CN115356763A - Method for rapidly analyzing Fe-55 in water - Google Patents
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- CN115356763A CN115356763A CN202210858402.XA CN202210858402A CN115356763A CN 115356763 A CN115356763 A CN 115356763A CN 202210858402 A CN202210858402 A CN 202210858402A CN 115356763 A CN115356763 A CN 115356763A
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- 238000000034 method Methods 0.000 title claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 230000000694 effects Effects 0.000 claims abstract description 15
- 238000000746 purification Methods 0.000 claims abstract description 15
- 238000005259 measurement Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 40
- 239000011347 resin Substances 0.000 claims description 19
- 229920005989 resin Polymers 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000589 Siderophore Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 238000003795 desorption Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 238000012937 correction Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 5
- 239000000084 colloidal system Substances 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 230000005526 G1 to G0 transition Effects 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 150000001805 chlorine compounds Chemical class 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 100
- 238000004458 analytical method Methods 0.000 description 19
- 238000011156 evaluation Methods 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 238000005349 anion exchange Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000002337 anti-port Effects 0.000 description 2
- 230000005250 beta ray Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 230000003313 weakening effect Effects 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- XEEYBQQBJWHFJM-AKLPVKDBSA-N Iron-59 Chemical compound [59Fe] XEEYBQQBJWHFJM-AKLPVKDBSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005514 radiochemical analysis Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/20—Measuring radiation intensity with scintillation detectors
- G01T1/204—Measuring radiation intensity with scintillation detectors the detector being a liquid
- G01T1/2042—Composition for liquid scintillation systems
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/20—Measuring radiation intensity with scintillation detectors
- G01T1/204—Measuring radiation intensity with scintillation detectors the detector being a liquid
- G01T1/2042—Composition for liquid scintillation systems
- G01T1/2047—Sample preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T7/00—Details of radiation-measuring instruments
- G01T7/02—Collecting means for receiving or storing samples to be investigated and possibly directly transporting the samples to the measuring arrangement; particularly for investigating radioactive fluids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T7/00—Details of radiation-measuring instruments
- G01T7/02—Collecting means for receiving or storing samples to be investigated and possibly directly transporting the samples to the measuring arrangement; particularly for investigating radioactive fluids
- G01T7/04—Collecting means for receiving or storing samples to be investigated and possibly directly transporting the samples to the measuring arrangement; particularly for investigating radioactive fluids by filtration
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention relates to the technical field of radioactivity monitoring, and particularly discloses a method for rapidly analyzing Fe-55 in water, which comprises the following steps: step 1: 55 enrichment of isotopes of Fe with other Fe; and 2, step: 55 purifying isotopes of Fe and other Fe; and 3, step 3: 55 measurement of the activity of Fe. The method can quickly complete the Fe-55 enrichment, fe-55 purification and the measurement of the activity of Fe-55 in the water sample.
Description
Technical Field
The invention belongs to the technical field of radioactivity monitoring, and particularly relates to a method for rapidly analyzing Fe-55 in water.
Background
The nuclear power plant effluent radioactivity monitoring specification (national nuclear power plant's emission 2020/44) requires that the nuclear power plant be developed into liquid effluent at 9/1/2020 55 And (5) monitoring Fe. However, at present, liquid effluent is not established yet in China 55 Method for rapid analysis of Fe 59 The analysis of Fe is carried out by GB/T15220-1994 analysis method of iron-59 in water. And then 59 Fe and 55 although there are parts which can be communicated in the steps of enriching and purifying the sample, the Fe analysis method has substantial difference in measurement and obvious difference, and cannot be used for analyzing the Fe 59 The analysis of Fe was applied after adaptation 55 In the analysis of Fe.
