Element content expansion adsorption device, automatic control system, method and its application
By designing an element content expansion adsorption device and an automatic control system, accurate detection of elements with high and low content has been achieved, solving the problems of limited detection range and insufficient accuracy in existing technologies, and improving the detection capability of elemental analyzers.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- INST OF COAL CHEM CHINESE ACAD OF SCI
- Filing Date
- 2024-02-02
- Publication Date
- 2026-06-30
AI Technical Summary
Existing elemental analyzers have limited detection range when detecting samples with high C/N ratios, C/S ratios, H/N ratios, and H/S ratios, making it difficult to accurately detect low-content elements. Furthermore, conventional methods can easily lead to column overload, affecting detection accuracy and instrument utilization.
An element content expansion adsorption device and automatic control system were designed. Through two sample weighing checks, combined with image recognition and a temperature control system, accurate detection of elements at high and low concentrations can be achieved. The system includes a U-shaped expansion adsorption column, a solenoid three-way valve, a temperature controller, and a camera, enabling automated control of the adsorption and desorption processes.
It expands the detection range of the elemental analyzer, improves detection accuracy, ensures accurate determination of elements with extremely high or low content, reduces the risk of adsorption column overload, and improves the efficiency of instrument use.
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Figure CN118001881B_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of element analyzer detection, and specifically relates to an adsorption device for expanding element content, an automatic control system, a method and their applications. Background Art
[0002] Element analyzers adopt unique purge and trap column technology, with high precision, good stability, high automation, simple operation, no need to use harmful chemical reagents, small sample consumption, unparalleled durability and lifespan, etc., and are important means for detecting the content of organic elements such as carbon, hydrogen, oxygen, nitrogen, and sulfur.
[0003] With the transformation of the scientific research direction towards major national needs, the basic research in fields such as coal conversion liquefaction to produce oil, catalytic conversion of biomass to produce liquid fuels, preparation and application of carbon-based new materials such as carbonaceous additives, special carbon / graphite materials, and functional carbon materials has developed greatly, and correspondingly new challenges have been posed to analytical detection. The presence of nitrogen and sulfur in oil products causes harm to the environment and human body on the one hand, and is unstable and unfriendly during storage and processing, and can damage equipment on the other hand. The standard stipulates that the sulfur content in oil products is between 0.5 - 0.01%, and the nitrogen content is 0.04% or even lower. The presence of sulfur in carbon materials reduces the corrosion resistance, stability, and electrochemical performance of the materials, and the presence of nitrogen affects the mechanical properties of the materials. The sulfur content is controlled at 0.4% - 0.05%, or even lower; the nitrogen content is less than 0.02% (200 ppm).
[0004] The protein content in dairy products is an important indicator of the quality of dairy products. Thiocyanate in dairy products is toxic and harmful to the human body, and the content of this substance has also become an important indicator. The impact of ionizing radiation on the human body is studied through the changes in the total carbon and total nitrogen content in urine and blood. The common feature of these samples is that the water content is particularly high. For dairy products, the water content is 70 - 80%, the nitrogen content ≥ 0.46%, and the sulfur content less than 0.02% is qualified.
[0005] In view of the above samples having high C / N ratio, C / S ratio, H / N ratio, and H / S ratio, new challenges have been posed to analytical detection accordingly. Conventional element analyzers are inadequate when detecting certain samples. For elements with small sample weights and low contents, the quantitative lower limit cannot be reached, and the measurement is inaccurate. Large sample weights will cause the adsorption column of elements with high contents to be overloaded, resulting in detection failure. Therefore, conventional element analyzers and detection methods not only have certain limitations in the measurement range, but also cannot meet the requirements of the above sample analysis and detection in terms of detection accuracy, and further reduce the utilization rate of the instrument. Summary of the Invention
[0006] To address the shortcomings and deficiencies of existing elemental analyzers in the background art, we designed and constructed an extended adsorption column on the Vario EL CUBE elemental analyzer, which boasts low detection limits and high accuracy. We employed an image recognition-based automatic control system for this extended adsorption column to accurately detect the content of different elements in the same sample using two separate weighings of varying sizes, thus achieving accurate determination of carbon, hydrogen, nitrogen, and sulfur. The first weighing, with a smaller sample size, allows for accurate detection of high-content elements using conventional methods. The second weighing, with a larger sample size, ensures accurate detection of low-content elements. This second weighing causes overload on the water vapor or carbon dioxide adsorption column, which is then adsorbed by the extended adsorption column. This two-step process completes the accurate determination of carbon, hydrogen, nitrogen, and sulfur. Based on this concept, this invention provides an elemental content extended adsorption device, an automatic control system, a method, and its applications.
