CN104849298A - Sample testing analysis meter and method for nuclear magnetism analysis - Google Patents
Sample testing analysis meter and method for nuclear magnetism analysis Download PDFInfo
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Abstract
The invention discloses a sample testing analysis meter and method for nuclear magnetism analysis. The sample testing analysis meter comprises a gas ionizer, an ion flow generator, an ion flow concentrator, a particle mass filter, an optical lens device, a sample injector, a particle beam controller, an optical signal transduction device, an electric field analyzer, a particle energy analyzer, a signal refractor, a motional magnetic field resolver, a particle conductor, a signal concentrator, a particle electric field controller, a particle channel plate, a fluorescent display screen, a signal observer, a particle camera, a video signal transduction device, a particle multiplier and a computer. The gas ionizer is connected with the ion flow concentrator through a composite conduit made of polyether-ether-ketone chlorobenzene hydrazine. The gas ionizer comprises a high frequency ionization tube; a pipe network coil and M-type electrodes are wound outside the high frequency ionization tube, the pipe network coil is located in the middle outside the high frequency ionization tube, and the M-type electrodes are located at two end parts outside the high frequency ionization tube.
Description
Technical field
The present invention relates to sample detection analyser and method, particularly a kind of sample detection analyser for nmr analysis and method.
Background technology
Sample detection analysis principle for nmr analysis is based on the non-vanishing atomic nucleus of magnetic moment, energy level generation Zeeman splitting of spinning under outside magnetic field effect, the physical process of the radio-frequency radiation of resonance absorption certain frequency.Nmr analysis is a branch of spectroscopy, and its resonant frequency is in radio-frequency range, and corresponding transition is the transition of nuclear spin in core Zeeman level.Nowadays the nmr analysis technology used often adopts CW-NMR analytical technology, although this technical scheme is cheap, temperature, easy to operate, but poor sensitivity, need sample size large, and core as very high in 1H/19F/31P and so on natural abundance can only be measured, then cannot measure the low-abundance core of such as 13C and so on.Therefore, the Improvement and perfection in addition for prior art is necessary.
Summary of the invention
The object of the invention is to, carry out detecting the nmr analysis poor sensitivity in analytic process to sample again for overcoming prior art, need sample size large, and the very high core of natural abundance can only be measured, to low-abundance core then unmeasured defect, thus provide a kind of sample detection analyser for nmr analysis and method.
For achieving the above object, the invention provides a kind of sample detection analyser for nmr analysis, it is characterized in that, comprise: Gas Ionizer, the stage casing of its high frequency ionization tube is wound with pipe network coil, and its one end is provided with positive pole M type electrode, and the other end is provided with negative pole M type electrode;
Ion current manifold, it is connected with mass particle filtrator with described Gas Ionizer, ion airflow generator respectively by ion current conduit; Described ion airflow generator is positioned at the below of described Gas Ionizer, and it comprises positive stepup transformer and negative stepup transformer; Described mass particle filtrator is connected with optical lens device;
Described optical lens is connected with light signal transduction device with particle beams controller respectively, and be connected with injector by photoelectric sensor, described light signal transduction device is also connected with analysis of electric field device, described analysis of electric field device is also connected with particle energy analyzer, and is provided with particle sizing plate in it;
Described particle beams controller comprises the particle bombardment plate being located at its front end, and the anion electrode in portion located therein, control electrode and cation electrode successively from front to back;
Described particle energy analyzer is connected with signal refractor, and described signal refractor is also connected with moving magnetic field resolver, and described moving magnetic field resolver is connected with particle conduction device, and described particle conduction device is also connected with signal manifold;
Described signal manifold is connected with particle control device of electric field, and described particle control device of electric field is connected with particle multiplier with particle channel plate respectively; Described particle channel plate is connected with fluorescent display screen, and described fluorescent display screen is connected with vision signal transmitter with signal observer, particle image pick-up device respectively; Described particle multiplier is also connected with computing machine.
Preferably, described light signal transduction device comprises ground floor photoelectricity conversion thin film and second layer photoelectricity conversion thin film; The thickness of described ground floor photoelectricity conversion thin film is 3.66 microns-5.89 microns, and the thickness of described second layer photoelectricity conversion thin film is 8.67 microns-11.76 microns;
Preferably, described ion current conduit is arranged at the below of described negative pole M type electrode, and it is polyetherketone acetyl nitrile azoles ester composite material tube.
Preferably, the left side of the positive pole M type electrode of described Gas Ionizer has extraction electrode, and has sparking electrode on the right side of it.
Preferably, described particle sizing plate offers three circular holes, and three described circular holes are arranged in a linear, from top to bottom, the diameter of three described circular holes is respectively: 5nm, 8nm, 12nm.
