CN103901461A - Method for rapidly analyzing strontium-90 in liquid state efflux of nuclear power plant - Google Patents
Method for rapidly analyzing strontium-90 in liquid state efflux of nuclear power plant Download PDFInfo
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Abstract
The invention relates to a method for rapidly analyzing strontium-90 in liquid state efflux of a nuclear power plant. The method includes the following steps that (a) the liquid state efflux of the nuclear power plant is made to flow through a cation exchange color layer pillar under the acidic condition, a salpeter solution is used for leaching, and first eluant is obtained through collection; (b) the first eluant is made to flow through a P204 levextrel resin color layer pillar to be separated and purified, the salpeter solution is used for leaching, and second eluant is obtained through collection; (c) a scintillation solution is added and mixed and then is placed on a liquid scintillation spectrometer so that the counting rate of yttrium-90 can be measured; (d) an average value is acquired through repeated measurement, and the specific activity of yttrium-90 is calculated; (e) the specific activity of strontium-90 is calculated. On one hand, the liquid state efflux of the nuclear power plant is made to flow through the cation exchange color layer pillar under the acidic condition, so that radioactive substances in the liquid state efflux of the nuclear power plant are gathered; on the other hand, the first eluant is made to flow through the P204 levextrel resin color layer pillar to be separated and purified, hence, yttrium-90 can be separated from the first eluant, and strontium-89 and strontium-90 can be separated indirectly.
Description
Technical field
The invention belongs to the determination and analysis method of radioactive nuclide, relate to the rapid analysis of Strontium-90, be specifically related to the rapid analysis of Strontium-90 in a kind of nuclear power plant liquid effluent.
Background technology
Strontium-90 (
90sr) be the fission product of U-235 and Pu-239, be mainly derived from nuclear weapon blasts and nuclear reactor, in nuclear power plant's reactor, may enter reactor-loop due to fuel can defect or breakage, and along with Radioactive Liquid Effluent is to environmental emission.In the isotope of radiostrontium, Strontium-90 harm maximum, is because its physical half time (28.6) and biological half-life (49.3) are grown and can be deposited on enduringly in the skeletal system of hematopoiesis, causes Radiation sickness (for example leukaemia) thereby substituted calcium; Its daughter Yttrium-90 (simultaneously
90y) the high energy β ray producing can cause major injury to marrow.
After Chernobyl nuclear accident, radioactivity ecological study finds than other radioactive nuclide (as the isotope of caesium, being conventionally easy to be adsorbed by clay mineral), and radiostrontium has high animal migration in surrounding medium.State compulsory standard " regulation of protection of nuclear power plant environmental radiation " (GB 6249-2011) regulation: the specific activity that must analyze and measure continuously or termly Strontium-90 in nuclear power station and other power reactor effluents.By the specific activity of Strontium-90 in monitoring Radioactive Liquid Effluent, whether damaged to confirm that fuel can in nuclear power plant's reactor is in operation, and the radiation effect that can may cause the public for assessment of nuclear power plant radioactivity discharge.In prior art, generally adopt fuming nitric aicd method (GB 6764-86) or chromes (GB 6766-86), measure by proportional counter.These two kinds of analytical approachs all have the features such as analytical procedure is loaded down with trivial details, analysis time is long, but nuclear power plant's Radioactive Liquid Effluent has complicated components, radioactivity is high, to features such as human body radiation dosage are large, therefore in liquid effluent, the analysis of Strontium-90 should adopt the analysis process that analytical procedure is simple, analysis time is short, and existing Strontium-90 analytical approach does not possess above advantage.Therefore set up the rapid analysis of Strontium-90 in nuclear power plant's liquid effluent by reducing greatly the relevant man power and material of nuclear power plant, increase work efficiency.
