Gas sampling control label and thermal desorption automatic processing system and method based on CTC automatic sampler

Abstract

The present invention discloses a gas sampling tube label and thermal desorption fully automatic processing system and method based on a CTC automatic sampler, comprising: a sleeve module for accommodating a sampling tube; a tray for placing a plurality of sleeve modules; a label making module for accommodating the sleeve module and performing label making operations on the sampling tube in the sleeve module; a thermal desorption module for accommodating the sleeve module and performing thermal desorption operations on the sampling tube in the sleeve module. The present invention provides a gas sampling tube label and thermal desorption fully automatic processing system based on a CTC automatic sampler and a pre-processing method thereof, so as to solve the problems of serious manual dependence, long time consumption, low efficiency and large error in the pre-processing operation of the CTC automatic sampler in the prior art, and achieve the purpose of improving the automation degree of the pre-processing process of the CTC automatic sampler, reducing manual dependence, and improving the accuracy and efficiency of pre-processing.

Description

Technical Field

[0001] The present invention relates to the field of air detection in disease control occupational health workplaces and environmental health public spaces, and in particular to a gas sampling control mark and thermal desorption fully automatic processing system and method based on a CTC automatic sampler. Background Art

[0002] The air quality in the workplace and public spaces is a key area of ​​focus for routine disease control monitoring. Through daily monitoring of relevant hazardous factors in the workplace and public spaces, protection can be provided for different groups of people. Volatile organic compounds (VOCs) refer to organic compounds that have a high saturated vapor pressure (greater than 13.33 Pa), a low boiling point, a small molecular weight, and are volatile at room temperature under standard conditions. Most VOCs have a special odor that makes people uncomfortable, and are toxic, irritating, teratogenic, and carcinogenic. Therefore, timely monitoring of VOCs is conducive to protecting the health of relevant groups of people.

[0003] The CTC autosampler is an integrated autosampler mounted on a gas chromatograph (GC) or a gas chromatograph-mass spectrometer (GC / MS). It can realize multiple injection methods such as headspace injection, liquid injection, and SPEM injection. The advantages of the CTC autosampler are large modification space, small footprint (directly mounted on the GC or GC / MS, no separate laboratory table is required), and multiple integrated functions. It is currently the largest autosampler in the disease control system laboratory, providing a hardware foundation for subsequent modification.

[0004] In occupational and environmental health, gas chromatographs (GC) or gas chromatography-mass spectrometry (GC / MS) are often used to detect VOCs in workplace air and / or indoor air of public spaces. Thermal desorption is a common pretreatment method for this type of detection: it uses activated carbon and silica gel sampling tubes according to the different polarities of the compounds, and collects the volatile organic compounds in several liters of gas into the sampling tubes through an atmospheric sampler; after sampling, before testing in the laboratory, each batch of samples needs to be calibrated for analytical efficiency and working curves. This calibration operation is also called "calibration", which requires analytical efficiency detection and analysis of the sampling tubes and the preparation of working curves.

[0005] There are at least the following disadvantages in the labeling and thermal desorption work in the prior art: (1) The thermal desorption instrument and labeling device are manually operated. When labeling or analyzing the desorption efficiency of sampling tubes, only one sampling tube can be processed at a time. The processing of a single sampling tube requires purging with carrier gas for 5-10 minutes. A set of working curves (including one blank) requires processing 6-8 sampling tubes, and a desorption efficiency analysis requires processing 10 or more sampling tubes. Therefore, the manpower consumption is large and the work efficiency is extremely low. (2) The operation process needs to be completed manually, which is time-consuming and wastes manpower. In addition, manual operation can easily lead to increased system errors, resulting in low calibration accuracy. (3) Some semi-automatic and fully automatic thermal desorption systems have also appeared in the prior art. (4) Existing semi-automatic and fully-automatic thermal desorption instruments are large in size and require a large amount of laboratory bench space. At present, VOCs detection in the workplace is mainly completed by grassroots disease control departments. Most laboratories are old, have limited funds, and have relatively scarce laboratory bench space, making it difficult to integrate existing semi-automatic and fully-automatic thermal desorption instruments. (5) Existing semi-automatic and fully-automatic thermal desorption instruments require modification of the inlet of the gas chromatograph or gas chromatograph-mass spectrometer before they can be used. This is a highly destructive modification to the instrument and is likely to have an adverse effect on the sensitivity of the instrument itself.

[0006] In summary, it is necessary to improve and optimize the labeling and thermal desorption facilities corresponding to the CTC automatic sample injector in the current disease control system. Summary of the invention

[0007] The present invention provides a gas sampling tube labeling and thermal desorption fully automatic processing system and method based on a CTC automatic sampler, so as to solve the problems in the prior art that the pre-processing operation of the gas sampling tube is seriously dependent on manual labor, is time-consuming, inefficient and has large errors, so as to achieve the purpose of using the CTC automatic sampler to improve the automation degree of the pre-processing process, reduce manual dependence, and improve the accuracy and efficiency of pre-processing.

