CN112834547A - Nuclear magnetic resonance device - Google Patents
Nuclear magnetic resonance device Download PDFInfo
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- CN112834547A CN112834547A CN202011643558.3A CN202011643558A CN112834547A CN 112834547 A CN112834547 A CN 112834547A CN 202011643558 A CN202011643558 A CN 202011643558A CN 112834547 A CN112834547 A CN 112834547A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D23/00—Control of temperature
- G05D23/19—Control of temperature characterised by the use of electric means
- G05D23/1927—Control of temperature characterised by the use of electric means using a plurality of sensors
- G05D23/193—Control of temperature characterised by the use of electric means using a plurality of sensors sensing the temperaure in different places in thermal relationship with one or more spaces
- G05D23/1931—Control of temperature characterised by the use of electric means using a plurality of sensors sensing the temperaure in different places in thermal relationship with one or more spaces to control the temperature of one space
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D23/00—Control of temperature
- G05D23/19—Control of temperature characterised by the use of electric means
- G05D23/20—Control of temperature characterised by the use of electric means with sensing elements having variation of electric or magnetic properties with change of temperature
- G05D23/24—Control of temperature characterised by the use of electric means with sensing elements having variation of electric or magnetic properties with change of temperature the sensing element having a resistance varying with temperature, e.g. a thermistor
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D23/00—Control of temperature
- G05D23/19—Control of temperature characterised by the use of electric means
- G05D23/27—Control of temperature characterised by the use of electric means with sensing element responsive to radiation
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- Engineering & Computer Science (AREA)
- Automation & Control Theory (AREA)
- High Energy & Nuclear Physics (AREA)
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the technical field of nuclear magnetic resonance, in particular to a nuclear magnetic resonance device, which comprises: the liquid storage device is a sealing device, an air outlet is formed in the liquid storage device, the air outlet is communicated with an insulating pipeline, one end, close to the air outlet, of the insulating pipeline is provided with a pressure sensor, a heater is installed in the liquid storage device, a refrigerant medium is installed in the liquid storage device, and the refrigerant medium is liquid nitrogen or liquid helium; and one end of the warming pipeline is communicated with one end of the heat insulation pipeline, which is far away from the gas outlet, the other end of the warming pipeline is communicated with a sample chamber for placing a sample to be tested, a heating component is installed in the warming pipeline, a temperature sensor is installed in the sample chamber, and the temperature sensor is electrically connected with the heating component. The temperature control device comprises a temperature control device, a temperature control device and a temperature control device, wherein the temperature control device is used for controlling the temperature of the sample to be tested, and the temperature control device is used for controlling the temperature of the sample to be tested.
Description
Technical Field
The invention relates to the technical field of nuclear magnetic resonance, in particular to a nuclear magnetic resonance device.
Background
Meanwhile, with the deepening of various application researches, the nuclear magnetic resonance test of a sample in a specific high-temperature environment or a specific low-temperature environment can provide more physical property information of the sample. For example, a cross-linking density test of a rubber material in a high temperature environment, a glass transition temperature test of a polymer material in a low temperature environment, a pore structure test of a porous material in a low temperature environment, and the like. However, the temperature adjustment range of the nuclear magnetic resonance equipment in the prior art is limited, and when a sample needs to be tested in different temperature ranges, different equipment needs to be built so as to be carried out on different nuclear magnetic resonance equipment, so that the nuclear magnetic resonance testing cost is increased.
Disclosure of Invention
Therefore, the technical problem to be solved by the present invention is to overcome the defect of small temperature adjustment range of the nuclear magnetic resonance equipment in the prior art, thereby providing a nuclear magnetic resonance device.
In order to solve the above-described problems, the present invention provides a nuclear magnetic resonance apparatus including:
the liquid storage device is a sealing device, an air outlet is formed in the liquid storage device, the air outlet is communicated with an insulating pipeline, one end, close to the air outlet, of the insulating pipeline is provided with a pressure sensor, a heater is installed in the liquid storage device, a refrigerant medium is installed in the liquid storage device, and the refrigerant medium is liquid nitrogen or liquid helium;
and one end of the warming pipeline is communicated with one end of the heat insulation pipeline, which is far away from the gas outlet, the other end of the warming pipeline is communicated with a sample chamber for placing a sample to be tested, a heating component is installed in the warming pipeline, a temperature sensor is installed in the sample chamber, and the temperature sensor is electrically connected with the heating component.