The present invention also provides a kind of sample detection analytical approach for nmr analysis, comprises the following steps:
1) testing sample is carried out high-frequency discharge after having been gasified by Gas Ionizer sample gas is ionized, and produces low charge state positive ion; Then in the high-frequency electric field of Gas Ionizer, charged ion and sample atoms and molecular collision, make ionized sample molecule, and charged particle multiplication forms electrodless discharge, produces a large amount of sample belt electron ion;
2) in step 1) in, charged ion coordinates with negative stepup transformer the negative ions producing different charge ratio by the positive stepup transformer contained in ion airflow generator, and then the negative ions produced is passed through ion current conduit to ion current manifold by ion airflow generator;
3) ion current manifold accepts from the ion current of Gas Ionizer, ion airflow generator, then the ion current after collecting is transferred to mass particle filtrator;
4) after mass particle filtrator accepts the ion current of ion current manifold transmission, carry out screening and filtering according to the difference of mass of ion and ionic charge, and the ion signal after screening is converted to optical signal transmission to optical lens device;
5) optical lens device accepts the light signal of mass particle filter transmission, accept simultaneously from injector introduce sample analysis test signal and particle beams controller to the control signal of particle beams direction and intensity, carry out light signal converting transmission, and then transfer signals to light signal transduction device;
6) light signal transduction device accepts the signal that optical lens transmits, and by the Signal transmissions that receives in analysis of electric field device;
7) analysis of electric field device accepts the signal of light signal transduction device transmission, and is sent in particle energy analyzer by the signal after process;
8) particle energy analyzer accepts the signal transmission of analysis of electric field device, the particle of screening different-energy size, then by the Particle Delivery after analyzing to signal refractor;
9) signal refractor accepts the particle from particle energy analyzer, controls the change in light signal transduction direction, and is sent in moving magnetic field resolver by the particle signal after process and particle;
10) moving magnetic field resolver accepts from the particle signal of signal refractor and particle, by the movement locus of introduction by magnetic field particle, then by particle signal and Particle Delivery to particle conduction device;
11) particle conduction device accepts particle signal and the particle of moving magnetic field resolver, controls the conduction path length of particle conveying channels, then by particle conduction signal and Particle Delivery to signal manifold;
12) signal manifold accepts from the particle conduction signal of particle conduction device and particle, control signal and particle-stabilised, then by the particle signal after collecting and Particle Delivery to particle control device of electric field;
13) particle control device of electric field accepts, from the particle signal of signal manifold and particle, to control particle running status by electrostatic field, then by Particle Delivery to particle channel plate, particle and particle signal are transferred to particle multiplier;
14) particle multiplier accepts particle from the transmission of particle control device of electric field and particle signal, adjustment and control the motion state of particle, then by particle analysis Signal transmissions to computing machine;
15) computing machine accepts the particle analysis signal from particle multiplier, analyzes sample particle and detects data, preserve testing result.
Further, the control signal of particle beams direction and intensity is transferred to optical lens device by described particle beams controller.
Further, the test signal of sample is transferred to optical lens device by described injector.
Further, described particle channel plate accepts the particle from the transmission of particle control device of electric field, the shape of the restriction particle beams, strengthen particle energy, the particle of high velocity impact on inwall passage is increased, and it is incremental to carry out particle, then by Particle Delivery to fluorescent display screen;
Fluorescent display screen accepts the transmission particle from particle channel plate, by the picture signal that detection of particles signal is changed, the form changed with brightness at receiving end is reappeared on video screen, and particle signal is transferred to signal observer, particle image pick-up device, vision signal transmitter;
Signal observer accepts the particle signal from fluorescent display screen, observing samples particle analysis signal; Particle image pick-up device accepts the particle signal from fluorescent display screen, record particle analysis signal; Vision signal transmitter accepts the particle signal from fluorescent display screen, conducting particles analytic signal.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of the sample detection analyser for nmr analysis;
Fig. 2 is the molecular structure A of sample 1;
Fig. 3 is the molecular structure B of sample 1;
Fig. 4 is the testing result of sample 1 by a kind of sample detection analyser for nmr analysis;
Fig. 5 is the molecular structure A of sample 2;
Fig. 6 is the molecular structure B of sample 2;
Fig. 7 is the testing result of sample 2 by a kind of sample detection analyser for nmr analysis.
Description of reference numerals:
1, Gas Ionizer 2, ion airflow generator 3, ion current manifold 4, mass particle filtrator 5, optical lens device 6, injector 7, particle beams controller 8, light signal transduction device 9, analysis of electric field device 10, particle energy analyzer 11, signal refractor 12, moving magnetic field resolver 13, particle conduction device 14, signal manifold 15, particle control device of electric field 16, particle channel plate 17, fluorescent display screen 18, signal observer 19, particle image pick-up device 20, vision signal transmitter 21, particle multiplier 22, computing machine
Embodiment
The present invention is illustrated below in conjunction with accompanying drawing and further detailed description in detail.It is pointed out that following explanation is only illustrating the technical scheme that application claims is protected, any restriction not to these technical schemes.
