CN109839302A - The minimizing technology of Bi-210 in a kind of pedotheque Sr-90 analysis - Google Patents
The minimizing technology of Bi-210 in a kind of pedotheque Sr-90 analysis Download PDFInfo
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- CN109839302A CN109839302A CN201711214595.0A CN201711214595A CN109839302A CN 109839302 A CN109839302 A CN 109839302A CN 201711214595 A CN201711214595 A CN 201711214595A CN 109839302 A CN109839302 A CN 109839302A
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- minimizing technology
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- bismuth
- exchange resin
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Abstract
The invention belongs to radiation environmental monitoring technical fields, are related to a kind of pedotheque90In Sr analysis210The minimizing technology of Bi.The minimizing technology in turn includes the following steps: (1) pedotheque of acquisition being carried out Radionuclide analysis according to the operating procedure of EJ/T 1035-2011, until desorbing yttrium with strippant；(2) bismuth carrier solution is added into stripping liquid, makes stripping liquid with natural flow velocity by anion-exchange resin column, after mixing evenly to realize the quick removal of bismuth；(3) anion-exchange resin column is washed with a small amount of desorption liquid stream, the yttrium remained on anion-exchange resin column is all rinsed.Utilize pedotheque of the invention90In Sr analysis210The minimizing technology of Bi can optimize existing pedotheque90Bismuth means are removed in Sr analytical standard method, to reach more preferable, more stable except bismuth effect, to make90It is more accurate and reliable that Sr analyzes result.
Description
Technical field
The invention belongs to radiation environmental monitoring technical fields, are related to a kind of pedotheque90In Sr analysis210The removal side of Bi
Method.
Background technique
90Sr is one of main human nuclide, belongs to long lived nuclides (physical half time 28.1a).90Sr mainly leads to
It crosses and eats or inhalation route enters human body.Due to strontium and calcium category congeners, chemistry, biochemical property are similar, thus strontium can and
Calcium accumulates on bone and tooth together.90Sr decay generates daughter90Y,90Y emit high energy β ray (2.28Mev), to the mankind with
Come carcinogenic risk, especially osteocarcinoma and leukaemia.And90Sr has as important fission products in nuclear emergency
A large amount of source item release, after some time it is possible to reach PBq magnitude.Therefore, it is paid close attention to during Chernobyl and Fukushima nuclear accident
Both nucleic.
It is domestic to be directed to different medium at present90Sr analysis has corresponding national standard or a professional standard, including water, soil,
Biology and food etc.90The standard of Sr analysis.Only soil media requires operate except bismuth existing analytical standard, but in routine analysis
Find also there is the presence of bismuth -210 in other media (such as aerosol sample), thereby increases and it is possible to which contents level is higher in work.Cause
This, it is proposed that increase the removal operation of bismuth during other medium analysis.
Except the existing standard method of bismuth is the bismuth sulfide precipitation method, but there are many drawbacks for this method, such as: bismuth sulfide precipitating is originally
Body is unstable, is also gradually decomposing while being formed, and influences to remove bismuth effect；Sodium sulfide reagent used is hygroscopic, is unfavorable for growing
Phase saves, and influences the accuracy of institute's formulating vulcanization sodium solution content, is easy to cause vulcanized sodium when except bismuth excessive, except sample is molten after bismuth
There is simple substance Sulfur releasing in liquid, influences upper prop effect.
In order to preferably monitor nuclear facilities operation conditions, environment and personnel health are protected, it is necessary to optimize existing soil-like
Product90Bismuth means are removed in Sr analytical standard method, to reach more preferable, more stable except bismuth effect, to make90Sr analyzes result
It is more accurate and reliable.
Summary of the invention
The object of the present invention is to provide a kind of pedotheques90In Sr analysis210The minimizing technology of Bi, it is existing can optimize
Pedotheque90Bismuth means are removed in Sr analytical standard method, to reach more preferable, more stable except bismuth effect, to make90Sr points
It is more accurate and reliable to analyse result.
In order to achieve this, the present invention provides a kind of pedotheque in the embodiment on basis90In Sr analysis210Bi's
Minimizing technology, the minimizing technology in turn include the following steps:
(1) pedotheque of acquisition is subjected to Radionuclide analysis according to the operating procedure of EJ/T 1035-2011, until with desorption
Agent desorbs yttrium；
(2) in order to realize the quantitative exchange adsorption of bismuth, bismuth carrier solution is added into stripping liquid, makes to desorb after mixing evenly
Liquid passes through anion-exchange resin column with natural flow velocity, to realize the quick removal of bismuth；
(3) anion-exchange resin column is washed with a small amount of desorption liquid stream, the yttrium remained on anion-exchange resin column is complete
Portion is rinsed.
