Amino acid sample containing device for crushing, sample preparation and integrated detection

Abstract

The application relates to the technical field of amino acid detection equipment, in particular to a sample smashing and sample preparation integrated detection device for amino acid-containing samples, which comprises a shell, a smashing bin is fixedly installed at the top of the inner side of the shell, a cutter is rotationally connected to the lower end of the smashing bin, a No.1 motor is fixedly connected in the shell, the output shaft of the No.1 motor is coaxially connected with the cutter, an air inlet for introducing inert gas is arranged on the lower side of the smashing bin, a material conveying pipe is arranged on the outer wall of the smashing bin, and the material conveying pipe is connected with the smashing bin through a communication port. The smashing, screening, moisture detection and packaging links are integrated in situ, compared with the traditional segmented sample preparation process, the sample transfer steps of the amino acid sample between different devices are greatly reduced, the risks of sample residue loss, oxidative degradation and secondary moisture absorption are reduced from the process source, and a higher-stability standardized pretreatment sample is provided for amino acid quantitative analysis.

Description

Technical Field

[0001] This invention relates to the field of amino acid detection equipment technology, specifically to an integrated detection device for pulverizing and preparing amino acid-containing samples. Background Technology

[0002] Current mainstream amino acid sample processing procedures typically consist of discrete steps such as mechanical crushing, sieving and mixing, and sample preparation and packaging, connecting to subsequent hydrolysis, derivatization, and detection stages. In existing technologies, the above pretreatment processes generally adopt a segmented working mode, where the crusher, vibrating screen, and sample preparation workbench are completely independent in space, and the transfer of samples between different workstations requires manual operation or discrete containers. Although this segmented structural layout can meet the requirements of single-step experiments, in actual large-scale detection and production, since crushing and sieving are open or semi-open mechanical processing steps, samples are easily exposed to the external environment during frequent opening, transfer, and loading. Amino acid samples are highly hygroscopic and heat-sensitive; moisture and clumping not only lead to clogging of sieve pores and uneven mixing, but also cause significant container wall adhesion during transfer, resulting in serious material loss and distortion of component ratios. Furthermore, under segmented processes, the localized high temperatures and ambient humidity generated during crushing cannot be monitored in real time or physically isolated, leading to irreversible oxidation and deterioration of materials during cross-station transfer. This is especially problematic for subsequent processes involving acid hydrolysis reactions. If the physical properties of the materials in the preceding sample preparation stages are inconsistent, it will directly result in incomplete hydrolysis, extending the single testing cycle and reducing data reproducibility. This makes it unsuitable for the high efficiency and continuity requirements of automated testing lines.

[0003] To address the aforementioned issues, existing technologies offer several solutions, such as configuring automated tracked robotic arms to simulate manual actions in connecting crushing and sample preparation equipment. However, this only achieves a superficial transfer and cannot eliminate material oxidation and transfer losses caused by physical gaps between equipment. Furthermore, the complex connecting mechanisms increase the system's failure rate. Another example is the development of partial crushing and screening machines, which integrate the physical crushing process, but a physical disconnect still exists between them and the subsequent packaging stage, requiring manual intervention for sample transfer. This fails to fundamentally solve the problems of low process integration and poor connection stability.

[0004] Therefore, there is an urgent need for an integrated pretreatment device for amino acid sample crushing and preparation, which can integrate the entire process from mechanical crushing of the original sample to final sealing and preparation on a single mechanical platform. This would completely isolate the environmental interference and transfer loss caused by segmented processes, and achieve high efficiency and consistency of physical properties in the pretreatment process for amino acid detection. Summary of the Invention

[0005] The purpose of this invention is to provide an integrated detection device for amino acid sample crushing and preparation. This device achieves in-situ integration of the entire process from raw sample crushing to final sealed preparation through a single mechanical platform, eliminating the physical barriers and manual intervention issues between traditional segmented processes.

[0006] To achieve the above objectives, the present invention provides the following technical solution: An integrated sample preparation and testing device for amino acid-containing samples includes a housing. A grinding chamber is fixedly installed on the top inner side of the housing. A cutter is rotatably connected to the lower end of the grinding chamber. A primary motor is fixedly connected inside the housing, and the output shaft of the primary motor is coaxially connected to the cutter. An air inlet is provided on the lower side of the grinding chamber. A conveying pipe is provided on the outer wall of the grinding chamber. The conveying pipe is connected to the grinding chamber through a connecting port located on the upper side of the grinding chamber and the conveying pipe. A ventilation opening is provided on the upper side of the side wall of the conveying pipe. A discharge port is provided at the lower end of the conveying pipe. Multiple layers of screens are provided inside the conveying pipe. A rotating... The transfer indexing plate is rotatably connected to a second motor on the lower side of the housing. The transfer indexing plate is coaxially fixedly connected to the upper end of the output end of the second motor. At least four mounting holes are arranged in a rectangular array on the circumferential edge of the transfer indexing plate. A sample bottle is embedded in each mounting hole. The transfer indexing plate rotates and passes sequentially through a receiving station located below the feed pipe and a sealing station arranged along the rotation direction. A sealing assembly is provided above the sealing station to seal the upper end of the sample bottle. A pressure relief valve is provided on the lower side wall of the housing. The opening pressure of the pressure relief valve is set to 1.05 bar to 1.2 bar.

