Nuclear magnetic resonance spectrometer probe for real-time detection of sample heat-moisture treatment process

Abstract

The utility model discloses a nuclear magnetic resonance spectrometer probe for real-time detection of a sample heat-moisture treatment process, which comprises a probe cylinder (1) and a sample bin (2) positioned in the probe cylinder (1), a sample to be tested is accommodated in the sample bin (2), the bottom of the probe cylinder (1) is provided with an airflow leading-in port (3), and the airflow leading-in port (3) is communicated with the probe cylinder (1). And air flow enters the probe cylinder (1) through the air flow inlet (3) and is in contact with a sample to be tested in the sample bin (2). According to the utility model, wet and hot airflow is introduced into the probe of the nuclear magnetic resonance spectrometer, so that on-line monitoring of the change rule of the proton relaxation spectrum of a sample in the processes of thermophysics, thermochemistry and the like under the conditions of specific temperature and humidity can be carried out on the premise of non-destructive pretreatment of the sample.

Description

Technical Field

[0001] The utility model relates to the field of tobacco processing technology, in particular to a nuclear magnetic resonance instrument probe used for real-time detection of a sample wet heat treatment process. Background Art

[0002] Nuclear magnetic resonance technology is an effective tool for qualitative or quantitative analysis of the composition, structure, and tissue morphology of the sample to be tested based on the proton's absorption level of radio frequency radiation. According to Bohr's quantum theory, each atom consists of a positively charged nucleus and a number of negatively charged electrons moving around the nucleus. The magnetic nucleus has a spin magnetic field. When there is no external magnetic field, the nuclear spin is disordered and the macroscopic magnetic moment of the spin system is zero; when there is an external magnetic field, the microscopic magnetic moment is arranged in order along the direction of the magnetic field and has a macroscopic magnetization intensity along the direction of the external magnetic field. When the external action stops, the non-equilibrium state of the spin system cannot be maintained and it recovers to the equilibrium state. The process of restoring the spin system from an unbalanced state to an equilibrium state is called a relaxation process, and the time required for the recovery process is the relaxation time. The difference in relaxation time can be used to distinguish the water storage form in the sample.

[0003] In the fields of biomass, food, medicine, tobacco, etc., raw materials will go through multiple wet heat treatment processes, such as common extraction, drying, moisture resurgence, baking, mildew protection, etc., and the moisture content of tobacco in each process changes nonlinearly and time-varyingly. In addition, under special conditions such as ocean transportation, high temperature and high humidity environment, storage and transportation, and shelf life product quality are closely related to environmental conditions. Therefore, studying the moisture storage form and migration process in the wet heat treatment process of samples, and revealing the migration laws of various forms of moisture in samples under specific environmental conditions from a molecular level, is of great significance to achieve precise control of wet heat treatment processing technology and improve product quality assurance capabilities.

[0004] The existing nuclear magnetic resonance technology can meet the needs of sample testing under room temperature conditions, but cannot realize the function of online monitoring of the proton relaxation spectrum of samples under a certain temperature and humidity environment, that is, it lacks the ability to evaluate the moisture storage form and migration process in the sample wet heat treatment process.

[0005] Therefore, it is desirable to use nuclear magnetic resonance technology to detect the moisture storage form and migration process in real time during the wet heat treatment process of samples.

[0006] In order to solve the above problems, the present utility model is proposed. Utility Model Content

[0007] The utility model introduces a moist hot air flow into the nuclear magnetic resonance instrument probe, and can realize on-line monitoring of the proton relaxation spectrum change law of the sample in the process of thermal physics, thermochemistry, etc. under specific temperature and humidity conditions under the premise of non-destructive sample pretreatment, thereby revealing the structure-activity relationship between the environmental conditions and the internal component migration and structural changes of the sample in each process, which is helpful to carry out environmental condition regulation and component migration process monitoring of the sample in a specific moist heat treatment process.

