CN104181223B - A kind of method that super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement - Google Patents
A kind of method that super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement Download PDFInfo
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- CN104181223B CN104181223B CN201410417510.9A CN201410417510A CN104181223B CN 104181223 B CN104181223 B CN 104181223B CN 201410417510 A CN201410417510 A CN 201410417510A CN 104181223 B CN104181223 B CN 104181223B
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Abstract
The invention discloses a kind of method that super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement, it is characterised in that comprise the following steps: preparation can the super halogen anion BeF of output3 -Target sample；Bombardment target sample and PbF2Powder hybrid target cone produces BeF3 -Line；BeF3 -Line is crashed to pieces in tandem accelerator；After main analysis magnet9Be2+Enter removable Faraday cup measurement,10Be2+Pass through along main beam line；10Be2+Either directly through main electrostatic analyzer and second block of Magnet of high-energy tail, eventually enter into gas detector and be analyzed.The invention have benefit that: with BeF3 -As10The educt beaming flow that Be-AMS measures, namely effectively inhibited in the extraction stage10The interference of B so that drop at small-sized AMS high-energy tail can peel off by film secondary without re-using, cause10The efficiency of transmission of Be line is guaranteed (high-energy tail reaches 100% transmission), and without maintaining original good quality of beam after film；Effectively prevent BeO and there is, as airborne dust, the risk that experimenter is brought by significantly high toxicity.
Description
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 utilizing beryllium is accelerated device mass-spectrometer 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 nuclide10The research of Be (half-life is about 1.5Ma) obtains rapid development in short decades, and geoscience, environmental science each field in be widely used, for instance:
1, measure with accelerator mass spectrometry (AMS)10Be reviews solar activity change histories；
2, accelerator mass spectrometry (AMS) is measured10Be market demand is in meteorological research, and spike Global Precipitation is distributed；
3, measure with accelerator mass spectrometry (AMS)10Be determines the sedimentary age and the speed of glacier, lake or marine sediment；
4, measure with accelerator mass spectrometry (AMS)10Be is to measure the erosion rate on earth's surface, thus being applied to the research of all kinds of face；
5, accelerator mass spectrometry (AMS) is measured10Be result is for spike and the field such as earth's magnetic field excursion signal and geomagnetic field intensity change histories of reconstruction.
For10The AMS measurement of Be it is critical only that and effectively suppresses isobar10The interference of B (10B is the stable isotope of B, and its natural content is much larger than Long-lived Radionuclides10Be), can only carry out on the large-scale AMS that energy is higher in a very long time10Be measures, and along with AMS technology constantly improves, utilizes thin film secondary to peel off at high-energy tail, causes10Be is equally possible to be measured less than on the AMS of 3MV.Recent two decades is for many years10Be-AMS measures and depends on BeO always-Ion is at Cs+The stable output in plasma sputter source, and same BO-At Cs+Plasma sputter source is stablized generation and causes substantial amounts of10B interference is inevitable.Although small-sized AMS utilizes thin film to reduce dexterously10Nearly 500 times of the interference of B, but, for10The efficiency of transmission of Be line and quality also result in greater loss (under 6MeV energy10Be is only about 30% by being eventually adding the transfer rate of detector after the SiN film of 500nm, and quality of beam degenerates), and in preparation, there is significantly high toxicity in BeO sample used.Therefore, for10Other new method that Be measures on small-sized AMS is still significant.
In consideration of it, Canada Isotrace laboratory X-L.Zhao utilizes BeF equal within 2004, researching and proposing first-(single beryllium fluoride anion) is stablized and BF-Unstable characteristic, it is desirable to BeF-Carry out10The probability that the AMS of Be measures, but BeF-Compare BeO-Beam intensity too small (reducing 10-50 times), causes the method cannot substitute BeO comparatively satisfactorily-Measurement.
