CN208109749U - T and He-3 accelerator mass spectrometry high-sensitivity measurement device - Google Patents
T and He-3 accelerator mass spectrometry high-sensitivity measurement device Download PDFInfo
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- CN208109749U CN208109749U CN201820118954.6U CN201820118954U CN208109749U CN 208109749 U CN208109749 U CN 208109749U CN 201820118954 U CN201820118954 U CN 201820118954U CN 208109749 U CN208109749 U CN 208109749U
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Abstract
The utility model relates to a kind of T and He-3 accelerator mass spectrometry high-sensitivity measurement devices, including the ion source for generating cation, the ion that mass number is 3 is sent into accelerating tube by injection magnet by the cation that ion source generates, the accelerating tube connects stripper, molecular ion is broken down into monatomic ion by stripper, the stripper is connect with analysis magnet, by analysis magnet by T and3He is separated, and the analysis magnet connects detection system, detection system to after separating T and3He is measured respectively.The utility model drawn using cation combine accelerator mass spectrometry and film stripping technology remove all kinds of obstacles background realize T and3Highly sensitive, the efficient measurement of He, greatly improve T and3He measurement sensitivity and measurement efficiency.
Description
Technical field
The utility model relates to the measuring techniques of nucleic, and in particular to a kind of T and He-3 accelerator mass spectrometry high-sensitivity measurement
Device.
Background technique
T and3He suffers from extensive use in fields such as nuclear science, geology, environmental science, hydrology, medicine, for tritium
Measurement both at home and abroad mainly use gas ionization method and liquid scintillating detection method.Gas ionization method can realize the fast of sample
Fast continuous measurement, but these monitors can only the tritium gas sample to high-content detect, the range being generally capable of measuring is 6~
106Bq/L (is equivalent to 3 × 109--5×1014Tritium atom).Sample lower for tritium level generallys use Low background liquid and dodges spectrum
Instrument is measured, and the detection limit that liquid dodges method is about 0.5Bq/L, and time of measuring needs several hours.But measurement side is dodged with liquid
Method needs to carry out sample preparation processing to exclude the interference of other radionuclides and improve tritium sample concentration, this is that liquid dodges method
Measure necessary to committed step, sample treatment improved frequently with method for concentration such as electrolysis method, chromatography and thermal diffusion methods to
The concentration of tritium in sample.In addition, either gas ionization chamber or liquid scintillation methods are all the β radiated when being decayed using tritium
Ray is detected, and both methods is only capable of being measured radioactive activity, cannot achieve the identification of radionuclide, therefore
Origin of radioactivity can not be just differentiated in the presence of there are other beta activity nucleic in which nucleic, it is difficult to realize the standard of measurement result
True property and reliability, it is therefore desirable to carry out complicated Radiochemical Separation process before measuring.Some laboratories are in order to further mentioning
High Tritium measurement accuracy and sensitivity uses3He mass spectrograph is measured indirectly.The method is the decay daughter by measurement of tritium3The amount of He determines that the content of tritium, measurement sensitivity reach 0.15Bq/kg.When the shortcomings that the method, is firstly the need of passing through longer
Between (about three months) wait the decay of tritium, secondly need complicated sample treatment original in sample to exclude3He.In short, right
It is limited in these measurement methods of tritium by sample treatment, measurement efficiency, sensitivity and accuracy.And with research work
Deeply and quicker, sensitive, the efficient analysis means of the expansion of application field needs, gradually developed utilization in recent years thus
Accelerator mass spectrometry carries out Tritium measure technique study.The method can remove all kinds of obstacles and realize the direct measurement of tritium atom,
Without the β ray of measurement of tritium transmitting, therefore time of measuring only needs a few minutes while having very high sensitivity.Buddhist nun admires in Germany
Black polytechnical university establishes the measurement that accelerator mass spectrometry (AMS) device carries out tritium, and cooperation development has studied fusion reactor material
Work is applied in distribution of tritium etc. in material.They are passed through tandem accelerator (end voltage 100kV) using the negative-ion mode for drawing tritium
It is measured after acceleration, effectively eliminates various background interference, realize the Sensitive Determination of tritium.The characteristics of this measuring system is
It is excluded by drawing anion3The interference (He is that inert gas cannot form anion) of He excludes to divide using carbon film removing
The interference of sub- background, but the shortcomings that extraction anion is that ejection efficiency is low (1 to 2 orders of magnitude lower than extraction cation), together
When also cannot achieve3The measurement of He.And3He also has important researching value as the decay daughter of tritium, needs in some research fields
Will to tritium and3He is carried out while being measured；Livemore National Laboratory of the U.S. (LLNL) has developed positive ion source extraction, using penetrating
The dedicated accelerator mass spectrometry measuring system that the method that frequency quadrupole field (RFQ) accelerates establishes compact type carries out Tritium measurement.RFQ knot
Structure is complicated, and system requirements is high, they only carry out Tritium measurement with this system at present.
