Online analysis system for diphenyl sulfone in acetone

Abstract

The utility model relates to the technical field of chemical sample analysis, and provides an on-line analysis system for diphenyl sulfone in acetone, which comprises a sampling unit, a conveying unit, a chromatographic analyzer and a temperature control system, the conveying unit is connected with the sampling unit; the chromatographic analyzer comprises a constant-temperature box and a chromatographic column box provided with a chromatographic column, the chromatographic column box is arranged in the constant-temperature box, and a sample inlet is formed in the chromatographic column box; the temperature control system is arranged in the chromatographic analyzer and is used for controlling the temperature of the constant-temperature box and the temperature of the chromatographic column box and enabling the temperature of the chromatographic column box to be higher than that of the constant-temperature box; wherein the chromatographic analyzer is also provided with a carrier gas system, and the carrier gas system is connected with the liquid phase six-way valve and is used for bringing a sample into the sample inlet. Through the arrangement of the liquid phase six-way valve, the valve rod of the liquid sample injection valve is pushed by the air cylinder, a small amount of accurate and quantitative liquid sample is fed into the vaporizing chamber from the outside of the chromatographic column box, the liquid sample is completely vaporized under the dual action of the heater and carrier gas dilution, and the constant sample injection amount and the measurement repeatability are ensured.

Description

Technical Field

[0001] This utility model relates to the technical field of chemical sample analysis, and in particular to an online analysis system for diphenyl sulfone in industrial acetone. Background Technology

[0002] When measuring the concentration of diphenyl sulfone in acetone, the diphenyl sulfone needs to be separated in order to analyze the separated diphenyl sulfone and obtain the analytical results.

[0003] In related technologies, due to explosion-proof regulations, the maximum temperature of the constant temperature chamber for holding the chromatographic column cannot exceed 180℃. However, the boiling point of acetone is 56.1℃, and the boiling point of diphenyl sulfone is 325℃. The molecular weight and boiling point values ​​of acetone and diphenyl sulfone differ significantly, resulting in poor separation of acetone and diphenyl sulfone in the chromatographic column and severe peak dragging. Consequently, the peak area of ​​diphenyl sulfone cannot be automatically integrated and can only be integrated manually, leading to significant measurement deviations. Utility Model Content

[0004] This invention provides an online analysis system for diphenyl sulfone in acetone, which solves the problem of poor diphenyl sulfone separation in the prior art.

[0005] This invention provides an online analysis system for diphenyl sulfone in acetone, comprising: a sampling unit, a delivery unit, a chromatographic analyzer, and a temperature control system; the delivery unit is connected to the sampling unit; the chromatographic analyzer includes a constant temperature chamber and a column oven equipped with a chromatographic column, the column oven being located inside the constant temperature chamber and having an injection port; the temperature control system is located inside the chromatographic analyzer and is used to control the temperatures of the constant temperature chamber and the column oven, ensuring that the temperature of the column oven is higher than that of the constant temperature chamber; wherein, the chromatographic analyzer is also equipped with a carrier gas system, the carrier gas system being connected to a six-way liquid chromatography valve for carrying the sample into the injection port.

[0006] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, the chromatographic column oven is equipped with a detector, which is used to detect the concentration of diphenyl sulfone.

[0007] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, the detector is provided with a gas input port, which is connected to a compressed air pipeline and a carrier gas system.

[0008] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, an air pressure reducing filter is provided on the compressed air pipeline, and a hydrocarbon removal instrument is provided between the air pressure reducing filter and the chromatographic analyzer.

[0009] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, the detector includes a flame ionization detector.

[0010] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, the delivery unit is equipped with a preheating device, which is used to heat the sample in the delivery unit.

[0011] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, the liquid phase six-way valve is located on one side of the constant temperature chamber, and one valve port of the liquid phase six-way valve is connected to the sample inlet; the carrier gas system is connected to the liquid phase six-way valve so as to bring the sample into the sample inlet through the liquid phase six-way valve.

