Method for identifying Maotai-flavor liquor

Abstract

The invention discloses an identification method of Maotai-flavor liquor, and relates to the technical field of liquor identification, and the identification method comprises the following steps: 1, enriching volatile components in a Maotai-flavor liquor sample by using a solid-phase micro-extractor, injecting the volatile components into a sample inlet of a chromatographic instrument main body through a sample injector for desorption after extraction, and in the sample injection process, determining the volatile components in the Maotai-flavor liquor sample; the electric heating plate and the fan can provide heat for sample introduction of the sample injector; and 2, separating the desorbed volatile components through a chromatographic column arranged in the chromatographic instrument main body, when the separated components flow out of the chromatographic column and enter a detector, generating an electric signal by the detector, processing the electric signal, and recording the processed electric signal by data acquisition of the chromatographic instrument main body to form a chromatogram, so as to obtain a total ion chromatogram and mass spectrum data. The sample injector is innovatively designed, the multi-inner-diameter capillary tube switchable technology is advanced in the field of white spirit analysis and identification, the problem that the inner diameter of a capillary tube of an existing sample injector is single is solved, and the analysis precision and flexibility are improved.

Description

Technical Field

[0001] The present invention relates to the technical field of liquor identification, and particularly to a method for identifying Maotai-flavor liquor. Background Art

[0002] Maotai-flavor liquor occupies an important position in the global liquor market with its unique flavor and excellent quality, and is deeply loved and pursued by consumers. However, the influx of counterfeit and shoddy Maotai-flavor liquor products into the market has seriously disrupted the normal market order, damaged the rights and interests of consumers, as well as the reputation and interests of regular production enterprises.

[0003] In the field of liquor analysis and identification, gas chromatographs are widely used analytical instruments. As a key component for samples to enter the instrument, the injector of a gas chromatograph. Currently, there are various types of injectors for gas chromatographs on the market. Some of these injectors are equipped with a capillary that can finely regulate the process of the sample entering the chromatographic column, accurately controlling the sample injection volume and flow rate. In the split injection mode, the capillary can accurately split the sample into two parts according to a pre-set split ratio. One part is discharged from the system, and the other part enters the chromatographic column for analysis, thereby ensuring that the amount of sample entering the chromatographic column is within an appropriate range, avoiding peak overload or poor separation effect due to excessive injection volume, or affecting the detection sensitivity due to too small injection volume. In the splitless injection mode, the capillary can guide the sample to enter the chromatographic column at a stable and uniform speed and state, which is beneficial to obtaining a good chromatographic peak shape and separation effect. In addition, parameters such as the inner diameter of the capillary can be flexibly selected according to specific analysis requirements. A capillary with a relatively small inner diameter can form a narrow injection band when the sample enters the chromatographic column, significantly improving the resolution, which helps to clearly separate many volatile components with similar properties in liquor, thereby achieving accurate qualitative and quantitative analysis.

[0004] However, the capillary in the existing injector with a capillary is usually designed with a single inner diameter. In actual liquor identification work, different identification items and sample types often require capillaries with different inner diameters to optimize the injection process and chromatographic separation effect. However, due to the fixed inner diameter of the capillary in the existing injector, when it is necessary to replace the inner diameter of the capillary according to specific requirements, complex replacement operations usually need to be carried out after stopping the machine. This process is not only time-consuming and laborious, but also causes the instrument to stop running for a long time, reducing the detection efficiency and increasing the analysis cost, restricting the flexibility and efficiency of liquor analysis and detection work.

[0005] In view of this, the present application is specifically proposed. Summary of the Invention

[0006] The purpose of the present invention is to provide a method for identifying Maotai-flavor liquor to solve the problems raised in the above background art.

[0007] To solve the above technical problems, a method for identifying Maotai-flavor liquor provided by the present invention includes the following steps:

[0008] Step 1: Enrich the volatile components in the Maotai-flavor liquor sample by using a solid-phase microextractor. After extraction, inject through an injector into the injection port of the chromatograph main body for desorption. During the injection process, an electric heating plate and a blower can provide heat for the injection of the injector.

[0009] Step 2: Separate the desorbed volatile components through the chromatographic column provided in the chromatograph main body. When the separated components flow out of the chromatographic column and enter the detector, the detector generates an electrical signal and, after being processed, is recorded by the data acquisition of the chromatograph main body to form a chromatogram, obtaining a total ion current chromatogram and mass spectrometry data.

[0010] Step 3: Process the data, screen out the characteristic volatile component markers and their relative content ratio relationships; establish an identification model. According to the characteristic marker and its relative content data, input the characteristic marker data into the identification model to determine the authenticity and quality grade of the sample to be tested.

[0011] Among them, the injector includes

[0012] An injection tube, which is mounted on the upper part of the chromatograph main body and has a vaporization cavity and an injection cavity communicating with each other inside. On the inner bottom wall of the injection cavity, an output tube extending downward is provided. The heat from the electric heating plate is used to vaporize the liquor sample injected into the vaporization cavity and introduce it into the chromatographic column through the output tube.

[0013] Among them, a carrier gas tube and a blowing tube communicating with the vaporization cavity are provided on the upper side wall of the injection tube, and a shunt tube communicating with the vaporization cavity is provided on the lower side wall.

