CN108872290A - A kind of small-sized nuclear magnetic resonance spectrometer rotates and upgrades the method and device of resolution ratio automatically - Google Patents
A kind of small-sized nuclear magnetic resonance spectrometer rotates and upgrades the method and device of resolution ratio automatically Download PDFInfo
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Abstract
The present invention relates to the methods that a kind of small-sized nuclear magnetic resonance spectrometer of low field rotates and upgrades spectra resolution rate automatically,And the sample cell automatic rotating device for rotating and upgrading spectra resolution rate automatically for the small-sized nuclear magnetic resonance spectrometer of low field,When not changing existing system magnet and shim coil,Further increase the magnetic field homogeneity of low-field nuclear magnetic resonance spectrometer,Sample cell is driven to stablize rotation indirectly by controlling motor,Under different rotating speeds,Extract the related supplemental characteristic of nmr spectrum resolution ratio,Magnetic resonance experiments parameter related with spectra resolution rate is compared and analyzed,Iterate to calculate out corresponding revolving speed under optimal experiment parameter,Obtain overcoming magnetic field bump effect preferably when revolving speed,Then real-time automatic adjustment system operation is under this revolving speed,Exclude the otherness of sample and experiment parameter,Offset magnetic field inhomogeneities to a certain extent,Experiment optimal effectiveness is obtained to the maximum extent,Avoid a large amount of test comparison work of operator,Greatly improve conventional efficient.
Description
Technical field
The present invention relates to nuclear magnetic resonance apparatus to develop field, more specifically to a kind of small-sized nuclear magnetic resoance spectrum of low field
The method that instrument rotates and upgrades spectra resolution rate automatically, and spectrogram is rotated and upgraded automatically for the small-sized nuclear magnetic resonance spectrometer of low field
The sample cell automatic rotating device of resolution ratio.
Background technique
In order to improve sensitivity and resolution ratio of the nuclear magnetic resonance apparatus to sample detection spectral line, suitable magnetic field is needed
Intensity and guarantee magnetic field homogeneity, so that the high-resolution spectrogram of sample is obtained, usually from instrument hardware design and experimental method
Two aspects are set about.In the hardware design, the design and shim coil regulation of main magnet are relied primarily on, magnet design is to pass through increase
Magnetic field strength and promotion magnet processing technology, shim coil design are to increase shim coil high-order shimming, and use effective even
Field algorithm is realized.
After magnet and shim coil design are fixed, in order to further overcome the inhomogeneities in magnetic field, sample cell rotation side
Method comes across 1954 earliest, and document " F.Bloch, Phys.Rev., 94, (1954), 496 ", it is indicated that spinning sample can be improved
The resolution ratio of nmr spectrometer.
Currently, large-scale high field super NMR system usually makes detected sample quality control with specified using air turbine power
Velocity interval rotation, the magnetic field locating for homogeneous sample by way of rotating sample, to overcome perpendicular on pivot axis plane
The inhomogeneities in magnetic field.Typically there are external Brooker (Bruker) company, Agilent (Agilent) company, domestic force
The large-scale superconduction nuclear magnetic resonance spectrometer of Oxford spectroscopic technique Co., Ltd of Hanzhong section is all made of air compressor control rotation approach
Carry out sample cell rotation.In low field nuclear-magnetism instrument, such as the low field permanent magnet nuclear magnetic resonance spectrometer of equipment Co., Ltd of Shanghai Science and Education Equipment Co., Ltd. Huan Tong
Device uses turbine air-control device.
Domestic and international related patents and document also mainly use turbine gas control spinning solution to the research of sample cell rotating device,
Such as：Granted United States Patent (USP) " Sample Spinning Mechanism for NMR Probes " (United States Patent (USP) in 1981
Number：4275350), described is that air pneumatic device drives rotor rotation；Granted United States Patent (USP) " High in 1993
Temperature NMR sample spinner " (U.S. Patent number：5202633), it is described be high temperature Magic angle spinning gas
Dynamic rotating device；Granted United States Patent (USP) " Sample Spinning Mechanism for NMR Probes " (beauty in 2017
State's patent No.：9778332B2), the air impeller Rotation Controllers controls sample cell using the controllable impulse form of algorithm
Revolving speed；Document " Deuterium NMR in Solids with a Cylindrical Magic, Journal of
Magnetic Resonance,1980,41(3):440-446 ", described is in solid magnetic resonance experiments used in Magic angle spinning
Pneumatic high-speed rotating device；Document " Implementation of Fuzzy Self-tuning Proportional
Integral Derivative Controller on Sample-tube Spin Control System in Nuclear
Magnetic Resonance Spectrometer,Chinese Journal of Analytical Chemistry,2011,
39(4):506-510 ", described is gas control rotating device using improved pid control mode promotion signal-to-noise ratio.
