CN114280005A - Device and method for rapidly analyzing and detecting hydrogen and hydrogen isotopes - Google Patents
Device and method for rapidly analyzing and detecting hydrogen and hydrogen isotopes Download PDFInfo
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- CN114280005A CN114280005A CN202111624119.2A CN202111624119A CN114280005A CN 114280005 A CN114280005 A CN 114280005A CN 202111624119 A CN202111624119 A CN 202111624119A CN 114280005 A CN114280005 A CN 114280005A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 198
- 239000001257 hydrogen Substances 0.000 title claims abstract description 198
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 198
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 152
- 150000002500 ions Chemical class 0.000 claims abstract description 51
- 238000007405 data analysis Methods 0.000 claims abstract description 25
- 238000004458 analytical method Methods 0.000 claims description 17
- 238000012545 processing Methods 0.000 claims description 10
- 230000001133 acceleration Effects 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 6
- 230000005684 electric field Effects 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 239000012159 carrier gas Substances 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 15
- 238000005259 measurement Methods 0.000 description 11
- 230000001360 synchronised effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- 238000001196 time-of-flight mass spectrum Methods 0.000 description 1
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Abstract
The invention relates to a device and a method for rapidly analyzing and detecting hydrogen and hydrogen isotopes, wherein the device and the method comprise the following steps: the system comprises a detection system, a sample introduction system, a beam source vacuum system, a laser system and a data analysis system; the detection system comprises a detection vacuum chamber, a detector and an accelerating electrode; the beam source vacuum system includes a beam source vacuum chamber. Forming a pulse molecular beam by the sample through a beam source vacuum chamber and entering a detection vacuum chamber; the laser system sequentially provides laser light sources with corresponding wavelengths, enters the detection vacuum chamber through the first window, selectively ionizes the pulse molecular beams to obtain hydrogen and hydrogen isotope ions, and leaves the hydrogen and hydrogen isotope ions from the second window; the ionized hydrogen and hydrogen isotopes reach the detector in sequence under the pushing action of the accelerating electrode; the detector receives the ionized hydrogen and hydrogen isotope ion signals and then sends the ionized hydrogen and hydrogen isotope ion signals to a data analysis system so as to determine the mass number and the quantity of the hydrogen and hydrogen isotopes. The invention is not interfered by other carrier gases during detection, and realizes the rapid and high-sensitivity detection of hydrogen and hydrogen isotopes.
Description
Technical Field
The invention relates to the technical field of hydrogen and hydrogen isotope detection, in particular to a device and a method for rapidly analyzing and detecting hydrogen and hydrogen isotopes.
Background
At present, hydrogen and hydrogen isotopes are widely applied to hydrogen energy and nuclear energy, wherein an accurate and rapid quantitative analysis technology of the hydrogen isotopes has very important significance for the application of the hydrogen isotopes. In the prior art, a high-resolution isotope mass spectrometer imported from abroad is mainly used for analyzing hydrogen isotopes with the concentration of more than ppm, and the isotope mass spectrometer is high in accuracy and precision of analyzing hydrogen isotopes, good in stability, expensive in price, difficult to introduce, limited in maintenance and high in requirement on operators. In addition, the low temperature gas chromatography has the advantages of simple technical equipment, low system construction cost and capability of realizing on-line analysis in the aspect of analyzing hydrogen isotopes, but is often influenced by impurities and carrier gas, has relatively low detection sensitivity, is 500ppm in maturity, has great difficulty below 100ppm and is easily influenced by other impurities.
In view of the foregoing, there is a need for an apparatus and method that can rapidly and highly sensitively detect hydrogen and hydrogen isotopes.
