CN117434575A - In waste water 230 Th analysis method - Google Patents
In waste water 230 Th analysis method Download PDFInfo
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- CN117434575A CN117434575A CN202311172869.XA CN202311172869A CN117434575A CN 117434575 A CN117434575 A CN 117434575A CN 202311172869 A CN202311172869 A CN 202311172869A CN 117434575 A CN117434575 A CN 117434575A
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- 239000002351 wastewater Substances 0.000 title claims abstract description 45
- 238000004458 analytical method Methods 0.000 title claims description 20
- 239000000523 sample Substances 0.000 claims abstract description 36
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000000694 effects Effects 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 20
- 229920005989 resin Polymers 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000004070 electrodeposition Methods 0.000 claims abstract description 12
- 230000001105 regulatory effect Effects 0.000 claims abstract description 12
- 239000000700 radioactive tracer Substances 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000003795 desorption Methods 0.000 claims abstract description 7
- 239000012488 sample solution Substances 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 230000004913 activation Effects 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005485 electric heating Methods 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 230000008020 evaporation Effects 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 claims description 9
- 229910052776 Thorium Inorganic materials 0.000 claims description 9
- 238000007747 plating Methods 0.000 claims description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000007900 aqueous suspension Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000003456 ion exchange resin Substances 0.000 claims description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 12
- 229910052770 Uranium Inorganic materials 0.000 description 10
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 10
- 230000007613 environmental effect Effects 0.000 description 7
- 238000005272 metallurgy Methods 0.000 description 7
- 238000005065 mining Methods 0.000 description 7
- 238000012544 monitoring process Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 230000005855 radiation Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000005067 remediation Methods 0.000 description 2
- 150000001218 Thorium Chemical class 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000002659 electrodeposit Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003904 radioactive pollution Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012085 test solution 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
- 238000012418 validation experiment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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
- G01T1/167—Measuring radioactive content of objects, e.g. contamination
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
-
- 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
- G01T1/18—Measuring radiation intensity with counting-tube arrangements, e.g. with Geiger counters
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/36—Measuring spectral distribution of X-rays or of nuclear radiation spectrometry
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- High Energy & Nuclear Physics (AREA)
- Molecular Biology (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for treating wastewater 230 A method of analyzing Th comprising: (1) taking a wastewater sample, and adding a corresponding amount of nitric acid; (2) Adding to the sample to be tested 229 Th is used as a tracer; (3) preparation and activation of a resin column; (4) passing the sample solution obtained in the step (2) through a resin column; (5) Adding concentrated sulfuric acid into the desorption solution obtained in the step (4), and placing the solution on an electric heating plate for drying by evaporation; (6) Adding distilled water into the evaporated sample, adding concentrated sulfuric acid, stirring uniformly, and regulating the pH of the solution by using ammonia water; (7) Pouring into an electrodeposition tank, switching on a power supply, adding ammonia water, continuing electrodeposition for 1-3min, switching off the power supply, taking out a plated sheet, washing with water and absolute ethyl alcohol, airing, numbering, and measuring; (8) Placing the plated sheet obtained in the step (7)Counting and measuring Th in an alpha spectrometer; (9) Calculating the sample to be tested 230 Th activity concentration. The method of the invention can obtain higher 230 The full recovery rate of Th, better stability and high accuracy.
Description
Technical Field
The invention belongs to the technical field of radiation environment monitoring, and particularly relates to a method for treating wastewater 230 Analysis method of Th.
Background
In recent years, with development and utilization of mineral resources, the risk of migration of natural radionuclides in minerals to the surrounding environment is caused, and a large amount of radionuclides with complex components are generated in process wastewater generated in uranium mining and metallurgy operation, shutdown, retirement and environment remediation processes, wherein Th-230 is discharged into a nearby environmental water body in the form of uranium mining and metallurgy wastewater. Th-230 belongs to an extremely toxic alpha nuclide with long half-life (T 1/2 =75200a), will exist in the environment for a long period. The prior researches find that Th-230/Th-232 can be used as a tracing factor of uranium pollution, and can better trace the periphery of uranium mining areasEnvironmental sources and levels of uranium contamination. Therefore, the method has high importance on tracing in the process and influence on the environment, and the enhancement of monitoring of Th-230 in the environmental water is particularly important for judging whether the environmental water is polluted by radionuclides, and grasping the pollution range, the severity and other information after the environmental water is polluted.