Optionally, install coil skeleton in the sample room, coil skeleton includes from inside to outside overlap the chamber, skeleton body, thermal-insulated chamber and the coil body that holds of establishing in proper order, holds the axis collineation of chamber, skeleton body, thermal-insulated chamber and coil body, holds the chamber and is used for placing the sample that awaits measuring, and the pipeline that heaies up with hold the chamber intercommunication, temperature sensor locate and hold the intracavity.
Optionally, the heat insulation device further comprises an air suction pump, and an air suction end of the air suction pump is communicated with the heat insulation cavity.
Optionally, the heat insulation pipeline comprises an inner pipe and an outer pipe which are sleeved and connected, a heat insulation cavity is arranged between the inner pipe and the outer pipe in a sealing mode, an exhaust pipe is installed on the outer pipe, one end of the exhaust pipe is communicated with the heat insulation cavity, and the other end of the exhaust pipe is communicated with an exhaust end of the exhaust pump.
Optionally, the temperature sensor includes a first temperature sensor and a second temperature sensor, a temperature probe of the second temperature sensor is in contact with the sample to be measured to measure the temperature of the sample to be measured, and a temperature probe of the first temperature sensor is disposed away from the sample to be measured to measure the temperature of the gas in the sample chamber.
Optionally, the second temperature sensor is a fiber optic temperature sensor.
Optionally, a pressure switch is mounted on the air outlet, and a pressure relief valve is arranged on the pressure switch.
Optionally, a liquid level meter is installed in the liquid storage device.
Optionally, the temperature control device further comprises a temperature control assembly, and the heater, the temperature sensor and the heating assembly are all electrically connected with the temperature control assembly.
Optionally, the gas pump comprises a rotary vane vacuum pump and a molecular pump arranged in series.
The technical scheme of the invention has the following advantages:
1. the invention provides a nuclear magnetic resonance apparatus, comprising: the liquid storage device is a sealing device, an air outlet is formed in the liquid storage device, the air outlet is communicated with an insulating pipeline, one end, close to the air outlet, of the insulating pipeline is provided with a pressure sensor, a heater is installed in the liquid storage device, a refrigerant medium is installed in the liquid storage device, and the refrigerant medium is liquid nitrogen or liquid helium; and one end of the warming pipeline is communicated with one end of the heat insulation pipeline, which is far away from the gas outlet, the other end of the warming pipeline is communicated with a sample chamber for placing a sample to be tested, a heating component is installed in the warming pipeline, a temperature sensor is installed in the sample chamber, and the temperature sensor is electrically connected with the heating component.
When the temperature of the nuclear magnetic resonance device is adjusted, the liquid nitrogen or the liquid helium in the liquid storage equipment is heated by the heater, so that the cold medium liquid nitrogen or the liquid helium is evaporated into a gaseous state, the gaseous cold medium enters the heat insulation pipeline from the air outlet, the gaseous cold medium is heated to the temperature required to be used and then is introduced into the sample chamber from the heat insulation pipeline through the heating pipeline, and the gaseous refrigerant with constant temperature is continuously introduced into the sample chamber, so that the sample chamber is kept at the constant temperature, and a proper specific temperature is provided for sample testing. The low-temperature refrigerant gas in the heating pipeline is heated through the heating assembly, so that the refrigerant reaches the temperature required by the sample, and the real-time temperature in the sample chamber can be monitored by using the temperature sensor. Under the standard atmospheric pressure, the evaporation temperature of liquid nitrogen is-196 ℃, the evaporation temperature of liquid helium is-268.9 ℃, the temperature of liquid nitrogen or liquid helium after being evaporated into gas is near the respective evaporation temperature, gaseous cold medium substances close to the evaporation temperature are introduced into a sample chamber through an insulating pipeline and a heating pipeline, the gaseous cold medium substances can be heated and heated in the heating pipeline, so that different testing temperatures can be provided for different samples by using the same nuclear magnetic resonance device, the temperature of the samples is adjusted to the testing temperature, the testing temperature range which can be provided by the nuclear magnetic resonance device is wider, and the nuclear magnetic resonance device can be suitable for performing nuclear magnetic resonance testing on more types of samples at specific temperature.