[0008] The present invention is achieved through the following technical solutions:

[0009] Gas sampling control label and thermal desorption automatic processing system based on CTC automatic sampler, including:

[0010] A casing module, used for accommodating a sampling tube;

[0011] A tray for placing a number of casing modules;

[0012] A labeling module, used to accommodate the casing module and perform labeling operations on the sampling tubes in the casing module;

[0013] The thermal desorption module is used to accommodate the casing module and perform thermal desorption operation on the sampling tube in the casing module.

[0014] In view of the fact that the pre-processing operation of the gas sampling tube in the prior art heavily relies on manual work, which is time-consuming, inefficient and has large errors, the present invention first proposes a gas sampling tube label and thermal desorption automatic processing system based on a CTC automatic sampler. The system is configured to accommodate a sampling tube sleeve module, and the sampling tube to be pre-processed is placed in the sleeve module, and the sleeve module is used as a carrier for subsequent pre-processing operations. The tray matches the sleeve module, and a number of sleeve modules can be placed on it, thereby facilitating the removal and storage of the sleeve modules.

[0015] The structure of the sleeve module in the present application is matched with the specific CTC instrument, and it is only necessary to match the sleeve module with the existing robotic arm of the corresponding CTC automatic sampler and to be able to be taken and placed by the existing robotic arm of the CTC automatic sampler.

[0016] Labeling and thermal desorption are both processing operations required in the field of VOCs detection. This application sets up a labeling module and a thermal desorption module. When labeling is required, the robotic arm of the CTC automatic sampler grabs the designated sleeve module and places it in the labeling module; when thermal desorption is required, the robotic arm of the CTC automatic sampler grabs the designated sleeve module and places it in the thermal desorption module; after the corresponding pre-processing operation is completed, the robotic arm of the CTC automatic sampler can also grab the sleeve module and put it back on the tray for storage.

[0017] It can be seen that the present application solves the problem in the prior art that the detection operation of VOCs in the air is heavily dependent on manual work. The staff only needs to regularly or regularly replace the corresponding sampling tubes in each sleeve module according to specific work needs, and place them in the designated holes on the tray. The entire pretreatment process can be automatically completed based on the existing structure of the CTC automatic sample injector, which significantly reduces manpower consumption, thereby improving work efficiency and reducing work errors; in addition, when using the present application, there is no need to modify the sample inlet of the original gas chromatograph or gas chromatograph-mass spectrometer in the laboratory, avoiding destructive modifications to the instrument and equipment, and avoiding adverse effects on the sensitivity of the instrument itself; and the present application has a simple and compact structure and does not take up too much space. Compared with the relatively large automatic thermal desorption instruments in the prior art, it is more suitable for promotion and application in grassroots disease control departments with limited funds and site conditions.

[0018] Furthermore, the sleeve module includes a tube body and a tube cap that match each other, and the sleeve module has a first cavity for accommodating the sampling tube, and the first cavity is partially or completely located in the tube body; a second cavity is also arranged in the tube body, and the second cavity is located below the first cavity, and the bottom end of the first cavity is connected to the second cavity, and an air inlet channel connected to the first cavity is arranged on the tube cap, and the second cavity is connected to the exhaust channel.

[0019] In this solution, the sleeve module is a tubular structure, and the tube cap can be connected to the tube body in any existing manner; the first cavity is used to accommodate the sampling tube; the second cavity provides a channel for the sampling tube to be inserted, and provides a fluid outlet through the exhaust channel.

[0020] Furthermore, the sleeve module also includes a bearing plate slidably connected to the second cavity in the longitudinal direction, and the bearing plate is movably sleeved outside the exhaust channel; and also includes a first lifting mechanism for adjusting the height of the bearing plate.

[0021] In this solution, the bottom end of the sampling tube enters the second cavity and is placed on the carrying plate, which carries the sampling tube. In addition, the height of the carrying plate is adjustable, so that this solution can meet the use of sampling tubes of different lengths, significantly improving the versatility of this solution and facilitating the adaptation of sampling tubes of different specifications.

[0022] In addition, the supporting plate is movably sleeved outside the exhaust passage, so when the sampling tube is gradually placed downward onto the supporting plate, the exhaust passage gradually enters the sampling tube from the bottom.

[0023] Furthermore, the labeling module includes a first shell, a breathable partition located in the first shell, and a plurality of first accommodating cavities located above the breathable partition; it also includes a first shell cover matching the first shell, the first shell cover is provided with injection channels corresponding to the first accommodating cavities one by one; the first shell cover is provided with a first air inlet connected to each injection channel, and the first shell bottom is provided with a first exhaust port; the first shell has an air collecting cavity inside, the breathable partition is located in the air collecting cavity, the bottom end of the first accommodating cavity is connected to the top end of the air collecting cavity, and the top end of the first exhaust port is connected to the bottom end of the air collecting cavity.

[0024] In the prior art, in the pre-processing process of the CTC automatic sampler, the calibration operation needs to be completed manually, which is time-consuming and has large errors. The calibration module of the present scheme is used to calibrate the designated sampling tube; the module includes a first shell, a breathable partition is arranged inside the shell, and a plurality of first accommodating cavities are arranged above the breathable partition, and the first accommodating cavities are used to accommodate the sampling tubes to be calibrated; the first shell cover is provided with an injection channel and a first air inlet, which are respectively used to inject a standard solution and a carrier gas into the interior of the module.

