A rapid temperature control automatic sampling device and sampling method

Abstract

The application discloses a kind of quick temperature control automatic sampling device and sampling method, based on the test or production system of special equipment of gaseous working medium, including two parts of quick temperature control automatic sampling device and sampling method.The quick temperature control automatic sampling device is connected with test or processing system, vacuum pump is arranged in the device, the sampler and all pipelines in the device are extracted to vacuum state, gaseous material in the system is converted to solid or liquid state by relying on refrigeration temperature control mode and pressure difference, and is collected into the sampler, to complete later mass spectrum analysis.The application avoids the influence of human error and operation error in manual sampling operation mode on test or product sample, improves work efficiency, and reduces the probability of personal injury.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of gaseous working medium sampling analysis, and particularly relates to a device and method for automatically measuring and taking gaseous samples of raw materials and products with rapid temperature control. BACKGROUND

[0002] In the process of gaseous working medium being introduced into a special device for physical and chemical processing, the working efficiency parameters of the special device need to be obtained, and the method of comparing the component differences between raw materials and processed products can be used. The gaseous working medium and the processed products need to be collected and sampled for analysis, so as to obtain various physical and chemical parameters of the samples.

[0003] At present, in the test or production system of gaseous working medium, the sampling means used is still a manual operation mode, that is, the temperature control, timing and valve switching of the sampling process are completed by manual operation, and after the sample is obtained, the gas components are analyzed by a mass spectrometer, and finally the working efficiency evaluation of the special device is completed. The manual sampling operation mode has human errors and operation errors, which will affect the test or product samples. SUMMARY

[0004] The purpose of the application is to provide a rapid temperature control automatic sampling device and sampling method to avoid the influence of human errors and operation errors in the manual sampling operation mode on the test or product samples, improve the working efficiency and reduce the probability of personal injury.

[0005] The application is implemented by the following technical solutions:

[0006] A rapid temperature control automatic sampling device is connected with a test or production system, and comprises a control system, a vacuum pump assembly, a material collecting container, a sampler, a temperature controller, a liquid nitrogen assembly, an air compression assembly, a local exhaust assembly and a vacuum gauge assembly. The sampler is arranged in the temperature controller, and the material collecting container is nested in the liquid nitrogen assembly. The vacuum gauge assembly is installed at the inlet of the material collecting container, the inlet of the vacuum pump assembly and the pipeline of the sampling inlet of the sampler respectively for monitoring pressure changes. The local exhaust assembly is used for exhausting contaminated air. The sampler is connected with the vacuum pump assembly, the material collecting container and the liquid nitrogen assembly through an electromagnetic valve, a tee joint and a pipe respectively. The temperature controller is connected with the air compression assembly and the liquid nitrogen assembly through a pipe respectively. The air compression assembly is used for sending hot air into the temperature controller, and the liquid nitrogen assembly is used for sending liquid nitrogen into the temperature controller. The tail gas outlet of the local exhaust assembly is connected with the tail gas discharge port of the test or production system. The control system is connected with the vacuum pump assembly, the material collecting container, the sampler, the temperature controller, the liquid nitrogen assembly, the air compression assembly, the local exhaust assembly and the vacuum gauge assembly through control lines respectively.

[0007] Further, the vacuum pump assembly comprises a mechanical pump, a mechanical pump electric control valve, an inter-pump electric control valve, a direct pumping electric control valve, a tail gas electric control valve, a sampling tail gas port, a molecular pump, a partition electric control valve; the mechanical pump is connected in sequence with the molecular pump through the mechanical pump electric control valve and the inter-pump electric control valve, the molecular pump is connected with the material receiving outlet valve of the material receiving container through the partition electric control valve, the material receiving inlet valve of the material receiving container is connected with the sampling end of the sampler, the sampler completes the evacuation operation through the control of the direct pumping electric control valve; the vacuum pump assembly is further connected in sequence with the tail gas discharge line of the test or production system through the tail gas electric control valve and the sampling tail gas port, to complete the safe discharge of the evacuated tail gas.

[0008] Further, the sampler comprises a sampling container cavity, a sampler valve, a sampling electric control valve and a sampling inlet port connected in sequence, and the sampling inlet port is connected with the sampling target pipeline of the test or production system.

[0009] Further, the temperature controller comprises a temperature controller shell, a heat exchanger is arranged in the temperature controller shell, and an air compression inlet, an air compression outlet, a liquid nitrogen inlet and a liquid nitrogen outlet are arranged on the outer surface of the temperature controller shell, and the sampling container cavity is arranged in the temperature controller shell.

[0010] Further, the liquid nitrogen assembly comprises a liquid nitrogen container, upper liquid nitrogen valves, lower liquid nitrogen valves and blow washing liquid nitrogen valves are arranged on the outer surface of the liquid nitrogen container, the blow washing liquid nitrogen valves are connected in sequence with a blow washing copper pipe and a blow washing electric control valve; the material receiving container is nested in the liquid nitrogen container, and the material receiving outlet valve and the material receiving inlet valve are arranged on the outer surface of the liquid nitrogen container and connected with the material receiving container; the upper liquid nitrogen valve is connected with the liquid nitrogen inlet, and the lower liquid nitrogen valve is connected with the liquid nitrogen outlet.