[0007] To achieve the above objectives, the present invention adopts the following technical solution: an element content expansion adsorption device, comprising a temperature control box, mainly composed of a box body and a cover plate. A wind box is installed at the bottom of the box body, and a fan is installed inside it via a bracket. A U-shaped expansion adsorption column is installed inside the box body via a mounting plate. A heating wire is wound around the U-shaped expansion adsorption column, and a first thermocouple is attached to the outer wall of the U-shaped expansion adsorption column. The heating wire and the first thermocouple are respectively connected to a temperature controller via cables, thereby forming an automatic temperature control system to provide the required operating temperature for the U-shaped expansion adsorption column. Ventilation holes are respectively opened on the two side walls of the box body, and partitions are respectively installed inside the two side walls. The two partitions are sealed to the two side walls of the box body to form two air inlets. Air inlets are respectively opened on both sides of the bottom plate of the box body. The air duct connects the air inlet chamber to the air box. A flow hole is provided on the bottom plate of the box, and a protective mesh cover is installed over the flow hole. A first electromagnetic three-way valve and a second electromagnetic three-way valve are respectively installed inside the box, with their first interfaces connected by a connecting pipe. The second interface of the first electromagnetic three-way valve is connected to one of the ball joints via an air inlet pipe, and an air inlet pipe is connected to the third interface of the first electromagnetic three-way valve. The second interface of the second electromagnetic three-way valve is connected to the other ball joint via an air outlet pipe, and an air outlet pipe is connected to the third interface of the second electromagnetic three-way valve. The two ball joints are respectively located at both ends of the U-shaped extended adsorption column. The air inlet pipe and the air outlet pipe connect the U-shaped extended adsorption column in series with the corresponding adsorption column in the elemental analyzer adsorption system via the ball joints.
[0008] As a further supplement to the above technical solution, a third electromagnetic three-way valve is provided on the air inlet pipe, and a purge pipe is provided on the unused interface of the third electromagnetic three-way valve for connecting to an external purge air source. A fourth electromagnetic three-way valve is provided on the air outlet pipe, and an vent pipe is provided on the unused interface of the fourth electromagnetic three-way valve, thereby forming a purge system for the U-shaped extended adsorption column.
[0009] As a further supplement to the above technical solution, the first electromagnetic three-way valve, the second electromagnetic three-way valve, the third electromagnetic three-way valve, and the fourth electromagnetic three-way valve are all located above the mounting plate. An electric heating rod and a second thermocouple are respectively installed in the box located above the mounting plate, and both are connected to the temperature controller through cables, thereby forming a constant temperature control system to prevent water vapor in the pipeline above the mounting plate from condensing, which could cause inaccurate detection or blockage of the electromagnetic valves and pipelines.
[0010] As a further explanation of the above technical solution, a handle is provided on the top of the box to facilitate the movement of the temperature control box by on-site experimental personnel.
[0011] An automatic control system for an element content expansion adsorption device includes an elemental analyzer and a matching elemental analyzer adsorption system. The data output port of the elemental analyzer is connected to the input port of the host computer via a data cable. The output port of the host computer is connected to the input port of the display screen via a signal cable. A camera and a temperature controller are connected to the controller via signal cables. The camera is mounted on the display screen and is used to capture images of the elemental analyzer's operating status. The first, second, third, and fourth electromagnetic three-way valves are connected to the signal output port of the controller via cables. The controller processes and identifies the images of the elemental analyzer's operating status and controls the four electromagnetic three-way valves to achieve a U-shaped... The system expands the helium purging and adsorption operation of the adsorption column. The electric heating rod and the second thermocouple are connected to the output and input terminals of the temperature controller via cables. The temperature controller compares the preset temperature with the real-time temperature collected by the second thermocouple and controls the electric heating rod to maintain a constant temperature in the space above the mounting plate. The output terminal of the temperature controller is connected to the heating wire via a cable, and its input terminal is connected to the first thermocouple via cables. Based on the element analyzer's operating status image recognized by the controller and the real-time temperature collected by the first thermocouple, the temperature controller controls the heating wire and fan according to the preset adsorption temperature and desorption stability, thereby achieving automated temperature control of the U-shaped expanded adsorption column during adsorption and desorption.
[0012] A method for an automatic control system of an element content expansion adsorption device, comprising the automatic control system of the element content expansion adsorption device described in the above technical solution, mainly including the following steps:
[0013] Step 1: Connect the U-shaped extended adsorption column to the front end of the corresponding adsorption column in the elemental analyzer adsorption system, start the elemental analyzer, and the temperature controller controls the electric heating rod to heat according to the temperature collected by the second thermocouple, so as to maintain a constant temperature in the space above the mounting plate and prevent the pipeline from being condensed by cold water vapor during the adsorption process.