The content that protection scope of the present invention is recorded with appended claims is as the criterion.
As shown in Figure 1, sample detection analyser provided by the present invention comprises Gas Ionizer 1, ion airflow generator 2, ion current manifold 3, mass particle filtrator 4, optical lens device 5, injector 6, particle beams controller 7, light signal transduction device 8, analysis of electric field device 9, particle energy analyzer 10, signal refractor 11, moving magnetic field resolver 12, particle conduction device 13, signal manifold 14, particle control device of electric field 15, particle channel plate 16, fluorescent display screen 17, signal observer 18, particle image pick-up device 19, vision signal transmitter 20, particle multiplier 21, computing machine 22,
Wherein, Gas Ionizer 1 is connected with ion current manifold by the compound substance conduit of polyetheretherketone chlorophenyl hydrazine, Gas Ionizer 1 is containing high frequency ionization tube, high frequency ionization tube is around with pipe network coil and M type electrode, and pipe network coil is positioned at the middle part outside ionization tube, and M type electrode is positioned at the two-end part outside ionization tube, upper end M type electrode makes positive pole, what electrode material adopted is the compound substance of hafnium carbide silicon, and lower end M type electrode makes negative pole, the compound substance of what electrode material adopted is silicic acid chromium rhenium; Ion current guiding tube is contained in the below of the negative pole M type electrode of Gas Ionizer 1, and guide the ion current in Gas Ionizer to enter ion current manifold, the material of this ion current guiding tube is the compound substance of polyetherketone acetyl nitrile azoles ester; The left side of the positive pole M type electrode of Gas Ionizer 1 has extraction electrode, right side has sparking electrode, stationary magnetic field is produced by extraction electrode, high-frequency discharge is carried out again by sparking electrode, the cooperation of extraction electrode and sparking electrode, produces the ion concentration in non-uniform magnetic-field raising region of discharge by current resonance.
Above-mentioned ion airflow generator 2 is positioned at the below of Gas Ionizer 1, and is connected with ion current manifold 3 by ion current conduit; Ion airflow generator 2 is interior containing positive stepup transformer and negative stepup transformer, and positive stepup transformer coordinates with negative stepup transformer the negative ions producing different charge ratio, and then the negative ions produced is passed through ion current conduit to ion current manifold by ion airflow generator.
Above-mentioned ion current manifold 3 is connected with Gas Ionizer 1, ion airflow generator 2, mass particle filtrator 4 respectively, ion current manifold 3 accepts the ion current from Gas Ionizer 1, ion airflow generator 2, then the ion current after collecting is transferred to mass particle filtrator 4.Above-mentioned mass particle filtrator 4 is connected with optical lens device 5 with ion current manifold 3 respectively, after mass particle filtrator 4 accepts the ion current of ion current manifold 3 transmission, carry out screening and filtering according to the difference of mass of ion and ionic charge, and the ion signal after screening is converted to optical signal transmission to optical lens device 5.
This optical lens device 5 is connected with particle beams controller 7, light signal transduction device 8 with mass particle filtrator 4, injector 6 respectively, optical lens device 5 accepts the light signal that mass particle filtrator 4 transmits, accept the control signal of sample analysis test signal and the particle beams controller 7 pairs of particle beams direction and intensities introduced from injector 6 simultaneously, carry out light signal converting transmission, and then transfer signals to light signal transduction device 8.
Above-mentioned injector 6 is connected by photoelectric sensor with optical lens device 5, and the photoelectric signal transformation material of this photoelectric sensor is monox ring toluene fluoride, and sample analysis test signal is transferred to optical lens device 5 by injector.
Above-mentioned particle beams controller 7 is connected with optical lens device 5, and the control signal of particle beams direction and intensity is transferred to optical lens device 5 by particle beams controller 7; The below of particle beams controller 7 comprises a base, submount material is poly-methyl ether aniline, the front end of particle beams controller 7 comprises particle bombardment plate, this bombardment sheet material matter is poly-ethyl ester acyl chlorides, the middle part of particle beams controller 7 comprises an anion electrode, control electrode, a cation electrode, three kinds of electrodes put in order for: anion electrode is positioned at leading portion, control electrode is positioned at centre, cation electrode is positioned at tail end, by anion electrode, control electrode, the cooperatively interacting of cation electrode, regulate speed and the angle of the particle beams.
