CN108267773A - A kind of microdeposit method prepares the method that the α of polonium measures source - Google Patents
A kind of microdeposit method prepares the method that the α of polonium measures source Download PDFInfo
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- CN108267773A CN108267773A CN201710001444.0A CN201710001444A CN108267773A CN 108267773 A CN108267773 A CN 108267773A CN 201710001444 A CN201710001444 A CN 201710001444A CN 108267773 A CN108267773 A CN 108267773A
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- G—PHYSICS
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- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
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Abstract
The invention belongs to radioactive substance field of measuring technique, are related to a kind of microdeposit method and prepare the method that the α of polonium measures source.The method includes the following steps：(1) Te (VI) or Te (IV), sample containing polonium, radioactive tracer are added in aqueous solution209Po, reducing substances and miscible with water, and TeO can be reduced2Or the organic solvent of the solubility of simple substance Te, so as to make Te (VI) or Te (IV) and reducing substances that redox reaction occur, under the action of organic solvent, the TeO that obtains reduction2Or radioactivity polonium as carrier is carried and evenly spread in the aqueous solution by simple substance Te；(2) carrier of carrier band radioactivity polonium is made to be uniformly dispersed on filter membrane by filtering.The α that polonium is prepared by the method for the present invention measures source, auto-deposition method that can be more traditional prepares the α of polonium, and to measure the source used time short, it is easy to operate, it is easy to mass, it is at low cost, acid resistance and antijamming capability are stronger, and can obtain and be close with area method of drowning oneself or the higher polonium rate of recovery (85% 100%).
Description
Technical field
The invention belongs to radioactive substance field of measuring technique, are related to the side that a kind of microdeposit method prepares the α measurements source of polonium
Method.
Background technology
210Po is a kind of natural radionuclide, belong to natural radioactive series uranium series (238U)。210Po belongs to extremely toxic group of radioactivity
Nucleic only needs 1 microgram to be just enough fatal to a normal adult human, and toxicity is approximately 250000 times of hydrogen cyanide (HCN).210Po
It is volatile, it is widely present in the surrounding mediums such as soil, rock, water body, biology, it can be by eating and sucking into human body.By
In its toxicologic properties, it is therefore necessary to how to measure soil, deposit, aerosol, water, food, tobacco leaf, cigarette, urine
In liquid and biomaterial and geological sample210Po contents are studied.
Analysis polonium method mainly have the precipitation method, extraction, the way of distillation, chromatograph extraction, microdeposit method, electrodeposition process and
It drowns oneself area method.Measuring instrument uses α/β proportional counter and alpha spectrometer more.For the Po- α sources that alpha spectrometer measures generally by general
Polonium auto-deposition is on metal disk or sulfide microdeposit polonium is made, wherein the preparation principle of polonium auto-deposition it is following (referring to
Khater,A.E.M.J.Environ.Radioact.2004,71,33-41；Matthews,K.M.；Kim,C.K.；Martin,
P.Appl.Radiat.Isot.2007,65,267-279；Kelecom,A.；Gouvea,
R.C.S.J.Environ.Radioact.2011,102,443-447；Karali,T.；S.；
G.Yener.Appl.Radiat.Isot.1996,47,409-411；Eichrom Thecnologies,LLC.,Analytical
procedures,Lead-210and Polonium-210in Water,2009)。
Silver strip is often used as the plating piece of auto-deposition polonium, and nickel sheet, copper sheet, and stainless steel substrates are since cost is relatively low, also often
It is used as the plating piece of auto-deposition polonium.Metal disk as plating piece is polished and is cleaned with by dust before the use
It is removed with surface oxide layer.Then dilute HCl that these plating pieces are placed on small size (is usually by (such as 80-95 DEG C) at high temperature
0.1M to 1M) in spontaneous carry out electrochemical reducting reaction 3-6 hours to obtain high-recovery (being usually 90%).Then spend from
Sub- water washing plates piece and (being usually 300 DEG C) heating a few minutes aoxidize polonium to reduce pollution α at relatively high temperature
The risk of probe.
