Mass spectrum characterization platform for full-process inert gas protection high-flux sample injection and use method

Abstract

The invention relates to a mass spectrum characterization platform for full-process inert gas protection high-flux sample introduction and a use method, and the mass spectrum characterization platform comprises a novel glove box which can be connected with a transfer cavity, a high-flux detection mass spectrum ionization source which is connected to a mass spectrometer, and an inert gas protection transfer cavity, batches of to-be-detected trace samples with different dimensions are sampled in a glove box on the basis of the inert gas shielding transfer cavity, and the inert gas shielding transfer cavity is connected with a high-throughput detection mass spectrum ionization source, so that high-throughput analysis that a plurality of samples are sequentially detected on a mass spectrometer in one-time sample loading is realized. The sample is in a protective gas atmosphere in the sampling, transferring and detecting processes.

Description

Technical Field

[0001] The present invention relates to the technical field of mass spectrometry analysis sample delivery, and in particular to a mass spectrometry characterization platform for high-throughput sampling under full-process inert gas protection and a method of using the platform. Background Art

[0002] For synthetic chemistry, many key reactions need to be carried out in a glove box that uses an inert gas protection atmosphere. However, currently commercialized glove boxes only have the function of manipulation and cannot perform complex operations such as sample pretreatment.

[0003] For example, a glove box laser selective melting device based on a vacuum oxygen-free environment with announcement number CN106541134B provides a water-free and oxygen-free glove box operating environment. The left side of the vacuum glove box is connected to the vacuum transition cabin through an isolation protection locking device, the left side of the vacuum transition cabin is provided with a door clamping device, the lower left side of the vacuum glove box is provided with a protective gas inlet, and the right side of the vacuum glove box is connected to the vacuum pump group through a vacuum pipeline. A vacuum glove box turnover cabin with announcement number CN206855492U includes an outer cabin door, a turnover cabin, an inner cabin door, and a turnover cabin hinge. The outer cabin door and the inner cabin door are respectively rotatably connected to the two ends of the turnover cabin through the turnover cabin hinge. A vacuum glove box that is easy to adjust quickly with announcement number CN216731895U provides a vacuum glove box that is easy to adjust quickly, including a glove box and a transition box connected in sequence, a first through hole is provided in the middle of one end of the glove box, and a second through hole connected to the transition box is provided at the lower part of the other end, and an arc-shaped cover is provided on the outside of the first through hole. Its advantage is that the transformation of the transition chamber realizes a device for rapid adjustment. The patent number is CN217020473U, which is a new multi-purpose transition chamber for a vacuum glove box. The invention provides a new multi-purpose transition chamber for a vacuum glove box, including a transition chamber structure, and inner doors are arranged on both sides of the transition chamber structure. The feature of this patent is that there are two doors inside the transition chamber, which can be used for two-way sampling.

[0004] It can be seen from the contents of the prior art that as a precision equipment, the glove box must be equipped with a transition chamber. However, the existing transition chamber has a single structure and cannot realize the transfer of special samples. In actual use, its installation structure is not sufficiently sealed, which affects the experimental accuracy in the glove box. In addition, the prior art only sets a protective atmosphere for the internal gas atmosphere during the glove box experiment, and does not effectively protect the spatial position of the sample outside the glove box. For some special experiments or samples, it is easy to cause contamination during the sample transfer process, and the accuracy of the experiment is not considered. Summary of the invention

[0005] In response to the technical problems raised above, a mass spectrometry characterization platform and a method for using the platform are provided for high-throughput sampling under full-process inert gas protection.

[0006] The technical means adopted by the present invention are as follows:

[0007] A full-process inert gas-protected high-throughput sampling mass spectrometry characterization platform comprises a novel glove box capable of being connected to a transfer chamber, a high-throughput detection mass spectrometry ionization source connected to a mass spectrometer, and an inert gas-protected transfer chamber. Based on the inert gas-protected transfer chamber, batch trace samples of different dimensions to be tested are sampled in the glove box, and the inert gas-protected transfer chamber is connected to the high-throughput detection mass spectrometry ionization source to achieve high-throughput analysis of loading multiple samples at one time and sequentially detecting them on the mass spectrometer. During the sampling, transfer and detection processes, the samples are in a protective gas atmosphere.

[0008] Furthermore, the inert gas protection transfer chamber comprises an array probe storage chamber, a transfer sealing gate valve, an array probe assembly, a self-locking rotary sampling head and a self-locking rotary sampling head position adjustment mechanism. The array probe storage chamber is filled with a preset protective gas, the transfer sealing gate valve is installed at the end of the array probe storage chamber, and the self-locking rotary sampling head position adjustment mechanism is installed at the other end of the array probe storage chamber. The self-locking rotary sampling head is arranged inside the array probe storage chamber, and the distance of its output end relative to the transfer sealing gate valve can be adjusted by the self-locking rotary sampling head position adjustment mechanism, and the output end of the self-locking rotary sampling head can be detachably connected to the array probe assembly.

[0009] Furthermore, the protective gas includes an inert gas.

[0010] Furthermore, the array probe assembly includes an array probe lower end support base, an array probe upper end fixed cover plate and an array probe fixing screw. The upper surface of the array probe lower end support base is uniformly provided with a plurality of grooves parallel to its width direction along its length direction, and each groove forms a linear array arranged at equal intervals. The groove of the array probe lower end support base is a complete groove capable of accommodating sampling and ionization detection probes, or a groove matching the array probe lower end support base is provided on the bottom surface of the array probe upper end fixed cover plate. The bottom surface groove of the array probe upper end fixed cover plate and the groove of the array probe lower end support base form a complete groove capable of accommodating sampling and ionization detection probes. Screw holes are provided on the array probe lower end support base at a preset distance from the grooves, and screw holes matching the screw holes of the array probe lower end support base are also provided on the array probe upper end fixed cover plate. The array probe upper end fixed cover plate and the array probe lower end support base are detachably connected by the array probe fixing screws.

[0011] Furthermore, a protrusion is provided on one side of the support base at the lower end of the array probe of the array probe assembly, and the array probe assembly and the self-locking rotary sampling head can be separated and installed based on the cooperation between the output end of the self-locking rotary sampling head and the protrusion.

[0012] Furthermore, a protruding step structure is provided at the bottom of the support base at the lower end of the array probe of the array probe assembly, and the array probe assembly separated from the self-locking rotating sampling head is introduced into the experimental device based on the step structure.

[0013] Furthermore, the self-locking rotary sampling head position adjustment mechanism is a multi-layer nested structure, including a self-locking rotary sampling head storage cavity and a coarse position adjustment device, a linear telescopic precision adjustment component, the end of the array probe storage cavity is connected to one end of the self-locking rotary sampling head storage cavity, and the linear telescopic precision adjustment component is installed at one end of the self-locking rotary sampling head storage cavity close to the array probe storage cavity.

[0014] Furthermore, the self-locking rotary sampling head is connected to the output end of the magnetic internal connecting rod, the self-locking rotary sampling head storage chamber is specifically a magnetic support outer bracket, and the position coarse adjustment device includes a magnetic external driving component, which is sleeved on the outer wall of the magnetic support outer bracket. The magnetic external driving component can slide linearly on the magnetic support outer bracket to synchronously drive the linear sliding of the internal magnetic rod.

[0015] Furthermore, the magnetic external driving component is provided with a magnetic external locking screw, which is used to limit the magnetic external driving component to the magnetic support outer bracket after the magnetic external driving component reaches a preset position.

[0016] Furthermore, the linear telescopic precision adjustment component includes a linear telescopic bottom fixed support, a linear telescopic sliding thin rod support, a linear telescopic sliding thick rod support, a linear telescopic screw rotation drive, a linear telescopic linear drive translation, a linear telescopic top fixed support, a linear telescopic nut matching screw drive and a linear telescopic top rotation drive. The linear telescopic bottom fixed support and the linear telescopic linear drive translation are both provided with holes for the linear telescopic sliding thin rod support, the linear telescopic sliding thick rod support, the linear telescopic screw rotation drive and the magnetic support outer bracket to pass through, so that the linear telescopic sliding thin rod support, the linear telescopic sliding thick rod support, the linear telescopic screw rotation drive and the magnetic support outer bracket are arranged in parallel. The linear telescopic top fixed support is provided with a hole for the linear telescopic sliding thin rod support, the linear telescopic sliding thick rod support, the linear telescopic screw rotation drive and the magnetic support outer bracket to pass through. There are holes for the linear telescopic sliding thin rod support, the linear telescopic sliding thick rod support, and the linear telescopic screw rotation drive member to pass through. The bottom end of the linear telescopic top rotation drive member is connected to the linear telescopic screw rotation drive member. The top surface of the linear telescopic top rotation drive member is provided with a handle. The linear telescopic nut and the screw drive member are provided with a hole for the linear telescopic sliding thick rod support member to pass through. The linear telescopic nut and the screw drive member are arranged between the linear telescopic top fixed support member and the linear telescopic linear drive translation member. The magnetic support outer bracket is connected to the self-locking rotary sampling head storage cavity through a flange. The cross-sectional area of ​​the flange is larger than the cross-sectional area of ​​the opening of the linear telescopic bottom fixed support member. The cross-sectional area of ​​the magnetic external drive member is larger than the cross-sectional area of ​​the opening of the linear telescopic linear drive translation member.

[0017] Furthermore, a new type of glove box based on a plug-in valve injection connection transfer chamber, the side wall of the glove box is provided with a connection interface, the connection interface is equipped with an external plug-in valve type glove box transition chamber connecting the inside and outside of the glove box, the output end of the external plug-in valve type glove box transition chamber is provided with a glove box transition chamber external plug-in valve, the external plug-in valve type glove box transition chamber has a sealed working state and an open loading state for transferring samples to be tested, and a movable sample transfer assembly to be tested is provided inside the external plug-in valve type glove box transition chamber.

[0018] Furthermore, the external plug-in valve type glove box transition cabin comprises a flange and a glove box transition cabin shell, the glove box transition cabin shell is installed with the side wall of the glove box through the flange, the ends of the glove box transition cabin shell are rotatably connected with sealing panels, the sealing panel on the atmospheric side of the transition cabin away from the glove box is provided with a flange interface connected to the plug-in valve, and also includes a transition cabin door opening limiter, the transition cabin door opening limiter is installed on the outside of the transition cabin, and is used to limit the opening angle of the sealing panel on the atmospheric side of the transition cabin, the interior of the glove box transition cabin shell is provided with a glove box transition internal sliding support, which is used to adjust the position of the sample adapter assembly to be tested relative to the internal position of the glove box; a transition cabin door closing sealing locking member is also installed on the glove box transition cabin shell, and the transition cabin door closing sealing locking member cooperates with the sealing panel to complete the sealing state of the sealing panel in the working state.