But since turbine gas control rotation mode needs to configure the air-channel system of air compressor machine and complexity, for portable small
The nuclear magnetic resonance equipment of type permanent magnet is limited by magnet volume, structure and cost, can not use air turbine rotating device.
The sample cell rotating device that the NMR system of the prior art uses, by its sample cell of operator's manual setting
Revolving speed can not feed back the revolving speed for calculating and obtaining under optimal result according to the experimental result of acquisition.The revolving speed being then arranged in experiment can
It can not be the revolving speed under attainable best spectra resolution rate, and due to the spinning side band peak of different rotary generation and high rotation
The introduced noise of unstability also has larger impact to experimental result.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide the revolving speeds that one kind is capable of adjust automatically rotating mechanism
And the method that the small-sized nuclear magnetic resonance spectrometer of low field for obtaining optimal spectra resolution rate rotates and upgrades spectra resolution rate automatically, and
A kind of structure simplifies, is low in cost, is capable of the influence of offset magnetic field inhomogeneities to a certain extent, and according to experiment spectrogram
As a result sample cell rotation is automatically controlled, the automatic rotation for the small-sized nuclear magnetic resonance spectrometer of low field for being able to ascend conventional efficient mentions
Rise the sample cell automatic rotating device of spectra resolution rate.
Technical scheme is as follows：
A kind of method that the small-sized nuclear magnetic resonance spectrometer of low field rotates and upgrades spectra resolution rate automatically, is driven by rotating mechanism
Sample cell is rotated；Nuclear-magnetism experimental result based on current rotating speed obtains corresponding spectra resolution rate；Control rotating mechanism changes
Speed change degree obtains spectra resolution rate corresponding to the speed after changing；Control rotating mechanism is maintained to change speed, until obtaining most
Excellent spectra resolution rate, and control rotating mechanism and sample cell is driven to rotate under the corresponding revolving speed of optimal spectra resolution rate.
Control rotating mechanism changes the strategy of speed automatically and is：Noise threshold is set first, filters out the signal lower than threshold value,
Then nuclear magnetic resonance experiment is carried out, NMR signal is acquired, obtains resolution ratio, as first group of index, repeats to test, compare
The superiority and inferiority of the spectra resolution rate of front and back friction speed, if change after speed corresponding to spectra resolution rate better than change before
Spectra resolution rate corresponding to speed saves current rotating speed, and changes step motion control rotating mechanism according to current speed and continue
Change speed, re-starts experiment.
If spectra resolution rate corresponding to the speed after changing is primary identical compared to preceding, current speed is kept to change
Trend control rotating mechanism continues to change speed, re-starts experiment.
If under spectra resolution rate corresponding to spectra resolution rate corresponding to the speed after changing and the speed before change
Drop returns to a preceding revolving speed, and reversed speed changes trend control rotating mechanism and continues to change speed, re-starts experiment.
If spectra resolution rate constantly rises as speed increases, and after certain primary change speed under spectra resolution rate
Drop then reduces current speed and changes stepping, returns to a preceding revolving speed, and control rotating mechanism continues to change speed, re-start
It tests, until spectra resolution rate corresponding to the speed after changing is inferior to spectra resolution rate corresponding to the speed before changing, then
Previous revolving speed is the corresponding revolving speed of optimal spectra resolution rate.
The corresponding index parameter of spectra resolution rate includes the halfwidth and spinning side band of spectrogram area, spectral peak height, spectrogram
Peak peak height it is one or more, be typically due in rotary course to generate spinning side band peak, the spectrogram area at spinning side band peak is made
For one of the index parameter for measuring effect.
