EP0313843B1 - Procédé pour décontaminer des surfaces - Google Patents

Procédé pour décontaminer des surfaces Download PDF

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Publication number
EP0313843B1
EP0313843B1 EP88116003A EP88116003A EP0313843B1 EP 0313843 B1 EP0313843 B1 EP 0313843B1 EP 88116003 A EP88116003 A EP 88116003A EP 88116003 A EP88116003 A EP 88116003A EP 0313843 B1 EP0313843 B1 EP 0313843B1
Authority
EP
European Patent Office
Prior art keywords
treatment step
decontamination
acid
solution
surface layers
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.)
Expired - Lifetime
Application number
EP88116003A
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German (de)
English (en)
Other versions
EP0313843A1 (fr
EP0313843B2 (fr
Inventor
Erhard Schenker
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.)
Scherrer Paul Institut
ABB Reaktor GmbH
Original Assignee
Scherrer Paul Institut
ABB Reaktor 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.)
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Publication date
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Application filed by Scherrer Paul Institut, ABB Reaktor GmbH filed Critical Scherrer Paul Institut
Publication of EP0313843A1 publication Critical patent/EP0313843A1/fr
Application granted granted Critical
Publication of EP0313843B1 publication Critical patent/EP0313843B1/fr
Publication of EP0313843B2 publication Critical patent/EP0313843B2/fr
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Expired - Lifetime 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
    • 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