In a preferred embodiment, the present invention provides a kind of pedotheque90In Sr analysis210The minimizing technology of Bi,
Wherein in step (1), the strippant is 6mol/L nitric acid solution.
In a preferred embodiment, the present invention provides a kind of pedotheque90In Sr analysis210The minimizing technology of Bi,
Wherein in step (2), the bismuth carrier solution is bismuth nitrate solution.
In a preferred embodiment, the present invention provides a kind of pedotheque90In Sr analysis210The minimizing technology of Bi,
Wherein in step (2), the concentration of the bismuth carrier solution is 10-20mg/mL, additional amount 0.5-1.0mL.
In a preferred embodiment, the present invention provides a kind of pedotheque90In Sr analysis210The minimizing technology of Bi,
Wherein in step (2), the anion-exchange resin column is domestic 201 × 7 or domestic 201 × 8 anion-exchange resin columns.
In a preferred embodiment, the present invention provides a kind of pedotheque90In Sr analysis210The minimizing technology of Bi,
Wherein in step (2), the mean particle size of the anion exchange resin is 80-120 mesh.
In a preferred embodiment, the present invention provides a kind of pedotheque90In Sr analysis210The minimizing technology of Bi,
Wherein in step (2), the size of the anion-exchange resin column is not less than Φ 10mm × 100mm.
In a preferred embodiment, the present invention provides a kind of pedotheque90In Sr analysis210The minimizing technology of Bi,
Wherein in step (3), the volume that desorption liquid stream washes anion-exchange resin column is 8-15ml.
In a preferred embodiment, the present invention provides a kind of pedotheque90In Sr analysis210The minimizing technology of Bi,
Wherein the minimizing technology further includes following steps: after the operation of step (3), washing anion exchange using sodium carbonate liquor stream
Resin column realizes regeneration.
The beneficial effects of the present invention are utilize pedotheque of the invention90In Sr analysis210The minimizing technology of Bi, can
Optimize existing pedotheque90Bismuth means are removed in Sr analytical standard method, to reach more preferable, more stable except bismuth effect, thus
Make90It is more accurate and reliable that Sr analyzes result.
Minimizing technology of the invention can achieve more preferable, more stable except bismuth effect, make pedotheque90Sr analyzes result more
Add accurate and reliable.Minimizing technology of the invention is verified by mark-on pedotheque and IAEA international comparison sample, as a result
Show that minimizing technology of the invention can be applied in surroundings monitoring pedotheque90The analysis of Sr is eliminated bismuth and is tied to analysis
The influence of fruit.
Detailed description of the invention
Fig. 1 is illustrative pedotheque of the invention90In Sr analysis210The minimizing technology of Bi flow chart (including90Sr
Analytical procedure).
Specific embodiment
Illustrative pedotheque of the invention90In Sr analysis210The process of the minimizing technology of Bi as shown in Figure 1 (including90Sr analytical procedure), it in turn includes the following steps:
(1) soil is acquired, sample is obtained；
(2) strontium yttrium carrier is added into pedotheque, and (strontium carrier is the strontium nitrate solution of 50mg Sr/mL；Yttrium carrier is
The yttrium nitrate solution of 20mg Y/mL), Acid leaching liquid is prepared into after pre-treatment；
(3) oxalic acid is added into leaching liquid, and (addition is oxalic acid solid, and oxalic acid additional amount and pedotheque analyze dosage
Ratio is big for 1:1 or more；If desired a small amount of CaCl can be added2), pH value of solution=3-4 is adjusted with ammonium hydroxide, is sufficiently stirred and generates grass
Hydrochlorate precipitating, centrifugation discard supernatant liquid；
(4) it by oxalate precipitation drying and calcination, is dissolved after cooling with nitric acid and adjusts lysate pH=1.0；
(5) lysate is passed through into extraction chromatography resin column (P204 extration resin) with certain flow rate, after realizing nucleic separation
With 6mol/L HNO3Solution desorbs yttrium；
(6) bismuth carrier solution (10mg/mL, additional amount 1.0mL) is accurately added into 50mL stripping liquid, after mixing evenly
Make stripping liquid with natural flow velocity (4-5mL/min) by domestic 201 × 7 anion-exchange resin column (having a size of Φ 10mm ×
100mm, mean particle size 80-120 mesh), realize the quick removal of bismuth；
(7) 10ml 6mol/L HNO is used3Solution stream washes anion-exchange resin column, will remain in anion exchange resin
Yttrium on column all rinses, and the efflux of this step is merged with the efflux of step (3)；
(8) anion-exchange resin column is washed using sodium carbonate liquor (4mol/L, 100mL) stream realize regeneration；
(9) source processed and measurement are carried out according to the requirement of EJ/T 1035-2011, be calculated in sample90The activity of Sr is dense
Degree.