[0019] Furthermore, an outer handle of the adapter assembly is provided on the side of the sample adapter assembly facing the glove box in the direction of travel of the sample adapter assembly, and an array probe assembly clamping device is provided on the other side of the sample adapter assembly.

[0020] Furthermore, a transition compartment pressure gauge is installed on the outer shell of the glove box transition compartment, and a gas connecting pipe is connected to the outer shell of the glove box transition compartment, the other end of the gas connecting pipe is connected to a tee, and an angle valve is arranged on the input pipe section of the tee, the first input pipe section of the tee is connected to a protective gas source, and the other input pipe section of the tee is connected to a negative pressure vacuum device.

[0021] Furthermore, the gate valve can be docked with the transfer sealing gate valve of the inert gas protection transfer chamber, thereby completing the transfer of the sample to be tested between the glove box, the external gate valve type glove box transition chamber and the inert gas protection transfer chamber.

[0022] Furthermore, the inert gas protection transfer chamber includes an array probe storage chamber, a transfer sealing gate valve, an array probe assembly, a self-locking rotary sampling head and a self-locking rotary sampling head position adjustment mechanism. The array probe storage chamber is filled with a preset protective gas. The transfer sealing gate valve is installed at the end of the array probe storage chamber. The other end of the array probe storage chamber is installed with the self-locking rotary sampling head position adjustment mechanism. The self-locking rotary sampling head is arranged inside the array probe storage chamber, and the distance of its output end relative to the transfer sealing gate valve can be adjusted by the self-locking rotary sampling head position adjustment mechanism. The output end of the self-locking rotary sampling head can be detachably connected to the array probe assembly. After the gate valve and the transfer sealing gate valve are docked, the array probe assembly is in an atmosphere of protective gas throughout the entire process.

[0023] Furthermore, a mass spectrometry ionization source for high-throughput detection based on inert protection comprises a closed inert gas protection ionization source, the injection end of the closed inert gas protection ionization source is provided with an ionization source top sealing plug valve, the closed inert gas protection ionization source is provided with a spatial position adjustment device, so that the detection end of the closed inert gas protection ionization source can be connected to a mass spectrometry detector in a detection state, the bottom of the closed inert gas protection ionization source is connected with an ionization source bottom storage sample piece for storing a detected array probe assembly, the closed inert gas protection ionization source has a sealed working state and an open sample loading state for transferring a sample to be tested, and the closed inert gas protection ionization source is provided with a metal electrode for completing the ionization of the sample to be tested at one end close to the mass spectrometry detector.

[0024] Furthermore, the sealing gate valve at the top of the ionization source can be docked with the transfer sealing gate valve of the inert gas protection transfer chamber, thereby completing the transfer of the sample to be tested between the inert gas protection transfer chamber and the closed inert gas protection ionization source.

[0025] Furthermore, the inert gas protection transfer chamber includes an array probe storage chamber, a transfer sealing gate valve, an array probe assembly, a self-locking rotary sampling head and a self-locking rotary sampling head position adjustment mechanism. The array probe storage chamber is filled with a preset protective gas. The transfer sealing gate valve is installed at the end of the array probe storage chamber. The other end of the array probe storage chamber is installed with the self-locking rotary sampling head position adjustment mechanism. The self-locking rotary sampling head is arranged inside the array probe storage chamber, and the distance of its output end relative to the transfer sealing gate valve can be adjusted by the self-locking rotary sampling head position adjustment mechanism. The output end of the self-locking rotary sampling head can be detachably connected to the array probe assembly. After the gate valve and the transfer sealing gate valve are docked, the array probe assembly is in an atmosphere of protective gas throughout the entire process.

[0026] Furthermore, the spatial position adjustment device includes an upper flange, a lower flange, and an X-direction fine-tuning screw respectively arranged on the upper flange and a Y-direction fine-tuning screw arranged on the lower flange, the X-direction fine-tuning screw and the Y-direction fine-tuning screw are arranged vertically in space, the lower flange is installed on the upper plate of the closed inert gas shielded ionization source, and the upper flange and the lower flange are connected by a bellows.

[0027] Furthermore, the main body of the closed inert gas protection ionization source is a rectangular metal support, one side of which cooperates with the mass spectrometer detector, and a visible non-metallic lens is installed on the left side sealing panel of the ionization source and the right side sealing panel of the ionization source for sealing, and an ionization source positive side sealing panel is arranged on the side facing the ionization source injection port position, and a non-metallic transparent panel is installed on the ionization source positive side sealing panel.

[0028] Furthermore, two clamps are placed on both sides of the injection port of the mass spectrometer detector, both of which are used to place the locking shaft of the ionization source mass spectrometer injection port; after the mass spectrometer detector cavity is placed at a specific position of the injection port of the ionization source, the assembly of the two is completed by locking the shaft and the clamp, and a sealing device is provided at the locking position of the two.

[0029] Furthermore, a filling hole for inert gas and an extraction port for gas inside the cavity are provided on the main body of the closed inert gas protection ionization source, and the extraction port is connected to a connection port of an exhaust pump.

[0030] Furthermore, the base of the metal electrode is movable in at least one-dimensional plane, and the base is a non-metallic electrode support. The input end of the metal electrode is connected to the high-voltage input end of an external ionization source through an electrode connecting metal conductive member. A connecting wire connecting the metal electrode to the high-voltage input end of the ionization source is provided at a connection with a main sealing plate of a closed inert gas protection ionization source. The through-plate electrode is a through-plate metal electrode straight-through rod, and the through-plate metal electrode straight-through rod is connected to the sealing plate through a through-plate electrode radial sealing O-ring and a through-plate electrode axial sealing O-ring.

[0031] Furthermore, the device capable of completing movement in a one-dimensional plane specifically includes an electrode support connecting sliding member connected to the bottom of the non-metallic electrode support member, the electrode support connecting sliding member can move on a fixed slide rail arranged below it, the input end of the electrode support connecting sliding member is connected to a screw rotating head advancing member, the screw rotating head advancing member is provided with an identification device with scale markings, the screw rotating head advancing member is connected to the main sealing plate of the closed inert gas protection ionization source through a screw head external support member, and a screw advancement radial sealing O-ring is provided at the sealing position.

[0032] The present invention also discloses a method for using a mass spectrometry characterization platform for high-throughput sampling under full-process inert gas protection, comprising the following steps:

[0033] Based on the inert gas protection transfer chamber, batches of trace samples of different dimensions to be tested are sampled in a glove box;

[0034] Separate the inert gas protection transfer chamber and the glove box;

[0035] The inert gas protection transfer chamber is connected to a high-throughput detection mass spectrometer ionization source, and is detected sequentially on a mass spectrometer;

[0036] After the detection is completed, the inert gas protection transfer chamber and the high-throughput detection mass spectrometry ionization source are separated.

[0037] Furthermore, based on the inert gas protection transfer chamber, the batch of trace samples of different dimensions to be tested are sampled in the glove box, which specifically includes the following steps:

[0038] Open the sealing panel. Before opening, ensure that the internal pressure of the transition chamber of the external plug-in valve glove box is normal. Place the sample transfer assembly to be tested into the transition chamber of the external plug-in valve glove box.

[0039] The atmosphere side sealing panel of the transition chamber of the external plug-in valve glove box is covered, and the sealing locking piece is closed at the same time. During this process, the front plug-in valve is in a closed sealing state, and the sealing panel inside the glove box is also in a closed state; the interior of the transition chamber shell of the glove box is evacuated to provide a protective gas atmosphere;

[0040] Based on the experimental requirements, the self-locking rotary sampling head and array probe assembly were installed to form a protective gas atmosphere inside the micro-sample transfer chamber;

[0041] Connect the transfer sealing gate valve of the micro-sample transfer chamber to the gate valve of the gate valve type glove box;

[0042] The array probe assembly disposed at the end of the self-locking rotary sampling head is pushed out of the array probe storage cavity through the coarse adjustment and / or fine adjustment function of the position adjustment mechanism of the self-locking rotary sampling head;

[0043] The transfer sealing plug valve of the micro-sample transfer chamber and the plug valve of the plug valve type glove box are opened to transfer the array probe assembly into the glove box.

[0044] Furthermore, the inert gas protection transfer chamber comprises the following steps during use:

[0045] Based on experimental requirements, complete the separation or installation of the self-locking rotary sampling head and array probe assembly;

[0046] The array probe assembly disposed at the end of the self-locking rotary sampling head is retracted or pushed out of the array probe storage cavity through the coarse adjustment and / or fine adjustment function of the self-locking rotary sampling head position adjustment mechanism. Specifically, the magnetic internal connecting rod has three key positions:

[0047] One is the initial position of the magnetic rod, at which the array sampling probe is installed. The array sampling probe is stored in the cavity, and the gate valve can be closed or opened, and the gate valve and the array sampling probe do not interfere with each other;

[0048] The second is to manually adjust the magnetic external driving part to transfer the magnetic internal connecting rod to the initial position of the precision adjustment part, at which time the sample is separated from the array probe storage cavity and is located outside the plug valve;

[0049] The third is the start of fine adjustment. Through the rotation of the linear telescopic top rotary drive, the entire precision adjustment part is driven to move downward or upward, and the downward movement to the bottom end of the fine adjustment component is the longest position that the array sampling needle can extend.

[0050] Furthermore, the inert gas protection transfer chamber is connected to a high-throughput detection mass spectrometry ionization source, and is detected in sequence on a mass spectrometer, specifically comprising the following steps:

[0051] The closed inert gas protection ionization source is set to an inert gas protection gas atmosphere in advance;

[0052] The array probe assembly storing the sample to be tested is placed on the micro-sample transfer device, and the bottom of the micro-sample transfer device is connected to the sealing plug valve at the top of the ionization source;

[0053] Open the plug valve of the micro-sample transfer device and the sealing plug valve at the top of the ionization source. Before and after the valves are opened, the insides of the two chambers are in an inert gas protection atmosphere;

[0054] The height of the array probe assembly is adjusted by the locking rotary sampling head position adjustment mechanism. At this time, the probe should be at the upper end of the mass spectrometer injection port. The two-dimensional adjustment member is used to ensure that the lowermost probe is at the center of the mass spectrometer injection port. The height is further lowered to ensure that the lowermost probe is coaxial with the mass spectrometer injection port.

