CN114235973A - Method for determining content of Np-237 in urine sample - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 210000002700 urine Anatomy 0.000 title claims abstract description 45
- 238000000975 co-precipitation Methods 0.000 claims abstract description 5
- 238000004094 preconcentration Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 25
- 229910017604 nitric acid Inorganic materials 0.000 claims description 23
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000005259 measurement Methods 0.000 claims description 14
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004070 electrodeposition Methods 0.000 claims description 10
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052770 Uranium Inorganic materials 0.000 claims description 6
- 238000009713 electroplating Methods 0.000 claims description 6
- 238000011068 loading method Methods 0.000 claims description 5
- NQMRYBIKMRVZLB-UHFFFAOYSA-N methylamine hydrochloride Chemical compound [Cl-].[NH3+]C NQMRYBIKMRVZLB-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 235000010288 sodium nitrite Nutrition 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000003480 eluent Substances 0.000 claims description 4
- GPGMRSSBVJNWRA-UHFFFAOYSA-N hydrochloride hydrofluoride Chemical compound F.Cl GPGMRSSBVJNWRA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000700 radioactive tracer Substances 0.000 claims description 4
- 229910052776 Thorium Inorganic materials 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- 239000008151 electrolyte solution Substances 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 10
- 229910052781 Neptunium Inorganic materials 0.000 description 6
- LFNLGNPSGWYGGD-UHFFFAOYSA-N neptunium atom Chemical compound [Np] LFNLGNPSGWYGGD-UHFFFAOYSA-N 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 210000003608 fece Anatomy 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- LFNLGNPSGWYGGD-IGMARMGPSA-N neptunium-237 Chemical compound [237Np] LFNLGNPSGWYGGD-IGMARMGPSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 208000028571 Occupational disease Diseases 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000027939 micturition Effects 0.000 description 1
- AGQOEYDNNHWRSG-UHFFFAOYSA-N nitric acid;oxalic acid Chemical compound O[N+]([O-])=O.OC(=O)C(O)=O AGQOEYDNNHWRSG-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- -1 trilaurylamine-polytrichloroethylene Chemical group 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N2030/77—Detectors specially adapted therefor detecting radioactive properties
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the technical field of radionuclide analysis, and relates to a method for determining the content of Np-237 in a urine sample. The determination method comprises the following steps: (1) sample pretreatment; (2) coprecipitation pre-concentration; (3) adjusting the valence state; (4) separating and purifying; (5) preparing a measuring source; (6) and (6) measuring. The method for measuring the content of the Np-237 in the urine sample can be used for measuring the content of the Np-237 in the urine sample more conveniently, quickly and accurately.
Description
Technical Field
The invention belongs to the technical field of radionuclide analysis, and relates to a method for determining the content of Np-237 in a urine sample.
Background
237Np is a transuranic actinide nuclide produced by the action of neutrons and uranium, is an alpha nuclide, and belongs to a highly toxic group. In-nuclear testing and production of natural uranium as fuel239Pu, uranium enrichment reactor, post-treatment and other nuclear facilities are released in the operation process237Np. To engage in237The Np-related operators are all likely to inhale237Np。237After entering the human body, Np is mainly deposited in the lung, and then in the liver, kidney and other soft tissues, causing internal irradiation damage. According to the related standards of ICRP No. 78 publication of personal monitoring of irradiation in workers, GBZ129-2016 personal monitoring Specification of occupational irradiation, etc., the methods for monitoring irradiation in individuals are mainly divided into direct measurement in vitro, analysis of excreta, and analysis of air sampling. By using internal irradiation of the faeces in the urine sample237The radiochemical analytical measurement method of Np is engaged in237Np operates the basic method of in-person radiation monitoring and evaluation.