A kind of rotating and upgrading the sample cell of spectra resolution rate automatically and rotate automatically for the small-sized nuclear magnetic resonance spectrometer of low field
Device, including rotating mechanism, speed adjusting module, sample cell are set to rotating mechanism, drive sample cell to be revolved by rotating mechanism
Turn, speed adjusting module executes the method that the small-sized nuclear magnetic resonance spectrometer of low field rotates and upgrades spectra resolution rate automatically, automatic to adjust
The revolving speed of whole rotating mechanism, and obtain the spectra resolution rate under optimized rotating speed.
Rotating mechanism includes motor, synchronous transmission device, and the driving wheel rotation of motor driven synchronous transmission device drives same
The driven wheel rotation for walking transmission device follows driven wheel to rotate with the sample cell of driven wheel coaxial arrangement.
One end of driven wheel and transmission band connection, the other end of driven wheel is arranged in firm banking, non-magnetic driven
It is provided with two non-magnetic roller bearings driven wheels up and down between wheel and firm banking to rotate, prevents single bearing operation
Machinery of the sample cell caused by the process outside vertical axis swings excessive introducing noise, and firm banking is buckled by pedestal to be arranged
In the injection port of nuclear magnetic resonance spectrometer.
Motor is set to the side of nuclear magnetic resonance spectrometer by non-magnetic bracket, plays stabilization when servo motor operating
Operation effect.Bracket includes three vertical plates, and three vertical plates and nuclear magnetic resonance spectrometer surround installation cavity, and motor setting is empty in installation
It is intracavitary；Vertical plate offers through-hole, the cabling of motor control line.
Speed adjusting module controls software by revolving speed can be with the rotation parameter of manual setting motor, such as revolving speed, acceleration and angle
Degree, or start adjust automatically rotating mechanism by being provided with one-touch automatic rotational speed regulation control key, it is calculated using the algorithm
The rotation parameter of acquisition configures motor rotation speed, and the display of real-time status and parameter is carried out by display window.
Beneficial effects of the present invention are as follows：
The method that the small-sized nuclear magnetic resonance spectrometer of low field of the present invention rotates and upgrades spectra resolution rate automatically, is not changing
In the case of existing system magnet and shim coil, the magnetic field homogeneity of low-field nuclear magnetic resonance spectrometer is further increased, passes through control
Motor drives sample cell to stablize rotation indirectly, under different rotating speeds, extracts the related supplemental characteristic of nmr spectrum resolution ratio,
Magnetic resonance experiments parameter related with spectra resolution rate is compared and analyzed, is iterated to calculate out corresponding under optimal experiment parameter
Revolving speed, obtain overcoming magnetic field bump effect preferably when revolving speed, then the operation of real-time automatic adjustment system under this revolving speed,
Experiment optimal effectiveness is obtained to the maximum extent.
Method of the present invention can adjust sample cell revolving speed in real time automatically, exclude the difference of sample and experiment parameter
Property, the magnetic field bump perpendicular to pivot axis plane is overcome to a certain extent, thus offset magnetic field to a certain extent
Inhomogeneities improves the resolution ratio of nmr spectrum, avoids a large amount of test comparison work of operator, greatly improves experiment
Efficiency.
It is of the present invention to rotate and upgrade spectrogram automatically for the small-sized nuclear magnetic resonance spectrometer of low field based on the method
The sample cell automatic rotating device of resolution ratio is realized in the case where not changing existing magnet and shim coil performance and construction
The middle small-sized nuclear magnetic resonance spectrometer sample cell of low field rotates automatically.The sample cell automatic rotating device not only volume compact, easily
In installation, driven wheel and bearing are formed using non-magnetic material, prevent magnetic interference；Using synchronization transmission structure, it is applicable in and two axis
Center has good flexibility and antivibration kinetic force, ensure that the concentricity that sample cell rotates in magnetic field away from biggish transmission,
Avoid offset of the sample cell outside vertical axis.
Sample cell automatic rotating device suitability of the present invention is strong, can not only make for existing nuclear magnetic resonance spectrometer
With, and if replace other nuclear magnetic resonance equipments, machinery need to be only transformed in or the related system for needing closed loop to adjust revolving speed by a small margin
It still can be used after structure.