The specific activity that current domestic employing liquid dodges spectrometer measurement Strontium-90 rarely has report, dodges spectrometer measure Strontium-90 for liquid, conventionally adopts sample and scintillation solution to be undertaken under the high energy pattern of C-14, measuring after proportioning by 10 mL:10 mL.Have in the world the express-analysis technology for analysis environments water body Strontium-90, be mainly strontium specific resin chromatography and strontium Solid-Phase Extraction diaphragm technology, these two kinds of technology are all by separation and purification Strontium-90, dodge spectrometer Strontium-90 is carried out to Quick Measurement by liquid.This is because the radiostrontium in environmental sample only has Strontium-90, although strontium-89 and Strontium-90 are all fission products, derive from nuclear test and nuclear accident, but the half life period of strontium-89 shorter (50.5 days), therefore the strontium-89 in environmental sample is easy to decay, so strontium specific resin chromatography and strontium Solid-Phase Extraction diaphragm technology are applicable to the analysis of Strontium-90 in environmental sample.But, main current core dynamics factory take presurized water reactor as heap type, the strontium-89 content of its liquid effluent discharge is all much larger than the content of Strontium-90, and above two kinds of technology cannot separate the isotope of strontium, two kinds of technology more than being therefore difficult to adopt in the time carrying out the fast monitored of Strontium-90 in nuclear power plant's liquid effluent.
Summary of the invention
The present invention seeks to provide in order to overcome the deficiencies in the prior art a kind of can be to the method that in nuclear power plant's liquid effluent, Strontium-90 carries out express-analysis.
For achieving the above object, the technical solution adopted in the present invention is: the rapid analysis of Strontium-90 in a kind of nuclear power plant liquid effluent, comprises rapid following steps:
(a) get a certain amount of nuclear power plant liquid effluent, and add wherein strontium carrier and yttrium carrier, the cation exchange of being flowed through under acid condition chromatograph post, uses the cation exchange chromatograph post described in salpeter solution drip washing subsequently, collects eluent and obtains the first eluent;
(b) by the first described eluent stream through P204 extration resin chromatograph column separating purification, with the P204 extration resin chromatograph post described in salpeter solution drip washing, collect eluent and obtain the second eluent;
(c) by after the second eluent evaporate to dryness with dissolving with hydrochloric acid and be transferred in low potash glass bottle, add scintillation solution to mix to be placed on liquid and dodge the counting rate of measuring Yttrium-90 on spectrometer, calculate the radiochemical recovery yield of Yttrium-90 according to described Yttrium-90 counting rate;
(d) get many parts of a certain amount of nuclear power plant liquid effluents, repeating step (a), to step (c), calculates the average radiochemical recovery yield of Yttrium-90 again, and calculates the specific activity of Yttrium-90 according to the average radiochemical recovery yield of Yttrium-90 counting rate and Yttrium-90;
(e), according to the Decay relation between Yttrium-90 and Strontium-90, calculate the specific activity of Strontium-90 according to the specific activity of described Yttrium-90.
Optimally, in step (a), described nuclear power plant liquid effluent under the condition of pH=0.1 ~ 5 with the flow velocity of 8 ~ 10 ml/min cation exchange chromatograph post of flowing through.
Optimally, in step (b), the flow velocity of described the first eluent is 2 ml/min.
Optimally, in step (a), described salpeter solution drip washing is carried out at twice, first uses the salpeter solution drip washing of 0.1 ~ 0.5mol/L, then uses the salpeter solution wash-out of 6 ~ 10mol/L.
Optimally, in step (b), described salpeter solution drip washing is carried out at twice, first uses the salpeter solution drip washing of 1 ~ 3mol/L, then uses the salpeter solution wash-out of 5 ~ 8mol/L.
Optimally, in step (a), described the first eluent regulates pH to 0.1 ~ 0.5 with ammoniacal liquor.
Optimally, in described step (c), add supplementary deionized water in the low potash glass bottle of scintillation solution forward direction that liquor capacity is wherein compared for 1:1 with scintillation solution volume.
