CN113640721A - Sample bidirectional transmission device and method for low-field nuclear magnetic resonance spectrometer - Google Patents
Sample bidirectional transmission device and method for low-field nuclear magnetic resonance spectrometer Download PDFInfo
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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
- G01R33/307—Sample handling arrangements, e.g. sample cells, spinning mechanisms specially adapted for moving the sample relative to the MR system, e.g. spinning mechanisms, flow cells or means for positioning the sample inside a spectrometer
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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
- 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]
Abstract
The invention belongs to the field of sample transmission of low-field nuclear magnetic resonance, and particularly discloses a sample bidirectional transmission device and method for a low-field nuclear magnetic resonance spectrometer. The device includes first sample conveying system, second sample conveying system and detecting system, and first sample conveying system includes sample introduction pipe in first, the drive of first pneumatic appearance module, first sample capsule and first polarized magnet, and sample introduction pipe includes pneumatic appearance module of second, second sample capsule and polarized magnet in the second, and detecting system includes outer sample introduction pipe and weak magnetism detection sensor. The method comprises the steps of loading a sample, pre-polarizing the sample and acquiring and detecting signals. The invention has simple structure and convenient operation, adopts high temperature resistant materials, a multilayer heat insulation method and a high-performance damping technology, is suitable for carrying out the two-way transmission of the sample of magnetic resonance based on an atomic magnetometer method, can also be applied to the static magnetic field measurement based on low-field magnetic resonance, and can also be expanded to be used for the detection of gaseous nuclear magnetic samples.
Description
Technical Field
The invention belongs to the field of sample transmission of low-field nuclear magnetic resonance, and particularly relates to a sample bidirectional transmission device and method for a low-field nuclear magnetic resonance spectrometer.
Background
The pneumatic method is a general method for transmitting nuclear magnetic samples in a traditional high-field magnetic resonance spectrometer, the nuclear magnetic samples are transmitted to a detection area of the high-field spectrometer pneumatically, polarization of the nuclear magnetic samples and detection of magnetic resonance signals are completed in the same area in a superconducting magnet, and replacement and taking out of the nuclear magnetic samples are realized by pushing out the detection area pneumatically. In the low-field magnetic resonance research process, the pre-polarization area and the detection area need to be separated in space, the nuclear magnetic sample needs to be stably and quickly transferred between the pre-polarization area and the detection area for multiple times so as to reduce the loss of the polarization degree in the transfer process, and the nuclear magnetic sample is required to be constant in temperature so as to reduce the influence caused by the temperature change of the sample as much as possible.
There are several solutions for sample delivery to spectrometer devices in high and low field magnetic resonance studies, and some of the related articles and patents are exemplified by the following: US8212559 discloses a "NMR-MAS probe with integral transport device for an MAS-rotor" which describes that a sample-loaded NMR sample tube in a conventional high-field spectrometer is stably transported to a detection region of the NMR spectrometer by an air flow in a transport tube, and the NMR sample tube can be blown out of the detection region by reversing the air flow only when the sample is unloaded. The sample injection device described in Biancalana V et al, "A fast pneumatic sample-shunt with attached shocks", uses special openings on the sample injection tube and the sample injection slider to change the internal air flow to reduce the vibration of the nuclear magnetic sample tube during the sample injection process, but is not suitable for high temperature working environment. In addition, the chinese invention patent CN104807848B discloses a positioning sample injection method and device for a low-field magnetic resonance system, which provides a device that can directionally and non-rotatably transmit a nuclear magnetic sample tube to a laser and atom interaction detection region by using the constraint action of a non-circular sample injection tube.
In summary, the two nuclear magnetic samples cannot be simultaneously and effectively transferred to the detection region without mixing by using the existing sample injection method or technology. In order to increase the type of the nuclear magnetic sample for simultaneous sample introduction, improve the transmission efficiency of the nuclear magnetic sample, ensure the heat preservation performance of the nuclear magnetic sample and more effectively expand the function, the brand new sample bidirectional transmission method and device for the low-field nuclear magnetic resonance spectrometer, which have no physical contact between a sample introduction pipe and a multilayer magnetic shield as well as between weak magnetic detection sensors, are urgently needed to be developed.
Disclosure of Invention
Aiming at the defects or the improvement requirements of the prior art, the invention provides a sample bidirectional transmission device and a sample bidirectional transmission method for a low-field nuclear magnetic resonance spectrometer, which effectively transmit two nuclear magnetic samples to a detection area near a sealing partition plate at the same time under the condition of no mixing by utilizing the constraint action of an inner sample injection pipe, and are conveniently applied to low-field magnetic resonance research; a ventilation hole channel is arranged between the two inner sample introduction pipes and the outer sample introduction pipe, effective heat insulation can be realized by the double-layer framework, and the part of the outer sample introduction pipe, which is close to the detection area, is coated with a high-temperature-resistant heat-insulating material, so that the heat insulation effect can be further improved, and the temperature of the sample capsule can be kept; the outer sampling tube is supported and clamped by the sampling tube at the side surface of the weak magnetic detection sensor, the outer sampling tube is not in contact with the multilayer magnetic shielding and the weak magnetic detection sensor, and a damping sheet made of high-temperature silica gel or other materials with moderate elasticity and high temperature resistance can effectively play a damping role in the sample transmission process and reduce introduced technical noise; the outer coil can effectively reduce the leakage magnetic field and reduce the influence of the leakage magnetic field on the weak magnetic detection sensor; the sample capsule is made of nonmagnetic glass, can be fired by using a standard nuclear magnetic sample tube, is convenient to compare with a magnetic resonance signal obtained by a traditional high-field spectrometer, and can also be made of quartz or ceramics and other materials. The invention can be used for gaseous nuclear magnetic samples conveniently by a bidirectional sample transmission mode through simple modification.