[0025] When this scheme is used specifically, the sampling tube to be calibrated is first loaded into the first containing cavity, and then the first shell cover is closed, and the standard solution is injected into the corresponding sampling tube through the injection channel; then the carrier gas is injected through the air inlet to purge the sampling tube, and the purge time can be adjusted according to the volatility of the solution and the injection amount. In this process, the purpose of calibrating the analytical efficiency and calibrating the working curve can be achieved.

[0026] It can be seen that this solution overcomes the defects of the prior art in that the calibration process requires manual holding of the sampling tube for a long time, which results in a long time and high labor consumption; multiple sampling tubes can be processed simultaneously during the calibration process, thereby significantly improving the calibration efficiency; in addition, this solution can reduce the manual operation steps, thereby reducing the calibration error and improving the accuracy of the calibration results.

[0027] Furthermore, the air-permeable baffle is fixedly connected in the gas collecting cavity, and the inner diameter of the first accommodating cavity is equal to the outer diameter of the cannula module. This solution makes the inner diameter of the first accommodating cavity equal to the outer diameter of the cannula module, so the cannula module can be stably installed in the first accommodating cavity; and the cannula module entering the first accommodating cavity is carried by the air-permeable baffle, which is conducive to ensuring that the placement height of different cannula modules in the labeling module remains uniform, and thus is conducive to the matching use with the mechanical arm of the CTC automatic sampler.

[0028] Furthermore, the thermal desorption module includes a thermal desorption gas constant volume pipe, a second shell, a second accommodating cavity opened on the second shell, and a second shell cover matching the second shell;

[0029] A heating device is disposed in the second shell;

[0030] The second accommodating chamber is used to accommodate the sleeve module. A second air inlet is arranged at the bottom of the second accommodating chamber, and a second exhaust port is arranged on the second shell cover; the second exhaust port is connected to the thermal decomposition gas absorption constant volume pipe.

[0031] In this solution, the thermal desorption constant volume tube and the second shell are two independent structures. The second shell cover and the second shell can be connected in any existing way. A second accommodating cavity and a heating device are provided on the second shell. When in use, the second shell is preheated to the required temperature in advance by the heating device, the sampling tube to be thermally desorbed is placed in the sleeve module, the sleeve module is placed in the second accommodating cavity as a whole, and after the second shell cover is covered, the carrier gas is introduced from bottom to top for thermal desorption operation, and the gas is blown into the thermal desorption constant volume tube.

[0032] It can be seen that this solution can enable the thermal desorption operation in the pretreatment process to be automatically performed based on the existing CTC automatic sample injector, overcoming the defects of long time and high manpower consumption caused by the need to manually hold the sampling tube for a long time during the thermal desorption process.

[0033] Furthermore, the interior of the pyrolysis adsorption constant volume tube has a piston plate and a second lifting mechanism for driving the piston plate to rise and fall, and a sampling port is arranged at the top of the pyrolysis adsorption constant volume tube; it also includes an air inlet pipe, the top end of which is located above the piston plate inside the pyrolysis adsorption constant volume tube, and the bottom end of the air inlet pipe is located at the bottom of the pyrolysis adsorption constant volume tube and is connected to the second exhaust port.

[0034] In this solution, the piston plate divides the interior of the thermal desorption gas constant volume tube into two upper and lower areas, and the second lifting mechanism drives the piston plate up and down to drive the gas. Specifically, the gas after thermal desorption by the second shell enters the interior of the thermal desorption gas constant volume tube from the air inlet pipe and is located in the area above the piston plate; the second lifting mechanism drives the piston plate upward to squeeze the gas inside toward the sampling port. The sampling port in this solution can be matched with the injection needle of the corresponding CTC automatic sampler, and no specific limitation is made here; the injection needle is moved by the robotic arm, and the sample can be injected into the GC, GC / MS injection port to complete the injection process.

[0035] It can be seen that this scheme realizes gas injection from bottom to top in an actively driven manner. While fully automating the injection, there is no negative pressure in the entire operation process. Therefore, in the process from the constant volume tube to the injection needle, there is no situation where the gas pressure in the injection needle is inconsistent with that in the constant volume tube, resulting in the actual injection volume being less than the calibrated injection volume.

[0036] Furthermore, this solution can achieve stable automatic injection operation without modifying the injection port of the GC or GC / MS.

[0037] It should be noted that the first lifting mechanism and the second lifting mechanism in the present application can be implemented by any height adjustment technology that can be implemented by technical personnel in this field, and no specific limitation is made here.

[0038] The pretreatment method based on the fully automatic system for labeling and thermal desorption in the present application includes a labeling step and / or a thermal desorption step;

[0039] The labeling step comprises:

[0040] placing a cannula module containing sampling tubes to be calibrated on a tray;

[0041] The robotic arm of the CTC automatic sampler grabs the sleeve module on the tray and moves it to the label making module for label making.

[0042] The thermal desorption step comprises:

[0043] placing a cannula module containing sampled sampling tubes on a tray;

[0044] The robotic arm of the CTC automatic sampler grabs the sleeve module on the tray and moves it into the thermal desorption module;

[0045] Perform thermal desorption operation.

[0046] Furthermore, the labeling operation includes:

[0047] Closing the first shell cover in the label making module by means of a robotic arm;

[0048] Inject standard solution into the standard making module;

[0049] Blow carrier gas into the label making module from top to bottom.

