CN105651803A - Two-dimensional diffusion-ordered nuclear magnetic resonance spectroscopy method used for any magnetic field environments - Google Patents
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Abstract
The invention discloses a two-dimensional diffusion-ordered nuclear magnetic resonance spectroscopy method used for any magnetic field environments and relates to nuclear magnetic resonance spectroscopy detection methods. The method includes the steps of 1), measuring pi/2 nonselective radiofrequency pulse width and (pi/2)<I> solvent selective radiofrequency pulse width required by sample stimulation; 2), importing a nuclear magnetic resonance pulse sequence on a nuclear magnetic resonance spectrometer; 3), turning on an intermolecular zero-quantum coherence signal selection module, a time-invariant evolution module and a diffusion order module of the nuclear magnetic resonance pulse sequence and setting experiment parameters of all modules; 4), executing data sampling; 5), performing data post-processing to obtain high-resolution two-dimensional diffusion-ordered spectroscopy. The two-dimensional diffusion-ordered nuclear magnetic resonance spectroscopy method used for any magnetic field environments does not need any shimming operation, a sample preprocessing process and any special hardware devices, is simple, convenient and feasible and is applicable to any conventional nuclear magnetic resonance spectrometers.
Description
Technical field
The present invention relates to nuclear magnetic resonance, NMR (NMR, NuclearMagneticResonance) Wave Spectrum detection method, especially relates to mix ingredients under any magnetic field environment and separates a kind of nuclear magnetic resonance, NMR two-dimensional diffusion sequence spectral method for any magnetic field environment with composition analysis.
Background technology
Nuclear magnetic resonance, NMR (NuclearMagneticResonance, NMR) as a kind of important detection analysis means, due to plurality of advantages such as it is accurate, efficient, Non-Destructive Testings, have a wide range of applications at ambits such as physics, chemistry, biology and materials. For the detection of complex mixture nuclear magnetic resonance, NMR, the spectral peak of various different materials is all presented in same spectrum, often leads to spectral peak crowded and be difficult to obtain correct composition ownership. For this, blend sample is easily separated purification by general requirement before testing, and this is wasting manpower and material resources not only, and separating-purifying process may destroy the original structure of sample. Utilize nuclear magnetic resonance, NMR diffusion correlation technique, i.e. diffusion sequence spectrum (DiffusionOrderSpectroscopY, DOSY), can when without sample be carried out physics and chemistry separation, the difference utilizing diffusion coefficient realizes each component " void " in sample cell in solution mixture and separates, and the ingredients of a mixture composition is directly analyzed by the H NMR spectroscopy being associated by obtained diffusion coefficient and other spectroscopy information. This method has not only been saved the time of physics and chemistry separation but also has been avoided the specimen breakdown because separation causes.
But, existing diffusion sequence spectral method still suffers from significant limitation in actual mix is applied. Diffusion sequence spectrum only just can simulate correct diffusion dimension information when spectral peak is differentiated completely. In Magnetic field inhomogeneity situation, the uneven broadening effect of spectral line can make spectral peak to differentiate, and causes that diffusion sequence spectral method cannot be applied. Under normal circumstances, magnetic field homogeneity is had significantly high requirement by the experiment of diffusion sequence spectrum. But under many circumstances, magnetic field homogeneity often cannot absolute guarantee, even if utilize shimming technique that Magnetic field inhomogeneity that in experimentation various samples and environmental factors cause also cannot be completely eliminated. Such as, in the research of some biological medicine blend sample, sample molecule often only just has given activity and function when tissue coexists, and this organization internal susceptibility can cause the uneven of magnetic field, therefore existing diffusion sequence spectral method is generally difficult to be applied to this kind of mixture system.If able to breach the limitation that existing diffusion sequence spectral method is applied at non-uniform magnetic field, design one to be applied under any magnetic field environment (include field homogeneity situation and Magnetic field inhomogeneity situation that various sample causes with environmental factors) mix ingredients and separate and the high resolution 2 d diffusion sequence spectral method of component analysis is by significant, expand the application of diffusion sequence spectrum further.
Summary of the invention
It is an object of the invention to provide the composition that can be suitably used for blend sample and separate a kind of nuclear magnetic resonance, NMR two-dimensional diffusion sequence spectral method for any magnetic field environment with component analysis.