[0007] By integrating a crushing chamber and a conveying pipe within the housing, and using a cutter driven by a No. 1 motor, in-situ mechanical crushing of samples is achieved. Inert gas is introduced through an air inlet located on the lower side of the crushing chamber, which not only provides anti-oxidation protection for the crushing process but also removes the heat generated during sample crushing, preventing the sample from overheating and degrading. At the same time, pneumatic power drives the crushed sample powder to enter the conveying pipe through the connecting port on the upper side, achieving seamless pneumatic transport across workstations and effectively avoiding material loss and environmental pollution caused by traditional mechanical transport.

[0008] Furthermore, multiple layers of sieves are installed inside the feed pipe, allowing the samples to be graded and screened simultaneously during pneumatic transport, ensuring a high degree of consistency in the particle size of samples entering downstream processes. At the same time, the rotation of the transfer indexing plate driven by the No. 2 motor drives the circumferentially arranged sample bottles to pass sequentially through the receiving station and the sealing station. Together with the sealing assembly, this achieves continuous operation from material collection to automated packaging, significantly improving the efficiency of sample pretreatment.

[0009] Furthermore, by installing a pressure relief valve on the side wall of the casing and setting the opening pressure to 1.05 bar to 1.2 bar, a slightly positive pressure inert gas environment is continuously maintained inside the entire device under the action of the air inlet. This positive pressure environment not only provides a stable power source for pneumatic material conveying but also completely isolates the sample from moisture and oxygen in the external air. This fundamentally solves the problem of moisture absorption, clumping, and oxidative deterioration that easily occur in amino acid samples during crushing and sample preparation, ensuring the biochemical stability of the pretreated samples and laying the foundation for subsequent high-precision detection.

[0010] Preferably, the cutter includes a cutter bar and a cutter head. The cutter head is located at the upper end of the cutter bar and includes two sets of cutter heads arranged vertically. The lower end of the cutter bar is coaxially connected to a first motor. A gas channel with closed upper and lower ends is coaxially opened inside the cutter bar. Multiple first through holes and multiple second through holes communicating with the gas channels are opened on the side wall of the cutter bar. A rotating air intake ring is fixedly installed inside the housing. The rotating air intake ring is rotatably connected to the cutter bar. The air intake port is located on the outer side wall of the rotating air intake ring and communicates with multiple first through holes through the rotating air intake ring. Multiple second through holes are located between the two sets of cutter heads and the second through holes are inclined downwards.

[0011] By incorporating a cutter bar and two sets of cutter heads on the cutter, and creating a gas channel inside the cutter bar, a dynamic rotating air intake system is constructed in conjunction with a rotating air intake ring within the housing. During operation, inert gas enters the rotating air intake ring through the air inlet, is introduced into the gas channel inside the cutter bar via the first through-hole, and is finally ejected from the second through-hole located between the two sets of cutter heads. This hollow axial air intake design ensures a stable and continuous supply of inert gas to the grinding chamber during high-speed rotation of the cutter.

[0012] Furthermore, the second through-hole is positioned between the two sets of cutter heads and is arranged at an angle downwards, allowing the ejected high-pressure airflow to directly act on the core crushing area between the two sets of cutter heads. On the one hand, the downward-sloping airflow generates a strong turbulence effect, assisting the cutter heads in performing multi-dimensional shearing and collision on the material, significantly improving crushing efficiency; on the other hand, the ejected airflow can promptly clean the adhering substances on the surface of the cutter heads and cutter bars, effectively preventing the agglomeration of amino acid-containing samples due to heat generated during crushing or adsorption forces.

[0013] Furthermore, the airflow between the two sets of cutters creates localized aerodynamic lift at the bottom of the crushing chamber. Combined with the centrifugal force generated by the rotation of the cutters, this lifts the pulverized micro-powder to the upper part of the crushing chamber. Utilizing the mechanical structure of the cutter itself as an airflow distributor, the power crushing and pneumatic lifting are coupled, providing a stable and continuous initial power for the subsequent high-level transfer of materials through the connecting port to the conveying pipe. This reduces the system's dependence on an additional power source and enhances the overall structural integration of the device.

[0014] Preferably, the conveying pipe includes a horizontal section and a vertical section. The horizontal section is fixedly connected to the top of the inner wall of the shell, and the vertical section is attached to the side wall of the crushing chamber. Multiple screens are disposed in the vertical section, and multiple filter cloths are disposed in the horizontal section. The filter cloths near the crushing chamber are inclined, and the working surface of the filter cloths faces the lower side of the crushing chamber. The vent is disposed at the end of the horizontal section away from the crushing chamber.

[0015] By setting the conveying pipe to an L-shaped structure including a horizontal section and a vertical section, and fixing the horizontal section to the top of the inner wall of the shell, while the vertical section is attached to the side wall of the crushing chamber, the powder-laden airflow raised by the crushing chamber first enters the horizontal section through the connecting port during operation. The extended space of the horizontal section provides a primary buffer for the airflow, effectively suppressing the turbulent fluctuations caused by the high-speed airflow and ensuring the stability of the subsequent screening process.

