CN114487959B - Ultra-low field nuclear magnetic resonance measurement device and method - Google Patents
Ultra-low field nuclear magnetic resonance measurement device and method Download PDFInfo
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- CN114487959B CN114487959B CN202210093852.4A CN202210093852A CN114487959B CN 114487959 B CN114487959 B CN 114487959B CN 202210093852 A CN202210093852 A CN 202210093852A CN 114487959 B CN114487959 B CN 114487959B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
- G01R33/44—Arrangements or instruments for measuring magnetic variables involving magnetic resonance using nuclear magnetic resonance [NMR]
- G01R33/46—NMR spectroscopy
- G01R33/4608—RF excitation sequences for enhanced detection, e.g. NOE, polarisation transfer, selection of a coherence transfer pathway
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
- G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
- G01R33/30—Sample handling arrangements, e.g. sample cells, spinning mechanisms
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
- G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
- G01R33/30—Sample handling arrangements, e.g. sample cells, spinning mechanisms
- G01R33/31—Temperature control thereof
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
- G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
- G01R33/38—Systems for generation, homogenisation or stabilisation of the main or gradient magnetic field
- G01R33/387—Compensation of inhomogeneities
- G01R33/3875—Compensation of inhomogeneities using correction coil assemblies, e.g. active shimming
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
- G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
- G01R33/42—Screening
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Abstract
The invention discloses an ultralow field nuclear magnetic resonance measuring device which comprises eight connectors, optical fibers, a magnetic shielding box, a sampling sleeve, a sleeve tail light pump chamber, a double-group triaxial vector magnetic field coil, four pipelines, two atomic magnetic sensing modules, an optical fiber coupling collimator, a power supply/control module, a double-path control/data module and four vacuum valves, and is matched with a gas polarizer. The device has small volume and can realize real-time precise measurement. The invention also discloses an ultra-low field nuclear magnetic resonance measurement method, which utilizes the gas polarizer, and simultaneously uses two atomic magnetic sensing modules to respectively measure and compare the standard sample of the tail light pump chamber of the sleeve and the parameters of the laser polarized gas from the gas polarizer, so that the gas polarizer can better provide the laser polarized gas with optimized parameters, and the method is applied to the fields of magnetic resonance imaging of the lung or brain of an organism, surface enhancement of a chemical sample, aperture measurement of a material sample, nano material identification and the like.
Description
Technical Field
The invention relates to the fields of gas nuclear magnetic resonance signal enhancement, ultra-low field formed by magnetic shielding, nuclear polar moment magnetic field measurement, quantum magnetic sensor device application and the like, in particular to an ultra-low field nuclear magnetic resonance measurement device and an ultra-low field nuclear magnetic resonance measurement method, which are suitable for acquiring relevant parameters of laser polarized inert gas in real time.
Background
The "optical pump+collisional spin exchange" method is also known as spin-exchange optical pump (spin-exchangeoptical pumping, SEOP) method. It can effectively enhance the nuclear spin polarization of inert gas [ Navon G et al.science,1996,271:1848], for example, xenon-129 as one of inert gas, and by SEOP, the nuclear spin polarization can be enhanced by 10 5 times, which greatly improves the detection sensitivity of nuclear magnetic resonance signals, and is therefore called laser polarized xenon (or hyperpolarized xenon). Typically, laser polarized gases are used as "contrast agents" in the fields of biological lung, brain magnetic resonance spectroscopy, and imaging, as "probes" in the fields of chemical sample surface enhancement, material sample pore size measurement, and nanomaterial discrimination.
Gas polarizers are instruments that produce laser polarized gas, typically operating in either a continuous-flow (flow) or batch mode. For flow patterns [ Korchak S Eet al. Appl Magn Reson,2013,44 (1): 65-80 ], the control valves in front of and behind the optical pump cell are always open, and when the alkali metal vapor in the optical pump cell is irradiated with a high-power laser, a working gas (e.g., "xenon+nitrogen+helium" working gas) continuously flows through the optical pump cell, and after the gaseous xenon is collisional spin-exchanged with the polarized alkali metal atoms, the xenon nuclei are highly polarized and continuously flow out of the gas polarizer. For the intermittent mode [ Nikolaou P et al.J Phys Chem B,2014,118 (18): 4809-4816 ], control valves before and after the optical pump cell are controlled as required, when the working gas fills the optical pump cell, the laser irradiates alkali metal atom vapor in the optical pump cell, polarized alkali metal atoms and gaseous xenon undergo collision spin exchange for a period of time (typically, 20-30 min), the establishment of the nuclear spin polarization of the gaseous xenon is completed, and a high polarization balance is reached in the optical pump cell, and then all flows out of the gas polarizer at one time. Currently, both modes of operation gas polarizers are capable of providing high capacity, highly nuclear spin polarized laser polarized gas for the application requirements. For the application of magnetic resonance imaging of human lung gas, a mode of 'flow mode gas polarizer + solid state accumulation reservoir + thermal sublimator' is generally selected to be used, so that laser polarized gas becomes a 'contrast agent' which is convenient to use.