[0014] Step 2: When the camera captures the "Autozero delay" message following "wait for N peaks end" on the element analyzer's operating status, the controller's image recognition software automatically controls the first and second electromagnetic three-way valves to connect and disconnect the U-shaped extended adsorption column from the element analyzer's adsorption system. Simultaneously, it controls the third and fourth electromagnetic three-way valves to connect the U-shaped extended adsorption column to the purge tube and the vent tube, respectively. At the same time, the temperature controller starts the program to raise the temperature and meet the preset desorption temperature, causing the gas adsorbed on the absorbent in the U-shaped extended adsorption column to desorb and be discharged through the vent tube using inert gas purging, thus completing the desorption operation.
[0015] Step 3: When the camera captures the "H2O way off" message on the element analyzer's operating status screen, the controller's image recognition software automatically controls the third and fourth electromagnetic three-way valves to disconnect the U-shaped extended adsorption column from the purge tube and vent tube, respectively. Simultaneously, it controls the first and second electromagnetic three-way valves to disconnect the connecting tube and reconnect the U-shaped extended adsorption column to the element analyzer's adsorption system. At the same time, the temperature controller starts its cooling program to reach the preset adsorption temperature, allowing the gas in the element analyzer's adsorption system to be adsorbed by the absorbent in the U-shaped extended adsorption column, thus completing the adsorption operation.
[0016] Step four: When the camera captures the "Autozero delay" message following "wait for N peaks end" on the elemental analyzer's operating status again, the controller and temperature controller execute the instructions from step two to desorb the gas adsorbed by the U-shaped extended adsorption column in step three. Step two and step three are repeated to realize the desorption and adsorption process of the U-shaped extended adsorption column.
[0017] An elemental analyzer includes an element content expansion adsorption device as described above, used to expand the measurement range and improve detection accuracy.
[0018] An automatic control system for an extended adsorption column of an elemental analyzer includes an automatic control system for an elemental content extended adsorption device as described in the above technical solution. This system is used for the automatic operation of the elemental analyzer, adsorbing excess gas through a U-shaped extended adsorption column, and promptly purging with inert gas at high temperature to desorb the adsorbed gas, thus ensuring the cyclic use of the extended adsorption column.
[0019] An extended detection method for an elemental analyzer includes an automatic control system method for an element content extension adsorption device as described in the above technical solution, used to extend the element detection range of the elemental analyzer and meet the requirements for accurate detection of high and low content elements in samples with extremely high or extremely low element content.
[0020] Compared with the prior art, the present invention has the following advantages:
[0021] 1. This invention uses a ball-and-bowl quick-connect fitting connected in series with the front end of the corresponding adsorption column in the elemental analyzer's adsorption system, thus connecting the U-shaped extended adsorption column in series within the system. During the elemental analyzer's operation, this promptly adsorbs gases that could overload the adsorption column. Therefore, this invention ensures accurate detection of elements in samples containing extremely high or low concentrations; it also allows for the easy installation and removal of the extended adsorption system during testing, enabling the detection of high-concentration elements with small injection volumes and low-concentration elements with large injection volumes via the extended adsorption column.
[0022] 2. This invention adds an element content expansion adsorption device to the elemental analyzer. For samples containing extremely high and extremely low content elements, the high content element content is detected by the conventional sample injection volume of the elemental analyzer, and then the expansion adsorption automatic control system is used to increase the sample injection volume to accurately detect the low content element. The accurate detection of the content of extremely high and extremely low content elements in a sample is completed through two detections.
[0023] 3. This invention adds an image recognition system composed of a camera and a controller. The controller identifies key samples based on the operating status of the elemental analyzer captured by the camera. The image recognition software identifies time nodes and automatically controls the three-way valve to automatically disconnect or connect the U-shaped extended adsorption column with the corresponding adsorption column in the elemental analyzer adsorption system, so that the adsorption and desorption processes of the U-shaped extended adsorption column can be automated.
[0024] 4. This invention installs two electromagnetic three-way valves on the inlet and outlet gas pipes, and uses an image recognition system to adsorb overloaded gas in the U-shaped extended adsorption column. Inert gas is then used to purge the gas that has been desorbed at high temperature, thus satisfying the requirement for cyclic use of the U-shaped extended adsorption column.
[0025] 5. This invention adds a programmed heating and cooling automatic control system consisting of a temperature controller, thermocouple, heating wire, and fan. The temperature controller starts the programmed heating control system according to the time node identified by the image recognition software to ensure that the extended adsorption column reaches the adsorption and desorption temperature of the adsorbent in a timely and accurate manner, thus ensuring the accuracy of the detection data.
[0026] 6. This invention adds a constant temperature control system consisting of an electric heating rod, a second thermocouple, and a temperature controller to maintain a constant temperature in the space above the mounting plate, preventing water vapor condensation in the pipeline, which could cause blockage of the pipeline and solenoid valve, thereby affecting the detection accuracy of the elemental analyzer.
[0027] 7. This invention is not only applicable to H2O adsorption columns and CO2 adsorption columns of elemental analyzers, but can also be applied to SO2 adsorption columns by changing the extended adsorption connection points and the adsorbent in the U-shaped extended adsorption column and adjusting the time node of image recognition.