[0011] Further, the air compression assembly comprises an air compressor, a three-way valve, a heater and an exhaust valve, the exhaust valve is arranged on the air compressor, and the air compressor is connected with the heater and the air compression inlet of the temperature controller through the three-way valve.

[0012] Further, the automatic sampling device with rapid temperature control further comprises a movable trolley as a carrier and an external electric control valve; the external electric control valve is used to control the connection between the automatic sampling device and an external test or production system; the trolley is divided into a top portion, a first layer platform, a second layer platform and a bottom platform from top to bottom; the local exhaust assembly is installed on the top portion of the trolley, and the control system is placed below the local exhaust assembly; the liquid nitrogen assembly is installed on the first layer platform of the trolley; a through hole is formed on the first layer platform of the trolley, the sampler and the temperature controller are placed through the through hole, the side suction air vent of the local exhaust assembly is arranged on the first layer platform of the trolley, and the side suction air vent of the local exhaust assembly is located on one side of the through hole and the sampler; the molecular pump of the vacuum pump assembly and the heater of the air compression assembly are installed on the second layer platform of the trolley; the mechanical pump of the vacuum pump assembly and the air compressor of the air compression assembly are installed on the bottom platform of the trolley.

[0013] A sampling method by the automatic sampling device with rapid temperature control, comprising the following steps:

[0014] Step 1, automatic sampling device preparation: the pipeline and the sampler of the automatic sampling device are pre-evacuated, and then the automatic sampling device is connected with a test or production system;

[0015] Step 2, automatic sampling device sampling: the sampler in the automatic sampling device performs frozen collection, then the pipeline of the automatic sampling device is purged, after the purging is completed, the sampler is thawed and replaced;

[0016] Step 3, automatic sampling device sampling end: the automatic sampling device is disconnected with the test or production system, then the pipeline of the automatic sampling device and the newly replaced sampler are evacuated, and the automatic sampling device is shut down.

[0017] Further, in step 1, the specific operation is as follows:

[0018] Step 1.1, first fill the liquid nitrogen container with liquid nitrogen to pre-freeze the collection container therein, connect the sampling tail gas port and the local exhaust assembly to the local exhaust line pipe of the test or production system, and then complete the self-check of the sealing property of the automatic sampling device through the automatic control system; the specific steps of the self-check of the sealing property are as follows:

[0019] a. start the mechanical pump of the vacuum pump assembly, open the mechanical pump electric control valve, the collection outlet valve, the collection inlet valve and the sampling electric control valve, and evacuate the air in the device sampling pipeline and the sampler to below 10 Pa;

[0020] b. Close the sample inlet valve and seal the line. If the pressure increase monitored by the vacuum gauge assembly at the line of the sampling inlet of the sampler is less than 5 Pa / min, the sealing is confirmed to be qualified. If not, the sealing of the sampler can be checked, and the connection sealing member can be replaced. Then, the steps a and b can be performed again until the sealing is confirmed to be qualified.

[0021] After the sealing is qualified, the sampling inlet of the automatic sampling device is connected to the test or production system. Then, the device connection detection is automatically completed by the automatic control system. The specific steps of the connection detection are as follows:

[0022] a. The mechanical pump and the sample outlet valve and the sample inlet valve are kept in the state completed in step 1.1.

[0023] b. The sample inlet valve is opened, the sampler valve is kept closed, the sampling electric control valve and the device external electric control valve are opened, and the line pressure is extracted to be less than 10 Pa.

[0024] c. The sample inlet valve and the device external electric control valve are closed. If the pressure increase monitored by the vacuum gauge assembly at the line of the sampling inlet of the sampler is less than 5 Pa / min, the connection is confirmed to be qualified, and the device external electric control valve is opened.

[0025] After the connection is qualified, the device passivation is automatically completed by the automatic control system. The specific steps of the passivation are as follows:

[0026] a. The automatic sampling device is kept connected to the test or production system. The sampling electric control valve and the sampler valve are opened. The gaseous material is filled into the device sampling line and the sampler for passivation treatment. When the pressure monitored by the vacuum gauge assembly at the line of the sampling inlet of the sampler reaches 2 hPa, the device external electric control valve is closed, and the soaking is sealed.

[0027] b. After the soaking is completed, the sample inlet valve and the sampling electric control valve are opened. The material in the line and the sampler is collected into the sample container. The line is extracted for 30-90 min, and the device extraction pressure is recorded as the background pressure value.

[0028] Further, in step 2, the specific operation is as follows:

[0029] Step 2.1, the gaseous material is automatically frozen and collected by the automatic control system. The specific steps of the freezing and collecting of the gaseous material are as follows:

[0030] a. The sample inlet valve is closed.

