US20120138086A1 - Method for decontaminating surfaces - Google Patents

Method for decontaminating surfaces Download PDF

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Publication number
US20120138086A1
US20120138086A1 US13/371,891 US201213371891A US2012138086A1 US 20120138086 A1 US20120138086 A1 US 20120138086A1 US 201213371891 A US201213371891 A US 201213371891A US 2012138086 A1 US2012138086 A1 US 2012138086A1
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US
United States
Prior art keywords
decontamination
acid
aqueous solution
oxide layer
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.)
Abandoned
Application number
US13/371,891
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English (en)
Inventor
Rainer Gassen
Bertram Zeiler
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Areva GmbH
Original Assignee
Areva NP GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Areva NP GmbH filed Critical Areva NP GmbH
Publication of US20120138086A1 publication Critical patent/US20120138086A1/en
Assigned to AREVA NP GMBH reassignment AREVA NP GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GASSEN, RAINER, ZEILER, BERTRAM
Assigned to AREVA GMBH reassignment AREVA GMBH CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: AREVA NP GMBH
Abandoned legal-status Critical Current

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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
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • G21F9/12—Processing by absorption; by adsorption; by ion-exchange
    • 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
    • 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
    • G21F9/30—Processing

Definitions

  • the invention relates to a method for decontaminating surfaces of components of the coolant circuit of a pressurized water reactor.
  • the key element of the coolant circuit is a reactor pressure vessel in which fuel elements containing the reactor fuel are situated. Multiple cooling loops, each having a coolant pump and a steam generator, are usually connected to the reactor pressure vessel.
  • the nuclides are then distributed through the entire coolant system by the coolant flow, and are deposited in oxide layers which form on the surfaces of components of the coolant system during operation. Over extended operating periods the quantity of deposited activated nuclides accumulates, resulting in an increase in the radioactivity, i.e., the dose rate, of the components of the coolant system.
  • the oxide layers contain as the primary component iron oxide with bi- and trivalent iron and oxides of other metals, primarily chromium and nickel, which are present as alloy components in the above-mentioned steels. Nickel is always present in the bivalent form (Ni 2 +), and chromium, in the trivalent form (Cr 3 +).
  • the coolant system Before inspection, maintenance, repair, and dismantling procedures can be carried out on the coolant system, it is necessary to reduce the radioactive radiation of the components in question in order to decrease the level of personal radiation exposure. This is achieved by removing as much as possible of the oxide layer which is present on the surfaces of the components, using a decontamination method.
  • decontamination either the entire coolant system or a portion which is separated therefrom by valves, for example, is filled with an aqueous cleaning solution, or individual components of the system are treated in a separate container which contains the cleaning solution.
  • the oxide layer is first oxidatively treated (oxidation step), and the oxide layer is subsequently dissolved under acidic conditions in a so-called decontamination step using an acid, referred to below as decontamination acid or decon acid.
  • decontamination acid or decon acid an acid
  • the metal ions which pass from the oxide layer into the solution may then be removed from the solution by leading them through an ion exchanger.
  • oxidizing agent from the oxidation step is neutralized, i.e., reduced, in a reduction step by adding a reducing agent.
  • the dissolution of the oxide layer or the leaching of metal ions in the decontamination step occurs in the absence of an oxidizing agent.
  • the reduction of the excess oxidizing agent may be an independent treatment step, whereby a reducing agent which is used only for the purpose of reduction, for example ascorbic acid or citric acid, or hydrogen peroxide for the reduction of permanganate ions and manganese dioxide, is added to the cleaning solution.
  • excess oxidizing agent may also be reduced within the scope of the decontamination step, using, in addition to the reducing agent, a decontamination acid which causes the oxide layer to dissolve, or an acid which is able to reduce excess oxidizing agent, for example the frequently used permanganate ion and the resulting manganese dioxide.
  • a quantity of decontamination acid which is sufficient on the one hand to neutralize excess oxidizing agent and on the other hand to dissolve the oxide is added to the solution.
  • the treatment sequence “oxidation step-reduction step-decontamination step” or “oxidation step-decontamination step with simultaneous reduction” is applied multiple times to achieve the desired result.