At present, only the measurement of Netunium-237 in urine is performed in China (Yuanzu, Liaoxiangzhen, Netunium-237. atomic energy science and technology [ J)],1977(02): 203 plus 207.) and luyu chess (luyu chess, determination of neptunium-237 content in urine, prevention and treatment of Guangdong occupational disease [ J],1979(02): 18-19.) report in urination237Radiochemical analytical measurement of the Np content. Wherein the residual flare is in the urine237The key steps of measuring the Np content are as follows: adding bismuth phosphate to precipitate carrier neptunium; ② the neptunium is separated and purified by trilaurylamine-polytrichloroethylene chromatographic column; and thirdly, preparing the neptunium measuring source through electrodeposition of a nitric acid-oxalic acid system. The Ruyu chess is separated and purified by zirconium fluoride coprecipitation to concentrate neptunium in urine, extraction chromatography, and finally caught by lanthanum fluoride and fluorescent powderObtaining neptunium preparation measurement source. The main drawbacks of these two methods are: introducing new impurities of bismuth and zirconium in the process of coprecipitation and preconcentration of Np; secondly, the chemical recovery rate in the whole process is calculated by adopting the empirical recovery rate in the experimental process, so that the result error is large, and the data has contingency; thirdly, lanthanum fluoride and fluorescent powder are adopted for precipitation source preparation, so that the self-absorption is serious and the resolution ratio is low.
Disclosure of Invention
The invention aims to provide a method for measuring the content of Np-237 in a urine sample, which can more conveniently, quickly and accurately measure the content of Np-237 in the urine sample.
To achieve this object, in a basic embodiment, the present invention provides a method for determining the amount of Np-237 in a urine sample, said method comprising the steps of:
(1) sample pretreatment: adding urine sample236Pu tracer, adding nitric acid and hydrogen peroxide, and heating to slightly boil to digest the urine sample;
(2) coprecipitation pre-concentration: cooling the urine sample, adding phosphoric acid to adjust the pH value, stirring until the urine sample is fully precipitated, standing, centrifuging, dissolving the precipitate by using nitric acid and hydrogen peroxide, and heating until the urine sample is nearly dry and is white residue;
(3) adjusting the valence state: dissolving the white residue with nitric acid, adding hydroxylamine hydrochloride and Fe2+And adjusting the valence state of Np to Np (IV) by sodium nitrite;
(4) separation and purification: loading trialkyl methyl ammonium chloride chromatographic powder into a chromatographic column, washing the chromatographic column by nitric acid, loading the solution obtained in the step (3), washing the chromatographic column by nitric acid solution and hydrochloric acid solution to remove U and Th, and desorbing Np by using hydrochloric acid-hydrofluoric acid mixed solution to obtain Np eluent;
(5) preparing a measurement source: preparing an Np measuring source by using an electrodeposition method for the Np eluent obtained in the step (4);
(6) measurement: and (4) placing the Np measurement source prepared in the step (5) into an alpha spectrometer for measurement.
In a preferred embodiment, the invention provides a method for determining the content of Np-237 in a urine sample, wherein in the step (1), the concentrations of nitric acid and hydrogen peroxide are respectively 12-16mol/L and 20-30 wt%, and the time for micro-boiling digestion of the urine sample is 0.5-2 h.
In a preferred embodiment, the present invention provides a method for determining the amount of Np-237 in a urine sample, wherein in step (2), the pH is adjusted to 8 to 9, and the standing time is 2 to 12 hours.
In a preferred embodiment, the present invention provides a method for determining the content of Np-237 in a urine sample, wherein in step (2), the concentrations of nitric acid and hydrogen peroxide are 12-16mol/L and 20-30 wt%, respectively.
In a preferred embodiment, the present invention provides a method for determining the amount of Np-237 in a urine sample, wherein in step (2), said heating to near dryness is heating to remove 85-95% of the water.
In a preferred embodiment, the invention provides a method for determining the content of Np-237 in a urine sample, wherein in step (3), the nitric acid, hydroxylamine hydrochloride and Fe are used2+And the concentration of sodium nitrite is 2.5-4.5mol/L, 1-3mol/L, 0.5-1.5mol/L and 3-5mol/L respectively.
In a preferred embodiment, the present invention provides a method for determining the amount of Np-237 in a urine sample, wherein in step (4), trialkyl methyl ammonium chloride chromatographic powder is loaded into a chromatographic column by dry-loading.
In a preferred embodiment, the invention provides a method for determining the content of Np-237 in a urine sample, wherein in the step (4), a chromatographic column is washed by a nitric acid solution with the concentration of 7.5-8.5mol/L and a hydrochloric acid solution with the concentration of 8.5-9.5mol/L in sequence, and the concentrations of hydrochloric acid and hydrofluoric acid in a hydrochloric acid-hydrofluoric acid mixed solution are respectively 0.08-0.12mol/L and 0.02-0.08 mol/L.