[0031] b. The sampler valve is opened. The liquid nitrogen valve of the sampler freezing container and the liquid nitrogen container pressure increasing valve are opened. The liquid nitrogen is filled into the liquid nitrogen container. When the liquid level reaches the limit, the liquid nitrogen valve and the liquid nitrogen container pressure increasing valve are closed.

[0032] c. Open the electric control valve outside the device, and keep the material collection for 10-30 min;

[0033] d. Close the electric control valve outside the device, and close the sampler valve after 1-5 min;

[0034] e. After the sampling operation is completed, open the material collection inlet valve to recycle the material in the device pipeline, monitor the pipeline pressure to be below 10 Pa, and close the sampling electric control valve;

[0035] Step 2.2, automatically complete the sampling pipeline flushing through the automatic control system; the specific steps of the sampling pipeline flushing are as follows:

[0036] a. Close the material collection inlet valve, open the liquid nitrogen valve and the liquid nitrogen container pressure increasing valve, and close the liquid nitrogen valve and the liquid nitrogen container pressure increasing valve when the vacuum gauge assembly monitors that the pressure at the pipeline of the sampling inlet of the sampler reaches 100 hPa, open the material collection inlet valve, and pump the pipeline pressure to be below 10 Pa;

[0037] b. After repeating the above operation for 8 times, close the material collection inlet valve, open the liquid nitrogen valve and the liquid nitrogen container pressure increasing valve, and monitor that the pressure at the pipeline of the sampling inlet of the sampler reaches 10 Pa through the vacuum gauge assembly; 5

[0038] Step 2.3, raise the temperature of the temperature controller through the automatic control system, use the frozen container to heat and thaw the used sampler, control the temperature to be 30-50℃, heat for 5-20 min, and then replace the sampler.

[0039] Further, in step 3, the specific operation is as follows:

[0040] Step 3.1, close the electric control valve outside the device, remove the adapter, close the system part by using the DN10 valve plug, remove the connecting part of the device part, and close the electric control valve outside the device by using the valve blind plate;

[0041] Step 3.2, complete the pipeline and new sampler pumping through the automatic control system; the specific steps of the pipeline and new sampler pumping are as follows:

[0042] a. Open the material collection inlet valve, open the sampling electric control valve and the sampler valve, and pump the device sampling pipeline and the sampler to be below 10 Pa;

[0043] b. Close the material collection inlet valve, close the pipeline, if the pressure monitored by the vacuum gauge assembly at the pipeline of the sampling inlet of the sampler increases less than 5 Pa / min, it is confirmed that the sealing property is qualified; if it is unqualified, the sampler sealing property can be checked, the connecting closure part is replaced, and then the steps a and b are operated until the sealing property is confirmed to be qualified;

[0044] ​Step 3.3, close the inlet valve, close the outlet valve, check the closed valve of liquid nitrogen container and heating equipment, close all the valves of vacuum pump assembly. BRIEF DESCRIPTION OF DRAWINGS

[0045] Figure 1 To constitute the automatic sampling device;

[0046] Figure 2 To constitute the automatic sampling device;

[0047] Figure 3 To constitute the automatic sampling device;

[0048] Figure 4 To constitute the automatic sampling device;

[0049] Figure 5 To constitute the automatic sampling device;

[0050] Figure 6 To constitute the automatic sampling device;

[0051] Figure 7 To constitute the automatic sampling device;

[0052] Figure 8 To constitute the automatic sampling device;

[0053] Figure 9 To constitute the automatic sampling device;

[0054] Wherein, the reference signs are:

[0055] 1-Control system, 2-Vacuum pump assembly, 201-Mechanical pump, 202-Mechanical pump electric valve, 203-Inter-pump electric valve, 204-Direct pumping electric valve, 205-Exhaust electric valve, 206-Sampling exhaust port, 207-Molecular pump, 208-Partition electric valve, 3-Collection container, 301-Collection outlet valve, 302-Collection inlet valve, 4-Sampler, 401-Sampler valve, 402-Sampling container cavity, 403-Sampling electric valve, 404-Blowing electric valve, 405-Sampling inlet, 406-External electric valve, 5-Thermostat, 501-Thermostat shell, 502-Heat exchanger, 503-Compressed air inlet, 504-Compressed air outlet, 505-Liquid nitrogen inlet, 506-Liquid nitrogen outlet, 6-Liquid nitrogen assembly, 601-Liquid nitrogen container, 602-Upper liquid nitrogen valve, 603-Lower liquid nitrogen valve, 604-Blowing liquid nitrogen valve, 605-Blowing copper pipe, 7-Compressed air assembly, 701-Compressed air machine, 702-Three-way valve, 703-Heater, 704-Exhaust valve, 8-Local exhaust assembly, 801-Upper local exhaust, 802-Sampling local exhaust, 803-Sampling local exhaust pipe, 804-System exhaust pipe, 9-Vacuum gauge assembly, 901-Pipeline vacuum gauge, 902-Container vacuum gauge, 903-Vacuum pump vacuum gauge. DETAILED DESCRIPTION

[0056] Hereinafter, a rapid temperature control automatic sampling device and a sampling method according to the present application will be described in detail with reference to the accompanying drawings and examples, which are basic configurations of the present application, and are not intended to limit the scope of the present application.