Above-mentioned light signal transduction device 8 is connected with analysis of electric field device 9 with optical lens device 5 respectively, and light signal transduction device 8 accepts the signal that optical lens device 5 transmits, and by the Signal transmissions that receives in analysis of electric field device 9; Light signal transduction device 8 is containing two layers of photoelectricity conversion thin film, ground floor membraneous material is the nano composite material of triamido Sulforidazine ketone, film thickness is 3.66 microns---5.89 microns, second layer membraneous material is the nano composite material of three amidine phenyl aldoximes, and film thickness is 8.67 microns---11.76 microns; Light signal, by two layers of photoelectricity conversion thin film, improves transmission conversion efficiency and the conductive mass of photosignal.
Above-mentioned analysis of electric field device 9 is connected with light signal transduction device 8, particle energy analyzer 10 respectively, analysis of electric field device 9 accepts the signal that light signal transduction device 8 transmits, and the signal after process is sent in particle energy analyzer 10, analysis of electric field device 9 is containing particle sizing plate, and particle sizing plate material is polypyrrole acetyl nitrile, and three circular holes are contained in the centre of particle sizing plate, three circular holes are arranged in a linear, the diameter of three circular holes is respectively from top to bottom: 5nm, 8nm, 12nm.
Above-mentioned particle energy analyzer 10 is connected with signal refractor 11 with analysis of electric field device 9 respectively, particle energy analyzer 10 accepts the signal transmission of analysis of electric field device 9, the particle of screening different-energy size, then by the Particle Delivery after analyzing to signal refractor 11.
Above-mentioned signal refractor 11 is connected with moving magnetic field resolver 12 with particle energy analyzer 10 respectively, signal refractor 11 accepts the particle from particle energy analyzer 10, control the change in light signal transduction direction, and the particle signal after process and particle be sent in moving magnetic field resolver 12.
Above-mentioned moving magnetic field resolver 12 is connected with particle conduction device 13 with signal refractor 11 respectively, moving magnetic field resolver 12 accepts particle signal from signal refractor 11 and particle, by the movement locus of introduction by magnetic field particle, then by particle signal and Particle Delivery to particle conduction device 13.
Above-mentioned particle conduction device 13 is connected with signal manifold 14 with moving magnetic field resolver 12 respectively, particle conduction device 13 accepts particle signal and the particle of moving magnetic field resolver 12, control the conduction path length of particle conveying channels, then by particle conduction signal and Particle Delivery to signal manifold 14.
Above-mentioned signal manifold 14 is connected with particle control device of electric field 15 with particle conduction device 13 respectively, signal manifold 14 accepts particle conduction signal from particle conduction device 13 and particle, control signal and particle-stabilised, then by the particle signal after collecting and Particle Delivery to particle control device of electric field 15.
Above-mentioned particle control device of electric field 15 is connected with signal manifold 14, particle channel plate 16, particle multiplier 21 respectively, particle control device of electric field 15 accepts particle signal from signal manifold 14 and particle, particle running status is controlled by electrostatic field, then by Particle Delivery to particle channel plate 16, particle and particle signal are transferred to particle multiplier 21.
Above-mentioned particle channel plate 16 is connected with fluorescent display screen 17 with particle control device of electric field 15 respectively, particle channel plate 16 accepts the particle from the transmission of particle control device of electric field, the shape of the restriction particle beams, strengthen particle energy, the particle of high velocity impact on inwall passage is increased, carry out particle incremental, then by Particle Delivery to fluorescent display screen 17.
Above-mentioned fluorescent display screen 17 is connected with particle channel plate 16, signal observer 18, particle image pick-up device 19, vision signal transmitter 20 respectively, fluorescent display screen 17 accepts the transmission particle from particle channel plate 16, by the picture signal that detection of particles signal is changed, the form changed with brightness at receiving end is reappeared on fluorescent display screen 17, and particle signal is transferred to signal observer 18, particle image pick-up device 19, vision signal transmitter 20.
Above-mentioned signal observer 18 is connected with fluorescent display screen 17, and signal observer 18 accepts the particle signal from fluorescent display screen 17, observing samples particle analysis signal.
Above-mentioned particle image pick-up device 19 is connected with fluorescent display screen 17, and particle image pick-up device 19 accepts the particle signal from fluorescent display screen 17, record particle analysis signal.
Above-mentioned vision signal transmitter 20 is connected with fluorescent display screen 17, and vision signal transmitter 20 accepts the particle signal from fluorescent display screen 17, conducting particles analytic signal.
Above-mentioned particle multiplier 21 is connected with particle control device of electric field 15, computing machine 22 respectively, particle multiplier 21 accept from particle control device of electric field 15 transmit particle and particle signal, adjustment and control the motion state of particle, then by particle analysis Signal transmissions to computing machine 22.