Because the structural design, component combination, working state, etc. of the gas polarizer may affect the generation of high-capacity and high-polarization laser polarized gas, in order to further improve the gas polarizer, the working parameters of the gas polarizer need to be continuously adjusted and optimized in the use process, and whether the generated laser polarized gas is suitable for the application environment or not is determined, so that the measurement of the laser polarized gas parameters is essential. In addition to the use of adiabatic fast-passing methods of photodetection and methods of measuring alkali metal atom zeeman resonance frequency shift in early studies, a variety of techniques and methods have been used to measure important parameters such as nuclear spin polarization setup time, nuclear magnetic resonance signal enhancement factor, relaxation rate of laser polarized gas, and it is generally preferred to directly measure using a magnetic resonance spectrometer or a magnetic resonance imager, among applications in a variety of fields of interest. For example, (1) a low field (tens to hundreds Gauss) or commercial electromagnet magnetic field (-1.8T magnetic field strength) spectrometer measurement method, wherein laser polarized gas generated by a gas polarizer flows into a sampling tube placed in a low field spectrometer magnet measurement area through a connected glass tube or teflon tube, and is measured after equilibrium is reached; (2) In the magnetic resonance imaging (animal 4.7T, 7.0T, or human 1.5T, 3.0T magnetic field intensity) measuring method, laser polarized gas generated by a gas polarizer is input into a sampling container (glass tube or Teflon air bag), and then is put into a nuclear magnetic resonance measuring area of a superconducting magnet of the magnetic resonance imaging instrument for measurement. Note that the technical problems presented here are: a) For the measurement mode of the laser polarized gas parameters, a sampling container is firstly used for filling sample water as a thermal polarization standard sample, or high-pressure (about several atm) gas (for example, xenon) and oxygen are packaged as the thermal polarization standard sample, and the measured thermal polarized water protons or the measured parameters of the thermal polarized xenon and the laser polarized gas are subjected to data processing and comparison, so that the nuclear spin polarization degree or nuclear magnetic resonance signal enhancement multiple of the laser polarized gas can be obtained. Namely: the method comprises the steps of sequentially carrying out thermal polarization standard sample measurement and nuclear magnetic resonance measurement of laser polarization gas, wherein the operation flow comprises the steps of putting the thermal polarization standard sample in, taking out the thermal polarization standard sample and putting the laser polarization gas sample in; b) In the measurement method of the human lung magnetic resonance imager, a radio frequency coil which is independently manufactured is used for respectively measuring a thermal polarization standard sample and a laser polarization gas parameter from a gas polarizer, and then the human lung magnetic resonance imaging is carried out by replacing the lung coil. Therefore, the complexity of the operation flow is increased, and the influence on the measurement accuracy of the laser polarized gas parameters is brought.
Therefore, a novel device and a novel method for measuring the laser polarization gas parameters are developed, the problems are overcome, the measuring method is simpler, the process is more convenient, the result is more accurate, and the device and the method have important practical values.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides an ultralow field nuclear magnetic resonance measuring device and an ultralow field nuclear magnetic resonance measuring method.
Under the condition that the normal operation of the gas polarizer is not affected, the invention utilizes the related functional modules-1-to respectively provide air heating and laser pumping for the tail light pump chamber of the sleeve; (2) Providing vacuum environment and laser polarized gas for the sampling sleeve respectively; (3) Respectively controlling a power supply/control module and a two-way control/data module; and operating the two atomic magnetic sensing modules in an ultra-low field (< 0.1 μt) environment, conveniently precisely measuring in real time a plurality of parameters (e.g., nuclear spin polarization setup time, nuclear magnetic resonance signal enhancement factor, relaxation rate, etc.) of the laser polarized gas generated by the gas polarizer.
In order to achieve the above object, the present invention adopts the following technical measures:
The ultra-low field nuclear magnetic resonance measuring device comprises a gas polarizer, wherein a first connector, an eighth connector, a seventh connector and a sixth connector are arranged on the gas polarizer, and the first connector, a first pipeline, a second connector and an inner pipe of a sleeve tail light pump chamber are sequentially connected; the eighth connector, the second pipeline, the third connector and the outer pipe of the sleeve tail light pump chamber are sequentially connected; one end of the optical fiber is connected with the gas polarizer, and the other end of the optical fiber is connected with the optical fiber coupling collimator arranged on the inner tube of the sleeve tail light pump chamber; the double-group triaxial vector magnetic field coil is externally provided with a magnetic shielding box, a first atomic magnetic sensing module and a second atomic magnetic sensing module are internally provided with the magnetic shielding box, and a measuring chamber of the sampling sleeve and an optical pump chamber of a sleeve tail optical pump chamber are respectively positioned above the first atomic magnetic sensing module and the second atomic magnetic sensing module; one end of a computer control/data cable is connected with the gas polarizer, the other end of the computer control/data cable is respectively connected with the power supply/control module and the double-path control/data module, the double-path control/data module is respectively connected with the first atomic magnetic sensing module and the second atomic magnetic sensing module through the double-path control/data cable, and the power supply/control module is connected with the double-group triaxial vector magnetic field coils through the power supply/control cable; the third pipeline is provided with a first vacuum valve and is connected with the outer pipe of the sampling sleeve through a fourth connector; the fourth pipeline is the four-way pipeline, and the fourth pipeline includes four lateral pipelines, is first lateral pipeline, second lateral pipeline, third lateral pipeline respectively, and fourth lateral pipeline, and first lateral pipeline passes through the fifth connector and is connected with sampling sheathed tube inner tube, and second vacuum valve, third vacuum valve and fourth vacuum valve are installed respectively to second lateral pipeline, third lateral pipeline, fourth lateral pipeline, and third lateral pipeline passes through the sixth connector and is connected with the gas polarizer, and fourth lateral pipeline passes through the seventh connector and is connected with the gas polarizer.
The gas polarizer comprises an optical pump pool module, a Helmholtz coil, a laser and optical module, a computer, a vacuum module, a gas output control module, an air heating and temperature control module and a gas purifying and distributing module,
The Helmholtz coil is arranged outside the optical pump pool module, laser L generated by the laser and the optical module is incident to the optical pump pool module, the laser L is output through an optical fiber, the optical pump pool module is also connected with the gas purification and distribution module, working gas Q RP is purified by the gas purification and distribution module and then is input into the optical pump pool module,
The air heating and temperature controlling module is used for controlling the temperature in the optical pump pool module, outputting hot air to the first connector and recovering the hot air from the eighth connector,
The gas output control module is connected with the optical pump pool module and is used for outputting laser polarized gas Q LP in the optical pump pool module to the sixth connector,
The vacuum module is respectively connected with the optical pump tank module and the seventh connector,
The computer is respectively connected with the Helmholtz coil, the laser, the optical module, the vacuum module, the gas output control module, the air heating and temperature control module, the gas purifying and distributing module and the computer control/data cable,
The alkali metal in the optical pump cell module is the same as the alkali metal in the optical pump chamber of the sleeve tail optical pump cell.