[0057] Example 1

[0058] As shown in Figure 1 , Figure 3 , Figure 4 , Figure 5 , the rapid temperature control automatic sampling device according to the present application is provided on a movable trolley.

[0059] Installation method: install the local exhaust assembly 8 on the top of the trolley, and then place the control system 1 below; install the liquid nitrogen assembly 6 on the first platform of the trolley, and nest the collection container 3 inside the liquid nitrogen assembly 6; place the sampler 4 and the thermostat 5 on the hole of the second platform of the trolley, and set the side suction vent of the local exhaust assembly 8 on the side of the trolley; place the molecular pump assembly of the vacuum pump assembly 2 and the heater part (heater 703) of the thermostat 5 on the second platform of the trolley; place the compressed air assembly 7 and the mechanical pump assembly of the vacuum pump assembly 2 on the bottom platform of the trolley; and install the vacuum gauge assembly 9 on the pipeline of the inlet of the collection container 3, the inlet of the vacuum pump assembly 2, and the sampling inlet of the sampler, respectively.

[0060] Connection: The sampler 4 is connected with the vacuum pump assembly 2, the sample container 3 and the liquid nitrogen assembly 6 through the electromagnetic valve, tee and corrugated tube of KF16. The sampler 4 is placed in the temperature controller 5, which is connected with the air compressor assembly 7 and the liquid nitrogen assembly 6 through copper tube. The tail gas outlet of the local exhaust assembly 8 is connected with the tail gas discharge port of the test system. The control system 1 is connected with the control lines of the vacuum pump assembly 2, the sample container 3, the sampler 4, the temperature controller 5, the liquid nitrogen assembly 6, the air compressor assembly 7 and the local exhaust assembly 8, and the pressure changes are monitored through the vacuum gauge assembly 9, and the components are operated according to the sampling process through signal output and feedback control.

[0061] Example 2

[0062] Further, as shown in Figure 2 、 Figure 3 、 Figure 4 , the automatic sampling system completes the sampling operation process by controlling each system component and monitoring the pressure change in the system, and the specific operation is as follows:

[0063] The mechanical pump 201 in the vacuum pump assembly 2 is connected with the molecular pump 207 through the mechanical pump electric control valve 202 and the pump interconnection electric control valve 203, and then the molecular pump 207 is connected with the sample container 3 through the partition electric control valve 208, the sample outlet valve 301 and the sample inlet valve 302 of the sample container 3 and the sampler 4. In addition, the sampler 4 can be connected to the mechanical pump 201 through the direct pumping electric control valve 204, the sample inlet valve 302 and the sample outlet valve 301 of the sample container 3, the mechanical pump electric control valve 202, to complete the evacuation operation.

[0064] The vacuum pump assembly 2 is connected with the tail gas discharge line of the test system through the tail gas electric control valve 205 to complete the safe discharge of the evacuated tail gas.

[0065] The sampler 4 is connected with the sample target pipeline of the test system through the sample inlet electric control valve 403, and during the sampling process, the liquid nitrogen in the liquid nitrogen container 601 is filled into the temperature controller 5 through the upper liquid nitrogen valve 602 to complete the freezing of the sample material. After the sampling is completed, the sample pipeline pressure is pumped to below 100 Pa through the direct pumping electric control valve 204, the sample inlet valve 302 and the sample outlet valve 301 of the sample container 3, then the direct pumping electric control valve 204 is closed, the partition electric control valve 208 is opened, and the molecular pump 207 is used to complete the deep pumping of the sample pipeline. Then, the partition electric control valve 208 and the sample inlet valve 302 and the sample outlet valve 301 of the sample container 3 are closed, the lower liquid nitrogen valve 603 and the purge electric control valve 404 are opened, the liquid nitrogen in the temperature controller 5 is put into the sample pipeline to complete the purge operation, and the operation is repeated 8 times.

[0066] The air compressor 701 is used to complete the heating of the temperature controller 5 through the tee valve 702 and the heater 703, and the exhaust valve 704 is opened to remove the internal liquid nitrogen, so that the temperature of the sampler 4 becomes room temperature.

[0067] When the new sampler is removed and installed, the contaminated air is discharged through the tail gas discharge port of the test system by opening the sampling station row 802 and the upper station row 801.