3He is stable nuclide, but content is extremely low, is existed everywhere in nature gas, liquid and solid,3He/4The ratio of He
Value is 10-6—10-10Between, their ratio has highly important meaning in carrying out geochemistry and geophysical research
Justice represents different geological environments.3The measurement of He utilizes substantially3He mass spectrograph, its basic principle is exactly will3He ionization
It afterwards, after accelerating compared with low energy (~kV), will using magnetic analyzer3He carries out selection and recycles Faraday cup pair3He is surveyed
Amount.But it is measured using the method3The molecular ion interference (such as HD, 3H) of hydrogen can be encountered when He and also will receive in special circumstances
The interference of tritium, the HD ratio in natural sample3He is at least higher by 103-104Times, and3He and T, HD molecule, 3H molecule it is of poor quality
It is not respectively only 1.2 × 10-3、1.9×10-3With 2.5 × 10-3.Therefore mass-spectrometer measurement is being utilized3HD, 3H, T etc. can be encountered when He
Interference and limit its measurement sensitivity.In order to improve measurement sensitivity,3He mass spectrograph is needed before sample measurement using multiple
Thus miscellaneous dehydrogenation process reduces the molecular ion interference of hydrogen to exclude the content of hydrogen in sample, while narrow by reducing mass spectrograph
Seam etc. improves mass resolution to further decrease the interference of molecular ion, these all significantly limit measurement efficiency.Even if
In this way, this spectrometer measurement sensitivity it is best be also only 10-8(3He/4He), so that some sample sizes it is small or3He content is low
Sample be unable to measure.Also trial carries out using AMS technology3The method of measuring of He, the method use end voltage for
The accelerator of 0.8MV carries out3The measurement of He effectively eliminates the interference of molecule background, but the method has only done a method
It explores, without further system research.
Utility model content
The purpose of this utility model is that in view of the deficiencies in the prior art, provide it is a kind of and meanwhile measure T with3He's
Highly sensitive, quick, efficient measuring device.
The technical solution of the utility model is as follows：A kind of T and3He accelerator mass spectrometry high-sensitivity measurement device, including be used for
The ion source of cation is generated, the ion that mass number is 3 is sent into accelerating tube by injection magnet by the cation that ion source generates,
The accelerating tube connects stripper, and molecular ion is broken down into monatomic ion, the stripper and analysis of magnetic by stripper
Iron connection, by analysis magnet by T and3He is separated, and the analysis magnet connects detection system, and detection system is to the T after separating
With3He is measured respectively.
Further, T as described above and3He accelerator mass spectrometry high-sensitivity measurement device, wherein in ion source and injection magnetic
Preaceleration pipe is equipped between iron.
Further, T as described above and3He accelerator mass spectrometry high-sensitivity measurement device, wherein the ion source is base
In the double-plasma ion source of gas sampling.
Further, T as described above and3He accelerator mass spectrometry high-sensitivity measurement device, wherein in the side of injection magnet
Equipped with for separating to injection magnet4The Faraday cup that He and D are measured.