Disclosure of Invention
The invention aims to provide a device and a method for rapidly analyzing and detecting hydrogen and hydrogen isotopes, which can rapidly and highly sensitively detect the hydrogen and the hydrogen isotopes.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a rapid analysis and detection device for hydrogen and hydrogen isotopes, which comprises: the system comprises a detection system, a sample introduction system, a beam source vacuum system, a laser system and a data analysis system;
the detection system comprises: a detection vacuum chamber, a detector and an accelerating electrode; the detector and the accelerating electrode are both positioned in the detection vacuum chamber; a first window is arranged on the first side wall of the detection vacuum chamber, and a second window is arranged on the second side wall of the detection vacuum chamber; the first window and the second window are arranged oppositely, and are positioned on the same horizontal line with the accelerating electrode; the detector is positioned on the top wall of the detection vacuum chamber and is positioned vertically above the accelerating electrode;
the beam source vacuum system comprises a beam source vacuum chamber; the beam source vacuum chamber is in communication with the detection vacuum chamber;
the sample to be detected enters the detection vacuum chamber after the pulse molecular beam is formed in the beam source vacuum chamber through the sample introduction system; the laser system sequentially provides laser light sources with wavelengths corresponding to hydrogen and hydrogen isotopes, the laser light sources enter the detection vacuum chamber through the first window, the pulse molecular beams are selectively ionized to obtain ionized hydrogen and hydrogen isotope ions, and the ionized hydrogen and hydrogen isotope ions leave the detection vacuum chamber from the second window; the ionized hydrogen and hydrogen isotope ions sequentially reach the detector under the pushing action of the electric field applied by the accelerating electrode; the detector is used for receiving the ionized hydrogen and hydrogen isotope ions to obtain a detection signal; and processing and analyzing the detection signals through the data analysis system to determine the mass number and the content of the hydrogen and the hydrogen isotopes.
Optionally, the sample introduction system comprises:
the pulse valve is positioned in the beam source vacuum chamber and used for spraying pulse molecular beams to the detection vacuum chamber when a valve port of the pulse valve is opened;
the pulse valve controller is connected with the pulse valve and is used for controlling the opening and closing of the pulse valve;
the first air inlet pipeline is connected with the pulse valve and is used for sample introduction of a sample to be detected;
and the first air inlet container is connected with the first air inlet pipeline and is used for containing the sample to be detected.
Optionally, the apparatus further comprises:
a first opening on a third sidewall of the detection vacuum chamber and in the same horizontal line as the pulse valve; the third sidewall is a sidewall connecting the beam source vacuum chamber and the detection vacuum chamber;
the pulse valve injects a pulsed molecular beam through the first opening into the detection vacuum chamber.
Optionally, the apparatus further comprises:
and the collimator is positioned on the third side wall of the detection vacuum chamber, is fixed at the first opening, is arranged corresponding to the acceleration electrode, and is used for collimating the pulse molecular beam emitted from the pulse valve and ensuring that the pulse molecular beam is incident to a laser ionization area of the acceleration electrode.
Optionally, the center of the pulse valve is located on the same horizontal line as the center of the collimator.
Optionally, the apparatus further comprises:
a first vacuum pump set communicated with the detection vacuum chamber for providing a vacuum environment for the detection vacuum chamber;
a second vacuum pump set in communication with the beam source vacuum chamber for providing a vacuum environment for the beam source vacuum chamber.
Optionally, the first window and the second window are both made of transparent glass.
Optionally, the laser system comprises: YAG laser, dye laser, and nonlinear crystal;
the YAG laser is a pumping source of the dye laser, laser light sources with different wavelengths are obtained by replacing dye of the dye laser, and ionized laser light sources are obtained through nonlinear crystals.