In order to achieve the above object, according to one aspect of the present invention, there is provided a sample bidirectional transfer device for a low-field nuclear magnetic resonance spectrometer, comprising a first sample feeding system, a second sample feeding system and a detection system, wherein,
the first sample feeding system comprises a first inner sample feeding pipe, a first sample capsule driven by a first pneumatic sample feeding module is placed in the first inner sample feeding pipe, and a first polarizing magnet is arranged at the sample feeding end of the first inner sample feeding pipe and used for pre-polarizing a sample in the first sample capsule;
the second sample feeding system comprises a second inner sample feeding pipe, the second inner sample feeding pipe and the first inner sample feeding pipe are symmetrically arranged, a second sample capsule driven by a second pneumatic sample feeding module is placed in the second inner sample feeding pipe, and a second polarizing magnet is arranged at the sample feeding end of the second inner sample feeding pipe and used for pre-polarizing a sample in the second sample capsule;
detecting system advances appearance pipe and weak magnetism detection sensor including outer, and this advances appearance pipe is established along the axial cover advance the periphery of appearance pipe in first interior appearance pipe and the second, the periphery of advancing appearance pipe is provided with outer solenoid coil, and this outer solenoid coil is used for providing the precession magnetic field of sample, the periphery cover of outer solenoid coil is equipped with the magnetic field coil, outer solenoid coil periphery is provided with the multilayer magnetic screen, and this multilayer magnetic screen surrounds the detection area of regional formation sample, weak magnetism detection sensor is used for surveying the NMR signal of the weak magnetic field change that the sample produced in detecting the region.
As further preferred, outer introduction tube middle part inner wall is equipped with sealed partition, first interior introduction tube with sealed partition interval arrangement, second interior introduction tube with sealed partition interval arrangement, the both ends of outer introduction tube are equipped with the gas outlet, and with this mode outer introduction tube inner wall with form first vent between the first interior introduction tube outer wall outer introduction tube inner wall with form the second vent between the second interior introduction tube outer wall.
Preferably, a first damping sheet and a second damping sheet are respectively arranged on two side surfaces of the sealing partition plate, the first damping sheet is arranged on one side close to the gas outlet of the first inner sample inlet pipe, and the second damping sheet is arranged on one side close to the gas outlet of the second inner sample inlet pipe;
the first damping sheet and the second damping sheet are both made of high-temperature-resistant elastic materials. If first shock attenuation piece and second shock attenuation piece all adopt high temperature resistant silica gel to prepare and form, also can adopt other soft high temperature material, the moderate high temperature resistant material of elasticity such as silicon aerogel, graphite alkene aerogel of the big point of density.
As a further preferred option, the first sample sending system further includes a first air duct and a first air sealing block, the first air sealing block is used for packaging the sample introduction end of the first inner sample introduction tube, one end of the first air duct is connected with the first pneumatic sample introduction module, and the other end of the first air duct passes through the first air sealing block and is communicated with the first inner sample introduction tube;
the second sample conveying system further comprises a second air sealing block and a second air duct, the second air sealing block is used for packaging a sample introduction end of the sample introduction pipe in the second, one end of the second air duct is connected with the second pneumatic sample introduction module, and the other end of the second air duct penetrates through the second air sealing block and the sample introduction pipe in the second.
As a further preferred option, the two gas outlet end portions of the outer sampling tube are respectively provided with a first sampling tube support and a second sampling tube support, the first sampling tube support is disposed at one end close to the first polarized magnet, and the second sampling tube support is disposed at one end close to the second polarized magnet.
As further preferred, detecting system includes first precision power supply, second precision power supply and controller, first precision power supply is connected with the magnetic field coil, the second precision power supply with outer coil connection, the controller with first pneumatic appearance module, the pneumatic appearance module of second, first precision power supply, the precise power supply of second and weak magnetism detection sensor communication connection.
More preferably, the magnetic field coil is a three-axis helmholtz coil;
the first polarized magnet and the second polarized magnet are both magnets of a sea shell array structure;
the multilayer magnetic shield is permalloy.
As further preferred, first pneumatic appearance module and the same of second pneumatic appearance module structure all include air compressor, vacuum pump, first solenoid valve, second solenoid valve and pneumatic controller, air compressor is connected with first solenoid valve one end through first pipeline, the first solenoid valve other end passes through pipeline and second solenoid valve one end intercommunication, the second solenoid valve other end and vacuum pump connection, first solenoid valve and second solenoid valve all with pneumatic controller communication connection.
