CN112683829A - Sampling detection method for corrosion products in nuclear power plant water sample - Google Patents
Sampling detection method for corrosion products in nuclear power plant water sample Download PDFInfo
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- CN112683829A CN112683829A CN202110157890.7A CN202110157890A CN112683829A CN 112683829 A CN112683829 A CN 112683829A CN 202110157890 A CN202110157890 A CN 202110157890A CN 112683829 A CN112683829 A CN 112683829A
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- filter membrane
- corrosion products
- nuclear power
- detection method
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- 230000007797 corrosion Effects 0.000 title claims abstract description 63
- 238000005260 corrosion Methods 0.000 title claims abstract description 63
- 238000005070 sampling Methods 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000001514 detection method Methods 0.000 title claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 73
- 230000029087 digestion Effects 0.000 claims abstract description 26
- 229920002678 cellulose Polymers 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 17
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 39
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 238000005485 electric heating Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000001479 atomic absorption spectroscopy Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 229910052742 iron Inorganic materials 0.000 description 10
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- -1 cellulose nitrate ester Chemical class 0.000 description 4
- 239000000020 Nitrocellulose Substances 0.000 description 3
- 229920001220 nitrocellulos Polymers 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- GPFIZJURHXINSQ-UHFFFAOYSA-N acetic acid;nitric acid Chemical compound CC(O)=O.O[N+]([O-])=O GPFIZJURHXINSQ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011217 control strategy Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of monitoring of corrosion products of nuclear power plants, and particularly discloses a sampling detection method of corrosion products in a water sample of a nuclear power plant. According to the method, the corrosion product is intercepted by the mixed cellulose ester filter membrane, and the method that the strong acid is heated to the micro-boiling state is adopted, so that the corrosion product intercepted by the filter membrane and the filter membrane can be completely dissolved, meanwhile, the splashing of the solution is avoided, the loss of the corrosion product is effectively reduced, and the accuracy of the content determination of the corrosion product is improved; the method is simple to operate, the used equipment and reagents are completely from a laboratory, the method is convenient and easy to obtain, the problem of complex filter membrane digestion steps in the prior art is effectively solved, and the method is easy to popularize and apply.
Description
Technical Field
The invention belongs to the technical field of monitoring of corrosion products of nuclear power plants, and particularly relates to a sampling detection method of corrosion products in a water sample of a nuclear power plant.
Background
The deposition amount of corrosion products in the steam generator, which is a key device of a nuclear power plant, can be used for evaluating the performance of the heat transfer pipe and reflecting the effectiveness of the current chemical control strategy. In order to monitor the corrosion condition of the steam generator, a nuclear power plant generally uses a suspended solid sampling device to continuously sample the blowdown and feed water of the steam generator, a filter membrane is arranged in the suspended solid sampling device, corrosion products are intercepted on the filter membrane, and then the collected filter membrane is analyzed for corrosion elements such as iron.
In the process of sampling and analyzing the corrosion products of the steam generator, the problem that the filter membrane and the intercepted corrosion products are difficult to separate exists, at present, the filter membrane and the corrosion products are subjected to acid dissolution together, the material of the filter membrane is generally cellulose nitrate ester, and the filter membrane is insoluble in acid at normal temperature, in the prior art, concentrated hydrochloric acid and concentrated nitric acid are prepared into aqua regia according to the volume ratio of 3:1, and then the filter membrane is stirred and dissolved in the aqua regia under the heating condition, and the treatment method has obvious defects: although the aqua regia can completely dissolve corrosion products such as iron and the like intercepted by the sampling filter membrane, the filter membrane made of cellulose nitrate ester cannot be completely dissolved, and a fine flocculent precipitate can be formed, the precipitate can adsorb iron elements, and the complete recovery of the iron elements is not easily ensured through filtration or repeated elution, so that the accuracy of measurement is influenced; in addition, the aqua regia is easy to splash in the heating and stirring process, the corrosivity of the aqua regia is very strong, the safety of operators is threatened, and the splashing of the aqua regia can cause the loss of iron elements in a sample and also can influence the accuracy of measurement.
CN109115709A discloses a digestion method of a filter membrane entrapping iron and a determination method of iron content in cooling water of a nuclear power plant. This patent forms the acidic environment of a high temperature high pressure through sealed heating mode, promotes digesting of filter membrane, and this kind of method can effectively improve the degree of digesting of filter membrane, also can avoid splashing of acidic digestion liquid to make iron content measurement result more accurate, nevertheless have following defect: the heating temperature needs to be strictly controlled, the experimental environment is harsh, the operation process is complex, the cost is high, and the popularization and the application are difficult.