Above computer 22 is connected with particle multiplier 21, and computing machine 22 accepts the particle analysis signal of particle multiplier 21, analyzes high energy particle and detects data, preserve testing result.
The present invention also provides a kind of sample detection analytical approach for nmr analysis, comprises the following steps:
1) testing sample is carried out high-frequency discharge after having been gasified by Gas Ionizer sample gas is ionized, and produces low charge state positive ion; Then in the high-frequency electric field of Gas Ionizer, charged ion and sample atoms and molecular collision, make ionized sample molecule, and charged particle multiplication forms electrodless discharge, produces a large amount of sample belt electron ion;
2) in step 1) in, charged ion coordinates with negative stepup transformer the negative ions producing different charge ratio by the positive stepup transformer contained in ion airflow generator, and then the negative ions produced is passed through ion current conduit to ion current manifold by ion airflow generator;
3) ion current manifold accepts from the ion current of Gas Ionizer, ion airflow generator, then the ion current after collecting is transferred to mass particle filtrator;
4) after mass particle filtrator accepts the ion current of ion current manifold transmission, carry out screening and filtering according to the difference of mass of ion and ionic charge, and the ion signal after screening is converted to optical signal transmission to optical lens device;
5) optical lens device accepts the light signal of mass particle filter transmission, accept simultaneously from injector introduce sample analysis test signal and particle beams controller to the control signal of particle beams direction and intensity, carry out light signal converting transmission, and then transfer signals to light signal transduction device;
6) light signal transduction device accepts the signal that optical lens transmits, and by the Signal transmissions that receives in analysis of electric field device;
7) analysis of electric field device accepts the signal of light signal transduction device transmission, and is sent in particle energy analyzer by the signal after process;
8) particle energy analyzer accepts the signal transmission of analysis of electric field device, the particle of screening different-energy size, then by the Particle Delivery after analyzing to signal refractor;
9) signal refractor accepts the particle from particle energy analyzer, controls the change in light signal transduction direction, and is sent in moving magnetic field resolver by the particle signal after process and particle;
10) moving magnetic field resolver accepts from the particle signal of signal refractor and particle, by the movement locus of introduction by magnetic field particle, then by particle signal and Particle Delivery to particle conduction device;
11) particle conduction device accepts particle signal and the particle of moving magnetic field resolver, controls the conduction path length of particle conveying channels, then by particle conduction signal and Particle Delivery to signal manifold;
12) signal manifold accepts from the particle conduction signal of particle conduction device and particle, control signal and particle-stabilised, then by the particle signal after collecting and Particle Delivery to particle control device of electric field;
13) particle control device of electric field accepts, from the particle signal of signal manifold and particle, to control particle running status by electrostatic field, then by Particle Delivery to particle channel plate, particle and particle signal are transferred to particle multiplier;
14) particle multiplier accepts particle from the transmission of particle control device of electric field and particle signal, adjustment and control the motion state of particle, then by particle analysis Signal transmissions to computing machine;
15) computing machine accepts the particle analysis signal from particle multiplier, analyzes sample particle and detects data, preserve testing result.
Further, the control signal of particle beams direction and intensity is transferred to optical lens device by described particle beams controller.
Further, the test signal of sample is transferred to optical lens device by described injector.
Further, described particle channel plate accepts the particle from the transmission of particle control device of electric field, the shape of the restriction particle beams, strengthen particle energy, the particle of high velocity impact on inwall passage is increased, and it is incremental to carry out particle, then by Particle Delivery to fluorescent display screen;
Fluorescent display screen accepts the transmission particle from particle channel plate, by the picture signal that detection of particles signal is changed, the form changed with brightness at receiving end is reappeared on video screen, and particle signal is transferred to signal observer, particle image pick-up device, vision signal transmitter;
Signal observer accepts the particle signal from fluorescent display screen, observing samples particle analysis signal; Particle image pick-up device accepts the particle signal from fluorescent display screen, record particle analysis signal; Vision signal transmitter accepts the particle signal from fluorescent display screen, conducting particles analytic signal.Below for a kind of sample detection analyser for nmr analysis carries out the case study on implementation of analytical test to different sample:
Sample 1:
(4-sulfamoyl phenyl amino) methanesulfonic sodium carries out high-frequency discharge after having been gasified by Gas Ionizer that sample gas is ionized, and produces low charge state positive ion; Then in the high-frequency electric field of Gas Ionizer, charged ion and sample atoms and molecular collision, make ionized sample molecule, and charged particle multiplication forms electrodless discharge, produces a large amount of sample belt electron ion;
Then the positive stepup transformer by containing in ion airflow generator 2 coordinates with negative stepup transformer the negative ions producing different charge ratio, and then the negative ions produced is passed through ion current conduit to ion current manifold by ion airflow generator; Ion current manifold accepts from the ion current of Gas Ionizer, ion airflow generator, then the ion current after collecting is transferred to mass particle filtrator;
Mass particle filtrator 4 carries out screening and filtering according to the difference of mass of ion and ionic charge after accepting the ion current of ion current manifold transmission, and the ion signal after screening is converted to optical signal transmission to optical lens device 5; Optical lens device accepts the light signal of mass particle filter transmission, accept simultaneously from injector introduce sample analysis test signal and particle beams controller to the control signal of particle beams direction and intensity, carry out light signal converting transmission, and then transfer signals to light signal transduction device; Then, by injector, the test signal of (4-sulfamoyl phenyl is amino) methanesulfonic sodium and test solvent MSO-d6 is transferred to optical lens device;
Then, the control signal of particle beams direction and intensity is transferred to optical lens device by particle beams controller; Light signal transduction device accepts the signal that optical lens transmits, and by the Signal transmissions that receives in analysis of electric field device;
Then, analysis of electric field device accepts the signal of light signal transduction device transmission, and is sent in particle energy analyzer by the signal after process, and particle energy analyzer accepts the signal transmission of analysis of electric field device, the particle of screening different-energy size, then by the Particle Delivery after analyzing to signal refractor;
Signal refractor accepts the particle from particle energy analyzer, controls the change in light signal transduction direction, and is sent in moving magnetic field resolver by the particle signal after process and particle; Moving magnetic field resolver accepts from the particle signal of signal refractor and particle, by the movement locus of introduction by magnetic field particle, then by particle signal and Particle Delivery to particle conduction device;
Particle conduction device accepts particle signal and the particle of moving magnetic field resolver, controls the conduction path length of particle conveying channels, then by particle conduction signal and Particle Delivery to signal manifold; Then, signal manifold accepts from the particle conduction signal of particle conduction device and particle, control signal and particle-stabilised, then by the particle signal after collecting and Particle Delivery to particle control device of electric field; Particle control device of electric field accepts, from the particle signal of signal manifold and particle, to control particle running status by electrostatic field, then by Particle Delivery to particle channel plate, particle and particle signal are transferred to particle multiplier;
Particle channel plate accepts the particle from the transmission of particle control device of electric field, and the shape of the restriction particle beams, strengthens particle energy, and the particle of high velocity impact on inwall passage is increased, and it is incremental to carry out particle, then by Particle Delivery to fluorescent display screen;
Fluorescent display screen receives the transmission particle from particle channel plate, by the picture signal that detection of particles signal is changed, the form changed with brightness at receiving end is reappeared on video screen, and particle signal is transferred to signal observer, particle image pick-up device, vision signal transmitter;
Signal observer accepts the particle signal from fluorescent display screen, observing samples particle analysis signal; Then, particle image pick-up device accepts the particle signal from fluorescent display screen, record particle analysis signal; Then, vision signal transmitter accepts the particle signal from fluorescent display screen, conducting particles analytic signal;
Particle multiplier accepts particle from the transmission of particle control device of electric field and particle signal, adjustment and control the motion state of particle, then by particle analysis Signal transmissions to computing machine;
Computing machine accepts the particle analysis signal from particle multiplier, analyzes sample particle and detects data, preserve testing result.
Its analysis result is as shown in Fig. 2-Fig. 4 and table 1.