[0012] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, the liquid phase six-way valve is connected to the sample injection line, and a first filter is provided on the sample injection line.

[0013] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, the sampling unit includes multiple sampling ports, and the corresponding delivery unit includes multiple sample delivery pipelines. The sample delivery pipelines are connected one-to-one with the sampling ports, and the multiple sample delivery pipelines are connected in parallel and connected to the injection pipeline. Each sample delivery pipeline is provided with a second filter and a shut-off valve. The shut-off valve is electrically connected to the control module, and the control module is used to control the opening and closing of the shut-off valve based on the needs of the chromatograph.

[0014] According to the online analysis system for diphenyl sulfone in acetone provided by this utility model, the liquid phase six-way valve is also provided with a sample output port, which is connected to the sample output pipeline; the second filter on each of the sample delivery pipelines is connected to the sample output pipeline through a connecting pipe, and a flow meter is provided on the connecting pipe.

[0015] The online analysis system for diphenyl sulfone in acetone provided by this invention effectively heats the column oven to a high temperature (210 degrees Celsius) by placing the column oven inside a constant temperature chamber, thus improving the separation efficiency of the column components with a relative deviation of ≤3%. The column oven is now controlled by a temperature control system, which increases the heating rate, saves preheating time, and greatly improves the separation efficiency. Furthermore, after a period of use, the temperature control system can raise the column oven temperature to 300°C to age the column and extend its service life.

[0016] Furthermore, by setting up a six-way liquid phase valve, the liquid injection valve is pushed by a cylinder to send a precisely quantified small amount of liquid sample from outside the column oven into the vaporization chamber, so that the liquid sample is completely vaporized under the dual action of the heater and carrier gas dilution, ensuring constant injection volume and measurement repeatability.

[0017] Furthermore, a hydrocarbon removal instrument is installed before the chromatograph. This instrument effectively removes impurities and oil from the air, ensuring the cleanliness of the compressed air and improving the stability of the chromatograph baseline. Adding a filter effectively removes PEEK ultrafine powder from the solvent, preventing column clogging. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the overall flow path of the online analysis system for diphenyl sulfone in acetone provided by this utility model.

[0020] Figure 2 This is a schematic diagram of the closed flow path of the six-way liquid phase valve in the online analysis system for diphenyl sulfone in acetone provided by this utility model.

[0021] Figure 3 This is a schematic diagram of the opening flow path of the liquid phase six-way valve in the online analysis system for diphenyl sulfone in acetone provided by this utility model.

[0022] Figure 4 The peak shape of diphenyl sulfone is output using a conventional analysis system.

[0023] Figure 5 The image shows the peak shape of diphenyl sulfone output by the online analysis system for diphenyl sulfone in acetone provided by this invention.

[0024] Figure label:

[0025] 10. Sampling unit; 20. Delivery unit; 21. Shut-off valve; 22. Preheating device; 23. Flow meter; 24. Second filter; 25. Control module; 26. Control system; 27. Reflux path; 28. Recovery system; 30. Chromatography analyzer; 31. Incubator; 32. Column oven; 33. Detector; 40. Liquid chromatography six-way valve; 41. Quantitative loop; 50. Compressed air pipeline; 51. Air pressure reducing filter; 52. Hydrocarbon removal instrument; 60. Carrier gas system; 70. Sample injection pipeline; 71. First filter; 80. Sample output pipeline; 90. Exhaust gas emission system. Detailed Implementation

[0026] To make the objectives, technical solutions, and advantages of this utility model clearer, the technical solutions of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this utility model.

[0027] In the description of the embodiments of this utility model, it should be noted that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings. They are only for the purpose of clarifying the embodiments of this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of this utility model. In addition, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0028] In the description of the embodiments of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "connected" and "linked" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in the embodiments of this utility model according to the specific circumstances.