An ultra-low field nuclear magnetic resonance measurement method comprising the steps of:
Step 1, active magnetic field compensation is carried out by a computer in the gas polarizer through a power supply/control module operating a double-group triaxial vector magnetic field coil under the passive magnetic shielding action of a magnetic shielding box, so that an ultra-low field environment is formed in a nuclear magnetic resonance measurement area at the central position inside the magnetic shielding box;
Step 2, closing the first vacuum valve, the second vacuum valve and the third vacuum valve, opening the fourth vacuum valve, pumping the seventh connector, the fourth pipeline, the fifth connector, the sampling sleeve and the fourth connector to a vacuum state by a vacuum module in the gas polarizer, and then closing the fourth vacuum valve;
step 3, hot air provided by an air heating and temperature controlling module of the gas polarizer flows into the first connector and sequentially flows through the first pipeline, the second connector and the inner pipe of the sleeve tail light pump chamber to heat the sleeve tail light pump chamber, the hot air flows into the outer pipe of the sleeve tail light pump chamber and sequentially flows through the third connector, the second pipeline and the eighth connector and flows back into the gas polarizer;
Step 4, laser L from a laser and an optical module irradiates alkali metal atom vapor in a sleeve tail light pump chamber after passing through an optical fiber 2 and an optical fiber coupling collimator, and then polarized alkali metal atoms collide with mixed gas of xenon and nitrogen for spin exchange to obtain laser polarized gas, wherein a computer in the gas polarizer provides excitation pulse sequences for double groups of triaxial vector magnetic field coils through a power supply/control module, and the excitation pulse sequences are measured by a second atomic magnetic sensing module;
Step 5, opening a third vacuum valve, enabling laser polarized gas Q LP from a gas polarizer to flow through a sixth connector, a fourth pipeline and a fifth connector, entering an inner pipe of a sampling sleeve, closing the third vacuum valve, enabling a computer in the gas polarizer to provide an excitation pulse sequence for a double-group triaxial vector magnetic field coil through a power supply/control module, and enabling a first atomic magnetic sensing module to perform nuclear magnetic resonance measurement on the laser polarized gas Q LP in the sampling sleeve;
Step 6, after the measurement is completed, the nuclear spin of the laser polarized gas Q LP is recovered to a thermal equilibrium state to become hot polarized gas, and the hot polarized gas flows out from the third pipeline after the first vacuum valve is opened;
Step 7, closing the first vacuum valve, and repeating the step 2;
And 8, a computer in the gas polarizer obtains data measured by the first atomic magnetic sensing module and the second atomic magnetic sensing module through a two-way control/data module, compares and calculates the data, and obtains a measurement result of the Q LP parameter of the laser polarized gas.
Compared with the prior art, the invention has the following beneficial effects:
1. Providing a completely different mode from high-field or low-field nuclear magnetic resonance measurement by using a radio frequency coil, and measuring nuclear magnetic resonance signals and parameters of laser polarized gas in an ultra-low field (< 0.1 mu T) environment in real time by using an atomic magnetic sensing module, so that the method is faster;
2. compared with a low-field or high-field nuclear magnetic resonance measurement method, the magnetic shielding mode of the magnetic shielding box and the double-group triaxial vector magnetic field coil can realize smaller volume, lighter weight and more convenient integration with a gas polarizer or matched use without a magnet;
3. The sleeve tail light pump chamber fixed in the ultra-low field environment is used as a standard sample, so that a plurality of important parameters of laser polarized gas generated by the gas polarizer can be directly measured and compared in real time, and the method is simpler and more accurate;
4. The sleeve tail light pump chamber for preparing a plurality of samples with different proportions comprises alkali metal (cesium or rubidium) +mixed gas (xenon+nitrogen) with different gas pressure ratios, and the sleeve tail light pump chamber is calibrated in advance, so that the sleeve tail light pump chamber is suitable for the requirements of gas polarizers of various light pump types;
5. By means of the special designed gas polarizer partial functional module, the device of the invention is assisted to work, and special laser, temperature controller, vacuum module, computer and other instruments or equipment are not needed to be additionally configured, so that the whole structure is simpler.
Description of the drawings:
FIG. 1 is a schematic diagram of an ultra-low field nuclear magnetic resonance measurement apparatus;
In the figure: 1-a first connector; 2-optical fiber; 3-a magnetic shield box; 4-sampling a sleeve; 5-a cannula tail light pump chamber; 6-double groups of triaxial vector magnetic field coils; 7-a first pipe; 8-a second pipe; 9-a second connector; 10-a first atomic magnetic sensing module; 11-a second atomic magnetic sensor module; 12-a third connector; 13-an optical fiber coupling collimator; 14-power/control cable; 15-a power/control module; 16-computer control/data cable; 17-two-way control/data module; 18-two-way control/data cable; 19-a third conduit; 20-a first vacuum valve; 21-fourth connector; 22-a fifth connector; 23-fourth piping; 24-a second vacuum valve; 25-a third vacuum valve; 26-sixth connector; 27-a fourth vacuum valve; 28-seventh connector; 29-eighth connector; an L-laser; 101-gas polarizer.