In order to achieve the above object, the present invention further provides a method for rapid analysis and detection of hydrogen and hydrogen isotopes, the method being applied to the apparatus, the method comprising:
forming a pulse molecular beam in a beam source vacuum chamber of a sample to be detected through a sample introduction system, and injecting the pulse molecular beam into the detection vacuum chamber;
the laser light source with the wavelength corresponding to the hydrogen and hydrogen isotopes enters the detection vacuum chamber from the first window of the detection vacuum chamber in sequence, selectively ionizes the pulse molecular beam to obtain ionized hydrogen and hydrogen isotope ions, and leaves the detection vacuum chamber from the second window;
the ionized hydrogen and hydrogen isotope ions sequentially reach the detector under the pushing action of the accelerating electrode;
receiving the ionized hydrogen and hydrogen isotope ions through the detector and obtaining a detection signal;
and processing and analyzing the detection signals through the data analysis system to determine the mass number and the content of the hydrogen and the hydrogen isotopes.
Optionally, the processing and analyzing the detection signal by the data analysis system to determine the mass number and the content of hydrogen and the hydrogen isotope specifically includes:
the detection signal includes: the intensity of different ions in the hydrogen and hydrogen isotopes reaching the detector and the time of different ions in the hydrogen and hydrogen isotopes reaching the detector;
determining the content of hydrogen and the isotope thereof in the sample to be detected through the data analysis system according to the strength of different ions reaching the detector;
and determining the mass numbers of the hydrogen and the isotopes thereof in the sample to be detected through the data analysis system according to the time of the different ions reaching the detector.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention provides a device and a method for rapidly analyzing and detecting hydrogen and hydrogen isotopes, wherein the device comprises: a detection system, comprising: a detection vacuum chamber, a detector and an accelerating electrode; the detector and the accelerating electrode are both positioned in the detection vacuum chamber; a first window is arranged on the first side wall of the detection vacuum chamber, and a second window is arranged on the second side wall of the detection vacuum chamber; the first window and the second window are arranged oppositely, and are positioned on the same horizontal line with the accelerating electrode; the detector is positioned on the top wall of the detection vacuum chamber and is positioned right above the accelerating electrode; the beam source vacuum chamber is communicated with the detection vacuum chamber; a sample to be detected enters a detection vacuum chamber after pulse molecular beams are formed in a beam source vacuum chamber through a sample introduction system; the laser system sequentially provides laser light sources with wavelengths corresponding to hydrogen and hydrogen isotopes, the laser light sources enter the detection vacuum chamber through the first window, the pulsed molecular beams are selectively ionized to obtain hydrogen and hydrogen isotope ions, and the hydrogen and hydrogen isotope ions leave the detection vacuum chamber from the second window; the ionized hydrogen and hydrogen isotopes reach the detector in sequence under the pushing action of an electric field applied by the accelerating electrode; the detector is used for receiving the ionized hydrogen and hydrogen isotope ions to obtain detection signals; and the data analysis system processes and analyzes the detection signals to determine the mass number and the quantity of the hydrogen and the hydrogen isotopes. The invention is not interfered by other carrier gases during detection, can realize the measurement of the hydrogen isotope with the concentration of 50ppm within 30 seconds, has excellent resolution on the signals of the hydrogen and the hydrogen isotope, and realizes the rapid and high-sensitivity detection of the hydrogen and the hydrogen isotope.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a cross-sectional view of a rapid analysis and detection apparatus for hydrogen and hydrogen isotopes according to the present invention;
FIG. 2 is a cross-sectional view of a collimator according to the present invention;
FIG. 3 is a graph of the analysis results of the embodiment of the present invention.
Description of the symbols:
a detection vacuum chamber-1, a detector-2, an accelerating electrode-3, a beam source vacuum chamber-4, an adjustable support component 5, a pulse valve-6, a first opening-7, a collimator-8, a first vacuum pump group-9 and a second vacuum pump group-10.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a device and a method for rapidly analyzing and detecting hydrogen and hydrogen isotopes, which can rapidly and highly sensitively detect the hydrogen and the hydrogen isotopes.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The invention relates to a rapid analysis and detection device for hydrogen and hydrogen isotopes, which comprises: the system comprises a detection system, a sample introduction system, a beam source vacuum system, a laser system and a data analysis system.
