CN117524833A - Thermal desorption ionization device and application thereof in ion trap mass spectrum - Google Patents
Thermal desorption ionization device and application thereof in ion trap mass spectrum Download PDFInfo
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- CN117524833A CN117524833A CN202210896720.5A CN202210896720A CN117524833A CN 117524833 A CN117524833 A CN 117524833A CN 202210896720 A CN202210896720 A CN 202210896720A CN 117524833 A CN117524833 A CN 117524833A
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- 238000003795 desorption Methods 0.000 title claims abstract description 85
- 238000001819 mass spectrum Methods 0.000 title claims description 17
- 238000005040 ion trap Methods 0.000 title claims description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000000534 ion trap mass spectrometry Methods 0.000 claims abstract description 5
- 239000012159 carrier gas Substances 0.000 claims description 18
- 238000005485 electric heating Methods 0.000 claims description 17
- 238000005070 sampling Methods 0.000 claims description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- 230000003287 optical effect Effects 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000003814 drug Substances 0.000 claims description 8
- 229940079593 drug Drugs 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000002360 explosive Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000005587 bubbling Effects 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000575 pesticide Substances 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 12
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000002347 injection Methods 0.000 description 9
- 239000007924 injection Substances 0.000 description 9
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 238000004949 mass spectrometry Methods 0.000 description 3
- MYWUZJCMWCOHBA-VIFPVBQESA-N methamphetamine Chemical compound CN[C@@H](C)CC1=CC=CC=C1 MYWUZJCMWCOHBA-VIFPVBQESA-N 0.000 description 3
- 229960001252 methamphetamine Drugs 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- -1 acetone dimer ions Chemical class 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000001871 ion mobility spectroscopy Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 229940035674 anesthetics Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003193 general anesthetic agent Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000021 stimulant Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004885 tandem mass spectrometry Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
- H01J49/049—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample with means for applying heat to desorb the sample; Evaporation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
- G01N27/628—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas and a beam of energy, e.g. laser enhanced ionisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/161—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission using photoionisation, e.g. by laser
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a rapid thermal desorption ionization device and application thereof in ion trap mass spectrometry. A thermal desorption ionization device mainly comprises a desorption ionization cavity, a VUV lamp and a heating lamp. The advantages are that: and the ionization region and the desorption region are perfectly combined, so that the detection sensitivity is improved.
Description
Technical Field
The invention relates to a rapid thermal desorption ionization device and application thereof in ion trap mass spectrometry, in particular to a device integrating rapid thermal desorption and ionization functions, which can realize full ionization reaction between a sample and reaction ions, thereby improving ionization efficiency and detection sensitivity.
Background
The demand and development of miniaturized mass spectrometry has very good prospect in many fields and becomes a research hotspot. The ion trap mass spectrum has the functions of MS/MS, can bear higher pressure (such as 0.1 Pa), has the advantages of smaller volume, low cost and the like, and is widely used for detecting drugs, stimulants, anesthetics and explosives. There is a great need for good detection instruments in various fields such as environment, public safety, etc. The invention provides an organic combination of desorption and ionization which can realize high efficiency under the atmospheric pressure on the basis of the requirement.
Workflow of ion trap: the solid and liquid samples are put into a thermal desorption sample injector to be gasified, and the solid and liquid samples are carried by carrier gas to enter an ionization region; ionization is realized by combining with the reaction ions in an ionization region; and then enters an ion trap mass spectrum through a sample injection capillary for detection. The final detection sensitivity is determined by the efficiency of thermal desorption and ionization at atmospheric pressure and the detection performance of the back-end mass spectrum. And the detection performance of the back-end mass spectrum is limited by the performance of the device, so that the device is difficult to significantly improve. How to achieve the efficiency of thermal desorption and ionization at atmospheric pressure is a hotspot of current research. Jiang Jichun et al (patent number CN 201911258506.1) discloses an in situ thermal desorption ionization source for mass spectrometry. The invention relates to a mass spectrometry instrument, in particular to an in-situ thermal desorption ionization source, which comprises a gas source, a steady flow valve, a desorption cavity, a enrichment pipe, an ion photon generating device, an ionization pipe, an ion transmission cavity, an ion transmission electrode and a mass spectrometer. According to the invention, through reasonable design, the thermal desorption device and the ion photon generation device are tightly combined, so that sample molecules sucked by thermal desorption are fully contacted with ions or photons generated by the ion photon generation device, and high-efficiency ionization is obtained. The disadvantage is that it is aimed at gaseous samples. Li Haiyang et al disclose a pulse-purge negative pressure thermal desorption sample-feeding method and injector for ion mobility spectrometry (application number: CN202111535952. X). Pulse purge, negative pressure and thermal desorption techniques are combined to detect solid, liquid and gaseous samples. And the sample to be tested is heated under a negative pressure state to generate a phase change process, and gaseous sample molecules are carried into an ion mobility spectrometry by carrier gas purged through pulses to carry out ionization and detection. The method is suitable for detecting substances to be detected in solid, liquid or gaseous matrixes, the application range of a sample is enlarged, a complex sample pretreatment process is not needed, the effective sample injection amount of the sample is increased by means of the combination of carrier gas pulse purging, negative pressure sampling and thermal desorption in a sealed sample injection cavity, and the reaction efficiency of the sample is improved. The disadvantage is that the direct transfer losses of the desorption and ionization chambers are severe.
