A device for detecting raw and auxiliary materials for liquor brewing
By using a gas introduction system with arc-shaped structure and disturbance components in the detection device for raw and auxiliary materials for liquor brewing, the turbulent mixing principle and fin structure are used to solve the problem of uneven mixing of reference gas and sample gas, and efficient and accurate isotope ratio detection is achieved.
Patent Information
- Application Number
- CN202510765500.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-10
- Publication Date
- 2025-08-15
- Estimated Expiration
- 2045-06-10
AI Technical Summary
In the detection of raw and auxiliary materials for liquor brewing, the calculation error of isotope ratio due to uneven dilution of reference gas and sample gas is large, which affects the detection accuracy.
The gas introduction unit and disturbance assembly with arc-shaped structure are adopted. Through the principle of turbulent induced mixing, combined with the fin structure and electromagnet control, the gas is efficient and uniformly mixed and the isotope ratio calculation error is reduced.
It significantly improves the mixing dilution efficiency and uniformity, reduces the δ value error of isotope ratio, and improves the accuracy and accuracy of the detection of raw and auxiliary materials for liquor brewing.
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Figure CN120275481B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of liquor detection, and in particular to a device for detecting raw and auxiliary materials for liquor brewing. Background Art
[0002] In the baijiu (white liquor) brewing process, the quality of raw and auxiliary materials, at the source of the production chain, not only determines the style and flavor of the finished liquor but also directly impacts product safety indicators and economic parameters of yield. For this reason, modern brewing companies have widely adopted isotope detection technology. Through the analysis of stable isotope ratios of carbon, hydrogen, and oxygen, they systematically establish a full-chain quality assurance system, from raw material traceability, auxiliary material authenticity verification, dynamic monitoring of the fermentation process, to the quality control standards of the finished liquor.
[0003] Existing isotope detection techniques typically rely on isotope ratio mass spectrometry (IRMS), which uses a high-precision mass spectrometer to determine the isotope ratio in a sample. In an elemental analyzer-isotope ratio mass spectrometer (EA-IRMS) system, the sample undergoes high-temperature combustion / pyrolysis to generate target gases (such as CO2, N2, H2, etc.), which are carried into the mass spectrometer by a carrier gas (usually high-purity helium). Simultaneously, a reference gas of known isotopic composition is introduced to calibrate instrument drift and mass discrimination in real time. Therefore, measurement accuracy is highly dependent on the accurate and stable introduction of both the reference and sample gases.
[0004] To ensure accurate and stable introduction of reference and sample gases, patent publication CN105705929A discloses a gas inlet system for an isotope ratio mass spectrometer. This system utilizes a variable-volume reservoir combined with an open flow divider to dilute the analyte concentration using carrier gas. The commonly used EA IsoLink™ IRMS system incorporates multiple fixed and retractable capillaries within an interface tube, respectively used to input inert gas, reference / sample gas, and output the diluted gas to the isotope ratio mass spectrometer.
[0005] The above-mentioned existing technologies use straight tube or simple cavity structures to achieve gas mixing and dilution. Under low Reynolds number (Re < 2000) conditions, the gas flows through the mixing cavity in a stratified flow form, and the molecules are mixed only through slow axial diffusion. The radial mixing rate of the reference gas and the carrier gas / the sample gas and the carrier gas is low, which may lead to the formation of a concentration gradient in the mixing cavity. The mixed and diluted reference gas and sample gas are continuously and rapidly introduced into the mass spectrometer, causing the mass spectrometer detection signal to fluctuate (such as 13 CO2 / 12 CO2 ratio changes instantaneously), which leads to increased errors in isotope ratio calculations.
[0006] In summary, in the current EA-IRMS system, the δ value error caused by uneven laminar mixing and dilution concentration in trace isotope analysis has become a key bottleneck restricting the detection accuracy of raw and auxiliary materials for liquor brewing. The traditional mixing and dilution structure can no longer meet the demand; there is an urgent need for a liquor brewing raw and auxiliary material detection device that integrates a gas introduction system that can efficiently and evenly mix the dilution gas. Summary of the Invention
[0007] In order to solve the above problems, the present invention provides a device for detecting raw and auxiliary materials for liquor brewing, which is used to promote the efficient and uniform mixing and dilution of reference gas and carrier gas / sample gas and carrier gas during the detection process of raw and auxiliary materials for liquor brewing, reduce the isotope ratio calculation error, and improve the detection accuracy.
