EP2564394A1 - Method for surface decontamination - Google Patents
Method for surface decontaminationInfo
- Publication number
- EP2564394A1 EP2564394A1 EP11721251A EP11721251A EP2564394A1 EP 2564394 A1 EP2564394 A1 EP 2564394A1 EP 11721251 A EP11721251 A EP 11721251A EP 11721251 A EP11721251 A EP 11721251A EP 2564394 A1 EP2564394 A1 EP 2564394A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- oxidation step
- solution
- oxide layer
- decontamination
- oxidation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000005202 decontamination Methods 0.000 title claims abstract description 22
- 230000003588 decontaminative effect Effects 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000003647 oxidation Effects 0.000 claims abstract description 36
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000004140 cleaning Methods 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000012670 alkaline solution Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract 4
- 238000009390 chemical decontamination Methods 0.000 claims abstract 2
- 239000007800 oxidant agent Substances 0.000 claims description 13
- 230000002378 acidificating effect Effects 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 230000003113 alkalizing effect Effects 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 18
- 239000002826 coolant Substances 0.000 description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- 239000011651 chromium Substances 0.000 description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 229910052804 chromium Inorganic materials 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000002285 radioactive effect Effects 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000003929 acidic solution Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- GUTLYIVDDKVIGB-OUBTZVSYSA-N Cobalt-60 Chemical compound [60Co] GUTLYIVDDKVIGB-OUBTZVSYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229940093915 gynecological organic acid Drugs 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 125000005385 peroxodisulfate group Chemical group 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/001—Decontamination of contaminated objects, apparatus, clothes, food; Preventing contamination thereof
- G21F9/002—Decontamination of the surface of objects with chemical or electrochemical processes
- G21F9/004—Decontamination of the surface of objects with chemical or electrochemical processes of metallic surfaces
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/28—Treating solids
Definitions
- the invention relates to a method for surface decontamination of components or systems of a nuclear power plant, for example a pressurized water reactor (PWR).
- Kern ⁇ piece of a nuclear power plant is a reactor pressure vessel in which nuclear fuel containing fuel elements are arranged.
- a coolant circuit forming tube system is connected, which is in the case of a PWR with at least one coolant pump and a steam generator ver ⁇ prevented.
- the oxide layers contain iron oxide with di- and tri-valent iron and oxides of other metals, especially chromium and nickel, which are present as alloying constituents in the steels mentioned above, depending on the type of alloy used for a component.
- Nickel is always present in divalent form (Ni 2+ ), chromium in trivalent (Cr 3+ ) form.
- Decontamination step is also often worked under reductive conditions.
- the oxidizing agent used in the preceding oxidation step is therefore removed or neutralized, as will be shown below.
- the oxidative treatment of the oxide layer is necessary because chromium-III oxides and trivalent chromium-containing mixed oxides, especially of the spinel type, in the mination in question decontamination acids, eg in oxalic acid, difficult to solve.
- ⁇ is first oxide layer with an aqueous Lö ⁇ solution of an oxidizing agent such as Ce 4+, HMn0 4, H 2 S 2 O 8, treated 4 or O3.
- an oxidizing agent such as Ce 4+, HMn0 4, H 2 S 2 O 8, treated 4 or O3.
- the result of this treatment is that Cr-III is oxidized to Cr-VI, which goes into solution as Cr0 4 2 ⁇ .
- the cleaning solution present at the end of an oxidative treatment is either discarded or processed to
- Decontamination step can be used. If the latter is the case, a remaining residual content of oxidizing agent must be removed or neutralized by a reducing agent, for example by using a corresponding excess of deconic acid.
- the decontamination step subsequent to the oxidation serves to dissolve the previously oxidatively treated oxide layer with the aid of one or mixtures of complex-forming organic acid.