The present invention comprises the steps:
1) measuring samples excites required pi/2 non-selective radio frequency pulse width and (pi/2)ISolvent selectivity RF pulse width;
2) on nuclear magnetic resonance chemical analyser, nuclear magnetic resonance pulse sequence is imported;
3) open genetic module and diffusion order module when the intermolecular zero quantum coherent signal selection module of nuclear magnetic resonance pulse sequence, perseverance, the experiment parameter of each module is set;
4) data sampling is performed;
5) carry out Data Post, obtain high resolution 2 d diffusion sequence spectrum.
In step 1) in, described measuring samples excites required pi/2 non-selective radio frequency pulse width to be utilize conventional one-dimensional pulse sequence to complete, by arranging a series of pulse operating time sampling corresponding signal, burst length corresponding when obtaining magnetization vector 90 degree upset is pi/2 non-selective radio frequency pulse width, this measurement simultaneously also obtain field homogeneity implementations, for spectrum width parameter, offer foundation, described (pi/2) are setIThe measurement of solvent selectivity RF pulse width is to be completed by conventional one-dimensional soft pulse sequence, it is thus achieved that selective pulse action time corresponding during solvent magnetization vector 90 degree upset.
In step 2) in, described nuclear magnetic resonance pulse sequence employs genetic module and diffusion order module when intermolecular zero quantum coherent signal selection module, perseverance;
Described intermolecular zero quantum coherent signal selection module is by a pi/2 non-selective radio frequency pulse, one (pi/2)ISolvent selectivity radio-frequency pulse and a relevant selection gradient G are constituted; It is solvent and the difference of resonant frequency of solute spin by its resonant frequency of signal selected by intermolecular zero quantum coherent signal selection module; In Magnetic field inhomogeneity situation, the difference of the resonant frequency between solvent and solute can eliminate the impact of Magnetic field inhomogeneity and obtain high-resolution spectroscopy information. In field homogeneity situation, high-resolution spectroscopy information can also be obtained equally;
Genetic module (t during described perseverance1CTModule) it is by t1/2����(��-t1/ 2) composition, t1For indirectly tieing up the evolution time, �� is the Time constant constant set, and is generally a few tens of milliseconds; Time permanent, genetic module can eliminate the spectral line that J coupling causes and splits a point effect so that signal is at t1Indirectly it is limited only by chemical shift effect in the dimension evolution time, simplifies spectrogram information.
Described diffusion order module is by two diffusion gradient GDConstitute with a �� non-selective radio frequency pulse; The interval time of two diffusion gradients is ��, i.e. diffusion time; For ensureing that signal is met again completely, the two diffusion gradient must be identical. In this module, obtain the signal amplitude change because molecule diffusion causes by diffusion gradient value one group descending, change according to the signal amplitude of gained and can simulate signaling molecule diffusion coefficient; Generally change number n of this group diffusion gradient value is set to 15��20, and ensure that minimum signal amplitude is maximum signal amplitudes 10%, to improve the accuracy of data fitting.
In step 3) in, the experiment parameter of described each module includes directly dimension spectrum width SW, indirectly dimension spectrum width SW1, one group of diffusion gradient intensity level GDAnd action time, diffusion time ��, it is concerned with and selects gradient intensity value G and action time, pi/2 and �� non-selective radio frequency pulse width, (pi/2)ISolvent selectivity RF pulse width, Time constant constant tau, indirectly dimension evolution phase t1The ni that counts, direct dimension sampling time t2��
In step 4) in, the detailed process of described execution data sampling is: often performing pulsatile once sequence, sample is carried out signal evolution effect by modules successively, finally at directly dimension sampling period t2Carry out data sampling; Above-mentioned sequence performs process simply to once indirectly tieing up t1Counting and the data of a specific diffusion gradient value are sampled, need to repeat ni �� n time for a complete data sampling, wherein n is that diffusion gradient changes number.
In step 5) in, described Data Post includes the extraction of the extraction of high-resolution One-Dimensional Pure chemical shift information dimension, the diffusion coefficient matching of signal and Error Calculation, diffusion dimension information, finally obtains the two-dimensional diffusion sequence spectrogram that diffusion coefficient pure chemistry displacement is relevant.