Definitions

  • the invention relates to a process for the decontamination of surfaces, in particular components of cooling circuits of nuclear reactors, an oxidizing agent being applied in a first treatment step to loosen up the radioactively contaminated surface layers, and the loosened surface layers being removed with the aid of a solvent in a second treatment step.
  • EP 0071336 A1 discloses a method for the chemical removal of deposits, in which decontamination is achieved in three steps using permanganate salt. The path taken there apparently avoids the use of chromic acid.
  • all known methods for decontaminating the surfaces of components of pressurized water reactors comprise two or more treatment steps, in a first step the insoluble Cr-III oxide being converted into soluble hexavalent chromium in an oxidizing phase and the entire oxide layer being loosened in the process. In a second treatment step, usually after an intermediate rinse, the loosened oxide layer is dissolved and removed in an acidic, regenerative and complex-forming solution.
  • the oxidative treatment step are a number of methods in use, such.
  • AP alkaline permanganate solution
  • NP nitric acid solutions
  • Other known processes provide for the use of permanganic acid, hydrogen peroxide, cerium IV salts or other oxidizing agents.
  • the decontamination solution used in the first treatment step contains chromic acid (chromium VI oxide) and permanganic acid. Both chromium and manganese are present in all steels commonly used in reactor construction as accompanying or alloying elements. These chemicals are not only inexpensive, but also relatively non-toxic and easy to handle in the concentrations used.
  • further substances are added to the decontamination solution used in the first treatment step, which the solvents Make the solution suitable for use in the second treatment step.
  • Reducing agents such as oxalic acid, ascorbic acid, formic acid, etc. can be considered as such further substances.
  • the reducing agents cause the chromic acid, as well as the permanganic acid and its decomposition products, that is to say also the manganese dioxide, to be converted into soluble chromium III or manganese II salts.
  • the permanganic acid can preferably be prepared by passing an aqueous solution of an alkali or alkaline earth permanganate over a cation exchanger, thus forming the free acid which is used as the decontamination agent after the addition of chromic acid.
  • Solutions of chromic acid and salts of permanganic acid are also suitable as decontamination agents; however, the additionally introduced cation with the radioactive waste will result in somewhat higher salt loads.
  • the pH value and the redox potential of the solution are characteristic of the effectiveness of the decontamination agent.
  • the first treatment step can therefore be monitored and controlled by means of these easily detectable measurement variables.
  • the reaction of the permanganic acid with constituents of the contaminated oxide layers and the spontaneous decomposition of the permanganic acid produces insoluble manganese dioxide ("manganese dioxide") even at normal room temperatures, which is deposited on the surfaces.
  • the discoloration shows the effectiveness of the decontamination solution in a visually verifiable manner. Due to the presence of chromic acid in the decontamination solution, no firmly adhering layers are formed which would then be difficult to remove.
  • the surfaces of the cooling circuit components cannot yet be completely freed of radioactive substances by the oxidative first treatment step, which is why a second treatment step is additionally required to remove the surface layers modified by the oxidative treatment.
  • the success of the second treatment step can also be checked visually, since the brownish-red-violet colored surface layers disappear from the decontaminated surfaces.
  • the effect of the decontamination solution used in the first treatment step can be increased considerably by pumping around, stirring or using ultrasound.
  • the same measures can also accelerate the chemical removal of the modified surface layers in the second treatment step.
  • the surface layers modified in the first treatment step for example of carbon steels, stainless chromium steels, nickel alloys and other materials customary in reactor construction, can be removed solely by mechanical and / or hydraulic action, for example by means of a high-pressure water jet, in order to ensure that they are flawless To achieve decontamination.
  • the solution is then circulated through an ion exchanger and the treated surface is rinsed.
  • Samples a) made of ferritic chromium steel were treated at room temperature (290 to 295 K) for 16 hours with a solution of 0.05 mol of chromic and permanganic acids. After an intermediate rinse, a decontamination factor (ratio of measured activity before and after treatment) of 2 was determined. A further treatment at room temperature in an aqueous 0.1 mol solution of oxalic acid under the influence of ultrasound resulted in a decontamination factor of about 20 after 15 minutes and a decontamination factor of over 100 after 6 hours. After the treatment, the decontaminated surfaces of the samples were metallic bright and attacked neither macroscopically nor microscopically recognizable
  • Samples c) made of nickel-chromium-iron alloy under the trade name INCONEL 600 were treated at room temperature for 16 hours with a solution of 0.1 mol of chromic acid and 0.004 mol of potassium permanganate. After an intermediate rinse, a decontamination factor of only 1.2 was found. After a further treatment at room temperature with an aqueous solution of 0.1 mol oxalic acid for 6 hours with ultrasound exposure, a decontamination factor of 12 was determined.
  • Samples a) made of ferritic chrome steel, samples b) made of austenitic stainless steels and samples c) made of INCOLOY 800 and INCONEL 600 were each in aqueous solutions containing 0.01 to 0.1 mol of chromic acid and 0.001 to 0 for 16 hours at room temperature.
  • the samples were then each treated for 6 hours at room temperature in an aqueous solution with 0.1 mol of oxalic acid under the action of ultrasound.
  • decontamination factors between 10 and 1000 were measured on all samples.
  • Samples a) made of ferritic chromium steel and samples c) made from INCONEL 600 were each treated for 16 hours at room temperature in a solution with 0.1 mol of chromic acid and 0.05 mol of permanganic acid. After a subsequent treatment with a water jet of 2.4 kbar (240 Pa) pressure at a treatment speed of 3.6 m 2 / hour, decontamination factors of about 30 were obtained on samples a) made of ferritic chromium steel and on samples c) made of INCONEL 600 Decontamination factors measured over 100. Extensive follow-up examinations showed that these treatments did not attack the surfaces of the base materials.
  • Samples c) from INCONEL 600 were sprayed for 16 hours at room temperature with a solution of 0.05 mol of chromic acid and 0.002 mol of permanganic acid. After a further treatment with a water jet, as in Example 4, decontamination factors between 20 and 80 were determined.
  • a paste was prepared from an aqueous solution of 0.4 mol of chromic acid and 0.1 mol of permanganic acid by adding a thickener which is available on the market under the trade name AEROSIL (registered trademark of Degussa).
  • AEROSIL registered trademark of Degussa
  • the contaminated surfaces of samples a) made of ferritic chrome steel were coated with this paste. After an exposure time of 16 hours, the samples were treated with a water jet, as in Example 4. Decontamination factors between 5 and 15 resulted.