- a deconic acid can simultaneously also serve for the neutralization of the oxidizing agent used in the oxidation step. It is also possible to reduce an oxidant such as HMn0 4 with the aid of an additionally added for Dekontklare Reduktionsmit ⁇ means of, for example ascorbic acid, citric acid or water ⁇ peroxide, or to neutralize.
- the Cr-VI formed in the oxidation step is also reduced again to Cr-III.
- the cleaning solution contains Cr-III, Fe-II, Fe-III, Ni-II and radioactive isotopes such as Co-60. These metal ions can be removed from the cleaning solution with an ion exchanger.
- a number of treatment cycles comprising an oxidation step and a decontamination step are carried out in order to achieve sufficient purification success, ie to achieve the highest possible decontamination factor.
- Decontamination factor is the ratio of the initial value measured prior to the execution of a cleaning cycle and the end value of the radioactive radiation present at the end of the cleaning cycle, which starts from a component or system surface or the oxide layer present thereon.
- the object of the invention is to specify a method for surface decontamination with improved effectiveness.
- This object is achieved according to claim 1 by a method of the type mentioned, in which at least one oxidation step in acidic and at least one oxidation step are carried out in alkaline solution. It has been found that a change in the pH of the oxidation solution from the acidic to the alkaline region or vice versa - such an exchange is referred to below as a pH change - causes an increase in the decontactor. The pH change can take place in one and the same cleaning cycle. Preference ⁇ example, however, carried out ⁇ oxidation step in acidic or alkaline solution and in a subsequent cleaning cycle, an oxidation step in alka ⁇ Lischer and acid solution in a cleaning cycle.
- oxidizing agent are preferably 0 3
- S20s 2 ⁇ for example, used as Na salt and cerium-IV compound, but especially in (preferably Salpe ⁇ ter) -saurer solution HMnC ⁇ and KMnC ⁇ and in Alkaline solution KMnÜ 4 , in particular with NaOH, as an alkalizing agent.
- an oxide layer is located on a component of a nuclear power plant ⁇ at least partially removed by this oxide layer and the component is treated with several cleaning cycles ⁇ supply. ⁇ or for decontamination of an entire system, such as a coolant system of a boiling water reactor pressure is filled this supply solutions to the respective cleaning ⁇ .
- the system acts as its own container. If, on the other hand, individual components are decontaminated, a container is used in which the component is treated with the appropriate cleaning solutions.
- oxidation of the oxide layer is made to oxidize chromium III contained therein to chromium VI.
- oxidizing agent it would in principle be possible to use all oxidizing agents which are capable of oxidizing chromium-III to chromium-VI, for example ozone, peroxodisulfate, cerium-IV-oxide and
- Permanganic acid or permanganate The oxidation is conveniently effected at an elevated ⁇ temperature, about 80-95 ° C. To an exposure time, for example, of several hours, the cleaning solution is exchanged or, as described above, treated so that it in the following
- Decontamination step can be used.
- organic acids such as oxalic acid, citric acid, ascorbic acid and the like are used.
- a residual oxidizing agent still present in the solution of the oxidation step is produced by a corresponding excess
- a radial cylinder was removed from the tube and its former outer side forming the tube side and its peripheral surface were provided with a protective layer, so that only the front side of the radial cylinder, which ent ⁇ the former inside of the tube, are accessible to the cleaning solutions.
- the tube or the sample consisted of steel of the type AISI 316 L. Die
- Oxide layer contained about 50% iron, 40% chromium and 10% nickel, based on the total content of metals.
- the oxide layer or the end face of the sample carrying it had an area of 5.3 cm 2 .
- a total of 9 cleaning cycles were performed.
- oxidation was carried out in an acidic medium using permanganic acid at a concentration of 0.3 g / l and at a temperature of 95 ° C. This resulted in a pH of about 3 a.
- the duration of Oxida ⁇ tion was about 17 hours.