  • the same decon acid or mixture of decon acids is always used in the decontamination step.
  • the oxidative treatment of the oxide layer is necessary due to the fact that chromium(III) oxides and mixed oxides, primarily of the spinel type, containing trivalent chromium are only sparingly soluble in the acids which are suitable for decontamination. For this reason, to increase the solubility the oxide layer is first treated with an aqueous solution of an oxidizing agent such as Ce 4+ , HMnO 4 , H 2 S 2 O 8 , KMnO 4 , KMnO 4 with acid or base, or O 3 . As a result of this treatment, Cr(III) is oxidized to Cr(VI), which goes into solution as CrO 4 2 ⁇ .
  • an oxidizing agent such as Ce 4+ , HMnO 4 , H 2 S 2 O 8 , KMnO 4 , KMnO 4 with acid or base, or O 3 .
  • the Cr(VI) which is produced in the oxidation step and which is present as chromate in the cleaning solution is reduced back to Cr(III).
  • the cleaning solution contains Cr(III), Fe(II), Fe(III), and Ni(II), in addition to radioactive isotopes such as Co-60. These metal ions may be removed from the cleaning solution using an ion exchanger.
  • a frequently used decon acid in the decontamination step is oxalic acid due to its ability to dissolve oxide layers to be removed from component surfaces.
  • oxalate precipitates were produced in the preceding decontamination step, the corresponding metal ions, such as Ni in the case of a nickel oxalate precipitate, cannot be removed from the solution by using ion exchangers. As a result, in the subsequent oxidation step the oxalate residue of the precipitates is oxidized to form carbon dioxide and water, and therefore oxidizing agent is needlessly consumed.
  • the oxalate is present in solution, i.e., not bound in the form of a precipitate, the oxalate may be easily and cost-effectively decomposed by UV light, for example, i.e., converted to carbon dioxide and water, for example before the cleaning solution is led into an ion exchanger.
  • turbidity caused by an oxalate precipitate interferes with monitoring of the process, using photometry, for example.
  • This object is achieved by a decontamination method which is divided into two process stages.
  • At least one treatment cycle is performed, containing an oxidation step, a reduction step, and a subsequent first decontamination step.
  • a treatment cycle can be performed only once, or also multiple times.
  • the oxidation step the component is treated with an aqueous cleaning solution which contains an oxidizing agent whose oxidizing power is sufficient to convert the trivalent chromium contained in the oxide layer to hexavalent chromium.
  • the solubility of an oxide layer present on the component is increased.
  • the reduction step the component is treated with a solution containing a reducing agent in order to reduce excess oxidizing agent from the oxidation step.
  • the component is treated with an aqueous solution which exclusively or predominantly (i.e., in a proportion greater than 50 mol-%) contains at least one decontamination acid that forms no sparingly soluble precipitates with metal ions present in the solution, in particular bivalent metal ions such as Ni(II), Fe(II), Co(II), and Mn(II), as is the case for oxalic acid, for example.
  • metal ions present in the solution in particular bivalent metal ions such as Ni(II), Fe(II), Co(II), and Mn(II)
  • the reduction step and the decontamination step may also be carried out together, i.e., simultaneously, as described above.
  • a significant portion of the metal ions primarily Ni(II), Fe(II), and Co(II), which are critical with regard to the formation of sparingly soluble precipitates may be removed from the cleaning solution, and thus, from the component surface to be decontaminated, without the risk of forming sparingly soluble precipitates.
  • a second process stage there is the option of carrying out a second decontamination step in which highly effective oxalic acid may be easily used, primarily to leach out Fe(III) and Fe(II) present in the oxide layer, since the critical bivalent ions, primarily Ni(II), are no longer present or are present in a concentration in the cleaning solution which no longer results in precipitates.
  • two different decontamination variants are used, whereby in the first variant or the first decontamination step, ions which form sparingly soluble oxalate precipitates are removed, and remaining ions such as Fe(III) and Fe(II) may subsequently be brought into solution using oxalic acid, which is highly effective with regard to oxide dissolution. It is irrelevant per se whether the dissolution of Fe(II) or Fe(III) from the oxide layer, brought about by the “noncritical” decontamination acid used in the first process stage, is effective, since this may be effectively carried out in the second process stage using oxalic acid.
  • oxalic acid Preferably only oxalic acid is used in the second decontamination step.
  • a method according to the invention provides the option of preventing or at least greatly reducing the formation of sparingly soluble precipitates without decreasing the effectiveness of the decontamination.