As shown in fig. 1, the detection system includes: a detection vacuum chamber 1, a detector 2 and an accelerating electrode 3; the detector 2 and the accelerating electrode 3 are both positioned in the detection vacuum chamber 1; a first window is arranged on the first side wall of the detection vacuum chamber 1, and a second window is arranged on the second side wall of the detection vacuum chamber 1; the first window and the second window are arranged oppositely, and both the first window and the second window and the accelerating electrode 3 are positioned on the same horizontal line; the detector 2 is located on the top wall of the detection vacuum chamber 1 and vertically above the accelerating electrode 3, and can also be adjusted as required.
The beam source vacuum system comprises a beam source vacuum chamber 4; the beam source vacuum chamber 4 communicates with the detection vacuum chamber 1.
The sample to be detected passes through the sample introduction system and enters the detection vacuum chamber 1 after the beam source vacuum chamber 4 forms a pulse molecular beam; the laser system sequentially provides laser light sources with wavelengths corresponding to hydrogen and hydrogen isotopes, the laser light sources enter the detection vacuum chamber 1 through the first window, the pulsed molecular beams are selectively ionized to obtain ionized hydrogen and hydrogen isotope ions, and the ionized hydrogen and hydrogen isotope ions leave the detection vacuum chamber 1 from the second window; the ionized hydrogen and hydrogen isotope ions sequentially reach the detector 2 under the pushing action of the electric field applied by the accelerating electrode 3; the detector 2 is used for receiving the ionized hydrogen and hydrogen isotope ions to obtain a detection signal; and processing and analyzing the detection signals through the data analysis system to determine the mass number and the content of the hydrogen and the hydrogen isotopes.
Further, the beam source vacuum system further comprises: a first vacuum observation window and a first vacuum measurement system. The first vacuum viewing window is provided on a side wall of the beam source vacuum chamber 4 for viewing a vacuum condition within the beam source vacuum chamber 4. The first vacuum measurement system is used to measure the vacuum level condition within the beam source vacuum chamber 4.
Specifically, the sampling system includes: pulse valve 6, pulse valve controller, first inlet line and first inlet vessel.
The pulse valve 6 is positioned in the beam source vacuum chamber 4 and used for jetting the pulse molecular beam to the detection vacuum chamber 1 when a valve port of the pulse valve 6 is opened.
And the pulse valve controller is connected with the pulse valve 6 and is used for controlling the opening and closing of the pulse valve 6. The pulse valve controller can be externally triggered and controlled by a synchronous time delay device.
The first air inlet pipeline is connected with the pulse valve 6 and used for sample introduction of a sample to be detected. The pulse valve 6 is arranged in the beam source vacuum chamber 4 and is connected with the external sample gas to be measured through the first gas inlet pipeline.
The first air inlet container is connected with the first air inlet pipeline and used for containing the sample to be detected.
Further, the apparatus further comprises:
a first opening 7 located on a third side wall of the detection vacuum chamber 1 and level with the pulse valve 6; the third sidewall is a sidewall connecting the beam source vacuum chamber 4 and the detection vacuum chamber 1. In a particular embodiment of the present invention, the beam source vacuum chamber 4 is in communication with the detection vacuum chamber 1 through a first opening 7.
The pulse valve 6 injects a pulsed molecular beam into the detection vacuum chamber 1 through the first opening 7.
Further, the apparatus further comprises: the support member 5 is adjustable.
The adjustable supporting component 5 is positioned in the beam source vacuum chamber 4 and is connected with the pulse valve 6 and used for supporting the pulse valve 6, adjusting the position of the pulse valve 6 and positioning the pulse valve 6.
Further, the beam source vacuum system apparatus further comprises: first vacuum lead (feedthru). Wherein, the first vacuum lead and the first vacuum measurement system are connected by a CF35 flange reserved on the side wall of the beam source vacuum chamber 4; the pulse valve 6 is connected with an external pulse valve controller through a first vacuum lead.