[0016] Furthermore, multiple filter cloths are installed within the horizontal section, with the filter cloths closest to the pulverizing chamber arranged at an angle and their working surfaces facing downwards towards the pulverizing chamber. When the airflow carrying fine powder flows at high speed along the horizontal section, the inertia of the fine powder causes it to collide with the working surface of the angled filter cloth. This inertial collision separation mechanism allows fine powders with greater kinetic energy to lose momentum after the collision and fall back towards the pulverizing chamber under the influence of gravity, thus achieving preliminary separation of the gas and solid phases. At the same time, the angled arrangement expands the effective air-receiving area of ​​the filter cloth, reduces the carrying capacity of local wind pressure on overflowing fine powder, and plays a significant role in interception and capture.

[0017] Furthermore, by placing the vent at the end of the horizontal section away from the grinding chamber, the airflow is forced to pass through the entire horizontal section and multiple filter cloth barriers before it can be discharged. This extends the retention path of the micro powder in the feed pipe, effectively preventing material loss caused by the escape of amino acid samples from the vent with the airflow. At the same time, it also provides a good air pressure buffering effect. Combined with the multi-layer screen inside the vertical section, it realizes a stepped processing logic of inertial capture followed by gravity classification, ensuring that the device can achieve high-precision sample preparation with almost zero loss while maintaining a positive pressure environment of 1.05 bar to 1.2 bar.

[0018] Preferably, the plurality of screens are arranged in parallel, and the mesh size of the plurality of screens increases from top to bottom. The vertical part and the side wall of the crushing chamber are provided with a plurality of return ports equal to the number of screens. The plurality of screens are all arranged at an inclination, and the lower end of the screens extends into the return ports.

[0019] By arranging multiple layers of screens in parallel within the vertical section of the feed pipe, with the mesh size increasing from top to bottom, the material initially intercepted by the filter cloth in the horizontal section enters the vertical section during actual operation. It then passes through the multiple layers of screens using gravity and airflow pressure difference, achieving a step-by-step screening of amino acid sample particles from coarse to fine. The increasing pore size arrangement effectively avoids direct impact and clogging of the bottom fine-mesh screen by a single coarse particle, significantly improving screening efficiency and screen lifespan.

[0020] Furthermore, by opening multiple return ports in the vertical section and on the side wall of the crushing chamber, and coordinating with inclined screens, the lower end of each screen extends into the corresponding return port, thus forming a closed-loop circuit of screening, diversion, and powder return. Utilizing the inclined angle of the screens, large particles that fail to pass through the screen are guided to the return port by gravity and automatically slide back into the crushing chamber. In addition, the horizontal filter cloth is responsible for intercepting and returning high-speed fine powder, while the inclined screens in the vertical section are responsible for accurately guiding substandard particles back. Together, they ensure the dynamic circulation of materials within the system until all samples reach the preset sample fineness.

[0021] Furthermore, this gravity-guided material return design eliminates the need for additional mechanical conveying power. It utilizes the material's own gravity and the pneumatic pressure difference within the crushing chamber to achieve automatic cyclic crushing. Compared to the cumbersome operation of manually collecting coarse materials and feeding them a second time in traditional discrete equipment, this structure achieves in-situ integration of crushing and grading. This not only significantly reduces the residual loss of amino acid samples during the reciprocating cycle but also ensures that the final micro-powder entering the sample vial has extremely high quality consistency, providing a standardized and non-destructive sample basis for subsequent precise acid hydrolysis and quantitative analysis.

[0022] Preferably, a moisture detection sensor is fixedly installed on the side wall of the vertical part, the moisture detection sensor is located between the bottom screen and the discharge port, and the moisture detection sensor extends into the interior of the conveying pipe.

[0023] By fixing a moisture detection sensor to the side wall of the vertical part of the conveying pipe and precisely arranging the sensor on the material drop path between the bottom screen and the discharge port, a moisture content detection system for the pulverized powder is formed. The design of extending the moisture detection sensor into the inside of the conveying pipe ensures that the moisture monitoring head can directly and fully contact or sense the powder flow in a suspended or free-falling state within the detection area, thereby realizing in-situ, real-time and high-precision dynamic acquisition of the sample moisture content.

[0024] Furthermore, by positioning the moisture detection sensor after the bottommost sieve, it ensures that all monitored objects are final products that have passed full-stage screening and meet the preset particle size standards. Since amino acid samples undergo simultaneous dehydration by the drying nitrogen flow during the preceding pneumatic transport process, setting a monitoring point at this specific station provides the most accurate reflection of the material's moisture content before it enters the sample vial. This provides crucial quantitative parameters for the subsequent hydrolysis reaction, effectively avoiding incomplete derivatization reactions or quantitative calculation errors caused by fluctuations in sample moisture content, thus improving data reproducibility from the source of detection.

[0025] Furthermore, online monitoring replaces traditional discrete sampling and detection, avoiding the risk of secondary moisture absorption when samples leave the device for moisture determination. Combined with the overall positive pressure environment of the device, the moisture detection sensor not only plays a monitoring role but also serves as a criterion for process feedback: when the monitored value does not meet the preset drying standard, the environment can be optimized by adjusting the nitrogen flow rate at the air inlet or the pulverization time. This achieves a quality closed loop from mechanical pulverization to standardized sample preparation, fully meeting the stringent requirements of research institutions such as the Academy of Agricultural Sciences for high-standard amino acid pretreatment.

[0026] Preferably, the pressure relief valve is located on the side away from the vent, and a nitrogen concentration detection sensor is provided on the side wall of the housing where the pressure relief valve is located. The pressure relief valve and the nitrogen concentration detection sensor are respectively located on the front and rear sides.