[0008] In order to achieve the above-mentioned purpose, the technical solution of the present invention is as follows: A device for detecting raw materials and auxiliary materials for liquor brewing, comprising:
[0009] an injection system for automatic sampling;
[0010] A sample processing system for converting organic or inorganic components in a sample into a sample gas;
[0011] a gas supply system for supplying carrier gas and reference gas;
[0012] Gas introduction system for mixing, diluting, and introducing sample and reference gases
[0013] Detection systems for determining isotope ratios;
[0014] The gas introduction system includes a sample gas introduction unit and a reference gas introduction unit. The sample gas introduction unit and the reference gas introduction unit each include at least one container. An air inlet cavity for supplying gas is opened on the side wall of the container. A disturbance component is fixedly connected to the inside of the container. The disturbance component is used to promote turbulence in the container and control the gas in the air inlet cavity to enter the container. The container is also connected to a first pipeline and a second pipeline respectively, and the second pipeline is connected to the detection system.
[0015] Furthermore, the inner wall of at least one end of the container of the sample gas introduction unit is an arc-shaped structure, the disturbance component is arranged on the inner wall of the container adjacent to the arc-shaped structure area, the first pipeline extends into the container and the opening faces the arc-shaped structure area, and the second pipeline extends into the container and the opening is located on the inner wall of the container opposite to the arc-shaped structure area.
[0016] Furthermore, the container of the reference gas introduction unit has an arc-shaped structure at at least two ends, the disturbance component is arranged on the inner wall between the arc-shaped structure areas in the container, the number of openings of the first pipeline is at least two, the first pipeline extends into the container and the openings are respectively directed toward the arc-shaped structure areas at both ends, and the second pipeline extends into the container and the opening is located at the center position between the arc-shaped structure areas in the container.
[0017] Furthermore, the disturbance assembly includes a plurality of fixed brackets fixedly connected to the inner side wall of the container, the fixed brackets are evenly spaced along the axial direction of the container, and each fixed bracket is rotatably connected to a plurality of fins, and adjacent fins are in contact with each other. A control mechanism for independently controlling the locking and release of each layer of fins is provided in the air inlet cavity, and the control mechanism is used to release one or more layers of fins after the gas enters the air inlet cavity.
[0018] Furthermore, the fins are shield-scale shaped, and the fins on the inner wall of the container are arranged in a tiled or honeycomb manner as a whole. Ribs are provided in the center of the fins, the upstream side of the ribs faces the arc structure area, and the downstream side of the ribs faces the opening of the second pipeline, and a number of micro grooves are formed between the fins.
[0019] Furthermore, the edges of the fins are made of elastic material, and the surfaces of the fins are coated with a fluorinated nano-coating.
[0020] Furthermore, the control mechanism includes a controller and several groups of electromagnets installed on the inner side wall of the air inlet cavity. The electromagnets are evenly spaced along the axial direction of the container and correspond one-to-one to the fins. The electromagnets are all connected to the controller signal. A magnetic attraction member is provided on the surface of the fin facing the air inlet cavity. The magnetic attraction range of each group of electromagnets is less than or equal to the size of the magnetic attraction member.
[0021] The controller is used to cut off power to one or more sets of electromagnets after gas enters the air inlet chamber.
[0022] Furthermore, the controller is used to receive the type of gas entering the air inlet chamber, and cut off the power to the electromagnets in the specified position area based on the type of gas in the air inlet chamber, and cut off the power to a specified number of electromagnets based on the concentration of the mixed and diluted sample gas or reference gas.
[0023] Furthermore, the controller is also used to adjust the current of some electromagnets based on the gas flow entering the air inlet chamber and the gas flow introduced into the detection system through the second pipeline.
[0024] Furthermore, a groove is provided on the surface of the fin facing the air inlet cavity, the groove is located on the tail side of the fin, the magnetic part is arranged in the groove, and the distance from the rotating connection between the fin and the fixed bracket to the tail of the fin is greater than the spacing between adjacent fixed brackets.
[0025] The technical principles of the above solution are as follows:
[0026] This solution is based on an improved elemental analyzer (EA) + isotope ratio mass spectrometry (IRMS). The EA side uses the same injection system, sample processing system, and gas supply system. The injection system is mainly used for solid or liquid (such as grain, koji) sampling; the sample processing system is used to generate gas by burning or high-temperature oxidation of the sample; the gas supply system is used to supply carrier gas (usually He) and reference gas (usually N2, CO2, SO2, H2, CO). The IRMS side uses the detection system, which is mainly composed of an ion source, a mass analyzer, and a multi-receiver. The ion source is used to ionize gas molecules; the mass analyzer is used to deflect the ion path through a magnetic field and separate them according to mass-to-charge ratio; the multi-receiver is used to detect the ion flow of different mass numbers; and finally, the δ value of the sample is calculated by computer software.
[0027] Improve the existing gas introduction system. Based on the principles of turbulence-induced mixing and adaptive flow field control, the unique structural design breaks the limitations of traditional laminar mixing and improves the mixing uniformity of reference gas and sample gas.
