CN101483074B - Analysis method for sulphate pollution in nuclear power generating set starting process after large scale maitenance - Google Patents
Analysis method for sulphate pollution in nuclear power generating set starting process after large scale maitenance Download PDFInfo
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- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000004458 analytical method Methods 0.000 title claims abstract description 30
- 230000008569 process Effects 0.000 title claims description 42
- 229910021653 sulphate ion Inorganic materials 0.000 title 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 34
- 230000003647 oxidation Effects 0.000 claims abstract description 30
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 238000004088 simulation Methods 0.000 claims abstract description 18
- 230000005855 radiation Effects 0.000 claims abstract description 15
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical group OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 6
- 238000012360 testing method Methods 0.000 claims description 63
- 239000000446 fuel Substances 0.000 claims description 43
- 150000003839 salts Chemical class 0.000 claims description 40
- 241000196324 Embryophyta Species 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 28
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 18
- 238000013459 approach Methods 0.000 claims description 14
- 229910052717 sulfur Inorganic materials 0.000 claims description 14
- 239000011593 sulfur Substances 0.000 claims description 14
- 238000011835 investigation Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 10
- 238000012795 verification Methods 0.000 claims description 8
- 239000003344 environmental pollutant Substances 0.000 claims description 7
- 231100000719 pollutant Toxicity 0.000 claims description 6
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 6
- 235000009161 Espostoa lanata Nutrition 0.000 claims description 5
- 240000001624 Espostoa lanata Species 0.000 claims description 5
- 238000000429 assembly Methods 0.000 claims description 5
- 230000000712 assembly Effects 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004876 x-ray fluorescence Methods 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000003869 coulometry Methods 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 4
- 239000003729 cation exchange resin Substances 0.000 abstract 1
- 238000005115 demineralization Methods 0.000 abstract 1
- 230000002328 demineralizing effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 33
- 239000011347 resin Substances 0.000 description 18
- 229920005989 resin Polymers 0.000 description 18
- 239000000463 material Substances 0.000 description 10
- 239000002915 spent fuel radioactive waste Substances 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 9
- 230000002285 radioactive effect Effects 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 238000007689 inspection Methods 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- 239000013067 intermediate product Substances 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 239000003921 oil Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 125000000542 sulfonic acid group Chemical group 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001983 electron spin resonance imaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000012208 gear oil Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
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- 229910001055 inconels 600 Inorganic materials 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
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- 239000004590 silicone sealant Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- 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
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses an analytical method of nuclear power unit nuclear plant train startup procedure-loop sulfate pollution after general overhaul, including detection experiment, laboratory simulation, oxidation experiments, startup procedure system experiments after overhauling of nuclear power plant unit, and then analyzing to obtain that intense radiation is in the reactor, oxygen-enriched in the water and cationic ion-exchange resin with benzenesulfonic acid group in the demineralization bed in the startup procedure of the nuclear power plant unit after the general overhaul, thereby causing the nuclear power unit nuclear plant train startup procedure-loop sulfate pollution after general overhaul. The method of the invention is exhaustive and can reveal the source of nuclear power unit nuclear plant train startup procedure-loop sulfate pollution after general overhaul.
Description
Technical field
The present invention relates to a kind of analytical approach of sulfate pollution, relate in particular to a kind of analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution.
Background technology
At present, in the nuclear power station operational process, regularly need carry out large repairs to unit, wherein, start-up course mainly comprises static exhaust, dynamic steps of exhausting is carried out in a loop after the overhaul, and the RCP main pump starts operation then, again a loop is added N
2H
4Every index of chemical platform is checked in deoxygenation then, and is qualified down in index, and the RCP system is continued to heat up.2004, the problem of one loop sulfate pollution has all taken place in the start-up course behind four major overhauls of Daya Gulf/mountain range Australia nuclear power, (this code is the major overhaul numbering at the L201/L102/D210/D110 of Daya Gulf/mountain range Australia nuclear power station, wherein, L201 represents the overhaul for the first time of No. two units of mountain range Australia nuclear power station, the 10th overhaul of unit of D110 Daya Bay nuclear power plant etc.) unloading phase of 4 major overhauls, because the sulfate pollution in a loop causes the overhaul critical path to incur loss through delay 121 hours altogether, detailed data sees Table 1.