[0027] By installing a pressure relief valve on the side wall of the shell and arranging it away from the vent of the feed pipe, and integrating a nitrogen concentration detection sensor on the side wall, inert gas is continuously introduced into the air inlet during device operation. The long-distance diagonal distribution of the pressure relief valve and the vent in space forces the nitrogen gas flow to traverse the entire internal space of the shell before it can be discharged. The long-path airflow organization effectively eliminates dead zones in the flow inside the shell, ensuring that residual oxygen-containing gas can be completely replaced, thus providing a dead-zone-free inert protective barrier for the crushing and transport of amino acid samples.

[0028] Furthermore, nitrogen concentration sensors and pressure relief valves are respectively installed on the front and rear sides of the sidewall, enabling precise sampling of environmental indicators at the exhaust end. Since the area near the pressure relief valve is the dynamic equilibrium point of pressure release within the casing, placing sensors in this area can most accurately reflect the overall nitrogen coverage purity of the system. When the sensor detects that the nitrogen concentration has not reached the preset safety threshold, the system can automatically adjust the intake flow rate to ensure that the device maintains a high-purity, low-oxygen environment under positive pressure conditions of 1.05 bar to 1.2 bar, fundamentally eliminating the risk of oxidative degradation of amino acid components in complex pretreatment processes.

[0029] Furthermore, the separate placement of the pressure relief valve and sensor also ensures both operational safety and ease of maintenance. The pressure relief valve, as a physical pressure relief protection device, can respond in real time to pressure fluctuations within the housing, preventing excessive pressure from causing structural damage to the multi-layered screen and sealed outer shell. Meanwhile, the concentration sensor, working in conjunction with the valve, provides a logical-level safety interlock. The monitoring array formed by these two components not only guarantees the physical stability of the pretreatment process but also ensures the consistency of the biochemical environment during long-term continuous operation, fully demonstrating the invention's pursuit of ultimate environmental control in the field of fine chemical pretreatment.

[0030] Preferably, the sealing assembly includes a No. 3 motor, a guide rail, a lead screw, a nut, and a pressure plate. The No. 3 motor is fixedly connected to the housing, and the upper end of the output end of the No. 3 motor is fixedly connected to the lead screw. The nut is threadedly connected to the lead screw. The guide rail is fixedly connected inside the housing, and the nut is slidably connected to the guide rail. The free direction of the nut and the guide rail is vertical. The pressure plate is fixedly connected to the nut and is located directly above the sealing position. Two clamping plates are provided on the guide rail, and a sealing cap is held between the two clamping plates. The sealing cap is coaxially arranged on the sealing position.

[0031] By installing a sealing assembly consisting of a No. 3 motor, guide rail, lead screw, nut, and pressure plate above the sealing station, the No. 3 motor drives the lead screw to rotate during operation. The screw and nut's threaded transmission pair precisely converts the motor's rotational motion into the nut's vertical linear motion along the guide rail. Because the guide rail strictly restricts the nut's freedom in the horizontal direction, it ensures that the pressure plate maintains extremely high vertical alignment accuracy during lifting and lowering, thus enabling a smooth and uniform sealing operation on the sample bottle located directly below the sealing station.

[0032] Furthermore, two clamping plates are installed on the guide rail to hold the cap and keep the cap coaxial with the sealing station. This pre-positioning design ensures that the cap can achieve precise physical alignment with the sample bottle mouth rotated to the sealing station during the descent of the pressure plate. Utilizing the high speed ratio and strong self-locking characteristics of the screw drive, the pressure plate can provide stable and controllable downward pressure to force the cap to be pressed or screwed onto the sample bottle. This effectively solves the problem of uneven force or incomplete sealing that may occur during manual sealing, ensuring that each amino acid sample bottle meets the airtight sealing standard before leaving the device.

[0033] Furthermore, when the No. 2 motor drives the transfer indexing plate to accurately deliver the filled sample bottle to the sealing station, the sealing assembly immediately performs vertical compression. The entire process is carried out in a positive pressure inertial environment of 1.05 bar to 1.2 bar inside the shell. This processing mode minimizes the time window during which the pulverized amino acid sample is exposed to air. Combined with the high repeatability and positioning accuracy of the screw drive, it not only ensures the consistency of batch sample preparation but also locks in the biochemical activity of the sample from a physical and mechanical perspective, realizing a fully automated closed loop from pulverization to finished product packaging.

[0034] Preferably, the inner walls of the crushing chamber and the vertical section are coated with polytetrafluoroethylene, and the blade rod and blade head are made of stainless steel.

[0035] By applying a polytetrafluoroethylene (PTFE) coating to the inner walls of both the grinding chamber and the vertical section of the conveying pipe, the extremely low surface energy, excellent self-lubricating properties, and strong hydrophobic and oleophobic characteristics of PTFE effectively reduce the van der Waals forces and electrostatic adsorption forces between the amino acid-containing sample powder and the wall surface. In practical applications, even when the ground powder is damp or in a highly adherent state, the accumulation and adhesion of the sample on the chamber or pipe walls is reduced, thus ensuring the flow polarity of the material during pneumatic conveying and gravity reflux, significantly improving the final sample recovery rate.