[0055] The metal electrode is gradually moved forward by adjusting the screw to rotate the top advance member, and has a preset spatial distance with the lowest probe. At this time, the high-voltage switch is turned on to start the high-voltage input end of the high-voltage ionization source; then the probe is gradually moved closer to the mass spectrometer injection port, and the distance between the probe and the mass spectrometer injection port is gradually increased according to the strength of the generated ion flow, and the distance is maintained between 1-3mm. When the detection is completed, the voltage is turned off, and the metal electrode is moved back a distance away from the probe;

[0056] By adjusting the linear telescopic precision adjustment assembly, the probes are lowered one by one in sequence to complete the ionization of all subsequent probes. During this process, the metal electrode moves repeatedly and does not hinder the gradual descent of the array probe assembly in a non-ionized state.

[0057] After completing all sample inspections, the precision adjustment component is raised by rotating the linear telescopic component in the opposite direction, and the height is restored to the initial position, and then restored to the initial position by the magnetic external drive component.

[0058] Compared with the prior art, the present invention has the following advantages: the present invention places the sample from the transfer chamber, realizes gas replacement in the transition chamber, and places the sample in a vacuum glove box to realize sample weighing and filling. For some special samples, after sampling from the glove box, it is still necessary to maintain an anhydrous and oxygen-free environment. Therefore, during use, it is necessary to use the vacuum glove box in conjunction with the transfer chamber, and realize a transfer of the transfer chamber through a plug valve. During the glove box and mass spectrometry detection process, the whole process is covered by a protective atmosphere, which ensures the characteristics of the sample during the experiment and improves the accuracy of the experiment. BRIEF DESCRIPTION OF THE DRAWINGS

[0059] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0060] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0061] Figure 2 It is the front view of the overall structure of the present invention.

[0062] Figure 3 This is a usage diagram of the array probe assembly of the device of the present invention placed in a storage cavity.

[0063] Figure 4 This is a pattern diagram of the array probe assembly of the device of the present invention before being placed in the storage cavity.

[0064] Figure 5 It is a schematic diagram of the position change of the magnetic rod of the present invention.

[0065] Among them, (a) is a schematic diagram of the initial position of the magnetic rod.

[0066] (b) is a schematic diagram of the magnetic rod being lowered to the initial position for high precision adjustment.

[0067] (c) is a schematic diagram of the magnetic rod being lowered to the bottom end for high precision adjustment.

[0068] Figure 6 It is a schematic diagram of the position relationship between the magnetic rod and the internal slider of the present invention.

[0069] Among them, (a) is a schematic diagram of the position of the internal slider when the magnetic rod is in the initial position.

[0070] (b) is a schematic diagram of the position of the internal slider when the magnetic rod is lowered to the initial position for high precision adjustment.

[0071] (c) is a schematic diagram of the position of the internal slider when the magnetic rod is lowered to the bottom end of the height precision adjustment.

[0072] Figure 7 It is a schematic diagram of the explosion of the overall parts of the device of the present invention.

[0073] Figure 8 Schematic diagram of the split style of the linear telescopic precision adjustment component and the magnetic coupling rod of the present invention.

[0074] Fig. 9 This is an exploded view of the linear telescopic precision adjustment component of the present invention.

[0075] Fig.10 This is an exploded view of the array probe assembly of the present invention.

[0076] Fig.11 It is a schematic diagram of the array probe assembly and the self-locking rotary sampling head of the present invention in a decoupled state.

[0077] Fig.12 It is a schematic diagram of the locking state of the array probe assembly and the self-locking rotary sampling head of the present invention.

[0078] Fig.13 It is a schematic diagram of the overall structure of a new type of glove box based on a plug valve injection connection transfer chamber of the present invention.

[0079] Fig.14 This is a schematic diagram of the structure of the glove box with an external plug-in valve inlet according to the present invention.

[0080] Fig.15 The door of the transition chamber of the present invention is opened to place the sample transfer assembly to be tested.

[0081] Fig.16 This is a schematic diagram of the sample adapter assembly of the present invention being completely placed into the transition chamber.

[0082] Fig.17 The present invention closes the sealing panel on the atmosphere side of the transition compartment.

[0083] Fig.18 It is a schematic diagram for explaining the matching mode between the sample adapter assembly to be tested and the bottom of the array sampling probe assembly of the present invention.

[0084] Fig.19 It is an isometric schematic diagram of the cooperation between the sample adapter assembly and the array probe assembly of the present invention.

[0085] Fig. 20 It is a schematic diagram of the explosion of the sample adapter assembly to be tested of the present invention.

[0086] Fig.21 It is a schematic diagram showing that the inert gas protection transfer chamber and the external plug-in valve type transition chamber of the present invention are in a separated state.

[0087] Fig. 22 This is a schematic diagram of the inner sealing panel of the transition chamber glove box of the present invention being opened to prepare for placing the sample adapter assembly to be tested into the glove box.

[0088] Fig.23 This is a schematic diagram of closing the sealing panel inside the transition chamber glove box after the sample adapter assembly to be tested of the present invention is placed in the glove box.

[0089] Fig.24 This is a schematic diagram of the sample adapter assembly of the present invention removing the array probe assembly placed on the right.

[0090] Fig.25 This is a schematic diagram of the array probe assembly and the sample adapter assembly of the present invention being placed back into the transition chamber of the glove box.

[0091] Fig.26 This is a schematic diagram of the sealing panel inside the glove box of the closed transition compartment of the present invention.

[0092] Fig. 27 The present invention is a schematic diagram of separating the inert gas protection transfer chamber equipped with the array probe assembly from the transition chamber of the external plug-in valve type glove box.

[0093] Fig.28 The figure is a schematic diagram of the overall assembly of the mass spectrometry ionization source for high-throughput detection based on inert protection of the present invention.

[0094] Fig.29 This is a schematic diagram of the state in which the external plug-in valve ionization source of the present invention is not connected to the inert gas protection transfer chamber.

[0095] Fig.30 It is an isometric view of the structure of the closed inert gas protection ionization source of the present invention.

[0096] Fig.31 This is a macroscopic view of the sealed inert gas protection ionization source of the present invention assembled on a mass spectrometer detector.

[0097] Fig.32 This is an observation view of the sealed inert gas protection ionization source of the present invention assembled on the right side of the mass spectrometer detector.

[0098] Fig.33 This is an observation view of the closed inert gas protection ionization source of the present invention assembled on the left side of the mass spectrometer detector.

[0099] Fig.34 This is an enlarged view of the sealed inert gas protection ionization source of the present invention assembled on the left side of the mass spectrometer detector.

[0100] Fig.35 This is the explosion diagram of the closed inert gas protection ionization source of the present invention - observed from the right side.

[0101] Fig.36This is the explosion diagram of the closed inert gas protection ionization source of the present invention - observed from the left side.

[0102] Fig.37 This is the exploded view of the closed inert gas protection ionization source of the present invention - isometric side.

[0103] Fig.38 This is an exploded view of the structure of the core cavity component of the ionization source of the present invention.

[0104] Fig.39 It is an exploded view of the structure of the ionization source contact position moving component of the present invention.

[0105] Fig.40 This is a front view of the sealed inert gas shielded ionization source of the present invention, wherein the sensing electrode is close to the probe position.

[0106] Fig.41 It is a front view of the sealed inert gas shielded ionization source of the present invention, wherein the sensing electrode is far away from the probe position.

[0107] Fig.42 The inert gas protection transfer chamber of the present invention is placed at the initial position on the top of the ionization source - a local enlarged view.

[0108] Fig.43 The inert gas protection transfer chamber of the present invention has its internal array probe assembly moved downward to the last probe at the mass spectrometer injection port - a partial enlarged view.

[0109] In the figure: 001: inert gas protection transfer chamber; 002: new glove box for connecting the transfer chamber; 003: high-throughput detection mass spectrometry ionization source; 004: mass spectrometer; 101, array probe assembly; 102, magnetic internal connecting rod; 103, linear telescopic precision adjustment assembly; 104, magnetic support outer bracket; 105, magnetic external drive; 106, magnetic drive external locking screw; 107, array probe storage chamber; 108, transfer sealing plug valve; 109, self-locking rotary sampling head; 1011, array probe fixing screw; 1012, array probe upper end fixing cover; 1013, array probe lower end support base; 1014, sampling and ionization detection probe; 1031, linear telescopic top Rotary drive member; 1032, linear telescopic linear drive translation member; 1033, linear telescopic sliding thin rod support member; 1034, linear telescopic screw rotation drive member; 1035, linear telescopic top fixed support member; 1036, linear telescopic nut matching screw drive member; 1037, linear telescopic sliding thick rod support member; 1038, linear telescopic bottom fixed support member; 201: external plug-in valve glove box transition chamber; 202: glove box transition internal sliding support member; 203: sample transfer assembly to be tested; 204: glove box transition chamber shell; 205: gas connection pipe; 206: transition chamber atmospheric side sealing panel; 208: transition chamber door opening limit member; 209: transition chamber door closing sealing locking member; 210: glove box transition chamber External gate valve of transition chamber; 212: vacuum pump; 213: pressure gauge of transition chamber; 214: sealing panel inside the glove box of transition chamber; 2031: handle outside the adapter assembly; 2032: support of the adapter assembly; 2033: spring-type pressing piece of the adapter assembly; 2034: fixing screw of the pressing piece of the adapter assembly; 302: closed inert gas protection ionization source; 303: sealing gate valve at the top of the ionization source; 304: closed two-dimensional XY direction adjustment device; 305: metal support; 306: sample storage at the bottom of the ionization source; 307: mass spectrometer detector; 308: mass spectrometer injection port; 3021: inert gas inlet; 3022: vacuum pump connection port; 3023: sealing panel on the front of the ionization source; 3024: on the ionization source Plate; 3025: Ionization source and mass spectrometer injection port locking shaft; 3026: Ionization source contact electrode position moving assembly; 3027: Ionization source left sealing panel; 3028: Ionization source right sealing panel; 3031: Metal electrode; 3032: Non-metal electrode support; 3033: Electrode connection metal conductive member; 3034: Electrode support connection sliding member; 3035: Fixed slide rail; 3036: Screw rotating head forward member; 3037: External scale nut member; 3038: Screw head external support member; 3039: Screw advancement radial sealing O-ring; 401: Through-plate electrode seal; 402: Through-plate electrode axial sealing O-ring; 403: Through-plate metal electrode straight-through rod; 404: Through-plate electrode radial sealing O-ring;405: Ionization source high voltage input terminal; 406: Wire connecting the through-plate electrode and the metal electrode. ; DETAILED DESCRIPTION

[0110] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0111] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. The following description of at least one exemplary embodiment is actually only illustrative and is by no means intended to limit the present invention and its application or use. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0112] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit exemplary embodiments according to the present invention. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprising" and / or "including" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.