[0014] A rotating shaft, which is vertically rotatably arranged on the side wall of the injection tube, and a turntable is connected to its outer wall.

[0015] A plurality of positioning seats are equidistantly distributed along the outer wall of the turntable circumference. A positioning groove is opened along its central axis on the positioning seat. The capillary tube body is detachably installed inside the positioning groove. The inner diameters of the capillary tube bodies are not equal. When the turntable rotates, the plurality of positioning seats can alternately enter the injection cavity to make the positioning groove and the vaporization cavity sealed and conduct.

[0016] Furthermore, a variable-diameter groove expanding radially is provided on the inner wall of the positioning groove, and a flexible positioning member for fixing the capillary tube body is provided inside the variable-diameter groove. The flexible positioning member includes

[0017] A flexible sleeve, which is integrally sleeved outside the capillary tube body, and its outer wall is fixed to the inner wall of the variable-diameter groove. A sealed filling cavity is opened inside the flexible sleeve.

[0018] A thermoplastic filler is filled in the filling cavity inside the flexible sleeve without gaps, wherein the hardness of the thermoplastic filler increases when heated and decreases after cooling;

[0019] The flexible heat absorbing plate is installed inside the flexible sleeve and can generate flexible deformation when the flexible sleeve is squeezed.

[0020] Furthermore, a sliding groove is provided inside the positioning seat, a movable opening is provided on the side wall of the diameter-changing groove along the radial direction of the positioning seat, the diameter-changing groove and the sliding groove are connected through the movable opening, a resisting rod is provided inside the movable opening for sliding, and an extrusion plate is provided at one end of the resisting rod extending to the inside of the diameter-changing groove;

[0021] A sliding sleeve is slidably installed inside the sliding groove, a conical sleeve is connected to the bottom surface of the sliding sleeve, a reset spring is connected to the bottom surface of the conical sleeve, the bottom end of the reset spring is connected to the bottom wall of the sliding groove, one end of the resistance rod extends to the inside of the sliding groove and resists against the inner wall of the conical sleeve, when the sliding sleeve drives the conical sleeve to move axially upward along the positioning seat, multiple resistance rods can drive the extrusion plate to synchronously close to the central axis of the positioning seat.

[0022] Furthermore, a radially-distributed groove is provided on the side wall of the positioning seat, the groove is connected to the sliding groove, a transmission rod is slidably provided inside the groove, one end of the transmission rod is connected to the outer wall of the sliding sleeve, and the other end extends to the outside of the positioning seat;

[0023] An inclined plate is arranged on the upper surface of the output tube, and the transmission rod slides along the surface of the inclined plate when the positioning seat rotates to the inside of the injection cavity.

[0024] Furthermore, a cover plate is provided on the top surface of the sample injection tube, the cover plate is covered on the top surface of the turntable, and the bottom surface of the cover plate is in contact with the top surface of the turntable.

[0025] Furthermore, it also includes a locking assembly arranged on the sample injection tube for locking the rotation of the turntable, and the locking assembly includes:

[0026] A horizontal plate vertically extending along the radial direction of the sample injection tube, one end of which extends above the rotating disk and is rotatably connected to a rotating plate;

[0027] A pin rod is hinged at one end of the rotating plate, and a plurality of positioning holes for the pin rods to be inserted are provided on the top surface of the rotating plate, and the position of each positioning hole corresponds to the positioning seat;

[0028] A push spring is connected to the bottom surface of the pin rod away from one end of the rotating plate, and the other end of the push spring is fixed to the top surface of the horizontal plate.

[0029] Further, an inner liner tube that can slide vertically along the inner wall of the vaporization cavity is arranged inside the sample injection tube. A flow channel is opened inside the inner liner tube. The upper port of the flow channel communicates with the vaporization cavity, and the lower port of the flow channel communicates with the sample injection cavity. A connection seat is screwed inside the port at the top end of the sample injection tube. A receiving groove communicating with the vaporization cavity is penetrated through the connection seat; a septum is sleeved inside the receiving groove. A sealing cover is screwed outside the port at the top end of the sample injection tube. The inner wall of the sealing cover presses against the top surface of the septum. An injection hole communicating with the septum is opened at the center of the sealing cover.

[0030] Further, an annular groove communicating with the sliding groove is opened on the top surface of the positioning seat. One end of the sliding sleeve extending into the annular groove is connected with a rubber sealing ring. A sealing groove for the rubber sealing ring to extend into is opened on the end surface at the bottom end of the inner liner tube.

[0031] Further, an annular embedding groove is opened on the outer wall of the inner liner tube at the position between the carrier gas tube and the shunt tube. A sealing lip is embedded and installed inside the embedding groove. The sealing lip is attached to the inner wall of the sample injection tube.

[0032] Further, a limiting member is arranged on the bottom surface of the connection seat. An inwardly concave connection groove is arranged at the port at the top end of the inner liner tube. The limiting member is embedded in the connection groove opened on the inner liner tube;

[0033] Wherein, the limiting member includes a supporting portion and a limiting portion. The supporting portion is of a long columnar structure. One end of the supporting portion is connected to the bottom surface of the connection seat, and the other end extends along the axial direction of the sample injection tube and is connected to the limiting portion. The limiting portion is of a ring structure. A plurality of convex teeth distributed along its circumferential direction are arranged on the inner side wall of the inner ring of the limiting portion. Grooves for the convex teeth to be engaged are arranged on the inner wall of the connection groove.