[0028] On the one hand, the curved structure guides the flow through the cavity. The curved inner wall of the sample gas introduction unit and the double-ended curved structure of the reference gas introduction unit utilize the inertia of the airflow to generate centrifugal force, forcing the gas to flow along the curved surface and forming a lateral velocity gradient, inducing local turbulence and accelerating the diffusion of gas molecules. Furthermore, the shield-scale fins, arranged in a shingled or honeycomb pattern, with surface microgrooves, induce the airflow to slip parallel to the flow direction, reducing shear stress, lowering flow resistance, and enhancing airflow adhesion to the shield-scale fin surface, thereby allowing the input first-type gas to flow along the inner wall of the container. Because some of the fins are released, the second-type gas, passing through the inlet cavity, pushes the released fins at an angle. The tilted fins no longer induce the airflow (the first-type gas) to slip parallel to the original flow direction, but instead induce it to flow in an inclined direction. Simultaneously, the second-type gas is discharged tangentially to the first-type gas. The two airflows flow tangentially, with a velocity difference in the contact area, thus generating a velocity gradient. The velocity gradient causes shear force to be generated between the first type of gas layer and the second type of gas layer, causing deformation and disturbance of the airflow, destroying the stability of the laminar flow, and changing the airflow from laminar flow to turbulent flow, promoting the dilution and mixing of the two types of gases (usually He diluent gas and reference gas or sample gas). At the same time, because air flows through both the surface and back of the shield scale fins, the airflow speeds are different, making it in a non-fixed tilt state. Its tilt angle changes in real time, causing oscillations that disrupt the laminar flow of gas on its surface, making the kinetic energy distribution of the airflow uneven, generating local energy disturbances, and triggering tiny vortices within the airflow, providing the energy basis for the formation of turbulence.
[0029] Furthermore, a controller selectively de-energizes specific electromagnet groups based on gas type, concentration, and flow signals, releasing the corresponding fins. The fins, impacted by the airflow, oscillate freely, forming a dynamic turbulence barrier that adaptively adjusts mixing intensity. Based on data from the flow sensor at the second pipe outlet, the controller dynamically adjusts the electromagnet current and controls the fin opening and closing angles to balance mixing efficiency and system backpressure.
[0030] On the other hand, the fin surface is coated with a low surface energy fluorinated nano-coating to reduce the adsorption of polar molecules. At the same time, since the grooves can induce the fluid to slip parallel to the flow direction, the gas is promoted to flow toward the opening side of the second pipeline, reducing the adsorption residue of the gas in the container and eliminating the memory effect.
[0031] The beneficial effects of the present invention are as follows:
[0032] 1. Based on turbulent mixing efficiency, compared with the existing straight tube structure or simple cavity structure, the mixing dilution efficiency and uniformity are greatly improved, the error of the isotope ratio δ value is reduced, and the accuracy of the detection of raw and auxiliary materials for liquor brewing is improved, meeting the detection needs of raw and auxiliary materials for liquor brewing.
[0033] 2. Dynamic adaptive adjustment of dilution and mixing. Compared with the existing simple adjustment of input gas flow, the fin layered release and angle adjustment can adapt to different gas types and concentration gradients, making the mixing and dilution efficiency and uniformity more stable.
[0034] 3. Eliminate the memory effect. Compared with the existing straight tube structure or simple cavity structure, by applying a low surface energy fluorinated nano-coating and using the shield-scale fin micro-groove structure to promote the flow of gas to the output side, the adsorption residue of gas in the container is reduced. BRIEF DESCRIPTION OF THE DRAWINGS
[0035] Figure 1 This is a schematic diagram of the overall structure of an embodiment of a detection device for raw and auxiliary materials for liquor brewing according to the present invention;
[0036] Figure 2 This is a schematic structural diagram of a reference gas introduction unit of an embodiment of a device for detecting raw and auxiliary materials for liquor brewing according to the present invention;
[0037] Figure 3 This is a schematic structural diagram of a sample gas introduction unit of an embodiment of a device for detecting raw and auxiliary materials for liquor brewing according to the present invention;
[0038] Figure 4 This is a partially cutaway schematic diagram of a reference gas container of an embodiment of a device for detecting raw and auxiliary materials for liquor brewing according to the present invention;
[0039] Figure 5 This is a partially cutaway schematic diagram of a sample gas container of an embodiment of a device for detecting raw and auxiliary materials for liquor brewing according to the present invention;
[0040] Figure 6for Figure 4 A local enlarged schematic diagram;
[0041] Figure 7 This is a schematic diagram of the operating principle of the control mechanism of an embodiment of the white wine brewing raw and auxiliary material detection device of the present invention;
[0042] Figure 8 This is a schematic diagram of the fin installation structure of an embodiment of the white wine brewing raw and auxiliary material detection device of the present invention.