Because technique scheme is used, the present invention compared with prior art has following advantages: the rapid analysis of Strontium-90 in nuclear power plant of the present invention liquid effluent, the cation exchange chromatograph post of under acid condition, nuclear power plant's liquid effluent being flowed through on the one hand, for the radioactive nuclide of enrichment nuclear power plant liquid effluent; On the other hand by the first eluent stream through P204 extration resin chromatograph column separating purification, thereby will
90y separates from the first eluent, has indirectly realized separating of strontium-89 and Strontium-90; And can within a working day, complete all radiochemical analysises, and greatly improve work efficiency, reduce the radiation effect of liquid effluent to staff.
Accompanying drawing explanation
Accompanying drawing 1 is the rapid analysis process flow diagram of Strontium-90 in nuclear power plant of the present invention liquid effluent;
The detection limit value that accompanying drawing 2 is measured under different volumes for liquid sudden strain of a muscle spectrometer Tricarb 3180.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiment of the invention is elaborated:
The rapid analysis of Strontium-90 in nuclear power plant's liquid effluent as shown in Figure 1, comprise rapid following steps: (a) get a certain amount of nuclear power plant liquid effluent, and add wherein strontium carrier and yttrium carrier, the cation exchange of being flowed through under acid condition chromatograph post, use subsequently the cation exchange chromatograph post described in salpeter solution drip washing, collect eluent and obtain the first eluent; (b) by the first described eluent stream through P204 extration resin chromatograph column separating purification, with the P204 extration resin chromatograph post described in salpeter solution drip washing, collect eluent and obtain the second eluent; (c) by after the second eluent evaporate to dryness with dissolving with hydrochloric acid and be transferred in low potash glass bottle, add scintillation solution to mix to be placed on liquid and dodge the counting rate of measuring Yttrium-90 on spectrometer, calculate the radiochemical recovery yield of Yttrium-90 according to described Yttrium-90 counting rate; (d) get many parts of a certain amount of nuclear power plant liquid effluents, repeating step (a), to step (c), calculates the average radiochemical recovery yield of Yttrium-90 again, and calculates the specific activity of Yttrium-90 according to the average radiochemical recovery yield of Yttrium-90 counting rate and Yttrium-90; (e), according to the Decay relation between Yttrium-90 and Strontium-90, calculate the specific activity of Strontium-90 according to the specific activity of described Yttrium-90.The cation exchange chromatograph post of under acid condition, nuclear power plant's liquid effluent being flowed through on the one hand, for the radiomaterial of enrichment nuclear power plant liquid effluent, on the other hand by the first eluent stream through P204 extration resin chromatograph column separating purification, thereby will
90y separates from the first eluent, has indirectly realized separating of strontium-89 and Strontium-90; And can within a working day, complete all radiochemical analysises, and greatly improve work efficiency, reduce the radiation effect of liquid effluent to staff.
The making of cation exchange chromatograph post: 8.5 g Zeo-karbs (100-200 order) are packed in the ion exchange column that internal diameter is 7.5 mm (1000 mL column volumes, φ 100 × 130, φ 15 × 200), use the front HNO with 20 mL 0.1mol/L
3solution equilibria exchange column;
The making of P204 extration resin chromatograph post: 4.0 g P204 extration resins are packed in the chromatograph post that internal diameter is 0.5 mm (φ 10 × 200), use the front HNO with 20 mL 0.3mol/L
3balance chromatograph post.