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (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)
  • Chemical Treatment Of Metals (AREA)

Claims (5)

1. Procédé de décontamination de surfaces, en particulier sur des pièces constitutives de circuits de refroidissement de réacteurs nucléaires, dans lequel, dans une première étape de traitement, on utilise un oxydant pour désagréger les couches superficielles contaminées par radioactivité, et dans une seconde étape de traitement, on enlève les couches superficielles désagrégées à l'aide d'un solvant, procédé caractérisé en ce que l'on utilise, comme oxydant, une solution de décontamination contenant de l'acide chromique et de l'acide permanganique ou de leurs sels, et en ce que l'on ajoute un réducteur à cette solution de décontamination qui est ensuite utilisée pour la deuxième étape de traitement.
2. Procédé selon la revendication 1, caractérisé en ce que l'on réalise la première et/ou la seconde étape de traitement sous l'action d'ultrasons.
3. Procédé selon la revendication 1, caractérisé en ce que, dans la deuxième étape de traitement, les couches superficielles sont enlevées par voie mécanique ou par voie hydraulique.
4. Procédé selon la revendication 1, caractérisé en ce que l'on ajoute des acides organiques et/ou des agents complexants à la solution de décontamination à laquelle on a ajouté le réducteur.
5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que, à la suite de la deuxième étape de traitement, on réutilise la solution de décontamination, après l'avoir fait passer sur un échangeur d'ions, pour rincer les surfaces traitées.
EP88116003A 1987-10-02 1988-09-28 Procédé pour décontaminer des surfaces Expired - Lifetime EP0313843B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH3846/87A CH673545A5 (fr) 1987-10-02 1987-10-02
CH3846/87 1987-10-02

Publications (3)

Publication Number Publication Date
EP0313843A1 EP0313843A1 (fr) 1989-05-03
EP0313843B1 true EP0313843B1 (fr) 1992-07-08
EP0313843B2 EP0313843B2 (fr) 1998-05-13

Family

ID=4264738

Family Applications (1)

Application Number Title Priority Date Filing Date
EP88116003A Expired - Lifetime EP0313843B2 (fr) 1987-10-02 1988-09-28 Procédé pour décontaminer des surfaces

Country Status (8)

Country Link
US (1) US5093073A (fr)
EP (1) EP0313843B2 (fr)
JP (1) JPH02503600A (fr)
KR (1) KR970011260B1 (fr)
CH (1) CH673545A5 (fr)
DE (1) DE3872656D1 (fr)
ES (1) ES2034088T5 (fr)
WO (1) WO1989003113A1 (fr)