The ecological environment department of China also very important looks at monitoring of thorium and isotopes thereof in facility wastewater, in 2020, the country has exported a series of standards and regulations to standardize environmental protection in the industry, and the GB 23727-2020 "uranium mining and metallurgy radiation protection and radiation environmental protection regulations" explicitly indicates that "uranium mining and metallurgy with symbiotic thorium should also prevent and treat radioactive pollution of thorium series nuclides", wherein: the discharge concentration of Th-230 at the wastewater discharge port should not exceed 1.85Bq/L. Therefore, the measurement of Th-230 activity concentration in wastewater is required.
At present, the chemical content of total Th is mainly measured in China, the focus on Th-230 is less, the analysis method of Th isotopes and related research are less, and related analysis methods and standards are not released temporarily in China and internationally (the draft of the American society for materials and experiments for testing and materials is being compiled for a novel test method for rapidly radiochemically measuring thorium isotopes in water, and the analysis method and standards are not released). With the importance of the national environmental protection, the requirements on a monitoring system are higher and higher, and a complete analysis method of Th-230 in wastewater is established by developing the research of the analysis method of Th-230 in wastewater, so that technical support is provided for the wastewater monitoring in the uranium mining metallurgy daily monitoring and retired environment remediation stage.
Disclosure of Invention
In view of the drawbacks of the prior art, an object of the present invention is to provide a method for treating wastewater 230 Th analysis method, by which a relatively high level can be obtained 230 The full recovery rate of Th, better stability and high accuracy.
In order to achieve the above purpose, the invention adopts the technical scheme that: in waste water 230 A method of analyzing Th comprising the steps of:
(1) Taking a wastewater sample, adding a corresponding amount of nitric acid, and regulating the solution to be a 3-10mol/L nitric acid system;
(2) Adding to the sample to be tested 229 Th is used as a tracer;
(3) Preparing and activating a resin column;
(4) The sample solution obtained in the step (2) passes through a resin column, is leached by 3-10mol/L nitric acid, then is subjected to thorium desorption by 3-12mol/L hydrochloric acid, and is collected in a beaker;
(5) Adding 0.1-10mL of concentrated sulfuric acid into the desorption solution obtained in the step (4), and placing the solution on an electric heating plate for drying by evaporation;
(6) Adding distilled water into the evaporated sample, adding 0.1-10mL of concentrated sulfuric acid, uniformly stirring, and regulating the pH of the solution to 1.0-5.0 by using ammonia water;
(7) Pouring into an electrodeposition tank, switching on a power supply, regulating the current to 0.5-2.5A, adding ammonia water after the current is electrified for 30-200min, continuing electrodeposition for 1-3min, switching off the power supply, taking out a plating sheet, washing with water and absolute ethyl alcohol, airing, numbering, and measuring;
(8) Putting the plated sheet obtained in the step (7) into an alpha spectrometer for counting and measuring Th;
(9) According to 229 Th、 230 Th count 229 Th activity, calculating the measured sample 230 Th activity concentration.
Further, before the waste water sample is taken in the step (1), the waste water sample is acidified by nitric acid until the pH value is less than 2.
Further, in the step (1), 5-100mL of wastewater sample is taken, and corresponding amount of nitric acid is added according to the ratio of 1:1.
Further, in step (2), the tracer 229 The activity of Th is 0.03-1.00Bq.
Further, in the step (3), the preparation and activation method of the resin column comprises the following steps: the ion exchange resin is soaked in absolute ethyl alcohol, stirred continuously, suspended particles are removed by a water suspension method, then soaked in nitric acid, stored in a glass bottle for standby, packed by a wet method, washed by 3-12mol/L hydrochloric acid, and balanced by 3-10mol/L nitric acid for standby.