Although this sample preparation technology is widely used, entire sample preparation procedure, especially heating step
It suddenly, can be inconvenient and time-consuming more.
The problem of sulfide microdeposit polonium is another common method for preparing Po- α sources, this method be：Sulfide sinks
Shallow lake is also easy to produce the H with rotten egg smell in acid condition2S gases, and sulfide microdeposit method is typically low dense
It spends in HCl (being usually 0.1M to 1M) and is made, this α sources can also make probe by certain pollution.
Invention content
A kind of method that the α measurements source of polonium is prepared the object of the present invention is to provide microdeposit method, more traditional auto-deposition
The method used time is shorter, operation it is simpler, easy mass, cost is lower, and acid resistance and antijamming capability are stronger, and the rate of recovery approaches or
Higher.
In order to achieve this, in the embodiment on basis, the present invention provides the α that a kind of microdeposit method prepares polonium and measures source
Method, include the following steps：
(1) Te (VI) or Te (IV), sample containing polonium, radioactive tracer are added in aqueous solution209Po, reducing substances
And it is miscible with water, and TeO can be reduced2Or the organic solvent of the solubility of simple substance Te, so as to make the Te (VI) or Te
(IV) redox reaction occurs with the reducing substances, under the action of the organic solvent, makes what reduction obtained
TeO2Or radioactivity polonium as carrier is carried and evenly spread in the aqueous solution by simple substance Te；
(2) carrier of carrier band radioactivity polonium is made to be uniformly dispersed on filter membrane by filtering.
The principle of above-mentioned steps (1) is redox reaction.Wherein, oxidant is included with four valence states or hexavalent state Te
Compound, reducing agent include the substance with strong reducing property, such as SnCl2, TiCl3Deng.
Tellurium reduction microdeposit polonium is prepared in the method in α spectrometrys source, and oxidation state Te (IV) and Te (VI) can be reduced agent also
Originally it was Te simple substance or TeO2, these substances restored can carry polonium as carrier.It can be incited somebody to action comprising all in method
Oxidation state tellurium is reduced to the redox reaction of carrier.
Tellurium reduction microdeposit polonium is prepared in the method in α spectrometrys source, and the medium of redox reaction is aqueous solution, preferably
The aqueous solution of hydrochloric acid as non-oxidizing acid, but it is other do not influence tellurium reduction microdeposit polonium solution system (as acidification or
Not-acidified solution system) it is also suitable.It is worth noting that, HNO3Wait oxidizing acids that can influence the preparation process in α sources.
The effect of organic solvent is to make the carrier of generation to uniformly disperse in aqueous solution in above-mentioned steps (1), filters
Afterwards, carrier can be evenly distributed on filter membrane.The preferred isopropanol of the organic solvent, propylene glycol.
In a preferred embodiment, the present invention provides the method that the α that a kind of microdeposit method prepares polonium measures source,
Described in Te (VI) be H6TeO6Or its salt, the Te (IV) are H2TeO3Or its salt.
In a preferred embodiment, the present invention provides the method that the α that a kind of microdeposit method prepares polonium measures source,
Described in aqueous solution be the acidic aqueous solution formed by non-oxidizing acid.
In a preferred embodiment, the present invention provides the method that the α that a kind of microdeposit method prepares polonium measures source,
Described in non-oxidizing acid be hydrochloric acid.
In a preferred embodiment, the present invention provides the method that the α that a kind of microdeposit method prepares polonium measures source,
Described in non-oxidizing acid a concentration of 0.1-6mol/L.
In a preferred embodiment, the present invention provides the method that the α that a kind of microdeposit method prepares polonium measures source,
Described in organic solvent be isopropanol or propylene glycol.
In a preferred embodiment, the present invention provides the method that the α that a kind of microdeposit method prepares polonium measures source,
Described in reducing substances be SnCl2Or TiCl3。
In a preferred embodiment, the present invention provides the method that the α that a kind of microdeposit method prepares polonium measures source,
Reducing substances are excessive in middle step (1).
In a preferred embodiment, the present invention provides the method that the α that a kind of microdeposit method prepares polonium measures source,
The reaction time of middle step (1) is 10 minutes to 4 hours.