[0029] In this embodiment of the utility model, unless otherwise explicitly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0030] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0031] In some related technologies, online analysis systems for diphenyl sulfone in industrial acetone often employ a simulated manual syringe injection method for sample quantification, with a quantification loop of 1 μL. However, due to the small injection volume, insufficient sample enters the vaporization chamber and column, resulting in slow peak response and poor diphenyl sulfone separation. Furthermore, the injection volume from the quantification loop is not constant compared to the volume entering the vaporization chamber, affecting sample repeatability. Because acetone solvent is volatile, and the injection needle valve is located near the vaporization chamber (approximately 270°C), where the temperature exceeds 50°C, acetone (solvent) evaporates, resulting in lower acetone content and the presence of bubbles entering the column, leading to higher measured diphenyl sulfone concentrations (in ppm).

[0032] Furthermore, no fine filter is installed before the needle-type injection valve. Samples containing small solid particles will pass through the injection valve and vaporization chamber into the chromatographic column. Over time, this will clog the column injection port, increasing maintenance costs, shortening the maintenance cycle, and increasing labor intensity.

[0033] Furthermore, in related technologies, a hydrocarbon removal instrument is not installed on the compressed air delivery pipeline. This causes impurities in the compressed air to affect the accuracy of the output signal of the chromatographic detector, severely reducing measurement precision. Using an air generator or compressed gas cylinder would increase procurement costs and labor intensity. Therefore, to address the aforementioned problems, this utility model proposes an improved online analysis system for diphenyl sulfone in industrial acetone to solve these issues.

[0034] The following is combined Figure 1This invention describes an online analysis system for diphenyl sulfone in acetone, comprising a sampling unit 10, a delivery unit 20, a chromatographic analyzer 30, and a temperature control system. The delivery unit 20 is connected to the sampling unit 10. The chromatographic analyzer 30 includes a constant temperature chamber 31 and a column oven 32 containing a chromatographic column, the column oven 32 being located inside the constant temperature chamber 31 and having an injection port. The temperature control system is located within the chromatographic analyzer 30 and is used to control the temperatures of the constant temperature chamber 31 and the column oven 32, ensuring that the temperature of the column oven 32 is higher than that of the constant temperature chamber 31. The chromatographic analyzer 30 also includes a carrier gas system 60, which is connected to a six-way liquid chromatography valve 40 to carry the sample into the injection port. For online analysis of diphenyl sulfone in acetone, the diphenyl sulfone needs to be separated before analysis. In this embodiment, by placing the chromatographic column oven inside a constant temperature chamber, high-temperature heating of the chromatographic column oven (column temperature reaches 210 degrees Celsius) can be effectively achieved, as compared to... Figure 4-5 As shown, the separation efficiency of the chromatographic column components has been improved, with a relative deviation of ≤3%. The column oven was replaced with a temperature control system, which increased the heating rate and saved equipment preheating time, greatly improving the separation efficiency of the column. Moreover, after a period of use, the temperature control system can raise the temperature of the column oven to 300℃ to age the column and extend its service life.

[0035] in, Figure 4 and Figure 5 These are different peak shapes output for a diphenyl sulfone concentration of 15 ppm. The peak shapes show that, through the improvements in this embodiment, the peak column formation is more prominent, indicating better separation and lower relative deviation. Specifically, the column oven is made of high-strength explosion-proof material, such as thickened 304 stainless steel. The temperature control system within the chromatograph controls the temperatures of the incubator 31 and the column oven 32. This system enables temperature control of both the incubator 31 and the column oven 32, and allows for differentiated temperature control between the two.

[0036] Specifically, acetone (chemical formula C3H6O) has a molecular weight of 58.08 g / mol and a boiling point of 56.1 °C, while diphenyl sulfone (chemical formula C...)... 12 H 10 The molecular weight of diphenyl sulfone (O2S) is 218.29 g / mol, and its boiling point is 325℃. When measuring the concentration of diphenyl sulfone in acetone, it's important to note that acetone and diphenyl sulfone have significantly different molecular weights and boiling points, requiring complete separation during the measurement process. In this example, effective heating of diphenyl sulfone can be achieved by individually controlling the temperature of the column oven at 32℃, thus enabling its vaporization.