Detailed description of the invention
Fig. 1 is the flow chart of method of the present invention；
Fig. 2 is the structural schematic diagram of device of the present invention；
Fig. 3 is the setting schematic diagram of sample cell；
Fig. 4 is the assembling view of driven wheel, firm banking and pedestal buckle；
In figure：10 be motor, and 11 be driving wheel, and 12 be driven wheel, and 121 be groove, and 13 be firm banking, and 14 be the axis of rolling
It holds, 15 be pedestal buckle, and 151 be screw hole, and 16 be transmission belt, and 20 be bracket, and 21 be vertical plate, and 211 be through-hole, and 30 be nuclear magnetic resonance
Spectrometer, 31 be radio-frequency receiving-transmitting coil, and 32 be shim coil, and 40 be sample cell.
Specific embodiment
The present invention is further described in detail with reference to the accompanying drawings and embodiments.
The present invention in order to solve in the prior art, for miniaturization permanent magnet nuclear magnetic resonance equipment existing for structure is complicated,
The inconvenient, deficiencies such as accuracy rate is low provide a kind of small-sized nuclear magnetic resonance spectrometer of low field and rotate and upgrade spectra resolution rate automatically
Method and a kind of sample cell for rotating and upgrading spectra resolution rate automatically for the small-sized nuclear magnetic resonance spectrometer of low field rotate automatically
Device.
The method that the small-sized nuclear magnetic resonance spectrometer 30 of low field of the present invention rotates and upgrades spectra resolution rate automatically, passes through rotation
Rotation mechanism drives sample cell 40 to be rotated；Nuclear-magnetism experimental result based on current rotating speed show that corresponding spectra resolution rate refers to
Mark parameter；It controls rotating mechanism and changes speed, obtain spectra resolution rate index parameter corresponding to the speed after changing；Maintain control
Rotating mechanism processed changes speed, until obtaining optimal spectra resolution rate, and it is corresponding in optimal spectra resolution rate to control rotating mechanism
Revolving speed under drive sample cell 40 rotate.
In the present embodiment, the corresponding parameter of spectra resolution rate includes spectrogram area, spectral peak height, the halfwidth of spectrogram, rotation
Turn the one or more of sideband peak peak height.The corresponding relevant parameter of magnetic resonance experiments spectra resolution rate that the present invention obtains in real time,
Such as FID integral area, spectral line halfwidth, rotation speed is improved according to revolving speed incremental step value, by under comparison different rotating speeds
Spectral parameters retain more excellent as a result, constantly iteration finally obtains corresponding 40 revolving speed of sample cell of best experiment spectrogram result, realization
System adjust automatically revolving speed obtains higher spectra resolution rate, improves conventional efficient.
Theoretically, if in the case where other parameters are constant, the line width of spectrogram narrows, height rises, and for certain
Sample coupling, which is split, point to be become more apparent upon, and illustrates that current rotating speed overcomes the magnetic field unevenness of nuclear magnetic resonance spectrometer 30 to a certain extent
Even property.Continue adjust revolving speed, if improve revolving speed after compare original spectral line obtain line width it is narrower, height it is higher as a result, illustrating to revolve
Rotary speed overcomes magnetic field bump ability better fastlyer, and spectra resolution rate is higher.Vice versa.Then in order to quickly find most
The excellent corresponding revolving speed of spectra resolution rate, the strategy that control rotating mechanism changes speed are：Compare the nuclear-magnetism of front and back friction speed
The superiority and inferiority of the spectra resolution rate of experiment, if change after speed corresponding to spectra resolution rate better than change before speed institute it is right
The spectra resolution rate answered then changes trend control rotating mechanism according to current speed and continues to change speed.If after changing
Spectra resolution rate corresponding to spectra resolution rate corresponding to speed and the speed before change declines, and returns to a preceding revolving speed, and
Reversed speed changes trend control rotating mechanism and continues to change speed, re-starts experiment.
It in the present embodiment, is tested, is extracted by Fourier transformation by nuclear magnetic resonance spectrometer 30 in sample cell 40
Magnetic resonance experiments frequency-domain signal data, extracted valid data does average value processing under every group of revolving speed, compares spectrogram under different rotating speeds
Area, halfwidth, peak height and spinning side band peak, to obtain, spectrogram spectral peak area is maximum, under spinning side band peak minimum
Revolving speed, feedback real-time results are adjusted in real time, thus turn when obtaining experimental result best (i.e. spectra resolution rate is optimal)
Speed.