Further, the detection system further comprises: a second vacuum observation window, a second vacuum lead and a second vacuum measurement system. The second vacuum lead, the second vacuum measurement system and the second gas inlet pipeline are installed and connected through a CF35 flange reserved on the side wall of the detection vacuum chamber 1; the second vacuum observation window is used for checking the vacuum condition in the detection vacuum chamber 1. The second vacuum measurement system is used for measuring the vacuum degree state in the detection vacuum chamber 1. The accelerating electrode 3 and the detector 2 are both connected with an external power supply through a second vacuum lead. The first window is the entrance of the laser light source into the detection vacuum chamber 1 and the second window is the exit of the laser light source from the detection vacuum chamber 1.
Further, the apparatus further comprises: a collimator 8.
The collimator 8 is located on the third sidewall of the detection vacuum chamber 1, fixed at the first opening 7, and disposed corresponding to the acceleration electrode 3, and is configured to collimate the pulsed molecular beam emitted from the pulse valve 6 and ensure that the pulsed molecular beam is incident on the laser ionization region of the acceleration electrode 3, and a cross-sectional view thereof is shown in fig. 2. The third side wall is a side wall connecting the beam source vacuum chamber 4 and the detection vacuum chamber 1, i.e. the beam source vacuum chamber 4 and the detection vacuum chamber 1 are connected by the third side wall, the third side wall is provided with a first opening 7, a collimator 8 is fixed on the first opening 7, and the beam source vacuum chamber 4 and the detection vacuum chamber 1 are communicated by the collimator 8. In addition, the collimator is also used for realizing the differential pumping function and ensuring the high vacuum environment in the acquisition process of the detection vacuum chamber 1.
Further, the laser system includes: YAG laser and dye laser. YAG laser is used as the pumping source of dye laser, and laser light sources with different wavelengths can be obtained by replacing dye; the laser with any wavelength in the range of 190nm-700nm can be obtained by combining methods such as nonlinear crystals and the like, so that the state-selective ionization of different ions is realized. The laser system may be externally triggered and controlled by a synchronous delay.
Further, the data analysis system comprises a collection card and a data analysis device; the data analysis equipment comprises corresponding acquisition program software.
Specifically, in an embodiment of the present invention, the sample to be tested is connected to the pulse valve 6 in the beam source vacuum chamber 4 through a first gas inlet pipe, and after the beam source vacuum chamber 4 forms a pulse molecular beam, the pulse molecular beam enters the detection vacuum chamber 1 through the collimator 8 in a collimating manner, and is on the same horizontal plane with a connecting line of the first window center and the second window center in the detection vacuum chamber 1; a laser light source enters the detection vacuum chamber 1 through the center of the first window, the opening time of the pulse valve 6 and the opening time of the laser light source are adjusted through external synchronous delay equipment, so that laser and pulse molecular beams are overlapped in time and space, and the hydrogen and hydrogen isotopes in the pulse molecular beams are selectively ionized by adjusting the wavelength of the laser light source; the ionized hydrogen and hydrogen isotope ions reach the detector 2 under the pushing action of the electric field applied by the accelerating electrode 3; the detector 2 receives the ionized hydrogen and hydrogen isotope ions to obtain detection signals; and processing and analyzing the detection signals through the data analysis system to determine the mass number and the content of the hydrogen and the hydrogen isotopes. The detection signal obtained by the detector 2 is amplified and then sent to the acquisition card, and the data is analyzed and processed by computer software. Wherein each ion needs to be ionized for a specific wavelength. In addition, the direction of the pulse molecular beam entering the detection vacuum chamber 1, the direction of the laser entering and leaving the detection vacuum chamber 1 and the flight direction of the ionized ions are mutually perpendicular in pairs.