[0034] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0035] 1. In the present invention, the rotating shaft in the sampler drives the turntable to rotate, so that the capillary bodies with different inner diameters alternately enter the sample injection cavity and the vaporization cavity in the positioning groove of the positioning seat for sealed conduction. Thus, a capillary with a suitable inner diameter can be selected for sample injection according to requirements to optimize the sample injection and separation effects; the design of the sampler that can switch capillary tubes with different inner diameters improves the flexibility of sample injection and analysis, can meet the analysis requirements of different Baijiu samples, can select the most suitable capillary inner diameter for different Baijiu with different component concentrations and types, is beneficial to improving the resolution and detection accuracy, and provides a guarantee for the subsequent data processing and the reliability of the identification model.

[0036] 2. In the present invention, after the capillary body is inserted into the positioning groove, the flexible positioning piece starts to work, and the thermoplastic filler is in a relatively soft state at room temperature. When it is necessary to tightly wrap the flexible sleeve around the outside of the capillary body to prevent the vaporized sample from leaking from between the capillary body and the thermoplastic filler, the flexible heat absorbing plate can quickly absorb the heat from the electric heating plate inside the vaporization cavity, and can heat the flexible sleeve and the thermoplastic filler inside. The hardness of the thermoplastic filler increases when heated, thereby generating a tightening force on the capillary body to achieve sealing and fixation. After cooling, the hardness of the thermoplastic filler decreases, which facilitates the disassembly and replacement of the capillary body.

[0037] 3. In the present invention, when the sliding sleeve moves upward along the axial direction of the positioning seat under external power, the conical sleeve is driven to move upward, and its inner wall squeezes the resistance rod, so that the resistance rod drives the extrusion plate to close to the central axis of the positioning seat, thereby further clamping and fixing the capillary body and enhancing the fixing effect; multiple fixing and clamping functions of the capillary body are realized, and through cooperation with the flexible positioning piece, the position of the capillary body can be ensured to be stable during the injection process, and will not be displaced or loosened due to factors such as carrier gas flow and temperature changes, thereby improving the accuracy and repeatability of the injection. This precise injection control helps to improve the reliability of the chromatographic analysis results, making the detection data of the volatile components in the sauce-flavor liquor more accurate, which is conducive to the subsequent screening of characteristic markers and the establishment of identification models. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 It is a left-side structural schematic diagram of the present invention;

[0039] Figure 2 It is a right view structural schematic diagram of the present invention;

[0040] Figure 3 It is a schematic diagram of the cross-sectional structure of the present invention;

[0041] Figure 4 It is a structural schematic diagram of the sample injection tube in the present invention;

[0042] Figure 5 for Figure 4 Schematic diagram of the explosion structure;

[0043] Figure 6 It is a schematic diagram of the connection structure between the positioning seat and the rotating disk in the present invention;

[0044] Figure 7 It is a schematic diagram of the structure of the output tube in the present invention;

[0045] Figure 8 It is a structural schematic diagram of the positioning seat in the present invention;

[0046] Figure 9 It is a schematic diagram of the cross-sectional structure of the positioning seat in the present invention;

[0047] Figure 10 It is a schematic diagram of the connection structure between the sample injector of the present invention and the gas chromatograph.

[0048] In the figure: 1, injection tube; 2, carrier gas tube; 3, injection tube; 4, splitter tube; 5, liner tube; 6, flow channel; 7, connecting seat; 8, receiving groove; 9, septum; 10, sealing cover; 11, vaporization cavity; 12, injection cavity; 13, output tube; 14, rotating shaft; 15, turntable; 16, positioning seat; 17, cover plate; 18, positioning hole; 19, horizontal plate; 20, rotating plate; 21, pin rod; 22, push spring; 23, inclined plate; 24, capillary body; 25, positioning groove; 26 , reducing groove; 27, sliding groove; 28, annular groove; 29, sliding sleeve; 30, rubber sealing ring; 31, tapered sleeve; 32, transmission rod; 33, reset spring; 34, flexible sleeve; 35, resistance rod; 36, extrusion plate; 37, thermoplastic filler; 38, flexible heat absorbing plate; 39, yielding groove; 40, limiting piece; 100, injector; 200, chromatograph body; 300, detector; 400, chromatographic column; 500, electric heating plate; 600, fan; 700, solid phase microextractor. DETAILED DESCRIPTION

[0049] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions 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. 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.