The current international analysis method for common radioactive iron is as follows:
TABLE 1 analysis method of international common radioactive iron
(1) Hydroxide precipitation coupled anion exchange process
The method recommends the separation and purification of iron by using hydroxide precipitation and anion exchange in a plurality of standards and methods at home and abroad. In ASTM D4922-2009, elements such as Co, ni, fe and the like are enriched by hydroxide precipitation, and Fe is separated from interfering elements such as Mn, zr, nb, cs and the like through an anion exchange column.
The analytical procedure proposed by ISO/DIS 22515, which is being drafted, is as follows: 1) Adding a carrier and an antiport (comprising Fe carrier and the antiport of Sb, cs, ca, cr, co, mn and other elements); 2) Ammonia water adjustment, precipitation, centrifugation and desorption; 3) Dissolving by nitric acid, and separating and purifying Fe; 4) Adding Na 2 HPO 4 And precipitating the solution and ammonia water, desorbing, dissolving by adopting HCl, putting into a counting flask, and measuring on a liquid flash spectrometer. Two separation and purification methods are recommended, including separation using anion exchange resins (e.g., AG 1-X8) and extraction resins (e.g., TEVA, TRU, UTEVA).
The analysis process of the hydroxide precipitation and the anion exchange method has the advantages of multiple steps of precipitation, centrifugation and column treatment, generally three days of radiochemical analysis time and long time consumption.
(2) TRU resin extraction chromatography
The TRU resin is prepared by coating a CMPO extractant and a TBP extractant on an inert support (polyethylene or acrylate) together, and has relative selectivity to Fe.
Eichrom standard procedure "Eichrom analytical procedure (FEW 01): iron-55in water "is a purified iron solution obtained by evaporating a water sample to dryness, dissolving the residue of evaporation to dryness with 8M nitric acid solution, subjecting the solution to a TRU resin column with 8mol/L nitric acid solution system, and desorbing with 2mol/L nitric acid solution. ISO/DIS 22515, which is being drafted, recommends separation of extraction resins (e.g., TEVA, TRU, UTEVA). However, the conventional evaporation process takes a lot of time for a large volume of sample.
Therefore, it is necessary to provide a rapid analysis method for Fe-55 in water to solve the above problems.
Disclosure of Invention
The invention aims to provide a method for rapidly analyzing Fe-55 in water, which can rapidly and accurately analyze the radioactivity.
The technical scheme of the invention is as follows:
a method for rapidly analyzing Fe-55 in water comprises the following steps:
step 1: 55 enrichment of isotopes of Fe with other Fe
1.1 preparation of the siderophore solution, i.e. 56 FeCl 3 Mixing with HCl;
1.2 adding a solution of a siderophore to the sample, adjusting the pH =10 of the water sample, under which conditions, 55 fe and other isotopes of Fe form hydroxide colloidal particles;
1.3 heating the sample to quickly coagulate and precipitate colloid;
1.4 suction filtration, discarding the supernatant, using HNO 3 Dissolving the precipitate for several times in a small amount and transferring into a beaker 55 Enrichment solution of isotopes of Fe and other Fe;
and 2, step: 55 purification of isotopes of Fe with other Fe
2.1 preparing a purification material which comprises TRU resin, wherein a mixture of carbamyl-methylphosphoryl chloride derivatives and tributyl phosphate is adopted as a stationary phase;
2.2 adding HNO to the TRU resin column 3 Pre-balancing, slowly loading the enriched liquid to column, and adding HNO 3 Leaching, discarding effluent liquid, and enabling the resin after exchange to turn red due to Fe adsorption;
2.3 use of HNO 3 Desorbing, collecting desorption liquid, heating the desorption liquid to evaporate to dryness to obtain purified Fe residue;
2.4 adding phosphoric acid into the residue to dissolve the residue, transferring the residue into a volumetric flask, and diluting the residue with deionized water until the residue is marked 55 A purified solution of isotopes of Fe and other Fe;
and 3, step 3: 55 measurement of Fe Activity
By passing 55 Fe and 59 liquid flash spectrometer pair obtained by Fe standard substance scale 55 Fe and 59 the detection efficiency and quenching correction curve of Fe, after the purified liquid is measured by a liquid flash spectrometer, calculating the purified liquid by setting different interested areas 55 Radioactivity concentration AC of Fe Fe-55 The calculation formula is as follows:
in the formula:
AC Fe-55 — 55 the radioactivity concentration of Fe, bq/L;
R n,Fe-55 — 55 net count rate of Fe region of interest, counts per second, s -1 ；
R n,Fe-59 — 59 Net count rate of Fe region of interest, counts per second, s -1 ；
XT-from 59 Cross-talk factors obtained from the Fe quenching correction curve;
ε Fe-55 — 55 fe detection efficiency;
y-chemical recovery;
V s -volume of purified liquid, L;
DF-decay factor, e -λt ；
λ— 55 A Fe decay constant;
t-time difference from the reference date to the time in the middle of the experimental count.