Disclosure of Invention
In order to solve the problems, the invention provides a sampling detection method for corrosion products in water samples of nuclear power plants, which can completely digest a filter membrane, has good safety, is simple to operate, has high accuracy of a determination result of the content of corrosion elements, and can be used for determining the corrosion products of water samples of a corrosion product collection system and other systems of the nuclear power plants.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
a sampling detection method for corrosion products in a water sample of a nuclear power plant comprises the steps of firstly intercepting the corrosion products in the water sample by adopting a mixed cellulose ester filter membrane, then placing the mixed cellulose ester filter membrane with the intercepted corrosion products in a strong acid solution, heating to obtain a digestion solution, and then measuring the content of corrosion metal ions in the digestion solution. The metal ions are iron ions and copper ions conventionally, and can be adjusted according to the components of the water sample of the system. In the method, the mixed cellulose ester filter membrane is used for replacing the existing cellulose nitrate filter membrane, the mixed cellulose ester filter membrane is a nitric acid-acetic acid mixed cellulose ester filter membrane, the filter membrane made of the mixed cellulose ester material has the characteristics of weak acid resistance, weak alkali resistance, neutral oil resistance and the like, can be completely dissolved by adopting strong acid heating, can not form flocculent precipitates to adsorb corrosive elements, effectively reduces the loss of corrosive products, and improves the accuracy of the measured metal ion content.
Preferably, the strong acid solution is a mixed solution of concentrated nitric acid and concentrated hydrochloric acid. The mixed solution of concentrated nitric acid and concentrated hydrochloric acid can quickly and completely dissolve the mixed cellulose ester filter membrane and corrosion products intercepted by the filter membrane, and cannot interfere with subsequent analysis.
Further, the mass fraction of the concentrated nitric acid is 64-68%, and the mass fraction of the concentrated hydrochloric acid is 34-38%.
Furthermore, in the strong acid solution, the volume ratio of the concentrated nitric acid to the concentrated hydrochloric acid is (1-1.5): 1. The formulated solution has reduced corrosivity compared to aqua regia.
Further, the heating temperature is 79-82 ℃. The temperature range can keep the concentrated nitric acid-concentrated hydrochloric acid mixed solution in a micro-boiling state, can ensure that the filter membrane is completely dissolved, can not cause the solution to splash, and effectively improves the safety and the accuracy of subsequent corrosion element analysis and measurement.
Further, in the strong acid solution, the volume ratio of the concentrated nitric acid to the concentrated hydrochloric acid is 1: 1; the heating temperature was 80 ℃.
Preferably, the pore size of the mixed cellulose ester filter membrane is 0.4-0.65 μm. The aperture of the mixed cellulose ester filter membrane is controlled, so that the interception of other fine impurities is reduced while the corrosion product is intercepted as completely as possible, the impurity content in the digestion solution is further reduced, and a high-quality sample is provided for subsequent analysis and measurement.
Preferably, the surface of the mixed cellulose ester filter membrane is smooth, the smooth surface can reduce the blockage of corrosion products on one hand, and on the other hand, the separation of the corrosion products and the filter membrane can be accelerated, the digestion difficulty is further reduced, the digestion time is greatly shortened, the solution is not required to be stirred or heated to a bumping state, and the corrosion products and the filter membrane can be quickly separated under a micro-boiling state.
Preferably, the mixed cellulose ester filter membrane used is Millibo HAWP 04700.
Preferably, the sampling detection method for corrosion products in the water sample of the nuclear power plant specifically comprises the following steps:
step one, enabling a water sample to flow through a mixed cellulose ester filter membrane (generally, the filter membrane is placed in a suspended solid sampling device, and then the suspended solid sampling device is placed in a flow pipeline of the water sample), so as to obtain the filter membrane for intercepting the corrosion products;
drying the filter membrane in an oven, drying the filter membrane in a dryer until the weight is constant, and weighing the filter membrane;
putting the weighed filter membrane into a beaker, and adding a strong acid solution;
opening the electric heating plate, setting the heating temperature, placing the beaker on the electric heating plate, and heating until the solution is boiled;
keeping the solution in a boiling state until the filter membrane is completely dissolved to obtain a digestion solution;
step six, closing the electric heating plate to cool the digestion solution to room temperature; transferring the digestion solution in the beaker to a volumetric flask, and fixing the volume;
and step seven, measuring the content of the corrosion metal ions in the digestion solution with constant volume by adopting an atomic absorption spectrometry.