[0050] Furthermore, the thermal desorption operation includes:

[0051] Preheating the second shell in the thermal desorption module to a set temperature in advance by a heating device;

[0052] Closing the second shell cover in the thermal desorption module by a robotic arm;

[0053] Blowing carrier gas into the second shell from bottom to top, and blowing a set volume of desorption gas into the thermal desorption gas constant volume pipe;

[0054] The sampling needle is inserted from the top of the thermal desorption gas constant volume tube by the robotic arm, and the desorption gas is pressed into the sampling needle.

[0055] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0056] 1. The gas sampling tube label and thermal desorption fully automatic processing system and method based on the CTC automatic sampler of the present invention solves the problem that the pre-processing operation in the prior art is heavily dependent on manual work. The staff only needs to regularly or periodically replace the corresponding sampling tubes in each sleeve module according to specific work needs, and place them in the designated holes on the tray. The entire pre-processing process can be automatically completed based on the existing structure of the CTC automatic sampler, which significantly reduces manpower consumption, thereby improving work efficiency and reducing work errors.

[0057] 2. The present invention realizes the integrated operation of labeling and thermal desorption, ensuring that labeling and thermal desorption can be automatically completed by the same system; and realizes continuous sampling of the sampling tube. Due to the use of the sleeve module, the contact area with the outside air before thermal desorption is small, reducing exogenous pollution.

[0058] 3. The present invention does not require modification of the sample inlet of the original gas chromatograph or gas chromatography-mass spectrometer in the laboratory, thus avoiding destructive modification of the instrument and equipment and adverse effects on the sensitivity of the instrument itself.

[0059] 4. The structure of the present invention is simple and compact, and does not take up too much space. Compared with the bulky automatic thermal desorption instrument in the prior art, it is more suitable for promotion and application in grassroots disease control departments with limited funds and site conditions.

[0060] 5. The present invention can meet the use of sampling tubes of different lengths, significantly improves the versatility of the present solution, and is conducive to adapting to sampling tubes of different specifications.

[0061] 6. The present invention can add a pre-processing function to the existing CTC automatic sample injector, expand its ability to pre-process the sampling tube, and fill the gap in the prior art. BRIEF DESCRIPTION OF THE DRAWINGS

[0062] The drawings described herein are used to provide a further understanding of the embodiments of the present invention, constitute a part of this application, and do not constitute a limitation of the embodiments of the present invention. In the drawings:

[0063] Figure 1 It is an overall schematic diagram of a specific embodiment of the present invention;

[0064] Figure 2 A perspective view of a casing module in a specific embodiment of the present invention;

[0065] Figure 3 is a cross-sectional view of a sleeve module in a specific embodiment of the present invention;

[0066] Figure 4 It is a structural schematic diagram of a label making module in a specific embodiment of the present invention;

[0067] Figure 5 It is a cross-sectional view of a label making module in a specific embodiment of the present invention;

[0068] Figure 6 A perspective view of a thermal desorption module in a specific embodiment of the present invention;

[0069] Figure 7 A cross-sectional view of a thermal desorption module in a specific embodiment of the present invention;

[0070] Figure 8 It is a structural schematic diagram of a spare label making module in a specific embodiment of the present invention;

[0071] Fig. 9 It is a cross-sectional view of the spare label making module in a specific embodiment of the present invention.

[0072] Marks and corresponding parts names in the attached drawings:

[0073] 1-tube module, 101-tube body, 102-tube cap, 103-first cavity, 104-second cavity, 105-exhaust channel, 106-carrying plate, 107-intake channel, 108-first lifting mechanism, 2-tray, 3-labeling module, 301-first shell, 302-air-permeable partition, 303-first accommodating cavity, 304-first shell cover, 305-injection channel, 306-gas collecting cavity, 307-first air inlet, 308-first exhaust port, 4-thermal desorption module, 401-second shell, 402- The second accommodating chamber, 403-the second shell cover, 404-the thermal decomposition adsorption constant volume tube, 405-the second air inlet, 406-the second exhaust port, 407-the piston plate, 408-the second lifting mechanism, 409-the sampling port, 410-the air inlet pipe, 411-the hose, 412-the baffle, 501-the shell, 502-the load-bearing air permeable plate, 503-the third accommodating chamber, 504-the third shell cover, 505-the spare injection channel, 506-the third air inlet, 507-the third exhaust port, 508-the spare gas collecting chamber, 509-the third lifting mechanism. DETAILED DESCRIPTION

[0074] In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with the examples and the accompanying drawings. The schematic embodiments of the present invention and the description thereof are only used to explain the present invention and are not intended to limit the present invention. In the description of the present application, it should be understood that the orientation or positional relationship indicated by terms such as "front", "rear", "left", "right", "up", "down", "vertical", "horizontal", "high", "low", "inside", "outside", etc. is based on the orientation or positional relationship shown in the accompanying drawings, and is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the scope of protection of the present application.