[0050] See also Figures 1-10 The present invention provides a technical solution: a method for identifying Maotai-flavor liquor, comprising the following steps:

[0051] Step 1: The volatile components in the Maotai-flavor liquor sample are enriched by using a solid phase microextractor 700, and after extraction, the volatile components are injected into the injection port of the chromatograph body 200 through the injector 100 for desorption. During the injection process, the electric heating plate 500 and the fan 600 can provide heat for the injection of the injector 100;

[0052] Step 2: The desorbed volatile components are separated by the chromatographic column 400 provided in the chromatograph body 200. When the separated components flow out of the chromatographic column 400 and enter the detector 300, the detector 300 generates an electrical signal which is processed and recorded by the data acquisition of the chromatograph body 200 to form a chromatogram, thereby obtaining a total ion current chromatogram and mass spectrum data;

[0053] Step 3: Process the data, screen out the characteristic volatile component markers and their relative content ratio relationships; establish a discrimination model, and based on the characteristic marker and its relative content data, input the characteristic marker data into the discrimination model to determine the authenticity and quality grade of the sample to be tested.

[0054] Among them, the injector 100 includes

[0055] An injection tube 1, which is mounted on the upper part of the chromatograph main body 200, has a vaporization cavity 11 and an injection cavity 12 communicating with each other inside. An output tube 13 extending downward is provided on the inner bottom wall of the injection cavity 12. The white liquor sample injected into the vaporization cavity 11 is vaporized by the heat from the hot plate 500 and introduced into the chromatographic column 400 through the output tube 13.

[0056] Among them, a carrier gas tube 2 and a blowing tube 3 communicating with the vaporization cavity 11 are provided on the upper side wall of the injection tube 1, and a shunt tube 4 communicating with the vaporization cavity 11 is provided on the lower side wall.

[0057] A rotating shaft 14 is vertically rotatably provided on the side wall of the injection tube 1, and a turntable 15 is connected to its outer wall.

[0058] A plurality of positioning seats 16 are equidistantly distributed along the outer wall of the turntable 15 in the circumferential direction. A positioning groove 25 is provided on the positioning seat 16 along its central axis. A capillary tube body 24 is detachably installed inside the positioning groove 25. The inner diameters of the capillary tube bodies 24 are not equal. When the turntable 15 rotates, the plurality of positioning seats 16 can alternately enter the injection cavity 12 to make the positioning groove 25 in sealed communication with the vaporization cavity 11.

[0059] Specifically, the rotating shaft 14 in the injector 100 drives the turntable 15 to rotate, so that the capillary tube bodies 24 with different inner diameters alternately enter the injection cavity 12 and the vaporization cavity 11 in the positioning grooves 25 of the positioning seats 16 in sealed communication. Thus, a capillary tube with a suitable inner diameter can be selected for injection according to requirements to optimize the injection and separation effects; the design of the injector 100 that can switch capillary tubes with different inner diameters improves the flexibility of injection and analysis, can adapt to the analysis requirements of different white liquor samples, can select the most suitable capillary inner diameter for white liquors with different component concentrations and types, is beneficial to improving the resolution and detection accuracy, and provides a guarantee for subsequent data processing and the reliability of the discrimination model.

[0060] Refer to Figure 8 and Figure 9 , a variable diameter groove 26 expanding radially is provided on the inner wall of the positioning groove 25, and a flexible positioning member for fixing the capillary tube body 24 is provided inside the variable diameter groove 26. The flexible positioning member includes

[0061] The flexible sleeve 34 is integrally sleeved outside the capillary body 24, and its outer wall is fixed to the inner wall of the variable diameter groove 26. A sealed filling cavity is provided inside the flexible sleeve 34;

[0062] The thermoplastic filler 37 is filled in the filling cavity inside the flexible sleeve 34 without gaps. The hardness of the thermoplastic filler 37 increases when heated and decreases after cooling;

[0063] The flexible heat absorption plate 38 is installed inside the flexible sleeve 34 and can generate flexible deformation when the flexible sleeve 34 is squeezed.

[0064] Specifically,

[0065] After the capillary body 24 is inserted into the positioning groove 25, the flexible positioning member starts to work. The thermoplastic filler 37 is in a relatively soft state at normal temperature. When it is necessary to tightly wrap the flexible sleeve 34 outside the capillary body 24 to prevent the vaporized sample from leaking between the capillary body 24 and the thermoplastic filler 37, the flexible heat absorption plate 38 can quickly absorb the heat generated by the electric heating plate 500 inside the vaporization cavity 11, and can heat the flexible sleeve 34 and the internal thermoplastic filler 37. The hardness of the thermoplastic filler 37 increases when heated, thereby generating a fastening force on the capillary body 24 to achieve sealing and fixing. After cooling, the hardness of the thermoplastic filler 37 decreases, facilitating the disassembly and replacement of the capillary body 24;

[0066] Compared with the traditional fixing structure, this flexible positioning member can further improve the sealing performance of the connection between the capillary body 24 and the flexible sleeve 34 during the process of vaporizing the white liquor sample. At the same time, the thermoplastic filler 37 after heating and hardening further improves the fixing stability of the capillary body 24, improves the convenience of operation of the sampler 100. At the same time, it reduces the risk of capillary damage caused by the complex fixing structure, extends the service life of the capillary, and thus ensures the stability and continuity of the entire white liquor identification process.