One loop sulfate situation data gather the unloading phase of table 1L201/L102/D210/D110 overhaul
| Overhaul | Time | Reason is incured loss through delay in the overhaul path | Delay time at stop (h) | SO 4 2-Maximal value (μ g/Kg) |
| L201 | 2004.01.23 | Major loop SO 4 2-Content is higher, has exceeded unit and has been warming up to standard limit value more than 120 ℃ | 43 | 293 |
| L102 | 2004.03.14 | Do not exceed unit and be warming up to rule more than 120 ℃ | 6 | 99 |
| The model limit value, but judge because of waiting trend | ||||
| D210 | 2004.06.30 | Major loop SO 4 2-Content is higher, has exceeded unit and has been warming up to standard limit value more than 120 ℃ | 41 | 278 |
| D110 | 2004.11.03 | Major loop SO 4 2-Content is higher, has exceeded unit and has been warming up to standard limit value more than 120 ℃ | 31 | 270.3 |
The introduction that " the PWR one loop water chemistry guide rule " published according to U.S. EPRI is the 4th edition: " under the experimental study condition, SO
4 2-The danger that causes stainless steel stress-corrosion cracking (SCC) is not second to Cl
-Just because of SO
4 2-This harm, this guide rule third edition is with SO
4 2-Formally include controlling index in ".There is the inefficacy of ALLOY6OO heat-transfer pipe primary side of the steam generator of 2 PWR power plant to break relevant with the existence of sulfide.One of them occurs in during the overhaul, and one occurs in the power run duration.Power run duration, low amounts of resin enter a circuit system promptly to be enough in system to generate and to cause the break SO of (IGA) of intercrystalline corrosion
4 2-Concentration.1994, " control rod drive mechanisms (CRD) intercrystalline corrosion fracture accident (IGA) took place in Spain JOSE CABRERA nuclear power plant, and the fracture material is that ALLOY600 contains gold.Reason is this power plant 1980 and secondary generation resin leakage incident (40L and 200L) in 1981, makes a loop SO
4 2-Concentration raises and pH reduces ".
Just because of the harmfulness of sulfate radical, strict regulations have been given for reactor coolant loop (or RRA) among the D-TD/GNP/311 of Daya Bay nuclear power plant's " chemistry and radiochemistry technical manual ", for fear of producing a loop corrosion risk, the major loop SO of listed 4 overhauls in the table 1
4 2-When unusual all must stage of normal cold shut with SO
4 2-Handle qualified and then shutdown transition in the middle of single-phase.Processing procedure has greatly been incured loss through delay the overhaul critical path.Bring enormous economic loss to the power station.
EDF adds up demonstration (select from 2004 EDF/DNMC chemistry AC material) to the sulfate radical abnormal conditions in past 10 years (1994～2003): 30% unit is restarted the stage at major overhaul one loop SO was taken place
4 2-Pollute and content supergauge limit value phenomenon.The supergauge limit value time reaches 7 days most, and is average＜2 days.And up to the present most of major overhauls are restarted a loop SO of stage generation
4 2-The reason of contamination accident is not bright.Show that the problem that sulfate radical pollutes a loop in the unit starting stage singly is not the exclusive or of the same type power station of a DNMC ubiquity problem.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of and do not have omission, can disclose the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution of sulfate pollution essence.
The technical solution adopted for the present invention to solve the technical problems is: a kind of analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution, there is oxygen enrichment in the inner intense radiation of reactor, the water, removes the Zeo-karb that contains the benzene sulfonic acid group in the salt bed, cause starting process after nuclear plant major overhaul one loop sulfate pollution.
The analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution, be specially: through investigation test, laboratory simulation oxidation test, starting process after nuclear plant major overhaul system test, analysis draws in starting process after nuclear plant major overhaul, the reactor internal radiation reaches more than the 10Gy/h, oxygen concentration is during greater than 4mg/kg, can form certain density hydrogen peroxide in the water, with remove the Zeo-karb reaction that contains the benzene sulfonic acid group in the salt bed after progressively form sulfate, cause sulfate pollution.
Described investigation test comprises following steps:
1), carried out the investigation test experience of the chemicals relevant with a loop shutdown activity, got rid of the use chemicals and brought sulfate pollution;
2), carried out fresh fuel and introduced pollutant investigation test experience, got rid of fresh fuel and brought sulfate pollution;
3), the oxidation stage of nuclear plant major overhaul is detected investigation, detect to draw and adding H
2O
2After the situation that sulfate concentration sharply raises has appearred, side by side except H
2O
2Sulfur-bearing acid group own, remove the sulfate pollution that salt bed causes when putting into operation;
4), under unit starting stage cold shut pattern, the H unloading phase of the detection in real time
2O
2Concentration, sulfate radical content draw the H that the unit starting stage has also produced high concentration
2O
2, and cause sulfate pollution.
Described investigation test preferably comprises following steps:
1), sulfate radical content after the total sulfur content in the starting process after nuclear plant major overhaul use chemicals, the thermal decomposition is measured, the concentration of its result sulfate radical during well below a loop sulfate pollution, getting rid of used chemicals is the root of bringing sulfate pollution;
2), fresh fuel introduced pollutant detect, carried out fuel surface wipe test, fuel heat test, its result has got rid of fresh fuel and has brought sulfate pollution;
3), the oxidation stage of nuclear plant major overhaul is detected investigation, detect to draw and adding H
2O
2After the sulfate pollution situation has appearred, to the H that adds
2O
2In sulfate radical content, remove salt bed and when putting into operation, remove salt bed water delivering orifice water sample sulfate radical content and detect, got rid of H
2O
2Itself containing sulfate radical, purification flow rate changes and has brought sulfate pollution;
4), under unit starting stage cold shut pattern, the H unloading phase of the detection in real time
2O
2Concentration, sulfate radical content draw the H that the unit starting stage has also produced high concentration
2O
2, and cause sulfate pollution, to H
2O
2Generation source analyze.