[0036] Furthermore, both the blade shank and the blade head of the cutter are made of stainless steel, ensuring that the core pulverizing components possess extremely high mechanical strength, wear resistance, and excellent chemical stability. The stainless steel material can withstand the enormous centrifugal force and material impact force generated when the cutter rotates at high speed, preventing the blade from cracking or deforming when pulverizing hard, blocky samples. At the same time, the smooth and dense surface of the stainless steel, combined with the polytetrafluoroethylene coating on the inner wall, ensures both the thoroughness of physical pulverization and minimizes cross-contamination of sample components at the contact level, ensuring the purity of samples prepared between batches.

[0037] Preferably, the housing is equipped with an electronic control module, and the air inlet is equipped with a pulse valve. The pulse valve and the second motor are both electrically connected to the electronic control module.

[0038] By installing a pulse valve at the air inlet and electrically connecting it to the No. 2 motor driving the transfer indexing plate, during the actual working cycle, whenever the No. 2 motor drives the transfer indexing plate to complete a station switch, such as the instant the material receiving station moves to the sealing station, the pulse valve opens instantaneously in response to the electrical control signal, injecting a pulsed nitrogen gas flow with extremely high velocity into the crushing chamber and subsequent conveying pipeline. Utilizing the instantaneous high-pressure shock wave generated by the pulsed gas flow, a high-frequency "pneumatic brushing" is performed on the inner walls of the entire pipeline and the surface of the screen, ensuring that while the previous sample is being sealed, any residual micro-powder inside the device is thoroughly cleaned and forcibly fed into the current sample bottle at the receiving port.

[0039] Furthermore, the instantaneous mechanical force provided by the pulse valve solves the problem of amino acid-containing samples sticking to the sample wall due to their extremely fine particles, significantly reducing the risk of cross-contamination between different batches of samples. This precise timing control achieved through simple electrical linkage not only simplifies the hardware redundancy of the control system but also ensures the high self-cleaning ability and material consistency of the pretreatment unit during long-term, high-volume operation from a process logic perspective.

[0040] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. This invention integrates the crushing, sieving, moisture detection and packaging processes in situ, which significantly reduces the transfer steps of amino acid samples between different devices compared to the traditional segmented sample preparation process. It reduces the risk of sample residue loss, oxidative degradation and secondary moisture absorption from the source of the process, and provides a more stable standardized pretreatment sample for amino acid quantitative analysis.

[0041] 2. By integrating the inertial trapping structure and the multi-stage gravity screening structure into the L-shaped conveying pipe, a step-by-step processing logic is formed, which first separates the gas and solid and then classifies the particle size step by step. Combined with the gravity-guided automatic return design, the in-situ dynamic circulation of crushing and screening is realized, eliminating the need for manual secondary material replenishment. This not only improves the sample preparation efficiency but also ensures the consistency of sample fineness, while achieving high-precision sample preparation with almost zero loss.

[0042] 3. By creating a continuous positive pressure inert environment inside the device housing, and with the diagonally arranged pressure relief valves and nitrogen concentration sensors, the dead zones for oxygen flow inside the housing are completely eliminated. This provides stable anti-oxidation protection for amino acid samples and ensures the pressure safety of the entire machine, meeting the requirements of research institutions for high-standard amino acid pretreatment. Attached Figure Description

[0043] Figure 1 This is a schematic diagram of the integrated sample crushing and preparation detection device for amino acids according to the present invention; Figure 2 This is a schematic diagram of the internal structure of the integrated sample crushing and preparation detection device containing amino acids according to the present invention; Figure 3 for Figure 2 Full sectional view at point AA; Figure 4 for Figure 3 A magnified view of a section at point B in the middle; Figure 5 This is a schematic diagram of the sealing component in this invention; Figure 6 This is a schematic diagram of the transfer indexing plate in this invention.

[0044] In the diagram: 1. Shell; 2. Crushing chamber; 3. Cutter; 301. Cutter bar; 3011. Gas passage; 3012. Through hole No. 1; 3013. Through hole No. 2; 302. Cutter head; 4. Motor No. 1; 5. Feed pipe; 501. Connecting port; 502. Ventilation port; 503. Discharge port; 504. Return port; 6. Screen; 7. Transfer indexing plate; 701. Mounting hole; 702. Receiving station; 703. Sealing station; 8. Motor No. 2; 9. Sample bottle; 10. Pressure relief valve; 11. Rotary air inlet ring; 1101. Air inlet; 12. Filter cloth; 13. Moisture detection sensor; 14. Nitrogen concentration detection sensor; 15. Motor No. 3; 16. Guide rail; 17. Lead screw; 18. Nut; 19. Pressure plate; 20. Clamping plate; 21. Cap; 22. Pulse valve. Detailed Implementation