[0068] Further, as shown in Figure 5 , Figure 6 , the connection mode of the core components of the sampling device controlled by the automatic control system is decomposed. As shown in Figure 7 , Figure 8 , Figure 9 , the temperature controller 5 includes a temperature controller housing 501, a heat exchanger 502 (which can be a heat sink), a liquid nitrogen inlet 505, a liquid nitrogen outlet 506, an air inlet 503, and an air outlet 504. The sampler 4 is composed of a sampler valve 401 (which can be a solenoid valve) and a sampling container cavity 402. The sampling container cavity 402 is placed in the temperature controller, and liquid nitrogen is injected through the liquid nitrogen inlet 505 to freeze the sample; after sampling is completed, the vacuum pump assembly 2 is used to complete the sampling pipeline evacuation, all valves are closed, the purge electric control valve 404 is opened, and the liquid nitrogen is sent into the purge copper pipe 605 through the liquid nitrogen outlet 506 to complete the sampling pipeline purge. Then, the air compressor 701 and the heater 703 are used to send hot air into the temperature controller to warm up the sampler and complete the removal.

[0069] Further, the receiving container 3 is placed inside the liquid nitrogen container 601, and the receiving container is connected with a receiving outlet valve 301 and a receiving inlet valve 302. The receiving outlet valve 301 is connected to the inlet end of the vacuum pump, and the receiving inlet valve 302 is connected to the sample inlet end of the sampler. The liquid nitrogen container is connected with a container vacuum gauge 902 for monitoring the pressure change in the container. The upper liquid nitrogen valve 602 and the lower liquid nitrogen valve 603 are used for transporting liquid nitrogen, and the purge liquid nitrogen valve 604 completes the purge of the sampling pipeline through the purge copper pipe 605.

[0070] Example 3

[0071] The sampling method performed by the automatic sampling device with rapid temperature control of the present application comprises the following steps:

[0072] Step 1.1, fill the liquid nitrogen container 601 of the automatic sampling device with liquid nitrogen, freeze the receiving container 3 in the liquid nitrogen container 601 for 30 minutes in advance, and connect the sampling tail gas port 206 and the station row pipeline 802 in the device to the station row pipeline of the test or production system. The self-checking of the sealing property of the device is completed by the automatic control system, and each control system component is normal.

[0073] a. Start the mechanical pump 201 of the vacuum pump assembly 2, open the mechanical pump electric control valve 202, the receiving outlet valve 301, the receiving inlet valve 302, and the sample inlet electric control valve 403, and evacuate the air in the device sampling pipeline and the sampler 4 to below 10 Pa;

[0074] b. Close the material inlet valve 302, and check the pressure increase of the pipeline and sampler measuring point pipeline vacuum gauge 901 to be less than 5 Pa / min to confirm that the sealing meets the standard;

[0075] c. If the standard is not met, perform a sampler 4 sealing test, replace the connecting seal, and then perform steps a and b again until the standard is met.

[0076] Step 1.2. Connect the sampling inlet 405 of the automatic sampling device to the test or production system, and automatically complete the device connection detection operation through the automatic control system;

[0077] a. Detect the state of the mechanical pump 201 and the material outlet valve 301 and the material inlet valve 302, which are maintained as completed in step 1.1;

[0078] b. Open the material inlet valve 302, keep the sampler valve 401 closed, open the sampling electric control valve 403 of the automatic sampling device and the device external electric control valve 406 connected to the system, and the pipeline pressure is drawn to below 10 Pa;

[0079] c. Close the material inlet valve 302, close the device external electric control valve 406 connected to the system, and detect the pressure increase of the pipeline vacuum gauge 901 to be less than 5 Pa / min to confirm that the vacuum is qualified, and then open the device external electric control valve 406.

[0080] Step 1.3. The automatic control system automatically completes the device passivation operation;

[0081] a. Keep the device connected to the system, open the sampling electric control valve 403 and the sampler valve 401 to fill the gaseous material into the device sampling pipeline and the sampler for passivation treatment, close the device external electric control valve 406 connected to the system when the pipeline vacuum gauge 901 pressure reaches 2 hPa, and seal for 30 minutes;

[0082] b. Open the material inlet valve 302 and the sampling electric control valve 403 to collect the material in the pipeline and the sampler into the material container, and draw a vacuum for 60 min and record the device vacuum pressure as the background pressure value.

[0083] Step 2.1. Automatically freeze and collect various gaseous materials through the device automatic control system;

[0084] a. Close the material inlet valve 302;

[0085] b. Open the sampler valve 401, the liquid nitrogen valve for the freezing container, and the liquid nitrogen container pressure increasing valve to fill in liquid nitrogen, and close the liquid nitrogen valve and the liquid nitrogen container pressure increasing valve after reaching the limited liquid level;

[0086] c. Open the material pipeline valve connected to the system, and keep the material collection time for 20 min;

[0087] d. Close the pipeline valve connected with the system, and close the sampler valve 401 after 2 minutes;

[0088] e. After the sampling operation is completed, open the material inlet valve 302 to recycle the material in the device pipeline, and monitor the pipeline pressure to be below 10 Pa. Close the sampling electric valve 403.