Further, T as described above and3He accelerator mass spectrometry high-sensitivity measurement device, wherein the injection magnet with
Quadrupole lenses are equipped between accelerating tube；The quadrupole lenses use electrostatic quadrupole lenses.
Further, T as described above and3He accelerator mass spectrometry high-sensitivity measurement device, wherein the accelerating tube is using single
Electrostatic accelerated mode is held to realize that particle accelerates.
Further, T as described above and3He accelerator mass spectrometry high-sensitivity measurement device, wherein the stripper uses
Si3N4As stripping film.
Further, T as described above and3He accelerator mass spectrometry high-sensitivity measurement device, wherein analysis magnet is using deflection
Radius is 350mm, the double focusing magnetic analyzer that deflection angle is 90 degree.
Further, T as described above and3He accelerator mass spectrometry high-sensitivity measurement device, wherein the detection system packet
Include Au-Si surface barrier detector, Computation of Single Channel Multiplying device and the Faraday cup suitable for different counting rates.
The beneficial effects of the utility model are as follows：
(1) high sensitivity improves two magnitudes than other method sensitivity, and measurement sensitivity reaches 105Atom；
(2) be able to achieve T and3It is measured while He, obtains more fully information；
(3) sample preparation is simple, improves measurement efficiency, and measurement sample only needs a few minutes.
Detailed description of the invention
Fig. 1 be the utility model T and3He measuring system schematic illustration；
Fig. 2 be the utility model T and3The structural schematic diagram of He accelerator mass spectrometry high-sensitivity measurement device.
Specific embodiment
The utility model is described in detail with reference to the accompanying drawings and examples.
In existing Tritium measurement apparatus and method for, draw anion the shortcomings that be ejection efficiency it is low (than draw cation
Low 1 to 2 orders of magnitude), while also cannot achieve3The measurement of He.And3He also has important research valence as the decay daughter of tritium
Value, need to tritium in some research fields and3He is carried out while being measured；And3Can be encountered in the measuring device of He the molecule of hydrogen from
Son interferes and limits its measurement sensitivity and measurement efficiency.
Therefore, either tritium is still3He, current measuring technique is all by considerable restraining factors, it is difficult to meet more
Add the demand extensively and profoundly studied.The utility model have developed can measure simultaneously T and3Highly sensitive, quick, the efficient measurement of He fills
It sets, this is also current international development trend, and the foundation of this device will provide high quality for its application in every subjects
Research platform.
The utility model be based on Accelerator mass spectrometry establish T and3The Sensitive Determination device of He, design philosophy and totality
Structure is as shown in Figure 1.For realize T and3He it is quick, efficiently with measure simultaneously, meet more extensive Research Requirements, the utility model
Use positive ion source 1 with realize T and3The ionization of He；Using injection magnet 2 by mass number be 3 ion (including T, 3He, HD,
3H) it is sent into accelerating tube 3；For exclude T and3He measure when molecule background and T with3Interfering with each other between He, using by ion
Energy accelerates to~100keV；The film of stripper 4 is recycled to remove ion, so that passing through the molecular ion after film
It is broken down into monatomic ion, thus excludes the interference of molecular ion；Simultaneously according to T with3Dump energy is different after He passes through film, benefit
With analysis magnet 5 by T and3He is separated；Finally using detection system 6 to T after separately and3He is measured respectively, realize T and3He
Highly sensitive measure simultaneously.
Based on the above design philosophy and overall structure, the embodiments of the present invention devise measurement dress as shown in Figure 2
Set system.Using single-stage accelerated mode (being different from the common tandem accelerated mode of accelerator mass spectrometry), accelerating tube one end is system
About 100kV high potential, the other end are ground potential.The structure of device includes：
Ion source 1：The utility model be in order to realize T and3The efficient quick measurement of He, gas sampling are to realize quickly to survey
Fixed key, it is therefore desirable to use the ion source based on gas sampling；Since He cannot form anion, if drawing anion
It will be unable to realize3The detection of He, therefore ion source needs to use and meets gas sampling and can efficiently generate the ion source of cation
System.The utility model uses the double-plasma ion source based on gas sampling, and double-plasma ion source (double to wait sources) is adopted
With gas sampling and to have the characteristics that positive ion electrospray can be dissipated from high-efficient, ion small, is able to satisfy this requirements of one's work.This is practical
Novel proposed adoption is double to wait sources as ion source system.Draw cation carry out tritium and3Measurement is the utility model head while He
The technology of secondary use, this is also an innovative point of the utility model.Double equal sources are one just to grow up the sixties in last century
The common ion source of kind, is able to satisfy the requirement of the utility model completely.