  • the method may be carried out in such a way that in the first process stage, at least one treatment cycle is first carried out, and in the subsequent second process stage the component surface is treated without a preceding oxidation in the second decontamination step; i.e., the oxide layer of the component is treated with oxalic acid.
  • the oxide layer is first treated, for example using the above-mentioned oxidizing agents, and only then is the oxide layer dissolution with oxalic acid carried out. In this case, of course, a reduction step as described above is also necessary.
  • An organic acid is preferably used in the first decontamination step, since its organic component—provided that the acid consists of carbon, hydrogen, and oxygen—may be converted to carbon dioxide and water and thus removed with practically no residue, since the carbon dioxide escapes from the solution as a gas.
  • the organic constituents are removed in a manner known per se by irradiating the solution, to which an oxidizing agent such as hydrogen peroxide is added, with UV light.
  • Acids are preferably used which consist exclusively of carbon, hydrogen, and oxygen, so that no residues, resulting from elements such as nitrogen, remain behind which are removable only with the aid of ion exchangers, and which therefore result in the generation of secondary waste (additional exchanger material which must be disposed of).
  • An acid containing a maximum of two carbon atoms is preferably used in the first decontamination step.
  • the decomposition of such an acid to form carbon dioxide and water takes place more rapidly than the decomposition of acids containing three or more carbon atoms, so that time, energy, and oxidizing agent, and ultimately also costs, may be saved.
  • acids which are suitable for the decontamination step in the first process stage include inorganic acids such as HNO 3 , HBF 4 , and H 2 SO 4 , noncomplex-forming monocarboxylic acids such as formic acid, acetic acid, monohydroxyacetic acid, and dihydroxyacetic acid, and complex-forming acids such as EDTA, nitrilotriacetic acid, and tartronic acid.
  • inorganic acids such as HNO 3 , HBF 4 , and H 2 SO 4
  • noncomplex-forming monocarboxylic acids such as formic acid, acetic acid, monohydroxyacetic acid, and dihydroxyacetic acid
  • complex-forming acids such as EDTA, nitrilotriacetic acid, and tartronic acid.
  • Formic acid and glyoxylic acid have proven to be suitable for waste prevention, the best decontamination factors being achieved when only glyoxylic acid is used in the first process stage.
  • These acids form a soluble salt with the metal ions, in particular with
  • tests were conducted using samples from a primary circuit of a pressurized water reactor (see Table 1).
  • the samples were immersed in a 1-liter container containing a cleaning solution at a temperature of approximately 90° C.
  • a decontamination method the metal ions leached from an oxide layer are removed from the cleaning solution using an ion exchanger.
  • ion exchange was not performed in the tests; instead, the particular cleaning solution was discarded at the end of a treatment cycle (oxidation step and decontamination step) and replaced with a new cleaning solution. All of the tests described below were conducted in the acidic range of approximately pH 2.
  • Each treatment cycle included an oxidation step and a decontamination step.
  • formic acid and/or glyoxylic acid, not oxalic acid was used for the decontamination step (see Tables 1-3).
  • excess oxidizing agent (HMnO 4 ) was neutralized by adding an appropriate amount of reducing agent, followed by addition of the particular acid used in the decontamination step.
  • the time of exposure to the acid in the decontamination step was 5 hours in each case.
  • a decontamination factor of approximately 10 is generally sufficient. Such a factor is already achieved after the second cycle. It is further noted that glyoxylic acid is most effective for the decontamination, i.e., dissolution of the oxide layer, in particular when this acid is used in multiple, preferably all, decontamination cycles in the first process stage.
  • Residual oxidizing agent present after this step was neutralized with a mixture of hydrogen peroxide and nitric acid, the first component being necessary to dissolve the manganese dioxide (MnO 2 ) formed from HMnO 4 in the oxidation step.
  • MnO 2 manganese dioxide
  • HNO 3 nitric acid
  • the gamma activity of the sample dropped to a value of 2.18E+4 Bq after the decontamination step. Compared to the initial activity of 6.88E+4 Bq of the sample, this corresponds to a decontamination factor of 3.16.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (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)
  • Treatment Of Water By Oxidation Or Reduction (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)
US13/371,891 2009-12-04 2012-02-13 Method for decontaminating surfaces Abandoned US20120138086A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102009047524.9 2009-12-04
DE102009047524A DE102009047524A1 (de) 2009-12-04 2009-12-04 Verfahren zur Oberflächen-Dekontamination
PCT/EP2010/068602 WO2011067271A1 (de) 2009-12-04 2010-12-01 Verfahren zur oberflächen-dekontamination