According to another aspect of the present invention, there is also provided a method for bidirectional transfer of a sample for a low-field nuclear magnetic resonance spectrometer, comprising the steps of:
s1 sample loading: sealing a sample A into a first sample capsule, placing the first sample capsule filled with the sample A into a first inner sample introduction pipe, sealing the sample introduction end of the first inner sample introduction pipe, sealing a sample B into a second sample capsule, placing the second sample capsule filled with the sample B into a second inner sample introduction pipe, and sealing the sample introduction end of the second sample capsule;
pre-polarization of the S2 sample: the first pneumatic sample feeding module drives the first sample capsule to the area where the first polarizing magnet is located in a pneumatic mode, so that the sample A stays for a preset time in the area where the first polarizing magnet is located to achieve pre-polarization of the sample A, and meanwhile, the second pneumatic sample feeding module drives the second sample capsule to the area where the second polarizing magnet is located in a pneumatic mode, so that the sample B stays for a preset time in the area where the second polarizing magnet is located to achieve pre-polarization of the sample B;
s3 signal acquisition detection: first pneumatic advance kind module adopts pneumatic mode will first sample capsule drive to detecting area, and the pneumatic appearance module of second adopts pneumatic mode will second sample capsule drive to detecting area, simultaneously, outer coil of wire provides precession magnetic field for sample A and sample B, and the magnetic field coil of the periphery of cover-mounted outer coil of wire provides corresponding magnetic field environment as required according to surveying, and weak magnetism detection sensor then simultaneously or respectively surveys the NMR signal of the weak magnetic field change that sample A and sample B produced in detecting area.
Further preferably, the method further comprises the following steps:
s4 sample change: opening the first pneumatic sample introduction module, sucking a first sample capsule loaded with a sample A to the position near the first air sealing block, taking down the first air sealing block, then taking out or replacing the first sample capsule, opening the second pneumatic sample introduction module, sucking a second sample capsule loaded with a sample B to the position near the second air sealing block, taking down the second air sealing block, and then taking out or replacing the second sample capsule.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. the invention utilizes the constraint action of the first inner sample inlet pipe and the second inner sample inlet pipe to simultaneously and effectively transmit the sample capsules filled with two non-mixed nuclear magnetic samples to the detection area near the sealing partition plate, thereby facilitating the simultaneous detection of the two non-mixed samples, still reusing the samples after the use to avoid waste, and respectively transmitting the two sample capsules to the detection area.
2. The invention can effectively transmit two mixed nuclear magnetic samples to a detection area near the sealing clapboard simultaneously by utilizing the constraint action of the two inner sample injection pipes, and can be applied to low-field magnetic resonance research.
3. The first inner sample introduction pipe and the second inner sample introduction pipe are made of high-temperature-resistant glass and are inserted into the outer sample introduction pipe made of high-temperature glass, and a vent hole is formed between the inner sample introduction pipe and the outer sample introduction pipe, so that gas in the process of conveying a sample capsule can flow, effective heat insulation is realized, the first inner sample introduction pipe and the second inner sample introduction pipe can effectively work in a self-selection exchange function inhibition (SERF) based atomic magnetometer, and the first inner sample introduction pipe and the second inner sample introduction pipe are conveniently used for temperature-changing experiments of sample research.
4. The invention adopts the double-layer structure of the outer sampling pipe and the inner sampling pipe to realize effective heat insulation, and the part of the outer sampling pipe, which is close to the detection area, is coated with the high-temperature-resistant heat-insulating material to increase the heat insulation effect so as to keep the temperature of the sample capsule, avoid the temperature change of the nuclear magnetic sample in the measurement process, and be suitable for the nuclear magnetic sample temperature change experiment.
5. The opening of the side cover of the magnetic shield facilitates the placement of the sample inlet pipe, the first inner sample inlet pipe and the second inner sample inlet pipe which are inserted into the outer sample inlet pipe are arranged on the side surface of the weak magnetic detection sensor, the bidirectional sample conveying device is easy to use and improve, the sample is convenient to replace, and the bidirectional sample conveying device can be conveniently applied to the research of gaseous nuclear magnetic samples through simple transformation and is more widely applied.
6. The outer sampling tube is supported and clamped by the first sampling tube and the second sampling tube, and the outer sampling tube is not in contact with the multilayer magnetic shielding and weak magnetic detection sensors, so that technical noise generated by vibration in sample transmission can be effectively reduced.
7. The magnetic field coil is a three-axis Helmholtz coil, can be used for further compensating residual static magnetic fields in a magnetic shield, or generating a simulation static magnetic field when weak static magnetic field measurement based on magnetic resonance is carried out, and can also be used for generating a pulse static magnetic field so as to control the spin state of a nuclear magnetic sample.
8. The first damping sheet and the second damping sheet fixed on the sealing partition plate are made of high-temperature-resistant and high-elasticity materials, such as high-temperature-resistant silica gel, so that the damping effect can be effectively realized, and the introduced technical noise is reduced.
9. The outer sample injection pipe is wound with the compact outer solenoid coil, and the solenoid coil can effectively reduce the leakage magnetic field and reduce the influence of the leakage magnetic field on the weak magnetic detection sensor.
10. The sample capsule is made of non-magnetic glass or ceramic materials, and can be fired by using a standard nuclear magnetic sample tube, so that the stability of the sample materials is effectively ensured, and the magnetic resonance signal is conveniently compared with a magnetic resonance signal obtained by a traditional high-field spectrometer.