Step 1.1, in the prepared siderophore solution 56 The content of Fe element is 5mg/mL.
In step 1.2, the pH of the water sample was adjusted with NaOH solution =10.
In step 1.4, suction filtration is carried out through a Buchner funnel.
In step 2.1, the prepared TRU resin has a particle size of 100 to 150 μm.
In step 2.2, the adding flow rate of the Fe enrichment solution is controlled to be 0.5-1 mL/min.
In step 2.3, HNO is desorbed 3 The flow rate of (2) was 0.5mL/min.
In step 2.4, if the dissolution effect is poor, heating is carried out on an electric furnace to improve the solubility.
The entire purification process of step 2 takes no more than 1 hour.
In step 3, the purified liquid is taken out and put into a low-potassium glass bottle, hisafe III scintillation liquid is added, and a liquid scintillation counter is used for measuring the content of the sample 55 Fe and 59 the net counting rate of the interested area of Fe is calculated 55 The radioactivity concentration of Fe.
The invention has the following remarkable effects:
(1) The method adopts a rapid iron coagulation and precipitation method, and can rapidly complete the Fe-55 enrichment in the water sample.
(2) The method adopts the TRU resin to selectively adsorb the iron, and can quickly complete the purification of the Fe-55 in the water sample.
(3) The method adopts a conservative calculation mode for measurement by a liquid flash spectrometer, and can quickly and accurately complete the measurement of the activity of Fe-55 in water.
Drawings
FIG. 1 is a flow chart of an analysis method.
Detailed Description
The invention is further described in detail below with reference to the drawings and specific embodiments.
The method for rapidly analyzing Fe-55 in water as shown in figure 1 comprises the following steps:
step 1: 55 enrichment of Fe with other isotopes of Fe
1.1 preparation of the siderophore solution, i.e. 56 FeCl 3 Mixing with HCl, wherein 56 Fe element content is 5mg/mL, and the Fe element is used as a non-radioactive nuclide, 56 fe does not influence the final measurement result;
1.2 to 500mL of the sample, 0.3mL of the siderophore solution was added, and the pH of the water sample was adjusted to =10 using 10mol/L NaOH solution, under which conditions, 55 fe and other isotopes of Fe form hydroxide colloidal particles;
1.3, heating the sample by using an electric furnace, increasing the temperature, intensifying the movement of colloidal particles and increasing the collision chance among the colloidal particles, thereby weakening the adsorption effect of colloidal nuclei on ions, weakening the stability of colloid and quickly coagulating and precipitating the colloid;
1.4 suction filtration through Buchner funnel, discarding supernatant, using 8mol/L HNO 3 Dissolving the precipitate for several times in a small amount and transferring into a 50mL beaker 55 Enrichment solution of isotopes of Fe and other Fe;
step 2: 55 purification of Fe with other isotopes of Fe
2.1 preparing a purification material, wherein the TRU resin has the particle size of 100-150 mu m and is a product of Eichrom company of America; the stationary phase adopts a mixture of carbamyl-methyloxyphosphorus derivative (CMPO) and tributyl phosphate (TBP);
2.2 Add 5mL 8mol/L HNO to the TRU resin column 3 Pre-balancing for 5min, slowly loading the enriched liquid into column, and adding 1695l 8mol/L HNO 3 Leaching, discarding effluent liquid, and enabling the resin after exchange to turn red due to Fe adsorption; attention needs to be paid to the fact that the adding flow rate of the Fe enrichment solution is controlled to be 0.5-1 mL/min, so that the enrichment solution is ensured to be fully reacted with TRU resin, and the red strip-shaped object is prevented from moving too fast;
2.3 use 5mL of 0.1mol/L HNO 3 Desorbing at the flow rate of 0.5mL/min, collecting the desorption solution by using a beaker, placing the desorption solution on an electric furnace, and evaporating to dryness to obtain the purified Fe residue.