The invention can solve the problem, and can realize the high-efficiency thermal desorption of solid and liquid samples by utilizing a unique structural design; meanwhile, the gasified target molecules can fully react with the reaction ions in space, so that the ionization efficiency is improved, and the sensitivity is improved.
Disclosure of Invention
The invention relates to a rapid thermal desorption ionization device in an analysis instrument. The device integrating rapid thermal desorption and ionization functions can realize sufficient ionization reaction between a sample and reaction ions, so that ionization efficiency and detection sensitivity are improved.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the thermal desorption ionization device mainly comprises a desorption ionization cavity, a VUV lamp and a heating lamp;
wherein the desorption ionization chamber is a hollow closed chamber,
a sample table is arranged at the lower bottom surface in the desorption ionization cavity, and an electric heating element is arranged in the wall surface where the lower bottom surface in the desorption ionization cavity is positioned; a temperature sensing element is arranged in the wall surface of the desorption ionization cavity below the sample table;
a first light window is arranged on the upper wall surface of the desorption ionization cavity above the sample table, a heating lamp is arranged above the first light window outside the desorption ionization cavity, and light emitted by the heating lamp irradiates the sample table through the first light window;
1-6 (preferably 2, 3 or 4) second light windows are arranged on the side wall surface of the desorption ionization cavity, VUV lamps (vacuum ultraviolet lamps) are arranged at the second light windows outside the desorption ionization cavity, and light emitted by the VUV lamps irradiates an area above the sample table through the second light windows;
an outlet is arranged on the right side of the upper wall surface of the desorption ionization cavity, and a carrier gas inlet is arranged on the right side of the lower wall surface of the desorption ionization cavity; and a capillary sampling port is arranged on the side wall surface of the desorption ionization cavity.
The electric heating element is one or more than two of an electric heating wire and an electric heating rod electric heating belt of an electric heating block; the temperature sensing element is a thermocouple.
The upper surface of the sample table is provided with a groove for placing a sample; the light emitted by the heating lamp irradiates the sample placement position in the groove through the first light window (9).
The desorption ionization cavity is made of high-temperature resistant materials, and the materials can be one or more than two of metal, quartz and ceramic;
the first light window and the second light window are respectively formed by arranging a through hole on the wall surface of the desorption ionization cavity and arranging a transparent quartz glass sheet in the through hole, and the peripheral edges of the quartz glass sheet are hermetically connected with the inner wall surface of the through hole.
The heating lamp is an infrared lamp, and the power is 30W to 300W; the heating time is pulse type, and the opening time is between 10 microseconds and 10 seconds.
The sample is solid and/or liquid;
the carrier gas inlet is connected with a carrier gas source through a bubbling bottle filled with a reagent or a reagent volatilization bottle filled with a reagent, and gas carrying the reagent is introduced into the carrier gas inlet;
the carrier gas is air and/or nitrogen; the reagent is one or more of ketone, benzene series, alcohol and chlorinated hydrocarbon.
One end of a sampling capillary tube passing through the ion trap mass spectrum is inserted into the desorption ionization cavity through a sampling port, and the other end of the sampling capillary tube is connected with the ion trap mass spectrum to perform the combination of the thermal desorption ionization device in the ion trap mass spectrum.
The method is used for detecting one or more than two of drugs, explosives, pesticides and medicines. .
The invention has the beneficial effects that: the device with the rapid thermal desorption and ionization functions can be combined with an ion trap mass spectrum to realize the full ionization reaction of the sample and the reaction ions, so that the ionization efficiency and the detection sensitivity are improved.