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2010/068602 Continuation WO2011067271A1 (de) 2009-12-04 2010-12-01 Verfahren zur oberflächen-dekontamination

Publications (1)

Publication Number Publication Date
US20120138086A1 true US20120138086A1 (en) 2012-06-07

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US13/371,891 Abandoned US20120138086A1 (en) 2009-12-04 2012-02-13 Method for decontaminating surfaces

Country Status (11)

Country Link
US (1) US20120138086A1 (de)
EP (1) EP2417606B1 (de)
JP (1) JP5602241B2 (de)
KR (1) KR101309609B1 (de)
CN (1) CN102405500A (de)
CA (1) CA2755288A1 (de)
DE (1) DE102009047524A1 (de)
ES (1) ES2404895T3 (de)
TW (1) TW201131581A (de)
WO (1) WO2011067271A1 (de)
ZA (1) ZA201106436B (de)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140378733A1 (en) * 2013-06-19 2014-12-25 Korea Atomic Energy Research Institute Oxidation Decontamination Reagent for Removal of the Dense Radioactive Oxide Layer on the Metal Surface and Oxidation Decontamination Method Using the Same
JP2015531857A (ja) * 2012-07-26 2015-11-05 ドミニオン エンジニアリング, インク.Dominion Engineering, Inc. 洗浄溶液の再利用方法
JP2016504601A (ja) * 2013-01-30 2016-02-12 アレヴァ ゲゼルシャフト ミット ベシュレンクテル ハフツングＡｒｅｖａ ＧｍｂＨ 原子炉の冷却回路の構成部材の表面汚染除去方法
CN107240429A (zh) * 2017-06-28 2017-10-10 洛阳市琦安科技有限公司 一种放射性核污染物扩散迁移的压制材料及压制方法
CN109478437A (zh) * 2017-07-06 2019-03-15 法玛通有限公司 一种对核能发电工厂中的金属表面进行去污的方法
US10950360B2 (en) 2016-03-16 2021-03-16 Framatome Gmbh Method for treating waste water from the decontamination of a metal surface, waste-water treatment device and use of the waste-water treatment device
CN112700900A (zh) * 2020-12-10 2021-04-23 中国辐射防护研究院 一种注锌反应堆部件放射性沉积氧化物的清洗方法
US10998106B2 (en) 2017-04-07 2021-05-04 Rwe Power Aktiengeselleschaft Zinc dosing for decontaminating light-water reactors
CN113105955A (zh) * 2021-03-31 2021-07-13 山东核电有限公司 一种用于ap1000反应堆一回路部件放射性污染沉积氧化物的去污配方和去污方法
TWI799809B (zh) * 2020-03-17 2023-04-21 日商日立Ｇｅ核子能源股份有限公司 化學除汙方法及化學除汙裝置