Table 1: sample 1 is by a kind of analysis result of the sample detection analyser for nmr analysis
Sample 2:
| Sample ID: | Cyanobenzene |
| Molecular formula: | C7H5N |
| Molecular weight: | 103 |
| Test solvent: | CDCl3 |
| Test reference: | TMS |
Carrying out high-frequency discharge after cyanophenyl has been gasified by Gas Ionizer makes sample gas ionize, and produces low charge state positive ion; Then in the high-frequency electric field of Gas Ionizer, charged ion and sample atoms and molecular collision, make ionized sample molecule, charged particle multiplication forms electrodless discharge, produce a large amount of sample belt electron ion, then the positive stepup transformer by containing in ion airflow generator 2 coordinates with negative stepup transformer the negative ions producing different charge ratio, and then the negative ions produced is passed through ion current conduit to ion current manifold by ion airflow generator; Ion current manifold accepts from the ion current of Gas Ionizer, ion airflow generator, then the ion current after collecting is transferred to mass particle filtrator; Mass particle filtrator 4 carries out screening and filtering according to the difference of mass of ion and ionic charge after accepting the ion current of ion current manifold transmission, and the ion signal after screening is converted to optical signal transmission to optical lens device 5; Optical lens device accepts the light signal of mass particle filter transmission, accept simultaneously from injector introduce sample analysis test signal and particle beams controller to the control signal of particle beams direction and intensity, carry out light signal converting transmission, and then transfer signals to light signal transduction device; Then, by injector by sample: the test signal of cyanobenzene and test solvent: CDCl3 is transferred to optical lens device; Then, the control signal of particle beams direction and intensity is transferred to optical lens device by particle beams controller; Light signal transduction device accepts the signal that optical lens transmits, and by the Signal transmissions that receives in analysis of electric field device; Then, analysis of electric field device accepts the signal of light signal transduction device transmission, and is sent in particle energy analyzer by the signal after process, and particle energy analyzer accepts the signal transmission of analysis of electric field device, the particle of screening different-energy size, then by the Particle Delivery after analyzing to signal refractor; Signal refractor accepts the particle from particle energy analyzer, controls the change in light signal transduction direction, and is sent in moving magnetic field resolver by the particle signal after process and particle; Moving magnetic field resolver accepts from the particle signal of signal refractor and particle, by the movement locus of introduction by magnetic field particle, then by particle signal and Particle Delivery to particle conduction device; Particle conduction device accepts particle signal and the particle of moving magnetic field resolver, controls the conduction path length of particle conveying channels, then by particle conduction signal and Particle Delivery to signal manifold; Signal manifold accepts from the particle conduction signal of particle conduction device and particle, control signal and particle-stabilised, then by the particle signal after collecting and Particle Delivery to particle control device of electric field; Particle control device of electric field accepts, from the particle signal of signal manifold and particle, to control particle running status by electrostatic field, then by Particle Delivery to particle channel plate, particle and particle signal are transferred to particle multiplier; Particle channel plate accepts the particle from the transmission of particle control device of electric field, and the shape of the restriction particle beams, strengthens particle energy, and the particle of high velocity impact on inwall passage is increased, and it is incremental to carry out particle, then by Particle Delivery to fluorescent display screen; Fluorescent display screen accepts the transmission particle from particle channel plate, by the picture signal that detection of particles signal is changed, the form changed with brightness at receiving end is reappeared on video screen, and particle signal is transferred to signal observer, particle image pick-up device, vision signal transmitter; Signal observer accepts the particle signal from fluorescent display screen, observing samples particle analysis signal; Particle image pick-up device accepts the particle signal from fluorescent display screen, record particle analysis signal; Then, vision signal transmitter accepts the particle signal from fluorescent display screen, conducting particles analytic signal; Particle multiplier accepts particle from the transmission of particle control device of electric field and particle signal, adjustment and control the motion state of particle, then by particle analysis Signal transmissions to computing machine; Computing machine accepts the particle analysis signal from particle multiplier, analyzes sample particle and detects data, preserve testing result.Its analysis result is as shown in Fig. 5-7 and table 2.
Table 2: sample 2 is by a kind of analysis result of the sample detection analyser for nmr analysis
Above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted.Although with reference to embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, modify to technical scheme of the present invention or equivalent replacement, do not depart from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (9)
1., for a sample detection analyser for nmr analysis, it is characterized in that, comprising:
Gas Ionizer, the stage casing of its high frequency ionization tube is wound with pipe network coil, and its one end is provided with positive pole M type electrode, and the other end is provided with negative pole M type electrode;
Ion current manifold, it is connected with mass particle filtrator with described Gas Ionizer, ion airflow generator respectively by ion current conduit; Described ion airflow generator is positioned at the below of described Gas Ionizer, and it comprises positive stepup transformer and negative stepup transformer; Described mass particle filtrator is connected with optical lens device;
Described optical lens is connected with light signal transduction device with particle beams controller respectively, and be connected with injector by photoelectric sensor, described light signal transduction device is also connected with analysis of electric field device, described analysis of electric field device is also connected with particle energy analyzer, and is provided with particle sizing plate in it;
Described particle beams controller comprises the particle bombardment plate being located at its front end, and the anion electrode in portion located therein, control electrode and cation electrode successively from front to back;
Described particle energy analyzer is connected with signal refractor, and described signal refractor is also connected with moving magnetic field resolver, and described moving magnetic field resolver is connected with particle conduction device, and described particle conduction device is also connected with signal manifold;
Described signal manifold is connected with particle control device of electric field, and described particle control device of electric field is connected with particle multiplier with particle channel plate respectively; Described particle channel plate is connected with fluorescent display screen, and described fluorescent display screen is connected with vision signal transmitter with signal observer, particle image pick-up device respectively; Described particle multiplier is also connected with computing machine.
2. sample detection analyser according to claim 1, is characterized in that, described light signal transduction device comprises ground floor photoelectricity conversion thin film and second layer photoelectricity conversion thin film; The thickness of described ground floor photoelectricity conversion thin film is 3.66 microns-5.89 microns, and the thickness of described second layer photoelectricity conversion thin film is 8.67 microns-11.76 microns.