[0028] 8. This invention, through the modification of the elemental analyzer, not only expands the measurement range and improves the detection accuracy, but also enhances the efficiency of the instrument. Crucially, it can solve the analytical and detection problems in coal conversion and liquefaction, chemical liquefaction to liquid fuels, and carbon material research for research institutes and enterprises both inside and outside the institute. Attached Figure Description
[0029] Figure 1 This is a perspective view of the element content expansion adsorption device in this invention;
[0030] Figure 2 This is a structural diagram of the element content expansion adsorption device in this invention;
[0031] Figure 3 This is a top view of the element content expansion adsorption device in this invention;
[0032] Figure 4 This is a sectional view and internal structure diagram of section AA in the figure;
[0033] Figure 5 This is a front view of the internal structure of the element content expansion adsorption device in this invention;
[0034] Figure 6 This is a structural diagram of the automatic control system of the element content expansion adsorption device in this invention;
[0035] Figure 7 This is a control diagram of the automatic control system of the element content expansion adsorption device in this invention;
[0036] Figure 8 This is a diagram showing the adsorption process of the H2O adsorption extension column and the CO2 adsorption extension column in the elemental analyzer of this invention.
[0037] Figure 9 This is a diagram showing the desorption process of the H2O adsorption extension column and the CO2 adsorption extension column in the elemental analyzer of this invention.
[0038] Figure 10 This is a flowchart illustrating the adsorption and desorption processes of the element content expansion adsorption device in this invention.
[0039] In the diagram: 1. Temperature control box; 2. Handle; 3. Air box; 4. Bracket; 5. Fan; 6. Protective mesh cover; 7. Mounting plate; 8. Partition; 9. Air inlet chamber; 10. Air inlet slot; 11. U-shaped extended adsorption column; 12. Heating wire; 13. First thermocouple; 14. Electric heating rod; 15. Second thermocouple; 16. Ball-and-socket connector; 17. First electromagnetic three-way valve; 18. Second electromagnetic three-way valve; 19. Air inlet connecting pipe; 20. Air outlet connecting pipe; 21. Air inlet connecting pipe; 23. Connecting pipe; 24. Third electromagnetic three-way valve; 25. Purge pipe; 26. Fourth electromagnetic three-way valve; 27. Exhaust pipe; 28. Elemental analyzer adsorption system; 29. Elemental analyzer; 30. Main unit; 31. Display screen; 32. Camera; 33. Controller; 34. Temperature controller; 35. Temperature Controller.
[0040] The temperature control box includes: a box body (101), a cover plate (102), and ventilation holes (103). Detailed Implementation
[0041] To further illustrate the technical solution of the present invention, the following description is in conjunction with the appendix. Figures 1 to 10 Based on the actual implementation situation, we will further illustrate the present invention through the following embodiments.
[0042] As attached Figures 1 to 5As shown, an element content expansion adsorption device includes a temperature control box 1, which mainly consists of a box body 101 and a cover plate 102. A handle 2 is provided on the top of the box body 101 for easy movement by on-site personnel. A bellows 3 is provided at the bottom of the box body 101, and a fan 5 is installed inside through a bracket 4. A U-shaped expansion adsorption column 11 is installed inside the box body 101 through a mounting plate 7. An electric heating wire 12 is wound around the U-shaped expansion adsorption column 11. A first thermocouple 13 is attached to the outer wall of the U-shaped expansion adsorption column 11. The heating wire 12 and the first thermocouple 13 are respectively connected to the temperature controller 34 through cables, thus forming an automatic temperature control system to provide the required working temperature for the U-shaped expansion adsorption column 11. Ventilation holes 103 are respectively opened on the two side walls of the box 101, and partitions 8 are respectively installed inside the two side walls. The two partitions 8 are respectively sealed with the two side walls of the box 101 to form two air inlets 9. On the bottom plate of the box 101, two... The sides are provided with air inlet slots 10, which connect the air inlet chamber 9 to the air box 3. A flow hole is provided on the bottom plate of the box 101, and a protective mesh cover 6 is provided on the flow hole. A first electromagnetic three-way valve 17 and a second electromagnetic three-way valve 18 are respectively provided in the box 101, and their first interfaces are connected by a connecting pipe 23. The second interface of the first electromagnetic three-way valve 17 is connected to one of the ball joints 16 through an air inlet connecting pipe 19. An air inlet pipe 21 is connected to the third interface of the first electromagnetic three-way valve 17. The second interface of the second electromagnetic three-way valve 18 is connected to the other ball joint 16 through an air outlet connecting pipe 20. An air outlet pipe 22 is connected to the third interface of the second electromagnetic three-way valve 18. The two ball joints 16 are respectively set at both ends of the U-shaped extended adsorption column 11. The air inlet pipe 21 and the air outlet pipe 22 connect the U-shaped extended adsorption column 11 in series with the front end pipe of the corresponding adsorption column in the elemental analyzer adsorption system 28 through the ball joints 16.