The pulsed molecular beam enters the detection vacuum chamber 1 through the first opening 7 when the pulse valve 6 is in an open state. Specifically, when the pulse valve 6 is closed, a pulsed molecular beam cannot be generated; when the pulse valve 6 is opened, the sample gas to be measured enters the beam source vacuum chamber 4, forms a pulsed molecular beam, and enters the detection vacuum chamber 1 through the first opening 7. The pulse valve 6 is communicated with the sample gas to be detected outside the beam source vacuum chamber 4, the sample gas to be detected obtains the pulse molecular beam with high strength and high speed quality through the pulse valve 6, and the usage amount of the detection gas is greatly reduced. In practice, a continuous feed gas can also be used, but the sample gas is relatively wasted in this system. In a particular embodiment of the invention, using the pulse valve 6, a pulsed molecular beam of minimum width of 100us can be obtained; the frequency of the laser and the pulse valve 6 are both 30Hz, so that the gas consumption can be reduced by 300 times compared with the continuous beam current.
Preferably, the center of the pulse valve 6 is located on the same horizontal line as the center of the collimator 8 to ensure that the pulsed molecular beam enters the detection vacuum chamber 1 more.
Further, the apparatus further comprises: a first vacuum pump group 9 and a second vacuum pump group 10.
And the first vacuum pump group is communicated with the detection vacuum chamber and is used for providing a vacuum environment for the detection vacuum chamber.
A second vacuum pump set in communication with the beam source vacuum chamber for providing a vacuum environment for the beam source vacuum chamber.
Preferably, the first window and the second window are both made of transparent glass. In a specific embodiment of the present invention, the first window and the second window are made of colorless transparent glass.
In addition, the first window is also used for introducing tunable laser outside into the detection vacuum chamber 1, and by adjusting the time delay between the laser and the sample to be detected, the laser can just selectively ionize the pulse molecular beam at the arrival time of the pulse molecular beam, that is, the pulse molecular beam entering the detection vacuum chamber 1 and the pulse laser entering the detection vacuum chamber 1 are synchronized in time and overlapped in space, and the laser wavelength and the hydrogen and hydrogen isotopes in the pulse molecular beam are adjusted by the laser system to realize wavelength resonance, so that the selective ionization of the hydrogen and the isotopes in the pulse molecular beam is realized.
In order to achieve the above purpose, the invention also provides the following scheme:
the invention relates to a method for rapidly analyzing and detecting hydrogen and hydrogen isotopes, which is applied to the device and comprises the following steps:
s1: the sample to be detected enters the beam source vacuum chamber 4 through a first air inlet pipeline, and the pulse valve enables the sample to be detected to form pulse molecular beams under the control of the pulse valve controller and to be shot into the detection vacuum chamber 1 through the collimator.
S2: the laser light source enters the detection vacuum chamber 1 from a first window of the detection vacuum chamber 1, the opening time of the pulse valve and the opening time of the laser light source are adjusted by controlling the synchronous delay equipment, so that the laser and the pulse molecular beam are synchronous in time, the spatial overlapping is realized at the proper position of the accelerating electrode 3, and the hydrogen and the isotope thereof in the pulse molecular beam are selectively ionized by adjusting the wavelength of the laser pulse to obtain the ionized hydrogen and hydrogen isotope ions.
S3: the hydrogen and the hydrogen isotopes sequentially reach the detector 2 under the pushing action of the accelerating electrode 3.
S4: and the detector 2 is used for receiving the ionized hydrogen and hydrogen isotope ions to obtain detection signals.
S5: and processing and analyzing the detection signals through the data analysis system to determine the mass number and the content of the hydrogen and the hydrogen isotopes.
Further, S5: the processing and analyzing of the detection signals by the data analysis system to determine the mass number and content of hydrogen and hydrogen isotopes specifically comprises:
the detection signal includes: the intensity of the different ions in the hydrogen and hydrogen isotopes arriving at the detector and the time of arrival of the different ions in the hydrogen and hydrogen isotopes at the detector.
And determining the content of hydrogen and the isotope thereof in the sample to be detected through the data analysis system according to the strength of different ions reaching the detector. Specifically, a relative quantity measurement is obtained first, and after calibration by a standard gas, the relative quantity measurement can be converted into an absolute quantity measurement.