In summary, the sample bidirectional transfer device for the low-field nuclear magnetic resonance spectrometer provided by the invention has the following advantages:
the invention has the characteristics of capability of simultaneously measuring various samples, good heat insulation, high transmission speed, easy expansion and application, cost saving and the like. Because the invention adopts high temperature resistant material, advanced multilayer heat insulation method and high-performance damping technology, the signal-to-noise ratio and the signal detection sensitivity can be further improved, the invention has wide application prospect and can more precisely measure the NMR signal of the nuclear magnetic sample.
Drawings
FIG. 1 is a schematic structural diagram of a sample bidirectional transfer device for a low-field nuclear magnetic resonance spectrometer according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of another sample bidirectional transfer device for a low-field nuclear magnetic resonance spectrometer according to an embodiment of the present invention;
fig. 3 is an operation schematic diagram of a sample bidirectional transfer device for a low-field nuclear magnetic resonance spectrometer according to an embodiment of the present invention, where [ a ] in fig. 3 is pre-polarization of a sample, [ B ] in fig. 3 is signal acquisition by applying a B-magnetic field, and [ C ] in fig. 3 is signal acquisition by applying a B + magnetic field.
In all the figures, the same reference numerals denote the same features, in particular: 1-a first airtight block, 2-a first inner sample feeding tube, 3-a first polarized magnet, 4-a first sample feeding tube support, 5-an outer coil of a solenoid, 6-an outer sample feeding tube, 7-a multilayer magnetic shield, 8-a first nonmagnetic sealing cover, 9-a first sample capsule, 10-a sealing clapboard, 11-a second sample capsule, 12-a second nonmagnetic sealing cover, 13-a magnetic field coil, 14-a second sample feeding tube support, 15-a second polarized magnet, 16-a second inner sample feeding tube, 17-a second airtight block, 18-a first air vent, 19-a first vibration-damping sheet, 20-a second vibration-damping sheet, 21-a second air vent, 31-a first air guide tube, 32-a second air guide tube, 33-a first pneumatic sample feeding module, 34-a second pneumatic sample injection module, 41-a first precision power supply, 42-a weak magnetic detection sensor and 43-a second precision power supply.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1 and fig. 2, a sample bidirectional transfer device for a low-field nuclear magnetic resonance spectrometer according to an embodiment of the present invention includes a first sample feeding system, a second sample feeding system, and a detection system, where the first sample feeding system includes a first inner sample feeding tube 2, a first sample capsule 9 driven by a first pneumatic sample feeding module 33 is placed in the first inner sample feeding tube 2, and a first polarizing magnet 3 is disposed at a sample feeding end of the first inner sample feeding tube 2, and is used to pre-polarize a sample in the first sample capsule 9. The second sample feeding system comprises a second inner sample feeding pipe 16, the second inner sample feeding pipe 16 and the first inner sample feeding pipe 2 are symmetrically arranged, a second sample capsule 11 driven by a second pneumatic sample feeding module 34 is placed in the second inner sample feeding pipe 16, and a second polarization magnet 15 is arranged at the sample feeding end of the second inner sample feeding pipe 16 and used for pre-polarizing samples in the second sample capsule 11. The first polarized magnet 3 and the second polarized magnet 15 are in a Halbach array structure with a hole in the middle, and the magnetic field intensity is 2 Tesla. The method is used for pre-polarization and establishes thermal polarization degree for the nuclear magnetic sample in the nuclear magnetic sample tube. In the invention, the detection system comprises an outer sample introduction pipe 6 and a weak magnetic detection sensor 42, the sample introduction pipe 6 is axially sleeved on the peripheries of the first inner sample introduction pipe 2 and the second inner sample introduction pipe 16, an outer coil 5 is arranged on the periphery of the sample introduction pipe 6, the outer coil 5 is used for providing a precession magnetic field of a sample, a magnetic field coil 13 is sleeved on the periphery of the outer coil 5, a multilayer magnetic shield 7 is arranged on the periphery of the outer coil 5, the area surrounded by the multilayer magnetic shield 7 forms a detection area of the sample, and the weak magnetic detection sensor 42 is used for detecting NMR signals of the weak magnetic field change generated by the sample in the detection area.
More specifically, in the present invention, a first sample capsule 9 is sealed by a first non-magnetic cover 8, and a second sample capsule 11 is sealed by a second non-magnetic cover 12. This first sample capsule 9 and second sample capsule 11 are no magnetic glass or ceramic material, can use the nuclear magnetic sample pipe of standard to fire, have effectively guaranteed like this that the sample material is stable, and the convenience is compared with the magnetic resonance signal that traditional high field spectrometer obtained.
