system for measuring the solubility of a liquid sample in supercritical carbon dioxide as claimed in claim 1 wherein the liquid sample storage means is vertically higher than the autoclave top position.
3. the system for measuring the solubility of a liquid sample in supercritical carbon dioxide as claimed in claim 1, wherein the liquid sample storage device is a syringe or an adjustable quantitative liquid charger or a soft packaging bag for injecting or sucking the liquid sample into the autoclave.
4. the system for measuring the solubility of the liquid sample in the supercritical carbon dioxide according to any one of claims 1 to 3, wherein the open/close valve of the purging gas circuit and the open/close valve of the sample pipeline are the same open/close valve, the system further comprises a three-way electromagnetic valve, the gas inlet of the three-way electromagnetic valve is respectively connected with the sample pipeline or the purging pipeline, and the gas outlet of the three-way electromagnetic valve is connected with the open/close valve and used for conducting the sample pipeline or the purging pipeline.
5. The system for measuring the solubility of the liquid sample in the supercritical carbon dioxide as claimed in claim 4, further comprising a light source, a photodetector, a signal amplification circuit, and a processing unit, wherein the autoclave comprises two observation windows, the photodetector is connected to the processing unit through the signal amplification circuit and is configured to receive the detection light emitted by the light source and passing through the two observation windows of the autoclave, and the processing unit is configured to determine whether the liquid sample is precipitated according to the intensity variation of the detection light.
6. the system for measuring the solubility of the liquid sample in the supercritical carbon dioxide as claimed in claim 5, further comprising a piston and a motor, wherein the piston is slidably and hermetically arranged in the autoclave body along the central axis of the autoclave body and is used for changing the volume of the autoclave, and the motor is used for driving the piston to move up and down.
7. The system for measuring the solubility of the liquid sample in the supercritical carbon dioxide as claimed in claim 6, wherein the motor drives the piston to move up and down through a crank block or an eccentric wheel.
8. The system for measuring the solubility of a liquid sample in supercritical carbon dioxide as claimed in claim 5, wherein the photodetector is a photodiode and the processing unit is a single chip microcomputer.
9. The system for measuring the solubility of a liquid sample in supercritical carbon dioxide as claimed in claim 8, wherein the signal amplification circuit comprises an operational amplifier, a first resistor, a second resistor, a first capacitor, a second capacitor, and a third capacitor;
the positive pole of the photodiode is grounded, the negative pole of the photodiode is connected with the reverse input end of the operational amplifier, the forward input end of the operational amplifier is grounded, the output end of the operational amplifier is grounded sequentially through a first resistor, a point A and a third capacitor, the first capacitor is connected between the reverse input end and the output end of the operational amplifier, the second resistor and the second capacitor are connected between the reverse input end of the operational amplifier and the point A after being connected in parallel, and the point A is connected with the signal input pin of the single chip microcomputer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109932277A (en) * | 2019-04-24 | 2019-06-25 | 中国烟草总公司郑州烟草研究院 | The measurement method and system of liquid sample solubility in a kind of supercritical carbon dioxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109932277A (en) * | 2019-04-24 | 2019-06-25 | 中国烟草总公司郑州烟草研究院 | The measurement method and system of liquid sample solubility in a kind of supercritical carbon dioxide |
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