[0067] Refer to Figure 9 In the positioning seat 16, a sliding groove 27 is further provided. An activity opening is provided on the side wall of the variable diameter groove 26 along the radial direction of the positioning seat 16. The variable diameter groove 26 is communicated with the sliding groove 27 through the activity opening. A resisting rod 35 is slidably arranged inside the activity opening. One end of the resisting rod 35 extending into the variable diameter groove 26 is provided with a pressing plate 36;

[0068] A sliding sleeve 29 is slidably installed inside the sliding groove 27, a conical sleeve 31 is connected to the bottom surface of the sliding sleeve 29, a return spring 33 is connected to the bottom surface of the conical sleeve 31, the bottom end of the return spring 33 is connected to the inner bottom wall of the sliding groove 27, and one end of the resistance rod 35 extends to the inside of the sliding groove 27 and resists against the inner wall of the conical sleeve 31. When the sliding sleeve 29 drives the conical sleeve 31 to move axially upward along the positioning seat 16, multiple resistance rods 35 can drive the extrusion plate 36 to close synchronously toward the central axis of the positioning seat 16.

[0069] Specifically, the sliding groove 27, the reducing groove 26 and related components inside the positioning seat 16 work together. When the sliding sleeve 29 moves upward along the axial direction of the positioning seat 16 under external power, the conical sleeve 31 is driven to move upward, and its inner wall squeezes the abutment rod 35, so that the abutment rod 35 drives the extrusion plate 36 to close to the central axis of the positioning seat 16, thereby further clamping and fixing the capillary body 24 to enhance the fixing effect; multiple fixing and clamping functions of the capillary body 24 are realized, and through cooperation with the flexible positioning member, the position of the capillary body 24 can be ensured to be stable during the injection process, and will not be displaced or loosened due to factors such as carrier gas flow and temperature changes, thereby improving the accuracy and repeatability of the injection. This precise injection control helps to improve the reliability of the chromatographic analysis results, making the detection data of the volatile components in the sauce-flavored liquor more accurate, which is conducive to the subsequent screening of characteristic markers and the establishment of identification models.

[0070] See also Figures 6-9 A radially extending groove 39 is provided on the side wall of the positioning seat 16. The groove 39 is connected to the sliding groove 27. A transmission rod 32 is slidably provided inside the groove 39. One end of the transmission rod 32 is connected to the outer wall of the sliding sleeve 29, and the other end extends to the outside of the positioning seat 16.

[0071] An inclined plate 23 is disposed on the upper surface of the output tube 13 , and the transmission rod 32 slides along the surface of the inclined plate 23 when the positioning seat 16 rotates to the inside of the injection cavity 12 .

[0072] Specifically, when the positioning seat 16 rotates to the inside of the injection cavity 12, the inclined plate 23 on the output tube 13 contacts the transmission rod 32. As the positioning seat 16 rotates, the transmission rod 32 slides along the surface of the inclined plate 23. Due to the inclined surface design of the inclined plate 23, the transmission rod 32 drives the sliding sleeve 29 to move axially along the positioning seat 16, thereby triggering a series of actions such as the upper sliding sleeve 29 driving the tapered sleeve 31, thereby realizing the automatic clamping and fixing operation of the capillary body 24.

[0073] The automatic clamping and fixing function during the sample injection process is realized. Without additional manual operations or complex electronic control devices, through the ingenious design of the mechanical structure, the capillary body 24 is automatically clamped and fixed while the positioning seat 16 rotates into place. This improves the efficiency and automation level of the sample injection operation, reduces the errors and uncertainties that may be brought by manual operations, further ensures the accuracy and stability of the sample injection, and is conducive to improving the efficiency and reliability of the entire Baijiu identification process.

[0074] Refer to Figure 1 On the top surface of the sample injection tube 1, there is a cover plate 17, and the cover plate 17 covers the top surface of the turntable 15, and the bottom surface of the cover plate 17 fits with the top surface of the turntable 15.

[0075] Specifically,

[0076] The cover plate 17 provided on the top surface of the sample injection tube 1 covers and fits on the top surface of the turntable 15. The cover plate 17 plays a role in protecting components such as the turntable 15 and the internal capillary body 24, preventing external dust, impurities, etc. from entering the inside of the sample injection tube 1 and affecting the sample injection and analysis processes;

[0077] It effectively protects the internal components of the injector 100, reduces problems such as capillary blockage and component corrosion caused by external pollution, reduces the failure rate of the instrument, extends the maintenance cycle of the injector 100, ensures the normal progress of the Baijiu identification work, reduces analysis interruptions and data errors caused by instrument failures, and improves the stability and reliability of the entire identification process.

[0078] Refer to Figure 1 、 Figure 3 、 Figure 4 、 Figure 5 and Figure 6 ,It also includes a locking component provided on the sample injection tube 1 for locking the rotation of the turntable 15. The locking component includes,

[0079] A cross plate 19, extending vertically along the radial direction of the sample injection tube 1, and one end of it extending above the turntable 15 is rotatably connected to a rotating plate 20;

[0080] A pin rod 21, hinged at one end of the rotating plate 20. On the top surface of the turntable 15, there are multiple positioning holes 18 for the pin rod 21 to insert, and the positions of each positioning hole 18 correspond to the positioning seat 16;

[0081] A top - push spring 22, connected to the bottom surface of the pin rod 21 far from the rotating plate 20, and the other end of the top - push spring 22 is fixed to the top surface of the cross plate 19.