In a preferred embodiment, the invention provides a method for determining the content of Np-237 in a urine sample, wherein in the step (5), the Np measuring source prepared by the electrodeposition method is prepared by preparing a sample source by using an ammonium sulfate electrolyte solution, preparing the Np measuring source by electroplating for 0.5-2h under certain current by using a stainless steel sheet as a cathode and a platinum wire as an anode.
In a preferred embodiment, the present invention provides a method for determining the amount of Np-237 in a urine sample, wherein in step (6) said α spectrometer is a low background α spectrometer.
The method has the advantages that the method for measuring the content of the Np-237 in the urine sample can be used for measuring the content of the Np-237 in the urine sample more conveniently, quickly and accurately.
The invention is to do237The irradiation monitoring and evaluation in Np operation staff provides effective technical support, and the problem in urine sample is solved237Difficulties in radiochemical analytical measurement of Np content. The invention uses236Pu is used as tracer; only phosphoric acid is added for enrichment and concentration, and the interference of other impurity ions is not introduced; the system is stable and easy to control, the prepared electroplating source has no self-absorption and high resolution, thereby improving the internal irradiation urine sample237Accuracy of radiochemical analytical measurement of Np content. The invention aims to set internal irradiation in urine sample237The radiochemical analytical measurement method for the Np content provides the basis for the line standard or national standard.
Drawings
FIG. 1 is a schematic flow chart of an exemplary method for determining the amount of Np-237 in a urine sample according to the present invention.
Detailed Description
Example 1: determination of the Np-237 content in urine samples
1) Taking 24h urine samples of 6 professional staff, each about 1.6L, adding 3mBq236Pu standard tracer and 8.89mBq237Np standard solution, then respectively adding 30mL of 15mol/L HNO3Solution and 25mL of 25 wt% H2O2The solution was covered with a petri dish and boiled separately on a hot plate for 30min (to prevent splashing). Cooling to 80-90 ℃, then respectively adding 5mL of phosphoric acid, adding ammonia water while stirring, adjusting the pH value to 8-9, and continuing stirring for 30 min.
2) Standing for 2 hr respectively, centrifuging to remove supernatant, and treating with 15mol/L HNO3Solution and 25 wt% H2O2The solution dissolves the precipitate and is heated until it is nearly dry and a white residue is formed.
3) Respectively dissolving the white residue by using 20-30mL of 3mol/L nitric acid, adding 0.5mL of 2mol/L hydroxylamine hydrochloride solution, 0.5mL of 1mol/L ferrous ammonium sulfate solution and 0.5mL of 4mol/L sodium nitrite solution, and uniformly stirring to fully complete the reaction.
4) Passing the solution obtained in step 3) through a trialkyl methyl ammonium chloride (TEVA) chromatographic column prepared in advance at normal temperature, washing the original beaker with 10mL of a 3mol/L nitric acid solution, and passing the washing solution through the chromatographic column.
5) And washing the chromatographic column by using 30mL of 8mol/L nitric acid solution and 30mL of 9mol/L hydrochloric acid solution respectively to remove interference elements such as U, Th and the like.
6) Desorbing the neptunium by using 15mL of 0.1mol/L hydrochloric acid-0.05 mol/L hydrofluoric acid mixed solution respectively, collecting desorption solution in a beaker, and placing the beaker on an electric heating plate to evaporate slowly (prevent splashing).
7) The electroplating adopts an electrodeposition mode, the residues obtained in the step 6) are dissolved by 10mL0.1mol/L ammonium sulfate solution for 3 times respectively, and are transferred into an electrodeposition tank with the current density of 600-2And (3) performing electrodeposition for 1h, adding 1mL of ammonia water before termination, continuing electrodeposition for 1min, cutting off a power supply, discarding an electrodeposition solution, and washing the electroplated sheet by using water and absolute ethyl alcohol in sequence.
8) Drying each electroplating piece under an infrared lamp, burning for 1-3min at 400 ℃ on an electric furnace, and then placing each electroplating piece in a low-background alpha spectrum meter for measurement, wherein the measurement results are shown in table 1.
