CN104181223A - Method for carrying out accelerator mass spectrometry measurement by using super halogen anions of beryllium - Google Patents

Method for carrying out accelerator mass spectrometry measurement by using super halogen anions of beryllium Download PDF

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CN104181223A
CN104181223A CN201410417510.9A CN201410417510A CN104181223A CN 104181223 A CN104181223 A CN 104181223A CN 201410417510 A CN201410417510 A CN 201410417510A CN 104181223 A CN104181223 A CN 104181223A
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energy
mass spectrometry
bef
target sample
beryllium
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CN104181223B (en
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付云翀
张丽
赵国庆
刘起
武振坤
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Institute of Earth Environment of CAS
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Abstract

The invention discloses a method for carrying out accelerator mass spectrometry measurement by using super halogen anions of beryllium. The method is characterized by comprising the following steps: preparing a target sample capable of producing super halogen anions BeF3<->; bombarding the target sample and a PbF2 powder mixing target cone to generate a BeF3<-> beam; crushing the BeF3<-> beam in a tandem accelerator; enabling <9>Be<2+> to enter a mobile Faraday cup for measurement after passing through a main analysis magnet; enabling <10>Be<2+> to pass through along a main beam line and to directly pass through a main electrostatic analyzer and a second magnet at the high-energy end; and finally entering a gas detector for analysis. The method has the beneficial effects that interference of <10>B is effectively inhibited at the extraction stage by the extracted beam which is measured by taking BeF3<-> as <10>Be-AMS, so that the high-energy end of a miniature AMS does not need to be peeled off twice by using an energy-reducing film, and the transmission efficiency of the <10>Be beam is ensured (the high-energy end achieves 100% transmission), the original good beam quality is maintained in the absence of the film, and the risks to experimenters due to the fact that BeO as airborne dust has high toxicity are effectively avoided.