- reaction solution was replaced with an oxalic acid solution having a concentration of 2 g / l, and thus the oxide layer was treated at a temperature of 95 ° C for about 5 hours. Thereafter, two more cycles of the type described were performed.
Landscapes
- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Food Science & Technology (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102010028457A DE102010028457A1 (en) | 2010-04-30 | 2010-04-30 | Process for surface decontamination |
PCT/EP2011/056580 WO2011134958A1 (en) | 2010-04-30 | 2011-04-26 | Method for surface decontamination |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2564394A1 true EP2564394A1 (en) | 2013-03-06 |
EP2564394B1 EP2564394B1 (en) | 2013-12-11 |
Family
ID=44521403
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP11721251.4A Active EP2564394B1 (en) | 2010-04-30 | 2011-04-26 | Process for decontamination of surfaces |
Country Status (9)
Country | Link |
---|---|
US (1) | US20130220366A1 (en) |
EP (1) | EP2564394B1 (en) |
JP (1) | JP2013529299A (en) |
KR (1) | KR20130014494A (en) |
CN (1) | CN102667958A (en) |
DE (1) | DE102010028457A1 (en) |
ES (1) | ES2441589T3 (en) |
TW (1) | TW201201221A (en) |
WO (1) | WO2011134958A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10340050B2 (en) | 2015-02-05 | 2019-07-02 | Framatome Gmbh | Method of decontaminating metal surfaces in a cooling system of a nuclear reactor |
CN113605999A (en) * | 2017-06-13 | 2021-11-05 | 通用电气公司 | System and method for selectively cleaning turbine engine components |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5787588B2 (en) * | 2011-04-18 | 2015-09-30 | 三菱重工業株式会社 | Chemical cleaning method |
KR101523763B1 (en) * | 2013-06-19 | 2015-06-01 | 한국원자력연구원 | Oxidation decontamination reagent for removal of the dense radioactive oxide layer on the metal surface and oxidation decontamination method using the same |
JP6547224B2 (en) * | 2015-01-30 | 2019-07-24 | 三菱重工業株式会社 | Chemical decontamination method |
DE102016104846B3 (en) | 2016-03-16 | 2017-08-24 | Areva Gmbh | A method of treating waste water from decontamination of a metal surface, waste water treatment apparatus and use of the waste water treatment apparatus |
JP6580509B2 (en) * | 2016-03-31 | 2019-09-25 | 三菱重工業株式会社 | Solids removal method |
DE102017115122B4 (en) * | 2017-07-06 | 2019-03-07 | Framatome Gmbh | Method for decontaminating a metal surface in a nuclear power plant |
JP6901947B2 (en) * | 2017-09-29 | 2021-07-14 | 三菱重工業株式会社 | Chemical decontamination method |
CN108560003A (en) * | 2018-01-08 | 2018-09-21 | 绵阳科大久创科技有限公司 | A kind of metal surface radioactive pollution detergent and its application method |
CN113105955A (en) * | 2021-03-31 | 2021-07-13 | 山东核电有限公司 | Decontamination formula and decontamination method for radioactive contamination deposited oxide of primary loop component of AP1000 reactor |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4587043A (en) * | 1983-06-07 | 1986-05-06 | Westinghouse Electric Corp. | Decontamination of metal surfaces in nuclear power reactors |
SE451915B (en) * | 1984-03-09 | 1987-11-02 | Studsvik Energiteknik Ab | PROCEDURE FOR DECOMPOSITION OF PRESSURE WATER REACTORS |
DE3413868A1 (en) * | 1984-04-12 | 1985-10-17 | Kraftwerk Union AG, 4330 Mülheim | METHOD FOR CHEMICAL DECONTAMINATION OF METAL COMPONENTS OF CORE REACTOR PLANTS |