[0113] Unless otherwise specifically stated, the relative arrangement of the parts and steps described in these embodiments, the numerical expressions and numerical values ​​do not limit the scope of the present invention. At the same time, it should be clear that, for ease of description, the sizes of the various parts shown in the drawings are not drawn according to the actual proportional relationship. The technology, methods and equipment known to ordinary technicians in the relevant field may not be discussed in detail, but in appropriate cases, the technology, methods and equipment should be regarded as part of the authorization specification. In all examples shown and discussed here, any specific value should be interpreted as merely exemplary, rather than as a limitation. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar numbers and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further discussed in subsequent drawings.

[0114] In the description of the present invention, it is necessary to understand that the directions or positional relationships indicated by directional words such as "front, back, up, down, left, right", "lateral, vertical, perpendicular, horizontal" and "top, bottom" are usually based on the directions or positional relationships shown in the drawings. They are only for the convenience of describing the present invention and simplifying the description. Unless otherwise specified, these directional words do not indicate or imply that the device or element referred to must have a specific direction or be constructed and operated in a specific direction. Therefore, they cannot be understood as limiting the scope of protection of the present invention: the directional words "inside and outside" refer to the inside and outside relative to the contours of each component itself.

[0115] For ease of description, spatially relative terms such as "above", "above", "on the upper surface of", "above", etc. may be used here to describe the spatial positional relationship between a device or feature and other devices or features as shown in the figure. It should be understood that spatially relative terms are intended to include different orientations of the device in use or operation in addition to the orientation described in the figure. For example, if the device in the accompanying drawings is inverted, the device described as "above other devices or structures" or "above other devices or structures" will be positioned as "below other devices or structures" or "below their position devices or structures". Thus, the exemplary term "above" can include both "above" and "below". The device can also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatially relative descriptions used here are interpreted accordingly.

[0116] In addition, it should be noted that the use of terms such as "first" and "second" to limit components is only for the convenience of distinguishing the corresponding components. If not otherwise stated, the above terms have no special meaning and therefore cannot be understood as limiting the scope of protection of the present invention.

[0117] like Figure 1 As shown, an embodiment of the present invention discloses a mass spectrometry characterization platform for high-throughput sampling with inert gas protection throughout the entire process, including a new glove box 002 that can be connected to a transfer chamber, a high-throughput detection mass spectrometry ionization source 003 connected to a mass spectrometer 004, and an inert gas protection transfer chamber 001. Based on the inert gas protection transfer chamber 001, a batch of trace samples of different dimensions to be tested are sampled in the glove box 002, and the inert gas protection transfer chamber 001 is connected to the high-throughput detection mass spectrometry ionization source 003 to achieve a high-throughput analysis of loading multiple samples at a time and sequentially detecting them on the mass spectrometer 004. The samples are in a protective gas atmosphere during the sampling, transfer, and detection processes. In this embodiment, different dimensions specifically refer to that the solutions loaded in the array probes can be of the same concentration or different concentrations, and can be compounds of the same or different classes.

[0118] The inert gas protection transfer chamber 001 includes an array probe storage chamber 107, a transfer sealing gate valve 108, an array probe assembly 101, a self-locking rotary sampling head 109 and a self-locking rotary sampling head position adjustment mechanism. The array probe storage chamber 107 is filled with a preset protective gas, the transfer sealing gate valve 108 is installed at the end of the array probe storage chamber 107, and the other end of the array probe storage chamber 107 is installed with the self-locking rotary sampling head position adjustment mechanism. The self-locking rotary sampling head 109 is arranged inside the array probe storage chamber 107, and the distance of its output end relative to the transfer sealing gate valve 108 can be adjusted by the self-locking rotary sampling head position adjustment mechanism. The output end of the self-locking rotary sampling head 109 can be detachably connected to the array probe assembly 101.

[0119] The purpose of the present invention is to connect a certain type of cavity to a glove box or a mass spectrometer detector respectively, so that the internal sample holder can be well loaded with samples or tested. The key is to place a sample piece of an array sampler inside. When the gate valve is opened, it can be used to replace the gas in the chamber, and at the same time, the internal array sample piece can be removed from the outside of the cavity. The needle tip array piece can move forward and backward. In this embodiment, it is realized based on the magnetic sample transfer rod. The array needle tip can be transferred to the outside of the cavity for sampling of the needle tip. At the same time, through the sampling of the probe sampling rod, the sample is taken from the outside to the probe storage cavity. In this process, the transfer sealing gate valve can be closed, and the transfer chamber of the present invention can be moved or placed to other positions.

[0120] The protective gas includes an inert gas.

[0121] The built-in array sample assembly is composed of a series of drawn probe pieces, the array probe assembly 101 includes an array probe lower end support base 1013, an array probe upper end fixed cover plate 1012 and an array probe fixing screw 1011, the upper surface of the array probe lower end support base 1013 is uniformly provided with a plurality of grooves parallel to its width direction along its length direction, each groove forms a linear array arranged at equal intervals, the groove of the array probe lower end support base 1013 is a complete groove capable of accommodating the sampling and ionization detection probe 1014 or is provided on the bottom surface of the array probe upper end fixed cover plate 1012 In coordination with the groove of the array probe lower support base 1013, the bottom groove of the array probe upper fixed cover plate 1012 and the groove of the array probe lower support base 1013 form a complete groove capable of accommodating the sampling and ionization detection probe 1014; screw holes are provided on the array probe lower support base 1013 at a preset distance from the grooves, and screw holes matching the screw holes of the array probe lower support base are also provided on the array probe upper fixed cover plate 1012, and the array probe upper fixed cover plate 1012 and the array probe lower support base 1013 are detachably connected by the array probe fixing screws 1011. In this embodiment, the array probe upper fixed cover plate can be a non-metallic component, which is used to fix the probe well and has a certain insulation effect.

[0122] A protrusion is provided on one side of the array probe lower end support base 1013 of the array probe assembly 101. Based on the cooperation between the output end of the self-locking rotary sampling head 109 and the protrusion, the array probe assembly 101 and the self-locking rotary sampling head 109 can be separated and installed.

[0123] The bottom of the array probe lower end support base 1013 of the array probe assembly 101 is provided with a protruding step structure, and the array probe assembly 101 separated from the self-locking rotating sampling head 109 is introduced into the experimental device based on the step structure.

[0124] The self-locking rotary sampling head position adjustment mechanism is a multi-layer nested structure, the core of which is to place the arrayed sampling probes therein to play a protective role. And it enables the arrayed probes to move linearly in one dimension back and forth in the storage cavity. Specifically, it includes a self-locking rotary sampling head storage cavity and a position coarse adjustment device, a linear telescopic precision adjustment component 103, the end of the array probe storage cavity 107 is connected to one end of the self-locking rotary sampling head storage cavity, and the linear telescopic precision adjustment component 103 is installed at one end of the self-locking rotary sampling head storage cavity close to the array probe storage cavity 107.

[0125] The self-locking rotary sampling head 109 is connected to the output end of the magnetic internal connecting rod 102. The self-locking rotary sampling head storage chamber is specifically a magnetic support outer bracket 104. The position coarse adjustment device includes a magnetic external driving member 105. The magnetic external driving member 105 is sleeved on the outer wall of the magnetic support outer bracket 104. The magnetic external driving member 105 can slide linearly on the magnetic support outer bracket 104 to synchronously drive the linear sliding of the internal magnetic rod.

[0126] The magnetic external driving member 105 is provided with a magnetic external locking screw 106, which is used to limit the magnetic external driving member 105 to the magnetic support outer bracket 104 after reaching the preset position. By holding the magnetic external driving member, it can be moved within a relatively wide range of distances. When it is adjusted to a distance and wants to be locked, the position of the magnetic external driving member is tightened by the external locking screw of the magnetic external driving member, and a position limit of the array sample support is realized at the same time. When it is necessary to move the magnetic external driving member, the screw is loosened to achieve sliding again. When its position reaches the initial position of fine adjustment, the position of the magnetic link rod is finely adjusted by adjusting the telescopic precision adjustment component, and the adjustment accuracy can be achieved below 0.1mm.

[0127] The linear telescopic precision adjustment component 103 includes a linear telescopic bottom fixed support 1038, a linear telescopic sliding thin rod support 1033, a linear telescopic sliding thick rod support 1037, a linear telescopic screw rotation drive 1034, a linear telescopic linear drive translation member 1032, a linear telescopic top fixed support 1035, a linear telescopic nut matching screw drive 1036 and a linear telescopic top rotation drive 1031. The linear telescopic bottom fixed support 1038 and the linear telescopic linear drive translation member 1032 are both provided with holes for the linear telescopic sliding thin rod support 1033, the linear telescopic sliding thick rod support 1037, the linear telescopic screw rotation drive 1034 and the magnetic support outer bracket 104 to pass through, and the linear telescopic sliding thin rod support 1033, the linear telescopic sliding thick rod support 1037, the linear telescopic screw rotation drive 1034 and the magnetic support outer bracket 104 are arranged in parallel. The linear telescopic top fixed support 1035 is provided with a linear telescopic nut matching screw drive 1036 and a linear telescopic top rotation drive 1031. A hole is formed on 1035 for the linear telescopic sliding thin rod support 1033, the linear telescopic sliding thick rod support 1037, and the linear telescopic screw rotation driver 1034 to pass through. The bottom end of the linear telescopic top rotation driver 1031 is connected to the linear telescopic screw rotation driver 1034. The top surface of the linear telescopic top rotation driver 1031 is provided with a handle. A hole is formed on the linear telescopic nut and screw driver 1036 for the linear telescopic sliding thick rod support 1037 to pass through. The linear telescopic nut and screw driver 1036 are arranged between the linear telescopic top fixed support 1035 and the linear telescopic linear drive translation member 1032. The magnetic support outer bracket 104 is connected to the self-locking rotary sampling head storage chamber through a flange. The cross-sectional area of ​​the flange is larger than the cross-sectional area of ​​the opening of the linear telescopic bottom fixed support 1038. The cross-sectional area of ​​the magnetic external driver 105 is larger than the cross-sectional area of ​​the opening of the linear telescopic linear drive translation member 1032. The magnetic external driving member can be directly seated on the linear telescopic linear driving translation member by gravity, that is, the limit position of the magnetic external driving member, and the magnetic external driving member can also be manually adjusted to reach a preset position.