Description

A kind of method that super halogen anion that utilizes beryllium carries out accelerator mass spectrometry measurement
Technical field
The present invention relates to a kind of method that accelerator mass spectrometry is measured, be specifically related to a kind of method that super halogen anion that utilizes beryllium carries out accelerator mass spectrometry measurement, belong to accelerator mass spectrometry field of measuring technique.
Background technology
Along with the development of accelerator mass spectrometry (AMS) technology, to long-life cosmogenic nuclide 10the research of Be (about 1.5Ma of half life period) has obtained development rapidly in short decades, and is widely used in each field of geoscience, environmental science, for example:
1, with accelerator mass spectrometry (AMS), measure 10be reviews solar activity change histories;
2, will speed up device mass spectrum (AMS) measures 10be market demand is in meteorological research, and spike Global Precipitation distributes;
3, with accelerator mass spectrometry (AMS), measure 10be determines the sedimentary age and the speed of glacier, lake or oceanic sediment;
4, with accelerator mass spectrometry (AMS), measure 10be to be to measure the erosion rate on earth's surface, thereby is applied to the research of all kinds of faces;
5, will speed up device mass spectrum (AMS) measures 10be result is for spike and rebuild the fields such as terrestrial magnetic field drift event and geomagnetic field intensity change histories.
For 10the AMS of Be measures key and is effectively to suppress isobar 10the interference of B ( 10b is the stable isotope of B, and its natural content is much larger than Long-lived Radionuclides 10be), in a very long time, can only on the higher large-scale AMS of energy, carry out 10be measures, and along with AMS technology is constantly progressive, at high-energy tail, utilizes film secondary to peel off, and causes 10be can measure being less than on the AMS of 3MV equally.Recent two decades for many years 10be-AMS measures and depends on BeO always -ion is at Cs +the stable output in plasma sputter source, and same BO -at Cs +in plasma sputter source, stable generation causes a large amount of 10b disturbs inevitable.Although small-sized AMS utilizes film to reduce dexterously 10nearly 500 times of the interference of B, still, for 10the transfer efficiency of Be line and quality have also caused greater loss (under 6MeV energy 10after the SiN film of Be by 500nm, finally adding the transfer rate of detector is only 30% left and right, and quality of beam degenerates), and in preparation, there is very high toxicity in BeO sample used.Therefore, for 10other new method that Be measures on small-sized AMS is still significant.
Given this, Canadian Isotrace laboratory X-L.Zhao equals to research and propose first for 2004 and utilizes BeF -(single beryllium fluoride negative ion) stablized and BF -unsettled characteristic, expectation is with BeF -carry out 10the possibility that the AMS of Be measures, but BeF -compare BeO -beam intensity too small (reducing 10-50 doubly), causes the method cannot substitute comparatively satisfactorily BeO -measure.
Summary of the invention
For solving the deficiencies in the prior art, a kind of method that the object of the present invention is to provide super halogen anion that utilizes beryllium to carry out accelerator mass spectrometry measurement, the method not only can be avoided using and falling and can peel off by film secondary at small-sized AMS (< 3MV) high-energy tail, and 10the transfer efficiency of Be line can reach 100% transmission at high-energy tail, simultaneously 10the quality of Be line can access well and maintain.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
A method of utilizing the super halogen anion of beryllium to carry out accelerator mass spectrometry measurement, is characterized in that, comprises the following steps:
(1) preparation can the super halogen anion BeF of output 3 -target sample;
(2) in the target sample preparing, sneak into PbF 2powder, is then filled into AMS and measures with target cone, uses Cs in ion gun +ion continues the aforementioned target cone of bombardment and produces BeF 3 -line;
(3) by ion gun, draw BeF 3 -line, then BeF 3 -line is done first energy by the electrostatic analyzer of low energy end and is screened, and next enters jump magnet, then by BeF 3 -line injects tandem accelerator by low energy end, in aforementioned tandem accelerator strip gas by molion smash, 10be 2+being accelerated to energy is 5.97MeV, 9be 2+being accelerated to energy is 5.94MeV;
(4) 10be 2+with 9be 2+at high-energy tail, pass through main analysis magnet, then 9be 2+enter removable Faraday cup and measure, 10be 2+along main beam line, pass through;
(5) 10be 2+along main beam line, by rear main electrostatic analyzer and second block of magnet of high-energy tail of directly passing through, finally enter gas detector analysis.
The method that the aforesaid super halogen anion that utilizes beryllium carries out accelerator mass spectrometry measurement, is characterized in that, in step (), aforementioned target sample is the salt containing Be and F.
The method that the aforesaid super halogen anion that utilizes beryllium carries out accelerator mass spectrometry measurement, is characterized in that, in step (), aforementioned target sample is BaBeF 4.
The method that the aforesaid super halogen anion that utilizes beryllium carries out accelerator mass spectrometry measurement, is characterized in that, in step (two), and BaBeF 4target sample and PbF 2powder mixes according to the ratio of volume ratio 1:2-1:5.
The method that the aforesaid super halogen anion that utilizes beryllium carries out accelerator mass spectrometry measurement, is characterized in that, in step (three), the energy jitter value of aforementioned jump magnet is 0V ,-522V.
Usefulness of the present invention is:
1, with the super halogen anion BeF of beryllium 3 -as 10the educt beaming flow that Be-AMS measures (has replaced traditional BeO -mode as educt beaming flow), in measurement, utilized the super halogen anion BeF of beryllium 3 -superior performance, effectively suppressed in the stage of drawing 10the interference of B, make small-sized AMS (< 3MV), even compact AMS (< 1MV) high-energy tail without re-use fall can film the classic method peeled off of secondary, cause 10the transfer efficiency of Be line is guaranteed, and at high-energy tail, can reach 100% transmission (original BeO -mode high-energy tail transfer rate approximately 30% as educt beaming flow), and can not changed without quality of beam after film, maintained original good quality of beam, compact AMS really be accomplished compacter;
2, produce BeF 3 -initial target sample BaBeF 4replace traditional BeO target sample, effectively avoided BeO to have as airborne dust the risk that very high toxicity brings experimenter.
Accompanying drawing explanation
Fig. 1 prepares BaBeF in the method for measuring at accelerator mass spectrometry of the present invention 4the process flow diagram of target sample;
Fig. 2 is that background sample is at the energy spectrogram of first positive plate of detector;
Fig. 3 is that background sample is at the energy spectrogram of second positive plate of detector.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is done to concrete introduction.
The method that the present invention utilizes the super halogen anion of beryllium to carry out accelerator mass spectrometry measurement, comprises the following steps:
One, prepare target sample BaBeF 4
Target sample is for the super halogen anion BeF of efficient output 3 -, it can be that target sample is selected BaBeF in the present embodiment containing the salt of Be and F 4.
With reference to Fig. 1, BaBeF 4the concrete preparation flow of target sample is as follows:
1, in 1g Loess Samples, add successively 0.5mMole 9be carrier, 6ml H 2o 2solution (H 2o and H 2o 2volume ratio be 1:1), 6ml 12M HCl, mix rear filtering residue, the solution of reservation is designated as to sample solution A.