2.4 adding 4mL of 1mol/L phosphoric acid into the residue to dissolve the residue, heating the residue on an electric furnace to improve the solubility if the dissolving effect is poor, transferring the residue into a 5mL volumetric flask, and diluting the residue with deionized water until the mark line is formed 55 A purified solution of isotopes of Fe and other Fe;
the whole purification process takes no more than 1 hour;
and step 3: 55 measurement of Fe Activity
The iron-containing components in the reactor of the nuclear power plant can be simultaneously generated after neutron activation 55 Fe and 59 Fe。 55 the half-life period of Fe is 2.7 years, the characteristic X-ray of manganese is emitted after the orbital electron is captured, and the energy is 5.9keV; 59 the half-life of Fe was 44.5 days, and beta, gamma rays were emitted with beta ray energies of 475keV (51.2%), 273keV (48.5%), and gamma ray energies of 1.29MeV (43%), 1.09MeV (57%). The beta ray spectrum is a continuous spectrum, and when liquid flash measurement is carried out, 59 the beta rays with higher energy emitted by Fe can influence the low energy end, and are analyzed 55 Consideration of Fe 59 Contribution of Fe;
by passing 55 Fe and 59 liquid flash spectrometer pair obtained by Fe standard substance scale 55 Fe and 59 the detection efficiency and quenching correction curve of Fe, after the purified liquid is measured by a liquid flash spectrometer, calculating the purified liquid by setting different interested areas 55 Radioactivity concentration AC of Fe Fe-55 The calculation formula is as follows:
in the formula:
AC Fe-55 — 55 the radioactivity concentration of Fe, bq/L;
R n,Fe-55 — 55 net count rate of Fe region of interest, counts per second, s -1 ；
R n,Fe-59 — 59 Net count rate of Fe region of interest, counts per second, s -1 ；
XT-from 59 Cross-talk factors obtained from the Fe quenching correction curve;
ε Fe-55 — 55 the efficiency of Fe detection;
y-chemical recovery;
V s -volume of purified liquid, L;
DF-decay factor, e -λt ；
λ— 55 A Fe decay constant;
t-time difference between the reference date and the middle of the experimental count.
Taking 4.0mL of Fe purified solution into a low-potassium glass bottle, adding 16mL of Hisafe III scintillation solution, and measuring the content of the sample by using a liquid scintillation counter 55 Fe and 59 the net counting rate of the interested area of Fe is calculated 55 The concentration of radioactivity of Fe.
Examples
The method comprises adding excessive siderophore into the sample, adjusting pH with NaOH, and heating 55 The quick coagulation of the isotopes of Fe and other Fe is realized by suction filtration and dissolution 55 And (3) rapidly enriching isotopes of Fe and other Fe from the water body. Separating the enriched solution with a TRU resin column to obtain 55 The isotope purification solution of Fe and other Fe, finally the purification solution is measured by using a liquid scintillation counter, and a sample is obtained by calculation 55 The activity of Fe.