Adopt x-ray fluorescence analysis, coulometry respectively, use the total sulfur content in the chemicals to detect starting process after nuclear plant major overhaul.
The assay method of sulfate radical content is specially after the described thermal decomposition: under 110 ℃ the chemicals that adopts is carried out heating and decomposition, detect the content that decomposes sulfate radical in the afterproduct.
Described fuel surface wipe test is specially: with wet cotton balls wiping fuel rod surface and grid, detect the content of sulfate radical on the wet cotton balls then.
Described fuel heat test is specially: in the fuel clean groove demineralized water is heated to 90 ℃, sulfate radical content in the sample analysis water is as background values, random choose 3～5 group fuel assemblies are put into rinse bath respectively, be heated to 90 ℃ of constant temperature 2～3 hours, take out fuel assembly, get the water sample analysis sulfate radical content in the rinse bath, cut the sulfate radical content that background values is fuel assembly at last.
Described laboratory simulation test is: at laboratory simulation unit starting stage condition, check and analysis H
2O
2The condition, the H that produce
2O
2With the Zeo-karb generation oxidation reaction condition and the reaction result that contain the benzene sulfonic acid group.
Described starting process after nuclear plant major overhaul system test is: in starting process after nuclear plant major overhaul, and online verification lab analysis result, check and analysis H
2O
2Content is to the influence of the Zeo-karb that contains the benzene sulfonic acid group, and the situation that causes sulfate pollution.
The present invention is by the investigation test, the laboratory simulation oxidation test, starting process after nuclear plant major overhaul, the oxidizing process system test, analysis draws in starting process after nuclear plant major overhaul, under the condition of unit internal radiation greater than 10Gy/h, on-line real time monitoring is when oxygen concentration during greater than 4mg/kg, remove the Zeo-karb that contains the benzene sulfonic acid group in the salt bed and progressively form sulfate after oxidized, cause sulfate pollution, the method that the present invention adopts is detailed, do not have and omit, can disclose the essence of starting process after nuclear plant major overhaul one loop sulfate pollution.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is embodiment of the invention L202 one a loop oxidation stage sulfate radical content variation diagram;
Fig. 2 is that embodiment of the invention resin leaches the oxygenolysis variation diagram;
Sulfate radical and H in the one circuit cools agent unloading phase that Fig. 3 being embodiment of the invention D110 major overhaul
2O
2Content figure;
Sulfate radical and H in the one circuit cools agent unloading phase that Fig. 4 being embodiment of the invention D210 major overhaul
2O
2Content figure;
Fig. 5 is sulfate radical and H in the oxidation shutdown stage one circuit cools agent of embodiment of the invention L202 major overhaul
2O
2Content figure;
Fig. 6 is sulfate radical and H in the oxidation shutdown stage one circuit cools agent of embodiment of the invention L103 major overhaul
2O
2Content figure;
Fig. 7 is that embodiment of the invention D1PTR spentnuclear fuel pond and D1PTR001DE remove salt bed sulfate radical changing trend diagram.
Embodiment
Below by D210, L202 and L103 (the tenth overhaul of No. two units of Daya Bay nuclear power plant, the overhaul for the second time of No. two units of mountain range Australia nuclear power station and a unit overhaul for the third time), behind major overhaul in the start-up course, the analysis situation of sulfate pollution is described in detail technical scheme of the present invention.
One, the eliminating test of the chemicals of the shutdown activity use relevant with a loop:
1, at first according to the SO that takes place
4 2-Features of pollution, the sulfurous organic compound that uses during to the maintenance job of overhaul is investigated.