If spectra resolution rate constantly rises as speed increases, and after certain primary change speed under spectra resolution rate
Drop then reduces current speed and changes stepping, returns to a preceding revolving speed, and control rotating mechanism continues to change speed, re-start
It tests, until spectra resolution rate corresponding to the speed after changing is inferior to spectra resolution rate corresponding to the speed before changing, then
Previous revolving speed is the corresponding revolving speed of optimal spectra resolution rate.
As shown in Figure 1, the present invention realizes the revolving speed of adjust automatically rotating mechanism, and obtain the stream of optimal spectra resolution rate
Journey is as follows：
1) rotating mechanism and nuclear magnetic resonance spectrometer 30 power on and after stable operations, and the hardware and control software to the two are initial
Change.
2) experiment parameter for setting magnetic resonance tool, is arranged the revolving speed initial value v of rotating mechanism0With acceleration a appropriate0,
Rotating mechanism is opened, after 40 spin stabilization of sample cell, starts to carry out the 1st magnetic resonance experiments.
3) nuclear magnetic resonance experiment is carried out, collected magnetic resonance signal progress Fourier transformation is obtained its frequency by experiment software
Numeric field data is read the frequency domain data P of fixed points by automatic rotational speed regulation program0.dat.Signal is masked by threshold process
Bottom make an uproar, usual selections threshold value can effectively mask signal low noise, leave the progress data analysis of spectrogram effective coverage.Then
Acquire spectral peak height H0, the area S of spectrogram is acquired by integral calculation0, and position and acquire half width W at peak height 50%0, and
Since non-uniform field backspin transfers the sideband peak peak height E generated0, store supplemental characteristic.
4) revolving speed is improved according to equally spaced stepping △ n, continues magnetic resonance experiments.Judge whether to measure two groups of numbers
According to.If no, return step 2).Measure the spectrogram area S under the revolving speed1, spectral peak height H1, spectrogram halfwidth W1, sideband
Peak peak height E1, by revolving speed v0And v1Under four experiment parameter data be compared.Judge whether spectra resolution rate parameter improves,
If spectrogram integral area becomes larger, spectral peak is got higher, spectrogram halfwidth narrows, sideband peak peak height becomes smaller, then stores parameter and more preferably count
According to, if not improving, return step 2).Change revolving speed by stepping again later, by revolving speed vi-1And viUnder four experiments ginseng
Count data successively contrast conting.
5) judge whether that iteration is promoted always before the parameter calculated appearance, reduces suddenly under some revolving speed, illustrate to turn
Speed increases above tachometer value corresponding to optimum resolution parameter.If it is there is no more excellent parameter before, directly reduce, then
Do not save supplemental characteristic, return step 2).If iteration is promoted always before parameter, the feelings that are reduced suddenly under some revolving speed
Revolving speed step value is then taken negative value by condition, and gradually reduces stepping length, return step 2).According to reality corresponding under multiple groups revolving speed
Data are tested, if parameter is no longer promoted or is declined, the corresponding revolving speed v of the optimal experimental result being calculatedB, terminate operation stream
Journey, otherwise return step 2) it is tested next time, until meeting condition.
Based on the method for rotating and upgrading spectra resolution rate automatically, the present invention also provides one kind to be used for low field small cores
40 automatic rotating device of sample cell for rotating and upgrading spectra resolution rate automatically of nuclear magnetic resonance spectrometer 30, as shown in Figure 2 and Figure 3, including
Rotating mechanism, speed adjusting module, sample cell 40 are set to rotating mechanism, drive sample cell 40 to be rotated by rotating mechanism.Sample
The permanent magnet that quality control 40 is perpendicularly fixed at nuclear magnetic resonance spectrometer 30 is intracavitary, with main field B0The vertical appropriate location in direction guarantees
Sample in sample cell 40 is in 31 overlay area of solenoid radio frequency (RF) dispatch coil, radio-frequency receiving-transmitting coil 31 and its tuning
RF transmit-receive circuit with circuit connecting system.32 array of shim coil is individually positioned in the two poles of the earth magnet N, S, passes through shimming circuit
Adjust different directions magnetic field's regularity inside magnet.It is automatic that speed adjusting module executes the small-sized nuclear magnetic resonance spectrometer 30 of the low field
The method for rotating and upgrading spectra resolution rate, the revolving speed of adjust automatically rotating mechanism, and obtain optimal spectra resolution rate.