Further, in the step (3), the specification of the resin column is phi 8mm, the height of the column is 80-300mm, the volume of 3-12mol/L hydrochloric acid used for cleaning the resin is 20mL, and the volume of 3-10mol/L nitric acid used for balancing the resin is 20-30mL.
Further, in the step (4), the prepared sample solution is loaded on the column twice, the volume of 3-10mol/L nitric acid used for leaching the matrix is 60mL, and the volume of 3-12mol/L hydrochloric acid used for desorbing Th is 60-80mL.
Further, in the step (7), the volume of the electrodeposition bath is 20cm 3 The power supply is a direct-current stable power supply, the anode is a platinum electrode, and the plating sheet is a stainless steel wafer.
Further, the stainless steel wafer is washed with tap water before use, then with distilled water, and is disposable.
Further, in step (9), according to 229 Th、 230 Th count 229 Th activity, calculating the measured sample 230 The formula for Th activity concentration is as follows:
A 0 ＝(A 1 N 0 )/(N 1 v) formula (1)
In formula (1):
A 0 -in the sample 230 Radioactivity concentration of Th, bq/L;
A 1 -in the tracer 229 Radioactivity concentration of Th, bq/L;
N 0 —— 230 th peak position corresponds to net count rate in region of interest, S -1 ；
N 1 —— 229 Th peak position corresponds to net count rate in region of interest, S -1 ；
V-the volume used to analyze the sample, L.
The invention has the following effects: the invention provides a method for treating wastewater 230 Th analysis method can obtain relatively high level 230 The full recovery rate of Th, better stability and high accuracy; the method is experimentally verified through an actual aerosol sample, and the result shows that the method can be applied to daily environment monitoring as a recommended method.
Drawings
FIG. 1Is a waste water in the specific embodiment of the invention 230 Flow chart of analysis method of Th.
Detailed Description
The invention is further described below with reference to the detailed description and the accompanying drawings.
As shown in steps S1-S9 of FIG. 1, the invention provides a method for treating wastewater 230 The analysis method of Th comprises the following steps:
(1) Collecting a wastewater sample, and acidifying with nitric acid until the pH value is less than 2;
(2) Taking 5-100mL of wastewater sample, adding a proper amount of nitric acid according to the ratio of 1:1, and regulating the solution into a 3-10mol/L nitric acid system;
(3) Adding a certain activity to the sample to be tested 229 Th acts as a tracer, said tracer 229 The activity of Th is 0.03-1.00Bq;
(4) Preparation and activation of a resin column: soaking ion exchange resin in absolute ethanol for 24h, stirring, removing suspended particles by using a water suspension method, soaking in 0.1mol/L nitric acid, and storing in a glass bottle for later use; filling a column by a wet method, cleaning the resin by 3-12mol/L hydrochloric acid, and balancing the resin by 3-10mol/L nitric acid for later use;
(5) The sample solution obtained in the step (3) passes through a resin column, is leached by 3-10mol/L nitric acid, then is subjected to thorium desorption by 3-12mol/L hydrochloric acid, and is collected in a 100mL beaker;
(6) Adding 0.1-10mL of concentrated sulfuric acid into the desorption solution obtained in the step (5), and placing the solution on an electric heating plate for drying by evaporation;
(7) Adding 10mL of distilled water into the evaporated sample, adding 0.1-10mL of concentrated sulfuric acid, uniformly stirring, and regulating the pH of the solution to 1.0-5.0 by using concentrated ammonia water;
(8) Pouring into an electrodeposition tank, switching on a power supply, regulating the current to 0.5-2.5A, adding ammonia water after the current is electrified for 30-200min, continuing electrodeposition for 1-3min, switching off the power supply, taking out a plating sheet, washing with water and absolute ethyl alcohol, airing, numbering, and measuring;
(9) Putting the plated sheet obtained in the step (8) into an alpha spectrometer for counting and measuring Th;
(10) According to 229 Th、 230 Th count 229 Th activity, calculating the measured sample 230 Th activity concentration.