The inner wall of the middle part of the sampling tube 6 is provided with a sealing clapboard 10, and the sealing clapboard 10 divides the sampling tube 6 into two uniform and symmetrical one-way tubes along the axial direction. The first inner sampling pipe 2 is inserted into one end of the sampling pipe 6, the second inner sampling pipe 16 is inserted into the other end of the sampling pipe 6, and the first inner sampling pipe 2 and the second inner sampling pipe 16 are symmetrically arranged. First interior appearance pipe 2 with sealed baffle 10 interval arrangement, second interior appearance pipe 16 with sealed baffle 10 interval arrangement, the both ends of outer appearance pipe 6 are equipped with the gas outlet, and with this mode, outer appearance pipe 6 inner wall with form first venthole 18 between the first interior appearance pipe 2 outer wall outer appearance pipe 6 inner wall with form second venthole 21 between the second interior appearance pipe 16 outer wall. In the invention, the first inner sample introduction pipe and the second inner sample introduction pipe are made of high-temperature-resistant glass, the two inner sample introduction pipes are inserted into the outer sample introduction pipe made of high-temperature glass, and a vent hole is arranged between the inner sample introduction pipe and the outer sample introduction pipe, so that gas in the process of conveying a sample capsule can enter and exit, the effective heat insulation is realized, and the self-selection exchange-function-based inhibition (SERF) atomic magnetometer can effectively work. Simultaneously, utilize the restriction effect of advancing appearance pipe in first and the second, can effectively convey the sample capsule that is equipped with two kinds of non-mixed nuclear magnetic samples to the detection zone near sealed baffle simultaneously, conveniently survey two kinds of non-mixed samples simultaneously, and the sample still can reuse and avoid extravagant after finishing using, and two sample capsules also can be conveyed respectively to the detection zone.
The first sample sending system further comprises a first air duct 31 and a first air sealing block 1, wherein the first air sealing block 1 is used for packaging a sample inlet end of the first inner sample inlet pipe 2, one end of the first air duct 31 is connected with the first pneumatic sample inlet module 33, and the other end of the first air duct penetrates through the first air sealing block 1 and the first inner sample inlet pipe 2 to be communicated. The second system of sending a sample still includes second airtight piece 17 and second air duct 32, second airtight piece 17 is used for the encapsulation sample inlet pipe 16's sampling end in the second, second air duct 32 one end with the pneumatic sample introduction module 34 of second is connected, and the other end passes second airtight piece 17 with sample inlet pipe 16 intercommunication in the second. In the present invention, the first air duct 31 and the second air duct 32 are made of teflon or common flexible plastic tube. The gas path is used for providing a high-pressure gas outflow channel.
In a preferred embodiment of the present invention, the sealing spacer 10 is provided with a first damping sheet 19 and a second damping sheet 20 on both sides thereof, and the first damping sheet 19 and the second damping sheet 20 are bonded to the sealing spacer 10 by using high temperature glue. The first damping sheet 19 is arranged at one side close to the gas outlet of the first inner sampling tube 2, and the second damping sheet 20 is arranged at one side close to the gas outlet of the second inner sampling tube 16. The first damping piece 19 and the second damping piece 20 are both made of high-temperature-resistant elastic materials. For example, high temperature resistant silica gel, or other soft high temperature materials, such as silica aerogel with large density, graphene aerogel and other materials with moderate elasticity and high temperature resistance. During the sample detection, the first sample capsule 9 can be resisted on the first shock absorption plate 19 during the operation of the first pneumatic sample injection module 33 and/or the second pneumatic sample injection module 34, namely, the first sample capsule can be stably stopped in the detection area within a specified time, and meanwhile, the second sample capsule 11 can be resisted on the second shock absorption plate 20 and can be stably stopped in the detection area within a specified time. The shock absorption sheet can effectively play a shock absorption role and reduce introduced technical noise. Of course, other damping pieces that do not interfere with the magnetic field environment are also suitable for use with the present invention.
In the present invention, a first sample inlet support 4 and a second sample inlet support 14 are respectively disposed at two gas outlet end portions of the outer sample inlet 6, the first sample inlet support 4 is disposed at an end close to the first polarizing magnet 3, and the second sample inlet support 14 is disposed at an end close to the second polarizing magnet 15. Meanwhile, one end of the outer coil 5 is fixed on the first sample tube support, and the other end is fixed on the second sample tube support.
The detection system comprises a first precise power supply 41, a second precise power supply 42 and a controller, wherein the first precise power supply 41 is connected with the magnetic field coil 13, the second precise power supply 42 is connected with the outer coil 5, and the controller is in communication connection with the first pneumatic sample injection module 33, the second pneumatic sample injection module 34, the first precise power supply 41, the second precise power supply 42 and the weak magnetic detection sensor 42. First pneumatic appearance module 33 and the pneumatic appearance module 34 structure of second are the same, all include air compressor, vacuum pump, first solenoid valve, second solenoid valve and pneumatic controller, air compressor is connected through first pipeline and first solenoid valve one end, the first solenoid valve other end passes through pipeline and second solenoid valve one end intercommunication, the second solenoid valve other end and vacuum pump connection, first solenoid valve and second solenoid valve all with pneumatic controller communication connection. The pneumatic sample introduction module controls the gas to enter and exit the inner sample introduction pipe, and controls the sample capsule to be rapidly and precisely transferred between the permanent magnet and the multilayer magnetic shielding. In practice, the first precision power supply 41, the weak magnetic detection sensor 42 and the second precision power supply 43 provide the required bidirectional magnetic detection function of the sample, so as to further realize the low-field nuclear magnetic resonance detection function.
In the preferred embodiment of the present invention, the material of the multi-layer magnetic shielding 7 is permalloy, which shields stray magnetic fields, etc., and provides a low magnetic field environment for nuclear magnetic sample detection.