[0008] The utility model provides a nuclear magnetic resonance instrument probe for real-time detection of a sample wet heat treatment process, which includes a probe tube 1 and a sample compartment 2 located in the probe tube 1, wherein the sample compartment 2 contains a sample to be tested, and the bottom of the probe tube 1 has an airflow inlet 3, through which the wet heat airflow enters the probe tube 1 and contacts the sample to be tested in the sample compartment 2, so as to perform wet heat treatment on the sample. Thereby, real-time non-destructive monitoring of the moisture storage form of the sample during the wet heat treatment process is achieved. The wet heat airflow refers to a gas with a certain humidity and temperature, and the humidity and temperature of the wet heat airflow are determined according to actual needs during the specific test process.

[0009] Preferably, a heat-insulating layer 4 is provided on the outer side of the airflow inlet 3 to ensure that there is no heat loss when the airflow enters the probe tube 1 .

[0010] Preferably, the airflow inlet 3 is provided with a temperature sensor 5 and a humidity sensor 6. The temperature and humidity parameters of the hot and humid airflow entering the sample chamber are collected in real time by the temperature sensor and the humidity sensor, and the temperature and humidity parameters of the hot and humid airflow are fed back to the control unit, so as to adjust the temperature and humidity of the hot and humid airflow entering the sample chamber in real time, and ensure accurate and effective control of the test environment.

[0011] Preferably, the temperature sensor 5 and the humidity sensor 6 are fixed by a sensor fixing ring 12 and / or a sensor fixing tube 13. The fixing form of the sensor can be selected according to the actual situation.

[0012] Preferably, the chamber wall and / or bottom of the sample chamber 2 is provided with openings 7, and the airflow enters the sample chamber 2 through the openings 7 and contacts the sample to be tested in the sample chamber 2, so as to facilitate full contact between the sample and the external airflow, and more truly restore the gas-solid two-phase interaction state during the wet heat treatment process.

[0013] Preferably, the shape of the opening 7 includes but is not limited to a circle, a triangle or a quadrilateral.

[0014] Preferably, the probe tube 1 is further provided with a heat tracing aid 8 on one side close to the airflow inlet 3, and the heat tracing aid 8 can provide heat to prevent the humid hot airflow from condensing after entering the sample chamber 2, thereby ensuring that the humid hot gas and the sample to be tested can fully contact each other.

[0015] Preferably, the shape of the sample chamber 2 includes but is not limited to a cylinder, a cube, etc.

[0016] Preferably, the probe tube 1 also has an insulating tube 9 and a heat tracing tube 10 on its periphery. The insulating tube 9 is used to keep the hot and humid airflow in the probe tube 1 warm, while the heat tracing tube 10 is used to provide heat. The two tubes together ensure the temperature of the hot and humid airflow in the probe tube 1, thereby ensuring the temperature of the hot and humid airflow that enters the sample chamber 2 and contacts the sample to be tested. In addition, another function of the insulating tube 9 is to protect the magnet of the nuclear magnetic resonance instrument from being affected by the temperature of the hot and humid airflow in the probe tube, thereby ensuring that the magnet of the nuclear magnetic resonance instrument is in a reliable and stable operating state.

[0017] Preferably, the NMR probe further comprises a probe extension tube 11. In order to ensure that the hot and humid airflow can fully contact the sample to be tested in the sample chamber and ensure the stability of the test conditions, the length of the probe tube can be appropriately extended by the probe extension tube 11.

[0018] Preferably, the NMR probe also includes: probe frame cover plate, frame plate, sample chamber cover, sample chamber connecting rod, probe frame waveguide, probe frame waveguide cover, cap, positioning block and fixing device and other common parts of NMR probe. In addition, the NMR also includes other common parts such as magnets that generate magnetic fields in addition to the NMR probe.