And determining the mass numbers of the hydrogen and the isotopes thereof in the sample to be detected through the data analysis system according to the time of the different ions reaching the detector. Other mass number sample detection may also be achieved by other ionization methods, and is not limited herein.
Specifically, the process of different ions arriving at the detector from the accelerating electrode follows the following law:
then, the arrival times of different ions at the detector can be expressed as:
wherein, L represents the distance between the accelerating electrode and the detector, m is the ion mass number, V is the ion speed, V is the voltage of the electric field applied by the accelerating electrode, e is the electric quantity of the ion, and t is the time of the ion from the accelerating electrode to the detector. Therefore, the mass number m of hydrogen and hydrogen isotopes can be calculated from the time when they reach the detector from the accelerating electrode. Furthermore, since the mass numbers of hydrogen and hydrogen isotopes are different, t is theoretically different, andaccording to the strength (quantity) of the ions corresponding to different arrival times, the content of hydrogen and hydrogen isotopes in the sample to be detected can be detected.
In one embodiment of the invention, the helium carrier H2HD and D2The analysis result of the gas mixture is shown in FIG. 3, in which the first small peaks are the residues after background reduction of the laser signal, and the next several peaks correspond to H2And D2From FIG. 3, the laser is made to be different from H by changing the wavelength of the laser light2And D2Resonance, detected H2、D2The signals of (2) are arranged from left to right, the resolution is extremely high, the signals have no interference with each other at all, and are not affected by the carrier gas He gas.
The device combines the laser spectrum technology with the time-of-flight mass spectrum technology, and realizes the hydrogen and the isotope (H) thereof from two dimensions of the spectrum and the mass spectrum2，D2) The method can be used for qualitative and quantitative rapid detection with high sensitivity (the measurement of 50ppm concentration is realized within 30 seconds), and is not interfered by other carrier gases. The invention has the advantages of high detection sensitivity, convenient and rapid detection and the like. The invention can be extended to the detection of other gases by changing the laser wavelength.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A rapid analysis and detection device for hydrogen and hydrogen isotopes, comprising: the system comprises a detection system, a sample introduction system, a beam source vacuum system, a laser system and a data analysis system;
the detection system comprises: a detection vacuum chamber, a detector and an accelerating electrode; the detector and the accelerating electrode are both positioned in the detection vacuum chamber; a first window is arranged on the first side wall of the detection vacuum chamber, and a second window is arranged on the second side wall of the detection vacuum chamber; the first window and the second window are arranged oppositely, and are positioned on the same horizontal line with the accelerating electrode; the detector is positioned on the top wall of the detection vacuum chamber and is positioned vertically above the accelerating electrode;
the beam source vacuum system comprises a beam source vacuum chamber; the beam source vacuum chamber is in communication with the detection vacuum chamber;
the sample to be detected passes through the sample introduction system and enters the detection vacuum chamber after the beam source vacuum chamber forms the pulse molecular beam; the laser system sequentially provides laser light sources with wavelengths corresponding to hydrogen and hydrogen isotopes, the laser light sources enter the detection vacuum chamber through the first window, the pulse molecular beams are selectively ionized to obtain ionized hydrogen and hydrogen isotope ions, and the ionized hydrogen and hydrogen isotope ions leave the detection vacuum chamber from the second window; the ionized hydrogen and hydrogen isotope ions sequentially reach the detector under the pushing action of the electric field applied by the accelerating electrode; the detector is used for receiving the ionized hydrogen and hydrogen isotope ions to obtain a detection signal; and processing and analyzing the detection signals through the data analysis system to determine the mass number and the content of the hydrogen and the hydrogen isotopes.