FIG. 2 is a schematic diagram of a gas polarizer;
In the figure: 201-an optical pump cell module; 202-Helmholtz coils; 203-a laser and an optical module; 204-a computer; 205-vacuum module; 206-a gas output control module; 207-an air heating and temperature control module; 208-gas purification and distribution module; q RP -working gas; q LP -laser polarized gas; 101-gas polarizer.
Detailed Description
The present invention will be further described in detail below in conjunction with the following examples, for the purpose of facilitating understanding and practicing the present invention by those of ordinary skill in the art, it being understood that the examples described herein are for the purpose of illustration and explanation only and are not intended to limit the invention.
In the embodiment, the laser and optical module 203 in the gas polarizer 101 operates at a D1 line wavelength 894.6nm of an alkali metal cesium atom (or a D1 line wavelength 794.7nm of an alkali metal rubidium atom), and a laser light L is supplied thereto, and after passing through the optical fiber 2 and the optical fiber coupling collimator 13, the laser light L irradiates the ferrule tail light pump chamber 5 containing an alkali metal cesium (or rubidium) atom+a mixed gas (xenon+nitrogen).
The embodiment provides an ultra-low field nuclear magnetic resonance measurement device, under the normal working state that does not affect the normal generation of laser polarized gas Q LP by the gas polarizer 101, at the same time, part of modules in the gas polarizer 101 are allowed to bear the "second function", wherein: the air heating and temperature control module 207 provides air heating and temperature control for the sleeve tail pump chamber 5 to form an alkali metal cesium (or rubidium) atomic vapor density suitable for the SEOP; the laser and optical module 203 provides the laser L with proper power required by the optical pump alkali metal cesium (or rubidium) atomic vapor, the second atomic magnetic sensing module 11 samples the laser polarized xenon nuclear magnetic resonance signal and related parameters of the sleeve tail light pump chamber 5, and at this time, the sleeve tail light pump chamber 5 plays a role of a 'sample tube'; the vacuum module 205 provides a vacuum environment for the sampling sleeve 4, so that the gas output control module 206 can conveniently convey the laser polarized gas Q LP into the vacuum-cleaned sampling sleeve 4, and the first atomic magnetic sensing module 10 can sequentially perform nuclear magnetic resonance measurement on the laser polarized gas Q LP; the computer 204 respectively controls the power supply/control module 14 and the two-way control/data module 16 to realize active magnetic field compensation and finish respectively measuring and processing the laser polarized xenon of the sleeve tail light pump chamber 5 and the laser polarized gas Q LP data in the sampling sleeve 4; therefore, the device accurately measures and obtains a plurality of parameters such as the nuclear spin polarization establishment time, the enhancement multiple, the relaxation rate and the like of the laser polarization gas Q LP generated by the gas polarizer 101 in real time, so that the laser polarization gas Q LP with optimized parameters can be better applied to the fields such as magnetic resonance imaging of the lung or brain of an organism, surface enhancement of a chemical sample, pore diameter measurement of a material sample, nano material identification and the like.
An ultra-low field nuclear magnetic resonance measurement device of the embodiment comprises a first sleeve connector 1, an optical fiber 2, a magnetic shielding box 3, a sampling sleeve 4, a sleeve tail light pump chamber 5, a double-group triaxial vector magnetic field coil 6, a first pipeline 7, a second pipeline 8, a second connector 9, a first atomic magnetic sensing module 10, a second atomic magnetic sensing module 11, a third connector 12, an optical fiber coupling collimator 13, a power supply/control module 14, a power supply/control cable 15, a computer control/data module 16, a double-circuit control/data module 17, a double-circuit control/data cable 18, a third pipeline 19, a first vacuum valve 20, a fourth connector 21, a fifth connector 22, a fourth pipeline 23, a second vacuum valve 24, a third vacuum valve 25, a sixth connector 26, a fourth vacuum valve 27, a seventh connector 28, an eighth connector 29 and a gas polarizer 101.
The connection mode of the ultra-low field nuclear magnetic resonance measurement device in this embodiment is as follows: one end of the first connector 1 is connected with the gas polarizer 101, and the other end of the first connector 1, the first pipeline 7, the second connector 9 and the inner pipe of the sleeve tail light pump chamber 5 are sequentially connected; one end of the eighth connector 29 is connected with the gas polarizer 101, and the other end of the eighth connector 29, the second pipeline 8, the third connector 12 and the outer pipe of the sleeve tail light pump chamber 5 are sequentially connected; one end of the connecting optical fiber 2 is connected with the gas polarizer 101, and the other end is connected with the optical fiber coupling collimator 13 arranged on the inner tube of the sleeve tail light pump chamber 5; the double-group triaxial vector magnetic field coil 6 is externally provided with a magnetic shielding box 3, a first atomic magnetic sensing module 10 and a second atomic magnetic sensing module 11 are internally provided with the magnetic shielding box, and a measuring chamber of the sampling sleeve 4 and an optical pump chamber of the sleeve tail optical pump chamber 5 are respectively positioned above the first atomic magnetic sensing module 10 and the second atomic magnetic sensing module 11; one end of a computer control/data cable 16 is connected with the gas polarizer 101, the other end of the computer control/data cable is respectively connected with the power supply/control module 15 and the double-path control/data module 17, the double-path control/data module 17 is respectively connected with the first atomic magnetic sensing module 10 and the second atomic magnetic sensing module 11 through double-path control/data cables 18, and the power supply/control module 15 is connected with the double-group triaxial vector magnetic field coils 6 through the power supply/control cable 14; the third pipeline 19 is provided with a first vacuum valve 20 and is connected with the outer tube of the sampling sleeve 4 through a fourth connector 21; the fourth pipeline 23 is a four-way pipeline, and the fourth pipeline 23 includes four branch pipelines, namely a first branch pipeline, a second branch pipeline, a third branch pipeline and a fourth branch pipeline, wherein the first branch pipeline is connected with the inner pipe of the sampling sleeve 4 through a fifth connector 22, the second branch pipeline, the third branch pipeline and the fourth branch pipeline are respectively provided with a second vacuum valve 24, a third vacuum valve 25 and a fourth vacuum valve 27, the third branch pipeline is connected with the gas polarizer 101 through a sixth connector 26, and the fourth branch pipeline is connected with the gas polarizer 101 through a seventh connector 28.