When the device works, the computer drives the first sample capsule 9 and the second sample capsule 11 to respectively slide in the first inner sample inlet pipe 2 and the second inner sample inlet pipe 16 through the switching states of the first pneumatic sample inlet module 33 and the second pneumatic sample inlet module 34, so that the positioning and transmission of the nuclear magnetic sample between the central positions of the multi-layer magnetic shielding 7 of the polarizing magnet are realized. The pneumatic sample injection module is connected with the first inner sample injection pipe and the second inner sample injection pipe by using the gas guide pipe; the sealed clapboard 10 is used for controlling the sample capsule to reach the central position of the multilayer magnetic shielding, and the vibration of the sample feeding device is effectively reduced, so that the signal-to-noise ratio of the nuclear magnetic sample signal is improved. In practice, the weak magnetic detection sensor 42 is used to measure the NMR signal of the weak magnetic field change generated by the nuclear magnetic sample in the shielding box. The device has simple structure and convenient operation, and compared with the existing sample feeding device, the device realizes the bidirectional sample transmission and effective heat preservation of the nuclear magnetic sample.
According to another aspect of the present invention, there is also provided a bidirectional sample transfer method for a low-field nuclear magnetic resonance spectrometer, which specifically includes the following steps:
a) loading of the sample: and (2) filling the nuclear magnetic sample A to be detected into a first sample capsule 9, sealing the nuclear magnetic sample A through a first non-magnetic sealing cover 8, then taking down the first airtight block 1 on the first inner sample tube 2, putting the first sample capsule 9 filled with the sample into the first inner sample tube 2, and then returning the first airtight block 1. And (3) filling the nuclear magnetic sample B to be detected into a second sample capsule 11, sealing the second sample capsule by a second non-magnetic sealing cover 12, then taking down a first air sealing block 17 on a second inner sample tube 16, putting the second sample capsule 11 filled with the sample into the second inner sample tube 16, and finishing the loading of the nuclear magnetic sample.
b) Pre-polarization of the sample: the first pneumatic sample injection module 33 controls the first sample capsule 9 containing the nuclear magnetic sample a to be detected to stay in the first polarizing magnet 3 area for a period of time, so as to perform pre-polarization on the nuclear magnetic sample. The second pneumatic sample injection module 34 controls the second sample capsule 11 of the nuclear magnetic sample B to be detected to stay in the first polarized magnet 15 area for a period of time, so as to pre-polarize the nuclear magnetic sample. At the same time, the outer coil 5 pair is turned on to apply a precessional magnetic field.
c) Signal acquisition and detection: the first pneumatic sample injection module 33 operates to blow the first sample capsule 9 containing the sample a to be measured into the detection region in the multilayer magnetic shield 7 along the first inner sample injection tube 2 by the air flow, stay, and be measured. The second pneumatic sample injection module 34 operates to blow the second sample capsule 11 containing the sample B to be measured into the detection region within the multilayer magnetic shield 7 along the second inner sample injection tube 16 by the air flow, stay, and be measured. The first pneumatic sample feeding module 33 and the second pneumatic sample feeding module 34 may operate simultaneously to transport two samples to the detection position and measure the signal of the AB sample simultaneously, or may operate respectively to transport two samples to the detection position and measure the a sample and then the B sample or measure the B sample and then the a sample.
d) Unloading and replacing of samples: and (3) opening the first pneumatic sample injection module 33, sucking the first sample capsule 9 loaded with the nuclear magnetic sample into the vicinity of the first airtight block 1, taking off the airtight seal of the first airtight block, clamping the first nonmagnetic sealing cover 8 by using tweezers to take out the first sample capsule 9, and directly unloading or replacing the nuclear first sample capsule 1. And opening the second pneumatic sample injection module 34, sucking the second sample capsule 11 loaded with the nuclear magnetic sample to the vicinity of the second air sealing block 17, taking off the sealing block for air tightness, clamping the second nonmagnetic sealing cover 12 by using tweezers to take out the second sample capsule 11, and directly unloading or replacing the nuclear second sample capsule 11.
The invention can effectively transmit the sample capsule filled with two non-mixed nuclear magnetic samples to the detection area near the sealing clapboard simultaneously or respectively, and detect the two non-mixed samples simultaneously, so that the sample can be reused after being used, thereby avoiding waste; a ventilation hole channel is arranged between the two inner sample injection pipes and the outer sample injection pipe, the double-layer structure can realize effective heat insulation, the temperature change of a nuclear magnetic sample in the measuring process is avoided, and the device is suitable for a nuclear magnetic sample temperature change experiment; the outer sample inlet pipe is not in contact with the multilayer magnetic shielding and weak magnetic detection sensor, so that the technical noise generated by vibration in sample transmission can be effectively reduced; the invention has simple structure and convenient operation, adopts high temperature resistant materials, advanced multilayer heat insulation method and high-performance damping technology, is suitable for carrying out the two-way transmission of the sample of magnetic resonance based on the atomic magnetometer method, can also be applied to the static magnetic field measurement based on low-field magnetic resonance, and can also be expanded to be used for the detection of gaseous nuclear magnetic samples.