[0045] Please see Figures 1 to 6 This invention provides an integrated detection device for pulverizing and preparing amino acid-containing samples, the technical solution of which is as follows: Please refer to the integrated sample preparation and testing device for amino acid-containing samples. Figure 1 , Figure 2 and Figure 3 The device includes a housing 1. A crushing chamber 2 is fixedly installed on the top inner side of the housing 1. A cutter 3 is rotatably connected to the lower end of the crushing chamber 2. A first motor 4 is fixedly connected inside the housing 1. The output shaft of the first motor 4 is coaxially connected to the cutter 3. An air inlet 1101 is provided on the lower side of the crushing chamber 2. A conveying pipe 5 is provided on the outer wall of the crushing chamber 2. The conveying pipe 5 is connected to the crushing chamber 2 through a connecting port 501, which is located on the upper side of the crushing chamber 2 and the conveying pipe 5. A vent 502 is provided on the upper side of the side wall of the conveying pipe 5. A discharge port 503 is provided at the lower end of the conveying pipe 5. Three layers of screens 6 are provided inside the conveying pipe 5. A transfer indexing plate 7 is provided below the conveying pipe 5. A second motor 8 is provided at the lower end of the transfer indexing plate 7. The second motor 8 is fixedly connected to the housing 1. The output shaft of the transfer indexing plate 7 and the second motor 8 are connected to each other. The upper end of the sample bottle 9 is coaxially fixedly connected. At least four mounting holes 701 are arranged in a rectangular array at the circumferential edge of the transfer indexing plate 7. Each mounting hole 701 is embedded with a sample bottle 9. The transfer indexing plate 7 rotates and passes sequentially through the receiving station 702 located below the conveying pipe 5 and the sealing station 703 arranged along the rotation direction. A sealing assembly is provided above the sealing station 703. The sealing assembly is used to seal the upper end of the sample bottle 9. A pressure relief valve 10 is provided on the lower side wall of the housing 1. The opening pressure of the pressure relief valve 10 is set to 1.05 bar to 1.2 bar. The pressure relief valve 10 is located on the side away from the vent 502. A nitrogen concentration detection sensor 14 is provided on the side wall of the housing 1 where the pressure relief valve 10 is located. The pressure relief valve 10 and the nitrogen concentration detection sensor 14 are respectively located on the front and rear sides.

[0046] Please see Figure 3 and Figure 4 The cutter 3 includes a cutter bar 301 and a cutter head 302, both made of stainless steel. The cutter head 302 is located at the upper end of the cutter bar 301 and includes two sets arranged vertically. The lower end of the cutter bar 301 is coaxially connected to the first motor 4. A gas channel 3011, closed at both ends, is coaxially opened inside the cutter bar 301. Multiple first through holes 3012 and multiple second through holes 3013 communicating with the gas channel 3011 are opened on the side wall of the cutter bar 301. A rotating air intake ring 11 is fixedly installed inside the housing 1. The air intake ring 11 is rotatably connected to the cutter bar 301. The air intake port 1101 is located on the outer wall of the rotating air intake ring 11. An electronic control module is provided inside the housing 1. A pulse valve 22 is provided on the air intake port 1101. The first motor 4, the second motor 8, the third motor 15, the pulse valve 22, the moisture detection sensor 13, and the nitrogen sensor are all electrically connected to the electronic control module. The air intake port 1101 is connected to multiple first through holes 3012 through the rotating air intake ring 11. Multiple second through holes 3013 are located between the two sets of cutter heads 302, and the second through holes 3013 are inclined downwards.

[0047] For further details, please refer to Figure 3 The conveying pipe 5 includes a horizontal section and a vertical section. The horizontal section is fixedly connected to the top of the inner wall of the housing 1, and the vertical section is attached to the side wall of the crushing chamber 2. The inner walls of both the crushing chamber 2 and the vertical section are coated with polytetrafluoroethylene. Multiple screens 6 are located in the vertical section, and four layers of filter cloth 12 are located in the horizontal section. The filter cloth 12 closest to the crushing chamber 2 is inclined, with an angle of 60° between this layer of filter cloth 12 and the horizontal plane, and the working surface of the filter cloth 12 faces the lower side of the crushing chamber 2. The ventilation port 502 is located at the end of the horizontal section away from the crushing chamber 2. Three layers of screens 6 are arranged in parallel, and the mesh size of the three layers of screens 6 increases from top to bottom, namely 60 mesh, 120 mesh and 300 mesh respectively. Three return ports 504 are opened on the side wall of the vertical section and the crushing chamber 2. All three screens 6 are inclined, with an angle of 40° between the three screens 6 and the horizontal plane, and the lower end of the screens 6 extends into the return ports 504. A moisture detection sensor 13 is fixedly installed on the side wall of the vertical section. The moisture detection sensor 13 is located between the bottom screen 6 and the discharge port 503, and extends into the interior of the conveying pipe 5. Please refer to [link / reference]. Figure 5The sealing assembly includes a No. 3 motor 15, a guide rail 16, a lead screw 17, a nut 18, and a pressure plate 19. The No. 3 motor 15 is fixedly connected to the housing 1. The upper end of the output end of the No. 3 motor 15 is fixedly connected to the lead screw 17. The nut 18 is threadedly connected to the lead screw 17. The guide rail 16 is fixedly connected inside the housing 1. The nut 18 is slidably connected to the guide rail 16, and the free direction of the nut 18 and the guide rail 16 is vertical. The pressure plate 19 is fixedly connected to the nut 18 and is located at the sealing position 7. Directly above 03, two clamping plates 20 are provided on the guide rail 16, and a cover 21 is held between the two clamping plates 20. The cover 21 is coaxially set on the sealing station 703. In this specific embodiment, the operator needs to manually replenish the cover 21. When replenishing the cover 21, simply open the upper side of the two clamping plates 20, and then press the cover 21 down from the upper side of the clamping plates 20 into the space between the two clamping plates 20. Remove the force applied to the clamping plates 20, and the clamping plates 20 will hold the cover 21.