The gas polarizer 101 includes an optical pump cell module 201, a helmholtz coil 202, a laser and optics module 203, a computer 204, a vacuum module 205, a gas output control module 206, an air heating and temperature control module 207, and a gas purification and distribution module 208.
The helm hertz coil 202 is arranged outside the optical pump tank module 201, laser L generated by the laser and the optical module 203 is incident to the optical pump tank module 201, the laser L is output through the optical fiber 2, the optical pump tank module 201 is further connected with the gas purification and distribution module 208, and working gas Q RP is purified by the gas purification and distribution module 208 and then is input into the optical pump tank module 201.
The air heating and temperature control module 207 is used for controlling the temperature in the optical pump cell module 201, and also for outputting hot air to the first connector 1 and recovering hot air from the eighth connector 29.
The gas output control module 206 is connected to the optical pump cell module 201, and the gas output control module 206 is configured to output the laser polarized gas Q LP to the sixth connection head 26 in the optical pump cell module 201.
The vacuum module 205 is connected to the optical pump cell module 201 and the seventh connector 28, respectively, and is used for evacuating the pipes connected to the optical pump cell module 201 and the sixth connector 26.
The computer 204 is connected with the Helmholtz coil 202 and the Helmholtz coil 202;
the computer 204 is connected with the laser and the optical module 203 and controls the laser and the optical module 203;
the computer 204 is connected with the vacuum module 205 and controls the start and stop of the vacuum module 205;
The computer 204 is connected with the gas output control module 206 and controls the start and stop of the gas output control module 206;
The computer 204 is connected with the air heating and temperature control module 207 and controls the start and stop of the air heating and temperature control module 207;
The computer 204 is connected to the gas purification and distribution module 208 and controls the start and stop of the gas purification and distribution module 208,
The computer 204 is connected with the two-way control/data module 17 and the power supply/control module 15 through the computer control/data cable 16 respectively, controls the acquisition of the first atomic magnetic sensing module 10 and the second atomic magnetic sensing module 11, and excites the double-group triaxial vector magnetic field coil 6 through the power supply/control module 15.
The first connector 1 is made of teflon and is used for connecting the first pipeline 7 and the gas polarizer 101.
The optical fiber 2, polarization maintaining fiber, has an operating wavelength that matches the atomic resonance line wavelength of alkali metal cesium (or rubidium), and for example, typically, an optical fiber having an operating wavelength of 894.6nm is used for alkali metal cesium (or an optical fiber having an operating wavelength of 794.7nm is used for alkali metal rubidium).
The magnetic shielding box 3 is of a typical 5-layer cylindrical structure, is made of 1-layer aluminum alloy and 4-layer permalloy, provides magnetic shielding in a passive mode, is matched with a double-group triaxial vector magnetic field coil 6, and is formed in an ultra-low field environment in the inner central area of the magnetic shielding box 3, and the residual magnetic field is typically-1 nT.
The sampling sleeve 4 is made of high borosilicate glass material and is manufactured by welding a measuring chamber and a sleeve, the measuring chamber is arranged at the front end of the sleeve, an inner pipe and an outer pipe of the sampling sleeve are respectively communicated with the measuring chamber, the measuring chamber is the same as an optical pump chamber of a sleeve tail optical pump chamber 5 in size, and the inner pipe and the outer pipe of the sleeve are respectively an inflow channel and an outflow channel of laser polarized gas Q LP.
The sleeve tail light pump chamber 5 is made of the same material as the sampling sleeve 4, is formed by welding two parts of a light pump chamber and a sleeve tail, wherein an inner pipe of the sleeve tail is connected with the gas polarizer 101 through the second connector 9 and the first pipeline 7 in sequence, an outer pipe of the sleeve tail is connected with the gas polarizer 101 through the third connector 12 and the second pipeline 8 in sequence, the inner pipe and the outer pipe of the sleeve tail are respectively connected with the light pump chamber, and alkali metal (cesium or rubidium) +mixed gas (xenon+nitrogen) is packaged in the light pump chamber according to the working wavelength of a laser and the optical module 203 in the gas polarizer 101; two sets of 6 respective sleeve light pump chambers 5 were prepared, including mixtures of different pressure ratios (xenon + nitrogen), the sleeve light pump chambers 5 having been previously calibrated (e.g., calibrated using a thermally polarized sample on a magnetic resonance spectrometer, and the relationship of laser polarized xenon nuclear magnetic resonance signals to laser power, gas pressure, heating temperature, etc.), and therefore the sleeve light pump chambers 5 were used herein as "sample tubes".
The double-group triaxial magnetic field coil 6 is wound in a cylindrical or square shape, is formed by laminating two independent triaxial magnetic field coils, and is used for actively compensating the magnetic field in the magnetic shielding box 3 and providing a pulse sequence for controlling the xenon nuclear spin.
The first pipe 7 is made of teflon, and serves as a passage for hot air to flow into the inner pipe of the sleeve tail light pump chamber 5, and the pipe wall has a heat insulation effect on the hot air flowing through.
The second duct 8 is made of the same material as the first duct 7 and serves as a passage through which the hot air flows out from the outer tube of the sleeve tail light pump chamber 5.
The second connector 9 is made of the same material as the first connector 1 and is used for connecting the first pipeline 7 and the inner pipe of the sleeve tail light pump chamber 5.
The first atomic magnetic sensor module 10, which is used in cooperation with the two-way control/data module 17, works in an ultra-low field environment inside the magnetic shielding box 3, and typically has a sensitivity of 10fT/Hz 1/2.