[0075] Embodiment 1:

[0076] like Figure 1 The gas sampling control label and thermal desorption automatic processing system based on CTC automatic sampler shown includes:

[0077] The casing module 1 is used to accommodate the sampling tube;

[0078] A tray 2, used for placing a plurality of casing modules 1;

[0079] The labeling module 3 is used to accommodate the sleeve module 1 and perform labeling operations on the sampling tubes in the sleeve module 1;

[0080] The thermal desorption module 4 is used to accommodate the casing module 1 and perform thermal desorption on the sampling tube in the casing module 1 .

[0081] The casing module 1 in this embodiment is as follows Figure 2 and Figure 3 As shown, it includes a tube body 101 and a tube cap 102 that match each other. The sleeve module 1 has a first cavity 103 for accommodating a sampling tube, and the first cavity 103 is partially located in the tube body 101 and partially located in the tube cap 102; a second cavity 104 is also arranged in the tube body 101, and the second cavity 104 is located below the first cavity 103, and the bottom end of the first cavity 103 is connected to the second cavity 104; an air inlet channel 107 connected to the first cavity 103 is arranged on the tube cap 102, and the second cavity 104 is connected to the exhaust channel 105.

[0082] The sleeve module 1 further includes a bearing plate 106 slidably connected to the second cavity 104 along the longitudinal direction, and the bearing plate 106 is movably sleeved outside the exhaust channel 105; and further includes a first lifting mechanism 108 for adjusting the height of the bearing plate 106.

[0083] In this embodiment, the tube body 101 and the tube cap 102 are connected by threads; the bearing plate 106 is made of a metal mesh; and the exhaust channel 105 is coaxial with the first cavity 103 .

[0084] In one or more embodiments, the first lifting mechanism 108 can be implemented by using common lifting equipment such as a hydraulic cylinder, a pneumatic cylinder, an electric push rod, a scissor lift, etc.

[0085] In one or more preferred embodiments, the first lifting mechanism 108 includes a screw fixedly connected to the supporting plate 106, the screw passes through the side wall of the tube body 13 and is connected to a fixing nut, a longitudinally extending straight groove is provided on the side wall of the tube body 13, and the screw is dynamically sealed with the straight groove.

[0086] In one or more preferred embodiments, the first lifting mechanism 108 includes a gear rotatably connected to the supporting plate 106, a rack meshing with the gear, the rack is arranged on the inner wall of the tube body 13 and extends longitudinally, and also includes a motor with a self-locking function for driving the gear to rotate.

[0087] Embodiment 2:

[0088] A gas sampling control label and thermal desorption fully automatic processing system based on a CTC automatic sampler. Based on Example 1, this example describes the label making module 3 and the thermal desorption module 4 in detail.

[0089] The labeling module 3 of this embodiment is as follows Figure 4 and Figure 5As shown, it includes a first shell 301, a breathable partition 302 located in the first shell 301, and a plurality of first accommodating chambers 303 located above the breathable partition 302; it also includes a first shell cover 304 matching the first shell 301, and the first shell cover 304 is provided with injection channels 305 corresponding to the first accommodating chambers 303 one by one; the first shell cover 304 is provided with a first air inlet 307 connected to each injection channel 305, and the first shell 301 bottom is provided with a first exhaust port 308; the first shell 301 has an air collecting chamber 306 inside, the breathable partition 302 is fixed in the air collecting chamber 306, the bottom end of the first accommodating chamber 303 is connected to the top end of the air collecting chamber 306, and the top end of the first exhaust port 308 is connected to the bottom end of the air collecting chamber 306; the inner diameter of the first accommodating chamber 303 is equal to the outer diameter of the sleeve module 1.

[0090] The first shell cover 304 is slidably fitted on the top of the first shell 301 , and the first shell cover 304 is configured to be an L-shaped structure that matches the mechanical arm of the CTC automatic sample injector.

[0091] Preferably, corresponding one-way valves may be provided at the first air inlet 307 and the first air outlet 308 to prevent the fluid from flowing back.

[0092] The thermal desorption module 4 in this embodiment is as follows Figure 6 and Figure 7 As shown, it includes a thermal decomposition gas absorption constant volume pipe 404, a second shell 401, a second accommodating cavity 402 opened on the second shell 401, and a second shell cover 403 matching the second shell 401;

[0093] A heating device is arranged in the second shell 401, and a plurality of temperature sensors are arranged on the inner wall of the second accommodating cavity 402; a controller connected to the heating device and the temperature sensor is also included, and is used to control the preheating temperature in real time.

[0094] The second accommodating chamber 402 is used to accommodate the sleeve module 1 . A second air inlet 405 is disposed at the bottom of the second accommodating chamber 402 . A second exhaust port 406 is disposed on the second shell cover 403 . The second exhaust port 406 is connected to the thermal decomposition gas constant volume pipe 404 .

[0095] The interior of the thermal decomposition gas adsorption constant volume tube 404 is provided with a piston plate 407 and a second lifting mechanism 408 for driving the piston plate 407 to rise and fall, and a sampling port 409 is arranged at the top of the thermal decomposition gas adsorption constant volume tube 404; it also includes an air inlet pipe 410, the top end of the air inlet pipe 410 is located above the piston plate 407 inside the thermal decomposition gas adsorption constant volume tube 404, and the bottom end of the air inlet pipe 410 is located at the bottom of the thermal decomposition gas adsorption constant volume tube 404 and is connected to the second exhaust port 406.