[0048] It should also be noted that, for ease of cleaning and maintenance of the grinding chamber 2, the grinding chamber 2 is fixedly connected to the housing 1 by bolts. A sealing cover 21 is installed at the upper end of the grinding chamber 2 to seal it. The output shaft of the first motor 4 has a square shaft structure. The lower end of the cutter bar 301 is coaxially provided with a square hole adapted to the output shaft of the first motor 4. The square hole is not connected to the gas passage 3011. The rotating air intake ring 11 is coaxially rotatably connected to the cutter bar 301. Two sealing rings are provided on the inner wall of the inner ring of the rotating air intake ring 11. Located on the upper and lower sides of the first through hole 3012, the two sealing rings ensure that nitrogen gas can still smoothly enter the rotating gas channel 3011 from the stationary air inlet 1101 without significant pressure loss when the cutter bar 301 is rotating at a high speed of 3000rpm-5000rpm. Furthermore, to avoid complicated positioning steps when inserting the crushing chamber 2, two positioning angle steels are set inside the housing 1. Both positioning angle steels are located away from the feed pipe 5. When the crushing chamber 2 is inserted into the housing 1, it is positioned by the feed pipe 5 and the two positioning angle steels.

[0049] Working principle: Please refer to Figures 1 to 6Before operation, a system check is performed on the device to confirm that all transmission components are connected normally and the airtightness of the sealing structure meets the standards. Then, the amino acid-containing block sample to be tested is put into the crushing chamber 2, and the feeding end sealing cover 21 at the top of the shell 1 is closed. Then, dry nitrogen is continuously introduced into the rotating air inlet ring 11. The nitrogen is sprayed downwards from between the two sets of cutter heads 302 through the gas channel 3011, the first through hole 3012, and the second through hole 3013. The pulse valve 22 is kept open, and nitrogen is kept filling the shell 1. After the nitrogen concentration detection sensor 14 detects that the nitrogen concentration in the shell 1 has reached the set value, the first motor 4 is started, driving the cutter 3 to rotate at high speed to cut and crush the sample. At this time, the shell 1 is under a positive pressure of 1.05 bar to 1.2 bar. When the air pressure in the shell 1 is greater than 1.2 bar, the pressure relief valve 10 is activated to discharge the nitrogen and maintain the nitrogen pressure in the shell 1 below 1.2 bar.

[0050] As the pulverization process continues, the working logic of pulse valve 22 during this stage is as follows: During the first 3 minutes of pulverization, pulse valve 22 passes through every 5 seconds, with each pass lasting 5 seconds. After the pulverization time exceeds 3 minutes, pulse valve 22 passes through once every 3 seconds, with each pass lasting 5 seconds. Nitrogen gas is ejected obliquely downwards from between the two sets of cutter heads 302 through gas channels 3011, through-hole 3012, and through-hole 3013. The smaller sample powder particles in the pulverization chamber 2 are carried by the obliquely ejected nitrogen gas flow. The downward jet of nitrogen gas from through-hole 3013 rebounds at the bottom of the pulverization chamber 2, forming an upward airflow. This, combined with the centrifugal force and cyclone generated by the high-speed rotation of the cutter 3, ensures the pulverization reaches the required standard. The micro powder is in a suspended fluidized state and gathers at the top of the crushing chamber 2. Under the action of pressure difference, it enters the conveying pipe 5 through the connecting port 501. After passing through multiple layers of filter cloth 12, the airflow is discharged from the vent 502. The micro powder carried by it settles down the vertical part under the action of inertia. After the micro powder is initially separated by the filter cloth 12, it enters the vertical part and is graded and screened from top to bottom through multiple layers of inclined screens 6 with increasing mesh size. Coarse particles that do not meet the requirements are returned to the crushing chamber 2 through the corresponding return port 504 and crushed again by the cutter 3. The micro powder that meets the requirements finally passes through all the screens 6 and falls into the sample bottle 9 at the receiving station 702 of the transfer indexing plate 7 through the discharge port 503.

[0051] After all the micro powder has fallen into sample bottle 9, motor 8 drives the transfer indexing plate 7 to rotate, transporting the filled sample bottle 9 to the sealing station 703. During the transport process, pulse valve 22 is triggered by the electrical control signal of motor 8, instantly spraying out a high-speed pulse nitrogen gas flow to clean the micro powder remaining on the inner wall of the crushing chamber 2 and the conveying pipe 5, as well as the surface of the screen 6, ensuring that all residual micro powder is delivered into the sample bottle 9 at the current station to avoid cross-contamination. After sample bottle 9 arrives at the sealing station 703, motor 15 starts, driving the pressure plate 19 to descend vertically along the guide rail 16 through the lead screw 17 and nut 18 transmission pair, precisely pressing the cap 21 held by the clamping plate 20 onto the mouth of sample bottle 9, completing the hermetically sealed packaging. The sealed sample bottle 9 is then rotated out by the transfer indexing plate 7 and can be directly taken out for subsequent testing. The entire process of crushing, sieving, recycling, receiving, testing, and packaging is completed in a 1.05-1.2 bar positive pressure nitrogen environment inside the shell 1, without the need for manual intervention. This avoids sample oxidation and degradation and ensures sample preparation accuracy and consistency.

[0052] The specific embodiment of the present invention has been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the embodiments described above. For those skilled in the art, various changes, modifications, substitutions, and variations made to these embodiments without departing from the principles and ideas of the present invention should still fall within the protection scope of the present invention.