[0089] Step 2.2, the automatic control system of the device controls the sampling pipeline to perform a blowing operation;

[0090] a. Close the device material inlet valve 302, open the liquid nitrogen valve and the liquid nitrogen container pressure increasing valve, monitor the pipeline vacuum gauge 901 pressure to reach 100 hPa, close the liquid nitrogen valve and the liquid nitrogen container pressure increasing valve, open the device material inlet valve 302, and the pipeline vacuum gauge 901 pressure is extracted to below 10 Pa;

[0091] b. Repeat the operation of step a for 8 times, close the device material container inlet valve, open the liquid nitrogen valve and the liquid nitrogen container pressure increasing valve, and monitor the pipeline vacuum gauge 901 pressure to reach 10 5 Pa.

[0092] Step 2.3, the automatic control system of the device controls the temperature controller to heat, and the used sampler is heated and thawed using a freezing container. The temperature is controlled at 40°C, the heating time is 10 minutes, and the sampler is replaced.

[0093] Step 3.1, close the valve at the connection between the automatic sampling device and the test or production system, remove the adapter, close the system part using a DN10 valve plug, remove the connection part of the device, and close the device external electric valve 406 using a blind plate.

[0094] Step 3.2, the automatic control system of the device completes the evacuation of the new sampler and the pipeline;

[0095] a. Open the material inlet valve 302, open the sampling electric valve 403 and the sampler valve 401, and evacuate the device sampling pipeline and the sampler to below 10 Pa;

[0096] b. Close the material inlet valve 302, and close the pipeline and sampler pressure gauge 901 pressure growth is less than 5 Pa / min, which can confirm that the sealing performance is qualified;

[0097] c. If it is unqualified, the sampler sealing performance can be checked, and the connection sealing part is replaced, and then the operations of steps a and b are performed until it is qualified.

[0098] Step 3.3, close the material container inlet valve (302), close the material container outlet valve (301), check the closed liquid nitrogen container valve and heating equipment, and close all the valves of the vacuum pump.

[0099] The above merely describes the preferred embodiments of the present application, and it should be pointed out that, for those skilled in the art, several improvements and refinements can be made without departing from the principles of the present application, and these improvements and refinements should also be considered as falling within the protection scope of the present application.

Claims

1. An automatic sampling device with rapid temperature control, characterized in that: The rapid temperature-controlled automatic sampling device is connected to the test or production system and includes a control system (1), a vacuum pump assembly (2), a receiving container (3), a sampler (4), a temperature controller (5), a liquid nitrogen assembly (6), an air compressor assembly (7), a partial exhaust assembly (8), and a vacuum gauge assembly (9). The sampler (4) is located inside the temperature controller (5), and the receiving container (3) is nested inside the liquid nitrogen assembly (6); the vacuum gauge assembly (9) is installed at the inlet of the receiving container (3), the inlet of the vacuum pump assembly (2), and the pipeline of the sampling inlet (405) of the sampler (4) to monitor pressure changes; the exhaust assembly (8) is used to exhaust contaminated air. The sampler (4) is connected to the vacuum pump assembly (2), the receiving container (3), and the liquid nitrogen assembly (6) via electromagnetic valves, tees, and pipe fittings, respectively; the temperature controller (5) is connected to the air compressor assembly (7) and the liquid nitrogen assembly (6) via pipe fittings, respectively. The air compressor assembly (7) is used to send hot air into the temperature controller (5), and the liquid nitrogen assembly (6) is used to send liquid nitrogen into the temperature controller (5); the exhaust outlet of the partial exhaust assembly (8) is connected to the exhaust outlet of the test or production system, and the control system (1) is connected to the vacuum pump assembly (2), the receiving container (3), the sampler (4), the temperature controller (5), the liquid nitrogen assembly (6), the air compressor assembly (7), the partial exhaust assembly (8), and the vacuum gauge assembly (9) via control lines, respectively.

2. The automatic sampling device with rapid temperature control according to claim 1, characterized in that: The vacuum pump assembly (2) includes a mechanical pump (201), a mechanical pump control valve (202), an inter-pump control valve (203), a direct-pump control valve (204), a tail gas control valve (205), a sampling tail gas port (206), a molecular pump (207), and a diaphragm control valve (208). The mechanical pump (201) is connected to the molecular pump (207) in sequence through the mechanical pump control valve (202) and the pump inter-control valve (203). The molecular pump (207) is connected to the receiving outlet valve (301) of the receiving container (3) through the partition control valve (208). The receiving inlet valve (302) of the receiving container (3) is connected to the inlet end of the sampler (4). The sampler (4) completes the evacuation operation under the control of the direct extraction control valve (204). The vacuum pump assembly (2) is also connected to the exhaust gas emission line of the test or production system in sequence through the exhaust gas electronic control valve (205) and the sampling exhaust gas port (206) to complete the safe discharge of the evacuated exhaust gas.