[0128] By rotating the handle driving part at the top, the screw is driven to rotate, thereby driving the telescopic nut to drive the mating part, and driving the bottom driving translation part to move up and down. In order to achieve better adjustment accuracy, one manual rotation of 1 circle adjusts the height by 1mm. As an extended implementation method, it can not only be rotated manually, but also can be matched with a servo motor to achieve automatic rotation.

[0129] The side wall of the novel glove box 002 is provided with a connection interface, and the connection interface is equipped with an external plug-in valve glove box transition chamber 201 connecting the inside and outside of the glove box, and the output end of the external plug-in valve glove box transition chamber 201 is provided with a glove box transition chamber external plug-in valve 210, and the external plug-in valve glove box transition chamber 201 has a sealed working state and an open sample loading state for transferring the sample to be tested, and a movable sample transfer assembly 203 to be tested is provided inside the external plug-in valve glove box transition chamber 201. Based on the external plug-in valve of the glove box transition chamber, the sample can be seamlessly connected between the sample cavity and the transition chamber and the glove box under the protective gas atmosphere.

[0130] The external plug-in valve glove box transition chamber 201 includes a flange and a glove box transition chamber shell 204, wherein the glove box transition chamber shell 204 is installed with the glove box side wall through the flange, and the ends of the glove box transition chamber shell 204 are rotatably connected with a sealing panel, wherein the inner sealing panel 214 of the transition chamber glove box is arranged in the glove box. A flange interface for connecting the plug-in valve is arranged on the transition chamber atmosphere side sealing panel 206 away from the glove box, and also includes a transition chamber door opening limiter 208, wherein the transition chamber door opening limiter 208 is installed on the outer side of the transition chamber, and is used to limit the door opening angle of the transition chamber atmosphere side sealing panel 206, and the glove box transition chamber shell 204 is provided with a glove box transition internal sliding support 202 inside, which is used to adjust the position of the sample transfer assembly 203 to be tested relative to the internal position of the glove box; and a transition chamber door closing sealing locking member 209 is also installed on the glove box transition chamber shell 204, wherein the transition chamber door closing sealing locking member 209 cooperates with the sealing panel to complete the sealing state of the sealing panel in the working state.

[0131] The glove box provided in this embodiment is provided with two ways of opening the door. One is the same as the traditional glove box, and the hatch door is opened and closed by opening and closing the sealing panel as usual, and the external plug-in valve of the glove box transition chamber is in a closed and locked state. The other state is that when the external plug-in valve of the glove box transition chamber is connected to the outside of the cavity, the glove box can cooperate with the micro-sample transfer chamber to realize the convenient operation of sample transfer under inert gas.

[0132] The side of the sample adapter assembly 203 facing the glove box is provided with an adapter assembly outer handle 2031 , and the other side of the sample adapter assembly 203 is provided with a clamping device of the array probe assembly 101 .

[0133] A transition compartment pressure gauge 213 is installed on the glove box transition compartment shell 204, and a gas connecting pipe 205 is connected to the glove box transition compartment shell 204. The other end of the gas connecting pipe 205 is connected to a three-way pipe, and an angle valve is arranged on the input pipe section of the three-way pipe. The first input pipe section of the three-way pipe is connected to the protective gas source, and the other input pipe section of the three-way pipe is connected to the negative pressure vacuum pumping device. One side is a vacuum negative pressure pumping gear, and a negative pressure pumping pump is used to realize negative pressure pumping inside the cavity, wherein according to the performance of the pumping pump, a range of 1-500 Pa is acceptable. After the three-way connecting the gas circuit is placed in the inert gas charging gear, the inert gas charging operation is performed.

[0134] The external gate valve 210 of the glove box transition chamber can be docked with the transfer sealing gate valve 108 of the inert gas protection transfer chamber 001, thereby completing the transfer of the sample to be tested between the glove box, the external gate valve glove box transition chamber 201 and the inert gas protection transfer chamber 001.

[0135] In this embodiment, the sample adapter assembly 203 to be tested includes a main part of an adapter assembly support 2032, and the array probe assembly clamping device specifically includes an adapter assembly spring-type pressing piece 2033 arranged at one end of the main part of the adapter assembly support, and the array probe assembly is clamped by the adapter assembly spring-type pressing piece 2033.

[0136] The spring-type pressing piece 2033 in this embodiment is used to fix the array probe assembly, and the pressing piece is connected by the adapter assembly pressing piece fixing screws 2034 to fit it on both sides. The lifting handle 2031 can be provided to realize the overall movement of the sample adapter assembly to be tested.

[0137] The spring-type pressing piece 2033 has two parts with an outward turning angle, which is used to facilitate the insertion of the array probe assembly from the side. The insertion method is to insert from the side along the direction of travel. Due to the stress of the spring-type pressing piece 2033, the adapter assembly can be placed under the pressure of the pressing piece and the array probe assembly can be fixed. When the handle 2031 is used during sampling, the array probe assembly will not fall off. After the array probe is placed in the adapter, the adapter assembly can be used as an adapter to move the probe assembly from the chamber to the inside of the glove box chamber. The adapter assembly has a good matching effect with the slide rail in the middle of the transition chamber, which allows the sliding assembly to slide in the middle of the transition chamber.

[0138] The inert gas protection transfer chamber 001 includes an array probe storage chamber 107, a transfer sealing gate valve 108, an array probe assembly 101, a self-locking rotary sampling head 109 and a self-locking rotary sampling head 109 position adjustment mechanism. The array probe storage chamber 107 is filled with a preset protective gas. The transfer sealing gate valve 108 is installed at the end of the array probe storage chamber 107. The other end of the array probe storage chamber 107 is installed with the self-locking rotary sampling head 109 position adjustment mechanism. The self-locking rotary sampling head 109 is arranged inside the array probe storage chamber 107, and the distance of its output end relative to the transfer sealing gate valve 108 can be adjusted by the self-locking rotary sampling head 109 position adjustment mechanism. The output end of the self-locking rotary sampling head 109 can be detachably connected to the array probe assembly 101. After the gate valve and the transfer sealing gate valve 108 are docked, the array probe assembly 101 is formed in an atmosphere of protective gas throughout the entire process.

[0139] The mass spectrometry ionization source 003 for high-throughput detection based on inert protection comprises a closed inert gas protection ionization source 302, the injection end of the closed inert gas protection ionization source 302 is provided with an ionization source top sealing plug valve 303, the closed inert gas protection ionization source 302 is provided with a spatial position adjustment device, so that in the detection state, the detection end of the closed inert gas protection ionization source 302 can be connected to the mass spectrometry detector 307, the bottom of the closed inert gas protection ionization source 302 is connected with an ionization source bottom storage sample piece 306 for storing the detected array probe assembly 101, the closed inert gas protection ionization source 302 has a sealed working state and an open loading state for transferring the sample to be tested, and the closed inert gas protection ionization source 302 is provided with a metal electrode 3031 for completing the ionization of the sample to be tested at one end close to the mass spectrometry detector 307. The present invention can realize the capability of batch detection. During the sampling process, ionization needles are lowered one by one from the top to realize one-time sampling without repeated replacement of chamber gas, thereby realizing high-throughput detection of samples.

[0140] The ionization source top sealing gate valve 303 can be docked with the transfer sealing gate valve 108 of the inert gas protection transfer chamber 001 , thereby completing the transfer of the sample to be tested between the inert gas protection transfer chamber 001 and the closed inert gas protection ionization source 302 .

[0141] The spatial position adjustment device includes an upper flange, a lower flange and a closed two-dimensional XY direction adjustment device 304, wherein the closed two-dimensional XY direction adjustment device includes an X-direction fine-tuning screw respectively arranged on the upper flange and a Y-direction fine-tuning screw arranged on the lower flange, wherein the X-direction fine-tuning screw and the Y-direction fine-tuning screw are arranged in a spatial vertical manner, and the lower flange is installed on the upper plate 3024 of the closed inert gas protection ionization source, and the upper flange and the lower flange are connected by a bellows. Through the upper and lower flanges, the middle bellows is connected, and a small range adjustment in the XY plane is achieved, and the conditional distance setting can be within the range of ±10mm (the same adjustment range in the X direction and the Y direction). During the adjustment process, the upper flange drives the bellows to move a certain distance, and the main adjustment part does not touch the bellows to achieve interference of parts, and ensures the sealed connection between the upper and lower flanges and the bellows during use. Specifically, by moving the fine-tuning screw back and forth, the top flange is moved in the direction of one dimension.

[0142] The main body of the enclosed inert gas protection ionization source 302 is a rectangular metal support 305, one side of which cooperates with a mass spectrometer detector 307, and a visible non-metallic lens is installed on the left sealing panel 3027 of the ionization source and the right sealing panel 3028 of the ionization source for sealing, and an ionization source positive side sealing panel 3023 is provided on the side facing the ionization source injection port position, and a non-metallic transparent panel is installed on the ionization source positive side sealing panel. In the connection process with the mass spectrum, the two adopt the O-ring seal at the mass spectrometer injection port position. When the sealing plug valve at the top of the ionization source is closed, the sealing of the cavity can be achieved.

[0143] Two clamps are placed on both sides of the injection port of the mass spectrometer detector 307, both of which are used to place the locking shaft 3025 of the ionization source mass spectrometer injection port 308; after the mass spectrometer detector 307 cavity is placed at a specific position of the injection port of the ionization source, the assembly of the two is completed by locking the shaft and the clamp, and a sealing device is provided at the locking position of the two; the locking shaft has two functions, namely positioning and locking cooperation. When the mass spectrometer cavity is placed at a specific position of the injection port of the ionization source, the shaft can be rotated to a certain angle, and when it is rotated to a specific clamping position, the ionization source core cavity is assembled to the front end of the injection port of the mass spectrometer cavity. At this time, after rotating a certain angle again, the injection port locking shaft can be reliably matched to the mass spectrum, ensuring that the entire closed inert gas protection ionization source will not fall. This design is easy to install and disassemble, but after each installation, the ionization source cavity must be gas circulated once.