[0037] In specific settings, the temperature of the column oven 32 is higher than that of the constant temperature chamber 31. Due to the factory's explosion-proof requirements, the temperature of the constant temperature chamber 31 cannot be too high. However, because diphenyl sulfone has a high boiling point, in order to achieve its vaporization separation, this embodiment uses a temperature control system to achieve independent control, thereby enabling the temperature of the chromatographic column to be higher than that of the external constant temperature chamber 31. This allows the constant temperature chamber 31 to improve the separation effect of diphenyl sulfone while meeting relevant requirements.

[0038] In conjunction with the above embodiments, a liquid phase six-way valve 40 is also included. The liquid phase six-way valve 40 is located on one side of the constant temperature chamber 31, and one of the valve ports of the liquid phase six-way valve 40 is connected to the injection port. In this embodiment, the sample enters through the liquid phase six-way valve 40, and during the advancement process, the sample is carried in by the carrier gas. This allows for the precise quantification of a small amount of liquid sample from outside the column oven 32 into the vaporization chamber, where the liquid sample is completely vaporized under the dual action of the heater and the carrier gas dilution, ensuring a constant injection volume and measurement repeatability.

[0039] Specifically, similar to a conventional chromatograph 30, the chromatograph in this invention is also equipped with a carrier gas system 60, a temperature control system, a data processing system, an exhaust gas system 90, and other auxiliary systems. The carrier gas system 60 is connected to a liquid-phase six-way valve 40. When the liquid-phase six-way valve 40 is in the injection state, a constant amount of sample in the quantitative loop 41 is blown away by the carrier gas, carrying the sample into the column oven 32. The temperature control system is used to maintain a constant temperature inside the oven 31, ensuring that the sample is completely vaporized. The data processing system collects and analyzes the data, and then uses this data to control other flow paths. The exhaust gas system 90 is used to discharge the separated waste gas. In this embodiment, the key is the use of a liquid-phase six-way valve 40 for sample input. This method allows for stable control of the sample input volume and ensures complete sample vaporization through the combined effects of a heater and carrier gas dilution. On the other hand, by placing the column oven 32 inside the constant temperature chamber 31, the column oven 32 can be heated separately, thus avoiding excessive temperature in the constant temperature chamber 31.

[0040] The liquid phase six-way valve 40 is a commercially available liquid phase six-way valve 40, which has six valve ports. Two of the valve ports are connected by a metering ring 41. The remaining valve port is connected to the sample inlet, one valve port is connected to the carrier gas system 60, and one valve port is connected to the piston chamber of the valve stem. By inputting carrier gas, the valve stem can be moved, thereby realizing the input of the sample. The last valve port serves as the sample output port, used to output the separated sample.

[0041] Specifically, such as Figure 2 , Figure 3 As shown, Figure 2The diagram shows the flow path of the six-way liquid phase valve 40 when closed. The six valve ports are numbered. Valve port 1 and 4 are connected to a metering loop 41. At this time, valve port 4 is connected to the sample inlet valve (valve port 3), and the sample outlet valve (valve port 2) is connected to valve port 1. The remaining valve port (valve port 5) is connected to the carrier gas (nitrogen). Valve port 6 is connected to the valve stem. When the flow path of the six-way liquid phase valve 40 is open, valve port 1 and 4 are connected to a metering loop 41. At this time, valve port 4 is connected to valve port 5, which is connected to the carrier gas (nitrogen). Valve port 6 is connected to the valve stem, and valve port 2 (sample outlet) is connected to valve port 3 (sample inlet).

[0042] The following is a description of the above-mentioned liquid phase six-way valve 40.

[0043] The liquid phase six-way valve 40 consists of the following core components: Valve body: The main structure, typically made of corrosion-resistant materials (such as stainless steel), with six internal fluid channel interfaces. Valve core (rotor): A rotatable component that connects different channels by changing its position. Sealing ring: Ensures a tight seal between the valve body and the valve core, preventing fluid leakage. Handle or drive mechanism: Used for manual or automatic switching of the valve core position. Metering loop: A fixed-volume sample storage loop that determines the injection volume (e.g., 20 μl, 100 μl, etc.).