TABLE 1 determination of the content of Np-237 in urine samples
As can be seen from the results in table 1:237the recovery rate of the Np measurement is 86.8 +/-3.68%, the precision is 4.24%, and the relative error is less than 15%, which shows that the analysis method is stable and accurate.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (10)
1. A method for determining the content of Np-237 in a urine sample, which is characterized by comprising the following steps:
(1) sample pretreatment: adding urine sample236Pu tracer, adding nitric acid and hydrogen peroxide, and heating to slightly boil to digest the urine sample;
(2) coprecipitation pre-concentration: cooling the urine sample, adding phosphoric acid to adjust the pH value, stirring until the urine sample is fully precipitated, standing, centrifuging, dissolving the precipitate by using nitric acid and hydrogen peroxide, and heating until the urine sample is nearly dry and is white residue;
(3) adjusting the valence state: dissolving the white residue with nitric acid, adding hydroxylamine hydrochloride and Fe2+And adjusting the valence state of Np to Np (IV) by sodium nitrite;
(4) separation and purification: loading trialkyl methyl ammonium chloride chromatographic powder into a chromatographic column, washing the chromatographic column by nitric acid, loading the solution obtained in the step (3), washing the chromatographic column by nitric acid solution and hydrochloric acid solution to remove U and Th, and desorbing Np by using hydrochloric acid-hydrofluoric acid mixed solution to obtain Np eluent;
(5) preparing a measurement source: preparing an Np measuring source by using an electrodeposition method for the Np eluent obtained in the step (4);
(6) measurement: and (4) placing the Np measurement source prepared in the step (5) into an alpha spectrometer for measurement.
2. The method for measuring according to claim 1, wherein: in the step (1), the concentrations of the nitric acid and the hydrogen peroxide are respectively 12-16mol/L and 20-30 wt%, and the time for micro-boiling digestion of the urine sample is 0.5-2 h.
3. The method for measuring according to claim 1, wherein: in the step (2), the pH is adjusted to 8-9, and the standing time is 2-12 h.
4. The method for measuring according to claim 1, wherein: in the step (2), the concentrations of the nitric acid and the hydrogen peroxide are respectively 12-16mol/L and 20-30 wt%.
5. The method for measuring according to claim 1, wherein: in the step (2), the heating to be nearly dry is heating to remove 85-95% of water.
6. The method for measuring according to claim 1, wherein: in the step (3), the nitric acid, the hydroxylamine hydrochloride and the Fe2 +And the concentration of sodium nitrite is 2.5-4.5mol/L, 1-3mol/L, 0.5-1.5mol/L and 3-5mol/L respectively.
7. The method for measuring according to claim 1, wherein: and (4) filling the trialkyl methyl ammonium chloride chromatographic powder into a chromatographic column by adopting a dry method for filling the column.
8. The method for measuring according to claim 1, wherein: in the step (4), the chromatographic column is washed by 7.5-8.5mol/L nitric acid solution and 8.5-9.5mol/L hydrochloric acid solution in sequence, and the concentrations of hydrochloric acid and hydrofluoric acid in the hydrochloric acid-hydrofluoric acid mixed solution are 0.08-0.12mol/L and 0.02-0.08mol/L respectively.
9. The method for measuring according to claim 1, wherein: in the step (5), the Np measuring source is prepared by electroplating for 0.5-2h under a certain current by using an electrodeposition method to prepare the Np measuring source, namely a sample source prepared by using an ammonium sulfate electrolyte solution, a stainless steel sheet as a cathode and a platinum wire as an anode.
10. The method for measuring according to claim 1, wherein: in the step (6), the alpha spectrum analyzer is a low background alpha spectrum analyzer.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014380A (en) * | 2012-12-17 | 2013-04-03 | 中国原子能科学研究院 | Method for separating neptunium from uranium product by TEVA-UTEVA extraction chromatographic column |
| CN111830119A (en) * | 2020-07-27 | 2020-10-27 | 广西大学 | A kind of242Pu calibration237Np measuring method |
| CN113311465A (en) * | 2021-04-08 | 2021-08-27 | 中国辐射防护研究院 | Combined analysis method for content of Pu isotope and Np-237 in sample |
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