2. According to the nuclear magnetic resonance device, the coil framework is installed in the sample chamber and comprises the accommodating cavity, the framework body, the heat insulation cavity and the coil body which are sequentially sleeved from inside to outside, the axes of the accommodating cavity, the framework body, the heat insulation cavity and the coil body are collinear, the accommodating cavity is used for placing a sample to be tested, the heating pipeline is communicated with the accommodating cavity, and the temperature sensor is arranged in the accommodating cavity. Utilize thermal-insulated chamber to hold chamber and external isolation, reduce and hold chamber and external heat exchange, avoid being close to the performance that holds the electron device in the chamber and change in the nuclear magnetic resonance device that leads to because temperature variation.
3. The temperature probe of the first temperature sensor is arranged far away from the sample to be measured so as to measure the temperature of the gas in the sample chamber. The temperature of the gas in the accommodating cavity and the temperature of the sample are respectively measured by utilizing the two temperature sensors, so that the control precision of the actual temperature of the sample is increased, and the accuracy of the measurement experiment result is ensured.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic diagram of a nuclear magnetic resonance apparatus according to an embodiment of the present invention.
Description of reference numerals: 1. a stainless steel dewar tank; 2. an insulating pipeline; 3. a pressure gauge; 4. a resistance heater; 5. liquid nitrogen; 6. a pressure switch; 7. a pressure relief valve; 8. a heating pipeline; 9. resistance heating wires; 10. an accommodating chamber; 11. a skeleton body; 12. a thermally insulating cavity; 13. a coil body; 14. a sample to be tested; 15. an air pump; 16. an air exhaust pipe; 17. a first temperature sensor; 18. a second temperature sensor; 19. a temperature control assembly; 20. a liquid level meter.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Fig. 1 shows a nuclear magnetic resonance apparatus provided in this embodiment, including: liquid storage equipment, a warming pipeline 8 and a sample chamber.
The liquid storage equipment is a low-temperature heat insulation container and is used for storing low-temperature liquid refrigerant medium, so that the refrigerant medium can exist stably, and the refrigerant medium is prevented from evaporating to the air to cause waste. The reservoir is in this embodiment a sealed stainless steel dewar 1. The liquid storage device is provided with an air outlet, the air outlet is communicated with an insulated pipeline 2, one end of the insulated pipeline 2 close to the air outlet is provided with a pressure gauge 3 serving as a pressure sensor, a heater is arranged in the liquid storage device, and the heater is a resistance heater 4. The liquid storage device is internally provided with a refrigerant medium, the refrigerant medium is liquid nitrogen 5 or liquid helium, and in the embodiment, the refrigerant medium is liquid nitrogen 5. Liquid nitrogen 5 can be deposited and keep the liquid state for a long time in stainless steel dewar 1, when needs utilize nitrogen gas to control the temperature, opens resistance heater 4 and begins to heat liquid nitrogen 5, makes the evaporation of liquid nitrogen 5 become low temperature nitrogen gas, keeps resistance heater 4's heating power unchangeable, can control the interior low temperature nitrogen gas air current that produces the flow stability constancy of temperature of stainless steel dewar 1. In order to ensure the safety of the liquid nitrogen 5 evaporation process, a pressure gauge 3 and a pressure switch 6 are installed on the gas outlet of the stainless steel Dewar flask 1, and a pressure release valve 7 is arranged on the pressure switch 6. The pressure gauge 3 is used for displaying the gas pressure at the gas outlet, the pressure switch 6 is used for cutting off the power supply of the resistance heater 4 when the gas pressure is too high so as to stop evaporation, and the pressure release valve 7 is used for exhausting and releasing pressure when the pressure is too high. A liquid level meter 20 is also installed in the liquid storage device to monitor the residual amount of the liquid nitrogen 5 in the stainless steel dewar 1. The range of the pressure gauge 3 exceeds 0-0.25 MPa. The trigger pressure of the pressure switch 6 is adjustable within 0-0.1 MPa, and is generally set within 0.08 MPa. The pressure of the safety pressure relief valve 7 is not more than 0.15 MPa.