The sources and the control modes of the second atomic magnetic sensing module 11 are the same as those of the first atomic magnetic sensing module 10, and the working parameters and indexes of the second atomic magnetic sensing module 11 and the first atomic magnetic sensing module 10 are almost the same.
The third connector 12 is made of the same material as the first connector 1 and is used for connecting the second pipeline 8 and the outer pipe of the sleeve tail light pump chamber 5.
The optical fiber coupling collimator 13 has the same working wavelength as the optical fiber, and is used together with the optical fiber to couple and collimate the laser light from the optical fiber.
The power supply/control cable 14 is connected with the double-group triaxial vector magnetic field coil 6 and the power supply/control module 15 and is matched with the double-group triaxial vector magnetic field coil.
The power/control module 15 is matched with the double-group triaxial vector magnetic field coil 6 and provides power and operation pulses.
Computer control/data cable 16 connects computer 204 in gas polarizer 101 to power/control module 15 and two-way control/data module 17, respectively.
The two-way control/data module 17 is matched with the first atomic magnetic sensing module 10 and the second atomic magnetic sensing module 11 for use, and provides working conditions and data conversion.
A two-way control/data cable 18 connects the two-way control/data module 17 to the first atomic magnetic sensor module 10 and the second atomic magnetic sensor module 11, respectively.
The third conduit 19, which is the same material as the first connector 1, is the passage through which the laser polarized gas Q LP exits the device of the present invention. After the laser polarized gas Q LP flows through this conduit, it is delivered to the application environment or to a transition vessel. For example, when performing chemical sample surface enhancement, material sample pore size measurement, and nanomaterial discrimination applications, laser polarized gas Q LP is passed through it directly into the measurement chamber or container in which the sample is held; when the human lung magnetic resonance imaging is carried out, laser polarized gas Q LP flows through the device and is conveyed into a gas storage container or a solid-state storage; when performing magnetic resonance imaging of the rat lung, brain, laser polarized gas Q LP is delivered to the rat lung through this, and so on.
The materials of the first vacuum valve 20, the second vacuum valve 24, the third vacuum valve 25 and the fourth vacuum valve 27 are all teflon (or glass), and are consistent with the materials of the fourth pipeline 23, and the functions of the first vacuum valve, the second vacuum valve, the third vacuum valve and the fourth vacuum valve play a role of opening or closing valves in the pipeline.
The fourth connector 21 is made of the same material as the first connector 1 and is used for connecting the third pipeline 19 with the outer tube of the sampling sleeve 4.
The fourth conduit 23, which is made of teflon (or glass), is a channel through which the laser polarized gas Q LP from the gas polarizer 101 flows, and which is internally cleaned by providing a higher vacuum from the vacuum module 205 in the gas polarizer 101 during use.
The sixth connector 26 is made of the same material as the first connector 1, and the sixth connector 26 is connected to the gas output control module 206 in the gas polarizer 101, so as to connect the third branch pipe of the fourth pipe 23 to the gas output control module 206 in the gas polarizer 101.
The seventh connector 28 is made of the same material as the first connector 1, and the seventh connector 28 is connected to the vacuum module 205 in the gas polarizer 101, for connecting the fourth branch pipe of the fourth pipe 23 to the vacuum module 205 in the gas polarizer 101.
The eighth connector 29 is made of the same material as the first connector 1 and is used for connecting the second pipeline 8 to the gas polarizer 101;
The laser light L is provided by the laser and optical module 203 in the gas polarizer 101, is obtained by splitting the laser light with high power (in the order of hundred W) (typically, in the order of 10 mW), is guided by the optical fiber 2, is coupled to the collimator 13 via the optical fiber, and is used as an optical pump for alkali metal cesium (or rubidium) atoms in the optical pump chamber of the ferrule tail optical pump chamber 5;
The gas polarizer 101, which belongs to the prior art, works in a continuous-flow (continuous-flow) or batch (batch) mode, irradiates an alkali metal (cesium or rubidium) atom+unpolarized mixed gas (xenon+nitrogen+helium) Q RP with a high-power (typically 180W) laser, generates a high-capacity (typically-1L/h) high-nuclear spin-polarized (typically 25% -45%) laser polarized gas Q LP through a SEOP, and can meet the application fields of magnetic resonance imaging, chemical sample surface enhancement, material sample pore diameter measurement, nano material identification and the like of the lung or brain of an organism.