Filter out the chemicals that 13 kinds of sulfur content may be high, adopt the method for x-ray fluorescence analysis instrument and petrochemical industry standard " SH/T 0253 oils total sulfur content mensuration-coulometry " to measure the chemicals sulfur content.The sulfur content measurement result of these 13 kinds of chemicals is as shown in table 2:
Table 2 chemicals sulphur content determination result
| The chemicals numbering | Chemical name | X-ray fluorescence method is surveyed S | X-ray fluorescence method is surveyed Cl | The SH/T0253 method is surveyed S |
| 1 | The Wei Dier clean-out system | Do not detect | 0.241％ | 23mg/ |
| 2 | The bolt clean-out system | Do not detect | Do not detect | Do not detect |
| 3 | Detergent (07307509) | 34.3mg/kg | Do not detect | 4.2mg/kg |
| 4 | Detergent (07307501) | 50.5mg/kg | 0.0101％ | 2.0mg/kg |
| 5 | Leak detection liquid | 261mg/kg | Do not detect | 310mg/kg |
| 6 | The pressure vessel bolt with lubricator | Do not detect | Do not detect | 8mg/kg |
| 7 | Valve-seating inspection blue oil | 0.2％ | Do not detect | 0.16％ |
| 8 | Abrasive pastes | 0.2％ | Do not detect | 0.39％ |
| 9 | Gear oil | 1.5％ | Do not detect | 2.0％ |
| 10 | The extreme pressure consistent lubricant | 1.7％ | Do not detect | 2.4％ |
| 11 | Oil-proof Silicone Sealant | 90.5mg/kg | 25.9％ | 0.1％ |
| 12 | All purpose grease | Not inspection | Not inspection | 0.12％ |
| 13 | Railway grease | Not inspection | Not inspection | 41mg/kg |
For the ease of analyzing major loop SO
4 2-The root of polluting is with SO after chemicals sulphur, chlorinity and the 110 ℃ of thermal decompositions
4 2-, Cl
-The analysis result contrast is as follows:
Table 3 chemicals sulphur, chlorinity and 110 ℃ of thermal decomposition sulfate radicals, chlorions compare
According to above-mentioned chemicals sulfur content and the ability that decomposites sulfate radical, calculating 4 generation RCP sulfate radicals again is the needed chemicals total amount that chemicals causes unusually.See Table 4.
Four overhaul units of table 4 are restarted stage RCV and are removed salt bed removal sulfate radical total amount and the estimation of required amount of pollutant
| Overhaul | Time period | RCV removes salt bed and removes SO 4 2-Total amount (g) | Major loop produces SO 4 2-Total amount (g) | Pollutant sulfur content 0.1% is finished the amount (kg) that conversion needs | Pollutant sulfur content 0.5% is finished the amount (kg) that conversion needs | SO 4 2-Greater than the time (h) of 150 μ g/Kg |
| L201 | 2004-1-23?6:15～ 2004-1-26?21:30 | ?232.19 | 240.29 | ?80.10 | 16.02 | 43 |
| L102 | 2004-3-13?7:00～ 2004-3-16?13:35 | ?114.46 | 127.06 | ?42.35 | 8.47 | 0 |
| D210 | 2004-6-27?9:30～ 2004-7-8?11:20 | ?676.83 | 682.26 | ?227.42 | 45.48 | 88.5 |
| D110 | 2004-11-2?22:10～ 2004-11-6?10:20 | ?291.86 | 300.50 | ?100.17 | 20.03 | 35.5 |
| Add up to | ?1315.34 | 1350.11 | ?450.04 | 90.01 | 167 |
It is extremely low to this shows that non-grease class and grease class pollution source enter the possibility in a loop in a large number, and do not find that above-mentioned chemicals enters the sign in a loop in a large number in the control of follow-up chemicals, do not find that in conjunction with turbidity and the naked eyes supervision to reactor pit between loading period high SO does not appear in unusual greatly, PTR001BA (refuelling water storage tank, the PTR system is reactor and cooling of spentnuclear fuel pond and disposal system) pyrolytic test
4 2-Situation, got rid of chemical residues and caused sulfate pollution.
Two, fresh fuel is introduced the contaminant exclusion test:
At first carried out the fuel surface wipe test, with wet cotton balls wiping fuel rod surface and grid, the result shows the SO of wipe samples
4 2-Content is bigger 2～3 times than blank sample.Can have SO by qualitative explanation novel fuel assembly outside surface
4 2-Pollutant, but the SO that the wiping of whole group assembly is got off
4 2-Total amount is very low, quantitative Analysis, and the contribution of 70 new combustion fuel assemblies is for about 300m
3A loop can only increase SO
4 2-Several ppb levels are analyzed from quantitative concept, are not enough to impact.
For further whether the checking novel fuel assembly can be to major loop SO
4 2-Exert an influence, carried out fresh fuel heating simulation test.In test, in the fuel clean groove, demineralized water (about 900L) is heated to 90 ℃, sulfate radical content in the sample analysis water (as background 0# sample), (AFA3G) in 5 group fuel assemblies of random choose first group put into rinse bath, constant temperature 3 hours, take out fuel assembly, get the sample analysis sulfate radical content (sample number into spectrum 1#) in the rinse bath, the moisture that evaporates with demineralized water additional clean groove.Carry out the washing test of other 4 group fuel assembly in the same way, obtain water sample 2#, 3#, 4#, 5# respectively.Water sample send the Chinese nuclear power chemical analysis chamber analysis SO of design and research institute
4 2-Content.
Can draw from the result of heating simulation test: the water of same rinse bath continuously heated wash behind 5 groups of novel fuel assemblies, the SO in the rinse water
4 2-Content is the same with background values all below instrument detecting limit, and this explanation novel fuel assembly can be to the sulphur SO of major loop
4 2-Impact.Cause SO by fresh fuel
4 2-Pollution is excluded.