Rotating mechanism includes motor 10, synchronous transmission device, and motor 10 drives the driving wheel 11 of synchronous transmission device to rotate,
The driven wheel 12 of synchronous transmission device is driven to rotate, the sample cell 40 being coaxially disposed with driven wheel 12 follows driven wheel 12 to rotate.
In the present embodiment, synchronous transmission device uses train belt drive structure, as the driving wheel 11 of 10 rotor of motor and as sample
Transmission ratio between the driven wheel 12 of 40 rotor of pipe is 2：1, i.e. the linear velocity of driven wheel 12 is adopted greater than the linear velocity of driving wheel 11
Use " O " type rubber ring as transmission belt 16, motor 10 drives driving wheel 11 to rotate, and drives 12 turns of driven wheel by transmission belt 16
It is dynamic, so that sample cell 40 rotates.Transmission belt 16 is separately fixed to the groove 121 of driving wheel 11 Yu 12 end outer wall of driven wheel
It is interior, make the tight fixation of transmission belt 16, prevent from skidding in rotation process, transmission belt 16 and ground need to keep horizontal, prevent from being driven
The component other than driving face is generated in the process, causes fluctuation of service.
Motor 10 is embodied as servo motor, and is controlled using Serve Motor Control software, can according to user demand,
The revolving speed, acceleration and angle of servo motor are precisely controlled using upper computer software.Servo motor connects servo motor movement control
Device and power source drive unit processed control servomotor controller by upper computer software and enable servo motor, adjust servo motor
Revolving speed and acceleration, 10 driving function of Serve Motor Control software transfer bottom motor, realize setting parameter and motor 10 control
Conversion between device pulse frequency processed, Serve Motor Control software are responsible for enabled motor 10, and driving motor 10 is under different rotating speeds
Rotation, the function of setting initialization revolving speed, acceleration and angle and revolving speed stepping initial value.
In the present embodiment, 10 maximum speed of motor is 4800r/min, and driving wheel 11 and 12 transmission ratio of driven wheel are 2：1, root
According to theoretical formula, the rotation speed of sample cell 40 be must satisfy：->, both revolving speed can offset the unevenness of the magnetic field in sample scope
Even amount.In the case where not considering the situation of 16 frictional resistance of transmission belt and skidding, it is theoretical according to transmission ratio it is found that 40 rotor of sample cell most
High revolving speed is 160Hz, both 160 turns per second, theoretically can unevenly be measured with offset magnetic field and be up to 1.879*10-6T.Even if but
Design is rigorous, there are still friction and slipping phenomenon in rotary course, causes actual effect that can be slightly below theoretical value, for the mistake of permission
Difference.
As shown in figure 4, one end of driven wheel 12 is connect with transmission belt 16, the other end of driven wheel 12 is arranged in firm banking
In 13, it is (outer that nonmagnetic anti abrasive rolling bearing 14 is provided between nonmagnetic anti abrasive driven wheel 12 and firm banking 13
Shell and roller are nonmagnetic anti abrasive material), firm banking 13 is set to nuclear magnetic resonance spectrometer 30 by pedestal buckle 15
Injection port.Two rolling bearings 14, i.e. firm banking up and down are set in the present embodiment, between driven wheel 12 and firm banking 13
13 top and bottom fluting is embedded with a rolling bearing 14 respectively, and two rolling bearings 14 are inserted into one end of driven wheel 12
In inner ring, blend compounds hydropexis prevents from skidding.Driven wheel 12 is supported to rotate by upper and lower two rolling bearings 14, and by pedestal card
Button 15 is fixed by firm banking 13 and nuclear magnetic resonance spectrometer 30, and sample cell 40 is inserted into the appropriate location of driven wheel 12, driven wheel 12
It drives sample cell 40 to stablize rotation, reduces the coefficient of friction in rotary course, ensure the concentricity that sample cell 40 rotates, avoid
Offset of the sample cell 40 outside vertical axis improves the stability in operation process.Pedestal buckle 15 is by two M3 sizes
Plastics screw is fixed on the magnet cabinet of nuclear magnetic resonance spectrometer 30 by the screw hole 151 that pedestal buckle 15 is laterally opened, and is played
Stablize the effect that driven wheel 12 rotates.Polyoxymethylene can be selected in the material of driven wheel 12 and rolling bearing 14, and the material is tough and tensile
It is flexible, there is good geometrical stability and impact property.