3. The automatic sampling device with rapid temperature control according to claim 2, characterized in that: The sampler (4) includes a sampling container cavity (402), a sampler valve (401), an injection solenoid valve (403), and a sampling inlet (405) connected in sequence. The sampling inlet (405) is connected to the sampling target pipeline of the test or production system.

4. The automatic sampling device with rapid temperature control according to claim 3, characterized in that: The temperature controller (5) includes a temperature controller housing (501), a heat exchanger (502) is provided inside the temperature controller housing (501), and a compressed air inlet (503), a compressed air outlet (504), a liquid nitrogen inlet (505), and a liquid nitrogen outlet (506) are provided on the outer surface of the temperature controller housing (501). The sampling container cavity (402) is located inside the temperature controller housing (501).

5. The automatic sampling device with rapid temperature control according to claim 4, characterized in that: The liquid nitrogen assembly (6) includes a liquid nitrogen container (601), on the outer surface of which are provided an upper liquid nitrogen valve (602), a lower liquid nitrogen valve (603), and a purge liquid nitrogen valve (604). The purge liquid nitrogen valve (604) is connected in sequence to a purge copper pipe (605) and a purge electric control valve (404). The receiving container (3) is nested inside the liquid nitrogen container (601), and the receiving outlet valve (301) and the receiving inlet valve (302) are respectively provided on the outer surface of the liquid nitrogen container (601) and connected to the receiving container (3). The upper liquid nitrogen valve (602) is connected to the liquid nitrogen inlet (505), and the lower liquid nitrogen valve (603) is connected to the liquid nitrogen outlet (506).

6. The automatic sampling device with rapid temperature control according to claim 5, characterized in that: The air compressor assembly (7) includes an air compressor (701), a three-way valve (702), a heater (703), and an exhaust valve (704). The exhaust valve (704) is mounted on the air compressor (701). The air compressor (701) is connected to the heater (703) and the compressed air inlet (503) of the thermostat (5) respectively through the three-way valve (702).

7. The automatic sampling device with rapid temperature control according to claim 6, characterized in that: It also includes a mobile trolley as a carrier and an external electrically controlled valve (406) for controlling the connection between the automatic sampling device and an external testing or production system.

8. The automatic sampling device with rapid temperature control according to claim 7, characterized in that: The trolley is divided into a top platform, a first-level platform, a second-level platform, and a bottom platform from top to bottom. The local exhaust assembly (8) is installed on the top of the trolley, and the control system (1) is placed below the local exhaust assembly (8); The liquid nitrogen assembly (6) is installed on the first platform of the trolley; a through hole is opened on the first platform of the trolley, through which the sampler (4) and the temperature controller (5) are placed; a side suction vent of the local exhaust assembly (8) is set on the first platform of the trolley, and the side suction vent of the local exhaust assembly (8) is located on one side of the through hole and the sampler (4); The molecular pump (207) of the vacuum pump assembly (2) and the heater (703) of the air compressor assembly (7) are mounted on the second-level platform of the vehicle; The mechanical pump (201) of the vacuum pump assembly (2) and the air compressor (701) of the air compressor assembly (7) are mounted on the bottom platform of the trolley.

9. A sampling method using the automatic sampling device with rapid temperature control as described in any one of claims 3-8, characterized in that: Includes the following steps: Step 1, preparation of automatic sampling device: pre-evacuate the pipeline and sampler (4) of the automatic sampling device, and then connect the automatic sampling device to the test or production system; Step 2, Automatic sampling device sampling: The sampler (4) in the automatic sampling device is frozen and collected, and then the pipeline of the automatic sampling device is flushed. After the flushing is completed, the sampler (4) is thawed and replaced. Step 3, Automatic Sampling Device Completes Sampling: Disconnect the automatic sampling device from the test or production system, then evacuate the pipeline of the automatic sampling device and the newly replaced sampler, and stop the automatic sampling device.

10. The sampling method according to claim 9, characterized in that: In step 1, the specific operations are as follows: Step 1.1: First, fill the liquid nitrogen container (601) with liquid nitrogen to pre-freeze the receiving container (3) inside, and connect the sampling tail gas port (206) and the local exhaust component (8) to the local exhaust line of the test or production system. Then, complete the sealing self-test of the automatic sampling device through the automatic control system. Step 1.2: After the sealing meets the standard, connect the sampling inlet (405) of the automatic sampling device to the test or production system, and then automatically complete the device connection test through the automatic control system; Step 1.3: After the connection is qualified, the device passivation is automatically completed by the automatic control system.