One end of the warming pipeline 8 is communicated with one end, far away from the air outlet, of the heat insulation pipeline 2, the other end of the warming pipeline is communicated with a sample chamber for placing a sample 14 to be tested, a heating assembly is installed in the warming pipeline 8, and the heating assembly is a resistance heating wire 9. And a temperature sensor is arranged in the sample chamber and is electrically connected with the resistance heating wire 9. Install coil skeleton in the sample room, coil skeleton includes from inside to outside overlap in proper order establish hold chamber 10, skeleton body 11, thermal-insulated chamber 12 and coil body 13, holds the axis collineation of chamber 10, skeleton body 11, thermal-insulated chamber 12 and coil body 13, holds chamber 10 and is used for placing the sample 14 that awaits measuring, and the pipeline 8 that heaies up communicates with holding chamber 10, and temperature sensor locates and holds in the chamber 10. The heat insulation device also comprises an air extracting pump 15, and the air extracting end of the air extracting pump 15 is communicated with the heat insulation cavity 12. The heat insulation pipeline 2 is a stainless steel double-layer pipeline and comprises an inner pipe and an outer pipe which are sleeved and connected, a heat insulation cavity is arranged between the inner pipe and the outer pipe in a sealing mode, an exhaust pipe 16 is installed on the outer pipe, one end of the exhaust pipe 16 is communicated with the heat insulation cavity, and the other end of the exhaust pipe is communicated with an exhaust end of an exhaust pump 15. The air in the heat insulating chamber and the heat insulating chamber 12 is pumped out by the air pump 15, and the pressure in the heat insulating chamber and the heat insulating chamber 12 is controlled to be less than 1Pa, thereby ensuring the heat insulating effect of the heat insulating chamber and the heat insulating chamber 12. The air pump 15 includes a rotary vane vacuum pump and a molecular pump arranged in series, and the design limit pressure is of the order of 0.001 Pa. The low-temperature nitrogen is discharged from the air outlet of the stainless steel Dewar tank 1, then enters the heating pipeline 8 through the inner pipe of the heat insulation pipeline 2, and enters the accommodating cavity 10 after being heated in the heating pipeline 8 through the resistance heating wire 9.
The temperature sensor comprises a first temperature sensor 17 and a second temperature sensor 18, a temperature probe of the second temperature sensor 18 is contacted with the sample 14 to be measured so as to measure the temperature of the sample 14 to be measured, and a temperature probe of the first temperature sensor 17 is arranged far away from the sample 14 to be measured so as to measure the temperature of the gas in the sample chamber. The first temperature sensor 17 is a PT100 temperature sensor, uses A-level precision, has a temperature range of-200-450 ℃, and the second temperature sensor 18 is an optical fiber temperature sensor and needs linear current output of 4-20 mA.
The temperature control device further comprises a temperature control assembly 19, and the pressure switch 6, the resistance heater 4, the first temperature sensor 17, the second temperature sensor 18 and the resistance heating wire 9 are electrically connected with the temperature control assembly 19. The temperature control assembly 19 adopts an electrical control device, a PID temperature controller is arranged in the electrical control device, and the PID temperature controller is compatible with PT100 temperature sensor input and linear current 4-20 mA input. The heating power of the resistance heater 4 and the resistance heating wire 9 is controlled by a manual voltage regulating knob, and the output voltage of the resistance heater 4, the output voltage value of the resistance heating wire 9, the temperature reading of the first temperature sensor 17 and the temperature reading of the second temperature sensor 18 are respectively displayed on a display screen of the electric control device.
When the temperature of the nuclear magnetic resonance device is adjusted, the liquid nitrogen 5 or the liquid helium in the liquid storage equipment is heated by the heater, so that the cold medium liquid nitrogen 5 is evaporated to become gaseous low-temperature nitrogen, the low-temperature nitrogen enters the heat insulation pipeline 2 from the air outlet, the low-temperature nitrogen is heated to the temperature required to be used and then is introduced into the sample chamber through the heat insulation pipeline 2 and the heating pipeline 8, and the gaseous refrigerant with constant temperature is continuously introduced into the sample chamber, so that the sample chamber is kept at the constant temperature, and the proper specific temperature is provided for sample testing. The flow rate of air nitrogen is 30L/min, the temperature of the nitrogen at the air outlet is always lower than-150 ℃, the nitrogen introduced into the accommodating cavity 10 in the sample chamber can be accurately controlled within the temperature control range of-100 ℃ to 200 ℃ after being heated by the resistance heating wire 9, and the temperature control precision is +/-0.1 ℃.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A nuclear magnetic resonance apparatus, comprising:
the liquid storage device is a sealing device, an air outlet is formed in the liquid storage device, an insulating pipeline (2) is communicated with the air outlet, a pressure sensor is installed at one end, close to the air outlet, of the insulating pipeline (2), a heater is installed in the liquid storage device, a refrigerant medium is installed in the liquid storage device, and the refrigerant medium is liquid nitrogen (5) or liquid helium;
the temperature-raising device comprises a temperature-raising pipeline (8), one end of the temperature-raising pipeline (8) is communicated with one end, far away from the gas outlet, of the heat-insulating pipeline (2), the other end of the temperature-raising pipeline is communicated with a sample chamber used for placing a sample (14) to be measured, a heating assembly is installed in the temperature-raising pipeline (8), a temperature sensor is installed in the sample chamber, and the temperature sensor is electrically connected with the heating assembly.