[0096] The heating device in this embodiment can be implemented by any existing heating technology, such as a heating resistor wire embedded in the second housing 401. In addition, the second lifting mechanism 408 can be implemented by common lifting equipment such as a hydraulic cylinder, a pneumatic cylinder, an electric push rod, a scissor lift, etc.; when the second lifting mechanism 408 drives the piston plate 407 to reach the top of the stroke, the top of the intake pipe 410 is still located above the piston plate 407.

[0097] In this embodiment, the second exhaust port 406 matches the air inlet channel 107 in the sleeve module; when the sleeve module is installed in the second accommodating cavity 402 and the second shell cover 403 is closed, the second exhaust port 406 faces the air inlet channel 107, and the two are connected to each other.

[0098] In addition, the second exhaust port 406 is connected to the air inlet pipe 410 via a hose 411. A one-way valve may be provided on the hose 411, the air inlet pipe 410, the sampling port 409, etc. to prevent fluid from flowing back.

[0099] Preferably, the second shell cover 403 in this embodiment is further provided with a baffle 412 , and the baffle 412 and the second shell cover 403 together form an L-shaped structure for matching with the mechanical arm of the CTC automatic sample injector.

[0100] This embodiment uses the existing structure of the CTC automatic sampler to achieve continuous sampling of the sampling tube; and due to the use of the sleeve module, the contact area with the outside air before thermal desorption is small, reducing exogenous pollution.

[0101] In addition, the structure of this embodiment is relatively small, and the width of the labeling module 3 and the thermal desorption module 4 are both less than 15 cm, thus greatly saving laboratory bench space; there is no need to modify the GC or GC / MS injection port, and when necessary, the labeling module 3 or the thermal desorption module 4 can be removed and moved to other CTC injectors.

[0102] In one or more preferred embodiments, the tube body 101 , the tube cap 102 and the second shell 401 may all be made of heat-conducting materials, such as metal materials with good heat conduction performance.

[0103] In one or more preferred embodiments, the thermal decomposition absorption constant volume tube 404 is made of a material that is pressure-resistant, has good chemical stability, and has strong structural rigidity, such as tempered glass.

[0104] Embodiment 3:

[0105] A pretreatment method for a CTC automatic sample injector is implemented based on the fully automatic labeling and thermal desorption system in Example 1 or 2, and the method includes a labeling step and a thermal desorption step.

[0106] 1. The steps of label making include:

[0107] S1. When there is a need to calibrate a batch of sampling tubes, the sampling tubes to be calibrated are placed into the casing module 1;

[0108] S2, placing the sleeve module 1 containing the sampling tube to be calibrated on the tray 2;

[0109] S3. The robot arm of the CTC automatic sampler grabs the designated sleeve module 1 on the tray 2 and moves it to the label making module 3 to perform label making operation.

[0110] The process of placing the sampling tube to be calibrated into the casing module 1 includes:

[0111] S101, adjusting the height of the carrying plate 106 by the first lifting mechanism 108, so that the distance from the carrying plate 106 to the top of the first cavity 103 is equal to or greater than the length of the sampling tube to be calibrated;

[0112] S102, open the tube cap 102, put the sampling tube to be calibrated into the first cavity 103, and gradually insert the exhaust channel 105 from the bottom end into the sampling tube to be calibrated until the bottom end of the sampling tube to be calibrated reaches the surface of the carrier plate 106;

[0113] S103 , reconnect the tube cap 102 to the tube body 101 .

[0114] The process of making the standard includes:

[0115] S301, closing the first shell cover 304 in the label making module by a mechanical arm;

[0116] S302, the robotic arm draws the standard solution through the injection needle, and injects the standard solution into the label making module 3 located in the first accommodating cavity 303 through the injection channel 305;

[0117] S303, introducing carrier gas into the label making module through the first air inlet 307; the carrier gas enters the interior of the sampling tube through the air inlet channel 107, and passes through the exhaust channel 105, the air permeable partition 302, the gas collecting cavity 306 and the first exhaust port 308 from top to bottom, and then exits the label making module and enters the chromatograph or gas chromatograph-mass spectrometer;

[0118] S304, obtaining a chromatogram through analysis by a chromatograph or a gas chromatography-mass spectrometer;

[0119] S305, drawing a working curve: 5-7 standard solutions with different gradient concentrations are respectively injected into 5-7 gas sampling tubes, and after being processed in this embodiment, they are respectively processed in GC or GC / MS, and a linear working curve is drawn according to the integrated peak area of ​​the spectrum, which is used as a quantitative basis;

[0120] Analysis of analytical efficiency: Inject the standard solution of the same concentration into 10 gas sampling tubes respectively, quantify the integrated peak area of ​​its spectrum through the working curve, calculate the mean of the component in the 10 gas sampling tubes, and divide this mean by the actual injected concentration value to obtain the analytical efficiency.

[0121] Second, the thermal desorption step includes:

[0122] S4. When the CTC automatic sampler has a thermal desorption requirement before sample injection, the sampled sampling tube is placed into the sleeve module 1;

[0123] S5, placing the cannula module 1 containing the sampled sampling tube on the tray 2;

[0124] S6, using the mechanical arm of the CTC automatic sampler to grab the sleeve module 1 on the tray 2 and move it into the thermal desorption module 4;

[0125] S7. Perform thermal desorption operation.