[0043] As a preferred embodiment of the above embodiments, a third electromagnetic three-way valve 24 is provided on the air inlet pipe 19, and a purge pipe 25 is provided on the unused interface of the third electromagnetic three-way valve 24 for connecting to an external purge air source. A fourth electromagnetic three-way valve 26 is provided on the air outlet pipe 20, and an vent pipe 27 is provided on the unused interface of the fourth electromagnetic three-way valve 26, thereby forming a purge system for the U-shaped extended adsorption column 11.
[0044] In a preferred embodiment of the above embodiments, the first electromagnetic three-way valve 17, the second electromagnetic three-way valve 18, the third electromagnetic three-way valve 24, and the fourth electromagnetic three-way valve 26 are all located above the mounting plate 7. An electric heating rod 14 and a second thermocouple 15 are respectively installed in the housing 101 located above the mounting plate 7, and both are connected to the temperature controller 35 through cables, thereby forming a constant temperature control system to prevent water vapor in the pipeline above the mounting plate 7 from condensing, which could cause inaccurate detection or blockage of the electromagnetic valves and pipelines.
[0045] like Figure 6 As shown, an automatic control system for an element content expansion adsorption device includes an elemental analyzer 29 and a matching elemental analyzer adsorption system 28. The data output port of the elemental analyzer 29 is connected to the input port of the host 30 via a data cable. The output of the host 30 is connected to the input of the display screen 31 via a signal cable. A camera 32 is connected to the controller 33 and the temperature controller 34 via signal cables. The camera 32 is mounted on the display screen 31 and is used to capture images of the operating status of the elemental analyzer 29. The first electromagnetic three-way valve 17, the second electromagnetic three-way valve 18, the third electromagnetic three-way valve 24, and the fourth electromagnetic three-way valve 26 are connected to the signal output of the controller 33 via cables. The controller 33 processes and identifies the images of the operating status of the elemental analyzer 29 and controls the four electromagnetic three-way valves to operate. The helium purging and adsorption of the U-shaped extended adsorption column 11 are now automated. The electric heating rod 14 and the second thermocouple 15 are respectively connected to the output and input ends of the temperature controller 35 via cables. The temperature controller 35 compares the preset temperature with the real-time temperature collected by the second thermocouple 15 and controls the electric heating rod 14 to maintain a constant temperature in the space above the mounting plate 7. The output end of the temperature controller 34 is connected to the heating wire 12 via a cable, and its input end is connected to the first thermocouple 13 via cables. Based on the operating status image of the element analyzer 29 identified by the controller 33 and in conjunction with the real-time temperature collected by the first thermocouple 13, the temperature controller 34 controls the heating wire 12 and the fan 5 according to the preset adsorption temperature and desorption stability, thereby realizing the automated temperature control of the U-shaped extended adsorption column 11 during the adsorption and desorption process.
[0046] As attached Figures 7 to 9 As shown, the following uses H2O extended adsorption and CO2 extended adsorption as examples to illustrate the specific adsorption and desorption processes.
[0047] I. H2O Extended Adsorption and its Automatic Control: Before starting the elemental analyzer, we first fill the U-shaped extended adsorption column with H2O adsorbent. Then, the inlet and outlet pipes are connected to the front end of the H2O adsorption column of the elemental analyzer's adsorption system via a bowl-shaped interface. The programmed temperature rise and fall control system and the image recognition automatic control system of the extended adsorption automatic control system are activated. The solenoid valves are set to engage and disengage on the controller, and the temperature controller is set to 120℃. The programmed temperature rise and fall temperatures are set according to the adsorption and desorption temperatures of the adsorbent in the H2O extended adsorption column. The camera is activated to monitor the elemental analyzer's operating status. The entry of the extended adsorption column into adsorption or desorption states is controlled by four solenoid valves. When the instrument status indicates hydrogen integration is complete and the image recognizes the message "H2O way off", the controller automatically controls solenoid valves 1, 2, 3, and 4 via the image recognition control system to connect the U-shaped extended adsorption column to the gas path of the elemental analyzer's adsorption system, and the extended adsorption column enters the adsorption state. When the instrument status indicates "autozero delay", the controller automatically controls the solenoid valves via the image recognition software to isolate the elemental analyzer's adsorption system from the U-shaped extended adsorption column, and then controls the gas cylinder interface of solenoid valve 2 to connect with the outlet of solenoid valve 4 to form a passage, expelling the H2O gas desorbed from the extended adsorption column, thus completing the desorption process.