The present invention proposes a kind of high resolution nuclear magnetic resonance two-dimensional diffusion sequence spectral method that can be applicable to mix ingredients separation and composition analysis under any magnetic field environment, in the magnetic resonance detection of mixture, the spectral peak of various different materials is all presented in same spectrum, often leads to spectral peak crowded and be difficult to obtain correct composition ownership. Particularly in Magnetic field inhomogeneity situation, the uneven broadening effect of spectral line can cover spectroscopy information further, makes composition ownership become impossible. The present invention by combining diffusion sequence, permanent time develop and intermolecular zero quantum coherent technology realizes under any magnetic field environment (include field homogeneity situation and various sample and Magnetic field inhomogeneity situation that environmental factors causes) and obtains high resolution 2 d diffusion sequence spectrum, can be used for complex mixture composition and separate and composition analysis. First, the difference utilizing diffusion sequence Middle molecule diffusion coefficient realizes the separation of each component of mixture. Secondly, the elimination spectral line that develops when utilizing permanent splits point effect and obtains pure chemistry displacement information, simplifies spectrogram, it is achieved the two-dimensional diffusion sequence spectrum that diffusion coefficient chemical shift is associated. Finally, utilize the characteristic of intermolecular zero quantum coherent signal opposing non-uniform magnetic field to realize obtaining high-resolution diffusion sequence spectrum under any magnetic field environment, breach the limitation that existing diffusion sequence spectral method is applied at non-uniform magnetic field. This method is without the operation of any shimming and sample pretreatment process, simple and easy to do, and without any special hardware device, it is adaptable to any conventional nuclear magnetic resonance chemical analyser.
The present invention is by nuclear magnetic resonance pulse sequence design and corresponding data processing procedure, when utilizing diffusion order module and be permanent, genetic module is implemented in combination with the two-dimensional diffusion sequence spectrum that diffusion coefficient pure chemistry displacement is associated, effectively simplify and differentiate spectral peak information, it is simple to the separation of each component of mixture. The characteristic simultaneously utilizing intermolecular zero quantum coherent module opposing non-uniform magnetic field realizes under any magnetic field environment (include field homogeneity situation and various sample and Magnetic field inhomogeneity situation that environmental factors causes) and obtains high-resolution diffusion sequence spectrum, breaches the limitation that existing diffusion sequence spectral method is applied at non-uniform magnetic field. The present invention is easy to operation without the operation of any shimming and sample pretreatment process, and is applicable to any conventional nuclear magnetic resonance chemical analyser without any special hardware device, separates for complex mixture composition and component analysis provides a kind of effective means.
Accompanying drawing explanation
Fig. 1 is applied to blend sample composition to separate the pulse train used by spectral method of the high resolution 2 d diffusion sequence with component analysis, and wherein rectangular strip is pi/2 and �� non-selective radio frequency pulse, and the bar shaped of gaussian shape is (pi/2)ISolvent selectivity radio-frequency pulse, I represents solvent, and the rectangular block that oblique line is filled is select gradient G along Z-direction is linearly relevant, and the rectangular block that horizontal line is filled is along Z-direction diffusion gradient GD, �� is the diffusion time, t1CTGenetic module during for perseverance, t2For directly tieing up the sampling time.
The two-dimensional frequency spectrum that the method that Fig. 2 is proposed by the invention is applied under non-uniform magnetic field pyridine and propanol mixed solution is obtained, wherein dimension is for covering Magnetic field inhomogeneity degree 250Hz indirectly, and directly dimension is tieed up for high-resolution pure chemistry displacement. Carry out one-dimensional accumulation projection along directly dimension and just can extract high-resolution One-Dimensional Pure chemical shift information dimension.
Fig. 3 is that experimental data is tieed up after extraction through high-resolution One-Dimensional Pure chemical shift information, one-dimensional chemical shift dimensional signal amplitude of variation figure under diffusion gradient value effect one group descending in diffusion order module. Along with the enhancing of diffusion gradient value, signal is constantly decayed. Diffusion dimension information can be obtained by this series of signal being diffused Coefficient Fitting and Error Calculation thereof.
The high-resolution two-dimensional diffusion sequence spectrum that the method that Fig. 4 is proposed by the invention is applied under non-uniform magnetic field pyridine and propanol mixed solution obtains. Wherein vertical pivot is diffusion dimension information, and transverse axis is chemical shift information.