The invention has the following beneficial effects:
1. the method selects the mixed cellulose ester filter membrane and adopts a strong acid heating mode (the strong acid is a concentrated nitric acid-concentrated hydrochloric acid mixed solution), so that the corrosion products intercepted by the filter membrane and the filter membrane can be completely dissolved, the generation of flocculent precipitates is avoided, the loss of the corrosion products is effectively reduced, and the accuracy of the content determination of the corrosion products is improved.
2. According to the invention, through a mode of heating to micro-boiling, the filter membrane is ensured to be completely dissolved and not to splash, the safety of the test is improved, the corrosion product loss caused by the splashing of the solution is also avoided, and the accuracy of the content determination of the corrosion product is further improved.
3. According to the invention, the smooth filter membrane is adopted, so that the blockage of the corrosion product is reduced, the accuracy of the content determination of the corrosion product is further improved, the separation difficulty of the corrosion product and the filter membrane is reduced, the digestion time is greatly shortened, the rapid separation of the corrosion product and the filter membrane can be realized by combining the micro-boiling state of the solution without auxiliary means such as stirring, the operation is simplified, and the safety is further improved.
4. The method is simple to operate, the used equipment and reagents are completely from a laboratory, the convenience and the easy availability are realized, the problem of complex filter membrane digestion steps in the prior art is effectively solved, and the method is easy to popularize and apply; and each step is strictly controlled by the method, so that the result of the content measurement of the corrosion product is accurate and reliable.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A sampling detection method for corrosion products in a nuclear power plant water sample needs equipment and reagents comprising: measuring flask, volumetric flask, beaker, graduated cylinder, electric heating plate, concentrated nitric acid, concentrated hydrochloric acid, dryer, oven, atomic absorption spectrometer; wherein the dryer and the weighing bottle are respectively used for drying, weighing and keeping constant weight after the filter membrane sampling; the electric heating plate is used for heating the solution in the filter membrane digestion process; the volumetric flask is used for constant volume after the filter membrane is digested, so that subsequent measurement and analysis are facilitated; concentrated nitric acid and concentrated hydrochloric acid are used as reagents required in the digestion process.
The sampling detection method for corrosion products in the water sample of the nuclear power plant specifically comprises the following steps:
placing a filter membrane in a suspended solid sampling device, and enabling a water sample to flow through the filter membrane in a sewage discharge pipeline of a steam generator of the suspended solid sampling device to obtain the filter membrane for intercepting corrosion products, wherein the model of the filter membrane is Milliko HAWP04700 (the aperture is 0.45um, and the smooth surface);
step two, placing the filter membrane in an oven for drying, then placing the filter membrane in a dryer for constant weight for 15 minutes, and then weighing;
putting the weighed filter membrane into a 100ml beaker, and adding 10ml of 65% high-purity nitric acid and 10ml of 35% concentrated hydrochloric acid;
step four, opening the electric heating plate, setting a heating mode, and setting the target temperature to be 80 ℃; placing the beaker on an electric heating plate, and heating until the beaker is slightly boiled;
keeping the solution in a micro-boiling state until the filter membrane is completely dissolved, and keeping 15ml +/-5 ml of the solution in the beaker to obtain a clear and transparent digestion solution without precipitates;
step six, closing the electric heating plate to cool the digestion solution to room temperature; transferring the digestion solution in the beaker to a 50ml volumetric flask, washing the inner wall of the beaker by using a small amount of ultrapure water, and fixing the volume of the obtained sample to 50 ml;
and step seven, measuring the contents of iron ions and copper ions in the digestion solution with constant volume by adopting an atomic absorption spectrometry.
This detailed description is to be construed as illustrative only and is not to be taken as limiting the invention, as any changes that may be made by a person skilled in the art after reading the present specification will be protected by the patent laws within the scope of the appended claims.
Claims (10)
1. A sampling detection method for corrosion products in a nuclear power plant water sample is characterized by comprising the following steps: firstly, intercepting corrosion products in a water sample by adopting a mixed cellulose ester filter membrane, then placing the mixed cellulose ester filter membrane intercepted with the corrosion products in a strong acid solution, heating to obtain a digestion solution, and then measuring the content of corrosion metal ions in the digestion solution.