[0144] During use of the ionization source, the sealing of the core cavity needs to be ensured. For this purpose, an inert gas inlet 3021 and an extraction port for the gas inside the cavity are provided on the main body of the closed inert gas protection ionization source 302 , and the extraction port is connected to the vacuum pump connection port 3022 .

[0145] The base of the metal electrode 3031 is movable in at least one-dimensional plane, and the base is a non-metallic electrode support 3032. The input end of the metal electrode 3031 is connected to the external ionization source high-voltage input end 405 through the electrode connecting metal conductive part 3033. The connecting wire 406 connecting the metal electrode 3031 and the ionization source high-voltage input end 405 is provided with a through-plate electrode at the connection with the main sealing plate of the closed inert gas protection ionization source 302. The through-plate electrode is a through-plate metal electrode straight-through rod 403. The through-plate metal electrode straight-through rod 403 is connected to the sealing plate through the through-plate electrode seal 401, the through-plate electrode radial sealing O-ring 404 and the through-plate electrode axial sealing O-ring 402.

[0146] A device capable of completing movement in a one-dimensional plane, namely, an ionization source contact electrode position moving component 3026, specifically includes an electrode support connecting sliding member 3034 connected to the bottom of a non-metallic electrode support 3032, wherein the electrode support connecting sliding member 3034 can move on a fixed slide rail 3035 arranged thereunder, and an input end of the electrode support connecting sliding member 3034 is connected to a screw rotating head advancing member 3036, wherein the screw rotating head advancing member 3036 is provided with an identification device 3037 with scale markings, and the screw rotating head advancing member 3036 is connected to the main sealing plate of the closed inert gas protection ionization source 302 through a screw head external support member 3038, and a screw advancement radial sealing O-ring 3039 is provided at the sealing position.

[0147] The present invention also discloses a method for using a mass spectrometry characterization platform for high-throughput sampling under full-process inert gas protection, comprising the following steps:

[0148] Based on the inert gas protection transfer chamber 001, the batches of trace samples of different dimensions to be tested are sampled in the glove box 002;

[0149] Separate the inert gas protection transfer chamber 001 and the glove box 002;

[0150] The transfer chamber 001 is connected to a high-throughput detection mass spectrometer ionization source 003 through the inert gas protection, and is detected in sequence on a mass spectrometer 004;

[0151] After the detection is completed, the inert gas protection transfer chamber 001 and the high-throughput detection mass spectrometry ionization source 003 are separated.

[0152] Based on the inert gas protection transfer chamber 001, the batches of trace samples of different dimensions to be tested are sampled in the glove box 002.

[0153] The main steps are: the array probe assembly in the trace sample transfer chamber is fixed through the sealing plug valve of the transfer chamber and the plug valve outside the glove box transition chamber, and is moved from the trace sample transfer chamber to the sample transfer assembly to be tested, and is opened through the sealing panel inside the glove box, and the sample transfer assembly to be tested is taken out and placed inside the glove box. Through the sample transfer assembly to be tested, the array probe assembly can be taken into the glove box, and the probe can be operated, and a certain amount of the sample to be tested can be injected into it. The sampling method can choose to sample the inside of the probe one by one, and the entire array probe assembly can also be held by hand, and the sample is concentratedly sampled in turn using the injector. After the sampling is completed, the opposite method is used to put the array probe back into the trace sample transfer chamber in turn. After the transfer is completed, the trace sample transfer chamber is removed from the external plug valve glove box transition chamber.

[0154] The specific steps include:

[0155] Open the sealing panel. Before opening, ensure that the internal pressure of the external plug-in valve glove box transition chamber 201 is normal. Place the sample adapter assembly 203 to be tested into the internal pressure of the external plug-in valve glove box transition chamber 201. At this time, hold the bottom with your hand and put it into the chamber with the handle facing the chamber. Place the transition chamber into the chamber, send it into the guide rail, and then place the entire transition chamber into the transition chamber. In order to close the door, the protruding tip must also be placed in the transition chamber.

[0156] The atmosphere side sealing panel of the external plug-in valve glove box transition chamber 201 is covered, and the sealing locking piece is closed at the same time. During this process, the front plug-in valve is in a closed and sealed state, and the sealing panel inside the glove box is also in a closed state; the interior of the glove box transition chamber shell 204 is evacuated to provide a protective gas atmosphere; at this time, the interior of the transition chamber can be filled with nitrogen, and the three-way valve is controlled to ensure that the cavity is replaced by nitrogen;

[0157] Based on the experimental requirements, the self-locking rotary sampling head 109 and the array probe assembly 101 are installed to form a protective gas atmosphere inside the micro-sample transfer chamber;

[0158] Connect the transfer sealing gate valve 108 of the micro-sample transfer chamber to the gate valve of the gate valve type glove box;

[0159] The array probe assembly 101 disposed at the end of the self-locking rotary sampling head 109 is pushed out of the array probe storage cavity 107 through the coarse adjustment and / or fine adjustment function of the self-locking rotary sampling head position adjustment mechanism;

[0160] The transfer sealing gate valve of the micro-sample transfer chamber is connected to the gate valve of the gate valve type glove box; at this time, the air inside the micro-sample transfer chamber is mixed with the nitrogen in the transition chamber. Therefore, a vacuum pump is used in conjunction with nitrogen filling until all the gases in the two chambers are filled with high-concentration nitrogen. The indication of the pressure gauge is observed, and the two chambers are at the same pressure, and therefore at one atmospheric pressure concentration;

[0161] The transfer sealing gate valve 108 of the micro-sample transfer chamber and the gate valve of the gate valve type glove box are opened to transfer the array probe assembly 101 into the glove box.

[0162] Specifically, the magnetic telescopic rod inside the micro-sample transfer chamber is used to insert the array probe into the sample slot on the sample connection component to be tested. Using a glove box, the staff extends their hands into the glove box to open the inner sealed cabin. At this time, before opening, both cabins are in a nitrogen protection state. After opening the cabin door with their hands, the entire transition cabin transfer part is taken away with a handheld handle. At this time, the sample transfer assembly and the array sampling needle are placed in the glove box at the same time. After the above two components are placed in the glove box, for ease of operation, the inner sealing panel of the glove box can be closed. At this time, two hands can be used to operate, one hand fixes the transfer assembly, and the other hand takes out the array probe assembly by sliding on the right side. The above operations are all operated interactively by two gloves in the glove box. In the process of operating the above array probe, the probe can be fixed on the upper and lower cover plate equipment structure of the component for sampling, and the probe can be taken out at the same time. The method is to unscrew the three screws of the upper cover plate, and then each probe can be operated, wherein each probe can be added with different solvents, or the same solvent, and can be the same concentration or different concentrations. The concentration needs to be recorded when adding the solution. After completing the sample filling of the probes one by one, the probes need to be put back into the probe assembly one by one and the screws are installed. And they are inserted into the sample adapter assembly to be tested from the side for easy subsequent replacement.

[0163] After the sample addition is completed, the array probe is placed on the transfer assembly again, and the sealing panel on the inside of the glove box is opened. At this time, whether it is the glove box, the transition chamber, or even the trace sample transfer chamber, they are all filled with inert protective gas. Therefore, the trace samples operated in the glove box and filled into the probe can be well isolated from the air to avoid pollution such as oxygen and water vapor. Use the outer handle of the adapter to place the adapter into the end of the transition chamber to ensure that the array probe can be grabbed by the self-locking sampling head. By adjusting the connecting rod of the trace sample transfer chamber, the array probe is slowly moved into the array probe storage chamber. At this time, the gate valve of the glove box transition chamber is closed in turn, and the gate valve of the transfer chamber is also closed. At this time, the inside of the glove box transition chamber is filled with inert gas, and the inside of the trace sample transfer chamber is also filled with inert gas. The protection of the sample is achieved during the entire transfer process.

[0164] The inert gas protection transfer chamber 001 includes the following steps during use:

[0165] Based on the experimental requirements, the self-locking rotary sampling head 109 and the array probe assembly 101 are separated or installed;

[0166] The array probe assembly 101 disposed at the end of the self-locking rotary sampling head 109 is retracted or pushed out of the array probe storage cavity 107 through the coarse adjustment and / or fine adjustment function of the position adjustment mechanism of the self-locking rotary sampling head 109. Specifically, the magnetic internal connecting rod 102 has three key positions:

[0167] One is the initial position of the magnetic rod, at which the array sampling probe is installed. The array sampling probe is stored in the cavity, and the gate valve can be closed or opened, and the gate valve and the array sampling probe do not interfere with each other;

[0168] The second is to manually adjust the magnetic external driving member 105 to transfer the magnetic internal connecting rod 102 to the initial position of the precision adjustment member, at which time the sample is separated from the array probe storage cavity 107 and is located outside the gate valve;

[0169] The third is the start of fine adjustment, through the rotation of the linear telescopic top rotary drive 1031, the entire precision adjustment component is driven to move downward or upward, wherein the downward movement to the bottom end of the fine adjustment component is the longest position that the array sampling needle can extend.

[0170] If you want to restore the telescopic rod and install the probe assembly back into the cavity, you can manually pull up the magnetic external drive. Let the entire device be used in a horizontal state, and add a force to the magnetic external drive. At this time, the entire device can be used vertically under the action of gravity. But remember not to use the device upside down.

[0171] The inert gas protection transfer chamber 001 is connected to a high-throughput detection mass spectrometer ionization source, and is detected in sequence on a mass spectrometer 004, specifically including the following steps:

[0172] The inside of the sealed inert gas protection ionization source 302 is set to an inert gas protection gas atmosphere in advance;

[0173] The array probe assembly 101 storing the sample to be tested is placed on the micro-sample transfer device, and the bottom of the micro-sample transfer device is connected to the sealing gate valve 303 at the top of the ionization source;

[0174] The micro-sample transfer chamber is used to cooperate with the ionization source. After the cooperation is completed, the plug valve of the micro-sample transfer device and the sealing plug valve 303 at the top of the ionization source are opened. At this time, before and after the valve is opened, the inside of the two chambers are in an inert gas protection gas atmosphere;

[0175] The telescopic magnetic rod of the micro-sample transfer chamber can be used to roughly adjust the height of the array probe. The height of the array probe assembly is adjusted by the locking rotary sampling head position adjustment mechanism. At this time, the probe should be at the upper end of the mass spectrometer injection port. The two-dimensional adjustment member is used to ensure that the lowermost probe is at the center of the mass spectrometer injection port. The height is further lowered to ensure that the lowermost probe is coaxial with the mass spectrometer injection port. Specifically, during use, the probe is aligned with the center of the mass spectrometer injection port. When adjusting, the probe is kept between 1-3 mm and the mass spectrometer injection port, and is moved closer to or farther away from the mass spectrometer according to the needs of the detection.