Three, sulfate radical content and situation of change in the overhaul oxidizing process are detected:
Each stage of overhaul and a circuit system have been carried out comprehensive sulfate radical detected, grasped the variation of whole overhaul process sulfate radical, found to reach in the loop 80 ℃ and add H
2O
2After entering oxidation stage, in oxidizing process, find the variation abnormality of sulfate radical content, as shown in Figure 1, added H
2O
2Sulfate concentration among the RCP is 48ppb before, is adding H
2O
2Back sulfate concentration begins to rise, and is adding H
2O
2The back reached peak value 157ppb after 5.5 hours.Operation in the whole process only relates to and adds H
2O
2With adding H
2O
2When the about 10 minutes oxygen concentrations in back surpass 1.0ppm with purification flow rate from about 7m
3/ h fast lifting is to 26m
3/ h.Analyze whole operation process one loop and be connected system except adding H
2O
2Sealing fully outward can not have other chemicals to introduce.
According to adding H
2O
2The back after 5.5 hours in the loop sulfate concentration just reach peak value, and laboratory measurement H
2O
2Even in find H under heating condition during sulfate radical content
2O
2In only contain a spot of sulfate radical.So H
2O
2In contain sulfate radical possibility be excluded.
If purification flow rate changes and to cause removing salt bed and leak sulfate radical, its result removes the salt bed outlet to have a large amount of sulfate radicals, occurs the peak value that matches with leakage rate in the RCP system fast and because of the very fast reduction that tends towards stability of desalination bed operating.Really not so as sulfate radical performance among Fig. 1.Follow-uply the analysis showed that to what remove sulfate radical in the salt bed outlet water sample sulfate concentration is low, the hypothesis that discharges with the sulfate radical of high concentration misfits.Therefore fluctuations in discharge causes removing may being excluded of salt bed leakage sulfate radical.
Four, laboratory simulation test
Because H
2O
2Having strong oxidizing property, may be H
2O
2Cause the Zeo-karb part group that contains sulfonic acid group come off and chain rupture produces sulfate radical, so carried out laboratory simulation H
2O
2Oxidation contains the test of the Zeo-karb of sulfonic acid group.
Test method:
1), under lab, the 10ml Zeo-karb is immersed in 45 ℃ 0,2,4,6,10, the H of 100ppm concentration
2O
2In, test through the oxidation analog that constant temperature oxidation analog test in 96 hours is carried out.
2) oxidation analog is tested back clear water sample, again and be heated to 120 ℃, constant temperature carried out the decomposition simulation test of water sample in 24 hours.
3), with the sulfate concentration in each water sample of ion chromatography.
4), on the data processing sample sulfate concentration under 45 ℃ of conditions is deducted 0ppm H
2O
2Increment behind the sample concentration is decided to be Δ 1, with water sample when 45 ℃ of each sample sulfate concentrations that is heated to after 120 ℃ are compared 45 ℃ again increment be decided to be Δ 2.Fig. 2 is seen in the data trend analysis of laboratory simulation test.
As shown in Figure 2, draw as drawing a conclusion:
1), Zeo-karb is at 0ppm H
2O
2In the sulfate radical of 45 ℃ and 120 ℃ leachings change for a short time, illustrate that demineralized water soaks in the positive resin extract sulfate radical and do not vary with temperature nothing substantially and rise appreciably.
2), under 45 ℃, after constant temperature oxidation in 96 hours, Δ 1 is with H
2O
2The rising of concentration and raising, but not obvious, H
2O
2Concentration is under 2～10ppm, and Δ 1 only is 40～110ppb; 100ppm H
2O
2The time sulfate radical obviously increase.
3), oxidation analog test back clear water sample is at 120 ℃, constant temperature is after 24 hours, Δ 2 significantly increases, H
2O
2Concentration is under 2～10ppm, and sulfate concentration is 20～550ppb, and Δ 2 is bigger than Δ 1, and 100ppm H
2O
2The time Δ 2 bigger.
4), see on the trend that Δ 1, Δ 2 are with H
2O
2Concentration increases and increases.
5), in theory Δ 2 should to hang down very much be the straight line that overlaps with horizontal ordinate, but in fact its slope greater than the slope of Δ 1.Theory does not conform to the actual conditions.Data basically identical after the revision test.Therefore can draw as drawing a conclusion:
1), under 45 ℃-120 ℃ temperature, Zeo-karb is through H
2O
2Can produce sulfate radical after the immersion, sulfate concentration is along with H
2O
2The rising of concentration and present the rising phenomenon.
2), there is the intermediate material that can change into sulfate radical in the final proof after the positive resin oxidation.This material is not detected by chromatography of ions before conversion, its generation and H
2O
2Concentration is directly proportional, and keeps slowly being converted into the trend of sulfate radical, high temperature can facilitate conversion to carry out, and this material derives from Zeo-karb, name unknown.