In the present embodiment, as shown in Figure 1, the rapid analysis of Strontium-90 in nuclear power plant's liquid effluent, concrete steps are as follows:
(a) get 1.0 L nuclear power plant liquid effluents, and add wherein strontium carrier and yttrium carrier, pass through cation exchange column with the flow velocity of 8 ~ 10 mL/min, follow the HNO with 25 mL 0.1M
3the HNO of drip washing exchange column, 50 mL 8M
3wash-out exchange column, regulates pH to 0.1 by ammoniacal liquor for the first eluent of collecting, like this can be efficiently, stably Strontium-90 in liquid effluent is effectively extracted and enrichment, and organic efficiency reaches more than 95%;
(b) pass through P204 extration resin chromatograph post with the flow velocity of 2 mL/min subsequently, with the HNO of 30 mL 1.5 M
3the HNO of drip washing chromatograph post, 40 mL 6M
3wash-out chromatograph post, collects to obtain the second eluent, like this can be efficiently, stably by liquid effluent
90y effectively extracts and enrichment, and organic efficiency reaches 80% left and right;
(c) by the second eluent on electric furnace after evaporate to dryness by 0.1M dissolving with hydrochloric acid precipitation, solution in beaker is proceeded in the low potash glass bottle of mark 10 mL positions, deionized water is mended mark, adds 10 mL GoldStar LT
2scintillation solution fully mixes and is placed on liquid and dodges the counting rate of measuring Yttrium-90 on spectrometer, calculates the radiochemical recovery yield of Yttrium-90 by formula (1);
（1）
In formula:
y: the radiochemical recovery yield of Yttrium-90, %;
n 0 : sample measurement counting rate, cpm;
n b : background counting rate, cpm;
n c : actual mark-on counting rate, dpm;
e: the detection efficiency of instrument to Yttrium-90 standard source, %;
The disintegration constant of λ: Y-90, equals 0.693/T, and T is herein
9064.2 hours half life period of Y;
(d) get again 17 part of 1.0 L nuclear power plant liquid effluent and 6 part of 2.0 L nuclear power plant liquid effluent, repeating step (a) is to step (c), after calculating respectively the radiochemical recovery yield of Yttrium-90, calculate the average radiochemical recovery yield of Yttrium-90, and calculate the specific radioactivity of Yttrium-90 by formula (2);
In formula:
a: the specific radioactivity of Yttrium-90 in sample, Bq/L;
n: sample net counting rate, cpm; (be numerically equal to
n 0 -
n b )
e: the detection efficiency of instrument to Yttrium-90 standard source, %;
y: the radiochemical recovery yield (%) of Yttrium-90, adopt repeatedly mark-on to test the average radiochemical recovery yield of the Yttrium-90 obtaining herein, measurement result is listed in table 1;
V: sample volume, L;
(e), according to the Decay relation between Yttrium-90 and Strontium-90, calculate the specific activity of Strontium-90 according to the specific activity of described Yttrium-90;
?
Because the half life period T of parent (Strontium-90)
1very long, and the half life period T of daughter (Yttrium-90)
2very short, as time long enough (t>=5T
2) time, the radioactivity of mother and sons' body has reached balance, and Strontium-90 activity now equals the activity of Yttrium-90.Because Strontium-90 produces to the balance of measuring the time used and can guarantee Strontium-90 and Yttrium-90 from reactor, therefore calculate the specific activity of gained Yttrium-90 and be the specific activity of Strontium-90.
As can be seen from Figure 1, this analytical approach only needs about 20 hours can complete analytical work altogether, has greatly improved work efficiency, has reduced the radiation effect of liquid effluent to staff.
Putting of table 1 mark-on liquid effluent sample recovery measurement result
Can be seen by putting of mark-on liquid effluent sample recovery measurement result, experiment has been carried out 24 groups altogether, the putting recovery that rapid analysis obtains is between 73.04% ~ 88.61%, its mean value is 79.77%, for easy calculating, get 80.00% on average the putting recovery as Strontium-90 rapid analysis, this recovery can meet routine measurement requirement.And it is consistent with 1 putting of the L liquid effluent sample gained recovery that this rapid analysis is processed 2 putting of the L liquid effluent sample gained recovery, and therefore the method applicability is wider.