11. The sampling method according to claim 10, characterized in that: In step 1.1, the specific steps of the self-test for sealing performance are as follows: a. Start the mechanical pump (201) of the vacuum pump assembly (2) and open the mechanical pump control valve (202), the receiving outlet valve (301), the receiving inlet valve (302), and the sample injection control valve (403) to extract the air in the sampling pipeline and sampler (4) to below 10 Pa; b. Close the receiving inlet valve (302) and seal the pipeline. If the pressure increase monitored by the vacuum gauge assembly (9) at the sampling inlet (405) pipeline of the sampler (4) is less than 5 Pa / min, the sealing performance is confirmed to be up to standard. If it is not up to standard, perform a sealing performance check on the sampler (4), replace the connecting seal and then perform steps a and b until the sealing performance is confirmed to be up to standard. In step 1.2, the specific steps of the connection detection are as follows: a. Ensure that the mechanical pump (201), the receiving outlet valve (301), and the receiving inlet valve (302) remain in the state as they were when step 1.1 was completed; b. Open the receiving inlet valve (302), keep the sampler valve (401) closed, open the injection control valve (403) and the external control valve (406), and pump the pipeline pressure down to below 10Pa; c. Close the receiving inlet valve (302) and the external electric control valve (406). If the pressure increase monitored by the vacuum gauge assembly (9) at the sampling inlet (405) of the sampler (4) is less than 5 Pa / min, then confirm that the connection is qualified and open the external electric control valve (406). In step 1.3, the specific steps of passivation are as follows: a. Keep the automatic sampling device connected to the test or production system, open the injection control valve (403) and the sampler valve (401), and fill the gaseous material into the device injection pipeline and sampler (4) for passivation treatment. When the pressure monitored by the vacuum gauge assembly (9) at the sampling inlet (405) pipeline of the sampler (4) reaches 2 hPa, close the external control valve (406) and seal the soaking. b. After the closed soaking is completed, open the receiving inlet valve (302) and the sampling control valve (403) to collect the material in the pipeline and sampler (4) into the receiving container (3), evacuate for 30-90 minutes and record the evacuation pressure of the device as the background pressure value.

12. The sampling method according to claim 9, characterized in that: In step 2, the specific operations are as follows: Step 2.1: Automatically freeze and collect gaseous materials using an automated control system; Step 2.2: The sampling pipeline is automatically flushed by the automatic control system; Step 2.3: The temperature controller (5) is heated by the automatic control system. The sampler is thawed by heating the frozen container. The temperature is controlled at 30-50℃ and the heating time is 5-20 minutes. Then the sampler is replaced.

13. The sampling method according to claim 12, characterized in that: In step 2.1, the specific steps for freezing and collecting gaseous materials are as follows: a. Close the receiving inlet valve (302); b. Open the sampler valve (401), open the sampler freezing container liquid nitrogen valve and liquid nitrogen container pressurization valve to fill with liquid nitrogen, and close the liquid nitrogen valve and liquid nitrogen container pressurization valve after reaching the limit liquid level; c. Open the external electric control valve (406) and maintain the material collection time for 10-30 minutes; d. Close the external electric control valve (406), and close the sampler valve (401) 1-5 minutes later; e. After completing the sampling operation, open the receiving inlet valve (302) to recover the material in the device pipeline, monitor the pipeline pressure to be below 10Pa, and close the sampling control valve (403); In step 2.2, the specific steps for flushing the sampling pipeline are as follows: a. Close the receiving inlet valve (302), open the liquid nitrogen valve and the liquid nitrogen container pressurization valve. When the pressure monitored by the vacuum gauge assembly (9) at the sampling inlet (405) of the sampler (4) reaches 100 hPa, close the liquid nitrogen valve and the liquid nitrogen container pressurization valve, open the receiving inlet valve (302), and pump the pipeline pressure down to below 10 Pa. b. After repeating the previous step 8 times, close the receiving inlet valve (302), open the liquid nitrogen valve and the liquid nitrogen container pressurization valve, and monitor the pressure of the vacuum gauge assembly (9) at the sampling inlet (405) of the sampler (4) to reach 10 5 Pa.

14. The sampling method according to claim 9, characterized in that: In step 3, the specific operations are as follows: Step 3.1: Close the external solenoid valve (406), remove the adapter, seal the system part with a DN10 valve plug, remove the connecting parts from the device part, and seal the external solenoid valve (406) with a valve blind flange. Step 3.2: Evacuate the pipeline and new sampler using the automatic control system; Step 3.3: Close the receiving inlet valve (302), close the receiving outlet valve (301), check and close the liquid nitrogen container valve and heating equipment, and close all valves of the vacuum pump assembly.

15. The sampling method according to claim 14, characterized in that: In step 3.2, the specific steps for evacuating the pipeline and the new sampler are as follows: a. Open the receiving inlet valve (302), open the sampling control valve (403) and the sampler valve (401), and evacuate the sampling pipeline and sampler to below 10Pa; b. Close the receiving inlet valve (302) and seal the pipeline. If the pressure increase monitored by the vacuum gauge assembly (9) at the sampling inlet (405) pipeline of the sampler (4) is less than 5 Pa / min, the sealing performance is confirmed to be qualified. If it is not qualified, the sealing performance of the sampler (4) is checked, the connecting seal is replaced, and then steps a and b are performed until the sealing performance is confirmed to be qualified.

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