Simple lens 7：Mainly the ion drawn from ion source is focused.The utility model is saturating using Einzel type
Mirror.
Preaceleration pipe 8：Ion energy is accelerated into 20keV, it is therefore an objective to ion energy and quality of beam are improved, to utilize
Injection magnet separates the ion of different quality number, be conducive to force down ion source can dissipate caused by background interfere.
Injection magnet 2：The effect of injection magnet is to select the ion of different quality, passes through injection magnet in ion
The ion of different quality is separated (as shown in Figure 1) afterwards, by T+(including3He+、HD+, 3H) be sent into accelerating tube while will
After separation4He and D is measured it using Faraday cup 9.The deflection radius of injection magnet is 200mm, and deflection angle is
90 degree.
Quadrupole lenses 10：The purpose of quadrupole lenses is to combine acceleration system by ion focusing at stripper.Quadrupole lenses
Using electrostatic quadrupole lenses.
Accelerating tube 3：The effect of accelerating tube is to carry out ion to accelerate to improve ion energy.The utility model is using single-ended quiet
Electric accelerated mode realizes that particle accelerates.In view of the needs of voltage shield and Ion identification, the utility model will be according to experiment feelings
Condition determines optimal acceleration voltage, at present selected voltage range 60keV--100KeV.There is the business of standard to accelerate in the world
Pipe, is able to satisfy the demand of the utility model.The NEC Corporation in the U.S. has been successfully established single-ended acceleration14The dedicated dress of C accelerator mass spectrometry
It sets, this device provides good reference for the utility model.
Stripper 4：Stripper be the utility model realize tritium and3One key link of He high-sensitivity measurement, stripper
Effect be to disintegrate molecular ion when ion passes through, while isobar ion being made to generate different energy losses.
Tritium,3Molecular ion HD with identical mass number when He is measured+、3H+It is sent to stripper together with tritium.Molecular ion exists
Disintegrate after stripping film as D+、H+Atomic ion is achieved in HD+The exclusion of molecule background；And T+With3He+For isobar
Plain ion, due to3The atomic number of He and T differs 2 times, energy loss (Δ E) and its nuclear power when passing through medium using ion
Square directly proportional (the Δ E ∝ KZ of lotus number (Z)2) characteristic may make T and3He generates different energy losses after passing through stripping film,
So that T+With3He+With different dump energies, in conjunction with magnetic analysis system by T+With3He+Separate (after film stripping,3He+
It is stripped into3He+With it is least a portion of3He++,3He++Can be excluded completely using analysis magnet), it can be achieved that T and3The measurement of He.Stripping
Uniformity from film thickness is to realize this desired key factor.The utility model proposed adoption Si3N4Film is as stripping film, Si3N4
The maximum feature of film is that its thickness uniformity is very good, it can effectively avoid the difference of energy loss caused by the thickness uniformity.
Si3N4Film is widely successfully applied in AMS technology, the utility model proposed adoption with a thickness of 30nm to 50nm Si3N4
As stripping film, specific thickness needs to test measurement.
Analysis magnet 5：The purpose of analysis system is exactly to exclude the molecular ion fragment after stripping film, simultaneously
By the T of different-energy+With3He+It is separated, this system uses deflection radius for 350mm, the double focusing that deflection angle is 90 degree
Magnetic analyzer carries out ion analysis.