[0043] The reference numerals in the drawings of the specification include: 1, electromagnet; 1a, first electromagnet; 1b, second electromagnet; 1c, third electromagnet; 1d, fourth electromagnet; 2, fin; 3, rib; 4, air inlet cavity; 5, fixing bracket; 6, groove; 7, magnetic element; 100, injection system; 200, sample processing system; 300, gas supply system; 400, reference gas introduction unit; 500, sample gas introduction unit; 600, detection system; 10, liquid automatic sampler; 20, solid automatic sampler; 30 , high-temperature cracking module; 40, dynamic fast combustion module; 50, water removal trap; 60, CG column; 70, TCD; 80, automatic switching valve; 301, N2 interface; 302, CO2 interface; 303, H2 interface; 304, SO2 interface; 305, CO interface; 306, dilution gas interface; 401, second carrier gas input pipeline; 402, reference gas output pipeline; 403, reference gas container; 501, first carrier gas input pipeline; 502, sample gas output pipeline; 503, sample gas container. DETAILED DESCRIPTION
[0044] The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.
[0045] In the description of the present invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings and are intended solely to facilitate and simplify the description of the present invention. They are not intended to indicate or imply that the devices or components referred to must have, be constructed, or operate in a specific orientation, and therefore should not be construed as limitations on the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.
[0046] In the description of the present invention, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they may refer to fixed, detachable, or integral connections; mechanical or electrical connections; direct or indirect connections through an intermediate medium; and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on the specific circumstances.
[0047] The following is further described in detail through specific implementation methods:
[0048] Example: A detection device for raw and auxiliary materials of liquor brewing, which is based on the improved design of elemental analyzer-isotope ratio mass spectrometry (EA-IRMS) system, mainly consists of a sampling system 100, a sample processing system 200 and a gas supply system 300 at the EA end. Figure 1 As shown, the sampling system 100 of this embodiment includes a liquid automatic sampler 10 and a solid automatic sampler 20, which are respectively used to automatically sample solid samples and liquid samples. The sample processing system 200 of this embodiment includes a pyrolysis module 30 and a dynamic fast combustion module 40. The pyrolysis module 30 is used to process liquid samples, and the dynamic fast combustion module 40 is used to process solid samples.
[0049] In this embodiment, the high-temperature cracking module 30 is mainly composed of a ceramic tube, a glassy carbon tube, a glassy carbon particle filler, a graphite crucible and an Ag filler. A sample inlet is set at the top of the ceramic tube, and a sample outlet and a carrier gas inlet are set at the bottom of the ceramic tube. The glassy carbon tube is set inside the ceramic tube. The glassy carbon tube is sequentially provided with Ag filler, glassy carbon particle filler and graphite crucible from bottom to top. The Ag filler and glassy carbon particle filler area is a high-temperature zone. The carrier gas is input into the carrier gas inlet, and the carrier gas flows to the sample inlet, carrying the sample to flow toward the sample outlet, thereby realizing high-temperature cracking of the sample. The process temperature is 1450°C.
[0050] In this embodiment, the dynamic rapid combustion module 40 consists of, from top to bottom, quartz wool (10 mm), Cr2O3 (50 mm), quartz wool (10 mm), reducing Cu (110 mm), quartz wool (10 mm), Ag2Co3O4 (30 mm), and quartz wool (30 mm). The sample passes through this module in sequence, achieving dynamic rapid combustion at a process temperature of 1100°C.
[0051] The rear end of the sample processing system 200 of this embodiment includes two groups of CG columns 60, which are respectively connected to the high-temperature cracking module 30 and the dynamic fast combustion module 40, and a water removal trap 50 (Mg(ClO4)2) is provided between the dynamic fast combustion module 40 and the CG columns 60. The rear ends of the two groups of CG columns 60 are provided with TCD70 and an automatic switching valve 80.
[0052] The gas supply system 300 of this embodiment comprises two dilution gas interfaces 306 and five reference gas interfaces, each used to supply dilution gas and reference gas. In this embodiment, both dilution gas interfaces 306 are used to supply He gas. One He gas interface is used as a dilution gas to mix with and dilute the sample gas, while the other He gas interface is used as a dilution gas to mix with and dilute the reference gas. The five reference gas interfaces are used to supply N2, CO2, SO2, H2, and CO, respectively: N2 interface 301, CO2 interface 302, SO2 interface 304, H2 interface 303, and CO interface 305.
[0053] The detection system 600 at the IRMS end is mainly composed of an ion source, a mass analyzer and a multi-receiver. The ion source is used to ionize gas molecules; the mass analyzer is used to deflect the ion path through a magnetic field and separate them according to the mass-to-charge ratio; the multi-receiver is used to detect the flow of ions with different mass numbers; and finally, the δ value of the sample is calculated by computer software.
[0054] This embodiment focuses on improving the gas introduction system. Existing straight tube structures or simple cavity structures for mixing and diluting sample and reference gases have difficulty meeting current requirements in terms of efficiency and uniformity. During the testing of raw and auxiliary materials for liquor brewing, there is a probability of δ-value errors in the mass spectrometry detection signal fluctuations. Therefore, this embodiment divides the gas introduction system into a sample gas introduction unit 500 and a reference gas introduction unit 400.