An ultra-low field nuclear magnetic resonance measurement method comprising the steps of:
Step 1, by the passive magnetic shielding effect of the magnetic shielding box 3 and the active magnetic field compensation performed by the computer 204 in the gas polarizer 101 operating the double-group tri-axial vector magnetic field coil 6 through the power/control module 15, the nuclear magnetic resonance measuring area at the central position inside the magnetic shielding box 3 forms an ultra-low field environment, and typically, the residual magnetic field is 10nT;
Step 2, closing the first vacuum valve 20, the second vacuum valve 24 and the third vacuum valve 25, opening the fourth vacuum valve 27, pumping the seventh connector 28, the fourth pipeline 23, the fifth connector 22, the sampling sleeve 4 and the fourth connector 21 to a vacuum state of-10 -3 Pa by the vacuum module 205 in the gas polarizer 101, and then closing the fourth vacuum valve 27;
Step 3, under the condition that the gas polarizer 101 works normally, hot air provided by the air heating and temperature control module 207 flows into the first connector 1 and sequentially flows through the first pipeline 7, the second connector 9 and the inner pipe of the sleeve tail light pump chamber 5 to heat the sleeve tail light pump chamber 5, and sequentially flows into the outer pipe of the sleeve tail light pump chamber 5, sequentially flows through the third connector 12, the second pipeline 8 and the eighth connector 29 and flows back into the gas polarizer 101, and the sleeve tail light pump chamber 5 can be controlled to a proper working temperature (typically, the temperature range is 310-360K) by adjusting the flow rate of the hot air;
step 4, at this time, after passing through the optical fiber 2 and the optical fiber coupling collimator 13, the laser L (typically, -15 mW) from the laser and the optical module 203 irradiates the alkali metal (cesium or rubidium) atomic vapor in the ferrule tail-light pump chamber 5, and then the polarized alkali metal (cesium or rubidium) atomic collides with the mixed gas (xenon+nitrogen) to perform spin exchange to obtain the laser polarized gas (laser polarized xenon), at this time, the computer 204 in the gas polarizer 101 provides the excitation pulse sequence for the dual-set triaxial vector magnetic field coil 6 through the power/control module 15, and the second atomic magnetic sensing module 11 performs measurement, because the laser polarized xenon parameter in the ferrule tail-light pump chamber 5 is calibrated in advance, and the obtained nuclear magnetic resonance measurement data is used for reference or comparison;
Step 5, opening a third vacuum valve 25, enabling laser polarized gas Q LP from the gas polarizer 101 to flow through a sixth connector 26, a fourth pipeline 23 and a fifth connector 22 and enter an inner tube of the sampling sleeve 4, then closing the third vacuum valve 25, enabling a computer 204 in the gas polarizer 101 to provide an excitation pulse sequence for the double-group triaxial vector magnetic field coil 6 through a power supply/control module 15, and enabling the first atomic magnetic sensor module 10 to perform nuclear magnetic resonance measurement on the laser polarized gas Q LP in the sampling sleeve 4;
Step 6, after the measurement is completed, the nuclear spin of the laser polarized gas Q LP is recovered to a thermal equilibrium state to become a thermal polarized gas, and the first vacuum valve 20 is opened, so that the thermal polarized gas flows out of the device of the invention from the third pipeline 19;
Step 7, then, closing the first vacuum valve 20, and repeating the step 2;
in step 8, the computer 204 in the gas polarizer 101 obtains the data measured by the first atomic magnetic sensing module 10 and the second atomic magnetic sensing module 11 through the two-way control/data module 17, and performs comparison and calculation processing, thereby obtaining an accurate measurement result of the parameter of the laser polarized gas Q LP of the gas polarizer 101, and the above process of obtaining the accurate measurement result of the parameter of the laser polarized gas Q LP according to the data processing measured by the first atomic magnetic sensing module 10 and the second atomic magnetic sensing module 11 is a prior art and is not repeated herein.
When it is desired to measure multiple parameters of the laser polarized gas Q LP, then steps 2, 5, 6, 7 and 8 can be repeated.
When the laser polarized gas Q LP generated by the gas polarizer 101 is continuously supplied to the application environment through the sampling sleeve 4, nuclear magnetic resonance measurement can be directly performed on the flowing laser polarized gas Q LP multiple times.
As described above, the nuclear magnetic resonance measurement of the laser polarized gas Q LP in the ferrule boot 5 and the sampling ferrule 4 may be performed separately or simultaneously.
The sleeve tail light pump chamber 5 is formed by welding the sleeve and the light pump chamber together, the inner tube is a hot air inflow channel for heating the light pump chamber and a laser L incidence channel for irradiating the light pump chamber, and the outer tube is a hot air outflow channel.
The alkali metal (cesium or rubidium) in the optical pump chamber of the ferrule boot optical pump chamber 5 as described above remains the same as the alkali metal in the optical pump cell module 201 in the gas polarizer 101.
The use of the optical pump L for the ferrule end light pump chamber 5 as described above is provided by the laser and optical module 203 in the gas polarizer 101, the wavelength of which always coincides with the alkali metal (cesium or rubidium) atomic resonance line used.
The sampling sleeve 4 is welded into a whole by the sleeve and the measuring chamber, the measuring chamber has the same size as the optical pump chamber of the sleeve tail optical pump chamber 5, and the inner pipe and the outer pipe of the sampling sleeve 4 are respectively designed into an inflow channel and an outflow channel of laser polarized gas Q LP.
The specific embodiments described in the specification are to be considered in all respects as illustrative and not restrictive. Various modifications or additions to the described embodiments may be made by those skilled in the art to which the invention pertains, or similar alternatives may be substituted without departing from the spirit of the invention or beyond the scope of the appended claims.