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JP2014041100A (ja) * 2012-08-23 2014-03-06 Shimizu Corp コンクリート構造体の表層除染方法
TWI489489B (zh) * 2013-04-08 2015-06-21 Yi Hsing Huang 放射性廢料除污劑及其製造處理方法
DE102015120722B4 (de) * 2015-11-30 2017-07-27 Areva Gmbh Kernkraftwerk und Verfahren zum Betreiben eines Kernkraftwerks
CN107170503B (zh) * 2017-06-02 2019-04-02 苏州热工研究院有限公司 一种降低在役压水堆核电厂集体剂量的化学清洗方法
CN108242273A (zh) * 2017-12-28 2018-07-03 中核四0四有限公司 一种用于放射性混凝土构筑物浅层剥离的装置

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WO2012009781A1 (en) * 2010-07-21 2012-01-26 Atomic Energy Of Canada Limited Reactor decontamination process and reagent

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US5045273A (en) * 1988-08-24 1991-09-03 Siemens Aktiengesellschaft Method for chemical decontamination of the surface of a metal component in a nuclear reactor
US5305360A (en) * 1993-02-16 1994-04-19 Westinghouse Electric Corp. Process for decontaminating a nuclear reactor coolant system
WO2012009781A1 (en) * 2010-07-21 2012-01-26 Atomic Energy Of Canada Limited Reactor decontamination process and reagent

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015531857A (ja) * 2012-07-26 2015-11-05 ドミニオン エンジニアリング, インク.Dominion Engineering, Inc. 洗浄溶液の再利用方法
JP2016504601A (ja) * 2013-01-30 2016-02-12 アレヴァ ゲゼルシャフト ミット ベシュレンクテル ハフツングＡｒｅｖａ ＧｍｂＨ 原子炉の冷却回路の構成部材の表面汚染除去方法
US20140378733A1 (en) * 2013-06-19 2014-12-25 Korea Atomic Energy Research Institute Oxidation Decontamination Reagent for Removal of the Dense Radioactive Oxide Layer on the Metal Surface and Oxidation Decontamination Method Using the Same
US9390822B2 (en) * 2013-06-19 2016-07-12 Korea Atomic Energy Research Institute Oxidation decontamination reagent for removal of the dense radioactive oxide layer on the metal surface and oxidation decontamination method using the same
US10950360B2 (en) 2016-03-16 2021-03-16 Framatome Gmbh Method for treating waste water from the decontamination of a metal surface, waste-water treatment device and use of the waste-water treatment device
US10998106B2 (en) 2017-04-07 2021-05-04 Rwe Power Aktiengeselleschaft Zinc dosing for decontaminating light-water reactors
CN107240429A (zh) * 2017-06-28 2017-10-10 洛阳市琦安科技有限公司 一种放射性核污染物扩散迁移的压制材料及压制方法
CN109478437A (zh) * 2017-07-06 2019-03-15 法玛通有限公司 一种对核能发电工厂中的金属表面进行去污的方法
TWI799809B (zh) * 2020-03-17 2023-04-21 日商日立Ｇｅ核子能源股份有限公司 化學除汙方法及化學除汙裝置
CN112700900A (zh) * 2020-12-10 2021-04-23 中国辐射防护研究院 一种注锌反应堆部件放射性沉积氧化物的清洗方法
CN113105955A (zh) * 2021-03-31 2021-07-13 山东核电有限公司 一种用于ap1000反应堆一回路部件放射性污染沉积氧化物的去污配方和去污方法

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CA2755288A1 (en) 2011-06-09
JP5602241B2 (ja) 2014-10-08
EP2417606A1 (de) 2012-02-15
CN102405500A (zh) 2012-04-04
WO2011067271A1 (de) 2011-06-09
JP2013513098A (ja) 2013-04-18
TW201131581A (en) 2011-09-16
DE102009047524A1 (de) 2011-06-09
EP2417606B1 (de) 2013-02-20
KR20120057568A (ko) 2012-06-05
ZA201106436B (en) 2012-08-29
KR101309609B1 (ko) 2013-09-17
ES2404895T3 (es) 2013-05-29

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