[0055] Combine Figure 2-Figure 5 As shown, the sample gas introduction unit 500 of this embodiment comprises a container with an inner wall having a curved structure at one end and a flat structure at the other end, while the reference gas introduction unit 400 comprises a container with inner walls having curved structures at both ends. In this embodiment, the container of the sample gas introduction unit 500 is named sample gas container 503, and the container of the reference gas introduction unit 400 is named reference gas container 403 for ease of distinction.
[0056] The inner walls of both the sample gas container 503 and the reference gas container 403 are provided with an inlet cavity 4 for supplying gas. A disturbance component is located near the center of the inlet cavity 4 to promote turbulence within the container and control the flow of gas from the inlet cavity 4 into the container. Both the sample gas container 503 and the reference gas container 403 are connected by a first pipeline and a second pipeline, with the second pipeline communicating with the detection system 600.
[0057] In this embodiment, the first pipeline connected to the sample gas container 503 is named the first carrier gas input pipeline 501, and the second pipeline is named the sample gas output pipeline 502. The first pipeline connected to the reference gas container 403 is named the second carrier gas input pipeline 401, and the second pipeline is named the reference gas output pipeline 402. One of the sample gas input pipelines is connected to the dilution gas interface 306 for delivering He gas into the sample gas container 503, while the sample gas output pipeline 502 is used to deliver the sample gas, which has been mixed and diluted with He gas, to the detection system 600. The second carrier gas input pipeline 401 is connected to the other dilution gas interface 306 for delivering He gas into the reference gas container 403, while the reference gas output pipeline 402 is used to deliver the reference gas, which has been mixed and diluted with He gas, to the detection system 600.
[0058] Next, the internal structures of the sample gas container 503 and the reference gas container 403 are described respectively:
[0059] The disturbance component of the sample gas container 503 is located on the inner wall (i.e., the side wall in this embodiment) adjacent to the curved structural region (i.e., the bottom wall in this embodiment). The planar structural region is located on the top wall in this embodiment. The opening (output end) of the first carrier gas input line 501 faces the curved structural region, while the opening (input end) of the sample gas output line 502 is located near the planar structural region and also faces the curved structural region. The inlet chamber 4 of the sample gas container 503 is connected to the automatic on / off valve 80, allowing sample gas to enter the inlet chamber 4.
[0060] The disturbance component of reference gas container 403 is located on the inner wall (i.e., the lower and upper sidewalls in this embodiment) between the two curved structural regions (i.e., the bottom and top walls in this embodiment). The disturbance component does not cover the middle sidewall region of reference gas container 403. The second carrier gas input line 401 has a T-shaped opening with two ends, located in the middle region of the container, with the two ends opening toward the two curved structural regions of reference gas container 403. The gas inlet chamber 4 of reference gas container 403 is connected to five reference gas ports. In this embodiment, two reference gas ports (CO2 and CO) connect to the upper gas inlet chamber 4, and three reference gas ports (N2, SO2, and H2) connect to the lower gas inlet chamber 4. The reference gas input into the gas inlet chamber 4 of reference gas container 403 is regulated by a solenoid valve, ensuring that the designated reference gas enters the gas inlet chamber 4.
[0061] The disturbance assembly includes several fixed brackets 5 fixedly connected to the inner wall of the container. The fixed brackets 5 are adapted to the internal structure of the sample gas container 503 and the reference gas container 403. For example, in this embodiment, the interior of the sample gas container 503 and the reference gas container 403 are cylindrical, while the fixed brackets 5 are annular and adapted to the inner wall of the sample gas container 503 and the reference gas container 403. The fixed brackets 5 are evenly spaced along the axial direction of the container, and the diameter of the fixed brackets 5 in the arc structure area gradually decreases.
[0062] Combine Figure 6-Figure 8 As shown, a plurality of fins 2 are rotatably connected to the fixed bracket 5, and the fins 2 are shield-scale-shaped; adjacent fins 2 are in contact with each other, and the preferred fins 2 are arranged in a tiled or honeycomb style as a whole. Ribs 3 are provided in the center of the fins 2, and the upstream side of the ribs 3 faces the arc-shaped structure area, and the downstream side of the ribs 3 faces the openings of the sample gas output pipeline 502 and the reference gas output pipeline 402, and a plurality of micro grooves are formed between the fins 2. The edges of the fins 2 need to be made of elastic material to enhance the sealing of the contact parts between the fins 2. The fins 2 can also be made of elastic material as a whole, preferably fluororubber, which is resistant to high temperature and acidic gas corrosion and extends the service life. In addition, the surface of the fins 2 is coated with a fluorinated nano-coating, which has the characteristics of low surface energy, corrosion resistance, hydrophobicity and oleophobicity, and can reduce the adsorption of polar molecules.