[0019] Preferably, the nuclear magnetic resonance apparatus including the nuclear magnetic resonance apparatus probe further includes a control unit;

[0020] The air flow inlet 3 is provided with a temperature sensor 5 and a humidity sensor 6. The temperature sensor 5 and the humidity sensor 6 collect the temperature and humidity parameters of the air flow entering the sample chamber 2 in real time, and feed back the temperature and humidity parameters of the air flow to the control unit. The control unit controls the hot and humid air flow generating unit to adjust the temperature and humidity parameters of the generated hot and humid air flow in real time.

[0021] Preferably, the nuclear magnetic resonance instrument probe is in airflow communication with a humid hot airflow generating unit, and the humid hot airflow generating unit generates humid hot airflow according to set temperature and humidity parameters, and the humid hot airflow enters the sample chamber 2 through the airflow inlet 3 to contact the sample to be tested. The utility model does not limit the structure of the humid hot airflow generating unit, and any humid hot airflow generating unit that can generate humid hot airflow with the humidity and temperature required for the test can be applied to the utility model, and the structure of the humid hot airflow generating unit can be selected according to actual needs during the specific implementation process.

[0022] The airflow output by the moist and hot airflow generating unit is communicated with the nuclear magnetic resonance instrument probe of the utility model, so as to provide reliable environmental testing conditions for the samples in the sample chamber inside the probe.

[0023] Compared with the prior art, the utility model has the following beneficial effects:

[0024] 1. The utility model introduces a moist hot air flow into the nuclear magnetic resonance instrument probe, which can realize the online monitoring of the proton relaxation spectrum change law of the sample under specific temperature and humidity conditions during the thermal physical and thermal chemical processes without loss of sample pretreatment, thereby revealing the structure-activity relationship between the environmental conditions in each process and the internal component migration and structural changes of the sample, which is helpful for the environmental condition regulation and process monitoring of the sample moist heat treatment process in a specific process.

[0025] 2. The nuclear magnetic resonance probe of the utility model is particularly suitable for real-time detection of samples during the wet heat treatment process of the samples. The bottom of the probe tube of the nuclear magnetic resonance probe of the utility model has an airflow inlet, and the airflow enters the probe tube through the airflow inlet, and then enters the sample bin in the probe tube, and contacts the sample to be tested in the sample bin. The airflow inlet has airflow temperature and humidity monitoring. The nuclear magnetic resonance probe of the utility model can collect the temperature and humidity parameters of the wet and hot airflow entering the sample bin in real time through the temperature sensor and the humidity sensor, and feed back the temperature and humidity parameters of the wet and hot airflow to the control unit, so as to facilitate real-time regulation of the temperature and humidity of the wet and hot airflow entering the sample bin, and ensure accurate and effective control of the test environment.

[0026] 3. The airflow inlet of the nuclear magnetic resonance instrument probe of the utility model is also provided with a heat tracing auxiliary on one side, which can provide heat to prevent the humid hot airflow from condensing after entering the sample chamber, thereby ensuring that the humid hot gas and the sample to be tested can be in full contact.

[0027] 4. The probe tube of the nuclear magnetic resonance instrument probe of the utility model also has a heat insulation tube and a heat tracing tube on the periphery. The function of the heat insulation tube is to keep the hot and humid airflow in the probe tube warm, while the function of the heat tracing tube is to provide heat. The two together ensure the temperature of the hot and humid airflow in the probe tube, thereby ensuring the temperature of the hot and humid airflow that enters the sample chamber and contacts the sample to be tested. In addition, another function of the heat insulation tube is to protect the magnet of the nuclear magnetic resonance instrument from being affected by the temperature of the hot and humid airflow in the probe tube, ensuring that the magnet of the nuclear magnetic resonance instrument is in a reliable and stable operating state.

[0028] 5. The wall and / or bottom of the sample chamber of the nuclear magnetic resonance instrument probe of the utility model are provided with openings, and the airflow entering the probe tube can enter the sample chamber through the openings, so that the sample and the external airflow can be fully contacted, and the gas-solid two-phase interaction state during the wet heat treatment process can be more truly restored. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 Schematic diagram of the NMR probe structure.