Drawings
FIG. 1 is a schematic diagram of a thermal desorption ionization device;
the system comprises a desorption ionization cavity, a heating lamp, a 3.VUV lamp, a temperature measuring module, a sample stage, a carrier gas inlet, an outlet, a capillary sampling port, a first optical window, a second optical window and an electric heating element, wherein the desorption ionization cavity, the heating lamp, the 3.VUV lamp, the temperature measuring module, the sample stage, the carrier gas inlet, the outlet, the capillary sampling port, the first optical window, the second optical window and the electric heating element are respectively arranged in sequence, and the electric heating element is arranged in sequence;
FIG. 2 is a schematic diagram of a thermal desorption ionization device coupled with an ion trap mass spectrum;
the desorption ionization chamber 1, the heating lamp 2, the 3.VUV lamp 4, the temperature measuring module 5, the sample platform 6, the carrier gas inlet 7, the outlet 8, the capillary sampling port 9, the first optical window 10, the second optical window 11 and the electric heating element. DAPI (discontinuous pulse injection) injection system, 13 injection capillary, 14 end electrode pairs, 15 upper and lower electrode pairs, 16 side electrode pairs, 17 slits and 18 ion detector; ion trap mass spectrometry consisting of components 12-18;
FIG. 3 is a graph of the detection of methamphetamine.
Detailed Description
The invention is used for a pyrolysis light absorption ionization device for solid and liquid samples. Comprising the following steps: a metal desorption ionization chamber 1, a vacuum ultraviolet VUV lamp 3 with photon energy of 10.6eV and a halogen heating lamp 2 with power of 150W;
the desorption ionization chamber 1 is a hollow closed chamber, a sample table 5 is arranged at the lower bottom surface in the metal desorption ionization chamber 1, and an electric heating rod 11 is arranged in the wall surface where the lower bottom surface in the desorption ionization chamber 1 is positioned; a temperature sensing element PT100 is arranged in the wall surface of the metal desorption ionization cavity 1 below the sample table 5;
a first light window 9 is arranged on the upper wall surface of the desorption ionization chamber 1 above the sample table 5, a halogen heating lamp 2 is arranged above the first light window 9 outside the desorption ionization chamber 1, and the light emitted by the halogen heating lamp 2 irradiates the sample table 5 through the first light window 9;
2 second light windows 10 are arranged on the side wall surface of the metal desorption ionization chamber 1, 2 VUV lamps (vacuum ultraviolet lamps) are arranged at the second light windows 10 outside the desorption ionization chamber 1, and vacuum ultraviolet light emitted by the VUV lamps irradiates the area above the sample table 5 through the second light windows 10;
an outlet 7 is arranged on the right side of the upper wall surface of the metal desorption ionization chamber 1, and a carrier gas inlet 6 is arranged on the right side of the lower wall surface of the metal desorption ionization chamber 1; a capillary sampling port 8 is arranged on the side wall surface of the metal desorption ionization chamber 1.
The upper surface of the sample table 5 is provided with a groove for placing a sample; the light emitted from the halogen lamp 2 is irradiated to the sample placement place in the groove through the first light window 9.
The first optical window 9 and the second optical window 10 are respectively formed by arranging a through hole on the wall surface of the desorption ionization cavity 1 and arranging a transparent quartz glass sheet in the through hole, and the peripheral edges of the quartz glass sheet are hermetically connected with the inner wall surface of the through hole.
The pyrolytic light absorbing ionization device described above was used in conjunction with an ion trap mass spectrum. The process of detecting the sample is as follows:
as shown in fig. 1, during positive ion detection, reagent molecule acetone enters a desorption ionization cavity 1 through a photo-carrier gas inlet 6, and is photoionization of 10.6eV emitted by a VUV lamp 3 to generate acetone dimer ions; the drug sample on the sample table 5 is gasified under the action of the heating lamp 2, and reacts with acetone dimer ions to be ionized;
as shown in fig. 2, DAPI (discontinuous pulse sample injection, a silica gel tube with an electromagnetic pinch valve in the middle, wherein the electromagnetic pinch valve is in a pulse working mode, one end of the electromagnetic pinch valve is connected with a sampling capillary 14, the other end of the electromagnetic pinch valve is connected with a mass spectrum sample inlet through a sample injection capillary 23), and drug ions enter an ion trap mass spectrum through a sample injection capillary 13 under the action of air pressure difference; the electric potential well formed by the side electrode pair 16 is cooled and excited in the end electrode pair 14, the upper and lower electrode pairs 15, and then passes through the slit 17 in the side electrode pair 16 to be detected by the detector 18.