[0063] The air inlet chamber 4 is equipped with a control mechanism that independently controls the locking and release of each layer of fins 2. This mechanism is used to release one or more layers of fins 2 after gas enters the air inlet chamber 4. Specifically, the control mechanism includes a controller and several groups of electromagnets 1 mounted on the inner wall of the air inlet chamber 4. The electromagnets 1 are coated with a protective film to prevent interference with the reference gas within the air inlet chamber 4. The electromagnets 1 are evenly spaced along the axial direction of the container and correspond one-to-one with each fin 2. Each electromagnet 1 is connected to the controller signal. The surface of the fins 2 facing the air inlet chamber 4 is provided with a magnetic element 7. The magnetic attraction range of each group of electromagnets 1 is less than or equal to the size of the magnetic element 7.
[0064] The fin 2 has a groove 6 on the side facing the air inlet cavity 4. The groove 6 is located on the rear end of the fin 2. A magnetic element 7 is disposed within the groove 6. The distance between the pivotal connection between the fin 2 and the fixing bracket 5 and the rear end of the fin 2 is greater than the distance between adjacent fixing brackets 5. Therefore, when the fin 2 is locked, its groove 6 can fit on the fixing bracket 5 of the lower fin 2, limiting the position of the entire fin 2.
[0065] The controller is used to de-energize one or more groups of electromagnets 1 after gas enters the inlet chamber 4. The controller's specific control strategy is as follows: it receives the type of gas entering the inlet chamber 4 and de-energizes electromagnets 1 in a specified area based on the type of gas in the inlet chamber 4. Furthermore, it de-energizes a specified number of electromagnets 1 based on the concentration of the mixed and diluted sample gas or reference gas. In some embodiments, the current of some electromagnets 1 is also adjusted based on the flow rate of gas entering the inlet chamber 4 and the flow rate of gas introduced into the detection system 600 through the second pipeline.
[0066] Since the mixing rates of different types of gases with He diluent are different, the core mechanism of the mixing rate is the diffusion between gas molecules, which follows Fick's law:
[0067]
[0068] Where D is the diffusion coefficient, which is directly related to the type of gas and is affected by molecular weight, molecular diameter and polarity; is the concentration C along the spatial direction rate of change. Since different gases (reference gas and sample gas) have different diffusion coefficients, different mixing times are required to achieve the purpose of uniform mixing and dilution to the specified concentration. At the same time, the position where the fin 2 is released directly affects the efficiency of the mixed and diluted gas reaching the opening of the sample gas output pipeline 502 and the reference gas output pipeline 402. If the fin 2 that is farther away from the opening of the sample gas output pipeline 502 and the reference gas output pipeline 402 is released, the airflow sliding parallel to the original flow direction is disturbed in advance, and the opening time of the flow to the sample gas output pipeline 502 and the reference gas output pipeline 402 is prolonged. Therefore, it is necessary to release the fin 2 that is closer to the opening of the sample gas output pipeline 502 and the reference gas output pipeline 402 as much as possible in combination with the type of gas to be mixed and diluted, so that the gas is uniformly mixed and diluted to the specified concentration and can efficiently reach the opening of the sample gas output pipeline 502 and the reference gas output pipeline 402.
[0069] Since the concentration of the reference gas supplied by the reference gas interface is known, and the concentration after mixing and diluting with the He dilution gas is also known, the greater the difference between the two groups of concentrations, the greater the difference between the volume of He dilution gas required to be input into the reference gas container 403 and the volume of the reference gas. By releasing a specified number of fins 2, the flow rate of reference gas input from the air inlet chamber 4 to the reference gas container 403 can be adjusted to match the flow rate of the He dilution gas input, ensuring that the input of He dilution gas and reference gas is completed synchronously within a similar time.
[0070] By adjusting the current of electromagnet 1, the magnetic attraction of electromagnet 1 to magnetic element 7 can be adjusted. When the air pressure in intake chamber 4 is similar, the inclination (opening) of fin 2 is inversely proportional to the current, thereby further finely controlling the gas flow output from intake chamber 4. This meets the demand for more precise air intake rate control in some embodiments.
[0071] Combine Figure 7 As shown, the electromagnets 1 are numbered in sequence as the first electromagnet 1a, the second electromagnet 1b, the third electromagnet 1c, the fourth electromagnet 1d...the Nth electromagnet. The controller records the numbers and positions of the corresponding electromagnets 1. When it is necessary to lock or release the electromagnets 1 with the corresponding numbers, the controller controls the power on and off of the electromagnets 1 at the corresponding positions or adjusts the current.