Minimizing technology of the invention is in pedotheque90In Sr standard analysis process, uses domestic 201 × 7 anion instead and hand over
Resin is changed to carry out except bismuth.The experimental results showed that the resin has bismuth good, quantitative exchange adsorption effect, simultaneously for
Strontium and yttrium are substantially without exchange adsorption.Therefore, minimizing technology of the invention can be applied to pedotheque90The conventional analysis of Sr is examined
Survey work.
Below to the pedotheque of the invention of above-mentioned example90In Sr analysis210It is detailed that the minimizing technology of Bi makes citing
Explanation.
Embodiment 1: domestic anion exchange resin pair210The selective absorption of Bi removes verification test
1, exchange adsorption of the domestic anion exchange resin to bismuth
50ml 6mol/L HNO is separately added into 4 beakers3Solution, each accurate addition 1.00ml bismuth carrier solution
(10.15mg Bi/mL) makes it pass through anion-exchange resin column, anion-exchange resin column with natural flow velocity after mixing evenly
Under it is each place 1 be equipped with sodium sulfide solution beaker, observe beaker in whether have bismuth sulfide precipitating generate.Experiment discovery, beaker
In do not there is macroscopic precipitating to generate, show that anion-exchange resin column has good exchange adsorption effect to bismuth.Yin from
After sub-exchange resin is finished, regenerated using sodium carbonate liquor.
2, exchange adsorption of the domestic anion exchange resin to strontium
50ml 6mol/L HNO is separately added into 4 beakers3Solution, each accurate addition 1.00ml strontium carrier solution
(50.95mg Sr/mL) makes it, by anion-exchange resin column, be collected efflux with natural flow velocity and make carbonic acid after mixing evenly
Strontium precipitating and the chemical recovery rate that strontium is calculated with gravimetric method.The experimental results showed that the chemical recovery rate of strontium reach (98.5 ±
0.7) % shows that the domestic anion exchange resin does not adsorb strontium substantially.Experimental result is listed in table 1.
3, exchange adsorption of the domestic anion exchange resin to yttrium
50ml6mol/L HNO is separately added into 4 beakers3Solution, each accurate addition 2.00ml yttrium carrier solution
(19.45mg Y/mL) makes it, by anion-exchange resin column, be collected efflux with natural flow velocity and make oxalic acid after mixing evenly
Yttrium precipitating and the chemical recovery rate that yttrium is calculated with gravimetric method.The experimental results showed that the chemical recovery rate of yttrium reach (98.6 ±
0.8) % shows that the domestic anion exchange resin does not adsorb yttrium substantially.Experimental result is listed in table 1.
Exchange adsorption experimental result of the domestic anion exchange resin of table 1 to strontium and yttrium
When removing bismuth using domestic 201 × 7 anion exchange resin, solution system is 6mol/L HNO for above-mentioned test3
Solution, it is identical as the EJ/T 1035-2011 standard method desorption solution system of yttrium is used, that is, do not have to conversion solution body when removing bismuth
System.Stripping liquid can realize the quick removal of bismuth all by anion exchange resin in 10min.
Embodiment 2: the feasibility and superiority verification test of bismuth minimizing technology of the invention
1, mark-on sample analysis is verified
Method validation is carried out using the mark-on pedotheque that primary comparison activity is retained, sample has been subjected to uniformity testing,
Its radioactivity theoretical value is 30.3Bq/kg (having corrected to the measurement date).
The bismuth sulfide precipitation method (method that EJ/T1035-2011 is used) and domestic 201 × 7 anion exchange tree is respectively adopted
Rouge method (as previously described) is carried out except bismuth, remaining operation is carried out according to operation identical with EJ/T1035-2011 standard method.Two sides
Method weighs 4 samples in parallel, and bismuth sulfide precipitation method sample number into spectrum is respectively YZTR-1, YZTR-2, YZTR-3 and YZTR-4；State
Producing 201 × 7 anion-exchange resin method sample number into spectrum is respectively YZTR-5, YZTR-6, YZTR-7 and YZTR-8.Two methods
's90Sr, which analyzes result and compares, is listed in following table 2.