2. The apparatus for rapid analysis and detection of hydrogen and hydrogen isotopes according to claim 1, wherein the sample injection system comprises:
the pulse valve is positioned in the beam source vacuum chamber and used for spraying pulse molecular beams to the detection vacuum chamber when a valve port of the pulse valve is opened;
the pulse valve controller is connected with the pulse valve and is used for controlling the opening and closing of the pulse valve;
the first air inlet pipeline is connected with the pulse valve and is used for sample introduction of a sample to be detected;
and the first air inlet container is connected with the first air inlet pipeline and is used for containing the sample to be detected.
3. The apparatus for rapid analysis and detection of hydrogen and hydrogen isotopes according to claim 2, further comprising:
a first opening on a third sidewall of the detection vacuum chamber and in the same horizontal line as the pulse valve; the third sidewall is a sidewall connecting the beam source vacuum chamber and the detection vacuum chamber;
the pulse valve injects a pulsed molecular beam through the first opening into the detection vacuum chamber.
4. The apparatus for rapid analysis and detection of hydrogen and hydrogen isotopes according to claim 3, further comprising:
and the collimator is positioned on the third side wall of the detection vacuum chamber, is fixed at the first opening, is arranged corresponding to the acceleration electrode, and is used for collimating the pulse molecular beam emitted from the pulse valve and ensuring that the pulse molecular beam is incident to a laser ionization area of the acceleration electrode.
5. The apparatus for rapid analysis and detection of hydrogen and hydrogen isotopes according to claim 3, wherein the center of said pulse valve is located on the same horizontal line as the center of said collimator.
6. The apparatus for rapid analysis and detection of hydrogen and hydrogen isotopes according to claim 1, further comprising:
a first vacuum pump set communicated with the detection vacuum chamber for providing a vacuum environment for the detection vacuum chamber;
a second vacuum pump set in communication with the beam source vacuum chamber for providing a vacuum environment for the beam source vacuum chamber.
7. The apparatus for rapid analysis and detection of hydrogen and hydrogen isotopes according to claim 1, wherein the first window and the second window are made of transparent glass.
8. The apparatus for rapid analysis and detection of hydrogen and hydrogen isotopes according to claim 1, wherein said laser system comprises: YAG laser, dye laser, and nonlinear crystal;
the YAG laser is a pumping source of the dye laser, laser light sources with different wavelengths are obtained by replacing dye of the dye laser, and ionized laser light sources are obtained through nonlinear crystals.
9. A method for rapid analytical detection of hydrogen and hydrogen isotopes, said method being applied to the device according to any one of claims 1 to 8, said method comprising:
forming a pulse molecular beam in a beam source vacuum chamber of a sample to be detected through a sample introduction system, and injecting the pulse molecular beam into the detection vacuum chamber;
the laser light source with the wavelength corresponding to the hydrogen and hydrogen isotopes enters the detection vacuum chamber from the first window of the detection vacuum chamber in sequence, selectively ionizes the pulse molecular beam to obtain ionized hydrogen and hydrogen isotope ions, and leaves the detection vacuum chamber from the second window;
the ionized hydrogen and hydrogen isotope ions sequentially reach the detector under the pushing action of the accelerating electrode;
receiving the ionized hydrogen and hydrogen isotope ions through the detector and obtaining a detection signal;
and processing and analyzing the detection signals through the data analysis system to determine the mass number and the content of the hydrogen and the hydrogen isotopes.
10. The method for rapid analysis and detection of hydrogen and hydrogen isotopes according to claim 9, wherein the processing and analysis of the detection signals by the data analysis system to determine the mass number and content of hydrogen and hydrogen isotopes specifically comprises:
the detection signal includes: the intensity of different ions in the hydrogen and hydrogen isotopes reaching the detector and the time of different ions in the hydrogen and hydrogen isotopes reaching the detector;
determining the content of hydrogen and the isotope thereof in the sample to be detected through the data analysis system according to the strength of different ions reaching the detector;
and determining the mass numbers of the hydrogen and the isotopes thereof in the sample to be detected through the data analysis system according to the time of the different ions reaching the detector.
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