The uncertainty that we also bring the method is analyzed: main uncertainty of measurement source has by analysis: the uncertain component that measuring repeatability is introduced
u 1 , the uncertain component that apparatus measures is introduced
u 2 , the uncertainty component that detection efficiency is introduced
u 3 , the uncertain component that standard solution is introduced
u 4 .The uncertain component that measuring repeatability is introduced
u 1 by above-mentioned 24 groups of nuclear power plant's liquid effluent sample mark-on measurement results, express method is carried out to uncertainty evaluation.Use on average the putting recovery to calculate the specific radioactivity of nuclear power plant's liquid effluent sample, the actual specific radioactivity obtaining and actual value are compared, the uncertain component that uses Bessel Formula computation and measurement repeatability to introduce
u 1 .
Adopt Bessel Formula to evaluate the formula of relative uncertainty as follows:
In formula:
u r ---Relative combined uncertainty;
a i ---the specific radioactivity that the experiment of i group obtains, Bq/L;
a si ---the actual radiation specific activity that the experiment of i group adds, Bq/L
n---experiment total degree.
Calculated by the data in above-mentioned formula his-and-hers watches 1, can obtain, measuring repeatability introduce relative uncertainty (
u r1 ) be 6.84%.By analysis, apparatus measures introduce relative uncertainty (
u r2 ) be 0.79%, detection efficiency introduce relative uncertainty (
u r3 ) be 3.0%, standard solution introduce relative uncertainty (
u r4 ) be 1.5%, the Relative combined uncertainty of Strontium-90 rapid analysis (
u r ) be 7.66%, relative expanded uncertainty (
u r ) be 15.32%, spreading coefficient (k) is 2.The expanded uncertainty of gained experimental technique meets the requirement of environment measuring.
Also utilize following formula to calculate to the detection limit of the method, the results are shown in Fig. 2 simultaneously:
In formula:
mDC---detection limit, Bq/L
n b ---background counting rate, cpm
t---gate time, min
e---the detection efficiency of instrument to Sr-90 standard source, cpm/dpm
y---the chemical recovery rate of strontium, %
v---sample size, L
The liquid providing according to nuclear power plant dodges the correlated performance parameter of spectrometer Tricarb 3180, can obtain the detection limit (Fig. 2) of method under different volumes.As seen from Figure 2, adopt 2 L liquid effluents, measure 8 h and can obtain the detection limit of 0.01 Bq/L, if strengthen sample size or increase Measuring Time the detection limit that can continue to reduce method.Detection limit can be reduced to more low-level (0.003 Bq/L) if adopt low background liquid to dodge spectrometer and extend Measuring Time.
By test result of the present invention and GB6766 method mark-on control experiment:
Experiment adopts mark-on in 8.0 L liquid effluents, proceeds in 42 L beakers after mixing, and is respectively used to this patent method and GB6766 method, by experiment the feasibility of result determination methods.Can calculate Strontium-90 in liquid effluent (mark-on) testing result according to measurement result, experimental result is in table 2.In table, last classifies testing result and the relative deviation that adds scale value as, from table, can see, adopt the method for quick acquired results of Strontium-90 to be respectively-8.94% and 5.03% with the relative deviation that adds scale value, adopt GB6766 method acquired results and the relative deviation that adds scale value to be respectively-12.01% and-9.77%.Therefore, adopt this patent method gained measurement result more accurate, meet and measure requirement.
In GB6766 analyzing liquid effluent, the testing result mean value of Strontium-90 (mark-on) is 3.19 Bq/L, and in the method for quick analyzing liquid effluent of Strontium-90, the testing result mean value of Strontium-90 (mark-on) is 3.51 Bq/L.To, by GB6766 method experimental results as with reference to value, use
e n method is tested to Strontium-90 rapid analysis gained measured value.
Formula:
In formula:
e n : normalization errors index;
y r : reference value;
y c : measured value;
u r : reference method expanded uncertainty;
u c : measuring method expanded uncertainty.