Claims (2)
1. The ultra-low field nuclear magnetic resonance measuring device comprises a gas polarizer (101), and is characterized in that a first connector (1), an eighth connector (29), a seventh connector (28) and a sixth connector (26) are arranged on the gas polarizer (101), and inner pipes of the first connector (1), a first pipeline (7), a second connector (9) and a sleeve tail light pump chamber (5) are sequentially connected; the eighth connector (29), the second pipeline (8), the third connector (12) and the outer tube of the sleeve tail light pump chamber (5) are connected in sequence; one end of the optical fiber (2) is connected with the gas polarizer (101), and the other end is connected with the optical fiber coupling collimator (13) arranged on the inner tube of the sleeve tail light pump chamber (5); the double-group triaxial vector magnetic field coil (6) is externally provided with a magnetic shielding box (3), a first atomic magnetic sensing module (10) and a second atomic magnetic sensing module (11) are internally provided with a measuring chamber of the sampling sleeve (4) and an optical pump chamber of the sleeve tail optical pump chamber (5) which are respectively positioned above the first atomic magnetic sensing module (10) and the second atomic magnetic sensing module (11); one end of a computer control/data cable (16) is connected with the gas polarizer (101), the other end of the computer control/data cable is respectively connected with the power supply/control module (15) and the double-path control/data module (17), the double-path control/data module (17) is respectively connected with the first atomic magnetic sensing module (10) and the second atomic magnetic sensing module (11) through double-path control/data cables (18), and the power supply/control module (15) is connected with the double-group triaxial vector magnetic field coil (6) through the power supply/control cable (14); the third pipeline (19) is provided with a first vacuum valve (20) and is connected with the outer pipe of the sampling sleeve (4) through a fourth connector (21); the fourth pipeline (23) is a four-way pipeline, the fourth pipeline (23) comprises four branch pipelines which are respectively a first branch pipeline, a second branch pipeline, a third branch pipeline and a fourth branch pipeline, the first branch pipeline is connected with the inner pipe of the sampling sleeve (4) through a fifth connector (22), the second branch pipeline, the third branch pipeline and the fourth branch pipeline are respectively provided with a second vacuum valve (24), a third vacuum valve (25) and a fourth vacuum valve (27), the third branch pipeline is connected with the gas polarizer (101) through a sixth connector (26), the fourth branch pipeline is connected with the gas polarizer (101) through a seventh connector (28),
The gas polarizer (101) comprises an optical pump tank module (201), a Helmholtz coil (202), a laser and optical module (203), a computer (204), a vacuum module (205), a gas output control module (206), an air heating and temperature control module (207) and a gas purifying and distributing module (208),
The Helmholtz coil (202) is arranged outside the optical pump tank module (201), laser L generated by the laser and the optical module (203) enters the optical pump tank module (201), the laser L is output through the optical fiber (2), the optical pump tank module (201) is also connected with the gas purification and distribution module (208), the working gas Q RP is input into the optical pump tank module (201) after being purified by the gas purification and distribution module (208),
The air heating and temperature control module (207) is used for controlling the temperature in the optical pump tank module (201), outputting hot air to the first connector (1) and recovering the hot air from the eighth connector (29),
The gas output control module (206) is connected with the optical pump tank module (201), the gas output control module (206) is used for outputting laser polarized gas Q LP to a sixth connector (26) in the optical pump tank module (201),
The vacuum module (205) is respectively connected with the optical pump tank module (201) and the seventh connector (28),
The computer (204) is respectively connected with the Helmholtz coil (202), the laser and optical module (203), the vacuum module (205), the gas output control module (206), the air heating and temperature control module (207), the gas purifying and distributing module (208) and the computer control/data cable (16),
The alkali metal in the optical pump tank module (201) is the same as the alkali metal in the optical pump chamber of the sleeve tail optical pump chamber (5),
The computer (204) of the gas polarizer (101) obtains the data measured by the first atomic magnetic sensing module (10) and the second atomic magnetic sensing module (11) through the two-way control/data module (17), and compares and calculates the data to obtain the measurement result of the parameters of the laser polarized gas Q LP.
2. An ultra-low field nuclear magnetic resonance measurement method using the ultra-low field nuclear magnetic resonance measurement apparatus according to claim 1, comprising the steps of:
Step 1, active magnetic field compensation is carried out by operating a double-group triaxial vector magnetic field coil (6) through a power supply/control module (15) by a computer (204) in a gas polarizer (101) through the passive magnetic shielding effect of a magnetic shielding box (3), so that an ultra-low field environment is formed in a nuclear magnetic resonance measurement area at the central position inside the magnetic shielding box (3);
Step2, closing the first vacuum valve (20), the second vacuum valve (24) and the third vacuum valve (25), opening the fourth vacuum valve (27), vacuumizing the seventh connector (28), the fourth pipeline (23), the fifth connector (22), the sampling sleeve (4) and the fourth connector (21) by a vacuum module (205) in the gas polarizer (101), and then closing the fourth vacuum valve (27);
Step 3, hot air provided by an air heating and temperature control module (207) of the gas polarizer (101) flows into the first connector (1) and sequentially flows through the first pipeline (7), the second connector (9) and the inner pipe of the sleeve tail light pump chamber (5) to heat the sleeve tail light pump chamber (5), the hot air flows into the outer pipe of the sleeve tail light pump chamber (5) and sequentially flows through the third connector (12), the second pipeline (8) and the eighth connector (29) and flows back into the gas polarizer (101);
Step 4, after laser L from a laser and an optical module (203) passes through an optical fiber (2) and an optical fiber coupling collimator (13), irradiating alkali metal atom vapor in a sleeve tail light pump chamber (5), then, carrying out collision spin exchange on polarized alkali metal atoms and mixed gas of xenon and nitrogen to obtain laser polarized gas, and providing an excitation pulse sequence for a double-group triaxial vector magnetic field coil (6) by a computer (204) in a gas polarizer (101) through a power supply/control module (15) and measuring by a second atomic magnetic sensing module (11);
Step 5, opening a third vacuum valve (25), enabling laser polarized gas Q LP from a gas polarizer (101) to flow through a sixth connector (26), a fourth pipeline (23) and a fifth connector (22) and enter an inner tube of a sampling sleeve (4), then closing the third vacuum valve (25), enabling a computer (204) in the gas polarizer (101) to provide excitation pulse sequences for the double-group triaxial vector magnetic field coils (6) through a power supply/control module (15), and enabling a first atomic magnetic sensing module (10) to perform nuclear magnetic resonance measurement on the laser polarized gas Q LP in the sampling sleeve (4);
Step 6, after the measurement is completed, the nuclear spin of the laser polarized gas Q LP is recovered to a thermal equilibrium state to become a thermal polarized gas, and the first vacuum valve (20) is opened, so that the thermal polarized gas flows out from the third pipeline (19);
step 7, closing the first vacuum valve (20), and repeating the step 2;
And 8, a computer (204) in the gas polarizer (101) obtains data measured by the first atomic magnetic sensing module (10) and the second atomic magnetic sensing module (11) through a two-way control/data module (17), compares and calculates the data, and obtains a measurement result of the parameters of the laser polarized gas Q LP.
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