3), data show at H
2O
2Concentration is during greater than 4ppm, H
2O
2Oxidation generation sulfate radical to Zeo-karb is obvious relatively.
Five, online verification test under the cold shut pattern unloading phase:
1, H in the circuit cools agent in the start-up course after the analyzing and testing overhaul
2O
2Production respectively to the H under Daya Gulf/mountain range Australia nuclear power station one loop and PTR system different location and the state
2O
2(comprising keeping sample in the overhaul in the past), concentration was analyzed, and gathered these test for data and saw table 5 for details.
Table 5 a circuit cools agent and spentnuclear fuel pond H
2O
2Analyze data
| System | State | ?H 2O 2(ppm) |
| The RCP major loop | Power run duration: radioactive intensity height, oxygen deprivation | ?＜0.5 |
| The RCP major loop | During the one loop bulge test: radioactive intensity is low, oxygen enrichment | ?2.0 |
| The RCP major loop | Major loop is between the starting period: hot, oxygen enrichment | ?14～20 |
| D1PTRFP | Spentnuclear fuel is many, and radioactive intensity is higher, oxygen enrichment | ?7.0 |
| D2PTRFP | Spentnuclear fuel is many, and radioactive intensity is higher, oxygen enrichment | ?7.0 |
| L1PTRFP | Spentnuclear fuel is few, and radioactive intensity is lower, oxygen enrichment | ?5.0 |
| L2PTRFP | Spentnuclear fuel is few, and radioactive intensity is lower, oxygen enrichment | ?5.0 |
Analysis result has proved 1: all there is H in all the other investigation samples except that power mode of operation
2O
2, and the unloading phase a loop also have H
2O
2Find H
2O
2Water in its concentration all reach the ppm level.
Table 5 data also have following feature:
According to O
2+ 2H
2O---irradiation catalysis → 2H
2O
2Principle, in the reactor start-up stage, have H in the loop really
2O
2, the reason of its generation is generated by oxygen and water reaction under radiation parameter.
2, under the cold shut pattern unit starting stage at thread test:
In vitro resin soaks and water sample decomposition simulated experiment has proved H
2O
2Positive resin influence is produced sulfate radical, needed system to carry out online verification experimental verification hot and hyperbaric environment H
2O
2To negative resin in the influence of positive resin and the ion-exchanger to the influence of test findings.
Sample unloading phase of the D110 overhaul is analyzed, as shown in Figure 3, find unit the unloading phase do not introducing H
2O
2Situation under occurred concentration unexpectedly and reached 12ppm H
2O
2, 12ppm H
2O
2Concentration is equivalent to have added to a loop at oxidation stage 12 liter 35% H
2O
2(amount that adds in the oxidizing process is 18 liters).Moreover, H among the figure
2O
2Compare discovery with sulfate radical and work as H
2O
2Sulfate radical had also risen when concentration rose, and worked as H
2O
2Quick decline had appearred in sulfate radical when concentration was very low.
Equally as shown in Figure 4, same situation has also appearred the D210 overhaul unloading phase.
At H occurring in the condition in unit oxidation shutdown stage and the unit starting process
2O
2The characteristics of the ambient condition basically identical during with sulfate radical, the shutdown oxidation stage of overhaul is carried out online detection further proves H
2O
2Can resene and produced sulfate radical.
80 ℃-40 ℃ of one loop oxidation and startup temperature rise period RCP temperature, pressure is 25-27bar.TEP006DE removes salt bed and RCV001/002DE is to mix bed except that salt bed, and each removes in the salt bed 40% Zeo-karb all is housed.At overhaul one loop oxidation stage, TEP006DE removes salt bed and moves continuously; Start-up course is used RCV001/002DE after overhaul.
Process of the test: the sulfate radical and the H that one circuit system are carried out at the L202 overhaul initial stage
2O
2Concentration is followed the tracks of, and data are seen Fig. 5.
In order to verify the data of L202 overhaul, detect carrying out online in real time during the L103 overhaul one loop oxidation, purification equally, see Fig. 6.
As Fig. 5, shown in Figure 6, H among the figure
2O
2Very similar with the time dependent situation of sulfate radical.H
2O
2Performance be: a loop adds H
2O
2After, its concentration rises to 10～12ppm immediately, H occurs because be consumed and partly decompose afterwards
2O
2Concentration reduces.Along with after the oxidized and RCV of RCP system holds the control case and implement the air purge supplemental, in the circuit cools agent H appears once more
2O
2, its concentration begins to rise and is up to 10～15ppm, last slowly reduction.And the performance of sulfate radical is: when H having occurred
2O
2The sulfate pollution phenomenon has appearred in the RCP system behind the peak value, and reaches a peak value.Downtrending afterwards is very slowly far below theoretical decline rate, and reflecting has sulfate radical to produce continuously in the process.The generation speed of sulfate radical and the purification rate of sulfate radical are depended in the variation of sulfate concentration fully.As a loop H
2O
2After concentration was reduced to 4～5ppm, big reduction had appearred in sulfate concentration in the circuit cools agent, and purification efficiency begins to improve.