Detailed description of the invention
Method proposed by the invention (include field homogeneity situation and Magnetic field inhomogeneity situation that various sample causes with environmental factors) can obtain mix ingredients and separates and high resolution 2 d diffusion sequence spectrum needed for component analysis under any magnetic field environment. This method is easy to operation without the operation of any shimming and sample pretreatment process, and is applicable to any conventional nuclear magnetic resonance chemical analyser without any special hardware device, separates for complex mixture composition and component analysis provides a kind of effective means. Each step in specific implementation process of the present invention is as follows:
Step 1, the measurement of RF pulse width
Measurement including non-selective pulse and solvent selectivity pulse. Utilize conventional one-dimensional pulse sequence and a series of pulse operating time sampling corresponding signal is set, it is thus achieved that in the burst length corresponding to magnetization vector flip angle, also offer foundation being set for relevant spectrum width parameter simultaneously.
Step 2, the importing of pulse train used
On nuclear magnetic resonance spectrometer operating board, open spectrometer and operate software accordingly, import pulse train (as shown in Figure 1) compiled in advance, select specific test block, then call in above-mentioned pulse train.
Step 3, experiment parameter used by pulse train is arranged
Open each correlation module of imported pulse train, genetic module and diffusion order module during including intermolecular zero quantum coherent signal selection module, perseverance. Corresponding experiment parameter is set then according to detection sample practical situation, including including directly dimension spectrum width SW, indirectly dimension spectrum width SW1, one group of diffusion gradient intensity level GDAnd action time, diffusion time ��, it is concerned with and selects gradient intensity value G and action time, pi/2 and �� non-selective radio frequency pulse width, (pi/2)ISolvent selectivity RF pulse width, Time constant constant tau, indirectly dimension evolution phase t1The ni that counts, direct dimension sampling time t2. Wherein dimension spectrum width SW1 arranges the line width values being referred to conventional the obtained spectral line of one-dimensional spectrum of step 1 indirectly.
Step 4, data sampling
The detailed process of data sampling is: often performing pulsatile once sequence, sample is carried out signal evolution effect by modules successively, finally at directly dimension sampling period t2Carry out data sampling. Above-mentioned sequence performs process simply to once indirectly tieing up t1Counting and the data of a specific diffusion gradient value are sampled, need to repeat ni �� n time for a complete data sampling, wherein n is that diffusion gradient changes number.After completing a sampled data, performing next step, otherwise continuing sampling until having sampled.
Step 5, Data Post
The extraction of extraction, the diffusion coefficient matching of signal and Error Calculation, diffusion dimension information that high-resolution One-Dimensional Pure chemical shift information is tieed up, finally obtains the two-dimensional diffusion sequence spectrogram that diffusion coefficient pure chemistry displacement is relevant.
Below in conjunction with drawings and Examples, the present invention will be further described:
The sample that the present embodiment uses is the mixed solution of a kind of pyridine and propanol, and instrument used is a Varian500MHz NMR (Nuclear Magnetic Resonance) spectrum view. In whole experimentation, main field remains uneven. According to the operating process of the invention described above proposed method, measure the RF pulse width used by pulse train, and record Magnetic field inhomogeneity degree in this experiment and be about 250Hz. Then, importing compiled pulse train as shown in Figure 1, open each correlation module of pulse train, during including intermolecular zero quantum coherent signal selection module, perseverance, genetic module and diffusion order module, arrange corresponding experiment parameter. Particularly for the sample that the present embodiment adopts, its experiment parameter is provided that directly dimension spectrum width SW is 5000Hz; Dimension spectrum width SW1 is 320Hz indirectly; One group of diffusion gradient intensity level GD, wherein minima 2.0G/cm, maximum 40G/cm, totally 20 step, the gradient effect time is 1.0ms; Diffusion time �� is 60ms; Relevant selection gradient intensity value G1For 10.0G/cm and action time 1.2ms, pi/2 and �� non-selective radio frequency pulse width respectively 11 �� s and 22 �� s; (pi/2)ISolvent selectivity RF pulse width is 8.3ms; Time constant constant tau is 50ms; Dimension evolution phase t indirectly1The ni that counts be 30; Directly dimension sampling time t2For 15ms. The whole experiment sampling time is 20min.