[0176] By adjusting the screw to rotate the head advancing member 3036, the metal electrode 3031 is gradually moved forward and has a preset spatial distance with the probe at the bottom. At this time, the high-voltage switch is turned on to start the high-voltage input terminal 405 of the high-voltage ionization source; then the probe is gradually moved closer to the mass spectrometer injection port 308, and the distance between the probe and the mass spectrometer injection port 308 is gradually increased according to the strength of the generated ion flow, and the distance is maintained between 1-3 mm. When the detection is completed, the voltage is turned off, and the metal electrode 3031 is moved back a distance away from the probe;

[0177] By adjusting the linear telescopic precision adjustment assembly 103, the probes are lowered one by one in sequence to complete the ionization of all subsequent probes. During this process, the metal electrode 3031 repeatedly moves and does not hinder the gradual descent of the array probe assembly 101 in a non-ionized state.

[0178] After all sample tests are completed, the linear telescopic precision adjustment component 103 is raised by reverse rotation, and the height is restored to the initial position, and then restored to the initial position by the magnetic external drive component.

[0179] During the ionization process, the induction ionization method is adopted, and the metal electrode is brought close to the injection port of the ionization needle, and an AC voltage is applied to the metal electrode.

[0180] The specific process of the gas circulation mentioned above is: when the entire ionization source core cavity assembly is installed in the mass spectrometry system, the gas inside the ionization source core cavity needs to be replaced. When just installed, the inside of the cavity is air, which contains a large amount of water vapor and oxygen, so it is necessary to replace the gas inside the cavity. An inert gas inlet and a vacuum pump connection port are respectively provided in the core cavity. First, the inside of the ionization source is evacuated to a negative pressure using the vacuum port, and an external pressure gauge is used for observation (not shown in the figure). When the pressure in the cavity is below 100pa, an inert gas is filled, wherein the inert gas can be nitrogen. Observe the change in pressure, wherein the pressure in the cavity can be 100kPa one atmosphere, complete the above cycle once, and then go through two cycles, a total of 3 cycles, it can be determined that the gas in the chamber is an ionization injection cavity with an inert gas atmosphere. At this time, the subsequent ionization source detection meets the conditions.

[0181] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A full-process inert gas protection high-throughput mass spectrometry characterization platform, characterized in that: The invention comprises a new glove box (002) that can be connected to a transfer chamber, a high-throughput detection mass spectrometer ionization source (003) connected to a mass spectrometer (004), and an inert gas protection transfer chamber (001). Based on the inert gas protection transfer chamber (001), batches of trace samples of different dimensions to be tested are sampled in the glove box (002). The inert gas protection transfer chamber (001) is connected to the high-throughput detection mass spectrometer ionization source (003) to achieve high-throughput analysis in which multiple samples are loaded at one time and detected sequentially on the mass spectrometer (004). During the sampling, transfer and detection processes, the samples are in a protective gas atmosphere.

2. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 1, characterized in that: The inert gas protection transfer chamber (001) comprises an array probe storage chamber (107), a transfer sealing gate valve (108), an array probe assembly (101), a self-locking rotary sampling head (109) and a self-locking rotary sampling head position adjustment mechanism. The array probe storage chamber (107) is filled with a preset protective gas. The transfer sealing gate valve (108) is installed at the end of the array probe storage chamber (107). The other end of the array probe storage chamber (107) is installed with the self-locking rotary sampling head position adjustment mechanism. The self-locking rotary sampling head (109) is arranged inside the array probe storage chamber (107) and can adjust the distance of its output end relative to the transfer sealing gate valve (108) through the self-locking rotary sampling head position adjustment mechanism. The output end of the self-locking rotary sampling head (109) can be detachably connected to the array probe assembly (101).

3. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 2, characterized in that: The array probe assembly (101) comprises an array probe lower end support base (1013), an array probe upper end fixed cover plate (1012) and an array probe fixing screw (1011); the upper surface of the array probe lower end support base (1013) is uniformly provided with a plurality of grooves parallel to its width direction along its length direction, and each groove forms a linear array arranged at equal intervals; the groove of the array probe lower end support base (1013) is a complete groove capable of accommodating a sampling and ionization detection probe (1014), or a groove is provided on the bottom surface of the array probe upper end fixed cover plate (1012) to cooperate with the array probe lower end support base (1014). The array probe upper end fixing cover plate (1012) has a groove, and the bottom surface groove of the array probe upper end fixing cover plate (1012) and the groove of the array probe lower end supporting base (1013) form a complete groove capable of accommodating the sampling and ionization detection probe (1014); screw holes are provided on the array probe lower end supporting base (1013) at a preset distance from the grooves, and screw holes matching the screw holes of the array probe lower end supporting base are also provided on the array probe upper end fixing cover plate (1012), and the array probe upper end fixing cover plate (1012) and the array probe lower end supporting base (1013) are detachably connected by the array probe fixing screws (1011).

4. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 2, characterized in that: A protrusion is provided on one side of the support base (1013) at the lower end of the array probe of the array probe assembly (101), and the array probe assembly (101) and the self-locking rotary sampling head (109) can be separated and installed based on the cooperation between the output end of the self-locking rotary sampling head (109) and the protrusion.

5. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 2, characterized in that: The bottom of the array probe lower end support base (1013) of the array probe assembly (101) is provided with a protruding step structure, and the array probe assembly (101) separated from the self-locking rotating sampling head (109) is introduced into the experimental device based on the step structure.

6. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 2, characterized in that: The self-locking rotary sampling head position adjustment mechanism is a multi-layer nested structure, comprising a self-locking rotary sampling head storage cavity, a position rough adjustment device, and a linear telescopic precision adjustment component (103); the end of the array probe storage cavity (107) is connected to one end of the self-locking rotary sampling head storage cavity; and the linear telescopic precision adjustment component (103) is installed at one end of the self-locking rotary sampling head storage cavity close to the array probe storage cavity (107); The self-locking rotary sampling head (109) is connected to the output end of the magnetic internal connecting rod (102); the self-locking rotary sampling head storage chamber is specifically a magnetic support outer bracket (104); the position coarse adjustment device comprises a magnetic external driving member (105); the magnetic external driving member (105) is sleeved on the outer wall of the magnetic support outer bracket (104); the magnetic external driving member (105) can slide linearly on the magnetic support outer bracket (104) to synchronously drive the linear sliding of the internal magnetic rod; The magnetic external driving component (105) is provided with a magnetic driving external locking screw (106) for limiting the magnetic external driving component (105) on the magnetic supporting outer bracket (104) after the magnetic external driving component (105) reaches a preset position.

7. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 6, characterized in that: The linear telescopic precision adjustment assembly (103) comprises a linear telescopic bottom fixed support (1038), a linear telescopic sliding thin rod support (1033), a linear telescopic sliding thick rod support (1037), a linear telescopic screw rotation drive (1034), a linear telescopic linear drive translation member (1032), a linear telescopic top fixed support (1035), a linear telescopic nut matching screw drive (1036) and a linear telescopic top rotation drive (1031), wherein the linear telescopic bottom fixed support (103 8) and the linear telescopic linear driving translation member (1032) are provided with holes for the linear telescopic sliding thin rod support member (1033), the linear telescopic sliding thick rod support member (1037), the linear telescopic screw rotating drive member (1034) and the magnetic support outer bracket (104) to pass through, so that the linear telescopic sliding thin rod support member (1033), the linear telescopic sliding thick rod support member (1037), the linear telescopic screw rotating drive member (1034) and the magnetic support outer bracket (104) are arranged in parallel, and the linear telescopic top is fixed The support member (1035) is provided with holes for the linear telescopic sliding thin rod support member (1033), the linear telescopic sliding thick rod support member (1037), and the linear telescopic screw rotation drive member (1034) to pass through; the bottom end of the linear telescopic top rotation drive member (1031) is connected to the linear telescopic screw rotation drive member (1034); the top surface of the linear telescopic top rotation drive member (1031) is provided with a handle; the linear telescopic nut matching screw drive member (1036) is provided with a hole for the linear telescopic sliding thick rod support member (1033), the linear telescopic sliding thick rod support member (1037), and the linear telescopic screw rotation drive member (1034) to pass through; 037) through a hole, the linear telescopic nut cooperates with the screw drive member (1036) to be arranged between the linear telescopic top fixed support member (1035) and the linear telescopic linear drive translation member (1032), the magnetic support outer bracket (104) is connected to the self-locking rotary sampling head storage chamber through a flange, the cross-sectional area of ​​the flange is larger than the cross-sectional area of ​​the opening of the linear telescopic bottom fixed support member (1038), and the cross-sectional area of ​​the magnetic external drive member (105) is larger than the cross-sectional area of ​​the opening of the linear telescopic linear drive translation member (1032).

8. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 1, characterized in that: The side wall of the novel glove box (002) is provided with a connection interface, the connection interface is equipped with an external plug-in valve type glove box transition chamber (201) communicating with the inside and outside of the glove box, the output end of the external plug-in valve type glove box transition chamber (201) is provided with a glove box transition chamber external plug-in valve (210), the external plug-in valve type glove box transition chamber (201) has a sealed working state and an open sample loading state for transferring a sample to be tested, and a movable sample transfer assembly (203) to be tested is provided inside the external plug-in valve type glove box transition chamber (201).

9. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 8, characterized in that: The externally mounted gate valve glove box transition chamber (201) comprises a flange and a glove box transition chamber shell (204), wherein the glove box transition chamber shell (204) is mounted on the glove box side wall via the flange, and both ends of the glove box transition chamber shell (204) are rotatably connected to a sealing panel, and a flange interface connected to the gate valve is provided on the sealing panel (206) on the atmosphere side of the transition chamber away from the glove box, and further comprises a transition chamber door opening stopper (208), wherein the transition chamber door opening stopper (208) is mounted on the outside of the transition chamber, The glove box transition chamber shell (204) is used to limit the door opening angle of the sealing panel (206) on the atmosphere side of the transition chamber. The interior of the glove box transition chamber shell (204) is provided with a glove box transition internal sliding support (202) for adjusting the position of the sample adapter assembly (203) to be tested relative to the interior of the glove box. The glove box transition chamber shell (204) is also provided with a transition chamber door closing sealing locking member (209). The transition chamber door closing sealing locking member (209) cooperates with the sealing panel to complete the sealing state of the sealing panel in the working state.

10. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 8, characterized in that: The side of the sample adapter assembly (203) facing the glove box in the direction of travel is provided with an adapter assembly outer handle (2031), and the other side of the sample adapter assembly (203) is provided with a clamping device of the array probe assembly (101).

11. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 9, characterized in that: A transition chamber pressure gauge (213) is installed on the glove box transition chamber shell (204), a gas connecting pipe (205) is connected to the glove box transition chamber shell (204), the other end of the gas connecting pipe (205) is connected to a tee, an angle valve is arranged on the input pipe section of the tee, a first input pipe section of the tee is connected to a protective gas source, and the other input pipe section of the tee is connected to a negative pressure vacuum device; The external gate valve (210) of the glove box transition chamber can be docked with the transfer sealing gate valve (108) of the inert gas protection transfer chamber (001), thereby completing the transfer of the sample to be tested between the glove box, the external gate valve type glove box transition chamber (201) and the inert gas protection transfer chamber (001).

12. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 1, characterized in that: A mass spectrometry ionization source (003) for high-throughput detection based on inert protection comprises a sealed inert gas protection ionization source (302), wherein the injection end of the sealed inert gas protection ionization source (302) is provided with an ionization source top sealing plug valve (303), and the sealed inert gas protection ionization source (302) is provided with a spatial position adjustment device, so that the detection end of the sealed inert gas protection ionization source (302) can be aligned with a mass spectrometry detector (307) in a detection state. The bottom of the sealed inert gas protection ionization source (302) is connected to an ionization source bottom end storage sample piece (306) for storing the detected array probe assembly (101), the sealed inert gas protection ionization source (302) has a sealed working state and an open sample loading state for transferring the sample to be tested, and the sealed inert gas protection ionization source (302) is provided with a metal electrode (3031) for completing the ionization of the sample to be tested at one end close to the mass spectrometer detector (307).

13. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 12, characterized in that: The ionization source top sealing gate valve (303) can be docked with the transfer sealing gate valve (108) of the inert gas protection transfer chamber (001), thereby completing the transfer of the sample to be tested between the inert gas protection transfer chamber (001) and the closed inert gas protection ionization source (302).

14. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 12, characterized in that: The spatial position adjustment device comprises an upper flange, a lower flange, and an X-direction fine-tuning screw arranged on the upper flange and a Y-direction fine-tuning screw arranged on the lower flange, respectively. The X-direction fine-tuning screw and the Y-direction fine-tuning screw are arranged vertically in space. The lower flange is mounted on an upper plate of a closed inert gas shielded ionization source (302), and the upper flange and the lower flange are connected via a bellows.

15. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 12, characterized in that: The main body of the sealed inert gas protection ionization source (302) is a rectangular metal support (305), one side of which cooperates with the mass spectrometer detector (307), the left side sealing panel of the ionization source and the right side sealing panel of the ionization source are installed with a visible non-metallic lens for sealing, and the side facing the ionization source injection port is provided with an ionization source front side sealing panel, and a non-metallic transparent panel is installed on the ionization source front side sealing panel.

16. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 12, characterized in that: Two clamps are placed on both sides of the injection port of the mass spectrometer detector (307), both of which are used to place the locking shaft of the ionization source mass spectrometer injection port (308); after the cavity of the mass spectrometer detector (307) is placed at a specific position of the injection port of the ionization source, the two are assembled by locking the shaft and the clamp, and a sealing device is provided at the locking position of the two; A filling hole for inert gas and an extraction port for gas inside the cavity are arranged on the main body of the sealed inert gas protection ionization source (302), and the extraction port is connected to a connection port of an exhaust pump (212).

17. The full-process inert gas protection high-throughput injection mass spectrometry characterization platform according to claim 12, characterized in that: The base of the metal electrode (3031) is movable in at least one-dimensional plane, the base is a non-metallic electrode (3031) support (3032), the input end of the metal electrode (3031) is connected to an external ionization source high-voltage input end (405) via an electrode connecting metal conductive member (3033), a through-plate electrode is provided at a connection point between the metal electrode (3031) and the ionization source high-voltage input end (405) and a main body sealing plate of a closed inert gas protection ionization source (302), the through-plate electrode is a through-plate metal electrode straight-through rod (403), and the through-plate metal electrode straight-through rod (403) is connected to the sealing plate via a through-plate electrode radial sealing O-ring (404) and a through-plate electrode axial sealing O-ring (402); The device capable of completing movement in a one-dimensional plane specifically comprises an electrode support connecting sliding member (3034) connected below a non-metallic electrode support member (3032), wherein the electrode support connecting sliding member (3034) is capable of moving on a fixed slide rail (3035) arranged below the electrode support connecting sliding member (3034), an input end of the electrode support connecting sliding member (3034) is connected to a screw rotating head advancing member (3036), an identification device with scale markings is arranged on the screw rotating head advancing member (3036), the screw rotating head advancing member (3036) is connected to a main sealing plate of a closed inert gas protection ionization source (302) through a screw head external support member (3038), and a screw advancing radial sealing O-ring (3039) is arranged at the sealing position.

18. A method for using the mass spectrometry characterization platform for high-throughput sampling with inert gas protection throughout the entire process according to any one of claims 1 to 17, characterized in that: The steps include: Based on the inert gas protection transfer chamber (001), batches of trace samples of different dimensions to be tested are sampled in a glove box (002); Separating the inert gas protection transfer chamber (001) and the glove box (002); The inert gas protection transfer chamber (001) is connected to a high-throughput detection mass spectrometry ionization source (003), and is detected in sequence on a mass spectrometer (004); After the detection is completed, the inert gas protection transfer chamber (001) and the high-throughput detection mass spectrometry ionization source (003) are separated.

19. The method according to claim 18, characterized in that Based on the inert gas protection transfer chamber (001), the batch of trace samples of different dimensions to be tested are sampled in the glove box (002), which specifically includes the following steps: The sealing panel is opened. Before opening, it is necessary to ensure that the interior of the external plug-in valve glove box transition chamber (201) is at normal pressure, and the sample transfer assembly (203) to be tested is placed inside the external plug-in valve glove box transition chamber (201); The atmosphere-side sealing panel of the external plug-in valve glove box transition chamber (201) is covered and the sealing locking member is closed at the same time. During this process, the front plug-in valve is in a closed and sealed state and the sealing panel inside the glove box is also in a closed state. The interior of the glove box transition chamber shell (204) is evacuated to provide a protective gas atmosphere. Based on the experimental requirements, the self-locking rotary sampling head (109) and the array probe assembly (101) are installed to form a protective gas atmosphere inside the micro-sample transfer chamber; Connecting the transfer sealing plug valve (108) of the micro-sample transfer chamber to the plug valve of the plug valve type glove box; The array probe assembly (101) disposed at the end of the self-locking rotary sampling head (109) is pushed out of the array probe storage cavity (107) through the coarse adjustment and / or fine adjustment function of the self-locking rotary sampling head position adjustment mechanism; The transfer sealing plug valve (108) of the micro-sample transfer chamber and the plug valve of the plug valve type glove box are opened to transfer the array probe assembly (101) into the glove box.

20. The method according to claim 18, characterized in that The inert gas protection transfer chamber (001) comprises the following steps during use: Based on experimental requirements, the self-locking rotary sampling head (109) and the array probe assembly (101) are separated or installed; The array probe assembly (101) disposed at the end of the self-locking rotary sampling head (109) is retracted or pushed out into the array probe storage cavity (107) through the coarse adjustment and / or fine adjustment function of the position adjustment mechanism of the self-locking rotary sampling head (109). Specifically, the magnetic internal connecting rod (102) has three key positions: One is the initial position of the magnetic rod, at which the array sampling probe is installed. The array sampling probe is stored in the cavity, and the gate valve can be closed or opened, and the gate valve and the array sampling probe do not interfere with each other; The second is to manually adjust the magnetic external driving member (105) to transfer the magnetic internal connecting rod (102) to the initial position of the precision adjustment member, at which time the sample is separated from the array probe storage cavity (107) and is located outside the gate valve; The third is the start of fine adjustment, through the rotation of the linear telescopic top rotary drive member (1031), the entire precision adjustment member is driven to move downward or upward, wherein the downward movement to the bottom end of the fine adjustment assembly is the longest position that the array sampling needle can extend; The inert gas protection transfer chamber (001) is connected to a high-throughput detection mass spectrometry ionization source, and is detected in sequence on a mass spectrometer (004), specifically comprising the following steps: Pre-setting the interior of the sealed inert gas protection ionization source (302) to an inert gas protection gas atmosphere; Placing the array probe assembly (101) storing the sample to be tested on a micro-sample transfer device, and docking the bottom of the micro-sample transfer device with the sealing plug valve (303) at the top of the ionization source; Open the plug valve of the micro-sample transfer device and the top sealing plug valve of the ionization source (303), and before and after the valves are opened, the insides of the two cavities are in an inert gas protection gas atmosphere; The height of the array probe assembly (101) is adjusted by a locking rotary sampling head position adjustment mechanism. At this time, the probe should be located at the upper end of the mass spectrometer injection port (308). The lowermost probe is ensured to be located at the center of the mass spectrometer injection port (308) by a two-dimensional adjustment member. The height is further lowered to ensure that the lowermost probe is coaxial with the mass spectrometer injection port (308). The metal electrode (3031) is gradually moved forward by adjusting the screw rotating head advancing member (3036) and has a preset spatial distance with the lowermost probe. At this time, the high-voltage switch is turned on to start the high-voltage input end (405) of the high-voltage ionization source; then, the probe is gradually moved closer to the mass spectrometer injection port (308), and the distance between the probe and the mass spectrometer injection port (308) is gradually increased according to the strength of the generated ion flow, and the distance is maintained between 1 and 3 mm. When the detection is completed, the voltage is turned off, and the metal electrode (3031) is moved back a distance away from the probe; By adjusting the linear telescopic precision adjustment component (103), the probes are lowered one by one in sequence to complete the ionization of all subsequent probes. During this process, the metal electrode (3031) repeatedly moves and does not hinder the gradual descent of the array probe component (101) in a non-ionized state. After all samples are tested, the linear telescopic precision adjustment component (103) is raised by reverse rotation, and the height is restored to the initial position, and then restored to the initial position by the magnetic external drive component.

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