Fig. 5, sulfate radical and H among Fig. 6
2O
2Variation and D210/D110 overhaul unit starting stage situation about occurring similar, the judgement that can further specify thus the unloading phase of the simulation with oxidation stage is correct.
Result according to laboratory simulation test: " Zeo-karb is subjected to H
2O
2The intermediate material of sulfur-bearing is leaked out in oxidation "; system will meet the result of laboratory simulation test except that the variation of sulfate radical in the salt bed outlet water in thread test so; promptly can measure the part of sulfuric acid root at that time, will occur the significantly rising of sulfate radical when measuring once more under the certain condition.Salt bed outlet water sample has carried out the sulfate radical supervision and analysis once more after placing month so online supervision removes TEP006DE in the works, as a result shown in the table 6.
Table 6TEP006DE removes salt bed outlet sample sulfate concentration and analyzes
| Analysis time | 2005.02.07 | 2005.03.08 |
| Sulfate radical (ppb) | 4 | 173 |
Table 6 shows: during major overhaul one loop oxidation, purification, 9TEP006DE is very low except that salt bed exports instant sample sulfate concentration, and the sulfate concentration in the sample has risen 40 times unexpectedly after 28 days and its sample is placed.Also be after resin is oxidized 9TEP006DE remove in the salt bed outlet water and have the free state sulfate radical of low concentration, and in through its water behind the certain condition unusual high sulfate radical has appearred.These data have not only negated to remove that negative resin spills sulfate radical in the salt bed, also further provide proof for the intermediate product conclusion.Consistent with the conclusion of laboratory simulation test.
For further checking removes the intermediate product that has sulfur-bearing in the salt bed outlet water, it is as follows that the keeping sample that TEP006DE removes the salt bed outlet unloading phase that we finding the D110 overhaul after to historical sample cleaning carries out measurement data:
Table 7TEP006DE removes salt bed outlet sample sulfate concentration and analyzes
| Analysis time | 2004.11.03 | 2005.03.08 |
| Sulfate radical (ppb) | 4 | 227 |
Data show TEP006DE remove salt bed export instant sample and its placement after 4 months the sulfate concentration of sample differ 55 times, the conclusion and the data in the table 6 that obtain are in full accord, the conclusion that can proof list 6 data obtains.
Gather above-mentioned on-line system conclusion (of pressure testing) as follows:
1, influences under the on all four situation of mechanism H under the loop oxidation shutdown pattern
2O
2The sulfate radical of 180-260ppb can appear in the RCP system when concentration reached 10-15ppm.So at same temperature, pressure, H
2O
2Under the one loop start stage similarity condition of concentration and mixed ion-exchanger also sulfate pollution can appear.H
2O
2Caused that RCP is subjected to sulfate pollution in the unit starting process.
2, H
2O
2Can oxidation the Zeo-karb that uses of this power station and cause its material that produces the non-sulfuric acid root morphology, coming off from resin enters the water.This material can be converted into sulfate radical at an easy rate.Temperature raises and can promote conversion rate to accelerate.
3,, very likely be to contain the sulfonic group functional group in the positive resin to have participated in reaction in conjunction with the composition and the structure situation of Zeo-karb.
4, H
2O
2Concentration roughly is judged as 4ppm to the influence degree of resin on data, the generation speed that is lower than sulfate radical in the 4ppm one circuit cools agent is near or below the purification rate of sulfate radical.
Six, the demonstration test of spentnuclear fuel pond and purification circuit thereof
Test method:
To D1PTR001DE remove salt bed carried out isolation, static, the system that puts into operation at thread test, and stop all other systems operations.Only PTR.F.P and D1PTR001DE are analyzed to judge whether sulfate radical continues to rise except that the sulfate ion of salt bed outlet at duration of test.
The result of the 1st test just finds to occur among the PTR.F.P ANOMALOUS VARIATIONS of sulfate radical, so revision test 2 times again.The relevant sulfate radical variation tendency that D1PTR001DE removes 3 tests of salt bed sees Fig. 7 for details, data show 3 supernormal growths that occurred sulfate radical when isolating PTR001DE except that the startup behind the salt bed 3 times among the PTR.F.P among the figure, and do not occur the sulfate radical appearance of high concentration in the sample except that the salt bed outlet.Discharge sulfate radical even negative resin is subjected to the influence of flow or pressure surge, that come out earlier according to resin properties generally is Cl
-, just may be sulfate radical then.And Cl does not appear among the PTR.F.P
-Growth.