Detection system 6：Including detector, electronic system and data analysis system.Detector for measure T and3He's
Number of ions.About in 100keV, this system (is suitable for counting the energy of this device ion using Au-Si surface barrier detector
Rate is less than 103/ s), Computation of Single Channel Multiplying device (be suitable for counting rate less than 107/ s) and Faraday cup (it is big to be suitable for counting rate
In 107/ s) to T and3He is measured.Experiment will select optimal detection system and reality according to situations such as counting rate, noise background
Test condition.Electronic system and data analysis system are mainly by pre-amplifier, main amplifier, multichannel analyzer and analysis
Software composition, for the electronic signal that ion generates to be amplified and analyzed.
The utility model is drawn using cation combines accelerator mass spectrometry and film stripping technology to remove all kinds of obstacles background reality
Existing T and3Highly sensitive, the efficient measurement of He, be in the world for the first time using a set of spectrometer realize T and3The measurement scheme of He, greatly mentions
High T and3He measurement sensitivity and measurement efficiency.
Obviously, it is practical without departing from this can to carry out various modification and variations to the utility model by those skilled in the art
Novel spirit and scope.If in this way, belonging to the utility model claims to these modifications and variations of the present invention
And its within the scope of equivalent technology, then the utility model is also intended to include these modifications and variations.
Claims (10)
1. a kind of T and He-3 accelerator mass spectrometry high-sensitivity measurement device, it is characterised in that：Including the ion for generating cation
The ion that mass number is 3 is sent into accelerating tube, the accelerating tube connection stripping by injection magnet by source, the cation that ion source generates
From device, molecular ion is broken down by monatomic ion by stripper, the stripper is connect with analysis magnet, passes through analysis of magnetic
Iron point opens T and 3He, and the analysis magnet connects detection system, detection system to after separating T and3He is measured respectively.
2. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as described in claim 1, it is characterised in that：Ion source with
Preaceleration pipe is equipped between injection magnet.
3. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as described in claim 1, it is characterised in that：The ion
Source is the double-plasma ion source based on gas sampling.
4. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as described in claim 1, it is characterised in that：In injection magnet
Side be equipped with for separating to injection magnet4The Faraday cup that He and D are measured.
5. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as described in claim 1, it is characterised in that：In the injection
Quadrupole lenses are equipped between magnet and accelerating tube.
6. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as claimed in claim 5, it is characterised in that：The level Four is saturating
Mirror uses electrostatic quadrupole lenses.
7. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as described in claim 1, it is characterised in that：The accelerating tube
Realize that particle accelerates using single-ended electrostatic accelerated mode.
8. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as described in claim 1, it is characterised in that：The stripper
Using Si3N4As stripping film.
9. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as described in claim 1, it is characterised in that：The analysis of magnetic
Iron uses deflection radius for 350mm, the double focusing magnetic analyzer that deflection angle is 90 degree.
10. T and He-3 accelerator mass spectrometry high-sensitivity measurement device as described in claim 1, it is characterised in that：The detection
System includes Au-Si surface barrier detector, Computation of Single Channel Multiplying device and the Faraday cup suitable for different counting rates.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108387633A (en) * | 2018-01-24 | 2018-08-10 | 中国原子能科学研究院 | T and He-3 accelerator mass spectrometry high-sensitivity measurement devices |
| CN110444461A (en) * | 2019-08-13 | 2019-11-12 | 中国原子能科学研究院 | Accelerator mass spectrometry device and accelerator mass spectrometry measurement method |
-
2018
- 2018-01-24 CN CN201820118954.6U patent/CN208109749U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108387633A (en) * | 2018-01-24 | 2018-08-10 | 中国原子能科学研究院 | T and He-3 accelerator mass spectrometry high-sensitivity measurement devices |
| CN108387633B (en) * | 2018-01-24 | 2023-12-15 | 中国原子能科学研究院 | T and 3 high-sensitivity measurement method for mass spectrum of He accelerator |
| CN110444461A (en) * | 2019-08-13 | 2019-11-12 | 中国原子能科学研究院 | Accelerator mass spectrometry device and accelerator mass spectrometry measurement method |
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