[0082] Specifically, the cross plate 19, rotating plate 20, pin rod 21 and pushing spring 22 in the locking component work together. When it is necessary to lock the position of the turntable 15, rotate the rotating plate 20, so that the pin rod 21 is inserted into the corresponding positioning hole 18 on the top surface of the turntable 15 under the action of the pushing spring 22, thereby restricting the rotation of the turntable 15, ensuring the fixed position of the currently selected capillary body 24, and guaranteeing the stability of the sampling process. When it is necessary to switch the capillary body 24, lift the pin rod 21 against the elastic force of the pushing spring 22 and rotate the turntable 15;

[0083] It realizes the precise locking and unlocking functions of the rotation of the turntable 15. During the sampling process, it can effectively prevent the turntable 15 from rotating due to accidental collision or vibration, ensuring the stability and accuracy of the sampling of the selected capillary body 24. When it is necessary to switch the capillary, it can be conveniently unlocked, improving the flexibility and reliability of the operation of the sampler 100, facilitating the rapid switching between different white liquor sample analysis requirements, and ensuring the efficiency and accuracy of the entire white liquor identification process.

[0084] Refer to Figures 1-3 As shown in the figure, inside the sampling tube 1, there is a lining tube 5 that can slide vertically along the inner wall of the vaporization cavity 11. A flow channel 6 is opened inside the lining tube 5. The upper port of the flow channel 6 communicates with the vaporization cavity 11, and the lower port of the flow channel 6 communicates with the sampling cavity 12. A connecting seat 7 is screwed inside the port at the top of the sampling tube 1, and a receiving groove 8 communicating with the vaporization cavity 11 is provided through the connecting seat 7; A septum 9 is sleeved inside the receiving groove 8. A sealing cover 10 is screwed outside the port at the top of the sampling tube 1, and the inner wall of the sealing cover 10 presses against the top surface of the septum 9. An injection hole communicating with the septum 9 is opened at the center of the sealing cover 10.

[0085] Specifically,

[0086] The lining tube 5 inside the sampling tube 1 connects the vaporization cavity 11 and the sampling cavity 12 through the flow channel 6, enabling the vaporized white liquor sample to smoothly enter the sampling cavity 12 from the vaporization cavity 11 and be introduced into the chromatographic column 400 through the output tube 13. The receiving groove 8 on the connecting seat 7 is used to accommodate the septum 9. The sealing cover 10 seals the top port of the sampling tube 1 by pressing the septum 9, and the injection hole is used to inject the white liquor sample into the vaporization cavity 11;

[0087] It optimizes the internal structure and sampling process of the sampling tube 1. The design of the lining tube 5 helps to stabilize the sample vaporization and transmission process, reducing sample residue and cross-contamination. The cooperation of the connecting seat 7, septum 9 and sealing cover 10 achieves a good sealing effect, preventing sample leakage and external gas from entering, ensuring the accuracy and stability of sampling, facilitating the improvement of the reliability of chromatographic analysis results, making the detection of volatile components in Maotai-flavor white liquor more accurate, and providing more reliable data support for white liquor identification.

[0088] Refer toFigure 3 , Figure 8 and Figure 9 , an annular groove 28 communicating with the sliding groove 27 is formed on the top surface of the positioning seat 16. One end of the sliding sleeve 29 extending into the annular groove 28 is connected with a rubber sealing ring 30, and a sealing groove for the rubber sealing ring 30 to extend into is formed on the end surface at the bottom end of the inner liner tube 5.

[0089] Specifically, the annular groove 28 on the top surface of the positioning seat 16, the rubber sealing ring 30 connected to the sliding sleeve 29, and the sealing groove on the end surface at the bottom end of the inner liner tube 5 cooperate with each other. When the relative position between the positioning seat 16 and the inner liner tube 5 changes, the rubber sealing ring 30 can be driven by the sliding sleeve 29 to extend into or withdraw from the sealing groove, so as to realize the sealing control of the connection part between the positioning seat 16 and the inner liner tube 5, prevent the leakage of samples or carrier gas; improve the sealing performance of the key connection parts inside the injector 100, effectively avoid problems such as sample loss and carrier gas leakage caused by poor sealing, ensure the stable flow of samples and carrier gas during the sampling process, improve the accuracy and repeatability of sampling, help to obtain more reliable chromatographic analysis data, and further improve the accuracy and credibility of the liquor identification results.

[0090] Refer to Figure 3 and Figure 5 , an annular embedding groove is formed on the outer wall of the inner liner tube 5 at the position between the carrier gas tube 2 and the shunt tube 4. A sealing lip is embedded in the embedding groove, and the sealing lip is in fit with the inner wall of the sampling tube 1.

[0091] Specifically, the sealing lip installed in the embedding groove on the outer wall of the inner liner tube 5 at the position between the carrier gas tube 2 and the shunt tube 4 is in fit with the inner wall of the sampling tube 1. During the flow of the carrier gas and the vaporization and transmission of the sample, the sealing lip plays a role in sealing and buffering, preventing the leakage or turbulence of the carrier gas and the sample at this part, and ensuring the stability of the sampling process;

[0092] enhance the sealing and fluid stability of a specific area inside the sampling tube 1, reduce the abnormal flow of the carrier gas and the sample caused by sealing problems, are beneficial to improving the precision and repeatability of sampling, enable the liquor sample to enter the chromatographic column 400 for separation and analysis more stably and accurately, and thus improve the reliability and accuracy of the data during the whole liquor identification process.