For being adapted to for sample cell 40 and driven wheel 12, the present invention provides two kinds of adapter structures.If necessary to be inserted into difference
The sample cell 40 of size can be matched using the driven wheel 12 of change different inner diameters specification with 40 size of sample cell.Or it uses
The driven wheel 12 of fixed inner diameter, in the insertion of the sample cell 40 matched flexible plastic conduit of outer diameter therewith, and plastic catheter outer diameter with from
The internal diameter of driving wheel 12 suits, so that sample cell 40 is fixed on driven wheel 12.Such as implement to be directed to nuclear magnetic resonance spectrometer 30
Injection port diameter be up to 10mm, fixed inner diameter can be set for the inner cavity of driven wheel 12 according to the diameter of sample cell 40
10mm, 5mm or 3mm etc..Or the driven of 10mm is set as using the flexible plastic conduit insertion inner cavity of same outer diameter, different inner diameters
Wheel 12, then the sample cell 40 of fixed corresponding diameter.
Motor 10 is set to the side of nuclear magnetic resonance spectrometer 30 by non-magnetic bracket 20, and bracket 20 can be locked securely
Tightly in the side of nuclear magnetic resonance spectrometer 30, play the role of stable operation when servo motor operating.Bracket 20 includes three vertical plates
21, three vertical plates 21 and nuclear magnetic resonance spectrometer 30 surround installation cavity, and motor 10 is arranged in installation cavity；Vertical plate 21 offers
Through-hole 211, the cabling of 10 control line of motor will not interfere the normal operation of MR system in 10 operational process of motor.This implementation
In example, non-magnetic bracket 20 is assembled by acrylic board, is bonded the bracket 20 spliced securely with glue.
Speed adjusting module is provided with one-touch automatic rotational speed regulation control key, can be embodied as hardware or soft according to demand is implemented
Part form for starting the revolving speed of adjust automatically rotating mechanism, and passes through the display of display window progress real-time status and parameter.
Specifically, in the present embodiment, Serve Motor Control software built in speed adjusting module, one-touch automatic rotational speed regulation in the form of software
Control key and rotation parameter real-time display window can be associated with, calculated turn of real-time acquisition algorithm with automatic rotational speed regulation algorithm
Speed is simultaneously delivered to completion 40 transformation of speed of sample cell of motor 10, while the multiple rotation status parameters of real-time display, monitors automatic rotation
Turn adjustment process, is compared convenient for user record.Serve Motor Control software can easily be embedded in nuclear-magnetism experiment software, have
It is preferable portable.
In the present embodiment, manually adjust the speed mode and self-regulating rotary fast mode can also be switched, it is implementable for speed regulation
Module controls software by revolving speed and is realized.It, can be with the rotation parameter of manual setting motor 10 under manually adjust the speed mode；
It is interrelated with automatic rotational speed regulation algorithm under self-regulating rotary fast mode, the rotation parameter obtained is calculated by algorithm to be configured
10 rotation speed of motor.
Above-described embodiment is intended merely to illustrate the present invention, and is not used as limitation of the invention.As long as according to this hair
Bright technical spirit is changed above-described embodiment, modification etc. will all be fallen in the scope of the claims of the invention.
Claims (9)
1. a kind of method that the small-sized nuclear magnetic resonance spectrometer of low field rotates and upgrades spectra resolution rate automatically, which is characterized in that pass through rotation
Rotation mechanism drives sample cell to be rotated；Nuclear-magnetism experimental result based on current rotating speed obtains corresponding spectra resolution rate index
Parameter；It controls rotating mechanism and changes speed, obtain spectra resolution rate index parameter corresponding to the speed after changing；Maintain control
Rotating mechanism changes speed, until obtaining optimal spectra resolution rate, and it is corresponding in optimal spectra resolution rate to control rotating mechanism
Sample cell rotation is driven under revolving speed.