Example 1
In this embodiment, the apparatus is composed of a first airtight block 1, a first inner sample inlet 2, a first polarized magnet 3, a first sample inlet support 4, an outer solenoid coil 5, an outer sample inlet 6, a multi-layer magnetic shield 7, a first nonmagnetic sealing cover 8, a first sample capsule 9, a sealing partition plate 10, a second sample capsule 11, a second nonmagnetic sealing cover 12, a magnetic field coil 13, a second sample inlet support 14, a second polarized magnet 15, a second inner sample inlet 16, a second airtight block 17, a first vent hole 18, a first shock absorption sheet 19, a second shock absorption sheet 20, a second vent hole 21, a first pneumatic sample inlet module 33 and a second pneumatic sample inlet module 34. The first pneumatic sample injection module 33 and the second pneumatic sample injection module 34 respectively comprise an oil-free piston air compressor with the model number DW35, a circulating water type multipurpose vacuum pump with the model number SHB-III, a desktop computer with the model number ThinkCentre E73 and electromagnetic valves with the model numbers ZS05-K and ZS05, and the first sample capsule 9 and the second sample capsule 11 are controlled to slide in the first inner sample inlet pipe 2 and the second inner sample inlet pipe 16. In this embodiment, some devices including the first precision power supply 41, the weak magnetic detection sensor 42, and the second precision power supply 43 are added, and the application to the apparatus for detecting low-field magnetic resonance is more practical. The weak magnetic detection sensor 42 may be a SQUID probe, a miniaturized atomic magnetometer, an induction coil, or other magnetic field sensor for low-field magnetic resonance.
As shown in fig. 3, in this embodiment, when the bidirectional sample transfer device for a low-field nuclear magnetic resonance spectrometer operates, the computer drives the first sample capsule 9 and the second sample capsule 11 to slide in the first inner sample tube 2 and the second inner sample tube 16 respectively through the on-off states of the first pneumatic sample injection module 33 and the second pneumatic sample injection module 34, so as to realize the positioning transfer of the nuclear magnetic sample between the central positions of the multiple magnetic shields 7 of the polarizing magnet. The pneumatic sample injection module is connected with the first inner sample injection pipe and the second inner sample injection pipe by using the gas guide pipe; the sealed clapboard 10 is used for controlling the sample capsule to reach the central position of the multilayer magnetic shielding, and the vibration of the sample feeding device is effectively reduced, so that the signal-to-noise ratio of the nuclear magnetic sample signal is improved. In practice, the weak magnetic detection sensor 42 is used to measure the NMR signal of the weak magnetic field change generated by the nuclear magnetic sample in the shielding box.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A sample bidirectional transmission device for a low-field nuclear magnetic resonance spectrometer is characterized by comprising a first sample feeding system, a second sample feeding system and a detection system, wherein,
the first sample feeding system comprises a first inner sample feeding pipe (2), a first sample capsule (9) driven by a first pneumatic sample feeding module (33) is placed in the first inner sample feeding pipe (2), and a first polarizing magnet (3) is arranged at the sample feeding end of the first inner sample feeding pipe (2) and used for pre-polarizing a sample in the first sample capsule (9);
the second sample conveying system comprises a second inner sample feeding pipe (16), the second inner sample feeding pipe (16) and the first inner sample feeding pipe (2) are symmetrically arranged, a second sample capsule (11) driven by a second pneumatic sample feeding module (34) is placed in the second inner sample feeding pipe (16), and a second polarization magnet (15) is arranged at the sample feeding end of the second inner sample feeding pipe (16) and used for pre-polarizing a sample in the second sample capsule (11);
detecting system advances appearance pipe (6) and weak magnetism and surveys sensor (42) including outer, and this advance appearance pipe (6) are established along the axial cover advance appearance pipe (16) in first interior appearance pipe (2) and the second periphery and will advance appearance pipe (16) separation in first interior appearance pipe (2) and the second, the periphery of advancing appearance pipe (6) is provided with outer solenoid coil (5), and this outer solenoid coil (5) are used for providing the precession magnetic field of sample, the periphery cover of outer solenoid coil (5) is equipped with magnetic field coil (13), outer solenoid coil (5) periphery is provided with multilayer magnetic screen (7), and this multilayer magnetic screen (7) surround the detection area of regional formation sample, weak magnetism surveys sensor (42) are used for surveying the NMR signal of the weak magnetic field change that the sample produced in the detection area.
2. The sample bidirectional conveying device for the low-field nuclear magnetic resonance spectrometer is characterized in that a sealing partition plate (10) is arranged on the inner wall of the middle of the outer sample inlet pipe (6), the first inner sample inlet pipe (2) and the sealing partition plate (10) are arranged at intervals, the second inner sample inlet pipe (16) and the sealing partition plate (10) are arranged at intervals, and air outlets are formed at two ends of the outer sample inlet pipe (6), so that a first ventilation hole (18) is formed between the inner wall of the outer sample inlet pipe (6) and the outer wall of the first inner sample inlet pipe (2), and a second ventilation hole (21) is formed between the inner wall of the outer sample inlet pipe (6) and the outer wall of the second inner sample inlet pipe (16).
3. The bidirectional sample conveying device for the low-field nuclear magnetic resonance spectrometer according to claim 2, wherein the two side surfaces of the sealing partition plate (10) are respectively provided with a first damping sheet (19) and a second damping sheet (20), the first damping sheet (19) is arranged on one side close to the gas outlet of the first inner sample inlet pipe (2), and the second damping sheet (20) is arranged on one side close to the gas outlet of the second inner sample inlet pipe (16);
the first damping sheet (19) and the second damping sheet (20) are both made of high-temperature-resistant elastic materials.