Families Citing this family (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4913849A (en) * 1988-07-07 1990-04-03 Aamir Husain Process for pretreatment of chromium-rich oxide surfaces prior to decontamination
DE4232246A1 (de) * 1992-09-25 1994-03-31 Siemens Ag Verfahren zur Zerstörung einer organischen Substanz
US5278743A (en) * 1992-11-20 1994-01-11 Westinghouse Electric Corp. Alkaline-permanganate process
FR2730641B1 (fr) * 1995-02-20 1997-03-14 Commissariat Energie Atomique Mousse de decontamination a l'ozone, et procede de decontamination utilisant cette mousse
US5678232A (en) * 1995-07-31 1997-10-14 Corpex Technologies, Inc. Lead decontamination method
US5591270A (en) * 1995-07-31 1997-01-07 Corpex Technologies, Inc. Lead oxide removal method
CZ233698A3 (cs) * 1996-02-07 1998-12-16 Buckman Laboratories International, Inc. Synergicky antimikrobiální prostředky obsahující ionenový polymer a sůl dodecylaminu a způsoby jeho použití
US5814204A (en) * 1996-10-11 1998-09-29 Corpex Technologies, Inc. Electrolytic decontamination processes
US6183547B1 (en) * 1998-03-05 2001-02-06 The University Of Notre Dame Du Lac Environmentally acceptable inhibitor formulations for metal surfaces
JP2001124891A (ja) * 1999-07-09 2001-05-11 Hitachi Ltd 原子力プラント構造物の表面処理方法および原子力プラント
JP3977963B2 (ja) 1999-09-09 2007-09-19 株式会社日立製作所 化学除染方法
FR2841802B1 (fr) * 2002-07-08 2005-03-04 Commissariat Energie Atomique Composition, mousse et procede de decontamination de surfaces
KR100724710B1 (ko) * 2002-11-21 2007-06-04 가부시끼가이샤 도시바 방사화 부품의 화학적 오염제거 시스템 및 방법
KR20040077390A (ko) * 2003-02-28 2004-09-04 김성진 핵 방사능 잡 고체, 시멘트, 농축 폐 액 드럼을 천일염수와 천일염으로 절게 하여 고온으로 소각시켜 핵 방사능독을 흔적없이 공중 완전 소각 방법과, 농축 천일염(수)폐액 드럼.
JP3945780B2 (ja) * 2004-07-22 2007-07-18 株式会社日立製作所 原子力プラント構成部材の放射性核種の付着抑制方法および成膜装置
DE102009047524A1 (de) * 2009-12-04 2011-06-09 Areva Np Gmbh Verfahren zur Oberflächen-Dekontamination
DE102010028457A1 (de) * 2010-04-30 2011-11-03 Areva Np Gmbh Verfahren zur Oberflächen-Dekontamination
EP3033751B1 (fr) * 2013-08-14 2019-10-23 Framatome GmbH Procédé pour la réduction de la contamination radioactive d'une surface d'une composante utilisée dans un reacteur nucléair
DE102013108802A1 (de) * 2013-08-14 2015-02-19 Areva Gmbh Verfahren zur Verringerung der radioaktiven Kontamination eines wasserführenden Kreislaufs eines Kernkraftwerks
US9440847B2 (en) * 2013-10-03 2016-09-13 POSiFA MICROSYSTEMS, INC. Single silicon wafer micromachined thermal conduction sensor

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3615817A (en) * 1969-02-04 1971-10-26 Atomic Energy Commission Method of decontaminating radioactive metal surfaces
US4217192A (en) * 1979-06-11 1980-08-12 The United States Of America As Represented By The United States Department Of Energy Decontamination of metals using chemical etching
US4481040A (en) * 1981-06-17 1984-11-06 Central Electricity Generating Board Of Sudbury House Process for the chemical dissolution of oxide deposits
US4522928A (en) * 1982-10-18 1985-06-11 Exxon Research And Engineering Co. Removal of metal comtaminants from catalysts using buffered oxalic acid
SE435329B (sv) * 1983-02-09 1984-09-17 Studsvik Energiteknik Ab Dekontaminering av tryckvattenreaktorer
DE3413868A1 (de) * 1984-04-12 1985-10-17 Kraftwerk Union AG, 4330 Mülheim Verfahren zur chemischen dekontamination von metallischen bauteilen von kernreaktoranlagen
US4913849A (en) * 1988-07-07 1990-04-03 Aamir Husain Process for pretreatment of chromium-rich oxide surfaces prior to decontamination

Also Published As

Publication number Publication date
EP0313843A1 (fr) 1989-05-03
KR890702211A (ko) 1989-12-23
EP0313843B2 (fr) 1998-05-13
CH673545A5 (fr) 1990-03-15
ES2034088T3 (es) 1993-04-01
ES2034088T5 (es) 1998-10-01
US5093073A (en) 1992-03-03
KR970011260B1 (ko) 1997-07-08
DE3872656D1 (de) 1992-08-13
WO1989003113A1 (fr) 1989-04-06
JPH02503600A (ja) 1990-10-25

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