Summary of the invention
For solving the deficiencies in the prior art, it is an object of the invention to provide a kind of method that super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement, the method is possible not only to avoid using at small-sized AMS (< 3MV) high-energy tail dropping and peeling off by film secondary, and10The efficiency of transmission of Be line can reach 100% transmission at high-energy tail, simultaneously10The quality of Be line can well be maintained.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that:
A kind of method that super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement, it is characterised in that comprise the following steps:
(1) preparation can the super halogen anion BeF of output3 -Target sample；
(2) in the target sample prepared, it is mixed into PbF2Powder, is then filled into AMS measurement target cone, uses Cs in an ion source+The aforementioned target cone of ion constant bombardment produces BeF3 -Line；
(3) BeF is drawn by ion source3 -Line, then BeF3 -Line does the screening of first energy by the electrostatic analyzer of mental retardation end, next enters jump Magnet, then by BeF3 -Line by mental retardation end inject tandem accelerator, in aforementioned tandem accelerator strip gas molecular ion is smashed,10Be2+Being accelerated to energy is 5.97MeV,9Be2+Being accelerated to energy is 5.94MeV；
(4)10Be2+With9Be2+At high-energy tail by main analysis magnet, then9Be2+Enter removable Faraday cup measurement,10Be2+Pass through along main beam line；
(5)10Be2+Either directly through main electrostatic analyzer and second block of Magnet of high-energy tail after passing through along main beam line, eventually enter into gas detector and be analyzed.
The method that the aforesaid super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement, it is characterised in that in step (), aforementioned target sample is the salt containing Be and F.
The method that the aforesaid super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement, it is characterised in that in step (), aforementioned target sample is BaBeF4。
The method that the aforesaid super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement, it is characterised in that in step (two), BaBeF4Target sample and PbF2Powder mixes according to the ratio of volume ratio 1:2-1:5.
The method that the aforesaid super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement, it is characterised in that in step (three), the energy jitter value of aforementioned jump Magnet is 0V ,-522V.
The invention have benefit that:
1, with the super halogen anion BeF of beryllium3 -As10The educt beaming flow that Be-AMS measures (instead of traditional BeO-Mode as educt beaming flow), measurement make use of the super halogen anion BeF of beryllium3 -Superior performance, namely effectively inhibited in the extraction stage10The interference of B so that drop, without re-using, the traditional method that energy film secondary is peeled off at small-sized AMS (< 3MV), even compact AMS (< 1MV) high-energy tail, cause10The efficiency of transmission of Be line is guaranteed, and can reach 100% transmission (originally BeO at high-energy tail-Mode high-energy tail transfer rate about 30% as educt beaming flow), and will not be changed without quality of beam after film, maintain original good quality of beam so that compact AMS is truly realized compacter；
2, BeF is produced3 -Initial target sample BaBeF4Instead of traditional BeO target sample, effectively prevent BeO and there is, as airborne dust, the risk that experimenter is brought by significantly high toxicity.
Accompanying drawing explanation
Fig. 1 is preparation BaBeF in the method that the accelerator mass spectrometry of the present invention is measured4The flow chart of target sample；
Fig. 2 is the background sample energy spectrogram at first piece of positive plate of detector；
Fig. 3 is the background sample energy spectrogram at second piece of positive plate of detector.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention done concrete introduction.
The present invention utilizes the method that the super halogen anion of beryllium is accelerated device mass-spectrometer measurement, comprises the following steps:
One, target sample BaBeF is prepared4
Target sample is used for the super halogen anion BeF of efficient output3 -, it can be the salt containing Be and F, and BaBeF selected by target sample in the present embodiment4。
With reference to Fig. 1, BaBeF4The concrete preparation flow of target sample is as follows:
1, in 1g Loess Samples, it is sequentially added into 0.5mMole9Be carrier, 6mlH2O2Solution (H2O and H2O2Volume ratio be 1:1), 6ml12MHCl, filter residue after mix homogeneously, the solution of reservation be designated as sample solution A.
Proceed residue to process:
First, residue 25ml6MHCl is soaked 24h, centrifugal treating, supernatant is merged with sample solution A；
Then, residue 20ml secondary deionized water second time obtained is soaked, and supernatant is merged by centrifugal treating with sample solution A.
2, it is evaporated sample solution A, is subsequently adding 2ml1MHCl and dissolves, centrifugal treating, leave and take supernatant, supernatant is designated as sample solution B.
3, process sample solution B with cation exchange resin, and carry out drip washing with 110ml1MHCl, it is thus achieved that eluent.
4, eluent heating is concentrated into 20ml, adjusts pH value to 8.5 (pH value is within the scope of 8-9) with ammonia, stand；Then adjust pH value to 14 with NaOH, stand, take supernatant after centrifugal treating, then use HNO3Supernatant is adjusted to acidity, stands；Finally adjusting pH value to 8.5 (pH value is within the scope of 8-9), centrifugal treating with ammonia, leave and take precipitation, this is precipitated as Be (OH)2Precipitation.