[0126] The process of placing the sampled sampling tube into the casing module 1 includes:

[0127] S401, cutting open the sealed ends of the sampling tube and placing it in the sleeve module 1; the cutting method can be achieved by using equipment such as an ampoule grinding wheel;

[0128] S402, adjusting the height of the carrier plate 106 to match the cut sampling tube through the first lifting mechanism 108; matching here means that the distance from the carrier plate 106 to the top of the first cavity 103 is equal to or greater than the length of the corresponding sampling tube;

[0129] S402, open the tube cap 102, put the sampling tube into the first cavity 103, and gradually insert the exhaust channel 105 into the sampling tube from the bottom until the bottom of the sampling tube reaches the surface of the carrier plate 106;

[0130] S403 , reconnect the tube cap 102 to the tube body 101 .

[0131] The process of thermal desorption operation includes:

[0132] S701, preheating the second shell 401 in the thermal desorption module to a set temperature by a heating device;

[0133] S702, closing the second shell cover 403 in the thermal desorption module by a mechanical arm;

[0134] S703, injecting carrier gas into the second housing 401 from bottom to top, that is, making the carrier gas enter the second accommodating chamber 402 from the second air inlet 405, and sequentially pass through the exhaust channel 105, the first cavity 103, the air inlet channel 107, the second exhaust port 406, and enter the hose 411 and the air inlet pipe 410, until the set volume of desorption gas is purged into the thermal desorption gas constant volume pipe 404;

[0135] S704, inserting the sampling needle of the CTC automatic sampler into the sampling port 409 at the top of the thermal desorption constant volume tube 404 through the mechanical arm;

[0136] S705 , the piston plate 407 is driven upward by the second lifting mechanism 408 to press the desorbed gas into the injection needle, thereby completing the injection process.

[0137] In this embodiment, the carrier gas used is nitrogen.

[0138] Embodiment 4:

[0139] Based on any of the above embodiments, the fully automatic labeling and thermal desorption system also includes a spare labeling module.

[0140] The injection needle used to inject the standard solution into the label making module in any of the above embodiments is preferably a headspace injection needle, which has a capacity of 1 ml, is larger and has a thicker needle than the injection needle of the gas sampling tube, and is more suitable for this application. However, since the injection needle needs to be replaced after each blowing, some old-fashioned CTC automatic samplers may not have the function of automatically switching the injection needle, and can only rely on the traditional 10uL injection needle to blow in the standard solution; and this type of 10uL injection needle needs to be replaced manually. Therefore, this type of old-fashioned CTC automatic sampler may not be suitable for fully automatic operation using the label making module recorded in Example 1 or 2. This embodiment overcomes this problem by providing a spare label making module for the system.

[0141] Specifically, the standby label making module is as follows: Figure 8 and Fig. 9 As shown, it includes a shell 501, a bearing air-permeable plate 502 located in the shell 501, and a plurality of third accommodating cavities 503 located above the bearing air-permeable plate 502; it also includes a third shell cover 504 hinged to the shell 501, and the third shell cover 504 is provided with spare injection channels 505 corresponding to the third accommodating cavities 503 one by one; the third shell cover 504 is provided with a third air inlet 506 connected to each spare injection channel 505, and the shell 501 bottom is provided with a third exhaust port 507.

[0142] The shell 501 has a spare gas collecting chamber 508 inside, the bearing air permeable plate 502 is located in the spare gas collecting chamber 508, the bottom end of the third accommodating chamber 503 is connected to the top of the spare gas collecting chamber 508, and the top end of the third exhaust port 507 is connected to the bottom end of the spare gas collecting chamber 508.

[0143] In this embodiment, the inner diameter of the third accommodating chamber 503 is equal to the outer diameter of the sampling tube; the bearing air permeable plate 502 is slidably connected in the standby gas collecting chamber 508 along the longitudinal direction, and also includes a third lifting mechanism 509 for adjusting the height of the bearing air permeable plate 502; the third shell cover 504 is hinged on the top of the shell 501; the bearing air permeable plate 502 uses a metal mesh. In addition, the standby injection channel 505 vertically penetrates the third shell cover 504; the third air inlet 506 is horizontally opened on the side wall of the third shell cover 504.

[0144] In a more preferred embodiment, the inner wall of the spare air collecting cavity 508 is provided with a guide rail for supporting the air permeable plate 502 to slide.

[0145] In one or more implementations, the third lifting mechanism 509 can be implemented using common lifting equipment such as a hydraulic cylinder, a pneumatic cylinder, an electric push rod, a scissor lift, etc.

[0146] The use of the spare label making module of this embodiment to replace the label making module described in Embodiment 1 or 2 can be more suitable for the use of CTC automatic sample injectors that cannot automatically switch the injection needle. When the spare label making module is used for label making, there is no need to put the sampling tube into the sleeve module, but directly put the sampling tube into the third accommodating cavity 503, and the use of sampling tubes of different lengths can be adapted by adjusting the height of the bearing air permeable plate 502.

[0147] The specific implementation methods described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific implementation method of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

[0148] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In addition, the term "connected" used in this article can be directly connected or indirectly connected via other components without special explanation.

