CN108508475A - C-14 high-sensitivity measurement devices based on gas sampling positive ion source - Google Patents
C-14 high-sensitivity measurement devices based on gas sampling positive ion source Download PDFInfo
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- CN108508475A CN108508475A CN201810068308.8A CN201810068308A CN108508475A CN 108508475 A CN108508475 A CN 108508475A CN 201810068308 A CN201810068308 A CN 201810068308A CN 108508475 A CN108508475 A CN 108508475A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/24—Measuring radiation intensity with semiconductor detectors
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Abstract
The present invention relates to a kind of 14 high-sensitivity measurement devices of C based on gas sampling positive ion source, it include the microwave ion source of the cation for generating carbon, the microwave ion source is connect with charge-exchange device, the cation of carbon is converted into anion by charge-exchange device, the charge-exchange device connects injection magnet, the injection magnet is accelerated the anion injection of carbon and gas stripping system by beam focusing system, accelerate that molecular ion is disintegrated the anion stripping by carbon simultaneously to further accelerate after cation with gas stripping system, the acceleration and gas stripping system linking parsing magnet and electrostatic analyzer, the molecular ion disintegrated is excluded and is incited somebody to action by analysis magnet14C、13C、12C is detached so that14C enters electrostatic analyzer, and the electrostatic analyzer is connected with detector.The present invention realizes14The rapidly and efficiently measurement of C sample, while meeting miniaturization14C Sensitive Determinations.
Description
Technical field
The present invention relates to radioactive isotope measuring techniques, and in particular to a kind of C-14 based on gas sampling positive ion source
High-sensitivity measurement device.
Background technology
14C is cosmogenic nuclide, and half-life period is 5730 ± 40 years.Due to the presence of carbon cycle, in a long time,14C
It can constantly be accumulated in atmospheric environment and biotic environment, decay to and generate again, until reaching dynamic equilibrium.Just because of this,14C
It is widely used in the natural subject such as archaeology, geology, life science.14C, which has, to be so widely applied, then measurement method
Accuracy, the stability of survey tool and the high efficiency of time of measuring are ensuring that14One important prerequisite item of C applications
Part.Tradition14For C measurement methods based on liquid scintillation counting, basic principle is generated according to ray and matter interaction
Fluorescent effect.This mode is just not accurate enough, stable, efficient for detection Trace elements and for analyzing rare particle.Accelerate
Device mass spectrum (AMS) technology is a kind of measurement method to grow up middle and later periods the 1970s, compared with conventional method, the party
The composite construction of method substance not monitored and the influence of matrix effect can also effectively exclude various background interference and (divide
Sub- background and isobar background), greatly improving measurement sensitivity, (isotope abundance reaches 10-16), it is kernel analysis skill
The highest Nuclide measurement method of art sensitivity so far.Therefore, at present in the world substantially all use accelerator mass spectrometry method into
Row14The measurement of C.For14Also from pervious large-scale accelerator to miniaturization and low energyization development for C measuring apparatus, at present
The compact type that terminal voltage is 0.5MV is developed14C measuring devices, the Unipolar electrostatic type that accelerating potential is 0.25MV14C measuring devices
And terminal voltage is the miniature of 0.2MV14C measuring devices.But all these devices all there are one common feature be exactly from from
Component draws anion, and to draw anion just need to prepare sample preparation at form of graphite graphite process it is not only time-consuming but also
Arduously, and these anion source systems also have ionizing efficiency low, the defects of needing to clean ion source, need to be bored with caesium and target.
Therefore, at present in the world also in development based on cation14The AMS high-sensitivity measurement technique studies of C, and research and develop based on gas into
Sample and positive ion electrospray from14C high-sensitivity measurement methods.
Invention content
The purpose of the present invention is to provide it is a kind of based on gas sampling and positive ion electrospray from14The small-sized highly sensitive accelerators of C
Mass-spectrometer measurement device, to realize14The rapidly and efficiently measurement of C sample, while meeting miniaturization14C Sensitive Determinations.