[0048] II. CO2 Extended Adsorption and its Automatic Control System: Before starting the elemental analyzer, we first fill the U-shaped extended adsorption column with CO2 adsorbent, and then connect the inlet and outlet pipes to the front end of the CO2 adsorption column of the elemental analyzer's adsorption system through the bowl-shaped interface. The programmed temperature rise and fall control system and the image recognition automatic control system of the extended adsorption automatic control system are activated. The solenoid valves are set to engage and disengage on the controller, and the temperature controller is set to 120℃. The programmed temperature rise and fall temperatures are set according to the adsorption and desorption temperatures of the adsorbent in the CO2 extended adsorption column. The camera is activated to monitor the operating status of the elemental analyzer. The entry of the extended adsorption column into the adsorption or desorption state is controlled by four solenoid valves. When the instrument status indicates hydrogen integration is complete and the image recognizes the message "H2O way off", the controller automatically controls solenoid valves 1, 2, 3, and 4 via the image recognition control system to connect the U-shaped extended adsorption column to the gas path of the elemental analyzer's adsorption system, and the extended adsorption column enters the adsorption state. When the instrument status indicates "autozero delay", the controller automatically controls the solenoid valves via the image recognition software to isolate the elemental analyzer's adsorption system from the U-shaped extended adsorption column, and then controls the gas cylinder interface of solenoid valve 2 to connect with the outlet of solenoid valve 4, forming a passage to discharge the CO2 gas desorbed from the extended adsorption column, completing the desorption process.
[0049] As attached Figure 10As shown, a method for an automatic control system of an element content expansion adsorption device includes the automatic control system of the element content expansion adsorption device in the above embodiment, which mainly includes the following steps:
[0050] Step 1: Connect the U-shaped extended adsorption column 11 to the front end of the corresponding adsorption column in the adsorption system 28 of the element analyzer, start the element analyzer 29, and the temperature controller 35 controls the electric heating rod 14 to heat according to the temperature collected by the second thermocouple 15, so as to maintain the space above the mounting plate 7 at a constant temperature and prevent the pipeline from getting cold and generating condensate during the adsorption process.
[0051] Step 2: When the camera 32 captures the "Autozero delay" message following "wait for N peaks end" on the element analyzer 29's operating status, the image recognition software of the controller 33 automatically controls the first electromagnetic three-way valve 17 and the second electromagnetic three-way valve 18 to connect the connecting pipe 23 and disconnect the connection between the U-shaped extended adsorption column 11 and the element analyzer adsorption system 28. At the same time, it controls the third electromagnetic three-way valve 24 and the fourth electromagnetic three-way valve 26 to connect the U-shaped extended adsorption column 11 to the purge pipe 25 and the exhaust pipe 27, respectively. Simultaneously, the temperature controller 34 starts the program to raise the temperature and meet the preset desorption temperature, causing the gas adsorbed on the absorbent in the U-shaped extended adsorption column 11 to desorb and be discharged through the exhaust pipe 27 using inert gas purging, thus completing the desorption operation.
[0052] Step 3: When the camera 32 captures the "H2O way off" message on the element analyzer 29, the image recognition software of the controller 33 automatically controls the third electromagnetic three-way valve 24 and the fourth electromagnetic three-way valve 26 to disconnect the U-shaped extended adsorption column 11 from the purge pipe 25 and the vent pipe 27, respectively. At the same time, it controls the first electromagnetic three-way valve 17 and the second electromagnetic three-way valve 18 to disconnect the connecting pipe 23 and connect the U-shaped extended adsorption column 11 to the element analyzer adsorption system 28. Simultaneously, the temperature controller 34 starts the cooling program to meet the preset adsorption temperature, allowing the gas in the element analyzer adsorption system 28 to be adsorbed by the absorbent in the U-shaped extended adsorption column 11, thus completing the adsorption operation.
[0053] Step four: When the camera 32 captures the "Autozero delay" message following "wait for N peaksend" on the element analyzer 29's operating status again, the controller 33 and the temperature controller 34 execute the instructions from step two to desorb the gas adsorbed by the U-shaped extended adsorption column 11 in step three. Step two and step three are repeated to realize the desorption and adsorption process of the U-shaped extended adsorption column 11.
[0054] In the above embodiments, the U-shaped extended adsorption column requires a programmed heating and cooling automatic control system to meet the temperature requirements during the adsorption and desorption of the adsorbent material. When the extended adsorption column is in the adsorption state, the temperature controller, according to the adsorption command sent by the controller, stops the heating wire on the U-shaped extended adsorption column and simultaneously starts the cooling fan to lower the temperature to the set temperature. When adsorption is complete and the column enters the desorption state, the temperature controller, according to the desorption command sent by the controller, starts the heating wire on the extended adsorption column to heat and maintains it at the set desorption temperature. The entire programmed heating and cooling automatic control system reaches the required temperature within a specified time by adjusting the heating rate controller, cooling fan power, etc.
[0055] The element content expansion adsorption device, automatic control system and method in the above embodiments are described in conjunction with the elemental analyzer, and three corresponding application scenarios are introduced respectively.