After data sampling completes, according to the Data Post process of above-mentioned steps 5, the sampled data obtained is processed. First it is the extraction process of high-resolution One-Dimensional Pure chemical shift information dimension, carries out two-dimensional Fourier transform and rotation transformation can obtain two-dimensional spectrum as shown in Figure 2 by the direct peacekeeping of data is tieed up indirectly. In this two-dimensional spectrum, dimension is for covering Magnetic field inhomogeneity degree 250Hz indirectly, and directly dimension is eliminate the high-resolution pure chemistry displacement information of Magnetic field inhomogeneity impact. Carry out one-dimensional accumulation projection along directly dimension and just can extract high-resolution One-Dimensional Pure chemical shift information dimension. Secondly, the extraction of the diffusion coefficient matching of signal and Error Calculation, diffusion dimension information. After high-resolution One-Dimensional Pure chemical shift information dimension is extracted, obtained data eliminate the impact of Magnetic field inhomogeneity. But data are subject to the diffusion that diffusion gradient value one group descending in diffusion order module produces, its signal amplitude shown as in One-Dimensional Pure chemical shift information dimension increases along with diffusion gradient value and constantly decays (as shown in Figure 3). Diffusion information dimension can be obtained by this series of signal being diffused Coefficient Fitting and Error Calculation thereof. Finally, spread information dimension in conjunction with pure chemistry displacement information peacekeeping and can reconstruct the high resolution 2 d diffusion sequence spectrum of pyridine and propanol mixed solution, as shown in Figure 4. Can intuitively finding out, this two-dimensional diffusion sequence spectrum has been completely free of the interference of magnetic field bump, and wherein vertical pivot is diffusion information dimension, and transverse axis is chemical shift dimension. Pyridine and alcohol component correspond to different molecule diffusion properties, show as different diffusion coefficients on vertical pivot, can realize the separation of both compositions in plotted.As shown in Figure 4, green dotted line is isolated propanol signal, and red dotted line is isolated pyridine signal. In sample, the content of pyridine and alcohol component also has difference, and the difference of this content chemically displacement can tie up upper acquisition, and both components can be carried out relevant content analysis by the spectral strength above corresponding by measuring chemical shift dimension.
Claims (9)
1. the nuclear magnetic resonance, NMR two-dimensional diffusion sequence spectral method for any magnetic field environment, it is characterised in that comprise the steps:
1) measuring samples excites required pi/2 non-selective radio frequency pulse width and (pi/2)ISolvent selectivity RF pulse width;
2) on nuclear magnetic resonance chemical analyser, nuclear magnetic resonance pulse sequence is imported;
3) open genetic module and diffusion order module when the intermolecular zero quantum coherent signal selection module of nuclear magnetic resonance pulse sequence, perseverance, the experiment parameter of each module is set;
4) data sampling is performed;
5) carry out Data Post, obtain high resolution 2 d diffusion sequence spectrum.
2. a kind of nuclear magnetic resonance, NMR two-dimensional diffusion for any magnetic field environment sorts spectral method as claimed in claim 1, it is characterized in that in step 1) in, described measuring samples excites required pi/2 non-selective radio frequency pulse width to be utilize conventional one-dimensional pulse sequence to complete, by arranging a series of pulse operating time sampling corresponding signal, burst length corresponding when obtaining magnetization vector 90 degree upset is pi/2 non-selective radio frequency pulse width, this measurement simultaneously also obtain field homogeneity implementations, for spectrum width parameter, offer foundation, described (pi/2) are setIThe measurement of solvent selectivity RF pulse width is to be completed by conventional one-dimensional soft pulse sequence, it is thus achieved that selective pulse action time corresponding during solvent magnetization vector 90 degree upset.
3. a kind of nuclear magnetic resonance, NMR two-dimensional diffusion for any magnetic field environment sorts spectral method as claimed in claim 1, it is characterized in that in step 2) in, described nuclear magnetic resonance pulse sequence employs genetic module and diffusion order module when intermolecular zero quantum coherent signal selection module, perseverance.
4. a kind of nuclear magnetic resonance, NMR two-dimensional diffusion for any magnetic field environment sorts spectral method as claimed in claim 1, it is characterized in that in step 2) in, described intermolecular zero quantum coherent signal selection module is by a pi/2 non-selective radio frequency pulse, one (pi/2)ISolvent selectivity radio-frequency pulse and a relevant selection gradient G are constituted; It is solvent and the difference of resonant frequency of solute spin by its resonant frequency of signal selected by intermolecular zero quantum coherent signal selection module; In Magnetic field inhomogeneity situation, the difference of the resonant frequency between solvent and solute can eliminate the impact of Magnetic field inhomogeneity and obtain high-resolution spectroscopy information; In field homogeneity situation, high-resolution spectroscopy information can also be obtained equally.