[0044] Working principle step by step: The working process of the liquid phase six-way valve is divided into two main states: sampling (Load) and injection (Inject).

[0045] like Figure 2 As shown, in the sampling state (Load), the channel connections are as follows: when the valve core is rotated to the Load position, the fluid channel connections are 3→4→1→2, 5→6. Operating procedure: The mobile phase flows directly to the column after entering the valve body from the pump, maintaining stable system pressure. The sample is injected into the quantitative loop through the injection needle; excess sample is discharged from the waste outlet, ensuring the quantitative loop is completely filled. Key function: Preventing sample mixing with the mobile phase and maintaining baseline stability.

[0046] like Figure 3 As shown, in the Inject state, channel switching occurs as follows: rotating the handle 60° switches the valve core to the Inject position, and the channels change to 5→4→1→6, 3→2. The operating procedure is as follows: the mobile phase changes its path, propelling the sample within the quantitative loop into the chromatographic column. The quantitative loop is thoroughly flushed by the mobile phase, ensuring complete sample transfer and avoiding residual contamination.

[0047] As can be seen from the above, the liquid phase six-way valve in this embodiment can achieve a metering loop of 20 microliters (compared to only about 10 microliters in traditional technology), and the required amount can be adjusted according to the needs, while ensuring that the residue is small.

[0048] In conjunction with the above embodiments, the chromatographic column oven 32 is equipped with a detector 33, which is used to detect the concentration of diphenyl sulfone. During online analysis, the analytical structure needs to be output in real time. In this embodiment, the detector 33 is configured to detect the concentration of the separated diphenyl sulfone.

[0049] Specifically, detector 33 can be a flame ionization detector (FID), which can detect diphenyl sulfone concentration and transmit the detection results to the data processing system, thus enabling timely feedback of the detection results.

[0050] In a specific embodiment, the detector 33 is provided with a gas input port, which is connected to the compressed air pipeline 50 and the carrier gas system 60. As can be understood from the above, this embodiment uses a flame ionization detector 33, which requires compressed air as an oxidizer and hydrogen as fuel during the detection process. In this embodiment, hydrogen is input through the carrier gas system 60 through the gas input port, and compressed air is input through the compressed air pipeline 50, thereby achieving combustion.

[0051] Specifically, the aforementioned auxiliary system includes a hydrogen tank, a nitrogen tank, and a compressed air tank. The compressed air tank and the hydrogen tank are used to provide compressed air and hydrogen, respectively, to enable the fuel supply of the detector 33. The nitrogen tank is used to provide nitrogen, which is used as a carrier gas to deliver the sample to the chromatographic column. The pneumatic actuator of the liquid phase six-way valve 40 is driven by compressed air. Nitrogen is an inert gas and does not participate in the reaction; it only acts as a transport carrier.

[0052] Among them, the flame ionization detector 33 is a commonly used detector in conventional technology. It has two gas input ports, one for hydrogen and one for compressed air, which can be mixed and ignited to generate a flame, so that the organic compounds in the sample are ionized in the flame and generate positive and negative ions, thus achieving detection.

[0053] According to some embodiments of this invention, an air pressure reducing filter 51 is provided on the compressed air pipeline 50, and a hydrocarbon removal device 52 is provided between the air pressure reducing filter 51 and the chromatograph 30. In conventional analytical systems, compressed air is directly introduced into the detector 33, but hydrocarbon impurities in the compressed air can affect the accuracy of the output signal of the chromatograph detector 33, severely reducing measurement accuracy. In this embodiment, the air entering the chromatograph undergoes hydrocarbon removal through the hydrocarbon removal device 52, which effectively removes impurities and oil from the air, ensuring the cleanliness of the compressed air and improving the stability of the chromatograph baseline.