For the sulfate radical release of the reliable of verification msg and discovery high concentration, project team tests on the LINAO unit again.Obtain identical test findings.And do not find to occur among the PTR.F.P Cl equally
-With the situation of removing the high sulfate radical of appearance in the salt bed outlet.The general principle opinion can't be explained this phenomenon.Removing salt bed outlet sample sulfate concentration after placing a period of time simultaneously progressively rises above 100ppb from 30-40ppb.
There is the phenomenon of a small amount of sulfate radical in the PTR.F.P test findings coupling system midium or long term.And can obtain to draw a conclusion:
1, under the situation that oxygen, Zeo-karb and irradiation field exist the sulfate radical abnormal ascending has appearred in PTR.F.P.
2, D1PTR001DE removes salt bed and is immersed in H for a long time
2O
2In, the constantly oxidized intermediate material that discharges enters in the water, decomposites sulfate radical gradually.Because the temperature that circulation ability is strong and spentnuclear fuel is surperficial of PTR.F.P is high slightly or factor such as radiation parameter, the intermediate product decomposition rate is very fast.
3, owing to always have sulfate pollution source and detergent power, always there is a spot of sulfate radical among the PTR.F.P.
4, after D1PTR001DE removes salt bed and puts into operation, be kept at except that the intermediate product in the salt bed and be discharged into hot rapidly and contain H
2O
2The warm water environment after be converted into sulfate radical rapidly.
5, sulfate radical rises irrelevant with negative resin release sulfate radical.
PTR.F.P also verification experimental verification H
2O
2Can cause that the resin oxidation causes sulfate radical unusual.
Claims (8)
1. the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution, it is characterized in that, through investigation test, laboratory simulation oxidation test, starting process after nuclear plant major overhaul system test, analysis draws in starting process after nuclear plant major overhaul, the reactor internal radiation reaches more than the 10Gy/h, oxygen concentration is during greater than 4mg/kg, can form certain density hydrogen peroxide in the water, with remove the Zeo-karb reaction that contains the benzene sulfonic acid group in the salt bed after progressively form sulfate, cause sulfate pollution.
2. the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution according to claim 1 is characterized in that, described investigation test comprises following steps:
1), sulfate radical content after the total sulfur content in the starting process after nuclear plant major overhaul use chemicals, the thermal decomposition is measured, the concentration of its result sulfate radical during well below a loop sulfate pollution, getting rid of used chemicals is the root of bringing sulfate pollution;
2), fresh fuel introduced pollutant detect, carried out fuel surface wipe test, fuel heat test, its result has got rid of fresh fuel and has brought sulfate pollution;
3), the oxidation stage of nuclear plant major overhaul is detected investigation, detect to draw and adding H
2O
2After the sulfate pollution situation has appearred, to the H that adds
2O
2In sulfate radical content, remove salt bed water delivering orifice water sample sulfate radical content when removing salt bed and putting into operation and detect, got rid of H
2O
2Itself containing sulfate radical, purification flow rate changes and has brought sulfate pollution;
4), under unit starting stage cold shut pattern, the H unloading phase of the detection in real time
2O
2Concentration, sulfate radical content draw the H that the unit starting stage has also produced high concentration
2O
2, and cause sulfate pollution, to H
2O
2Generation source analyze.
3. the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution according to claim 2, it is characterized in that, adopt x-ray fluorescence analysis, coulometry respectively, use the total sulfur content in the chemicals to detect starting process after nuclear plant major overhaul.
4. the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution according to claim 2, it is characterized in that, the assay method of sulfate radical content is after the described thermal decomposition: under 110 ℃ the chemicals that adopts is carried out heating and decomposition, detect the content that decomposes sulfate radical in the afterproduct.
5. the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution according to claim 2, it is characterized in that, described fuel surface wipe test is: with wet cotton balls wiping fuel rod surface and grid, detect the content of sulfate radical on the wet cotton balls then.
6. the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution according to claim 2, it is characterized in that, described fuel heat test is: in the fuel clean groove demineralized water is heated to 90 ℃, sulfate radical content in the sample analysis water is as background values, random choose 3～5 group fuel assemblies are put into rinse bath respectively, be heated to 90 ℃ of constant temperature 2～3 hours, take out fuel assembly, get the water sample analysis sulfate radical content in the rinse bath, cut the sulfate radical content that background values is fuel assembly at last.
7. the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution according to claim 1 is characterized in that, described laboratory simulation oxidation test is: at laboratory simulation unit starting stage condition, check and analysis H
2O
2The condition, the H that produce
2O
2With the Zeo-karb generation oxidation reaction condition and the reaction result that contain the benzene sulfonic acid group.
8. the analytical approach of starting process after nuclear plant major overhaul one loop sulfate pollution according to claim 1, it is characterized in that, described starting process after nuclear plant major overhaul system test is: in starting process after nuclear plant major overhaul, online verification lab analysis result, check and analysis H
2O
2Content is to the influence of the Zeo-karb that contains the benzene sulfonic acid group, and the situation that causes sulfate pollution.
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