JPH0631867B2 (en) * | 1984-07-09 | 1994-04-27 | 石川島播磨重工業株式会社 | Denitration concentrator clad melting method |
JPH0664191B2 (en) * | 1986-05-07 | 1994-08-22 | 科学技術庁原子力局長 | Decontamination method for chemically dissolving radioactive cladding |
CH673545A5 (en) * | 1987-10-02 | 1990-03-15 | Industrieorientierte Forsch | |
ES2045298T3 (en) * | 1988-08-24 | 1994-01-16 | Siemens Ag | PROCEDURE FOR THE CHEMICAL DECONTAMINATION OF THE SURFACE OF A METALLIC COMPONENT OF A NUCLEAR REACTOR INSTALLATION. |
JPH0699193A (en) * | 1992-09-24 | 1994-04-12 | Ebara Kogyo Senjo Kk | Chemical decontamination |
JP3859902B2 (en) * | 1998-06-23 | 2006-12-20 | 株式会社東芝 | Chemical decontamination method and apparatus for structural parts of radiation handling facilities |
US20030139047A1 (en) * | 2002-01-24 | 2003-07-24 | Thomas Terence M. | Metal polishing slurry having a static etch inhibitor and method of formulation |
BRPI0611248A2 (en) * | 2005-11-29 | 2009-07-07 | Areva Np Gmbh | A process for the decontamination of a surface containing a layer of oxide, component or system of a nuclear technology plant |
JP4204596B2 (en) * | 2006-02-09 | 2009-01-07 | 株式会社東芝 | Chemical decontamination apparatus and decontamination method thereof |
FR2897786B1 (en) * | 2006-02-24 | 2008-06-27 | Commissariat Energie Atomique | PROCESS FOR CLEANING A CONTAMINATED SUBSTRATE WITH PARTICULATE INORGANIC CONTAMINANTS USING DENSE FLUID UNDER PRESSURE |
FR2937054B1 (en) * | 2008-10-13 | 2010-12-10 | Commissariat Energie Atomique | METHOD AND DEVICE FOR DECONTAMINATING A METAL SURFACE |
-
2010
- 2010-04-30 DE DE102010028457A patent/DE102010028457A1/en not_active Withdrawn
-
2011
- 2011-04-26 KR KR1020127019683A patent/KR20130014494A/en not_active Application Discontinuation
- 2011-04-26 ES ES11721251.4T patent/ES2441589T3/en active Active
- 2011-04-26 JP JP2013506631A patent/JP2013529299A/en active Pending
- 2011-04-26 EP EP11721251.4A patent/EP2564394B1/en active Active
- 2011-04-26 WO PCT/EP2011/056580 patent/WO2011134958A1/en active Application Filing
- 2011-04-26 CN CN2011800048607A patent/CN102667958A/en active Pending
- 2011-04-28 TW TW100114859A patent/TW201201221A/en unknown
-
2012
- 2012-08-23 US US13/592,462 patent/US20130220366A1/en not_active Abandoned
Non-Patent Citations (1)
Title |
---|
See references of WO2011134958A1 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10340050B2 (en) | 2015-02-05 | 2019-07-02 | Framatome Gmbh | Method of decontaminating metal surfaces in a cooling system of a nuclear reactor |
CN113605999A (en) * | 2017-06-13 | 2021-11-05 | 通用电气公司 | System and method for selectively cleaning turbine engine components |
CN113605999B (en) * | 2017-06-13 | 2023-09-12 | 通用电气公司 | Method for selectively cleaning surfaces of turbine engine components |
Also Published As
Publication number | Publication date |
---|---|
JP2013529299A (en) | 2013-07-18 |
WO2011134958A1 (en) | 2011-11-03 |
DE102010028457A1 (en) | 2011-11-03 |
KR20130014494A (en) | 2013-02-07 |
TW201201221A (en) | 2012-01-01 |
CN102667958A (en) | 2012-09-12 |
ES2441589T3 (en) | 2014-02-05 |
EP2564394B1 (en) | 2013-12-11 |
US20130220366A1 (en) | 2013-08-29 |
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