2. the method that the small-sized nuclear magnetic resonance spectrometer of low field according to claim 1 rotates and upgrades spectra resolution rate automatically,
It is characterized in that, the strategy that control rotating mechanism changes speed is：Compare the spectra resolution rate of the nuclear-magnetism experiment of front and back friction speed
The superiority and inferiority of index, if change after speed corresponding to spectra resolution rate better than change before speed corresponding to spectra resolution
Rate then changes trend control rotating mechanism according to current speed and continues to change speed；If corresponding to the speed after changing
Spectra resolution rate is primary identical compared to preceding, then keeps current speed to change trend control rotating mechanism and continue to change speed；Such as
Spectra resolution rate corresponding to speed after fruit change compares preceding primary decline, then returns to a preceding revolving speed, reversed current speed
Degree change trend control rotating mechanism continues to change speed.
3. the method that the small-sized nuclear magnetic resonance spectrometer of low field according to claim 2 rotates and upgrades spectra resolution rate automatically,
It is characterized in that, if spectra resolution rate constantly rises as speed increases, and after certain primary change speed under spectra resolution rate
Drop then reduces current speed and changes stepping, returns to a preceding revolving speed, and control rotating mechanism continues to change speed, until changing
Spectra resolution rate corresponding to speed afterwards is inferior to spectra resolution rate corresponding to the speed before changing, then previous revolving speed is optimal
The corresponding revolving speed of spectra resolution rate.
4. the method that the small-sized nuclear magnetic resonance spectrometer of low field according to claim 3 rotates and upgrades spectra resolution rate automatically,
It is characterized in that, the corresponding index parameter of spectra resolution rate includes the halfwidth and spinning side band of spectrogram area, spectral peak height, spectrogram
Peak peak height it is one or more.
5. a kind of automatic rotating dress of sample cell for rotating and upgrading spectra resolution rate automatically for the small-sized nuclear magnetic resonance spectrometer of low field
It sets, which is characterized in that including rotating mechanism, speed adjusting module, sample cell is set to rotating mechanism, drives sample by rotating mechanism
Pipe is rotated, and speed adjusting module perform claim 1 to 4 described in any item small-sized nuclear magnetic resonance spectrometers of low field of requirement rotate automatically to be mentioned
The method for rising spectra resolution rate, the revolving speed of adjust automatically rotating mechanism, and obtain optimal spectra resolution rate.
6. the sample according to claim 5 that rotate and upgrade spectra resolution rate automatically for the small-sized nuclear magnetic resonance spectrometer of low field
Quality control automatic rotating device, which is characterized in that rotating mechanism includes motor, synchronous transmission device, motor driven Synchronous Transmission dress
The driving wheel rotation set, drives the driven wheel of synchronous transmission device to rotate, and follows with the sample cell of driven wheel coaxial arrangement driven
Wheel rotation.
7. the sample according to claim 6 that rotate and upgrade spectra resolution rate automatically for the small-sized nuclear magnetic resonance spectrometer of low field
Quality control automatic rotating device, which is characterized in that one end of driven wheel and transmission band connection, the other end of driven wheel are arranged in fixation
In pedestal, it is provided with two non-magnetic rolling bearings up and down between non-magnetic driven wheel and firm banking, supports driven wheel
Rotation, firm banking are set to the injection port of nuclear magnetic resonance spectrometer by pedestal buckle.
8. the sample according to claim 6 that rotate and upgrade spectra resolution rate automatically for the small-sized nuclear magnetic resonance spectrometer of low field
Quality control automatic rotating device, which is characterized in that motor is set to the side of nuclear magnetic resonance spectrometer, bracket by non-magnetic bracket
Including three vertical plates, three vertical plates and nuclear magnetic resonance spectrometer surround installation cavity, and motor is arranged in installation cavity；Vertical plate opens up
There are through-hole, the cabling of motor control line.
9. the sample according to claim 5 that rotate and upgrade spectra resolution rate automatically for the small-sized nuclear magnetic resonance spectrometer of low field
Quality control automatic rotating device, which is characterized in that speed adjusting module is provided with one-touch automatic rotational speed regulation control key, automatic for starting
The revolving speed of rotating mechanism is adjusted, and carries out the display of real-time status and parameter by display window.
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