2. The nuclear magnetic resonance device according to claim 1, wherein the coil skeleton is installed in the sample chamber, the coil skeleton comprises a containing cavity (10), a skeleton body (11), a heat insulation cavity (12) and a coil body (13) which are sequentially sleeved from inside to outside, the containing cavity (10), the skeleton body (11), the heat insulation cavity (12) and the coil body (13) are collinear in axis, the containing cavity (10) is used for placing a sample (14) to be tested, the warming pipeline (8) is communicated with the containing cavity (10), and the temperature sensor is arranged in the containing cavity (10).
3. The nmr device according to claim 2, further comprising a suction pump (15), wherein a suction end of the suction pump (15) is in communication with the insulated chamber (12).
4. The nuclear magnetic resonance device according to claim 3, wherein the heat insulation pipeline (2) comprises an inner pipe and an outer pipe which are sleeved and connected, a heat insulation cavity is arranged between the inner pipe and the outer pipe in a sealing mode, an air suction pipe (16) is installed on the outer pipe, one end of the air suction pipe (16) is communicated with the heat insulation cavity, and the other end of the air suction pipe is communicated with the air suction end of the air suction pump (15).
5. The NMR apparatus according to any of claims 1 to 4, wherein the temperature sensors comprise a first temperature sensor (17) and a second temperature sensor (18), the temperature probe of the second temperature sensor (18) being in contact with the sample (14) to be measured to measure the temperature of the sample (14) to be measured, the temperature probe of the first temperature sensor (17) being located remotely from the sample (14) to be measured to measure the temperature of the gas in the sample chamber.
6. The NMR apparatus of claim 5, wherein the second temperature sensor (18) is a fiber optic temperature sensor.
7. The NMR apparatus according to any of claims 1 to 6, wherein a pressure switch (6) is mounted on the gas outlet, and a pressure relief valve (7) is provided on the pressure switch (6).
8. The NMR apparatus of any of claims 1-7, wherein a liquid level gauge (20) is mounted in the reservoir.
9. The NMR apparatus according to any of claims 1 to 8, further comprising a temperature control assembly (19), wherein the heater, the temperature sensor, and the heating assembly are electrically connected to the temperature control assembly (19).
10. Nuclear magnetic resonance apparatus according to claim 3 or 4, characterized in that the suction pump (15) comprises a rotary-vane vacuum pump and a molecular pump arranged in series.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011643558.3A CN112834547A (en) | 2020-12-30 | 2020-12-30 | Nuclear magnetic resonance device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011643558.3A CN112834547A (en) | 2020-12-30 | 2020-12-30 | Nuclear magnetic resonance device |
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| Publication Number | Publication Date |
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| CN112834547A true CN112834547A (en) | 2021-05-25 |
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| CN202011643558.3A Pending CN112834547A (en) | 2020-12-30 | 2020-12-30 | Nuclear magnetic resonance device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023087729A1 (en) * | 2021-11-19 | 2023-05-25 | 苏州纽迈分析仪器股份有限公司 | Nuclear magnetic resonance coil structure and nuclear magnetic resonance device having same |
-
2020
- 2020-12-30 CN CN202011643558.3A patent/CN112834547A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023087729A1 (en) * | 2021-11-19 | 2023-05-25 | 苏州纽迈分析仪器股份有限公司 | Nuclear magnetic resonance coil structure and nuclear magnetic resonance device having same |
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