Residue is proceeded to process:
First, residue is soaked to 24h with 25ml 6M HCl, centrifugal treating, merges supernatant and sample solution A;
Then, the residue obtaining is for the second time soaked by 20ml secondary deionized water, centrifugal treating, merges supernatant and sample solution A.
2, evaporate to dryness sample solution A, then adds 2ml 1M HCl to dissolve, and centrifugal treating, leaves and takes supernatant, and supernatant is designated as to sample solution B.
3, by Zeo-karb processing sample solution B, and carry out drip washing with 110ml 1M HCl, obtain eluent.
4, eluent heating is concentrated into 20ml, with ammoniacal liquor adjust pH to 8.5 (pH value within the scope of 8-9 all can), standing; Then use NaOH adjust pH to 14, standing, after centrifugal treating, get supernatant, then use HNO 3supernatant is adjusted to acidity, standing; Finally use ammoniacal liquor adjust pH to 8.5 (pH value within the scope of 8-9 all can), centrifugal treating, leaves and takes precipitation, and this is precipitated as Be (OH) 2precipitation.
5, with 1ml 0.2M HCl, dissolve Be (OH) 2precipitation, obtains solution, and this solution is designated as sample solution C.
6, in sample solution C, add 0.5ml 1M CsF, mix and move liquid, and rinse with 1ml 0.2M HCl, obtain solution, this solution is designated as sample solution D.
7, in sample solution D, add 0.25ml 0.2M BaCl 2, then under 80 ℃ of conditions, dry, obtain BaBeF 4target sample.
In the method for the invention, use BaBeF 4target sample produces BeF 3 -, replaced traditional BeO target sample, effectively avoided BeO to have as airborne dust the risk that very high toxicity brings experimenter.
Two, produce BeF 3 -line
1, to the BaBeF preparing 4in target sample, sneak into PbF 2powder, BaBeF 4target sample and PbF 2powder mixes (volume ratio within the scope of 1:2-1:5 all can), PbF according to the ratio of volume ratio 1:3 2powder itself is a kind of good ion conductor (do not possess electric conductivity during normality, but it having good electric conductivity under ionic state), meanwhile, and PbF 2the entrained F ion of powder can fully provide BeF 3 -produce needed excessive F ion.
Traditional BeO target sample, in filling process, is sneaked into 300 object Cu powder (or the better metal powder of other electric conductivity) as assist medium according to volume ratio 1:3, to realize the electric conductivity of target cone.
2, BaBeF 4target sample and PbF 2powder is filled into AMS and measures with target cone after mixing, target cone, as the carrying container of target sample, also exists as drawing negative electrode simultaneously.
3, in ion gun, use the Cs of 6keV energy +ion continues bombardment BaBeF 4target sample and PbF 2powder hybrid target cone, makes PbF 2the characteristic of ion conductor is embodied, now with PbF 2in sputtering target for assist medium, produce BeF 3 -line, the super halogen anion BeF of beryllium 3 -electron binding energy is large, compared with other negative ion stable (selection of fluorine is that its electron affinity is the strongest in adjacent elements, its quality be in halogen minimum and without other isotopes or isobar).
Due to 10the isobar of Be 10b will be converted into by large portion 10bF 4 -, only have a little to be converted into 10bF 3 -, therefore, excessive a little F ion is particularly important.
Three, 10be 2+with 9be 2+in tandem accelerator, accelerate
1, by ion gun, draw the BeF with 35keV energy 3 -line, then BeF 3 -line is done first energy by 54 ° of electrostatic analyzers of low energy end and is screened, and next entering radius is 400mm, 90 ° of jump magnet, and 90 ° of jump magnet select and guarantee BeF as momentum 3 -in 9beF 3 -with 10beF 3 -all can prolong main beam line and pass through, therefore the energy of this magnet " jump " is worth by former BeO -the 0V of method ,-1346V are set as 0V ,-522V, and quality of beam is regulated and guaranteed by simple lens and guiding during this period.
2, by BeF 3 -line injects tandem accelerator by low energy end, and in this tandem accelerator, strip gas is by BeF 3 -molion smashes, and peels off nucleic electronics and make the final positively charged of Be ion, is able to secondary and accelerates.
3, for making BeF 3 -molion is crashed to pieces and peels off to Be 2+, in the situation that keeping final identical energy, Ar strip gas amount is reduced to former BeO -method 40% (by original 8.3 * 10 -3mbar is reduced to 3.4 * 10 -3mbar), terminal voltage is adjusted to 2778kV by original 2500kV simultaneously, now, 10be 2+being accelerated to energy is 5.97MeV, 9be 2+being accelerated to energy is 5.94MeV (former BeO -method 10be 2+energy be 5.97MeV, 9be 2+energy be 5.91MeV).
Four, high-energy tail 10be 2+with 9be 2+separated
10be 2+with 9be 2+at high-energy tail through 115 ° of main analysis magnets, after 115 ° of main analysis magnets 9be 2+enter removable Faraday cup and measure, and 10be 2+along main beam line, pass through.
Five, 10be 2+enter gas detector
Former BeO -going out in method connects the SiN film that secondary peels off after 115 ° of main analysis magnets and do not re-use, but 10be 2+along main beam line, by rear 65 ° of main electrostatic analyzers and second block of 30 ° of magnet of high-energy tail of directly passing through, finally enter gas detector analysis.
The SiN film of peeling off due to secondary does not re-use, and makes 10be 2+not only the transport stream at high-energy tail has guaranteed 100%, and the quality of line is also guaranteed.Former two groups of quadrupole lenses only need one group of work just can keep good quality of beam.
10be 2+enter after gas detector, originally BeO -method is by SiN film and in conjunction with can reducing by 10 after the inhibition of B after 65 ° of main electrostatic analyzers and second block of 30 ° of magnet of high-energy tail 6times, and method of the present invention will reduce by 10 after the inhibition of B 4doubly, although the magnitude that does not have former method to reduce is many, be reduced to the analyzable magnitude of detector, enough 10the measurement of Be.
Fig. 2 and Fig. 3 have shown that respectively background sample is at first positive plate of detector and the energy spectrogram of second positive plate.
As seen from Figure 2: 10be and 10between the energy spectrum region of B, separate completely, 10beNeng road can there is no other interference.
As seen from Figure 3: 10be and 10between the energy spectrum region of B, separate completely, and 10in between Be energy spectrum region, there is the interference of other fragments.
Because final measurement is according to first positive plate and second positive plate coincidence measurement, the ion that simultaneously meets the interval condition of two pole plates just can be considered to effective 10be event, therefore, method of the present invention can be carried out completely 10be-AMS measures.
In sum, method of the present invention is with the super halogen anion BeF of beryllium 3 -as 10the educt beaming flow that Be-AMS measures (has replaced traditional BeO -mode as educt beaming flow), in measurement, utilized the super halogen anion BeF of beryllium 3 -superior performance, effectively suppressed in the stage of drawing 10the interference of B, makes without re-using, to fall the classic method that energy film secondary is peeled off at small-sized AMS (< 3MV) high-energy tail, causes 10the transfer efficiency of Be line is guaranteed, and at high-energy tail, can reach 100% transmission (original BeO -mode high-energy tail transfer rate approximately 30% as educt beaming flow), and can not changed without quality of beam after film, maintained original good quality of beam.
It should be noted that, above-described embodiment does not limit the present invention in any form, and all employings are equal to replaces or technical scheme that the mode of equivalent transformation obtains, all drops in protection scope of the present invention.