Drugs were detected based on the high-efficiency desorption ionization device and ion trap mass spectrometry described above. A typical spectrum of methamphetamine is shown in FIG. 3. A distinct peak of methamphetamine precursor ion spectrum was observed at the mass number 150 position.
Claims (9)
1. A thermal desorption ionization device, characterized in that:
mainly comprises a desorption ionization cavity (1), a VUV lamp (3) and a heating lamp (2);
wherein the desorption ionization chamber (1) is a hollow closed chamber,
a sample table (5) is arranged at the lower bottom surface in the desorption ionization cavity (1), and an electric heating element (11) is arranged in the wall surface where the lower bottom surface in the desorption ionization cavity (1) is positioned; a temperature sensing element is arranged in the wall surface of the desorption ionization cavity (1) below the sample table (5);
a first light window (9) is arranged at the upper wall surface of the desorption ionization cavity (1) above the sample table (5), a heating lamp (2) is arranged above the first light window (9) outside the desorption ionization cavity (1), and light emitted by the heating lamp (2) irradiates the sample table (5) through the first light window (9);
1-6 (preferably 2, 3 or 4) second light windows (10) are arranged on the side wall surface of the desorption ionization cavity (1), a VUV lamp (vacuum ultraviolet lamp) is arranged at the second light windows (10) outside the desorption ionization cavity (1), and light emitted by the VUV lamp irradiates an area above the sample table (5) through the second light windows (10);
an outlet (7) is arranged on the right side of the upper wall surface of the desorption ionization cavity (1), and a carrier gas inlet (6) is arranged on the right side of the lower wall surface of the desorption ionization cavity (1); a capillary sampling port (8) is arranged on the side wall surface of the desorption ionization cavity (1).
2. The thermal desorption ionization device of claim 1 wherein:
the electric heating element is one or more than two of an electric heating wire and an electric heating rod electric heating belt of an electric heating block;
the temperature sensing element is a thermocouple.
3. The thermal desorption ionization device of claim 1 wherein:
the upper surface of the sample table (5) is provided with a groove for placing a sample; the light emitted by the heating lamp (2) irradiates the sample placement position in the groove through the first light window (9).
4. The thermal desorption ionization device of claim 1 wherein:
the desorption ionization cavity (1) is made of high-temperature resistant materials, and the materials can be one or more than two of metal, quartz and ceramic;
the first optical window (9) and the second optical window (10) are respectively formed by arranging a through hole on the wall surface of the desorption ionization cavity (1) and arranging a transparent quartz glass sheet in the through hole, and the peripheral edges of the quartz glass sheet are hermetically connected with the inner wall surface of the through hole.
5. The thermal desorption ionization device of claim 1 wherein: the heating lamp (2) is an infrared lamp, and the power is 30W to 300W; the heating time is pulse type, and the opening time is between 10 microseconds and 10 seconds.
6. The thermal desorption ionization device of claim 1 wherein: the sample is solid and/or liquid;
the carrier gas inlet (6) is connected with a carrier gas source through a bubbling bottle filled with a reagent or a reagent volatilization bottle filled with a reagent, and the carrier gas inlet (6) is filled with gas carrying the reagent;
the carrier gas is air and/or nitrogen; the reagent is one or more of ketone, benzene series, alcohol and chlorinated hydrocarbon.
7. Use of a thermal desorption ionization device according to any one of claims 1 to 6 in ion trap mass spectrometry.
8. The use according to claim 7, wherein:
one end of a sampling capillary tube passing through the ion trap mass spectrum is inserted into the desorption ionization cavity (1) through a sampling port (8), and the other end of the sampling capillary tube is connected with the ion trap mass spectrum to perform the combination of the thermal desorption ionization device in the ion trap mass spectrum.
9. Use according to claim 7 or 8, characterized in that:
the method is used for detecting one or more than two of drugs, explosives, pesticides and medicines.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210896720.5A CN117524833A (en) | 2022-07-28 | 2022-07-28 | Thermal desorption ionization device and application thereof in ion trap mass spectrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210896720.5A CN117524833A (en) | 2022-07-28 | 2022-07-28 | Thermal desorption ionization device and application thereof in ion trap mass spectrum |
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| Publication Number | Publication Date |
|---|---|
| CN117524833A true CN117524833A (en) | 2024-02-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210896720.5A Pending CN117524833A (en) | 2022-07-28 | 2022-07-28 | Thermal desorption ionization device and application thereof in ion trap mass spectrum |
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| Country | Link |
|---|---|
| CN (1) | CN117524833A (en) |
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- 2022-07-28 CN CN202210896720.5A patent/CN117524833A/en active Pending
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