5. a kind of nuclear magnetic resonance, NMR two-dimensional diffusion for any magnetic field environment sorts spectral method as claimed in claim 1, it is characterised in that in step 2) in, described permanent time genetic module be by t1/2����(��-t1/ 2) composition, t1For indirectly tieing up the evolution time, �� is the Time constant constant set, and is generally a few tens of milliseconds; Time permanent, genetic module can eliminate the spectral line that J coupling causes and splits a point effect so that signal is at t1Indirectly it is limited only by chemical shift effect in the dimension evolution time, simplifies spectrogram information.
6. a kind of nuclear magnetic resonance, NMR two-dimensional diffusion for any magnetic field environment sorts spectral method as claimed in claim 1, it is characterised in that in step 2) in, described diffusion order module is by two diffusion gradient GDConstitute with a �� non-selective radio frequency pulse;The interval time of two diffusion gradients is ��, i.e. diffusion time; For ensureing that signal is met again completely, the two diffusion gradient must be identical; In this module, obtain the signal amplitude change because molecule diffusion causes by diffusion gradient value one group descending, change according to the signal amplitude of gained and can simulate signaling molecule diffusion coefficient; Generally change number n of this group diffusion gradient value is set to 15��20, and ensure that minimum signal amplitude is maximum signal amplitudes 10%, to improve the accuracy of data fitting.
7. a kind of nuclear magnetic resonance, NMR two-dimensional diffusion for any magnetic field environment sorts spectral method as claimed in claim 1, it is characterized in that in step 3) in, the experiment parameter of described each module includes directly dimension spectrum width SW, indirectly dimension spectrum width SW1, one group of diffusion gradient intensity level GDAnd action time, diffusion time ��, it is concerned with and selects gradient intensity value G and action time, pi/2 and �� non-selective radio frequency pulse width, (pi/2)ISolvent selectivity RF pulse width, Time constant constant tau, indirectly dimension evolution phase t1The ni that counts, direct dimension sampling time t2��
8. a kind of nuclear magnetic resonance, NMR two-dimensional diffusion for any magnetic field environment sorts spectral method as claimed in claim 1, it is characterized in that in step 4) in, the detailed process of described execution data sampling is: often perform pulsatile once sequence, sample is carried out signal evolution effect by modules successively, finally at directly dimension sampling period t2Carry out data sampling; Above-mentioned sequence performs process simply to once indirectly tieing up t1Counting and the data of a specific diffusion gradient value are sampled, need to repeat ni �� n time for a complete data sampling, wherein n is that diffusion gradient changes number.
9. a kind of nuclear magnetic resonance, NMR two-dimensional diffusion for any magnetic field environment sorts spectral method as claimed in claim 1, it is characterized in that in step 5) in, described Data Post includes the extraction of the extraction of high-resolution One-Dimensional Pure chemical shift information dimension, the diffusion coefficient matching of signal and Error Calculation, diffusion dimension information, finally obtains the two-dimensional diffusion sequence spectrogram that diffusion coefficient pure chemistry displacement is relevant.
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| CN109636725B (en) * | 2018-12-13 | 2022-05-17 | 厦门大学 | High-resolution reconstruction method of magnetic resonance diffusion sequencing spectrum |
| CN110044944A (en) * | 2019-04-22 | 2019-07-23 | 中国科学院山西煤炭化学研究所 | A kind of magnetic resonance detection method for F- T synthesis waste water component analysis |
| CN110361681A (en) * | 2019-06-21 | 2019-10-22 | 厦门大学 | A method of improving pure chemistry displacement spectra signal-to-noise ratio under non-uniform magnetic field |
| CN113049623A (en) * | 2019-12-11 | 2021-06-29 | 日本电子株式会社 | Nuclear magnetic resonance measuring method and apparatus |
| CN113049623B (en) * | 2019-12-11 | 2023-12-12 | 日本电子株式会社 | Nuclear magnetic resonance measurement method and device |
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