2 two kinds of method of bismuth removal of table90Sr analyzes result and compares
Infuse *: appended behind average value is standard deviation (± 1 σ)
From above-mentioned 2 result of table it can be seen that the analysis result of the bismuth sulfide precipitation method is between 32.2-35.7Bq/kg, put down
Mean value is 33.6 ± 1.6Bq/kg, and the relative standard deviation of average value is 4.77%；Domestic 201 × 7 anion of the invention is handed over
The analysis result of resin method is changed between 29.4-32.1Bq/kg, average value be 30.9 ± 1.3Bq/kg, average value it is opposite
Standard deviation is 4.21%.Thus the accuracy and precision for illustrating bismuth minimizing technology of the invention are significantly better than that existing mark
Quasi- method of bismuth removal, i.e. the bismuth sulfide precipitation method.
2, IAEA international comparison sample analysis is verified
Utilize 2015 and IAEA international comparison sample (respectively ALMERA Proficiency Test in 2016
IAEA-TEL-2015-04 and ALMERA Proficiency Test IAEA-TEL-2016-04) to method of bismuth removal of the invention
(anion-exchange resin method) has carried out the verifying of project as shown in table 3 below, in strict accordance with of the invention when analyses and comparison sample
Method of bismuth removal, comparison result are specifically listed in table 4.
Table 3 participates in IAEA international comparison Project Information Table
Table 4 is using IAEA international comparison sample to the verification result of method of bismuth removal of the present invention
From the results shown in Table 4, method of bismuth removal analysis result of the invention is good, is indicated above of the invention except bismuth
Method has good application effect, can be applied to pedotheque90In Sr routine monitoring work.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind 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.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 of the invention
Main idea or substantive characteristics.Therefore, the embodiment of description is regarded as illustrative and non-limiting in any way.This
The range of invention should be illustrated that any variation equivalent with the intention and range of claim also should include by appended claims
Within the scope of the invention.
Claims (9)
1. a kind of pedotheque90In Sr analysis210The minimizing technology of Bi, which is characterized in that the minimizing technology successively includes such as
Lower step:
(1) pedotheque of acquisition is subjected to Radionuclide analysis according to the operating procedure of EJ/T 1035-2011, until will with strippant
Yttrium desorbs；
(2) bismuth carrier solution is added into stripping liquid, stripping liquid is made to pass through anion exchange tree with natural flow velocity after mixing evenly
Rouge column, to realize the quick removal of bismuth；
(3) anion-exchange resin column is washed with a small amount of desorption liquid stream, the yttrium remained on anion-exchange resin column is all rushed
It washes.
2. minimizing technology according to claim 1, it is characterised in that: in step (1), the strippant is 6mol/L nitre
Acid solution.
3. minimizing technology according to claim 1, it is characterised in that: in step (2), the bismuth carrier solution is nitric acid
Bismuth solution.
4. minimizing technology according to claim 1, it is characterised in that: in step (2), the concentration of the bismuth carrier solution
For 10-20mg/mL, additional amount 0.5-1.0mL.
5. minimizing technology according to claim 1, it is characterised in that: in step (2), the anion-exchange resin column
For domestic 201 × 7 or domestic 201 × 8 anion-exchange resin columns.
6. minimizing technology according to claim 1, it is characterised in that: in step (2), the anion exchange resin
Mean particle size is 80-120 mesh.
7. minimizing technology according to claim 1, it is characterised in that: in step (2), the anion-exchange resin column
Size be not less than Φ 10mm × 100mm.
8. minimizing technology according to claim 1, it is characterised in that: in step (3), desorption liquid stream washes anion exchange tree
The volume of rouge column is 8-15ml.
9. minimizing technology according to claim 1, which is characterized in that the minimizing technology further includes following steps: step
Suddenly after the operation of (3), anion-exchange resin column is washed using sodium carbonate liquor stream and realizes regeneration.
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| CN201711214595.0A CN109839302A (en) | 2017-11-28 | 2017-11-28 | The minimizing technology of Bi-210 in a kind of pedotheque Sr-90 analysis |
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| CN201711214595.0A CN109839302A (en) | 2017-11-28 | 2017-11-28 | The minimizing technology of Bi-210 in a kind of pedotheque Sr-90 analysis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111551978A (en) * | 2020-05-08 | 2020-08-18 | 中国辐射防护研究院 | Method for evaluating uncertainty of radioactive soil sample sampling process |
| CN113359177A (en) * | 2021-04-08 | 2021-09-07 | 中国辐射防护研究院 | Combined analysis method for content of Pu, Am and Sr-90 in large-mass solid environment |
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| CN111551978A (en) * | 2020-05-08 | 2020-08-18 | 中国辐射防护研究院 | Method for evaluating uncertainty of radioactive soil sample sampling process |
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| CN113359177A (en) * | 2021-04-08 | 2021-09-07 | 中国辐射防护研究院 | Combined analysis method for content of Pu, Am and Sr-90 in large-mass solid environment |
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