For the actual wastewater sample to be tested, according to the measurement 229 Th、 230 Th count 229 Th activity can be calculated in the wastewater to be tested according to the formula (1) 230 Th activity concentration:
A 0 ＝(A 1 N 0 )/(N 1 v) formula (1)
In formula (1):
A 0 -in the sample 230 Radioactivity concentration of Th, bq/L;
A 1 -in the tracer 229 Radioactivity concentration of Th, bq/L;
N 0 —— 230 th peak position corresponds to net count rate in region of interest, S -1 ；
N 1 —— 229 Th peak position corresponds to net count rate in region of interest, S -1 ；
V-the volume used to analyze the sample, L.
Description of the preferred embodiments
And collecting a wastewater sample.
The specific operation method of the analysis and determination is as follows:
(1) Preparing 6 small beakers, and accurately transferring 10mL uranium mining and metallurgy wastewater samples in each beaker;
(2) Adding 10mL of concentrated nitric acid into each sample, regulating the solution to be 3-10mol/L of nitric acid system, and uniformly stirring;
(3) 1.0mL of each 229 A Th tracer (-0.1 Bq/mL) is stirred uniformly for standby;
(4) Loading and activating a resin column: weighing a certain amount of ion exchange resin, soaking in absolute ethanol, continuously stirring, removing suspended fine powder by using a water suspension method, soaking in nitric acid, and storing in a glass bottle for standby.
(5) Activation of the resin column: the packed column was rinsed with 20mL of hydrochloric acid (9 mol/L) and then equilibrated with 20-30mL of 3-10mol/L nitric acid for further use.
(6) The pretreated sample solution is loaded on the column for two times, and after the whole test solution flows out, 60mL of nitric acid is used for leaching impurities for four times;
(7) Thorium was eluted with 60mL hydrochloric acid and collected in a 100mL small beaker.
(8) Adding 0.1-10mL of concentrated sulfuric acid into the separated and purified thorium solution, steaming on an electric hot plate until the thorium solution is nearly dry, taking down a beaker, and slightly cooling;
(9) Adding 10mL of deionized water for dissolution, adding 0.1-10mL of concentrated sulfuric acid, stirring uniformly, and adding concentrated ammonia water to adjust the pH to 1.0-5.0;
(10) Transferring all the solution into an electrodeposition tank, switching on a power supply, regulating the current to 0.5-2.5A, and continuously electrodepositing for 120min;
(11) Adding a plurality of drops of ammonia water into the electrodeposition tank, continuing to electrodeposit for 1-3min, cutting off the power supply, taking out the plated sheet, washing with water and absolute ethyl alcohol in sequence, airing, numbering and preparing for measurement;
(12) Putting the plated sheet into an alpha spectrometer for measurement;
(13) According to the nuclide to be measured 230 Th (Th) 229 Counting of Th tracers 229 Calculation of known Activity of Th in Water sample to be measured 230 Activity concentration of Th.
The results of validation experiments for Th-230 analysis in real uranium metallurgy wastewater are shown in Table 1.
TABLE 1 in wastewater 230 Th content
According to the experimental data analysis of Table 1, the overall conversion recovery rate is 88.5% -94.9%, and the average value is 91.95 + -4.6%. In waste water 230 The Th content is 19.55+ -1.38 Bq/L.
The above-described embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or with 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 are intended to be encompassed within the scope of the invention.