2. The sampling detection method for corrosion products in water samples of nuclear power plants according to claim 1, characterized in that: the strong acid solution is a mixed solution of concentrated nitric acid and concentrated hydrochloric acid.
3. The sampling detection method for corrosion products in water samples of nuclear power plants according to claim 2, characterized in that: the mass fraction of the concentrated nitric acid is 65-68%, and the mass fraction of the concentrated hydrochloric acid is 35-38%.
4. The sampling detection method for corrosion products in water samples of nuclear power plants according to claim 3, characterized in that: in the strong acid solution, the volume ratio of the concentrated nitric acid to the concentrated hydrochloric acid is (1-1.5): 1.
5. The sampling detection method for corrosion products in water samples of nuclear power plants according to claim 4, characterized in that: the heating temperature is 79-82 ℃.
6. The sampling detection method for corrosion products in water samples of nuclear power plants according to claim 5, characterized in that: in the strong acid solution, the volume ratio of concentrated nitric acid to concentrated hydrochloric acid is 1: 1; the heating temperature was 80 ℃.
7. The sampling detection method for corrosion products in water samples of nuclear power plants according to claim 1, characterized in that: the aperture of the mixed cellulose ester filter membrane is 0.4-0.65 μm.
8. The sampling detection method for corrosion products in water samples of nuclear power plants according to claim 1, characterized in that: the surface of the mixed cellulose ester filter membrane is smooth.
9. The sampling detection method for corrosion products in water samples of nuclear power plants according to claim 1, characterized in that: the model of the mixed cellulose ester filter membrane adopted is Millibo HAWP 04700.
10. The sampling detection method for corrosion products in water samples of nuclear power plants according to any one of claims 1 to 9, characterized in that: the method specifically comprises the following steps:
step one, enabling a water sample to flow through a mixed cellulose ester filter membrane to obtain a filter membrane retaining the corrosion product;
drying the filter membrane in an oven, drying the filter membrane in a dryer until the weight is constant, and weighing the filter membrane;
putting the weighed filter membrane into a beaker, and adding a strong acid solution;
opening the electric heating plate, setting the heating temperature, placing the beaker on the electric heating plate, and heating until the solution is boiled;
keeping the solution in a boiling state until the filter membrane is completely dissolved to obtain a digestion solution;
step six, closing the electric heating plate to cool the digestion solution to room temperature; transferring the digestion solution in the beaker to a volumetric flask, and fixing the volume;
and step seven, measuring the content of the corrosion metal ions in the digestion solution with constant volume by adopting an atomic absorption spectrometry.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110157890.7A CN112683829A (en) | 2021-02-05 | 2021-02-05 | Sampling detection method for corrosion products in nuclear power plant water sample |
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| CN202110157890.7A CN112683829A (en) | 2021-02-05 | 2021-02-05 | Sampling detection method for corrosion products in nuclear power plant water sample |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109115709A (en) * | 2018-10-23 | 2019-01-01 | 岭澳核电有限公司 | Retention has the measuring method of iron content in the digestion procedure and nuclear power plant's cooling water of the filter membrane of iron |
| CN210071429U (en) * | 2019-04-11 | 2020-02-14 | 岭东核电有限公司 | Suspended iron sampling system applied to secondary loop of nuclear power station |
-
2021
- 2021-02-05 CN CN202110157890.7A patent/CN112683829A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109115709A (en) * | 2018-10-23 | 2019-01-01 | 岭澳核电有限公司 | Retention has the measuring method of iron content in the digestion procedure and nuclear power plant's cooling water of the filter membrane of iron |
| CN210071429U (en) * | 2019-04-11 | 2020-02-14 | 岭东核电有限公司 | Suspended iron sampling system applied to secondary loop of nuclear power station |
Non-Patent Citations (4)
| Title |
|---|
| 刘广山: "《海洋放射性核素测量方法》", 海洋出版社, pages: 233 * |
| 徐颖等: "多级大气颗粒物中超痕量铀的ＨＲ⁃ＩＣＰ⁃ＭＳ分析方法研究", 《中华放射医学与防护杂志》 * |
| 徐颖等: "多级大气颗粒物中超痕量铀的ＨＲ⁃ＩＣＰ⁃ＭＳ分析方法研究", 《中华放射医学与防护杂志》, vol. 37, no. 3, 31 March 2017 (2017-03-31), pages 213 - 214 * |
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Application publication date: 20210420 |