The α that polonium is prepared by the method for the present invention measures source, and the α that auto-deposition method that can be more traditional prepares polonium measures the source used time
Short, easy to operate, easy mass, at low cost, acid resistance and antijamming capability are stronger, and can obtain be close with area method of drowning oneself or
The higher polonium rate of recovery (85%-100%).In addition, suitable microdeposit may be selected for different samples in the method for the present invention
Condition is to achieve the purpose that quickly and effectively to measure polonium, and the detection of this polonium in various samples during nuclear emergency is coped with is with great
Meaning.
Description of the drawings
Fig. 1 is the affecting laws figure of the microdeposit rate of recovery in the α measurements source that acidity prepares the microdeposit method of the present invention polonium.
Fig. 2 is the influence of the microdeposit rate of recovery in the α measurements source that Te (IV) contents prepare the microdeposit method of the present invention polonium
Rule figure.
Fig. 3 is the microdeposit rate of recovery in the α measurements source for preparing polonium the redox reaction time to the microdeposit method of the present invention
Affecting laws figure.
Specific embodiment
The specific embodiment of the present invention is further illustrated with attached drawing with reference to embodiments.
Embodiment 1：Acidity prepares microdeposit method the influence of the microdeposit rate of recovery in the α measurements source of polonium
In 10mL hydrochloric acid solutions, add 25mBq successively209Po standard radioactive sources, 100 μ g Te (IV), 5mL isopropanols, mixing,
It is eventually adding 1mL 10%SnCl2Solution shakes up, and stands 10min, filters (0.1- μm of filter membrane), retains to obtain Po- α spectrometrys source,
Investigate influence of the hydrochloric acid of various concentration (acidity) to the microdeposit rate of recovery, the result is shown in Figure 1.The wherein calculating of the microdeposit rate of recovery
Formula is as follows：
Wherein：
The microdeposit rate of recovery of R-Po；
CR209Radioactive tracer in-sample209Decay rate (the secondary s of Po-1)；
I209Selected energy in-spectrogram209The abundance of Po；
A209It is added in-sample209The initial activity (Bq) of Po；
The detection efficient of ε-alpha spectrometer.
It will be seen from figure 1 that with the increase of concentration of hydrochloric acid, the microdeposit efficiency of the polonium wave between 80%-100%
It is dynamic.Experiment is repeated several times to find, when reaction system is 1mol/L HCl, the microdeposit rate of recovery of tellurium reduction microdeposit polonium can be with
Reach 98%, and react very stable.Therefore, peak optimization reaction acidity is 1mol/L HCl.In addition, pass through this research and subsequent implementation
The method that the research of example also found the present invention shows very strong relative to traditional auto-deposition and sulfide microdeposit method
Acid resistance.
Embodiment 2：Te (IV) contents prepare microdeposit method the influence of the microdeposit rate of recovery in the α measurements source of polonium
In 10mL 1M HCl, 25mBq is sequentially added209Po standard radioactive sources, Te (IV), 5mL isopropanols, mixing, finally
Add in 1mL 10%SnCl2Solution shakes up, and stands 10min, filters (0.1- μm of filter membrane), and retention prepares Po- α spectrometrys source, examines
Influence of different Te (IV) contents to the microdeposit rate of recovery is examined, as a result sees Fig. 2.
As seen from Figure 2, polonium effectively can be carried by Te (IV) contents in the range of 10-250 μ g,
And the spectra resolution rate of polonium is all fine.Final preferably 100 μ g Te (IV) are to ensure the microdeposit rate of recovery of polonium.
Embodiment 3：The redox reaction time prepares microdeposit method the influence of the microdeposit rate of recovery in the α measurements source of polonium
In 10mL 1M HCl, 25mBq is sequentially added209Po standard radioactive sources, 100 μ g Te (IV), 5mL isopropanols mix
It is even, it is eventually adding 1mL 10%SnCl2Solution shakes up, and stands a period of time, filters (0.1- μm of filter membrane), and retention prepares Po- α
Spectrometry source investigates influence of the different redox reaction times to the microdeposit rate of recovery, as a result sees Fig. 3.