[0056] An elemental analyzer includes an element content expansion adsorption device as described in the above embodiments. This elemental analyzer can expand its measurement range and further improve detection accuracy by utilizing the newly added element content expansion adsorption device.
[0057] An automatic control system for an extended adsorption column of an elemental analyzer includes an automatic control system for the elemental content extended adsorption device in the above embodiments. This automatic control system can assist the elemental content extended adsorption device in achieving automatic operation on the elemental analyzer. The automatic control system adsorbs excess gas through the U-shaped extended adsorption column and promptly uses inert gas to purge and desorb the adsorbed gas at high temperature, thus satisfying the requirement for cyclic use of the extended adsorption column.
[0058] An extended detection method for an elemental analyzer includes an automatic control system method for the element content extension adsorption device described in the above embodiments, used to extend the element detection range of the elemental analyzer and meet the requirements for accurate detection of high and low content elements in samples with extremely high or extremely low element content.
[0059] The foregoing has shown and described the main features and advantages of the present invention. It will be apparent to those skilled in the art that the specific embodiments of the present invention are not limited to the details of the exemplary embodiments described above. Furthermore, without departing from the spirit or essential characteristics of the present invention, the inventive concept and design ideas of the present invention can be implemented in other specific forms, and these should be equivalently included within the protection scope disclosed in the technical solutions of the present invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects. The scope of the present invention is defined by the appended claims rather than the foregoing description, and thus all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included within the present invention.
[0060] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. An automatic control system for an element content expansion adsorption device, comprising an elemental analyzer (29) and a matching elemental analyzer adsorption system (28), wherein the data output port of the elemental analyzer (29) is connected to the input port of a host (30) via a data cable, and the output terminal of the host (30) is connected to the input terminal of a display screen (31) via a signal cable, characterized in that: It also includes an element content expansion adsorption device, a camera (32), a controller (33), and a temperature controller (34). The element content expansion adsorption device includes a temperature control box (1), which consists of a box body (101) and a cover plate (102). A wind box (3) is provided at the bottom of the box body (101), and a fan (5) is installed inside it through a bracket (4). A U-shaped expansion adsorption column (11) is installed inside the box body (101) through a mounting plate (7). An electric heating wire (12) is wound around the U-shaped expansion adsorption column (11), and a first thermocouple (13) is attached to the outer wall of the U-shaped expansion adsorption column (11). The electric heating wire (12) and the first thermocouple (13) are respectively connected to a temperature controller (34) through cables, thereby forming an automatic temperature control system to provide the required working temperature of the U-shaped expansion adsorption column (11). Ventilation holes (103) are provided on both sides of the body (101), and partitions (8) are installed inside the two sides of the body (101). The two partitions (8) are sealed with the two sides of the body (101) to form two air inlet chambers (9). Air inlet slots (10) are provided on both sides of the bottom plate of the body (101) so that the air inlet chambers (9) are connected to the air box (3). A flow hole is provided on the bottom plate of the body (101), and a protective mesh cover (6) is provided on the flow hole. A first electromagnetic three-way valve (17) and a second electromagnetic three-way valve (18) are provided in the body (101), and the first interfaces of the two are connected through a connecting pipe (23). The second interface of the first electromagnetic three-way valve (17) is connected to its air inlet pipe (19). A ball-and-socket connector (16) is connected to the first electromagnetic three-way valve (17). An air inlet pipe (21) is connected to the third port of the first electromagnetic three-way valve (17). The second port of the second electromagnetic three-way valve (18) is connected to another ball-and-socket connector (16) via an air outlet pipe (20). An air outlet pipe (22) is connected to the third port of the second electromagnetic three-way valve (18). The air inlet pipe (21) and the air outlet pipe (22) are connected in series via the ball-and-socket connector (16) to the front end of the corresponding adsorption column in the adsorption system (28) of the elemental analyzer. A third electromagnetic three-way valve (24) is provided on the air inlet pipe (19). A purge pipe (25) is provided on the spare port of the third electromagnetic three-way valve (24) for external purge. A purge gas source is connected, and a fourth electromagnetic three-way valve (26) is installed on the outlet connecting pipe (20). An exhaust pipe (27) is installed on the unused interface of the fourth electromagnetic three-way valve (26), thereby forming a purge system for the U-shaped extended adsorption column (11). The first electromagnetic three-way valve (17), the second electromagnetic three-way valve (18), the third electromagnetic three-way valve (24), and the fourth electromagnetic three-way valve (26) are all located above the mounting plate (7). An electric heating rod (14) and a second thermocouple (15) are respectively installed in the box (101) located above the mounting plate (7), and both are connected to the temperature controller (35) through cables, thereby forming a constant temperature control system to prevent water vapor in the pipe above the mounting plate (7) from condensing.This can lead to inaccurate detection or blockage of solenoid valves and pipelines; The camera (32), controller (33), and temperature controller (34) are connected by signal lines. The camera (32) is mounted on the display screen (31) and is used to capture images of the operating status of the element analyzer (29). The first electromagnetic three-way valve (17), the second electromagnetic three-way valve (18), the third electromagnetic three-way valve (24), and the fourth electromagnetic three-way valve (26) are connected to the signal output terminal of the controller (33) via cables. The controller (33) processes and identifies the images of the operating status of the element analyzer (29) and controls the four electromagnetic three-way valves to achieve automated operation of helium purging and adsorption of the U-shaped extended adsorption column (11). The electric heating rod (14) and the second thermocouple (15) are connected to the temperature controller (34) via cables. At the output and input ends of 5), the temperature controller (35) compares the preset temperature with the real-time temperature collected by the second thermocouple (15) and controls the electric heating rod (14) to keep the temperature of the space above the mounting plate (7) constant; the output end of the temperature controller (34) is connected to the heating wire (12) through a cable, and its input end is connected to the first thermocouple (13) through a cable. The temperature controller (34) controls the heating wire (12) and the fan (5) respectively according to the preset adsorption temperature and desorption stability, based on the image of the element analyzer (29) identified by the controller (33) and the real-time temperature collected by the first thermocouple (13), thereby realizing the automatic temperature control of the U-shaped extended adsorption column (11) during the adsorption and desorption process.