[0054] Specifically, the air pressure reducing filter 51 can reduce the pressure of compressed air and filter impurities. After impurity filtration, the hydrocarbon removal instrument 52 can remove hydrocarbon impurities, reducing the impact on the chromatograph.

[0055] In some embodiments, the delivery unit 20 is equipped with a preheating device 22, which is used to heat the sample within the delivery unit 20. By providing the preheating device 22, the separation effect of diphenyl sulfone in the sample can be improved, thereby increasing the accuracy of the final analytical data.

[0056] Furthermore, the preheating device 22 can increase the sample heating rate, which greatly helps the separation effect of the chromatographic column. After a period of use, the temperature of the chromatographic column oven 32 can be raised to 300°C to age the chromatographic column and extend its service life.

[0057] According to some embodiments provided by this utility model, the liquid chromatography six-way valve 40 is connected to the injection line 70, and a first filter 71 is provided on the injection line 70. The first filter 71 can avoid the risk of column clogging. The filter element is made of sintered stainless steel, which can be cleaned by ultrasonic cleaning of powder impurities attached to the pores of the stainless steel filter, achieving the effect of reuse and reducing the maintenance cost of the chromatograph.

[0058] Understandably, in conventional systems, samples are directly input into the chromatograph for analysis via a mechanism similar to that of a manual needle pusher. In this example, the setting of the first filter 71 enables the filtration of impurities in the sample, avoiding clogging and improving the stability of system operation.

[0059] Specifically, the first filter 71 is a fine filter, which can effectively remove tiny particles, impurities and contaminants from liquids or gases. The filtration accuracy can usually reach the micron or submicron level, ensuring that the filtered sample is purer.

[0060] According to some embodiments provided by this utility model, the sampling unit 10 includes multiple sampling ports, and the corresponding delivery unit 20 includes multiple sample delivery pipelines. Each sample delivery pipeline is connected to a sampling port, and the multiple sample delivery pipelines are connected in parallel and connected to the injection pipeline 70. Each sample delivery pipeline is equipped with a second filter 24 and a shut-off valve 21. The shut-off valve 21 is electrically connected to the control module 25, which can control the opening and closing of the shut-off valve 21 based on the needs of the chromatograph 30. The multiple sampling ports and sample delivery pipelines allow the system to be used for different analytical purposes. For example, one flow path may be used for online monitoring of sample concentration, another for periodic laboratory analysis, a third for checking for impurities, and a fourth for backup sampling in case of system failure. By splitting the samples, the system can better meet different analytical needs.

[0061] Specifically, the control module 25 is connected to the control system 26. The control module 25 can control the opening and closing of the shut-off valve 21 based on the feedback information, thereby realizing the on-off control of each flow path.

[0062] In conjunction with the above embodiments, the liquid phase six-way valve 40 is also provided with a sample output port, which is connected to the sample output pipeline 80; the second filter 24 on each sample delivery pipeline is connected to the sample output pipeline 80 through a connecting pipe, and a flow meter 23 is provided on the connecting pipe. This arrangement enables sample reuse, that is, a portion of the sample is returned, which helps to ensure proper sample handling and avoid waste, while also facilitating the control and adjustment of the sample volume of the analysis system.

[0063] Specifically, the end of the sample output pipeline 80 is connected to the recovery system 28 via a return flow path 27. A branch hole is provided on the return flow path 27, which is connected to a connecting pipe. This allows a portion of the recovered sample to be fed into the sample delivery pipeline through the second filter 24 for reuse, and then recovered by the recovery system 28, preventing contamination or unnecessary chemical leaks. Furthermore, the sample return design allows for repeated analysis, sample adjustment, or replenishment.