[0072] When using this device, first, turn on the power of the elemental analyzer (EA), preheat the high-temperature cracking module from 30 to 1450°C and the dynamic fast combustion module from 40 to 1100°C; start the isotope ratio mass spectrometer (IRMS), evacuate the vacuum system to <10-6 mbar, and preheat the ion source and mass analyzer.
[0073] Connect two He diluent gas cylinders (purity ≥99.999%) and adjust the pressure reducing valve output pressure to 0.3 MPa. Check the five reference gas connections (N2, CO2, SO2, H2, CO) to ensure cylinder pressures are ≥5 MPa and there are no leaks. Calibrate the system using standard reference materials (e.g., USGS40, IAEA-600) and input the reference gas delta values into the control software.
[0074] The fin 2 release strategy is preset in the controller (the fin 2 close to the sample gas output pipeline 502 may be released preferentially by default); the He dilution ratio is automatically matched according to the reference gas type (eg, CO2:He=1:100).
[0075] For example, a solid sample (such as sorghum or rice husk) is ground to a mesh size of ≤200, and 5-10 mg is weighed and placed in a tinfoil cup. The cup is compressed, degassed, and folded into pellets. The sample is then pushed into the sample inlet of the dynamic fast combustion module 40 using a solid autosampler 20. A carrier gas (He) carries the sample through the combustion layers (Cr2O3, Ag2Co3O4, and reducing Cu) in sequence. The generated gases (CO2, N2, and H2O) are then dehydrated by a dehydration trap 50 (Mg(ClO4)2) before entering a CG column 60 for separation.
[0076] Open the first carrier gas input pipeline 501 and adjust the He flow rate. After the controller identifies the type of sample gas (such as CO2), it releases the preset position of fin 2 (electromagnet 1 is powered off). If air flow fluctuations are detected, the opening of fin 2 is automatically increased (the current of electromagnet 1 is reduced). The controller selects a matching reference gas (such as detecting δ 13 C) selects CO2 as the reference gas; open the second carrier gas input line 401 and adjust the He flow rate to a preset dilution ratio. The controller releases the middle region fin 2 based on the reference gas molecular weight (e.g., CO2 molecular weight 44) to promote turbulent mixing.
[0077] Alternately introduce diluted sample and reference gases into an isotope ratio mass spectrometer (IRMS) using an electron impact energy of 70 eV to ionize gas molecules (e.g., CO₂ → CO⁺). The magnetic field is set to 0.8 Tesla to isolate target ions (e.g., m / z 44, 45, and 46). Multiple receivers simultaneously collect ion currents, and software calculates isotope ratios.
[0078] The software generates a test report that includes: sample isotope δ value, data credibility index, automatic matching database, and prompts for raw material origin or adulteration risks.
[0079] The following comparative tests and analyses were conducted on the device of this embodiment and the existing element analyzer-isotope ratio mass spectrometry (EA-IRMS) system:
[0080] Test sample:
[0081] Sample type: Sorghum (starch δ 13 C), rice husk (mildew rate δ 34 S).
[0082] Standard material: USGS40 (δ 13 C=-26.39‰), IAEA-SOIL (δ 34 S=+5.3‰).
[0083] Test parameters:
[0084] Mixing uniformity (RSD): standard deviation of the tracer gas (SF6) concentration distribution.
[0085] Isotope detection precision: δ value repeatability (standard deviation of 10 measurements).
[0086] Detection time: the total time from sample injection to result output.
[0087] Test results: see Table 1
[0088] Table 1 Comparative test results between the device of this embodiment and the EA-IRMS system
[0089] Test indicators This device EA-IRMS Improvement Test Method Mixing uniformity (RSD) <![CDATA[≤1.2% (SF6 tracer)]]> 5%-8% Increased by 4-7 times Multi-point concentration sampling + mass spectrometry analysis <![CDATA[δ 13 C Detection Error]]> ±0.04‰ (USGS40) ±0.2‰ Accuracy increased by 5 times Standard deviation of 10 repeated measurements <![CDATA[δ 34 S detection error]]> ±0.2‰ (IAEA-SOIL) ±0.5‰ Accuracy increased by 5 times Standard deviation of 10 repeated measurements Single detection time 8 minutes (solid sample) 15 minutes (solid sample) Efficiency increased by 47% Full process timing (from injection to data output)
[0090] Test conclusion: Through the arc cavity + shield-scale fins to induce turbulence, the SF6 tracer gas RSD is ≤1.2%; the mixing efficiency is significantly improved, and the isotope signal baseline fluctuation is reduced. Dynamic calibration + intelligent fin control, δ 13 C error is ±0.04‰; it meets the testing needs of raw and auxiliary materials for liquor brewing.
[0091] Obviously, the above embodiments are merely examples for clarity of explanation and are not intended to limit the implementation methods. Those skilled in the art will readily appreciate that other variations or modifications based on the above descriptions are possible. It is not necessary and impossible to enumerate all implementation methods here. Obvious variations or modifications arising therefrom remain within the scope of protection of the present invention.