Claims

1. An integrated detection device for pulverizing and preparing amino acid-containing samples, characterized in that, The device includes a housing (1), on which a crushing chamber (2) is fixedly installed at the top inner side. An air inlet (1101) for introducing inert gas is provided on the lower side of the crushing chamber (2). The air inlet (1101) is used to introduce positive pressure inert gas. A conveying pipe (5) is provided on the outer wall of the crushing chamber (2). The conveying pipe (5) is connected to the crushing chamber (2) through a connecting port (501). The connecting port (501) is located on the upper side of the crushing chamber (2) and the conveying pipe (5). A vent (502) is provided on the upper side of the side wall of the conveying pipe (5). A discharge port is provided at the lower end of the conveying pipe (5). The feed pipe (5) is equipped with a multi-layer screen (6), and a transfer indexing plate (7) is provided below the feed pipe (5). At least four sample bottles (9) are arranged in a circular array at the circumferential edge of the transfer indexing plate (7). The transfer indexing plate (7) rotates and passes through the receiving station (702) located below the feed pipe (5) and the sealing station (703) arranged along the rotation direction. A sealing assembly is provided above the sealing station (703). The sealing assembly is used to seal the upper end of the sample bottle (9). A pressure relief valve (10) is provided on the lower side wall of the shell (1). The conveying pipe (5) includes a horizontal part and a vertical part. The horizontal part is fixedly connected to the top of the inner wall of the shell (1). The vertical part is attached to the side wall of the crushing chamber (2). Multiple screens (6) are arranged in the vertical part. Multiple filter cloths (12) are arranged in the horizontal part. The filter cloths (12) near the crushing chamber (2) are inclined and the working surface of the filter cloths (12) faces the lower side of the crushing chamber (2). The vent (502) is located at the end of the horizontal part away from the crushing chamber (2). Multiple screens (6) are arranged in parallel, and the mesh count of the multiple screens (6) increases from top to bottom. The vertical part and the side wall of the crushing chamber (2) are provided with multiple return ports (504) with the same number as the screens (6). The multiple screens (6) are all arranged at an angle, and the lower end of the screens (6) extends into the return port (504).

2. The integrated sample preparation and detection device for amino acid-containing samples according to claim 1, characterized in that, The lower end of the crushing chamber (2) is rotatably connected to a cutter (3). The cutter (3) includes a cutter bar (301) and a cutter head (302). The cutter head (302) is provided with the upper end of the cutter bar (301), and the cutter head (302) includes two sets arranged vertically. The lower end of the cutter bar (301) is coaxially connected to a No. 1 motor (4). A gas channel (3011) with closed upper and lower ends is coaxially opened inside the cutter bar (301). Multiple No. 1 channels communicating with the gas channel (3011) are opened on the side wall of the cutter bar (301). The housing (1) has a hole (3012) and multiple second through holes (3013). A rotating air intake ring (11) is fixedly installed inside the housing (1). The rotating air intake ring (11) is rotatably connected to the cutter bar (301). The air inlet (1101) is located on the outer wall of the rotating air intake ring (11), and the air inlet (1101) is connected to multiple first through holes (3012) through the rotating air intake ring (11). Multiple second through holes (3013) are located between two sets of cutter heads (302), and the second through holes (3013) are inclined downwards.

3. The integrated sample preparation and detection device for amino acid-containing samples according to claim 1, characterized in that, A moisture detection sensor (13) is fixedly installed on the side wall of the vertical part. The moisture detection sensor (13) is located between the bottom screen (6) and the discharge port (503), and the moisture detection sensor (13) extends into the interior of the conveying pipe (5).

4. The integrated sample preparation and detection device for amino acid-containing samples according to claim 1, characterized in that, The pressure relief valve (10) is located on the side away from the vent (502). The housing (1) is provided with a nitrogen concentration detection sensor (14) on the side wall where the pressure relief valve (10) is located. The pressure relief valve (10) and the nitrogen concentration detection sensor (14) are respectively located on the front and rear sides.

5. The integrated sample preparation and detection device for amino acid-containing samples according to claim 1, characterized in that, The sealing assembly includes a No. 3 motor (15), a guide rail (16), a lead screw (17), a nut (18), and a pressure plate (19). The No. 3 motor (15) is fixedly connected to the housing (1). The upper end of the output end of the No. 3 motor (15) is fixedly connected to the lead screw (17). The nut (18) is threadedly connected to the lead screw (17). The guide rail (16) is fixedly connected inside the housing (1). The nut (18) is slidably connected to the guide rail (16), and the free direction of the nut (18) and the guide rail (16) is vertical. The pressure plate (19) is fixedly connected to the nut (18), and the pressure plate (19) is located directly above the sealing station. Two clamping plates (20) are provided on the guide rail (16). A sealing cap (21) is held between the two clamping plates (20). The sealing cap (21) is coaxially set on the sealing station (703).

6. The integrated sample preparation and detection device for amino acid-containing samples according to claim 2, characterized in that, The inner walls of the crushing chamber (2) and the vertical part are coated with polytetrafluoroethylene, and the blade (301) and the blade head (302) are made of stainless steel.

7. The integrated sample preparation and detection device for amino acid-containing samples according to claim 1, characterized in that, The lower end of the transfer indexing plate (7) is provided with a second motor (8), the housing (1) is provided with an electrical control module, and the air inlet (1101) is provided with a pulse valve (22). The pulse valve (22) and the second motor (8) are both electrically connected to the electrical control module.

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