According to " assessment of waterborne radioactivity nucleic Strontium-90 uncertainty of measurement " (environmental monitoring management and technology, 2004) GB6766 experimental technique being carried out to relative expanded uncertainty evaluation result is 10.0%, the relative expanded uncertainty (Ur) of this method is 15.32%, substitution data:
Due to En < 1, meet acceptance criterion, the method for quick gained measurement result of Strontium-90 and GB6766 method acquired results do not have significant difference.Therefore, the rapid analysis of Strontium-90 can accurately obtain the concentration of Strontium-90 in nuclear power plant's liquid effluent.
Strontium-90 in table 2 liquid effluent (mark-on) testing result
Analytical approach of the present invention is applied to respectively to Ningde nuclear power plant and red nuclear power plant along the river carries out analytical test, the results are shown in Table 3 for it.
Strontium-90 measurement data table in table 3 nuclear power plant liquid effluent
Above-described embodiment is only explanation technical conceive of the present invention and feature; its object is to allow person skilled in the art can understand content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences that Spirit Essence is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (7)
1. a rapid analysis for Strontium-90 in nuclear power plant's liquid effluent, is characterized in that, comprises rapid following steps:
(a) get a certain amount of nuclear power plant liquid effluent, and add wherein strontium carrier and yttrium carrier, the cation exchange of being flowed through under acid condition chromatograph post, uses the cation exchange chromatograph post described in salpeter solution drip washing subsequently, collects eluent and obtains the first eluent;
(b) by the first described eluent stream through P204 extration resin chromatograph column separating purification, with the P204 extration resin chromatograph post described in salpeter solution drip washing, collect eluent and obtain the second eluent;
(c) by after the second eluent evaporate to dryness with dissolving with hydrochloric acid and be transferred in low potash glass bottle, add scintillation solution to mix to be placed on liquid and dodge the counting rate of measuring Yttrium-90 on spectrometer, calculate the radiochemical recovery yield of Yttrium-90 according to described Yttrium-90 counting rate;
(d) get many parts of a certain amount of nuclear power plant liquid effluents, repeating step (a), to step (c), calculates the average radiochemical recovery yield of Yttrium-90 again, and calculates the specific activity of Yttrium-90 according to the average radiochemical recovery yield of Yttrium-90 counting rate and Yttrium-90;
(e), according to the Decay relation between Yttrium-90 and Strontium-90, calculate the specific activity of Strontium-90 according to the specific activity of described Yttrium-90.
2. the rapid analysis of Strontium-90 in nuclear power plant according to claim 1 liquid effluent, it is characterized in that: in step (a), described nuclear power plant liquid effluent under the condition of pH=0.1 ~ 5 with the flow velocity of 8 ~ 10 ml/min described cation exchange chromatograph post of flowing through.
3. the rapid analysis of Strontium-90 in nuclear power plant according to claim 1 liquid effluent, is characterized in that: in step (b), the flow velocity of described the first eluent is 2 ml/min.
4. the rapid analysis of Strontium-90 in nuclear power plant according to claim 1 liquid effluent, it is characterized in that: in step (a), described salpeter solution drip washing is carried out at twice, first uses the salpeter solution drip washing of 0.1 ~ 0.5mol/L, then uses the salpeter solution wash-out of 6 ~ 10mol/L.
5. the rapid analysis of Strontium-90 in nuclear power plant according to claim 1 liquid effluent, it is characterized in that: in step (b), described salpeter solution drip washing is carried out at twice, first uses the salpeter solution drip washing of 1 ~ 3mol/L, then uses the salpeter solution wash-out of 5 ~ 8mol/L.
6. the rapid analysis of Strontium-90 in nuclear power plant according to claim 1 liquid effluent, is characterized in that: in step (a), described the first eluent regulates pH to 0.1 ~ 0.5 with ammoniacal liquor.
7. the rapid analysis of Strontium-90 in nuclear power plant according to claim 1 liquid effluent, it is characterized in that: in described step (c), add supplementary deionized water in the low potash glass bottle of scintillation solution forward direction that liquor capacity is wherein compared for 1:1 with scintillation solution volume.
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