2. The automatic control system for the element content expansion adsorption device according to claim 1, characterized in that: A handle (2) is provided on the top of the box (101) to facilitate the movement of the temperature control box (1) by on-site experimental personnel.
3. A method for an automatic control system of an element content expansion adsorption device, characterized in that: The automatic control system for the element content expansion adsorption device as described in claim 1 mainly includes the following steps: Step 1: Connect the U-shaped extended adsorption column (11) to the front end of the corresponding adsorption column in the adsorption system (28) of the element analyzer, start the element analyzer (29) to run, and the temperature controller (35) controls the electric heating rod (14) to heat according to the temperature collected by the second thermocouple (15) to maintain a constant temperature in the space above the mounting plate (7) and prevent the pipeline from being condensed by cold water vapor during the adsorption process. Step 2: When the camera (32) captures the "Autozero delay" message following "wait for N peaks end" on the element analyzer (29) in its operating state, the image recognition software of the controller (33) automatically controls the first electromagnetic three-way valve (17) and the second electromagnetic three-way valve (18) to connect and disconnect the U-shaped extended adsorption column (11) from the element analyzer adsorption system (28). At the same time, the third electromagnetic three-way valve (24) and the fourth electromagnetic three-way valve (26) are controlled to connect the U-shaped extended adsorption column (11) to the purge pipe (25) and the exhaust pipe (27) respectively. Meanwhile, the temperature controller (34) starts the program to raise the temperature and meet the preset desorption temperature, so that the gas adsorbed on the absorbent in the U-shaped extended adsorption column (11) is desorbed and discharged through the exhaust pipe (27) by inert gas purging, thus completing the desorption operation. Step 3: When the camera (32) captures the "H2O way off" message on the element analyzer (29), the image recognition software of the controller (33) automatically controls the third electromagnetic three-way valve (24) and the fourth electromagnetic three-way valve (26) to disconnect the U-shaped extended adsorption column (11) from the purge tube (25) and the vent tube (27) respectively. At the same time, it controls the first electromagnetic three-way valve (17) and the second electromagnetic three-way valve (18) to disconnect the connecting tube (23) and connect the U-shaped extended adsorption column (11) to the element analyzer adsorption system (28). Meanwhile, the temperature controller (34) starts the program to cool down and meet the preset adsorption temperature, so that the gas in the element analyzer adsorption system (28) is adsorbed by the absorbent in the U-shaped extended adsorption column (11) to complete the adsorption operation. Step 4: When the camera (32) captures the "Autozero delay" message after "wait for N peaksend" on the element analyzer (29) again, the controller (33) and the temperature controller (34) execute the instructions in Step 2 respectively to desorb the gas adsorbed by the U-shaped extended adsorption column (11) in Step 3. Step 2 and Step 3 are repeated to realize the desorption and adsorption process of the U-shaped extended adsorption column (11).
4. An automatic control system for an extended adsorption column of an elemental analyzer, characterized in that: The automatic control system of the element content expansion adsorption device as described in claim 1 is used for the automatic operation of the element analyzer. It adsorbs the overloaded gas through the U-shaped expansion adsorption column (11) and promptly uses inert gas to purge the adsorbed gas at high temperature to desorb it, so as to meet the requirements of the expansion adsorption column for recycling.
5. An extended detection method for an elemental analyzer, characterized in that: The method includes an automatic control system for an element content expansion adsorption device as described in claim 3, used to expand the element detection range of an elemental analyzer and meet the requirements for accurate detection of high and low content elements in samples with extremely high or extremely low element content.