4. The bidirectional sample conveying device for the low-field nuclear magnetic resonance spectrometer according to claim 1, wherein the first sample conveying system further comprises a first gas guide tube (31) and a first gas sealing block (1), the first gas sealing block (1) is used for packaging the sample inlet end of the first inner sample inlet tube (2), one end of the first gas guide tube (31) is connected with the first pneumatic sample inlet module (33), and the other end of the first gas guide tube passes through the first gas sealing block (1) to be communicated with the first inner sample inlet tube (2);
the second sample conveying system further comprises a second air sealing block (17) and a second air duct (32), the second air sealing block (17) is used for packaging a sample inlet end of the sample inlet pipe (16) in the second, one end of the second air duct (32) is connected with the second pneumatic sample inlet module (34), and the other end of the second air duct penetrates through the second air sealing block (17) and the sample inlet pipe (16) in the second is communicated.
5. The bidirectional sample transfer device for the low-field nuclear magnetic resonance spectrometer according to claim 1, wherein the two outlet end portions of the outer sample inlet (6) are respectively provided with a first sample inlet support (4) and a second sample inlet support (14), the first sample inlet support (4) is disposed at one end close to the first polarizing magnet (3), and the second sample inlet support (14) is disposed at one end close to the second polarizing magnet (15).
6. The bidirectional sample transfer device for a low-field nuclear magnetic resonance spectrometer according to claim 1, characterized in that the detection system comprises a first precision power supply (41), a second precision power supply (42), and a controller, wherein the first precision power supply (41) is connected with the magnetic field coil (13), the second precision power supply (42) is connected with the outer coil (5), and the controller is in communication connection with the first pneumatic sample injection module (33), the second pneumatic sample injection module (34), the first precision power supply (41), the second precision power supply (42), and the weak magnetic detection sensor (42).
7. The device for the bidirectional transfer of samples for low-field nuclear magnetic resonance spectrometers of claim 1, characterized in that said magnetic field coils (13) are triaxial helmholtz coils;
the first polarized magnet (3) and the second polarized magnet (15) are both magnets of a sea shell array structure;
the multilayer magnetic shield (7) is permalloy.
8. The sample bidirectional conveying device for the low-field nuclear magnetic resonance spectrometer according to claim 1, wherein the first pneumatic sample injection module (33) and the second pneumatic sample injection module (34) have the same structure and each comprise an air compressor, a vacuum pump, a first electromagnetic valve, a second electromagnetic valve and a pneumatic controller, the air compressor is connected with one end of the first electromagnetic valve through a first pipeline, the other end of the first electromagnetic valve is communicated with one end of the second electromagnetic valve through a pipeline, the other end of the second electromagnetic valve is connected with the vacuum pump, and the first electromagnetic valve and the second electromagnetic valve are both in communication connection with the pneumatic controller.
9. A method for bidirectional transfer of samples for a low-field nuclear magnetic resonance spectrometer, comprising the steps of:
s1 sample loading: the method comprises the steps of packaging a sample A into a first sample capsule (9), placing the first sample capsule (9) containing the sample A into a first inner sample inlet pipe (2), sealing the sample inlet end of the first inner sample inlet pipe (2), packaging a sample B into a second sample capsule (11), placing the second sample capsule (11) containing the sample B into a second inner sample inlet pipe (16), and sealing the sample inlet end of the second sample capsule (11);
pre-polarization of the S2 sample: the first pneumatic sample injection module (33) drives the first sample capsule (9) to the area where the first polarizing magnet (3) is located in a pneumatic mode, so that the sample A stays in the area where the first polarizing magnet (3) for a preset time to realize the pre-polarization of the sample A, and meanwhile, the second pneumatic sample injection module (34) drives the second sample capsule (11) to the area where the second polarizing magnet (15) is located in a pneumatic mode, so that the sample B stays in the area where the second polarizing magnet (15) for a preset time to realize the pre-polarization of the sample B;
s3 signal acquisition detection: first pneumatic advance kind module (33) adopt pneumatic mode will first sample capsule (9) drive to detecting area, second pneumatic advance kind module (34) adopt pneumatic mode will second sample capsule (11) drive to detecting area, simultaneously, outer solenoid coil (5) provide precession magnetic field for sample A and sample B, and the cover is established and is provided corresponding magnetic field environment as the needs of surveying in magnetic field coil (13) of the periphery of outer solenoid coil (5), and weak magnetism detection sensor (42) then simultaneously or respectively detect the NMR signal of the weak magnetic field change that sample A and sample B produced in detecting area.
10. The method of claim 9, further comprising the steps of:
s4 sample change: opening a first pneumatic sample injection module (33), sucking a first sample capsule (9) loaded with a sample A to the vicinity of a first air sealing block (1), taking off the first air sealing block (1), then taking out or replacing the first sample capsule (9), opening a second pneumatic sample injection module (34), sucking a second sample capsule (11) loaded with a sample B to the vicinity of a second air sealing block (17), taking off the second air sealing block (17), and then taking out or replacing the second sample capsule (11).
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