As seen from Figure 3, after reaction time 10min, the microdeposit polonium microdeposit rate of recovery can reach 95%, and
In the reaction time of 4h, the microdeposit rate of recovery of tellurium reduction microdeposit polonium is adsorbed between 95%-98%, and interior for 24 hours
The precipitation capacity of tube wall is less, and the microdeposit rate of recovery of polonium still can reach more than 90%.The redox of final preferably 10min is anti-
Between seasonable.
Embodiment 4：Other radionuclide interference eliminations are tested
The radionuclides (such as Ra, Th, U, Pu and Am) of some alpha-decays and Po (208Po,209Po,210Po) in microdeposit
It can be carried on filter membrane together in the process, so as to influence the measurement of polonium.Ra and Th, U, Pu and Am are to the decontamination factor such as table of polonium
Shown in 1.
In each sample, it is separately added into 25mBq Ra-226, Am-243, U-232, Pu-242 standard radioactive sources, dense salt
Acid dissolving precipitation, adjusting solution acidity are 1mol/L, add in 100 μ g Te (IV) and 5ml isopropanols, shake up, be eventually adding 5ml
10%SnCl2, 10min is reacted, is filtered, Po- α sources is prepared, is measured with alpha spectrometer.By measurement result calculate Ra, Th, U, Pu and
As a result Am is shown in such as the following table 1 the decontamination factor of Po.
Table 1 influences the decontamination factor for the radionuclide that polonium measures
*Decontamination factor：Nuclide radiation quality activity and the ratio between interference nuclide radiation quality activity after decontamination are interfered before decontamination
As shown in Table 1, this method is 75 to the decontamination factor of Ra, to the decontamination factor of actinides>100, so in tellurium
During restoring microdeposit polonium, these interfering radionuclides will not have an impact the measurement of radioactivity polonium.
Embodiment 5：The microdeposit method of the present invention is in practical pedotheque210The measure of Po
The pedotheque from Shandong and Fujian is acquired, the soil collection sample of 0.5g is taken, is put into glass beaker, accurately
Add in 25mBq209Po tracers.Then 20mL 6M HCl are added in, are leached 2 times, each 40min in the case of heating stirring,
Cooled and filtered filtrate will merge twice.0.5mL 7%TiOCl are added in merging filtrate2, liquid pH value is adjusted with concentrated ammonia liquor
It is 8 or so, generates HTiO precipitations, supernatant is abandoned in centrifugation, adds 1mL concentrated hydrochloric acids dissolving precipitation, and ultra-pure water is diluted to 10mL, adds in
100 μ g Te (IV) and 5mL isopropanols, shake up.1mL 10%SnCl are added at this time2, shake up, stand 10min, filter, Po- α processed
Source is put on alpha spectrometer and measures.It is measured according to analysis, calculates and deduct in blank sample210In soil after Po contents210Po lives
Degree, is calculation formula and result (table 2) as follows.
The calculation formula of the rate of recovery of Po is as follows：
Wherein：
The rate of recovery of Po in R-sample；
CR209Radioactive tracer in-sample209Decay rate (the secondary s of Po-1)；
I209Selected energy in-spectrogram209The abundance of Po；
A209It is added in-sample209The initial activity (Bq) of Po；
The detection efficient of ε-alpha spectrometer.
In soil210The calculation formula of Po activity is as follows：
Wherein：
A210In-soil210Po activity (Bq)；
CR210- measure what is obtained210Decay rate (the secondary s of Po-1)；
I210Selected energy in-spectrogram210The abundance of Po；
The rate of recovery of Po in R-sample；
The detection efficient of ε-alpha spectrometer.
In 2 practical pedotheque of table210The measure of Po
Analysis of experimental data according to this, the whole rate of recovery is 85%~90%.