5, Be (OH) is dissolved with 1ml0.2MHCl2Precipitation, it is thus achieved that solution, this solution is designated as sample solution C.
6, adding 0.5ml1MCsF in sample solution C, mixing moves liquid, and rinses with 1ml0.2MHCl, it is thus achieved that solution, this solution is designated as sample solution D.
7, in sample solution D, 0.25ml0.2MBaCl is added2, then dry under 80 DEG C of conditions, it is thus achieved that BaBeF4Target sample.
In the method for the invention, BaBeF is used4Target sample produces BeF3 -, instead of traditional BeO target sample, effectively prevent BeO and there is, as airborne dust, the risk that experimenter is brought by significantly high toxicity.
Two, BeF is produced3 -Line
1, to the BaBeF prepared4Target sample is mixed into PbF2Powder, BaBeF4Target sample and PbF2Powder mixes (volume ratio is within the scope of 1:2-1:5), PbF according to the ratio of volume ratio 1:32Powder itself is a kind of good ion conductor (do not possess electric conductivity during normality, but it has good electric conductivity under ionic state), meanwhile, and PbF2F ion entrained by powder can fully provide BeF3 -Produce required excessive F ion.
Traditional BeO target sample, in filling process, is mixed into the Cu powder (or the better metal dust of other electric conductivity) of 300 orders as assist medium according to volume ratio 1:3, to realize the electric conductivity of target cone.
2、BaBeF4Target sample and PbF2Being filled into AMS measurement target cone after powder mixing, target cone, as the carrying container of target sample, also serves as extraction negative electrode simultaneously and exists.
3, in an ion source with the Cs of 6keV energy+Ion constant bombardment BaBeF4Target sample and PbF2Powder hybrid target is bored so that PbF2The characteristic of ion conductor emerges from, now with PbF2For the sputtering target of assist medium produces BeF3 -Line, the super halogen anion BeF of beryllium3 -Electron binding energy is relatively big, relatively other anionic stabilization (selection of fluorine is its electron affinity is the strongest in adjacent elements, and its quality is minimum in halogen and without other isotopes or isobar).
Due to10The isobar of Be10B will be converted into by big portion10BF4 -, can be converted into only a little10BF3 -, therefore, slight excess of F ion is particularly important.
Three,10Be2+With9Be2+Tandem accelerator accelerates
1, the BeF with 35keV energy is drawn by ion source3 -Line, then BeF3 -Line does the screening of first energy by 54 ° of electrostatic analyzers of mental retardation end, and next entering radius is 400mm, 90 ° of jump Magnet, and 90 ° of jump Magnet select as momentum and ensure BeF3 -In9BeF3 -With10BeF3 -All can pass through along main beam line, therefore by energy " jump " value of this Magnet by former BeO-The 0V ,-1346V of method is set as 0V ,-522V, and quality of beam is by simple lens and guiding regulating guarantee during this period.
2, by BeF3 -Line is injected tandem accelerator by mental retardation end, and in this tandem accelerator, strip gas is by BeF3 -Molecular ion smashes, and stripping nucleic electronics makes final positively charged of Be ion, is able to secondary and accelerates.
3, for making BeF3 -Molecular ion is crashed to pieces and peels off to Be2+, when keeping final identical energy, Ar strip gas amount is reduced to former BeO-The 40% of method is (namely by original 8.3 × 10-3Mbar is reduced to 3.4 × 10-3Mbar), terminal voltage is adjusted to 2778kV by original 2500kV simultaneously, now,10Be2+Being accelerated to energy is 5.97MeV,9Be2+Being accelerated to energy is 5.94MeV (former BeO-Method10Be2+Energy be 5.97MeV,9Be2+Energy be 5.91MeV).
Four, high-energy tail10Be2+With9Be2+Separate
10Be2+With9Be2+At high-energy tail through 115 ° of main analysis magnets, after 115 ° of main analysis magnets9Be2+Enter removable Faraday cup measurement, and10Be2+Pass through along main beam line.
Five,10Be2+Enter gas detector
Former BeO-In method go out 115 ° of main analysis magnets be followed by secondary peel off SiN film not in use by, but10Be2+Either directly through 65 ° of main electrostatic analyzers and second block of 30 ° of Magnet of high-energy tail after passing through along main beam line, eventually enter into gas detector and be analyzed.