Claims
1. A device for detecting raw and auxiliary materials for liquor brewing, comprising: an injection system for automatic injection (100); a sample processing system (200) for converting organic or inorganic components in a sample into a sample gas; a gas supply system (300) for supplying carrier gas and reference gas; A gas introduction system for mixing, diluting, and introducing sample gas and reference gas; a detection system (600) for determining isotope ratios; The invention is characterized in that the gas introduction system includes a sample gas introduction unit (500) and a reference gas introduction unit (400), the sample gas introduction unit (500) and the reference gas introduction unit (400) each include at least one container, the side wall of the container is provided with an air inlet cavity (4) for supplying gas, a disturbance component is fixedly connected to the inside of the container, the disturbance component is used to promote the formation of turbulence in the container and control the gas in the air inlet cavity (4) to enter the container, the container is further connected to a first pipeline and a second pipeline respectively, and the second pipeline is connected to the detection system (600); The disturbance assembly comprises a plurality of fixed brackets (5) fixedly connected to the inner side wall of the container, the fixed brackets (5) being evenly spaced along the axial direction of the container, a plurality of fins (2) being rotatably connected to each fixed bracket (5), adjacent fins (2) being in contact with each other, and a control mechanism for independently controlling the locking and releasing of each layer of fins (2) being provided in the air inlet cavity (4), the control mechanism being used to release one or more layers of fins (2) after gas enters the air inlet cavity (4); The control mechanism includes a controller and a plurality of groups of electromagnets (1) installed on the inner wall of the air inlet cavity (4). The electromagnets (1) are evenly spaced along the axial direction of the container and correspond one to one with the fins (2). The electromagnets (1) are all connected to the controller signal. The surface of the fin (2) facing the air inlet cavity (4) is provided with a magnetic attraction member (7). The magnetic attraction range of each group of electromagnets (1) is less than or equal to the size of the magnetic attraction member (7). The controller is used to cut off power to one or more groups of electromagnets (1) after gas enters the air inlet chamber (4).
2. The device for detecting raw and auxiliary materials for brewing liquor according to claim 1, characterized in that: The inner wall of at least one end of the container of the sample gas introduction unit (500) is an arc-shaped structure, the disturbance component is arranged on the inner wall of the container adjacent to the arc-shaped structure area, the first pipeline extends into the container and opens toward the arc-shaped structure area, and the second pipeline extends into the container and opens at the inner wall of the container opposite to the arc-shaped structure area.
3. The device for detecting raw and auxiliary materials for brewing liquor according to claim 1, characterized in that: The reference gas introduction unit (400) has a container with at least two ends having an arc-shaped structure, a disturbance component is arranged on the inner wall between the arc-shaped structure areas in the container, the first pipeline has at least two openings, the first pipeline extends into the container and the openings are respectively oriented toward the arc-shaped structure areas at the two ends, and the second pipeline extends into the container and the opening is located at the center position between the arc-shaped structure areas in the container.
4. The device for detecting raw and auxiliary materials for brewing liquor according to claim 1, characterized in that: The fins (2) are shield-scale shaped, and the fins (2) on the inner side wall of the container are arranged in a tile-like or honeycomb-like manner as a whole. Ribs (3) are provided in the center of the fins (2), the upstream side of the ribs (3) faces the arc-shaped structure area, and the downstream side of the ribs (3) faces the opening of the second pipeline, and a plurality of micro grooves are formed between the fins (2).
5. The device for detecting raw and auxiliary materials for brewing liquor according to claim 4, characterized in that: The edges of the fins (2) are made of elastic material, and the surfaces of the fins (2) are coated with a fluorinated nano coating.
6. The device for detecting raw and auxiliary materials for brewing liquor according to claim 1, characterized in that: The controller is used to receive the type of gas entering the air inlet chamber (4), and to cut off the power of the electromagnets (1) in a designated position area based on the type of gas in the air inlet chamber (4), and to cut off the power of a designated number of electromagnets (1) based on the concentration of the mixed and diluted sample gas or reference gas.
7. The device for detecting raw and auxiliary materials for liquor brewing according to claim 6, characterized in that: The controller is also used to adjust the current of the electromagnet (1) based on the flow rate of gas entering the air inlet cavity (4) and the flow rate of gas introduced into the detection system (600) through the second pipeline.
8. The device for detecting raw and auxiliary materials for brewing liquor according to claim 1, characterized in that: A groove (6) is provided on the surface of the fin (2) facing the air inlet cavity (4), the groove (6) is located on the tail side of the fin (2), the magnetic attraction member (7) is arranged in the groove (6), and the distance from the rotation connection between the fin (2) and the fixed bracket (5) to the tail of the fin (2) is greater than the distance between adjacent fixed brackets (5).
Citation Information
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