[0093] Refer to Figure 3 and Figure 5 , a limiting member 40 is arranged on the bottom surface of the connecting seat 7, and a connecting groove recessed inward is arranged at the port at the top end of the inner liner tube 5. The limiting member 40 is embedded in the connecting groove formed on the inner liner tube 5;

[0094] Among them, the limiting member 40 includes a supporting portion and a limiting portion. The supporting portion is of a long cylindrical structure. One end thereof is connected to the bottom surface of the connecting seat 7, and the other end extends along the axial direction of the sampling tube 1 and is connected to the limiting portion. The limiting portion is of an annular structure, and a plurality of convex teeth distributed along its circumferential direction are provided on the inner sidewall of its inner circle. A groove for the convex teeth to be engaged with is provided on the inner wall of the connecting groove.

[0095] Specifically,

[0096] The limiting member 40 on the bottom surface of the connecting seat 7 cooperates with the connecting groove at the top end port of the inner liner tube 5. The supporting portion of the limiting member 40 plays a connecting and supporting role. The convex teeth of the limiting portion are engaged with the grooves on the inner wall of the connecting groove, restricting the vertical displacement and axial rotation of the inner liner tube 5 in the sampling tube 1, and ensuring the stable position of the inner liner tube 5 during the sampling process.

[0097] The precise limitation and fixation of the inner liner tube 5 are realized, preventing the inner liner tube 5 from displacing or shaking due to factors such as pressure and vibration during the sampling process, ensuring the stability of the sample vaporization and transmission channels, improving the accuracy and repeatability of sampling, being beneficial to obtaining more stable and reliable chromatographic analysis data, and providing more powerful technical support for the work of liquor identification.

Claims

1. A method for identifying Maotai-flavor liquor, characterized in that: The following steps are involved: Step 1: using a solid phase microextractor (700) to enrich the volatile components in the Maotai-flavor liquor sample, and injecting the extracted components into the injection port of the chromatograph body (200) through the injector (100) for desorption. During the injection process, the electric heating plate (500) and the fan (600) can provide heat for the injection of the injector (100); Step 2: Separating the desorbed volatile components through a chromatographic column (400) provided in the chromatograph body (200); when the separated components flow out of the chromatographic column (400) and enter the detector (300), the detector (300) generates an electrical signal which is processed and recorded by the data acquisition of the chromatograph body (200) to form a chromatogram, thereby obtaining a total ion current chromatogram and mass spectrum data; Step 3: Process the data to screen out characteristic volatile component markers and their relative content ratios; establish an identification model, input the characteristic marker data into the identification model based on the characteristic markers and their relative content data, and determine the authenticity and quality grade of the sample to be tested; Wherein, the sample injector (100) comprises: An injection tube (1) is mounted on the upper part of the chromatograph body (200), and has a vaporization cavity (11) and an injection cavity (12) that are interconnected. An output tube (13) extending downward is provided on the bottom wall of the injection cavity (12). The white wine sample injected into the vaporization cavity (11) is vaporized by heat from the electric heating plate (500) and introduced into the chromatographic column (400) through the output tube (13); The upper side wall of the sample injection tube (1) is provided with a carrier gas tube (2) and a blowing tube (3) which are in communication with the vaporization cavity (11), and the lower side wall is provided with a shunt tube (4) which is in communication with the vaporization cavity (11); A rotating shaft (14) is arranged on the side wall of the sample injection tube (1) in a vertically rotatable manner, and a rotating disk (15) is connected to the outer wall of the rotating shaft (14); A plurality of positioning seats (16) are evenly distributed along the circumferential outer wall of the rotating disk (15); a positioning groove (25) is provided on the positioning seat (16) along the central axis thereof; a capillary body (24) is detachably mounted inside the positioning groove (25); the inner diameters of the capillary bodies (24) are different; when the rotating disk (15) rotates, the plurality of positioning seats (16) can alternately enter the injection cavity (12) so that the positioning groove (25) and the vaporization cavity (11) are sealed and communicated.

2. The method for identifying a Maotai-flavor liquor according to claim 1, characterized in that: A diameter-reducing groove (26) expanding in the radial direction is arranged on the inner wall of the positioning groove (25), and a flexible positioning member for fixing the capillary body (24) is arranged inside the diameter-reducing groove (26). The flexible positioning member comprises: A flexible sleeve (34) is integrally sleeved on the outside of the capillary body (24), the outer wall of which is fixed to the inner wall of the diameter-changing groove (26), and a sealed filling cavity is opened inside the flexible sleeve (34); A thermoplastic filler (37) is filled in the filling cavity inside the flexible sleeve (34) without any gaps, and the hardness of the thermoplastic filler (37) increases when heated and decreases after cooling; The flexible heat absorbing plate (38) is installed inside the flexible sleeve (34) and can generate flexible deformation when the flexible sleeve (34) is squeezed.