3. sample detection analyser according to claim 2, is characterized in that, described ion current conduit is arranged at the below of described negative pole M type electrode, and it is polyetherketone acetyl nitrile azoles ester composite material tube.
4. sample detection analyser according to claim 3, is characterized in that, the left side of the positive pole M type electrode of described Gas Ionizer has extraction electrode, and has sparking electrode on the right side of it.
5. sample detection analyser according to claim 4, is characterized in that, described particle sizing plate offers three circular holes, and three described circular holes are arranged in a linear, and from top to bottom, the diameter of three described circular holes is respectively: 5nm, 8nm, 12nm.
6., for a sample detection analytical approach for nmr analysis, it is characterized in that, comprise the following steps:
1), testing sample carries out high-frequency discharge after having been gasified by Gas Ionizer that sample gas is ionized, and produces low charge state positive ion; Then in the high-frequency electric field of Gas Ionizer, charged ion and sample atoms and molecular collision, make ionized sample molecule, and charged particle multiplication forms electrodless discharge, produces a large amount of sample belt electron ion;
2), in step 1) in, charged ion coordinates with negative stepup transformer the negative ions producing different charge ratio by the positive stepup transformer contained in ion airflow generator, and then the negative ions produced is passed through ion current conduit to ion current manifold by ion airflow generator;
3), ion current manifold accepts from the ion current of Gas Ionizer, ion airflow generator, then the ion current after collecting is transferred to mass particle filtrator;
4), mass particle filtrator accept ion current manifold transmission ion current after, carry out screening and filtering according to the difference of mass of ion and ionic charge, and by screening after ion signal be converted to optical signal transmission to optical lens device;
5), optical lens device accepts the light signal of mass particle filter transmission, accept simultaneously from injector introduce sample analysis test signal and particle beams controller to the control signal of particle beams direction and intensity, carry out light signal converting transmission, and then transfer signals to light signal transduction device;
6), light signal transduction device accepts the signal that optical lens transmits, and by the Signal transmissions that receives in analysis of electric field device;
7), analysis of electric field device accepts the signal that light signal transduction device transmits, and is sent in particle energy analyzer by the signal after process;
8), particle energy analyzer accepts the signal transmission of analysis of electric field device, the particle of screening different-energy size, then by the Particle Delivery after analyzing to signal refractor;
9), signal refractor accepts, from the particle of particle energy analyzer, to control the change in light signal transduction direction, and is sent in moving magnetic field resolver by the particle signal after process and particle;
10), moving magnetic field resolver accepts from the particle signal of signal refractor and particle, by the movement locus of introduction by magnetic field particle, then by particle signal and Particle Delivery to particle conduction device;
11), particle conduction device accepts particle signal and the particle of moving magnetic field resolver, controls the conduction path length of particle conveying channels, then by particle conduction signal and Particle Delivery to signal manifold;
12), signal manifold accepts from the particle conduction signal of particle conduction device and particle, control signal and particle-stabilised, then by the particle signal after collecting and Particle Delivery to particle control device of electric field;
13), particle control device of electric field accepts, from the particle signal of signal manifold and particle, to control particle running status by electrostatic field, then by Particle Delivery to particle channel plate, particle and particle signal are transferred to particle multiplier;
14), particle multiplier accepts particle from the transmission of particle control device of electric field and particle signal, adjustment and control the motion state of particle, then by particle analysis Signal transmissions to computing machine;
15), computing machine accepts from the particle analysis signal of particle multiplier, analyzes sample particle and detects data, preserve testing result.
7. sample detection analytical approach according to claim 6, is characterized in that, the control signal of particle beams direction and intensity is transferred to optical lens device by described particle beams controller.
8. sample detection analytical approach according to claim 7, is characterized in that, the test signal of sample is transferred to optical lens device by described injector.
9. sample detection analytical approach according to claim 7, it is characterized in that, described particle channel plate accepts the particle from the transmission of particle control device of electric field, the shape of the restriction particle beams, strengthen particle energy, the particle of high velocity impact on inwall passage is increased, and it is incremental to carry out particle, then by Particle Delivery to fluorescent display screen;
Fluorescent display screen accepts the transmission particle from particle channel plate, by the picture signal that detection of particles signal is changed, the form changed with brightness at receiving end is reappeared on video screen, and particle signal is transferred to signal observer, particle image pick-up device, vision signal transmitter;
Signal observer accepts the particle signal from fluorescent display screen, observing samples particle analysis signal; Particle image pick-up device accepts the particle signal from fluorescent display screen, record particle analysis signal; Vision signal transmitter accepts the particle signal from fluorescent display screen, conducting particles analytic signal.
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