[0030] Figure 2 Schematic diagram of the partial structure of the sample chamber of the nuclear magnetic resonance probe.

[0031] The figure marks in the accompanying drawings are: 1-probe tube, 2-sample chamber, 3-air flow inlet, 4-insulation layer, 5-temperature sensor, 6-humidity sensor, 7-opening, 8-heating auxiliary, 9-insulation pipe, 10-heating pipe, 11-probe extension tube, 12-sensor fixing ring, 13-sensor fixing tube. DETAILED DESCRIPTION

[0032] The utility model is further described in detail below in conjunction with the embodiments.

[0033] Those skilled in the art will understand that the following examples are only used to illustrate the present invention and should not be considered to limit the scope of the present invention. If no specific techniques or conditions are specified in the examples, the techniques or conditions described in the literature in the field or the product instructions are used. If the manufacturer of the materials or equipment used is not specified, they are all conventional products that can be purchased.

[0034] Those skilled in the art will appreciate that, unless expressly stated otherwise, the singular forms "a", "an", "said" and "the" used herein may also include plural forms. It should be further understood that the term "comprising" used in the specification of the present utility model refers to the presence of the features, integers, steps, operations, elements and / or components, but does not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or groups thereof. It should be understood that when we refer to an element as being "connected" to another element, it may be directly connected to the other element, or there may be intermediate elements. In addition, the "connection" used here may include wireless connection.

[0035] In the description of the present invention, unless otherwise specified, "plurality" means two or more than two. The terms "inside", "upper", "lower", etc., indicating positions or state relationships, are based on the positions or state relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific position, be constructed and operate in a specific position, and therefore cannot be understood as limiting the present invention.

[0036] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "provided with" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium. For ordinary technicians in this field, the specific meanings of the above terms in the present invention will be understood according to specific circumstances.

[0037] It will be understood by those skilled in the art that, unless otherwise defined, all terms used herein, including technical terms and scientific terms, have the same meaning as the general understanding of ordinary technicians in the field to which the utility model belongs. It should also be understood that those terms such as those defined in general dictionaries should be understood to have the same meaning as the meaning in the context of the prior art, and will not be interpreted with idealized or overly formal meanings unless defined as herein.

[0038] like Figure 1-2 As shown, the nuclear magnetic resonance instrument probe for real-time detection of the wet heat treatment process of the sample includes a probe tube 1 and a sample compartment 2 located in the probe tube 1, wherein the sample compartment 2 contains the sample to be tested, and the bottom of the probe tube 1 has an airflow inlet 3, through which the airflow enters the probe tube 1 and contacts the sample to be tested in the sample compartment 2, so as to perform wet heat treatment on the sample. Thereby, real-time non-destructive monitoring of the moisture storage form of the sample during the wet heat treatment process is achieved. The wet heat airflow refers to a gas with a certain humidity and temperature, and the humidity and temperature of the wet heat airflow are determined according to actual needs during the specific test process.

[0039] The airflow inlet 3 has a heat-insulating layer 4 on its outer side to ensure that there is no heat loss when the airflow enters the probe tube 1 .

[0040] The airflow inlet 3 is provided with a temperature sensor 5 and a humidity sensor 6. The temperature and humidity parameters of the hot and humid airflow entering the sample chamber are collected in real time by the temperature sensor and the humidity sensor, and the temperature and humidity parameters of the hot and humid airflow are fed back to the control unit, so as to adjust the temperature and humidity of the hot and humid airflow entering the sample chamber in real time, thereby ensuring accurate and effective control of the test environment.

[0041] The temperature sensor 5 and the humidity sensor 6 are fixed by a sensor fixing ring 12 and a sensor fixing tube 13 .

[0042] The sample chamber 2 is provided with openings 7 on the chamber wall and / or bottom, through which airflow enters the sample chamber 2 and contacts the sample to be tested in the sample chamber 2, so as to facilitate full contact between the sample and the external airflow, and more truly restore the gas-solid two-phase interaction state during the wet heat treatment process.