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, belong 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.Above-described embodiment or embodiment are only to the present invention
For example, the present invention can also be implemented with other ad hoc fashions or other particular form, without departing from the present invention's
Main idea or substantive characteristics.Therefore, it is regarded as from the point of view of the embodiment of description is in terms of any illustrative and non-limiting.This
The range of invention should be illustrated that any variation equivalent with the intention and range of claim should also be included by appended claims
Within the scope of the invention.
Claims (9)
1. a kind of microdeposit method prepares the method that the α of polonium measures source, which is characterized in that includes the following steps：
(1) Te (VI) or Te (IV), sample containing polonium, radioactive tracer are added in aqueous solution209Po, reducing substances and
It is miscible with water, and TeO can be reduced2Or the organic solvent of the solubility of simple substance Te, so as to make the Te (VI) or Te (IV)
Redox reaction occurs with the reducing substances, under the action of the organic solvent, the TeO that obtains reduction2
Or radioactivity polonium as carrier is carried and evenly spread in the aqueous solution by simple substance Te；
(2) carrier of carrier band radioactivity polonium is made to be uniformly dispersed on filter membrane by filtering.
2. according to the method described in claim 1, it is characterized in that：The Te (VI) is H6TeO6Or its salt, the Te
(IV) it is H2TeO3Or its salt.
3. according to the method described in claim 1, it is characterized in that：The aqueous solution is the acidity formed by non-oxidizing acid
Aqueous solution.
4. according to the method described in claim 3, it is characterized in that：The non-oxidizing acid is hydrochloric acid.
5. according to the method described in claim 3, it is characterized in that：A concentration of 0.1-6mol/L of the non-oxidizing acid.
6. according to the method described in claim 1, it is characterized in that：The organic solvent is isopropanol or propylene glycol.
7. according to the method described in claim 1, it is characterized in that：The reducing substances are SnCl2Or TiCl3。
8. according to the method described in claim 1, it is characterized in that：Reducing substances are excessive in step (1).
9. according to the method described in claim 1, it is characterized in that：The reaction time of step (1) is 10 minutes to 4 hours.
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| CN110438536A (en) * | 2019-07-30 | 2019-11-12 | 华东师范大学 | A kind of electro-deposition-auto-deposition prepares αsource experimental provision and its experimental method |
| CN110987741A (en) * | 2019-11-06 | 2020-04-10 | 中国辐射防护研究院 | Method for estimating content of secondary aerosol in atmosphere |
| CN110988962A (en) * | 2019-11-06 | 2020-04-10 | 中国辐射防护研究院 | Method for rapidly analyzing polonium-210 in aerosol |
| CN111142167A (en) * | 2019-11-06 | 2020-05-12 | 中国辐射防护研究院 | Method for detecting position of spontaneous combustion source of coal by using polonium-210 method |
| CN113406114A (en) * | 2021-04-28 | 2021-09-17 | 中国辐射防护研究院 | Combined analysis method for content of Pu, Am and U in aerosol |
| CN114127340A (en) * | 2019-06-19 | 2022-03-01 | 日本医事物理股份有限公司 | Method for producing 226Ra target, method for producing 225Ac, and electrodeposition liquid for producing 226Ra target |
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| CN114127340A (en) * | 2019-06-19 | 2022-03-01 | 日本医事物理股份有限公司 | Method for producing 226Ra target, method for producing 225Ac, and electrodeposition liquid for producing 226Ra target |
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| CN110987741A (en) * | 2019-11-06 | 2020-04-10 | 中国辐射防护研究院 | Method for estimating content of secondary aerosol in atmosphere |
| CN110988962A (en) * | 2019-11-06 | 2020-04-10 | 中国辐射防护研究院 | Method for rapidly analyzing polonium-210 in aerosol |
| CN111142167A (en) * | 2019-11-06 | 2020-05-12 | 中国辐射防护研究院 | Method for detecting position of spontaneous combustion source of coal by using polonium-210 method |
| CN110987741B (en) * | 2019-11-06 | 2022-05-17 | 中国辐射防护研究院 | Method for estimating content of secondary aerosol in atmosphere |
| CN113406114A (en) * | 2021-04-28 | 2021-09-17 | 中国辐射防护研究院 | Combined analysis method for content of Pu, Am and U in aerosol |
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