Claims

1. A gas sampling control label and thermal desorption automatic processing system based on a CTC automatic sampler, characterized in that: include: A casing module (1) for accommodating a sampling tube; A tray (2) for placing a plurality of casing modules (1); A labeling module (3) is used to accommodate the sleeve module (1) and perform labeling operations on the sampling tube in the sleeve module (1); A thermal desorption module (4) is used to accommodate the casing module (1) and perform a thermal desorption operation on the sampling tube in the casing module (1); The sleeve module (1) comprises a tube body (101) and a tube cap (102) which match each other. The sleeve module (1) has a first cavity (103) for accommodating a sampling tube, and the first cavity (103) is partially or completely located in the tube body (101); a second cavity (104) is also arranged in the tube body (101), and the second cavity (104) is located below the first cavity (103), and the bottom end of the first cavity (103) is connected to the second cavity (104); an air inlet channel (107) connected to the first cavity (103) is arranged on the tube cap (102), and the second cavity (104) is connected to the exhaust channel (105); the sleeve module also comprises a bearing plate which is slidably connected to the second cavity in the longitudinal direction, and the height of the bearing plate is adjustable; The labeling module (3) comprises a first shell (301), a breathable baffle (302) located in the first shell (301), and a plurality of first accommodating chambers (303) located above the breathable baffle (302); further comprising a first shell cover (304) matched with the first shell (301), wherein the first shell cover (304) is provided with injection channels (305) corresponding to the first accommodating chambers (303) one by one; the first shell cover (304) is provided with a first air inlet (307) connected to each injection channel (305), and a first exhaust port (308) is provided at the bottom of the first shell (301); the first shell (301) has an air collecting chamber (306) inside, the breathable baffle (302) is located in the air collecting chamber (306), the bottom end of the first accommodating chamber (303) is connected to the top end of the air collecting chamber (306), and the top end of the first exhaust port (308) is connected to the bottom end of the air collecting chamber (306); The thermal desorption module (4) comprises a thermal desorption gas constant volume pipe (404), a second shell (401), a second accommodating chamber (402) provided on the second shell (401), and a second shell cover (403) matching the second shell (401); A heating device is arranged in the second shell (401); The second accommodating chamber (402) is used to accommodate the sleeve module (1); a second air inlet (405) is provided at the bottom of the second accommodating chamber (402); and a second exhaust port (406) is provided on the second shell cover (403); the second exhaust port (406) is connected to the thermal decomposition gas absorption constant volume pipe (404); The interior of the pyrolysis gas absorption constant volume tube (404) comprises a piston plate (407) and a second lifting mechanism (408) for driving the piston plate (407) to rise and fall, and a sampling port (409) is arranged at the top of the pyrolysis gas absorption constant volume tube (404).

2. The gas sampling control label and thermal desorption automatic processing system based on CTC automatic sampler according to claim 1 is characterized in that: The bearing plate (106) is movably sleeved outside the exhaust passage (105); and also includes a first lifting mechanism (108) for adjusting the height of the bearing plate (106).

3. The gas sampling control label and thermal desorption automatic processing system based on CTC automatic sampler according to claim 1 is characterized in that: The air-permeable partition plate (302) is fixedly connected in the gas collecting cavity (306), and the inner diameter of the first accommodating cavity (303) is equal to the outer diameter of the sleeve module (1).

4. The gas sampling control label and thermal desorption automatic processing system based on CTC automatic sampler according to claim 1 is characterized in that: It also includes an air intake pipe (410), the top end of which is located above the piston plate (407) inside the thermal decomposition gas absorption constant volume pipe (404), and the bottom end of which is located at the bottom of the thermal decomposition gas absorption constant volume pipe (404) and is connected to the second exhaust port (406).

5. A processing method based on the gas sampling control mark and thermal desorption automatic processing system according to any one of claims 1 to 4, characterized in that: The method comprises a labeling step and a thermal desorption step; The labeling step comprises: Placing a cannula module (1) containing a sampling tube to be calibrated on a tray (2); Using a mechanical arm of the CTC automatic sampler, the sleeve module (1) on the tray (2) is grasped and moved to the labeling module (3) to perform labeling operations; The thermal desorption step comprises: Placing a cannula module (1) containing a sampled sampling tube on a tray (2); Using a mechanical arm of the CTC automatic sample injector, grab the sleeve module (1) on the tray (2) and move it into the thermal desorption module (4); Perform thermal desorption operation.

6. The processing method according to claim 5, characterized in that: The labeling work includes: Closing the first shell cover (304) in the labeling module (3) by means of a mechanical arm; Injecting a standard solution into the standard preparation module (3); The carrier gas is blown into the label making module (3) from top to bottom.

7. The processing method according to claim 5, characterized in that: The thermal desorption operation comprises: Preheating the second shell (401) in the thermal desorption module (4) to a set temperature in advance by means of a heating device; Closing the second shell cover (403) in the thermal desorption module (4) by means of a mechanical arm; Blowing a carrier gas into the second shell (401) from bottom to top, and blowing a set volume of desorption gas into the thermal desorption gas constant volume pipe (404); The sampling needle is inserted from the top of the thermal desorption gas constant volume tube (404) by the mechanical arm, and the desorption gas is pressed into the sampling needle.

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