Claims (5)

1. a method of utilizing the super halogen anion of beryllium to carry out accelerator mass spectrometry measurement, is characterized in that, comprises the following steps:
(1) preparation can the super halogen anion BeF of output 3 -target sample;
(2) in the target sample preparing, sneak into PbF 2powder, is then filled into AMS and measures with target cone, uses Cs in ion gun +ion continues the described target cone of bombardment and produces BeF 3 -line;
(3) by ion gun, draw BeF 3 -line, then BeF 3 -line is done first energy by the electrostatic analyzer of low energy end and is screened, and next enters jump magnet, then by BeF 3 -line injects tandem accelerator by low energy end, in described tandem accelerator strip gas by molion smash, 10be 2+being accelerated to energy is 5.97MeV, 9be 2+being accelerated to energy is 5.94MeV;
(4) 10be 2+with 9be 2+at high-energy tail, pass through main analysis magnet, then 9be 2+enter removable Faraday cup and measure, 10be 2+along main beam line, pass through;
(5) 10be 2+along main beam line, by rear main electrostatic analyzer and second block of magnet of high-energy tail of directly passing through, finally enter gas detector analysis.
2. the method that the super halogen anion that utilizes beryllium according to claim 1 carries out accelerator mass spectrometry measurement, is characterized in that, in step (), described target sample is the salt containing Be and F.
3. the method that the super halogen anion that utilizes beryllium according to claim 2 carries out accelerator mass spectrometry measurement, is characterized in that, in step (), described target sample is BaBeF 4.
4. the method that the super halogen anion that utilizes beryllium according to claim 3 carries out accelerator mass spectrometry measurement, is characterized in that, in step (two), and BaBeF 4target sample and PbF 2powder mixes according to the ratio of volume ratio 1:2-1:5.
5. the method that the super halogen anion that utilizes beryllium according to claim 1 carries out accelerator mass spectrometry measurement, is characterized in that, in step (three), the energy jitter value of described jump magnet is 0V ,-522V.
CN201410417510.9A 2014-08-22 2014-08-22 A kind of method that super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement Expired - Fee Related CN104181223B (en)

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CN106501291A (en) * 2016-10-18 2017-03-15 中国科学院地球环境研究所 One kind adopts AMS on-line measurements under same target sample7Be with10The method of Be abundance
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