The method is used for carrying out comparison among laboratories at Fuqing nuclear power, suzhou institute and Fujian province radiation environment monitoring station, a standard sample is added to the liquid effluent of Fuqing nuclear power 7ZLD, and 3 laboratories develop after receiving the comparison sample 55 Analysis of Fe with the dispensed prepared 7ZLD liquid effluent 55 Fe sample as background counting rate, reported in 3 laboratories 55 The normalized activity concentration of Fe. According to the requirements of statistical method for capacity verification by using laboratory comparison (GB/T28043-2019) and statistical processing and capacity evaluation guideline for capacity verification result (CNAS-GL 002), an En value method and a Z ratio score method are adopted for evaluation, and the comparison result and the evaluation result are shown in Table 2.
The En value method evaluation result shows that the analysis result of each laboratory has no obvious difference with the specified value under the 95% confidence probability, and the accuracy of the analysis method and the accuracy of the analysis results of 3 laboratories are verified; the evaluation result of the Z ratio score method shows that the comparison results of 3 laboratories are satisfactory, and the analysis capability of Fuqing nuclear power and the analysis capability of Fe-55 of the other 2 laboratories are confirmed.
TABLE 2 effluent Fe-55 analytical laboratory alignment and evaluation results (one) E n Evaluation result of value method
(II) evaluation results of Z ratio score method
Note: activity concentration y c The resulting normalized activity concentrations were measured for each laboratory.
While there have been shown and described what are at present considered the fundamental principles of the invention, its essential features and advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.
Claims (10)
1. A method for rapidly analyzing Fe-55 in water is characterized by comprising the following steps: the method comprises the following steps:
step 1: 55 enrichment of isotopes of Fe with other Fe
1.1 preparation of the siderophore solution, i.e. 56 FeCl 3 Mixing with HClA solution;
1.2 adding a solution of a siderophore to the sample, adjusting the pH =10 of the water sample, under which conditions, 55 fe and other isotopes of Fe form hydroxide colloidal particles;
1.3 heating the sample to quickly coagulate and precipitate colloid;
1.4 suction filtration, discarding the supernatant, using HNO 3 Dissolving the precipitate for several times in a small amount and transferring into a beaker 55 Enrichment solution of isotopes of Fe and other Fe;
step 2: 55 purification of isotopes of Fe with other Fe
2.1 preparing a purification material which comprises TRU resin, wherein a mixture of carbamyl-methylphosphoryl chloride derivatives and tributyl phosphate is adopted as a stationary phase;
2.2 adding HNO to the TRU resin column 3 Pre-balancing, slowly loading the enriched liquid to column, and adding HNO 3 Leaching, discarding effluent liquid, and enabling the resin after exchange to turn red due to Fe adsorption;
2.3 use of HNO 3 Desorbing, collecting desorption liquid, heating the desorption liquid to evaporate to dryness to obtain purified Fe residue;
2.4 adding phosphoric acid into the residue to dissolve the residue, transferring the residue into a volumetric flask, and diluting the residue with deionized water until the residue is marked 55 A purified solution of isotopes of Fe and other Fe;
and step 3: 55 measurement of Fe Activity
By passing 55 Fe and 59 liquid flash spectrometer pair obtained by Fe standard substance scale 55 Fe and 59 the detection efficiency and quenching correction curve of Fe, after the purified liquid is measured by a liquid flash spectrometer, calculating the purified liquid by setting different interested areas 55 Radioactivity concentration AC of Fe Fe-55 The calculation formula is as follows:
in the formula:
AC Fe-55 — 55 of FeRadioactivity concentration, bq/L;
R n,Fe-55 — 55 net count rate of Fe region of interest, counts per second, s -1 ；
R n,Fe-59 — 59 Net count rate of Fe region of interest, counts per second, s -1 ；
XT-from 59 Cross-talk factors obtained from the Fe quenching correction curve;
ε Fe-55 — 55 the efficiency of Fe detection;
y-chemical recovery;
V s -volume of purified liquid, L;
DF-decay factor, e -λt ；
λ— 55 A Fe decay constant;
t-time difference from the reference date to the time in the middle of the experimental count.