3. The method for identifying a Maotai-flavor liquor according to claim 2, characterized in that: A sliding groove (27) is also provided inside the positioning seat (16); a movable opening is provided on the side wall of the diameter-changing groove (26) along the radial direction of the positioning seat (16); the diameter-changing groove (26) and the sliding groove (27) are connected via the movable opening; a resisting rod (35) is slidably provided inside the movable opening; an extrusion plate (36) is provided at one end of the resisting rod (35) extending into the inside of the diameter-changing groove (26); A sliding sleeve (29) is slidably mounted inside the sliding groove (27), a conical sleeve (31) is connected to the bottom surface of the sliding sleeve (29), a return spring (33) is connected to the bottom surface of the conical sleeve (31), the bottom end of the return spring (33) is connected to the inner bottom wall of the sliding groove (27), one end of the abutment rod (35) extending into the sliding groove (27) abuts against the inner wall of the conical sleeve (31), when the sliding sleeve (29) drives the conical sleeve (31) to move axially upward along the positioning seat (16), the plurality of abutment rods (35) can drive the extrusion plate (36) to synchronously close to the central axis of the positioning seat (16).

4. The method for identifying a Maotai-flavor liquor according to claim 3, characterized in that: A radially extending clearance groove (39) is provided on the side wall of the positioning seat (16), the clearance groove (39) being connected to the sliding groove (27), a transmission rod (32) being slidably arranged inside the clearance groove (39), one end of the transmission rod (32) being connected to the outer side wall of the sliding sleeve (29), and the other end extending to the outside of the positioning seat (16); An inclined plate (23) is provided on the upper surface of the output tube (13), and when the positioning seat (16) rotates to the inside of the injection cavity (12), the transmission rod (32) slides along the surface of the inclined plate (23).

5. The method for identifying a Maotai-flavor liquor according to claim 1, characterized in that: The top surface of the sample injection tube (1) is provided with a cover plate (17), the cover plate (17) covers the top surface of the turntable (15), and the bottom surface of the cover plate (17) is in contact with the top surface of the turntable (15).

6. The method for identifying a Maotai-flavor liquor according to claim 1, characterized in that: It also includes a locking assembly arranged on the sample injection tube (1) for locking the rotation of the turntable (15), the locking assembly comprising: A horizontal plate (19) vertically extends along the radial direction of the sample injection tube (1), and one end of the horizontal plate (19) extending above the rotating disk (15) is rotatably connected to a rotating plate (20); A pin rod (21) is hinged at one end of the rotating plate (20), and a plurality of positioning holes (18) for inserting the pin rod (21) are provided on the top surface of the rotating disk (15), and the position of each positioning hole (18) corresponds to the positioning seat (16); A push spring (22) is connected to the bottom surface of one end of the pin rod (21) away from the rotating plate (20), and the other end of the push spring (22) is fixed to the top surface of the horizontal plate (19).

7. The method for identifying a Maotai-flavor liquor according to claim 3, characterized in that: The interior of the injection tube (1) is provided with an inner liner tube (5) which can slide vertically along the inner wall of the vaporization cavity (11); a flow channel (6) is provided inside the inner liner tube (5); an upper port of the flow channel (6) is connected to the vaporization cavity (11); a lower port of the flow channel (6) is connected to the injection cavity (12); a connecting seat (7) is screwed into the port at the top end of the injection tube (1); a receiving groove (8) connected to the vaporization cavity (11) is provided through the connecting seat (7); a septum (9) is sleeved inside the receiving groove (8); a sealing cover (10) is screwed outside the port at the top end of the injection tube (1); an inner wall of the sealing cover (10) is pressed against the top surface of the septum (9); an injection hole connected to the septum (9) is provided at the center of the sealing cover (10).

8. The method for identifying a Maotai-flavor liquor according to claim 7, characterized in that: An annular groove (28) communicating with the sliding groove (27) is provided on the top surface of the positioning seat (16); one end of the sliding sleeve (29) extending into the annular groove (28) is connected to a rubber sealing ring (30); and a sealing groove for the rubber sealing ring (30) to extend into is provided on the end surface of the bottom end of the liner tube (5).

9. The method for identifying a Maotai-flavor liquor according to claim 7, characterized in that: The inner liner tube (5) is provided with an annular embedding groove on its outer wall between the carrier gas tube (2) and the diversion tube (4), and a sealing lip is embedded in the embedding groove, and the sealing lip fits with the inner wall of the sample injection tube (1).

10. The method for identifying a Maotai-flavor liquor according to claim 7, characterized in that: A limiting member (40) is provided on the bottom surface of the connecting seat (7), and an inwardly recessed connecting groove is provided at the port at the top end of the inner liner tube (5), and the limiting member (40) is embedded in the connecting groove provided on the inner liner tube (5); The limiting member (40) comprises a supporting portion and a limiting portion, wherein the supporting portion is a long cylindrical structure, one end of which is connected to the bottom surface of the connecting seat (7), and the other end of which extends axially along the injection tube (1) and is connected to the limiting portion, and the limiting portion is a ring structure, and the inner ring side wall thereof is provided with a plurality of convex teeth distributed along its circumference, and a groove for the convex teeth to be inserted is provided on the inner wall of the connecting groove.

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