[0043] The opening 7 is circular.

[0044] The probe tube 1 is also provided with a heat tracing aid 8 on one side close to the airflow inlet 3 , which can provide heat to prevent the humid hot airflow from condensing after entering the sample chamber 2 , thereby ensuring that the humid hot gas and the sample to be tested can fully contact each other.

[0045] The sample chamber 2 is in the shape of a cylinder.

[0046] The probe tube 1 also has an insulation tube 9 and a heat tracing tube 10 on its periphery. The insulation tube 9 is used to keep the hot and humid airflow in the probe tube 1 warm, while the heat tracing tube 10 is used to provide heat. The two tubes together ensure the temperature of the hot and humid airflow in the probe tube 1, thereby ensuring the temperature of the hot and humid airflow that enters the sample chamber 2 and contacts the sample to be tested. In addition, another function of the insulation tube 9 is to protect the magnet of the nuclear magnetic resonance instrument from being affected by the temperature of the hot and humid airflow in the probe tube, thereby ensuring that the magnet of the nuclear magnetic resonance instrument is in a reliable and stable operating state.

[0047] The nuclear magnetic resonance instrument probe further includes a probe extension tube 11 .

Claims

1. A nuclear magnetic resonance probe for real-time detection of a sample during wet heat treatment, characterized in that: The invention comprises a probe tube (1) and a sample chamber (2) located in the probe tube (1); the sample chamber (2) contains a sample to be tested; the bottom of the probe tube (1) is provided with an air flow inlet (3); a moist hot air flow enters the probe tube (1) through the air flow inlet (3) and contacts the sample to be tested in the sample chamber (2).

2. The nuclear magnetic resonance probe according to claim 1, characterized in that: The airflow inlet (3) has a heat-insulating layer (4) on the outside.

3. The nuclear magnetic resonance probe according to claim 1, characterized in that: The air flow inlet (3) is provided with a temperature sensor (5) and a humidity sensor (6).

4. The nuclear magnetic resonance probe according to claim 3, characterized in that: The temperature sensor (5) and the humidity sensor (6) are fixed by a sensor fixing ring (12) and / or a sensor fixing cylinder (13).

5. The nuclear magnetic resonance probe according to claim 1, characterized in that: The sample chamber (2) is provided with an opening (7) on the chamber wall and / or the bottom, and airflow enters the sample chamber (2) through the opening (7) and contacts the sample to be tested in the sample chamber (2).

6. The nuclear magnetic resonance probe according to claim 1, characterized in that: The probe tube (1) also has a heat tracing auxiliary (8) on one side close to the airflow inlet (3).

7. The nuclear magnetic resonance probe according to claim 1, characterized in that: The probe tube (1) also has a heat insulation pipe (9) and a heating pipe (10) on its periphery.

8. The nuclear magnetic resonance probe according to claim 1, characterized in that: The nuclear magnetic resonance instrument probe also includes a probe extension tube (11).

9. The nuclear magnetic resonance probe according to claim 1, characterized in that: The nuclear magnetic resonance instrument including the nuclear magnetic resonance instrument probe further includes a control unit; The air flow inlet (3) is provided with a temperature sensor (5) and a humidity sensor (6), and the temperature sensor (5) and the humidity sensor (6) collect the temperature and humidity parameters of the air flow entering the sample chamber (2) in real time, and feed back the temperature and humidity parameters of the air flow to the control unit, and the control unit controls the hot and humid air flow generating unit to adjust the temperature and humidity parameters of the generated hot and humid air flow in real time.

10. The nuclear magnetic resonance probe according to any one of claims 1 to 9, characterized in that: The nuclear magnetic resonance instrument probe is in airflow communication with a moist hot airflow generating unit, and the moist hot airflow generating unit generates a moist hot airflow according to set temperature and humidity parameters, and the moist hot airflow enters the sample chamber (2) through the airflow inlet (3) and contacts with the sample to be tested.

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