Technical scheme is as follows：It is a kind of based on gas sampling positive ion source14C high-sensitivity measurement devices, including
Microwave ion source for the cation for generating carbon, the microwave ion source are connect with charge-exchange device, pass through charge-exchange device
The cation of carbon is converted into anion, the charge-exchange device connects injection magnet, and the injection magnet passes through beam focusing
The anion injection acceleration of carbon and gas stripping system are accelerated to disintegrate molecular ion with gas stripping system and simultaneously will by system
The anion stripping of carbon is further accelerates after cation, the acceleration and gas stripping system linking parsing magnet and coulostatic analysis
The molecular ion disintegrated is excluded and is incited somebody to action by device, analysis magnet14C、13C、12C is detached so that14C enters electrostatic analyzer, described quiet
Electroanalyzer is connected with detector, realizes14The measurement of C.
Further, as described above based on gas sampling positive ion source14C high-sensitivity measurement devices, wherein described is micro-
The CO that wave ion source generates sample combustion2It is ionized into the cation of carbon.
Further, as described above based on gas sampling positive ion source14C high-sensitivity measurement devices, wherein charge-exchange
Charge-exchange medium in device is magnesium steam or isobutane gas.
Further, as described above based on gas sampling positive ion source14C high-sensitivity measurement devices, wherein the injection
Magnet side is equipped with biasing Faraday cup and leads to while injection magnet accelerates the anion injection of carbon with gas stripping system
Cross biasing Faraday cup pair12C-、13C-It is measured.
Further, as described above based on gas sampling positive ion source14C high-sensitivity measurement devices, wherein the beam
It flows focusing system and uses electrostatic quadrupole lenses.
Further, as described above based on gas sampling positive ion source14C high-sensitivity measurement devices, wherein described adds
Speed and gas stripping system include gas stripper and are arranged accelerating tube at gas stripper both ends.
Further, as described above based on gas sampling positive ion source14C high-sensitivity measurement devices, wherein the analysis
Magnet side is equipped with biasing Faraday cup, and biasing Faraday cup pair is utilized near analysis magnet image point13C and12C carries out ratio
Measurement.
Further, as described above based on gas sampling positive ion source14C high-sensitivity measurement devices, wherein the spy
Device is surveyed using golden surface barrier semiconductor detector.
Beneficial effects of the present invention are as follows：
1. the present invention uses gas sampling, the lengthy process that conventional method prepares graphite is avoided, time and people are saved
Power greatly improves measurement efficiency；
2. compared with conventional anion ionization method, the present invention is using positive ion electrospray from improving ionizing efficiency；
3. the ion source of the present invention is in ground potential so that gas feed-in and ion source operation are more convenient；
4. the compact type of whole system and Miniaturization Design, have saved lab space and measurement cost；
5. system has the advantages that measurement sensitivity is high, good basis is provided for its application in all fields.
Description of the drawings
Fig. 1 be gas sampling and positive ion electrospray from14C-AMS system principle schematic diagrames；
Fig. 2 be gas sampling positive ion electrospray from14C-AMS system structure diagrams.
Specific implementation mode
The present invention is described in detail below with reference to the accompanying drawings and embodiments.
The present invention provides it is a kind of based on gas sampling and positive ion electrospray from14The small-sized highly sensitive accelerator mass spectrometries of C measure
Device, to realize14The rapidly and efficiently measurement of C sample, while meeting miniaturization14C Sensitive Determinations.Whole device system
Realize that gas sampling need not be graphitized flow, test sample efficiency can be improved twice or more, using positive ion electrospray from improve from
Ionizing efficiency, can be improved a magnitude by component ionizing efficiency, and whole system carries out Miniaturization Design and makes easy to operate, measurement
Flow is convenient and floor space is small.