[0064] The overall flow path is described below, such as... Figure 1As shown in the diagram, four sampling ports are located on the left side. Each of the four sampling units 10 is connected to the sample delivery pipeline in the delivery unit 20. During sampling, samples are automatically collected and input into the injection pipeline 70 via the delivery unit 20. The delivery unit 20 includes a preheating device 22 to preheat the sample, thereby increasing the heating rate of subsequent samples. The injection pipeline 70 is connected to a six-way liquid chromatography valve 40, enabling the sample to be input into the chromatograph for separation and chromatogram output. To control each delivery pipeline, a control module 25 is provided. The control module 25 controls each sampling flow path based on feedback data collected by the control system 26. Connected to the liquid phase six-way valve 40 is a carrier gas system 60. Nitrogen gas from the carrier gas system 60 is introduced into the liquid phase six-way valve 40 and carries the sample into the column oven 32. The carrier gas system 60 also includes hydrogen gas. Both the hydrogen gas and compressed air lines 50 are connected to the detector 33, thus providing fuel for the detector 33. One port of the liquid phase six-way valve 40 is configured as a sample output port. The sample output port returns a portion of the sample to the sample delivery line through the reflux path 27, while the remaining portion flows to the recovery system 28 (such as a recovery pit). Correspondingly, the chromatograph is also equipped with an exhaust gas system 90 for discharging exhaust gases.

[0065] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and not to limit it. Although this utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this utility model.

Claims

1. An on-line analysis system for diphenyl sulfone in acetone, characterized by, The application relates to a sample analysis device, which comprises: a sampling unit, a conveying unit connected with the sampling unit, a chromatographic analyzer comprising an incubator and a chromatographic column box provided with a chromatographic column, the chromatographic column box being arranged in the incubator and provided with a sample inlet, a temperature control system arranged in the chromatographic analyzer, which is used for controlling the temperatures of the incubator and the chromatographic column box and making the temperature of the chromatographic column box higher than that of the incubator, wherein the chromatographic analyzer is further provided with a carrier gas system which is used for bringing the sample into the sample inlet.

2. The on-line analysis system of diphenyl sulfone in acetone according to claim 1, characterized in that, The chromatographic column box is provided with a detector which is used for detecting the concentration of diphenyl sulfone.

3. The on-line analysis system of diphenyl sulfone in acetone according to claim 2, characterized in that, The detector is provided with a gas input port which is connected with a compressed air pipeline and the carrier gas system.

4. The on-line analysis system of diphenyl sulfone in acetone according to claim 3, characterized in that, The compressed air pipeline is provided with an air pressure reduction filter, and a hydrocarbon removal instrument is arranged between the air pressure reduction filter and the chromatographic analyzer.

5. The on-line analysis system for diphenyl sulfone in acetone according to claim 3, wherein The detector comprises a flame ionization detector.

6. The on-line analysis system for diphenyl sulfone in acetone according to claim 1, wherein The conveying unit is provided with a preheating device which is used for heating the sample in the conveying unit.

7. The on-line analysis system for diphenyl sulfone in acetone according to claim 1, wherein The device further comprises a liquid phase six-way valve which is arranged on one side of the incubator and one valve port of which is connected with the sample inlet; the carrier gas system is connected with the liquid phase six-way valve so as to bring the sample into the sample inlet through the liquid phase six-way valve.

8. The on-line analysis system for diphenyl sulfone in acetone according to claim 7, characterized in that, The liquid phase six-way valve is connected with a sample inlet pipeline which is provided with a first filter.

9. The on-line analysis system for diphenyl sulfone in acetone according to claim 8, characterized in that, The sampling unit comprises a plurality of sampling ports, and the conveying unit comprises a plurality of sample conveying pipelines which are connected with the sampling ports one by one, the sample conveying pipelines are connected in parallel and connected with the sample inlet pipeline. Wherein, each sample conveying pipeline is provided with a second filter and a shut-off valve, the shut-off valve is electrically connected with a control module, and the control module is used for controlling the on-off of the shut-off valve based on the requirement of the chromatographic analyzer.

10. The on-line analysis system for diphenyl sulfone in acetone according to claim 9, wherein The liquid phase six-way valve is further provided with a sample output port which is connected with a sample output pipeline; the second filter on each sample conveying pipeline is connected with the sample output pipeline through a communication pipe, and the communication pipe is provided with a flow meter.

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