2. The method for rapidly analyzing Fe-55 in water as claimed in claim 1, wherein: step 1.1 in the prepared siderophore solution 56 The content of Fe element is 5mg/mL.
3. The method for rapidly analyzing Fe-55 in water according to claim 1, wherein the method comprises the following steps: in step 1.2, the pH of the water sample was adjusted with NaOH solution =10.
4. The method for rapidly analyzing Fe-55 in water as claimed in claim 1, wherein: in step 1.4, suction filtration is carried out through a Buchner funnel.
5. The method for rapidly analyzing Fe-55 in water according to claim 1, wherein the method comprises the following steps: in step 2.1, the prepared TRU resin has a particle size of 100 to 150 μm.
6. The method for rapidly analyzing Fe-55 in water as claimed in claim 1, wherein: in step 2.2, the adding flow rate of the Fe enrichment solution is controlled to be 0.5-1 mL/min.
7. The method for rapidly analyzing Fe-55 in water as claimed in claim 1, wherein: in step 2.3, HNO is desorbed 3 The flow rate of (2) was 0.5mL/min.
8. The method for rapidly analyzing Fe-55 in water as claimed in claim 1, wherein: in step 2.4, if the dissolution effect is poor, heating is carried out on an electric furnace to improve the solubility.
9. The method for rapidly analyzing Fe-55 in water as claimed in claim 1, wherein: the entire purification process of step 2 takes no more than 1 hour.
10. The method for rapidly analyzing Fe-55 in water according to claim 1, wherein the method comprises the following steps: in step 3, the purified liquid is taken out and put into a low-potassium glass bottle, hisafe III scintillation liquid is added, and a liquid scintillation counter is used for measuring the content of the sample 55 Fe and 59 the net counting rate of the interested area of Fe is calculated 55 The radioactivity concentration of Fe.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5412216A (en) * | 1993-10-29 | 1995-05-02 | Beckman Instruments, Inc. | Method and apparatus for identifying a radionuclide in a liquid scintillation sample |
| CN112098557A (en) * | 2020-09-22 | 2020-12-18 | 中国人民解放军63653部队 | Combined analysis method for Pu-239, Sr-90 and Cs-137 in high-salinity water |
| CN114152488A (en) * | 2021-11-11 | 2022-03-08 | 苏州热工研究院有限公司 | In water55Fe and59fe monitoring device and monitoring method |
| CN114354301A (en) * | 2021-12-01 | 2022-04-15 | 中国辐射防护研究院 | Method for analyzing iron-55 in liquid |
| CN114740519A (en) * | 2022-04-19 | 2022-07-12 | 山东核电有限公司 | Combined analysis method of strontium-89, strontium-90, iron-55, iron-59 and nickel-63 in water |
-
2022
- 2022-07-20 CN CN202210858402.XA patent/CN115356763A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5412216A (en) * | 1993-10-29 | 1995-05-02 | Beckman Instruments, Inc. | Method and apparatus for identifying a radionuclide in a liquid scintillation sample |
| CN112098557A (en) * | 2020-09-22 | 2020-12-18 | 中国人民解放军63653部队 | Combined analysis method for Pu-239, Sr-90 and Cs-137 in high-salinity water |
| CN114152488A (en) * | 2021-11-11 | 2022-03-08 | 苏州热工研究院有限公司 | In water55Fe and59fe monitoring device and monitoring method |
| CN114354301A (en) * | 2021-12-01 | 2022-04-15 | 中国辐射防护研究院 | Method for analyzing iron-55 in liquid |
| CN114740519A (en) * | 2022-04-19 | 2022-07-12 | 山东核电有限公司 | Combined analysis method of strontium-89, strontium-90, iron-55, iron-59 and nickel-63 in water |
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