The overall technological scheme of the present invention is as shown in Figure 1:The CO generated using sample combustion2Enter microwave ion source by CO2Electricity
From the cation at carbon；The carbonium ion of generation is about to pass into charge-exchange device after -30KV accelerates to convert C+ through voltage
For C-；The anion of generation further accelerates ground potential, and anion cannot be formed based on nitrogen in this transfer process, to effectively
It will14Isobar when C is measured14N interference is effectively excluded；C- ions after acceleration are sent into the injection magnet of AMS by carbon
Isotopic separation, will14C utilizes biasing Faraday cup pair while being sent into accelerator12C and13C is measured, for reality
It is existing12C、13C、14The Accurate Determining of C will use alternately injection technique；It is admitted to accelerator14C-It is+150KV through head voltage
Enter gas stripping system after acceleration, molecule background is disintegrated while further accelerating the stripping of C- ions after cation；It is stripped
It is selected using analysis magnet and electrostatic analyzer after acceleration14C+ removes all kinds of obstacles background simultaneously, finally detector is utilized to survey
Amount14The counting of C；Biasing Faraday cup pair is utilized near analysis magnet image point simultaneously13C and12C is measured to realize13C、12The measurement of C ratios.
The specific embodiment of the invention provide based on gas sampling positive ion electrospray from14C-AMS system structures such as Fig. 2 institutes
Show, whole system includes mainly microwave ion source 1, charge-exchange device 2, injection magnet 3, beam focusing system 5, acceleration and gas
Stripper 6,10 several parts of analysis magnet 8, electrostatic analyzer 9 and detector, wherein in addition to charge-exchange device 2 and gas stripping
For 6 outer other parts of device all in ground potential, the wherein current potential of charge-exchange device is -30KV, the current potential of gas stripper is+
150KV。
Microwave ion source 1：The effect of this part is by CO2It is ionized into the cation of C；Using the microwave of frequency 2.45GHZ
By CO2C+ ions are ionized into, while to realize the measurement of small sample, the space of ion source is 40 cubic centimetres.
Charge-exchange device 2：The effect of this part is that the cation of carbon is converted to the anion of carbon, carbon is converted to bear from
The purpose of son is to exclude14N may be right14C is interfered caused by measuring.The medium of charge-exchange uses magnesium vapor or iso-butane
Gas.
Injection magnet 3：It will using injection magnet 314C-Ion (including12CH2-, 13CH-) it is sent into accelerating sections, it is set using side
Faraday cup 4 is right12C-With13C-It is measured.In order to realize the accurate measurement of carbon isotope, the present invention is using alternately injected system
Alternately will14C、13C and12C is sent into accelerator.The deflection radius of injection magnet 3 is 30cm.
Beam focusing system：Purpose is to combine acceleration system by ion focusing at stripper.Quadrupole lenses use electrostatic
Type quadrupole lenses 5.
Acceleration and stripping system：Including gas stripper 6 and accelerating tube 7 at gas stripper both ends is set, this is
System accelerating potential 150KV positive pressures, enter gas stripping system, the purpose of gas stripping system is will to bear after by C- ion accelerations
Ion stripping simultaneously will at cation12CH-、3H+Equimolecular is broken down into atomic ion, and it is right to exclude its14The interference of C, stripped production
Raw cation is accelerated again.
Analysis magnet 8：The molecular ion disintegrated is excluded using analysis magnet, simultaneously will14C、13C and12C is detached so that14C enters coulostatic analysis system.The deflection radius of analysis magnet is 35cm.
Electrostatic analyzer 9：In order to realize14The Sensitive Determination of C, it is necessary to need the joint of momentum and energy that could effectively arrange
Except background, the deflection radius of electrostatic analyzer 9 is 35cm.
Detection system：Including detector 10, electronic system and data analysis system.Detector 10 is using golden surface barrier type half
Conductor detector pair14C is measured.
This system has the characteristics that：(1) use the microwave gas ion source of gas sampling that can realize CO2It is direct into
Sample realizes online quickly measurement；(2) positive ion source is used to improve the ionizing efficiency of carbon, (3) ion source is in ground potential so that
Gas feed-in and ion source operation are convenient, and (4) convert C+ to C- ions using charge-exchange, eliminate14The interference (4) of N adds
Fast device mass spectrum uses small-sized 0.15MV tandems AMS systems, reduces instrument cost, simplifies measuring apparatus；(5) whole system in addition to
Two ion-exchangers are in the outer other parts of high potential and are in ground potential.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.If in this way, belonging to the model of the claims in the present invention and its equivalent technology to these modifications and changes of the present invention
Within enclosing, then the present invention is also intended to include these modifications and variations.