Due to secondary peel off SiN film not in use by so that10Be2+Not only ensure that 100% at the transmission stream of high-energy tail, and the quality of line have also been obtained guarantee.Former two groups of quadrupole lenss only need one group of work just can keep good quality of beam.
10Be2+After entering gas detector, originally BeO-Method can will reduce by 10 after the suppression of B by SiN film and in conjunction with after 65 ° of main electrostatic analyzers and second block of 30 ° of Magnet of high-energy tail6Times, and the method for the present invention will reduce by 10 after the suppression of B4Times, although do not have the magnitude that former method reduces many, but have already decreased to the analyzable magnitude of detector, enough10Be measures.
Fig. 2 and Fig. 3 respectively illustrates the energy spectrogram of the background sample first piece of positive plate at detector and second piece of positive plate.
As seen from Figure 2:10Be and10The power spectrum interval of B is completely separable,10Be can there is no other interference in road.
As seen from Figure 3:10Be and10The power spectrum interval of B is completely separable, and10The interference of other fragments is had in Be power spectrum interval.
Owing to final measurement is based on first piece of positive plate and second piece of positive plate coincidence measurement, the ion of the interval condition namely simultaneously meeting two pole plates can be considered as just effective10Be event, therefore, the method for the present invention can carry out completely10Be-AMS measures.
In sum, the method for the present invention is with the super halogen anion BeF of beryllium3 -As10The educt beaming flow that Be-AMS measures (instead of traditional BeO-Mode as educt beaming flow), measurement make use of the super halogen anion BeF of beryllium3 -Superior performance, namely effectively inhibited in the extraction stage10The interference of B so that drop, without re-using, the traditional method that energy film secondary is peeled off at small-sized AMS (< 3MV) high-energy tail, cause10The efficiency of transmission of Be line is guaranteed, and can reach 100% transmission (originally BeO at high-energy tail-Mode high-energy tail transfer rate about 30% as educt beaming flow), and will not be changed without quality of beam after film, maintain original good quality of beam.
It should be noted that above-described embodiment does not limit the present invention in any form, all employings are equal to the technical scheme that the mode of replacement or equivalent transformation obtains, and all fall within protection scope of the present invention.
Claims (5)
1. the method that the super halogen anion utilizing beryllium is accelerated device mass-spectrometer measurement, it is characterised in that comprise the following steps:
(1) preparation can the super halogen anion BeF of output3 -Target sample；
(2) in the target sample prepared, it is mixed into PbF2Powder, is then filled into AMS measurement target cone, uses Cs in an ion source+Described in ion constant bombardment, target cone produces BeF3 -Line；
(3) BeF is drawn by ion source3 -Line, then BeF3 -Line does the screening of first energy by 54 ° of electrostatic analyzers of mental retardation end, next enters 90 ° of jump Magnet, then by BeF3 -Line by mental retardation end inject tandem accelerator, in described tandem accelerator strip gas molecular ion is smashed,10Be2+Being accelerated to energy is 5.97MeV,9Be2+Being accelerated to energy is 5.94MeV；
(4)10Be2+With9Be2+At high-energy tail by 115 ° of main analysis magnets, then9Be2+Enter removable Faraday cup measurement,10Be2+Pass through along main beam line；
(5)10Be2+Either directly through 65 ° of main electrostatic analyzers and second block of 30 ° of Magnet of high-energy tail after passing through along main beam line, eventually enter into gas detector and be analyzed.
2. the method that the super halogen anion utilizing beryllium according to claim 1 is accelerated device mass-spectrometer measurement, it is characterised in that in step (), described target sample is the salt containing Be and F.
3. the method that the super halogen anion utilizing beryllium according to claim 2 is accelerated device mass-spectrometer measurement, it is characterised in that in step (), described target sample is BaBeF4。
4. the method that the super halogen anion utilizing beryllium according to claim 3 is accelerated device mass-spectrometer measurement, it is characterised in that in step (two), BaBeF4Target sample and PbF2Powder mixes according to the ratio of volume ratio 1:2-1:5.
5. the method that the super halogen anion utilizing beryllium according to claim 1 is accelerated device mass-spectrometer measurement, it is characterised in that in step (three), the energy jitter value of described jump Magnet is 0V ,-522V.
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| CN106501291B (en) * | 2016-10-18 | 2019-03-19 | 中国科学院地球环境研究所 | It is a kind of to use AMS on-line measurement under same target sample7Be with10The method of Be abundance |
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