Claims (10)
1. In waste water 230 A method of analyzing Th comprising the steps of:
(1) Taking a wastewater sample, adding a corresponding amount of nitric acid, and regulating the solution to be a 3-10mol/L nitric acid system;
(2) Adding to the sample to be tested 229 Th is used as a tracer;
(3) Preparing and activating a resin column;
(4) The sample solution obtained in the step (2) passes through a resin column, is leached by 3-10mol/L nitric acid, then is subjected to thorium desorption by 3-12mol/L hydrochloric acid, and is collected in a beaker;
(5) Adding 0.1-10mL of concentrated sulfuric acid into the desorption solution obtained in the step (4), and placing the solution on an electric heating plate for drying by evaporation;
(6) Adding distilled water into the evaporated sample, adding 0.1-10mL of concentrated sulfuric acid, uniformly stirring, and regulating the pH of the solution to 1.0-5.0 by using ammonia water;
(7) Pouring into an electrodeposition tank, switching on a power supply, regulating the current to 0.5-2.5A, adding ammonia water after the current is electrified for 30-200min, continuing electrodeposition for 1-3min, switching off the power supply, taking out a plating sheet, washing with water and absolute ethyl alcohol, airing, numbering, and measuring;
(8) Putting the plated sheet obtained in the step (7) into an alpha spectrometer for counting and measuring Th;
(9) According to 229 Th、 230 Th count 229 Th activity, calculating the measured sample 230 Th activity concentration.
2. In a waste water according to claim 1 230 The analysis method of Th is characterized in that before the wastewater sample is taken in the step (1), the wastewater sample is acidified by nitric acid until the pH value is less than 2.
3. In a waste water according to claim 2 230 The analysis method of Th is characterized in that in the step (1), 5-100mL of wastewater sample is taken, and corresponding amount of nitric acid is added according to the ratio of 1:1.
4. In a waste water according to claim 1 230 A method for analyzing Th, characterized in that in step (2), the tracer is used 229 The activity of Th is 0.03-1.00Bq.
5. In a waste water according to claim 1 230 The analysis method of Th is characterized in that in the step (3), the preparation and activation method of the resin column comprises the following steps: the ion exchange resin is soaked in absolute ethyl alcohol, stirred continuously, suspended particles are removed by a water suspension method, then soaked in nitric acid, stored in a glass bottle for standby, packed by a wet method, washed by 3-12mol/L hydrochloric acid, and balanced by 3-10mol/L nitric acid for standby.
6. In a waste water according to claim 5 230 The analysis method of Th is characterized in that in the step (3), the specification of the resin column is phi 8mm, the height of the column is 80-300mm, the volume of 3-12mol/L hydrochloric acid used for cleaning the resin is 20mL, and the volume of 3-10mol/L nitric acid used for balancing the resin is 20-30mL.
7. In a waste water according to claim 1 230 The analysis method of Th is characterized in that in step (45), the prepared sample solution is loaded in two columns, the volume of 3-10mol/L nitric acid used for leaching the matrix is 60mL, and the volume of 3-12mol/L hydrochloric acid used for desorbing Th is 60-80mL.
8. In a waste water according to claim 1 230 A method for analyzing Th, characterized in that in step (7), the volume of the electrodeposition bath is 20cm 3 The power supply is a direct-current stable power supply, the anode is a platinum electrode, and the plating sheet is a stainless steel wafer.
9. In a waste water according to claim 8 230 The analysis method of Th is characterized in that the stainless steel wafer is washed with tap water before use, then with distilled water, and is disposable.
10. In a waste water according to claim 1 230 A method for analyzing Th, characterized by comprising the step (9) of 229 Th、 230 Th count 229 Th activity, calculating the measured sample 230 The formula for Th activity concentration is as follows:
A 0 ＝(A 1 N 0 )/(N 1 v) formula (1)
In formula (1):
A 0 -in the sample 230 Radioactivity concentration of Th, bq/L;
A 1 -in the tracer 229 Radioactivity concentration of Th, bq/L;
N 0 —— 230 th peak position corresponds to net count rate in region of interest, S -1 ；
N 1 —— 229 Th peak position corresponds to net count rate in region of interest, S -1 ；
V-the volume used to analyze the sample, L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311172869.XA CN117434575A (en) | 2023-09-12 | 2023-09-12 | In waste water 230 Th analysis method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311172869.XA CN117434575A (en) | 2023-09-12 | 2023-09-12 | In waste water 230 Th analysis method |
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| Publication Number | Publication Date |
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| CN117434575A true CN117434575A (en) | 2024-01-23 |
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