Claims (8)
1. a kind of C-14 high-sensitivity measurement devices based on gas sampling positive ion source, it is characterised in that：Including being used to generate carbon
Cation microwave ion source, the microwave ion source connect with charge-exchange device, by charge-exchange device by carbon just from
Son is converted to anion, and the charge-exchange device connects injection magnet, and the injection magnet is by beam focusing system by carbon
Anion injection accelerates that molecular ion is disintegrated the anion by carbon simultaneously with gas stripping system with gas stripping system, acceleration
Stripping is further accelerates after cation, the acceleration and gas stripping system linking parsing magnet and electrostatic analyzer, analysis magnet
The molecular ion disintegrated is excluded and incited somebody to action14C、13C、12C is detached so that14C enters electrostatic analyzer, the electrostatic analyzer and spy
It surveys device to be connected, realize14The measurement of C.
2. the C-14 high-sensitivity measurement devices based on gas sampling positive ion source as described in claim 1, it is characterised in that：Institute
The CO that the microwave ion source stated generates sample combustion2It is ionized into the cation of carbon.
3. the C-14 high-sensitivity measurement devices based on gas sampling positive ion source as described in claim 1, it is characterised in that：Electricity
Charge-exchange medium in lotus exchanger is magnesium steam or isobutane gas.
4. the C-14 high-sensitivity measurement devices based on gas sampling positive ion source as described in claim 1, it is characterised in that：Institute
It states injection magnet side and is equipped with biasing Faraday cup, injection magnet accelerates the anion injection of carbon same with gas stripping system
When, by biasing Faraday cup pair12C-、13C- is measured.
5. the C-14 high-sensitivity measurement devices based on gas sampling positive ion source as described in claim 1, it is characterised in that：Institute
The beam focusing system stated uses electrostatic quadrupole lenses.
6. the C-14 high-sensitivity measurement devices based on gas sampling positive ion source as described in claim 1, it is characterised in that：Institute
The acceleration stated and gas stripping system include gas stripper and are arranged accelerating tube at gas stripper both ends.
7. the C-14 high-sensitivity measurement devices based on gas sampling positive ion source as described in claim 1, it is characterised in that：Institute
It states analysis magnet side and is equipped with biasing Faraday cup, biasing Faraday cup pair is utilized near analysis magnet image point13C and12C into
The measurement of row ratio.
8. the C-14 high-sensitivity measurement devices based on gas sampling positive ion source as described in claim 1, it is characterised in that：Institute
The detector stated is using golden surface barrier semiconductor detector.
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| CN201810068308.8A CN108508475A (en) | 2018-01-24 | 2018-01-24 | C-14 high-sensitivity measurement devices based on gas sampling positive ion source |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113490324A (en) * | 2021-06-24 | 2021-10-08 | 中国原子能科学研究院 | Stripping gas input device of small tandem accelerator |
| CN113866258A (en) * | 2021-09-08 | 2021-12-31 | 北京大学 | Positive ion mass spectrum14C measuring method and positive ion mass spectrum device |
| CN113905500A (en) * | 2021-10-12 | 2022-01-07 | 中国原子能科学研究院 | Tandem accelerator |
| CN114072669A (en) * | 2019-07-05 | 2022-02-18 | 积水化学工业株式会社 | Method for discriminating source of carbon raw material of chemical substance |
| CN115763215A (en) * | 2022-09-27 | 2023-03-07 | 广州聚智科技发展有限公司 | Thermal surface ionization mass spectrum structure |
| CN115825213A (en) * | 2022-09-28 | 2023-03-21 | 中国原子能科学研究院 | Rapid measurement method, storage medium and system for gas emission of nuclear facility |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114072669A (en) * | 2019-07-05 | 2022-02-18 | 积水化学工业株式会社 | Method for discriminating source of carbon raw material of chemical substance |
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| CN115763215A (en) * | 2022-09-27 | 2023-03-07 | 广州聚智科技发展有限公司 | Thermal surface ionization mass spectrum structure |
| CN115825213A (en) * | 2022-09-28 | 2023-03-21 | 中国原子能科学研究院 | Rapid measurement method, storage medium and system for gas emission of nuclear facility |
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